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Sample records for polarised neutron diffraction

  1. Polarised neutron scattering from dynamic polarised targets in biology

    NASA Astrophysics Data System (ADS)

    Knop, W.; Hirai, M.; Olah, G.; Meerwinck, W.; Schink, H.-J.; Stuhrman, H. B.; Wagner, R.; Wenkow-EsSouni, M.; Zhao, J.; Schärpf, O.; Crichton, R. R.; Krumpolc, M.; Nierhaus, K. H.; Niinikoski, T. O.; Rijllart, A.

    1991-10-01

    The contrast giving rise to neutron small-angle scattering can be enhanced considerably by polarisation of the hydrogen nuclei [J. des Coizeaux and G. Jannink, Les Polymères en Solution, Les Editions de Physique, F-91944 Les Ulis, France (1987)]. Using polarised neutrons the scattering from protonated labels in a deuterated matrix will increase by an order of magnitude. This is the basis of nuclear spin contrast variation, a method which is of particular interest for the in situ structure determination of macromolecular components. A new polarised target for neutron scattering has been designed by CERN and tested successfully at FRG-1 of the GKSS research centre. For the purpose of thermal-neutron scattering the frozen solutions of biomolecules are immersed in liquid helium 4, which is thermally coupled to the cooling mixture of helium 3/helium 4 of the dilution refrigerator. The nuclear spins are aligned with respect to the external magnetic field-parallel or antiparallel-by dynamic nuclear polarisation (DNP). The gain in neutron scattering compared to earlier experiments using direct cooling of the sample by helium 3 is a factor of 30. Another factor of 30 arises from the installation of the cold source and the beryllium reflector in FRG-1 [W. Knop et al., J. Appl. Cryst. 22 (1989) 352]. Pure nuclear spin targets are produced from dynamic polarised targets by selective depolarisation. In biological material only the hydrogen isotopes contribute significantly to polarised neutron scattering. Thus, saturation of the proton NMR yields a deuteron target, provided the target material has been enriched by the latter isotope. A proton target is obtained from the dynamic polarised target by saturation of deuteron NMR. This leads to six additional scattering functions reflecting the proton and deuteron spin densities and the correlations between the polarised isotopes. Polarised neutron scattering from nuclear spin targets of apoferritin and various derivatives of the

  2. Contributions of the electronic spin and orbital current to the CoCl{sub 4}{sup 2-} magnetic field probed in polarised neutron diffraction experiments

    SciTech Connect

    Cassam-Chenaie, Patrick; Jayatilaka, Dylan

    2012-08-14

    Polarised neutron diffraction experiments conducted at 4.2 K on Cs{sub 3}CoCl{sub 5} crystals have been analysed by using a four-dimensional model Hilbert space made of ab initio n-electron wave functions of the CoCl{sub 4}{sup 2-} molecular ion. Two spin-orbit mixing coefficients and several configuration interaction coefficients have been optimized by fitting calculated magnetic structure factors to experimental ones, to obtain the best ensemble density operator that is representable in the model space. A goodness of fit, {chi}{sup 2}, less then 1 has been obtained for the first time for the two experimental data sets available. In the present article, the optimized density operators are used to calculate the magnetic field densities that are the genuine observables probed in neutron diffraction experiments. Density maps of such observables are presented for the first time and numerical details are provided. The respective contributions of spin density and orbital current to the magnetic field density are analyzed.

  3. Polarised nuclei for neutron science: recent applications and perspectives

    NASA Astrophysics Data System (ADS)

    Glättli, Hans

    2004-08-01

    Neutron scattering on nuclei is spin dependent, particularly strongly for 1H. The means to achieve large nuclear polarisations and its use for structure analysis or as spin-handling device are reviewed. High resolution (diffraction) as well as low resolution (SANS) measurements can benefit from polarised nuclei by changing selectively the form factors of Bragg reflections or the contrasts (the scattering length density profiles) in SANS. The internal structure of ribosomes and the conformation of polymers in solution have been investigated by this method. A numerical simulation is presented to show the influence of steady-state polarisation of protons on the scattering from a protein-ARN model complex. In addition, a more recent technique, time-resolved SANS is described. It makes use of spatial polarisation gradients created around paramagnetic centres at the onset of nuclear polarisation. Such polarisation domains can enhance considerably the scattering amplitude of free radicals and thus contribute to determine their positions inside a complex protein. Examples of possible future experiments are proposed which combine simultaneously the selectivity of solid-state NMR techniques and neutron scattering.

  4. The strange history of polarised neutrons in Australia

    NASA Astrophysics Data System (ADS)

    Hicks, T. J.

    2016-04-01

    The history of polarised neutrons in Australia is unusual firstly because of the particular access that individuals in universities had to the facilities at the reactor site and because this resulted in the experiments being done almost all being with polarisation analysis. Two instruments were initially available. One was a conventional instrument albeit with a tilting counter. The other was a primitive polarisation analysis instrument purpose built for diffuse scattering. This latter instrument evolved over more than thirty years and produced results ranging from the separation of magnetic and nuclear diffuse scattering, for which it was conceived, to the isolation of magnetic features in inelastic spectra.

  5. Spin echo small angle neutron scattering using a continuously pumped {sup 3}He neutron polarisation analyser

    SciTech Connect

    Parnell, S. R.; Li, K.; Yan, H.; Stonaha, P.; Li, F.; Wang, T.; Baxter, D. V.; Snow, W. M.; Washington, A. L.; Walsh, A.; Chen, W. C.; Parnell, A. J.; Fairclough, J. P. A.; Pynn, R.

    2015-02-15

    We present a new instrument for spin echo small angle neutron scattering (SESANS) developed at the Low Energy Neutron Source at Indiana University. A description of the various instrument components is given along with the performance of these components. At the heart of the instrument are a series of resistive coils to encode the neutron trajectory into the neutron polarisation. These are shown to work well over a broad range of neutron wavelengths. Neutron polarisation analysis is accomplished using a continuously operating neutron spin filter polarised by Rb spin-exchange optical pumping of {sup 3}He. We describe the performance of the analyser along with a study of the {sup 3}He polarisation stability and its implications for SESANS measurements. Scattering from silica Stöber particles is investigated and agrees with samples run on similar instruments.

  6. Neutron diffraction on pulsed sources

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

    The current capabilities of 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 have been mainly the emergence of third-generation pulsed sources with a megawatt 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 from F L Shapiro, the centennial of whose birth was celebrated in 2015. The state of the art with respect to neutron sources for studies on extracted beams is reviewed in a special section.

  7. Industrial applications of neutron diffraction

    SciTech Connect

    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.

  8. High-pressure neutron diffraction

    SciTech Connect

    Xu, Hongwu

    2011-01-10

    This lecture will cover progress and prospect of applications of high-pressure neutron diffraction techniques to Earth and materials sciences. I will first introduce general high-pressure research topics and available in-situ high-pressure techniques. Then I'll talk about high-pressure neutron diffraction techniques using two types of pressure cells: fluid-driven and anvil-type cells. Lastly, I will give several case studies using these techniques, particularly, those on hydrogen-bearing materials and magnetic transitions.

  9. Polarisation Analysis Neutron Spectrometer, POLANO, at J-PARC - Concept and Magnetic Field Optimisation

    NASA Astrophysics Data System (ADS)

    Ohoyama, K.; Yokoo, T.; Itoh, S.; Nanbu, M.; Iwasa, K.; Ohkawara, M.; Kaneko, N.; Ino, T.; Hayashida, H.; Oku, T.; Kira, H.; Tasaki, S.; Takeda, M.; Kimura, H.; Sato, T. J.

    2016-04-01

    The status of the polarised neutron spectrometer constructed at the Japan Proton Accelerator Research Complex through a collaboration between Tohoku University and KEK will be reported. In particular, the optimisation of magnetic fields to minimise neutron- beam depolarisation using the finite element method will be discussed on the basis of several simulations using the finite element method.

  10. Structure of hydrogenous liquids: separation of coherent and incoherent cross sections using polarised neutrons

    NASA Astrophysics Data System (ADS)

    Stunault, A.; Vial, S.; Pusztai, L.; Cuello, G. J.; Temleitner, L.

    2016-04-01

    The determination of the coherent structure factor of hydrogenous liquids is very difficult: while X-rays are barely sensitive to hydrogen, neutrons results still lack accuracy due to the contamination of the scattering intensities by a huge spin-incoherent signal from the 1H atoms. Using polarised neutrons with polarisation analysis, one can experimentally separate the coherent and incoherent contributions to the scattered intensity. We present the upgrade of the D3 polarised hot neutron diffractometer at ILL to study hydrogenated liquids. We show first data obtained from a test sample of water and detail the data reduction leading to an unprecedented accuracy in the extraction of the coherent signal, representative of the structure.

  11. Optimizing Crystal Volume for Neutron Diffraction

    NASA Technical Reports Server (NTRS)

    Snell, Edward H.; vanderWoerd, Mark; Damon, Michael; Judge, Russell, A.; Myles, Dean; Meilleur, F.

    2006-01-01

    Neutron diffraction is uniquely sensitive to hydrogen positions and protonation state. In that context structural information from neutron data is complementary to that provided through X-ray diffraction. However, there are practical obstacles to overcome in fully exploiting the potential of neutron diffraction, Le. low flux and weak scattering. Several approaches are available to overcome these obstacles and we have investigated the simplest: increasing the diffracting volume of the crystals. Volume is a quantifiable metric that is well suited for experiment design and optimization techniques. By using response surface methods we have optimized xylose isomerase crystal volume, enabling neutron diffraction while we determined the crystallization parameters with the minimum of experiments. Our results suggest a systematic means of enabling neutron diffraction studies for a larger number of samples that require information on hydrogen position and/or protonation state.

  12. High-Accuracy Analysis of Compton Scattering in Chiral EFT: Proton and Neutron Polarisabilities

    NASA Astrophysics Data System (ADS)

    Griesshammer, Harald W.; Phillips, Daniel R.; McGovern, Judith A.

    2013-10-01

    Compton scattering from protons and neutrons provides important insight into the structure of the nucleon. A new extraction of the static electric and magnetic dipole polarisabilities αE 1 and βM 1 of the proton and neutron from all published elastic data below 300 MeV in Chiral Effective Field Theory shows that within the statistics-dominated errors, the proton and neutron polarisabilities are identical, i.e. no iso-spin breaking effects of the pion cloud are seen. Particular attention is paid to the precision and accuracy of each data set, and to an estimate of residual theoretical uncertainties. ChiEFT is ideal for that purpose since it provides a model-independent estimate of higher-order corrections and encodes the correct low-energy dynamics of QCD, including, for few-nucleon systems used to extract neutron polarisabilities, consistent nuclear currents, rescattering effects and wave functions. It therefore automatically respects the low-energy theorems for photon-nucleus scattering. The Δ (1232) as active degree of freedom is essential to realise the full power of the world's Compton data.Its parameters are constrained in the resonance region. A brief outlook is provided on what kind of future experiments can improve the database. Supported in part by UK STFC, DOE, NSF, and the Sino-German CRC 110.

  13. X-ray Polarisation in highly-magnetized neutron stars

    NASA Astrophysics Data System (ADS)

    Turolla, Roberto

    2016-07-01

    Radiation emitted in the vicinity of an isolated neutron star is expected to be intrinsically polarized because the high magnetic field (B˜10^{12}-10^{15} G) strongly affects the plasma opacity. The polarization fraction and polarization angle measured by an instrument, however, do not necessary coincide with the intrinsic ones, due to the effects of both quantum electrodynamics in the highly magnetized vacuum around the star (the vacuum polarization) and rotation of the Stokes parameters in the plane perpendicular to the line of sight induced by the non-uniform magnetic field. I'll review theoretical estimates for the polarization observables in the case of thermal surface emission from neutron stars and of the (soft) X-ray emission from magnetars, where magnetospheric reprocessing of radiation by resonant cyclotron scattering is important. The potentials of X-ray polarimetry to probe the physical conditions in neutron star sources and to test, for the first time, vacuum polarization are discussed in connection with the recently proposed polarimetric missions, like XIPE.

  14. A New High-Accuracy Analysis of Compton Scattering in Chiral EFT: Neutron Polarisabilities

    NASA Astrophysics Data System (ADS)

    Griesshammer, Harald W.; McGovern, Judith A.; Phillips, Daniel R.

    2015-04-01

    Low-energy Compton scattering tests the symmetries and interaction strengths of a target's internal degrees of freedom in the electric and magnetic fields of a real, external photon. In the single-nucleon sector, information is often compressed into the static scalar dipole polarisabilities which are experimentally not directly accessible but encode information on the pion cloud and the Δ(1232) excitation. The interaction of the photon with the charged pion-exchange also provides a conceptually clean probe of few-nucleon binding. After demonstrating the statistical consistency of the world's γd dataset including the new data from the MAX-IV collaboration described in the preceding talk, we present a new extraction of the neutron polarisabilities in Chiral Effective Field Theory: αn = [ 11 . 55 +/- 1 . 25(stat) +/- 0 . 2(BSR) +/- 0 . 8(th) ] and βn = [ 3 . 65 -/+ 1 . 25(stat) +/- 0 . 2(BSR) -/+ 0 . 8(th) ] , in 10-4 fm3, with χ2 = 45 . 2 for 44 degrees of freedom. The new data reduced the statistical uncertainties by 30%. We discuss data accuracy and consistency, the role of the Δ(1232) , and an estimate of residual theoretical uncertainties. Within statistical and systematic errors, proton and neutron polarisabilities remain identical. Supported in part by UK STFC and US DOE.

  15. Pulsed neutron diffraction in special sample environments

    SciTech Connect

    Jorgensen, J.D.

    1987-05-01

    Neutron diffraction is a powerful tool for structural studies of samples in special sample environments because of the high penetrating power of neutrons compared to x rays. The neutrons readily penetrate special sample containers, heat shields, pressure vessels, etc., making it unnecessary in most cases to compromise the effectiveness of the sample environment system by providing windows for the incident and scattered neutrons. Pulsed neutrons obtained from an accelerator-based pulsed neutron source offer the additional advantage that many diffraction experiments can be done at a single, fixed scattering angle by the time-of-flight technique. In the fixed-angle scattering geometry, shielding and collimation can be optimized in order to access the largest possible sample volume with neutrons while completely avoiding scattering from the surrounding sample vessel. Thus, the data are free from unwanted background scattering. In this paper, the basic principles of neutron diffraction in special sample environments are discussed and examples of apparatus used for neutron diffraction measurements at low temperature, high temperature, and high pressure are presented. 36 refs., 15 figs., 3 tabs.

  16. Oxygen as a site specific structural probe in neutron diffraction

    SciTech Connect

    Neuefeind, Joerg C; Simonson, J Michael {Mike}; Salmon, Phil; Zeidler, Anita; Fischer, Henry E; Rauch, Helmut; Markland, Thomas; Lemmel, Hartmut

    2011-01-01

    Oxygen is a ubiquitous element, playing an essential role in most scientific and technological disciplines, and is often incorporated within a structurally disordered material where examples include molten silicates in planetary science, glasses used for lasers and optical communication, and water in biological processes. Establishing the structure of a liquid or glassy oxide and thereby its relation to the functional properties of a material is not, however, a trivial task owing to the complexity associated with atomic disorder. Here we approach this challenge by measuring the bound coherent neutron scattering lengths of the oxygen isotopes with the sensitive technique of neutron interferometry. We find that there is a small but finite contrast of 0.204(6) fm between the scattering lengths of the isotope 18O and oxygen of natural isotopic abundance natO, contrary to tables of recommended values. This has enabled us to investigate the structure of both light and heavy water by exploiting, for the first time, the method of oxygen isotope substitution in neutron diffraction, thus circumventing many of the significant problems associated with more traditional methods in which hydrogen is substituted by deuterium. We find a difference of ~0.5% between the O-H and O-D intra-molecular bond distances which is much smaller than recent estimates based on diffraction data and is found to be in excellent agreement with path integral molecular dynamics simulations made with a flexible polarisable water model. Our results demonstrate the potential for using oxygen isotope substitution as a powerful and effective site specific probe in a plethora of materials, of pertinence as instrumentation at next generation neutron sources comes online

  17. Optimizing Crystal Volume for Neutron Diffraction Studies

    NASA Technical Reports Server (NTRS)

    Snell, E. H.

    2003-01-01

    For structural studies with neutron diffraction more intense neutron sources, improved sensitivity detector and larger volume crystals are all means by which the science is being advanced to enable studies on a wider range of samples. We have chosen a simplistic approach using a well understood crystallization method, with minimal amounts of sample and using design of experiment techniques to maximize the crystal volume all for minimum effort. Examples of the application are given.

  18. SPECIAL ISSUE DEVOTED TO THE 80TH ANNIVERSARY OF ACADEMICIAN N G BASOV'S BIRTH: An optically polarised dense 3He target as a spin filter for slow-neutron beams

    NASA Astrophysics Data System (ADS)

    Kolachevsky, Nikolai N.; Prokof'ichev, Yu V.; Skoi, V. R.; Sobel'man, Igor I.; Sorokin, Vadim N.

    2003-01-01

    The possibility of polarising 3He and preserving the polarisation in an external magnetic field of 0.05 Oe is demonstrated experimentally. A neutron filter with an extremely weak guiding field is fabricated for obtaining polarised neutron beams. The degree of polarisation equal to 25% was obtained for 0.025-eV neutrons. Some fields of application of other polarised noble gases are considered. The cross section for cross-relaxation of nuclear polarisation in the 129Xe — 131Xe mixture is estimated.

  19. Spectroscopy of ultracold neutrons diffracted by a moving grating

    NASA Astrophysics Data System (ADS)

    Kulin, G. V.; Frank, A. I.; Goryunov, S. V.; Geltenbort, P.; Jentschel, M.; Bushuev, V. A.; Lauss, B.; Schmidt-Wellenburg, P.; Panzarella, A.; Fuchs, Y.

    2016-03-01

    Spectra of ultracold neutrons that appeared in experiments on neutron diffraction by a moving grating were measured using the time-of-flight Fourier spectrometer. Diffraction lines of five orders were observed simultaneously. The obtained data are in good agreement with the theoretical predictions based on the multiwave dynamical theory of neutron diffraction by a moving grating.

  20. A neutron diffraction study of amorphous boron

    NASA Astrophysics Data System (ADS)

    Delaplane, R. G.; Lundström, T.; Dahlborg, U.; Howells, W. S.

    1991-07-01

    The structure of amorphous boron has been studied with pulsed neutron diffraction techniques using the ISIS facilities at the Rutherford Appleton Laboratory. The experimental static structure factor S(Q) and radial distribution function support a structural model based on units of B12 icosahedra resembling those found in crystalline β-rhombohedral boron, but with a certain degree of disorder occurring in the linking between these subunits.

  1. DNA hydration studied by neutron fiber diffraction

    SciTech Connect

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

    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.

  2. Neutron Laue diffraction in macromolecular crystallography

    NASA Astrophysics Data System (ADS)

    Myles, D. A. A.; Bon, C.; Langan, P.; Cipriani, F.; Castagna, J. C.; Lehmann, M. S.; Wilkinson, C.

    The time scales required for conventional neutron diffraction analysis of biological single crystals at, or near, atomic resolution are prohibitive - such studies are rarely performed. Laue (white beam) diffraction can provide a more rapid and efficient survey of reciprocal space, maximising the flux at the sample and stimulating large numbers of reflections simultaneously. A LAue DIffractometer (LADI), designed specifically for macromolecular crystallography, has been installed on a cold neutron guide at ILL. The detector comprises a large Gd 2O 3-doped neutron-sensitive image plate (400 × 800 mm) mounted on a cylindrical camera (318 mm diameter) that is read in phonographic mode after exposure. Detector response has been evaluated and performance indicators are given. Narrow (Quasi-Laue) band-passes (d/ gl/ λ = 8-20%) are often required for large unit-cell biological crystals in order to reduce reflection overlap and incoherent background. Laue and Quasi-Laue data have now been collected for a number of proteins and other biological crystals. Recent results are presented and future prospects reviewed.

  3. Unraveling protein catalysis through neutron diffraction

    NASA Astrophysics Data System (ADS)

    Myles, Dean

    Neutron scattering and diffraction are exquisitely sensitive to the location, concentration and dynamics of hydrogen atoms in materials and provide a powerful tool for the characterization of structure-function and interfacial relationships in biological systems. Modern neutron scattering facilities offer access to a sophisticated, non-destructive suite of instruments for biophysical characterization that provide spatial and dynamic information spanning from Angstroms to microns and from picoseconds to microseconds, respectively. Applications range from atomic-resolution analysis of individual hydrogen atoms in enzymes, through to multi-scale analysis of hierarchical structures and assemblies in biological complexes, membranes and in living cells. Here we describe how the precise location of protein and water hydrogen atoms using neutron diffraction provides a more complete description of the atomic and electronic structures of proteins, enabling key questions concerning enzyme reaction mechanisms, molecular recognition and binding and protein-water interactions to be addressed. Current work is focused on understanding how molecular structure and dynamics control function in photosynthetic, cell signaling and DNA repair proteins. We will highlight recent studies that provide detailed understanding of the physiochemical mechanisms through which proteins recognize ligands and catalyze reactions, and help to define and understand the key principles involved.

  4. Status of the Neutron Imaging and Diffraction Instrument IMAT

    NASA Astrophysics Data System (ADS)

    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.

  5. Growing Larger Crystals for Neutron Diffraction

    NASA Technical Reports Server (NTRS)

    Pusey, Marc

    2003-01-01

    Obtaining crystals of suitable size and high quality has been a major bottleneck in macromolecular crystallography. With the advent of advanced X-ray sources and methods the question of size has rapidly dwindled, almost to the point where if one can see the crystal then it was big enough. Quality is another issue, and major national and commercial efforts were established to take advantage of the microgravity environment in an effort to obtain higher quality crystals. Studies of the macromolecule crystallization process were carried out in many labs in an effort to understand what affected the resultant crystal quality on Earth, and how microgravity improved the process. While technological improvements are resulting in a diminishing of the minimum crystal size required, neutron diffraction structural studies still require considerably larger crystals, by several orders of magnitude, than X-ray studies. From a crystal growth physics perspective there is no reason why these 'large' crystals cannot be obtained: the question is generally more one of supply than limitations mechanism. This talk will discuss our laboratory s current model for macromolecule crystal growth, with highlights pertaining to the growth of crystals suitable for neutron diffraction studies.

  6. Neutron diffraction studies of natural glasses

    SciTech Connect

    Wright, A.C.; Erwin Desa, J.A.; Weeks, R.A.; Sinclair, R.N.; Bailey, D.K.

    1983-08-01

    A neutron diffraction investigation has been carried out of the structures of several naturally occurring glasses, viz. Libyan Desert glass, a Fulgurite, Wabar glass, Lechatelierite from Canon Diablo, a Tektite, Obsidian (3 samples), and Macusani glass. Libyan Desert sand has also been examined, together with crystalline ..cap alpha..-quartz and ..cap alpha..-cristobalite. A comparison of data for the natural glasses and synthetic vitreous silica (Spectrosil B) in both reciprocal and real space allows a categorisation into Silicas, which closely resemble synthetic vitreous silica, and Silicates, for which the resemblance to silica is consistently less striking. The data support the view that Libyan Desert glass and sand have a common origin, while the Tektite has a structure similar to that of volcanic glasses.

  7. Pulsed Neutron Powder Diffraction for Materials Science

    SciTech Connect

    Kamiyama, T.

    2008-03-17

    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 {delta}d/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 A{sup -1}

  8. Pulsed Neutron Powder Diffraction for Materials Science

    NASA Astrophysics Data System (ADS)

    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-1

  9. Neutron diffraction studies of viral fusion peptides

    NASA Astrophysics Data System (ADS)

    Bradshaw, Jeremy P.; J. M. Darkes, Malcolm; Katsaras, John; Epand, Richard M.

    2000-03-01

    Membrane fusion plays a vital role in a large and diverse number of essential biological processes. Despite this fact, the precise molecular events that occur during fusion are still not known. We are currently engaged on a study of membrane fusion as mediated by viral fusion peptides. These peptides are the N-terminal regions of certain viral envelope proteins that mediate the process of fusion between the viral envelope and the membranes of the host cell during the infection process. As part of this study, we have carried out neutron diffraction measurements at the ILL, BeNSC and Chalk River, on a range of viral fusion peptides. The peptides, from simian immunodeficiency virus (SIV), influenza A and feline leukaemia virus (FeLV), were incorporated into stacked phospholipid bilayers. Some of the peptides had been specifically deuterated at key amino acids. Lamellar diffraction data were collected and analysed to yield information on the peptide conformation, location and orientation relative to the bilayer.

  10. Neutron Diffraction Studies of Carbonate Apatite

    NASA Astrophysics Data System (ADS)

    Moghaddam, Hadi Y.; Leventouri, Theodora; Chakoumakos, Bryan C.

    1998-11-01

    Moghaddam H.Y., Leventouri Th.* (Dept. of Physics & Alloy Research Center, Florida Atlantic Univ.) Chakoumakos B.C. (Solid State Division, Oak Ridge National Lab.**,kou@ornl.gov) We report Rietveld structural refinements of neutron diffraction data of a highly crystalline, single-phase natural carbonate apatite,(francolite of Epirus, Greece), in order to elucidate the details of carbonate substitution in the apatites. The composition is Ca9.56Na0.38Mg0.08(PO4)4.82(CO3)0.946(SO4)0.2F2.34, as determined by electron microprobe analysis. We report refinements of data for the native francolite as a function of temperature between 296K and 10K after the material had been heated at 750 °C to drive off adsorbed water and CO2. The neutron diffractioii@data were collected using a wavelength 1.0912 A on the HB4 high resolution powder diffractometer at the High Flux Isotope Reactor at Oak Ridge National Laboratory. Analysis of the temperature dependence of the anisotropic displacement parameters can reveal the contribution from the temperature independent static positional disorder. Difference displacement parameters evaluated along various bonding directions are being used to describe the mechanics and dynamics of the carbonate for phosphate substitution.*Supported by a SURA-ORNL Summer Cooperative Research Program 1998.**Supported by the Division of Materials Sciences,U.S. D.O.E. (contract DE-AC05-96OR22464 with Lockheed Martin Energy Research Corporation).

  11. Structure of yttrium cobaltate from neutron diffraction

    SciTech Connect

    Mehta, A.; Berliner, R.; Smith, R.W.

    1997-05-01

    The crystal structure of YCoO{sub 3} has been determined from Rietveld analysis of the powder neutron diffraction data at 17, 100, and 300 K. At each temperature, the structure is a distorted perovskite with orthorhombic symmetry, space group Pbnm (Z = 4). The lattice parameters, at 300 K, are 5.1388 (5) x 5.4191(5) x 7.3658(7) {angstrom}. Structural analysis indicates that the formal valence of cobalt in YCoO{sub 3} is +3. Analysis of the Co-O distances and the absence of magnetic structure indicates that the majority of the Co{sup 3+} ions in YCoO{sub 3} are in the low-spin (i.e. t{sub 2g}{sup 6}e{sub g}{sup 0}) state. The data also show that perhaps 10% of the CO{sup 3+} ions at 300 K (but insignificant fractions at 100 and 17 K) are in the high-spin state.

  12. Future directions in high-pressure neutron diffraction

    NASA Astrophysics Data System (ADS)

    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.

  13. Cold neutron diffraction contrast tomography of polycrystalline material.

    PubMed

    Peetermans, S; King, A; Ludwig, W; Reischig, P; Lehmann, E H

    2014-11-21

    Traditional neutron imaging is based on the attenuation of a neutron beam through scattering and absorption upon traversing a sample of interest. It offers insight into the sample's material distribution at high spatial resolution in a non-destructive way. In this work, it is expanded to include the diffracted neutrons that were ignored so far and obtain a crystallographic distribution (grain mapping). Samples are rotated in a cold neutron beam of limited wavelength band. Projections of the crystallites formed by the neutrons they diffract are captured on a two dimensional imaging detector. Their positions on the detector reveal their orientation whereas the projections themselves are used to reconstruct the shape of the grains. Indebted to established synchrotron diffraction contrast tomography, this 'cold neutron diffraction contrast tomography' is performed on recrystallized aluminium for experimental comparison between both. Differences between set-up and method are discussed, followed by the application range in terms of sample properties (crystallite size and number, mosaicity and typical materials). Neutron diffraction contrast tomography allows to study large grains in bulky metallic structures. PMID:25274183

  14. Future directions in high-pressure neutron diffraction.

    PubMed

    Guthrie, M

    2015-04-22

    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. PMID:25789450

  15. A low temperature X-ray single-crystal diffraction and polarised infra-red study of epidote

    NASA Astrophysics Data System (ADS)

    Gatta, G. Diego; Alvaro, Matteo; Bromiley, Geoffrey

    2012-01-01

    The effects of low-temperature on the crystal structure of a natural epidote [Ca1.925Fe0.745Al2.265Ti0.004Si3.037O12(OH), a = 8.8924(7), b = 5.6214(3), c = 10.1547(6)Å and β = 115.396(8)° at room conditions, Sp. Gr. P21 /m] have been investigated with a series of structure refinements down to 100 K on the basis of X-ray single-crystal diffraction data. The reflection conditions confirm that the space group is maintained within the T-range investigated. Structural refinements at all temperatures show the presence of Fe3+ at the octahedral M(3) site only [%Fe(M3) = 70.6(4)% at 295 K]. Only one independent proton site was located and two possible H-bonds occur, with O(10) as donor and O(4) and O(2) as acceptors. The H-bonding scheme is maintained down to 100 K and is supported by single crystal room- T polarised FTIR data. FTIR Spectra over the region 4,000-2,500 cm-1 are dominated by the presence of a strongly pleochroic absorption feature which can be assigned to protonation of O(10)-O(4). Previously unobserved splitting of this absorption features is consistent with a NNN influence due to the presence of Al and Fe3+ on the nearby M(3) site. An additional relatively minor absorption feature in FTIR spectra can be tentatively assigned to protonation of O(10)-O(2). Low- T does not affect significantly the tetrahedral and octahedral bond distances and angles, even when distances are corrected for "rigid body motions". A more significant effect is observed for the bond distances of the distorted Ca(1)- and Ca(2)-polyhedra, especially when corrected for "non-correlated motion". The main low- T effect is observed on the vibrational regime of the atomic sites, and in particular for the two Ca-sites. A significant reduction of the magnitude of the thermal displacement ellipsoids, with a variation of U eq (defined as one-third of the trace of the orthogonalised U ij tensor) by ~40% is observed for the Ca-sites between 295 and 100 K. Within the same T-range, the U eq of

  16. Macromolecular structure phasing by neutron anomalous diffraction

    PubMed Central

    Cuypers, Maxime G.; Mason, Sax A.; Mossou, Estelle; Haertlein, Michael; Forsyth, V. Trevor; Mitchell, Edward P.

    2016-01-01

    In this report we show for the first time that neutron anomalous dispersion can be used in a practical manner to determine experimental phases of a protein crystal structure, providing a new tool for structural biologists. The approach is demonstrated through the use of a state-of-the-art monochromatic neutron diffractometer at the Institut Laue-Langevin (ILL) in combination with crystals of perdeuterated protein that minimise the level of hydrogen incoherent scattering and enhance the visibility of the anomalous signal. The protein used was rubredoxin in which cadmium replaced the iron at the iron-sulphur site. While this study was carried out using a steady-state neutron beam source, the results will be of major interest for capabilities at existing and emerging spallation neutron sources where time-of-flight instruments provide inherent energy discrimination. In particular this capability may be expected to offer unique opportunities to a rapidly developing structural biology community where there is increasing interest in the identification of protonation states, protein/water interactions and protein-ligand interactions – all of which are of central importance to a wide range of fundamental and applied areas in the biosciences. PMID:27511806

  17. Macromolecular structure phasing by neutron anomalous diffraction.

    PubMed

    Cuypers, Maxime G; Mason, Sax A; Mossou, Estelle; Haertlein, Michael; Forsyth, V Trevor; Mitchell, Edward P

    2016-01-01

    In this report we show for the first time that neutron anomalous dispersion can be used in a practical manner to determine experimental phases of a protein crystal structure, providing a new tool for structural biologists. The approach is demonstrated through the use of a state-of-the-art monochromatic neutron diffractometer at the Institut Laue-Langevin (ILL) in combination with crystals of perdeuterated protein that minimise the level of hydrogen incoherent scattering and enhance the visibility of the anomalous signal. The protein used was rubredoxin in which cadmium replaced the iron at the iron-sulphur site. While this study was carried out using a steady-state neutron beam source, the results will be of major interest for capabilities at existing and emerging spallation neutron sources where time-of-flight instruments provide inherent energy discrimination. In particular this capability may be expected to offer unique opportunities to a rapidly developing structural biology community where there is increasing interest in the identification of protonation states, protein/water interactions and protein-ligand interactions - all of which are of central importance to a wide range of fundamental and applied areas in the biosciences. PMID:27511806

  18. Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

    NASA Technical Reports Server (NTRS)

    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.

  19. Magnetic structures of actinide materials by pulsed neutron diffraction

    SciTech Connect

    Lawson, A.C.; Goldstone, J.A.; Huber, J.G.; Giorgi, A.L.; Conant, J.W.; Severing, A.; Cort, B.; Robinson, R.A.

    1990-01-01

    We describe some attempts to observe magnetic structure in various actinide (5f-electron) materials. Our experimental technique is neutron powder diffraction as practiced at a spallation (pulsed) neutron source. We will discuss our investigations of {alpha}-Pu, {delta}-Pu, {alpha}-UD{sub 3} and {beta}-UD{sub 3}. {beta}-UD{sub 3} is a simple ferromagnet: surprisingly, the moments on the two non-equivalent uranium atoms are the same within experimental error. {alpha}-UD{sub 3}, {alpha}-Pu and {delta}-Pu are non-magnetic, within the limits of our observations. Our work with pulsed neutron diffraction shows that it is a useful technique for research on magnetic materials.

  20. Grazing incidence neutron diffraction from large scale 2D structures

    SciTech Connect

    Toperverg, B. P.; Felcher, G. P.; Metlushko, V. V.; Leiner, V.; Siebrecht, R.; Nikonov, O.

    2000-01-13

    The distorted wave Born approximation (DWBA) is applied to evaluate the diffraction pattern of neutrons (or X-rays) from a 2D array of dots deposited onto a dissimilar substrate. With the radiation impinging on the surface at a grazing incidence angle {alpha}, the intensities diffracted both in and out the plane of specular reflection are calculated as a function of the periodicity of the array, height and diameter of the dots. The results are presented in the form of diffracted intensity contours in a plane with coordinates {alpha} and {alpha}{prime}, the latter being the glancing angle of scattering. The optimization of the experimental conditions for polarized neutron experiments on submicron dots is discussed. The feasibility of such measurements is confirmed by a test experiment.

  1. Feasibility studies for high pressure neutron powder diffraction experiments

    SciTech Connect

    Von Dreele, R.B. ); Parise, J. )

    1990-01-01

    We recently performed two neutron powder diffraction experiments on very small samples on the High Intensity Powder Diffractometer (HIPD). These were done to determine the feasibility of performing in situ high pressure/high temperature neutron diffraction experiments on HIPD at pressures which would exceed the previous limit of {approximately}50 kbar achievable in a neutron diffraction experiment. The first experiment consisted of examining the product from a high pressure preparation done at Stony Brook. The sample, which had been prepared at 65 kbar and 1000{degree}C, consisted of a small platinum capsule filled with CaGeO{sub 3} perovskite. The weights of the capsule included 225 mg of platinum and 49 mg of the germanate. A diffraction experiment taking {approximately}8.6 hrs at a LANSCE proton beam current of {approximately}53 {mu}A gave peaks of good intensity from both Pt and CaGeO{sub 3}; we could begin to see them after only 20 min of beam time. The second experiment was to test the possibility of diffraction from a high pressure apparatus. We placed in the HIPD sample position the central assembly from a 100 kbar octahedral press. Four tungsten carbide anvils and a copper block previously pressed to 65 kbar were held in an aluminum frame. The sample consisted of a small bit of nickel foil (175 mg) placed in a 3 mm hole in the copper block. The active sample volume is defined by the gap between the anvils and the length of the sample. A small portion of the copper block is also seen in this arrangement. This is viewed at 90{degree} 2{Theta} through a similar gap between the anvils by 4 1/2 in. {times} 12 in. {sup 3}He counter tubes. This arrangement simulates the operating conditions of a high pressure run at 100 kbar and takes advantage of the fixed instrument geometry possible in time-of-flight neutron diffraction experiments.

  2. Neutron Laue diffraction studies of coenzyme cob(II)alamin.

    PubMed

    Langan, P; Lehmann, M; Wilkinson, C; Jogl, G; Kratky, C

    1999-01-01

    Using a recently designed neutron single-crystal diffractometer utilizing a narrow-band Laue concept (LADI), diffraction data were collected from a crystal of the coenzyme cob(II)alamin (B12r), crystallized from a mixture of D2O and perdeuterated acetone. The instrument was placed at the end of a cold neutron guide at the Institute Laue Langevin (ILL, Grenoble, France), and data collection with neutrons of 1.8-8.0 A wavelength to a crystallographic resolution of 1.43 A was complete after about 36 h. This compares favourably with a previous experiment utilizing the same crystal specimen, where more than four weeks were required to collect monochromatic diffraction data to about 1 A resolution. Using the Laue data, the structure was solved by molecular replacement with the known X-ray crystal structure. Difference density maps revealed the atomic positions (including deuterium atoms) of seven ordered solvent water molecules and two (partially disordered) acetone molecules. These density maps were compared with corresponding maps computed with monochromatic neutron-diffraction data collected to 1. 0 A resolution using the same crystal specimen, as well as to maps derived from high-resolution (0.90 A) synchrotron X-ray data. In spite of the better definition of atomic positions in the two high-resolution maps, the 1.43 A LADI maps show considerable power for the determination of the location of hydrogen and deuterium positions. PMID:10089394

  3. The structure of liquid fluorosulfuric acid investigated by neutron diffraction

    NASA Astrophysics Data System (ADS)

    McLain, S. E.; Benmore, C. J.; Turner, J. F. C.

    2002-08-01

    The results of an investigation into the liquid structure of fluorosulfuric acid measured using neutron diffraction with isotopic substitution are reported. The first-order neutron difference function is extracted from data recorded at 300 and 193 K from isotopically labeled FSO3H and FSO3D. Analysis of the derived radial distribution functions shows that unique, multisite hydrogen bonding is present in the liquid. These results suggest hydrogen bonding between the hydrogen and fluorine as well as oxygen occurs in the liquid. The fraction of molecules that is hydrogen bound in each way varies with temperature, with the 193 K data showing a more tightly bound system.

  4. Neutron diffraction study of the deuterides of Ti Mo alloys

    NASA Astrophysics Data System (ADS)

    Sun, Kai; Yuan, Xuezhong; Wu, Erdong; Chen, Dongfeng; Gou, Cheng

    2006-11-01

    The structures of the deuterides of seven Ti-Mo alloys with different Mo contents ranging from 5 to 40 at% are studied by neutron diffraction. After deuterization at ∼150 kPa, the saturated deuterides containing ∼1.8-1.9 deuterium per alloy atom with a δ-phase titanium hydride type of structure have formed. The lattice constants of the deuterides decrease consistently with the increase of Mo content. The analysis of the line broadening of the diffraction patterns has revealed the relationship between lattice deformation and the contents of the alloying Mo in the deuterides.

  5. Investigation of Acrylic Acid at High Pressure Using Neutron Diffraction

    PubMed Central

    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 rationalized using the Pixel method. Acrylic acid undergoes a reconstructive phase transition to a new phase at ∼0.8 GPa and remains molecular to 7.2 GPa before polymerizing on decompression to ambient pressure. The resulting product is analyzed via Raman and FT-IR spectroscopy and differential scanning calorimetry and found to possess a different molecular structure compared with polymers produced via traditional routes. PMID:24650085

  6. Structural molecular biology: Recent results from neutron diffraction

    NASA Astrophysics Data System (ADS)

    Timmins, Peter A.

    1995-02-01

    Neutron diffraction is of importance in structural biology at several different levels of resolution. In most cases the unique possibility arising from deuterium labelling or contrast variation is of fundamental importance in providing information complementary to that which can be obtained from X-ray diffraction. At high resolution, neutron crystallography of proteins allows the location of hydrogen atoms in the molecule or of the hydration water, both of which may be central to biological activity. A major difficulty in this field has been the poor signal-to-noise ratio of the data arising not only from relatively low beam intensities and small crystals but, most importantly from the incoherent background due to hydrogen atoms in the sample. Modern methods of molecular biology now offer ways of producing fully deuterated proteins by cloning in bacteria grown on fully deuterated media. At a slightly lower resolution, there are a number of systems which may be ordered in one or two dimensions. This is the case in the purple membrane where neutron diffraction with deuterium labelling has complemented high resolution electron diffraction. Finally there is a class of very large macromolecular systems which can be crystallised and have been studied by X-ray diffraction but in which part of the structure is locally disordered and usually has insufficient contrast to be seen with X-rays. In this case the use of H 2O/D 2O contrast variation allows these components to be located. Examples of this are the nucleic acid in virus structures and detergent bound to membrane proteins.

  7. Diffraction measurements with a boron-based GEM neutron detector

    NASA Astrophysics Data System (ADS)

    Croci, Gabriele; Albani, Giorgia; Cazzaniga, Carlo; Perelli Cippo, Enrico; Schooneveld, Erik; Claps, Gerardo; Cremona, Anna; Grosso, Giovanni; Muraro, Andrea; Murtas, Fabrizio; Rebai, Marica; Scherillo, Antonella; Tardocchi, Marco; Gorini, Giuseppe

    2014-07-01

    The research of reliable substitutes of 3He detectors is an important task for the affordability of new neutron scattering instrumentation for future spallation sources like the European Spallation Source. GEM (Gas Electron Multiplier)-based detectors represent a valid alternative since they can combine high-rate capability, coverage of up to 1\\ \\text{m}^{2} area and good intrinsic spatial resolution (for this detector class it can be better than 0.5 mm). The first neutron diffraction measurements performed using a borated GEM detector are reported. The detector has an active area of 10 \\times 5\\ \\text{cm}^{2} and is equipped with a borated cathode. The GEM detector was read out using the standard ISIS Data Acquisition System. The comparison with measurements performed with standard 3He detectors shows that the broadening of the peaks measured on the diffractogram obtained with the GEM is 20-30% wider than the one obtained by 3He tubes but the active area of the GEM is twice that of 3He tubes. The GEM resolution is improved if half of its active area is considered. The signal-to-background ratio of the GEM is about 1.5 to 2 times lower than that of 3He. This measurement proves that GEM detectors can be used for neutron diffraction measurements and paves the way for their use at future neutron spallation sources.

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

    SciTech Connect

    Clausen, Bjorn; Brown, Donald W; Tome, Carlos N; Balogh, Levente; Vogel, Sven C

    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.

  9. Polarisation of Light

    NASA Astrophysics Data System (ADS)

    Spottiswoode, William

    2015-01-01

    Preface; 1. Methods of polarisation; 2. Double refraction: polariscopes; 3. Chromatic polarisation: the wave theory; 4. Circular polarisation; 5. Circular polarisation by reflexion; 6. Phenomena produced by mechanical means: unannealed glass; 7. Atmospheric and other polarisation: the polar clock; 8. Rings and brushes produced by crystal plates; 9. Composition of colours by polarised light; Index.

  10. Neutron Diffraction Studies of Intercritically Austempered Ductile Irons

    SciTech Connect

    Druschitz, Alan; Aristizabal, Ricardo; Druschitz, Edward; Hubbard, Camden R; Watkins, Thomas R

    2011-01-01

    Neutron diffraction is a powerful tool that can be used to identify the phases present and to measure the spacing of the atomic planes in a material. Thus, the residual stresses can be determined within a component and/or the phases present. New intercritically austempered irons rely on the unique properties of the austenite phase present in their microstructures. If these materials are to see widespread use, methods to verify the quality (behavior consistency) of these materials and to provide guidance for further optimization will be needed. Neutron diffraction studies were performed at the second generation neutron residual stress facility (NRSF2) at the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory on a variety of intercritically austempered irons. For similar materials, such as TRIP steels, the strengthening mechanism involves the transformation of metastable austenite to martensite during deformation. For the intercritically austempered ductile irons two different deformation/strengthening mechanisms, phase transformation and slip, dependent upon the iron chemistry, were observed. Lattice strain and phase fraction data as a function of applied stress are presented.

  11. Carbonation profiles in cement paste analyzed by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Galan, I.; Sanchez, J.; Andrade, C.; Evans, A.

    2012-02-01

    The present work deals with the carbonation process in cement based materials such as concrete. In order to clarify the evolution of the two main phases involved in the process, portlandite and calcium carbonate as a function of depth, spatially resolved neutron diffraction experiments have been performed at SALSA diffractometer at ILL in carbonated cement paste samples. Specimens submitted to different carbonation processes, both natural and accelerated, have been analyzed with this non destructive technique. The evolution of the main diffraction peaks of portlandite and calcite has been followed by means of neutron diffraction patterns measured at different depths. The results indicate that, in specimens subjected to CO2 atmospheres for 24 and 48 hours, the amount of calcite increases from the centre of the specimen to the surface. In both type of specimens calcite is formed at all depths analyzed, with higher quantities for the ones submitted to the longest carbonation period. Regarding the evolution of portlandite in these specimens, it almost completely disappeared, with only a low amount of the phase constant throughout the sample. In specimens subjected to air in a closed chamber for 21 months, higher amounts of portlandite were observed throughout the sample and little increase of calcite in the outer part, pointing out a much less severe reaction. The absorption effects are characterized by measuring in perpendicular directions and an absorption coefficient is calculated for portlandite.

  12. Neutron diffraction facilities at the high flux reactor, Petten

    NASA Astrophysics Data System (ADS)

    Ohms, C.; Youtsos, A. G.; Bontenbal, A.; Mulder, F. M.

    2000-03-01

    The High Flux Reactor in Petten is equipped with twelve beam tubes for the extraction of thermal neutrons for applications in materials and medical science. Beam tubes HB4 and HB5 are equipped with diffractometers for residual stress and powder investigations. Recently at HB4 the Large Component Neutron Diffraction Facility has been installed. It is a unique facility with respect to its capability of handling heavy components up to 1000 kg in residual stress testing. Its basic features are described and the first applications on thick piping welds are shown. The diffractometer at HB5 can be set up for powder and stress measurements. Recent applications include temperature dependent measurements on phase transitions in intermetallic compounds and on Li ion energy storage materials.

  13. Structural studies of magnesium nitride fluorides by powder neutron diffraction

    SciTech Connect

    Brogan, Michael A.; Hughes, Robert W.; Smith, Ronald I.; Gregory, Duncan H.

    2012-01-15

    Samples of ternary nitride fluorides, Mg{sub 3}NF{sub 3} and Mg{sub 2}NF have been prepared by solid state reaction of Mg{sub 3}N{sub 2} and MgF{sub 2} at 1323-1423 K and investigated by powder X-ray and powder neutron diffraction techniques. Mg{sub 3}NF{sub 3} is cubic (space group: Pm3m) and has a structure related to rock-salt MgO, but with one cation site vacant. Mg{sub 2}NF is tetragonal (space group: I4{sub 1}/amd) and has an anti-LiFeO{sub 2} related structure. Both compounds are essentially ionic and form structures in which nitride and fluoride anions are crystallographically ordered. The nitride fluorides show temperature independent paramagnetic behaviour between 5 and 300 K. - Graphical abstract: Definitive structures of the ternary magnesium nitride fluorides Mg{sub 3}NF{sub 3} and the lower temperature polymorph of Mg{sub 2}NF have been determined from powder neutron diffraction data. The nitride halides are essentially ionic and exhibit weak temperature independent paramagnetic behaviour. Highlights: Black-Right-Pointing-Pointer Definitive structures of Mg{sub 3}NF{sub 3} and Mg{sub 2}NF were determined by neutron diffraction. Black-Right-Pointing-Pointer Nitride and fluoride anions are crystallographically ordered in both structures. Black-Right-Pointing-Pointer Both compounds exhibit weak, temperature independent paramagnetic behaviour. Black-Right-Pointing-Pointer The compounds are essentially ionic with ionicity increasing with F{sup -} content.

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

    PubMed

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

    2015-09-10

    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 pressures. The first is observed at 0.39 GPa, where both phases were observed simultaneously and confirm our previous observations. This transition is followed by a second transition at 1.2 GPa to a new polymorph that is characterized for the first time. On increasing pressure, the diffraction pattern of phase III deteriorates significantly. On decompression phase III persists to 0.54 GPa before transformation to the ambient pressure phase. There is significant loss of signal after decompression, signifying that there has been a loss of material through polymerization. The orientation of the molecules in phase III provides insight into the possible polymerization reaction. PMID:26289930

  15. Non invasive measurement of strain and temperature by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Holden, T. M.; Root, J. H.; Tennant, D. C.; Kroeze, D. E.; Leggett, D.

    1990-06-01

    Two methods have been developed to determine temperature noninvasively within engineering components by neutron diffraction. The integrated intensity of a diffraction line depends on temperature through the Debye-Waller factor. The angular position of the line, in the absence of an applied load, depends on temperature through the thermal expansion coefficient. Temperature may thus be determined by accurate relative intensity measurements with respect to a reference temperature and, alternatively, by accurate measurement of the interplanar spacings. It was also shown to be feasible to measure the strain response to an applied load at elevated temperatures. Measurements were made on Waspalloy and the Ti alloy AMS 4928. For Waspalloy, the thermal expansion at zero stress gave the average temperature with a precision of +/- 4 K and agreed with thermocouple measurements to within 5 K on average. The intensity data suggest that temperature can be measured with a precision of +/- 10 K in a loaded component.

  16. Bayesian Library for the Analysis of Neutron Diffraction Data

    NASA Astrophysics Data System (ADS)

    Ratcliff, William; Lesniewski, Joseph; Quintana, Dylan

    During this talk, I will introduce the Bayesian Library for the Analysis of Neutron Diffraction Data. In this library we use of the DREAM algorithm to effectively sample parameter space. This offers several advantages over traditional least squares fitting approaches. It gives us more robust estimates of the fitting parameters, their errors, and their correlations. It also is more stable than least squares methods and provides more confidence in finding a global minimum. I will discuss the algorithm and its application to several materials. I will show applications to both structural and magnetic diffraction patterns. I will present examples of fitting both powder and single crystal data. We would like to acknowledge support from the Department of Commerce and the NSF.

  17. Crystal structure of human tooth enamel studied by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Ouladdiaf, Bachir; Rodriguez-Carvajal, Juan; Goutaudier, Christelle; Ouladdiaf, Selma; Grosgogeat, Brigitte; Pradelle, Nelly; Colon, Pierre

    2015-02-01

    Crystal structure of human tooth enamel was investigated using high-resolution neutron powder diffraction. Excellent agreement between observed and refined patterns is obtained, using the hexagonal hydroxyapatite model for the tooth enamel, where a large hydroxyl deficiency ˜70% is found in the 4e site. Rietveld refinements method combined with the difference Fourier maps have revealed, however, that the hydroxyl ions are not only disordered along the c-axis but also within the basal plane. Additional H ions located at the 6h site and forming HPO42- anions were found.

  18. Neutron diffraction studies of welds of aerospace aluminum alloys

    SciTech Connect

    Martukanitz, R.P.; Howell, P.R.; Payzant, E.A.; Spooner, S.; Hubbard, C.R.

    1996-10-01

    Neutron diffraction and electron microscopy were done on residual stress in various regions comprising variable polarity plasma arc welds of alloys 2219 (Al-6.3Cu) and 2195 (Al-4.0Cu-1.0Li-0.5Mg-0.5Ag). Results indicate that lattice parameter changes in the various weld regions may be attributed to residual stresses generated during welding, as well as local changes in microstructure. Distribution of longitudinal and transverse stress of welded panels shows peaks of tension and compression, respectively, within the HAZ and corroborate earlier theoretical results. Position of these peaks are related to position of minimum strength within the HAZ, and the magnitude of these peaks are a fraction of the local yield strength in this region. Weldments of alloy 2195-T8 exhibited higher peak residual stress than alloy 2219-T87. Comparison of neutron diffraction and microstructural analysis indicate decreased lattice parameters associated with the solid solution of the near HAZ; this results in decreased apparent tensile residual stress within this region and may significantly alter interpretation of residual stress measurements of these alloys. Considerable relaxation of residual stress occurs during removal of specimens from welded panels and was used to aid in differentiating changes in lattice parameters attributed to residual stress from welding and modifications in microstructure.

  19. Structural Study of PMN-xPT by Neutron Diffraction

    NASA Astrophysics Data System (ADS)

    Phelan, D.; Gehring, P. M.; Huang, Q.; Ye, Z.-G.; Stock, C.; Xu, G.; Wen, J.

    2009-03-01

    Stark differences between x-ray and neutron measurements of the structures of ferroelectric-relaxors PMN-xPT ((1-x)Pb(Mg1/3Nb2/3)O3+xPbTiO3) and PZN-xPT (Z=Zn) have been reported [1]. One explanation for these differences is that these crystals have strained surface layers on the order of several tens of μm thick, the crystal structure of which differs from that of the crystal bulk. This phenomenon has been coined the ``anomalous skin effect'' but has been recently challenged [2] and thus remains controversial. We reinvestigated the skin effect in PMN-xPT by considering the possibility that the oxygen stoichiometry might play a role. Two sets of powders (x=0.1, 0.2, 0.3, and 0.4) were grown, one with and one without oxygen annealing, and high resolution neutron powder diffraction measurements were carried out for both sets. For a given x, both sets of powders have the same structural phase, suggesting that the effects of oxygen annealing are minimal. For x=0.1 and x=0.2 both sets of powders are rhombohedral, which contrasts with the single crystal neutron diffraction measurements. This supports a skin effect in that the grain size of the powders is small enough that the Bragg peaks are dominated by the strained surface layer. References [1] G. Xu et al., Phase Transitions 79, 135 (2006) [2] E. H. Kisi and J.S. Forrester, J. Phys.:Condens. Matter 17, L381 (2005)

  20. Neutron diffraction characterization of Japanese artworks of Tokugawa age.

    PubMed

    Grazzi, F; Bartoli, L; Civita, F; Zoppi, M

    2009-12-01

    Neutron time-of-flight diffraction technique has been used to characterize some Japanese historical artifacts. With this method, metal samples can be analyzed in their bulk properties without need of sampling. Results shown here were obtained at the Italian Neutron Experimental Station (INES@ISIS) located at the pulsed neutron source ISIS (UK). The parallel use of a scanning electron microscope equipped with an energy-dispersive X-ray fluorescence device (SEM-EDX) permitted a full quantitative characterization of the investigated samples, namely four hand-guards (Tsubas) of Japanese swords attributed to the Tokugawa age. In particular, we were able to obtain, in a totally non-invasive non-destructive way, a full quantitative phase characterization of the samples, a detailed Bragg peak broadening analysis, and a quantitative texture determination. These results, complemented with those obtained via the traditional analysis method of SEM-EDX, allowed a full characterization of both the bulk and the surface of the artifacts. PMID:19711059

  1. Rotation of the compound nucleus 236U ∗ in the fission reaction 235U( n,f) induced by cold polarised neutrons

    NASA Astrophysics Data System (ADS)

    Goennenwein, F.; Mutterer, M.; Gagarski, A.; Guseva, I.; Petrov, G.; Sokolov, V.; Zavarukhina, T.; Gusev, Yu.; von Kalben, J.; Nesvizhevski, V.; Soldner, T.

    2007-08-01

    Surprisingly, for one of the best investigated nuclear reactions a new phenomenon was discovered. In an experiment performed at the High Flux Reactor of the Institut Laue Langevin in Grenoble, France, the reaction 235U(n , f) was studied. Fission was induced by cold polarised neutrons. Besides the two main fragments also ternary light charged particles were measured. The centres or the detector assemblies for fragments and light particles were positioned at right angles relative to each other in a plane perpendicular to the neutron beam. It is well known that the majority of ternary particles are emitted closely perpendicular to the fission axis. With the neutron spin pointing parallel or anti-parallel to the neutron beam it was observed that, upon flipping periodically the neutron spin, the distributions of angles between fragments and light particles are wobbling back and forth. The phenomenon is traced to the rotation of the scissioning nucleus while the light particles are ejected. This interpretation is corroborated by trajectory calculations for ternary α-particles being accelerated in a rotating Coulomb field provided by the two main fragments. The angle through which the fission axis and the trajectories of α-particles rotate is very small and barely exceeds 0.2°. This so far unreported feature of nuclear fission has been called the “ROT-effect”.

  2. Single crystal neutron diffraction for the inorganic chemist - a practical guide.

    SciTech Connect

    Piccoli, P.; Koetzle, T. F.; Schultz, A. J.; Intense Pulsed Neutron Source

    2007-01-01

    Advances and upgrades in neutron sources and instrumentation are poised to make neutron diffraction more accessible to inorganic chemists than ever before. These improvements will pave the way for single crystal investigations that currently may be difficult, for example due to small crystal size or large unit cell volume. This article aims to highlight what can presently be achieved in neutron diffraction and looks forward toward future applications of neutron scattering in inorganic chemistry.

  3. Neutron diffraction studies of amphipathic helices in phospholipid bilayers

    SciTech Connect

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

    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.

  4. Powder neutron diffraction studies of a carbonate fluorapatite

    SciTech Connect

    Leventouri, Th.; Chakoumakos, B. C.; Moghaddam, H. Y.; Perdikatsis, V.

    2000-02-01

    Atomic positional disorder of a single-phase natural carbonate fluorapatite (francolite) is revealed from analysis of the atomic displacement parameters (ADPs) refined from neutron powder diffraction data as a function of temperature and carbonate content. The ADPs of the francolite show a strong disturbance at the P, O3, and F sites. When it is heat treated to partially or completely remove the carbonate, the ADPs as well as the other structural parameters resemble those of a fluorapatite (Harding pegmatite) that was measured under the same conditions. The various structural changes are consistent with a substitution mechanism whereby the planar carbonate group replaces a phosphate group and lies on the mirror plane of the apatite structure. (c) 2000 Materials Research Society.

  5. Neutron diffraction studies of liquid iso-propanol

    NASA Astrophysics Data System (ADS)

    Zetterström, P.; Dahlborg, U.; Delaplane, R. G.; Howells, W. S.

    1991-07-01

    The structure of deuterated liquid iso-propanol has been studied with neutron diffraction at the LAD diffractometer at the ISIS spallation source. Measurements were performed at temperatures 190, 220, 250 and 275 K. To correct for inelastic effects a model for the dynamic structure factor which obeys detailed balance and included recoil effects was used. The static molecular structure factor SM(Q) exhibits a pre-peak at about 0.75 Å-1. The origin of the pre-peak, which increases in amplitude with temperature, is presently unknown. The structure of the iso-propanol molecule was obtained from the total pair distribution function and from a fit of the intramolecular form factor f1(Q) to the measured SM(Q) at large Q. The obtained values of the bond length and Debye-Waller factors are in good agreement to those obtained from lower alcohols.

  6. Neutron diffraction studies on rubredoxin from Pyrococcus furiosus.

    PubMed

    Bau, Robert

    2004-01-01

    Single-crystal neutron diffraction data up to a resolution of 1.5 A have been collected at room temperature on two forms of rubredoxin using the BIX-3 diffractometer at the JRR-3 reactor of the Japan Atomic Energy Research Institute (JAERI). Rubredoxin is a small iron-sulfur redox protein with 53 amino acid residues, and the source of this particular protein is the hyperthermophile Pyrococcus furiosus, a microorganism that normally lives at temperatures near that of boiling water. Data were collected on crystals of the wild-type protein and on a mutant in which three of the residues have been replaced. In this paper we will be describing several sets of results arising from these high-resolution neutron structure determinations: (a) the H/D exchange pattern of the N-H bonds of the main backbone, which give information about which regions of the molecule are more exposed to solvent; (b) the orientations of some of the O-D bonds in the protein, information which is often not obtainable from X-ray results; (c) the structure and appearance of water molecules in the protein crystals; and (d) some structural features which may help rationalize the remarkable thermal stability of the wild-type protein from this intriguing microorganism PMID:14646139

  7. Ultra high resolution neutron scattering: Neutron Resonance Spin-Echo and Larmor Diffraction

    NASA Astrophysics Data System (ADS)

    Walters, Andrew; Keller, Thomas; Keimer, Bernhard

    2012-02-01

    The TRISP spectrometer at the FRM II neutron source near Munich, Germany, is a unique world-leading neutron scattering instrument which employs the Neutron Resonance Spin-Echo technique (NRSE). Linewidths of dispersive excitations with energy transfers up to 50 meV can be measured with an energy resolution in the μeV range without the restrictive flux limitations that normally apply to high resolution neutron triple-axis spectrometers. Pioneering studies on the electron-phonon interaction in elemental superconductorsootnotetextP. Aynajian et al., Science 319 1509 (2008) and the lifetimes of magnetic excitations in archetypal magnetic systems will be reviewed.ootnotetextS. Bayrakci et al., Science 312 1928 (2006) The instrument can also be used as a Larmor diffractometer, enabling d-spacings to be measured with a resolution of δdd ˜10-6, i.e. more than one order of magnitude more sensitive than conventional diffraction techniques.ootnotetextC. Pfleiderer et al., Science 316 1871 (2007) Ongoing and future NRSE and Larmor diffraction projects will be outlined, especially in regard to prospective studies which will take full advantage of the new low temperature and high pressure sample environment capabilities now available at TRISP.

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

    PubMed

    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. PMID:23250059

  9. Three-port beam splitter for slow neutrons using holographic nanoparticle-polymer composite diffraction gratings

    SciTech Connect

    Klepp, J.; Fally, M.; Tomita, Y.; Pruner, C.; Kohlbrecher, J.

    2012-10-08

    Diffraction of slow neutrons by nanoparticle-polymer composite gratings has been observed. By carefully choosing grating parameters such as grating thickness and spacing, a three-port beam splitter operation for slow neutrons - splitting the incident neutron intensity equally into the {+-}1st and the 0th diffraction orders - has been realized. As a possible application, a Zernike three-path interferometer is briefly discussed.

  10. Powder diffraction in materials science using the KENS cold-neutron source

    SciTech Connect

    Kamiyama, T.; Oikawa, K.; Akiba, E.

    1997-12-01

    Since superconductivity fever spread around the world, neutron powder diffraction has become very popular and been widely used by crystallographers, physicists, chemists, mineralogists, and materials scientists. The purpose of present paper is to show, firstly, important characteristics of time-of-flight TOF powder diffraction using cold-neutron source in the study of materials science, and, secondly, recent studies on the structure and function of batteries at the Neutron Science Laboratory (KENS) in the High Energy Accelerator Research Organization (KEK).

  11. Powder Neutron Diffraction Study of HoCoGa5

    SciTech Connect

    Kabayashi, Riki; Kaneko, Koji; Wakimoto, Shuichi; Chi, Songxue; Sanada, Naoyuki; Watanuki, Ryuta; Suzuki, Kazuya

    2013-01-01

    We have studied successive magnetic transitions of HoCoGa5 at TN1 = 9.6 K and TN2 = 7.5 K by using powder neutron diffraction. Apparent superlattice peaks were observed at temperatures below TN1. With further decreases temperature, the patterns exhibit a substantial change at temperatures below TN2. The observed magnetic peaks at 8 K (AntiFerromagnetic InCommensurate (AFIC) phase : TN2 < T < TN1) can be represented by the propagation vector qL = (1/2 0 ) with = 0.35(2). In contrast, the magnetic structure becomes commensurate with qC = (1/2 0 1/2) at 4 K (AntiFerromagnetic Commensurate (AFC) phase : T < TN2). The temperature dependence of magnetic intensity shows an apparent temperature hysteresis at TN2, indicates a first-order transition at TN2. Analysis of the integrated intensity at 4 K reveals that the Ho moment with a size of 8.6(2) B, oriented parallel to the c-axis in the AFC phase. While the successive transitions of HoCoGa5 are different from those of TbCoGa5, the magnetic structure in the AFC phase of HoCoGa5 is the same as the AFTb I of TbCoGa5, and may indicate an additional transition at a lower temperature in HoCoGa5.

  12. Neutron diffraction studies for realtime leaching of catalytic Ni.

    PubMed

    Iles, Gail N; Devred, François; Henry, Paul F; Reinhart, Guillaume; Hansen, Thomas C

    2014-07-21

    The leaching of Al from intermetallic samples of Nickel Aluminium alloys to form Raney-type nickel catalysts is widely used in the hydrogenation industry, however, little is known of the leaching process itself. In this study, the leaching of Al was measured in realtime, in situ, using the high-flux powder neutron diffractometer, D20, at the Institut Laue-Langevin. Despite the liberation of hydrogen and effervescent nature of the reaction the transformation of the dry powder phases into Raney-type Ni was determined. Samples produced by gas-atomisation were found to leach faster than those produced using the cast and crushed technique. Regardless of processing route of the precursor powder, the formation of spongy-Ni occurs almost immediately, while Ni2Al3 and NiAl3 continue to transform over longer periods of time. Small-angle scattering and broadening of the diffraction peaks is an evidence for the formation of the smaller Ni particles. Understanding the kinetics of the leaching process will allow industry to refine production of catalysts for optimum manufacturing time while knowledge of leaching dynamics of powders produced by different manufacturing techniques will allow further tailoring of catalytic materials. PMID:25053313

  13. Neutron diffraction studies for realtime leaching of catalytic Ni

    SciTech Connect

    Iles, Gail N. Reinhart, Guillaume; Devred, François; Henry, Paul F. Hansen, Thomas C.

    2014-07-21

    The leaching of Al from intermetallic samples of Nickel Aluminium alloys to form Raney-type nickel catalysts is widely used in the hydrogenation industry, however, little is known of the leaching process itself. In this study, the leaching of Al was measured in realtime, in situ, using the high-flux powder neutron diffractometer, D20, at the Institut Laue-Langevin. Despite the liberation of hydrogen and effervescent nature of the reaction the transformation of the dry powder phases into Raney-type Ni was determined. Samples produced by gas-atomisation were found to leach faster than those produced using the cast and crushed technique. Regardless of processing route of the precursor powder, the formation of spongy-Ni occurs almost immediately, while Ni{sub 2}Al{sub 3} and NiAl{sub 3} continue to transform over longer periods of time. Small-angle scattering and broadening of the diffraction peaks is an evidence for the formation of the smaller Ni particles. Understanding the kinetics of the leaching process will allow industry to refine production of catalysts for optimum manufacturing time while knowledge of leaching dynamics of powders produced by different manufacturing techniques will allow further tailoring of catalytic materials.

  14. Neutron-diffraction study of liquid hydrogen iodide

    NASA Astrophysics Data System (ADS)

    Andreani, C.; Nardone, M.; Ricci, F. P.; Soper, A. K.

    1992-10-01

    Neutron-diffraction experiments on liquid DI, HI, and on an equimolar mixture of HI and DI are presented. All these three samples were in the same thermodynamic state corresponding to the orthobaric liquid at T=253 K. The three partial structure factors SII(Q), SHI(Q), SHH(Q) are derived exploiting the standard isotopic substitution procedure. The corresponding pair correlation functions gII(r), gHI(r), and gHH(r) are evaluated and compared with those given by a model that neglects all orientational correlations. Our data indicate that gII(r) (which is essentially the center-center correlation function) is well reproduced by the pair distribution function of a monatomic Lennard-Jones fluid and that gHI(r) (which should be sensitive to the correlations between molecular and intermolecular axes) is very similar to the one derived neglecting orientational correlations. On the contrary, orientational correlations between the molecular axes are clearly present in the gHH(r), which deviates significantly from the uncorrelated model results. These facts are consistent with the idea that H bonding is not present in liquid HI and indicate also that the only relevant terms of the anisotropic intermolecular potential are those due to the electric multipolar interactions.

  15. Exploring the magnetic phase diagram of dysprosium with neutron diffraction

    NASA Astrophysics Data System (ADS)

    Yu, J.; LeClair, P. R.; Mankey, G. J.; Robertson, J. L.; Crow, M. L.; Tian, W.

    2015-01-01

    With one of the highest intrinsic magnetic moments (10.6 μB/atom ) among the heavy rare-earth elements, dysprosium exhibits a rich magnetic phase diagram, including several modulated magnetic phases. Aided by the Ruderman-Kittel-Kasuya-Yosida interaction, the magnetic modulations propagate coherently over a long range. Neutron diffraction experiments were performed to determine the microscopic magnetic origin of the field induced phases in bulk Dy as a function of temperature, covering regions of the well-known ferromagnetic, helical antiferromagnetic, fan phases, and several possible new phases suggested by previous studies. A short-range ordered fan phase was identified as the intermediate state between ferromagnetism and long-range ordered fan. In a field of 1 T applied along the a axis, the temperature range of a coexisting helix/fan phase was determined. The magnetic phase diagram of Dy was thus refined to include the detailed magnetic origin and the associated phase boundaries. Based on the period of the magnetic modulation and the average magnetization, the evolution of the spin arrangement upon heating was derived quantitatively for the modulated magnetic phases.

  16. Neutron diffraction studies for realtime leaching of catalytic Ni

    NASA Astrophysics Data System (ADS)

    Iles, Gail N.; Devred, François; Henry, Paul F.; Reinhart, Guillaume; Hansen, Thomas C.

    2014-07-01

    The leaching of Al from intermetallic samples of Nickel Aluminium alloys to form Raney-type nickel catalysts is widely used in the hydrogenation industry, however, little is known of the leaching process itself. In this study, the leaching of Al was measured in realtime, in situ, using the high-flux powder neutron diffractometer, D20, at the Institut Laue-Langevin. Despite the liberation of hydrogen and effervescent nature of the reaction the transformation of the dry powder phases into Raney-type Ni was determined. Samples produced by gas-atomisation were found to leach faster than those produced using the cast and crushed technique. Regardless of processing route of the precursor powder, the formation of spongy-Ni occurs almost immediately, while Ni2Al3 and NiAl3 continue to transform over longer periods of time. Small-angle scattering and broadening of the diffraction peaks is an evidence for the formation of the smaller Ni particles. Understanding the kinetics of the leaching process will allow industry to refine production of catalysts for optimum manufacturing time while knowledge of leaching dynamics of powders produced by different manufacturing techniques will allow further tailoring of catalytic materials.

  17. Neutron diffraction observations of interstitial protons in dense ice

    PubMed Central

    Guthrie, Malcolm; Boehler, Reinhard; Tulk, Christopher A.; Molaison, Jamie J.; dos Santos, António M.; Li, Kuo; Hemley, Russell J.

    2013-01-01

    The motif of distinct H2O molecules in H-bonded networks is believed to persist up to the densest molecular phase of ice. At even higher pressures, where the molecule dissociates, it is generally assumed that the proton remains localized within these same networks. We report neutron-diffraction measurements on D2O that reveal the location of the D atoms directly up to 52 GPa, a pressure regime not previously accessible to this technique. The data show the onset of a structural change at ∼13 GPa and cannot be described by the conventional network structure of ice VII above ∼26 GPa. Our measurements are consistent with substantial deuteron density in the octahedral, interstitial voids of the oxygen lattice. The observation of this “interstitial” ice VII form provides a framework for understanding the evolution of hydrogen bonding in ice that contrasts with the conventional picture. It may also be a precursor for the superionic phase reported at even higher pressure with important consequences for our understanding of dense matter and planetary interiors. PMID:23757495

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

    SciTech Connect

    Jorgensen, J.D.

    1994-05-01

    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.

  19. Single crystal neutron diffraction refinement of bullvalene at 110 K

    SciTech Connect

    Luger, P.; Buschmann, J.; McMullan, R.K.; Ruble, J.R.; Matias, P.; Jeffrey, G.A.

    1986-11-26

    A low-temperature neutron diffraction refinement of the crystal structure of bullvalene, C/sub 10/H/sub 10/, tricyclo(3.3.2.0/sup 2.8/)deca-2,5,8-triene, shows that the molecule is distorted only very slightly from the C/sub 3 upsilon/ symmetry expected for the isolated molecule, although the crystal structure symmetry is monoclinic. There is a small but significant difference between the shortest and longest of the C-C bonds in the cyclopropane ring, which are 1.536 (1), 1.533 (1), and 1.530 (1) A. The three ethylenic wings of the molecule are virtually identical, except for small differences in planarity and C-C-H angles. One wing is exactly planar within 0.002 (3) A. In the other two, one of the hydrogen atoms in each is significantly displaced from the plane by 0.027 (3) and 0.023 (3) A. The mean bond lengths in the ethylenic wings are C/sub ring/-C, 1.4727 (7) A; C=C, 1.3423 (7) A; =C-C, 1.5163 (7) A. The C-H bond lengths range from 1.086 (2) to 1.092 (2) A. The thermal motion analysis gives an unusually good fit to the rigid-body model. Corrections for harmonic thermal motion lengthened all C-C and C=C bonds uniformly by 0.003 A. For the C-H bonds, the harmonic riding motion and anharmonicity corrections almost cancel, so that the thermally corrected bond lengths differ from those measured by +/- 0.001 A.

  20. X-ray structure of perdeuterated diisopropyl fluorophosphatase (DFPase): perdeuteration of proteins for neutron diffraction

    PubMed Central

    Blum, Marc-Michael; Tomanicek, Stephen J.; John, Harald; Hanson, B. Leif; Rüterjans, Heinz; Schoenborn, Benno P.; Langan, Paul; Chen, Julian C.-H.

    2010-01-01

    The signal-to-noise ratio is one of the limiting factors in neutron macromolecular crystallography. Protein perdeuteration, which replaces all H atoms with deuterium, is a method of improving the signal-to-noise ratio of neutron crystallography experiments by reducing the incoherent scattering of the hydrogen isotope. Detailed analyses of perdeuterated and hydrogenated structures are necessary in order to evaluate the utility of perdeuterated crystals for neutron diffraction studies. The room-temperature X-ray structure of perdeuterated diisopropyl fluorophosphatase (DFPase) is reported at 2.1 Å resolution. Comparison with an independently refined hydrogenated room-temperature structure of DFPase revealed no major systematic differences, although the crystals of perdeuterated DFPase did not diffract neutrons. The lack of diffraction is examined with respect to data-collection and crystallo­graphic parameters. The diffraction characteristics of successful neutron structure determinations are presented as a guideline for future neutron diffraction studies of macromolecules. X-ray diffraction to beyond 2.0 Å resolution appears to be a strong predictor of successful neutron structures. PMID:20383004

  1. In-situ neutron diffraction study of cathode/electrolyte interactions under electrical load and elevated temperature

    NASA Astrophysics Data System (ADS)

    Tonus, F.; Skinner, S. J.

    2016-05-01

    Fuel cells are proposed as a future energy conversion technology that will reduce greenhouse gas emissions at the point of operation due to their ability to produce electrical energy from non-hydrocarbon fuel sources. The Solid Oxide Fuel Cell (SOFC) is amongst the most efficient fuel cell types, however, due to the high cell operating temperature cation diffusion occurs between the different components of the cell, resulting in rapid degradation of the power output. In this paper we investigate cation migration between the promising intermediate temperature-SOFC cathode La1-xSrxCo1-yFeyO3-δ (LSCF) and a fluorite type electrolyte Ce1-xPrxO2-δ (CPO). The crystallographic structure evolution and degradation of the materials were studied by neutron diffraction in-situ under pseudo-operating conditions, i.e. at 600 °C under air and under electrical polarisation. The lattice parameter and cation occupancy evolution were analysed by Rietveld refinement as a function of time and applied potential. The materials were found to be stable, as no impurity formation, lattice parameter or site occupancy evolution was observed during the experiment. However La migration prior to the experiment from LSCF to CPO was observed as well as B-site vacancies in LSCF.

  2. Cottingham formula and nucleon polarisabilities

    NASA Astrophysics Data System (ADS)

    Gasser, J.; Hoferichter, M.; Leutwyler, H.; Rusetsky, A.

    2015-08-01

    The difference between the electromagnetic self-energies of proton and neutron can be calculated with the Cottingham formula, which expresses the self-energies as an integral over the electroproduction cross sections - provided the nucleon matrix elements of the current commutator do not contain a fixed pole. We show that, under the same proviso, the subtraction function occurring in the dispersive representation of the virtual Compton forward scattering amplitude is determined by the cross sections. The representation in particular leads to a parameter-free sum rule for the nucleon polarisabilities. We evaluate the sum rule for the difference between the electric polarisabilities of proton and neutron by means of the available parameterisations of the data and compare the result with experiment.

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

    SciTech Connect

    Niimura, Nobuo

    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.

  4. The early development of neutron diffraction: Science in the wings of the Manhattan Project

    SciTech Connect

    Mason, Thom; Gawne, Timothy J; Nagler, Stephen E; Nestor, Margaret Boone {Bonnie}; Carpenter, John M

    2012-01-01

    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 measurements 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.

  5. Neutron diffraction studies of Gd 2Zr 2O 7 pyrochlore

    NASA Astrophysics Data System (ADS)

    Kennedy, Brendan J.; Zhou, Qingdi; Avdeev, Maxim

    2011-07-01

    The structure of Gd 2Zr 2O 7 pyrochlore over the temperature range 4-300 K has been refined from powder neutron diffraction data. The sample was enriched in 160Gd to avoid the high neutron absorption of naturally occurring Gd. The diffraction pattern showed well resolved superlattice reflections indicative of the pyrochlore structure and no evidence is found for anion-disorder from the structural refinements.

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

    SciTech Connect

    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.

  7. Scientific Advancements and Technological Developments of High P-T Neutron Diffraction at LANSCE, Los Alamos

    NASA Astrophysics Data System (ADS)

    Zhao, Y.; Daemen, L. L.; Zhang, J.

    2003-12-01

    In-situ high P-T neutron diffraction experiments provide unique opportunities to study the crystal structure, hydrogen bonding, magnetism, and thermal parameters of light elements (eg. H, Li, B) and heavy elements (eg. Ta, U, Pu,), that are virtually impossible to determine with x-ray diffraction techniques. For example, thermoelasticity and Debye-Waller factor as function of pressure and temperature can be derived using in-situ high P-T neutron diffraction techniques. These applications can also be extended to a much broader spectrum of scientific problems. For instance, puzzles in Earth science such as the carbon cycle and the role of hydrous minerals for water exchange between lithosphere and biosphere can be directly addressed. Moreover, by introducing in-situ shear, texture of metals and minerals accompanied with phase transitions at high P-T conditions can also be studied by high P-T neutron diffraction. We have successfully conducted high P-T neutron diffraction experiments at LANSCE and achieved simultaneous high pressures and temperatures of 10 GPa and 1500 K. With an average 3-6 hours of data collection, the diffraction data are of sufficiently high quality for the determination of structural parameters and thermal vibrations. We have studied hydrous mineral (MgOD), perovskite (K.15,Na.85)MgF3, clathrate hydrates (CH4-, CO2-, and H2-), metals (Mo, Al, Zr), and amorphous materials (carbon black, BMG). The aim of our research is to accurately map bond lengths, bond angles, neighboring atomic environments, and phase stability in P-T-X space. Studies based on high-pressure neutron diffraction are important for multi-disciplinary science and we welcome researchers from all fields to use this advanced technique. We have developed a 500-ton toroidal press, TAP-98, to conduct simultaneous high P-T neutron diffraction experiments inside of HIPPO (High-Pressure and Preferred-Orientation diffractometer). We have also developed a large gem-crystal anvil cell, ZAP-01

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

    SciTech Connect

    Hodges, J. P.

    1998-08-27

    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.

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

    SciTech Connect

    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.

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

    SciTech Connect

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

    1990-11-01

    The irradiation behavior of high-density uranium silicides has been a matter of interest to the nuclear industry for use in high power or low enrichment applications. Transmission electron microscopy studies have found that heavy ion bombardment renders U{sub 3}Si and U{sub 3}Si{sub 2} amorphous at temperatures below about 250 C and that U{sub 3}Si becomes mechanically unstable suffering rapid growth by plastic flow. In this present work, crystallographic changes preceding amorphization by fission fragment damage have been studied by high-resolution neutron diffraction as a function of damage produced by uranium fission at room temperature. Initially, both silicides had tetragonal crystal structures. Crystallographic and amorphous phases were studied simultaneously by combining conventional Rietveld refinement of the crystallographic phases with Fourier-filtering analysis of the non-crystalline scattering component. 13 refs., 5 figs.

  11. Non-invasive temperature measurements by neutron diffraction in aero-engine components

    SciTech Connect

    Holden, T.M.; Root, J.H.; Tennant, D.C.; Leggett, D.

    1995-12-31

    A requirement exists in the aeronautical industry for measuring temperature non-invasively in critical components, such as the turbine disc in an operating engine. Neutron diffraction, unique among nuclear techniques, offers the possibility of measuring both temperature and strain within an operating engine by virtue of the high penetration of neutrons through industrial materials. Static diffraction experiments on Waspaloy and Ti6Al4V showed, by comparison with thermocouples, that both the diffraction peak position and the peak intensity can measure the temperature to within {+-}6 K at 800 K.

  12. Neutron diffraction measurements of residual stresses in friction stir welding: a review

    SciTech Connect

    Woo, Wan Chuck; Feng, Zhili; Wang, Xun-Li; David, Stan A

    2011-01-01

    Significant amounts of residual stresses are often generated during welding and result in critical degradation of the structural integrity and performance of components. Neutron diffraction has become a well established technique for the determination of residual stresses in welds because of the unique deep penetration, three-dimensional mapping capability, and volume averaged bulk measurements characteristic of the scattering neutron beam. Friction stir welding has gained prominence in recent years. The authors reviewed a number of neutron diffraction measurements of residual stresses in friction stir welds and highlighted examples addressing how the microstructures and residual stresses are correlated with each other. An example of in situ neutron diffraction measurement result shows the evolution of the residual stresses during welding.

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

    PubMed Central

    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. PMID:23250059

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

    SciTech Connect

    Budayova-Spano, Monika; Bonneté, Françoise; Ferté, Natalie; El Hajji, Mohamed; Meilleur, Flora; Blakeley, Matthew Paul; Castro, Bertrand

    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. Area detectors in single-crystal neutron diffraction

    NASA Astrophysics Data System (ADS)

    McIntyre, Garry J.

    2015-12-01

    The introduction of area detectors has brought about a gentle revolution in the routine application of single-crystal neutron diffractometry. Implemented first for macromolecular crystallography, electronic detectors subsequently gradually spread to chemical and physics-oriented crystallography at steady-state sources. The volumetric surveying of reciprocal space implicit in the Laue technique has required area detectors right from the start, whether using film and more recently image plates and CCD-based detectors at reactors, or scintillation detectors at spallation sources. Wide-angle volumetric data collection has extended application of neutron single-crystal diffractometry to chemical structures, sample volumes, and physical phenomena previously deemed impossible. More than 30 of the dedicated single-crystal neutron diffractometers at steady-state reactor and neutron spallation sources worldwide and accessible via peer-review proposal mechanisms are currently equipped with area detectors. Here we review the historical development of the various types of area detectors used for single crystals, discuss experimental aspects peculiar to experiments with such detectors, highlight the scientific fields where the use of area detectors has had a special impact, and forecast future developments in hardware, implementation, and software.

  16. Neutron Diffraction Study of LaSr3Fe3O10 in the Temperature Range 25 - 650 deg. C

    SciTech Connect

    Neov, S.; Prokhnenko, O.; Velinov, N.; Kozhukharov, V.; Neov, D.; Dabrowski, L.

    2007-04-23

    The effect of high temperature on the structure of LaSr3Fe3O10 has been studied by neutron diffraction. Neutron data have been correlated with Moessbauer spectroscopy results and electrical conductivity measurements.

  17. Investigation on Deformation Behavior of Nickel Aluminum Bronze by Neutron Diffraction and Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Xu, Xiaoyan; Wang, Hong; Lv, Yuting; Lu, Weijie; Sun, Guangai

    2016-05-01

    The deformation behavior, deformation microstructures, and generated inter-phase stresses of nickel aluminum bronze were investigated by in situ neutron diffraction instrument and transmission electron microscopy in this paper. Lattice strains calculated by both peak shifting and broadening by Gaussian fitting of α and κ phase neutron diffraction peak profiles at both holding stress conditions and unloaded stress conditions were compared. Twining and stacking faults in α matrix were observed after deformed by different tensile stresses. Compressive internal/residual stress in α matrix and tensile internal stress in κ phase in elasto-plastic region were calculated based on neutron diffraction analysis. The piled-up dislocations around hard κ phases increase with increasing the deformation degree, which raise the stress concentration near α/ κ interface and increase the internal stresses.

  18. in-situ chemistry mapping of hydrogen storage materials by neutron diffraction

    SciTech Connect

    Payzant, E Andrew; Bowman Jr, Robert C; Johnson, Terry A; Jorgensen, Scott W

    2013-01-01

    Neutron diffraction was used to nondestructively study the microstructures for two hydrogen storage media systems. In the first case, sodium alanate based hydrogen storage is a vehicle-scale candidate system developed by Sandia/GM. Neutron scattering was used to determine the distribution of phases in the storage media at different hydrogen loading levels, to help understand the absorption/desorption of hydrogen in large-scale systems. This study also included a 3D neutron tomographic study of the microstructure. In the second case, tin-doped lanthanum nickel alloys have been studied at JPL for space-based applications, for which the gradual degradation of the material due to segregation and disproportionation of phases is a known problem. A regenerative process developed to restore the storage properties of these alloys was studied, using in-situ neutron diffraction to relate the microstructure to the thermodynamic simulations.

  19. Adaptation of a neutron diffraction detector to coded aperture imaging

    SciTech Connect

    Vanier, P.E.; Forman, L.

    1997-02-01

    A coded aperture neutron imaging system developed at Brookhaven National Laboratory (BNL) has demonstrated that it is possible to record not only a flux of thermal neutrons at some position, but also the directions from whence they came. This realization of an idea which defied the conventional wisdom has provided a device which has never before been available to the nuclear physics community. A number of potential applications have been explored, including (1) counting warheads on a bus or in a storage area, (2) investigating inhomogeneities in drums of Pu-containing waste to facilitate non-destructive assays, (3) monitoring of vaults containing accountable materials, (4) detection of buried land mines, and (5) locating solid deposits of nuclear material held up in gaseous diffusion plants.

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

    SciTech Connect

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

    1994-03-01

    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.

  1. High-Pressure Neutron Diffraction Studies for Materials Sciences and Energy Sciences

    NASA Astrophysics Data System (ADS)

    Zhao, Y.; Los Alamos High Pressure Materials Research Team

    2013-05-01

    The development of neutron diffraction under extreme pressure (P) and temperature (T) conditions is highly valuable to condensed matter physics, crystal chemistry, materials sciences, as well as earth and planetary sciences. We have incorporated a 500-ton press TAP-98 into the HiPPO diffractometer at LANSCE to conduct in situ high P-T neutron diffraction experiments. We have worked out a large gem-crystal anvil cell, ZAP, to conduct neutron diffraction experiments at high-P and low-T. The ZAP cell can be used to integrate multiple experimental techniques such as neutron diffraction, laser spectroscopy, and ultrasonic interferometery. Recently, we have developed high-P low-T gas/fluid cells in conjunction with neutron diffraction and inelastic neutron scattering instruments. These techniques enable in-situ and real-time examination of gas uptake/release processes and allow high-resolution time-dependent determination of changes in crystal structure and related reaction kinetics. We have successfully used these techniques to study the equation of state, structural phase transition, and thermo-mechanical properties of metals, ceramics, and minerals. We have conducted researches on the formation of methane and hydrogen clathrates, and hydrogen adsorption of the inclusion compounds such as the recently discovered metal-organic frameworks (MOFs). The aim of our research is to accurately map phase diagram, lattice parameters, thermal parameters, bond lengths, bond angles, neighboring atomic environments, and phase stability in P-T-X space. We are currently developing further high P-T technology with a new "true" triaxial loading press, TAP_6x, to compress cubic sample package to achieve pressures up to 20 GPa and temperatures up to 2000 K in routine experiments. The implementation of TAP_6x300 with high-pressure neutron beamlines is underway for simultaneous high P-T neutron diffraction, ultrasonic, calorimetry, radiography, and tomography studies. Studies based on high

  2. Fatigue investigations of autofrettaged steel cylinders based on neutron-diffraction measurements

    NASA Astrophysics Data System (ADS)

    de Swardt, R. R.; Venter, A. M.; van der Watt, M. W.

    A series of cyclic internal pressurization fatigue experiments was conducted on partially autofrettaged cylinders with multiple internal radial elliptic shaped cracks covering a wide range of possible configurations. A theoretical model was developed to predict the theoretical fatigue life using as input data the actual measured position of the plastic boundary from neutron-diffraction measurements on the failed specimens, as well as a position calculated analytically from the autofrettage pressure. The theoretical fatigue-life predictions based on the neutron-diffraction results were found to give the best correlation with experimental fatigue results.

  3. Total neutron diffraction: the correct way to determine the true structure of crystalline materials?

    NASA Astrophysics Data System (ADS)

    Hibble, S. J.; Hannon, A. C.; Fawcett, I. D.

    1999-11-01

    Crystallography, using conventional Bragg diffraction, and the study of atomic correlation functions, using total diffraction, have historically been carried out separately. There exist two different scientific communities, which in the case of neutron diffraction normally use different instruments. However, modern time-of-flight neutron diffractometers allow data to be collected to high maximum momentum transfer, Qmax, and with good reciprocal-space resolution, icons/Journals/Common/Delta" ALT="Delta" ALIGN="TOP"/> d/d. The high Qmax yields correlation functions with good real-space resolution, whilst the good reciprocal-space resolution yields data well suited to conventional crystallographic analysis. We show how the Liquids and Amorphous Diffractometer, LAD, at the ISIS spallation neutron source at the Rutherford Appleton Laboratory has been used to obtain new information on a number of disordered crystalline molybdates, Li2MoO3, LiMoO2 and D2MoO3. The average crystal structures are determined using Rietveld refinement of the Bragg diffraction data, whilst the local structures are determined by modelling the correlation functions, T(r), obtained from total neutron diffraction data. Reconciling the information from the two techniques provides a deeper understanding of structures than is possible using either technique in isolation. Finally, we discuss how the next generation of instruments will allow the development of this technique with specific reference to the new General Materials Diffractometer, GEM, at ISIS.

  4. Determination of toluene hydrogenation kinetics with neutron diffraction.

    PubMed

    Falkowska, Marta; Chansai, Sarayute; Manyar, Haresh G; Gladden, Lynn F; Bowron, Daniel T; Youngs, Tristan G A; Hardacre, Christopher

    2016-06-29

    Total neutron scattering has been used to follow the hydrogenation of toluene-d8 to methylcyclohexane-d14 over 3 wt% platinum supported on highly ordered mesoporous silica (MCM-41) at 298 K and under 150 mbar D2 pressure. The detailed kinetic information so revealed indicates that liquid reorganisation inside pores is the slowest step of the whole process. Additionally, the results were compared with the reaction performed under 250 mbar D2 pressure as well as with toluene-h8 hydrogenation using D2 at 150 mbar. PMID:27052196

  5. Recent advances in the study of H environments and behavior in minerals using neutron powder diffraction

    NASA Astrophysics Data System (ADS)

    Welch, M. D.

    2002-12-01

    It is now possible to probe the structural environments and behavior of H atoms directly in complex minerals such as amphiboles, micas, chlorites and humites using neutron powder diffraction, in some cases as a function of pressure and/or temperature. A combination of high neutron flux and increased detector sensitivity and size offers the chance to see details of H behaviour. In the last year or so the advent of new gasket designs for the Paris-Edinburgh pressure cell allow the use of ethanol/methanol (EtOD/MeOD) as a pressure medium, removing peak broadening arising from deviatoric stress that occurs above 3 GPa for the standard fluorinert pressure medium. Essentially hydrostatic conditions obtain with EtOD/MeOD to 8 GPa at 298 K. A further recent development has been the design of a high P-T module for use with the Paris-Edinburgh cell. These technological improvements in pressure-cell design now allow us to make meaningful correlations between OH vibrational spectra collected at high P and/or T and detailed structural information on H behaviour obtained from neutron diffraction under similar conditions. In this talk I shall discuss recent neutron diffraction experiments on the effect of pressure upon hydrogen bonding in deuterated chlorite to 5 GPa (298 K), and a high P-T study of hydrogen bonding in deuterated brucite to 7 GPa, 1100 K. These two studies illustrate how far high-pressure neutron diffraction has come in the last 5 years. Finally, I shall describe a neutron powder diffraction study (ambient conditions) of leucophoenicite, Mn7Si3O12(OH)2, a close structural analogue of Phase-B and Superhydrous-B: the structure of leucophoenicite is topologically identical to the hydrous sheet of Phase-B and similar to that of Superhydrous-B. For various reasons it was not possible to deuterate the sample. Nonetheless, the two distinct H atoms were approximately located in difference-Fourier maps and then refined isotropically. The H positions in Phase-B were only

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

    NASA Astrophysics Data System (ADS)

    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).

  7. Neutron diffraction residual stress studies for aero-engine component applications

    NASA Astrophysics Data System (ADS)

    Clay, K.; Small, C.

    1991-12-01

    Computer graphics for a presentation describing how Rolls-Royce is refining the method of residual stress measurement by neutron diffraction to suit the characteristic stress fields of components are presented. Results to date are given. An outline of how this residual stress data is to be used in developing stress models for critical rotating components is given.

  8. Atom Pair Distribution Functions of Liquid Water at 25circC from Neutron Diffraction

    NASA Astrophysics Data System (ADS)

    Narten, A. H.; Thiessen, W. E.; Blum, L.

    1982-09-01

    The structure of liquid water is described by three atom pair distribution functions gOO(r), gOH(r), and gHH(r). These functions have now been derived from neutron diffraction data on four mixtures of light and heavy water. They will provide a crucial and sensitive test for proposed models of liquid water.

  9. Observation of an intermediate phase in dysprosium near the Neel point by neutron diffraction

    SciTech Connect

    Bessergenev, V.G.; Gogava, V.V.; Kovalevskaya, Y.A.; Mandzhavidze, A.G.; Fedorov, V.M.; Shilo, S.I.

    1985-11-25

    The magnetic structure of dysprosium near the point of magnetic disordering has been studied as a function of the thermal history of the sample by neutron diffraction. An intermediate vortex phase appears during cooling from the paramagnetic phase and then converts into a helicoidal phase.

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

    SciTech Connect

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

    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}.

  11. FAST TRACK COMMUNICATION Determination of atomic site susceptibility tensors from neutron diffraction data on polycrystalline samples

    NASA Astrophysics Data System (ADS)

    Gukasov, A.; Brown, P. J.

    2010-12-01

    Polarized neutron diffraction can provide information about the atomic site susceptibility tensor χij characterizing the magnetic response of individual atoms to an external magnetic field (Gukasov and Brown 2002 J. Phys.: Condens. Mater. 14 8831). The six independent atomic susceptibility parameters (ASPs) can be determined from polarized neutron flipping ratio measurements on single crystals and visualized as magnetic ellipsoids which are analogous to the thermal ellipsoids obtained from atomic displacement parameters (ADPs). We demonstrate now that the information about local magnetic susceptibility at different magnetic sites in a crystal can also be obtained from polarized and unpolarized neutron diffraction measurements on magnetized powder samples. The validity of the method is illustrated by the results of such measurements on a polycrystalline sample of Tb2Sn2O7.

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

    SciTech Connect

    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.

  13. Processing of Neutron Diffraction Data for Strain Measurement in Geological Materials

    SciTech Connect

    Polsky, Yarom; An, Ke; Anovitz, Lawrence {Larry} M; Bingham, Philip R; Carmichael, Justin R; Dessieux Jr, Luc Lucius

    2014-01-01

    : Conventional rock mechanics testing techniques typically involve the loading of samples and measurement of displacements or strains on the outer boundary of the specimen surface. Neutron diffraction based strain measurement techniques represent a unique and powerful tool for measuring the strain within geological materials under load. The structural variability and non-uniform crystallinity of geological materials, however, create many complexities in the intensity patterns that must be analyzed to quantify strains within the material. The attenuating and scattering properties of the pressure cell housing the sample further add difficulties to the data analysis. This paper describes the methods and processes used to process neutron scattering data for strain measurement in geological materials. It is intended to provide a primer for those in the rock mechanics community that are interested in utilizing this technique along with additional discussion of neutron diffraction experimental factors that may affect data quality.

  14. Neutron diffraction investigation of an in-plane biaxial fatigued stainless steel sample of cruciform geometry

    NASA Astrophysics Data System (ADS)

    Taran, Yu V.; Balagurov, A. M.; Sheverev, S. G.; Schreiber, J.; Korsunsky, A. M.; Vorster, W. J. J.; Bomas, H.; Stoeberl, C.

    2008-03-01

    Fatigue and fracture under multiaxial stresses are among the most important current research topics aimed at ensuring improved reliability of industrial components. An ex situ in-plane biaxial low cycle fatigued sample of cruciform geometry from austenitic stainless steel AISI 321 H was investigated on the FSD stress-diffractometer at the IBR-2 pulsed nuclear reactor by using the neutron strain scanner and the uniaxial stress rig. The phase composition of fatigued material was determined and the residual macrostresses and phase microstresses were measured. To the best of our knowledge, no neutron diffraction investigations of materials subjected to biaxial loading have been previously carried out. The first results of the neutron diffraction experiment are presented and discussed.

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

    SciTech Connect

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

    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 was 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.

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

    SciTech Connect

    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.

  17. Preliminary time-of-flight neutron diffraction study on diisopropyl fluorophosphatase (DFPase) from Loligo vulgaris

    SciTech Connect

    Blum, Marc-Michael; Koglin, Alexander; Rüterjans, Heinz; Schoenborn, Benno; Langan, Paul; Chen, Julian C.-H.

    2007-01-01

    Diisopropyl fluorophosphatase (DFPase) effectively hydrolyzes a number of organophosphorus nerve agents, including sarin, cyclohexylsarin, soman and tabun. Neutron diffraction data have been collected from DFPase crystals to 2.2 Å resolution in an effort to gain further insight into the mechanism of this enzyme. The enzyme diisopropyl fluorophosphatase (DFPase) from Loligo vulgaris is capable of decontaminating a wide variety of toxic organophosphorus nerve agents. DFPase is structurally related to a number of enzymes, such as the medically important paraoxonase (PON). In order to investigate the reaction mechanism of this phosphotriesterase and to elucidate the protonation state of the active-site residues, large-sized crystals of DFPase have been prepared for neutron diffraction studies. Available H atoms have been exchanged through vapour diffusion against D{sub 2}O-containing mother liquor in the capillary. A neutron data set has been collected to 2.2 Å resolution on a relatively small (0.43 mm{sup 3}) crystal at the spallation source in Los Alamos. The sample size and asymmetric unit requirements for the feasibility of neutron diffraction studies are summarized.

  18. Polarisation properties of pulsars at optical wavelengths

    NASA Astrophysics Data System (ADS)

    Mignani, Roberto; Marelli, Martino; Shearer, Andrew; Slowikowska, Agnieszka

    2016-07-01

    Polarisation measurements of pulsars offer unique insights into their highly-magnetised relativistic environments and represent a primary test for neutron star magnetosphere models and radiation emission mechanisms. Besides the radio band, optical observations have been, so far, best suited to these goals, with polarisation measurements in the X-rays becoming possible in the near future thanks to missions, such as XIPE and IXPE. In this talk, we review the status of the optical polarisation measurements of pulsars and we foresee possible synergies between X-ray polarimetry observations of selected pulsars with, e.g XIPE and IXPE, and optical observations with the next generation of extremely large telescope, such as the E-ELT.

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

    SciTech Connect

    Kinoshita, Takayoshi; Tamada, Taro; Imai, Keisuke; Kurihara, Kazuo; Ohhara, Takashi; Tada, Toshiji; Kuroki, Ryota

    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.

  20. Preliminary time-of-flight neutron diffraction study of human deoxyhemoglobin

    SciTech Connect

    Kovalevsky, A. Y.; Chatake, T.; Shibayama, N.; Park, S.-Y.; Ishikawa, T.; Mustyakimov, M.; Fisher, S. Z.; Langan, P.; Morimoto, Y.

    2008-04-01

    In order to investigate the role of the protonation states of protein residues in O{sub 2} binding, large crystals of deoxy HbA (∼20 mm{sup 3}) were grown in D{sub 2}O under anaerobic conditions for neutron diffraction studies. Human hemoglobin (HbA) is an intricate system that has evolved to efficiently transport oxygen molecules (O{sub 2}) from lung to tissue. Its quaternary structure can fluctuate between two conformations, T (tense or deoxy) and R (relaxed or oxy), which have low and high affinity for O{sub 2}, respectively. The binding of O{sub 2} to the heme sites of HbA is regulated by protons and by inorganic anions. In order to investigate the role of the protonation states of protein residues in O{sub 2} binding, large crystals of deoxy HbA (∼20 mm{sup 3}) were grown in D{sub 2}O under anaerobic conditions for neutron diffraction studies. A time-of-flight neutron data set was collected to 1.8 Å resolution on the Protein Crystallography Station (PCS) at the spallation source run by Los Alamos Neutron Science Center (LANSCE). The HbA tetramer (64.6 kDa; 574 residues excluding the four heme groups) occupies the largest asymmetric unit (space group P2{sub 1}) from which a high-resolution neutron data set has been collected to date.

  1. A rotator for single-crystal neutron diffraction at high pressure.

    PubMed

    Fang, J; Bull, C L; Hamidov, H; Loveday, J S; Gutmann, M J; Nelmes, R J; Kamenev, K V

    2010-11-01

    We present a modified Paris-Edinburgh press which allows rotation of the anvils and the sample under applied load. The device is designed to overcome the problem of having large segments of reciprocal space obscured by the tie rods of the press during single-crystal neutron-scattering experiments. The modified press features custom designed hydraulic bearings and provides controls for precision rotation and positioning. The advantages of using the device for increasing the number of measurable reflections are illustrated with the results of neutron-diffraction experiments on a single crystal of germanium rotated under a load of 70 tonnes. PMID:21133480

  2. Microscopic structure factor of liquid hydrogen by neutron-diffraction measurements

    NASA Astrophysics Data System (ADS)

    Celli, M.; Bafile, U.; Cuello, G. J.; Formisano, F.; Guarini, E.; Magli, R.; Neumann, M.; Zoppi, M.

    2005-01-01

    The center-of-mass structure factor of liquid para hydrogen has been measured, using neutron diffraction, in four thermodynamic states close to the triple point. Path integral Monte Carlo simulations have been carried out at the same temperatures and densities. The present experimental data are in reasonable quantitative agreement with the simulations and closer to these results than previous neutron determinations available in the literature. The thermodynamic derivatives of the structure factor, from both experiment and simulation, have been compared to previous measurements obtaining a quantitative consistency.

  3. MnO spin-wave dispersion curves from neutron powder diffraction

    SciTech Connect

    Goodwin, Andrew L.; Dove, Martin T.; Tucker, Matthew G.; Keen, David A.

    2007-02-15

    We describe a model-independent approach for the extraction of spin-wave dispersion curves from powder neutron total scattering data. Our approach is based on a statistical analysis of real-space spin configurations to calculate spin-dynamical quantities. The RMCPROFILE implementation of the reverse Monte Carlo refinement process is used to generate a large ensemble of supercell spin configurations from MnO powder diffraction data collected at 100 K. Our analysis of these configurations gives spin-wave dispersion curves for MnO that agree well with those determined independently using neutron triple-axis spectroscopic techniques.

  4. Heterogeneous Catalysis under pressure - In-situ neutron diffraction under industrial conditions

    NASA Astrophysics Data System (ADS)

    Kandemir, Timur; Girgsdies, Frank; Kasatkin, Igor; Kunkes, Edward; Liss, Klaus-Dieter; Peterson, Vanessa K.; Schlögl, Robert; Behrens, Malte

    2012-02-01

    The present work describes the application of a tubular reactor that allows in-situ neutron diffraction on working catalysts at high pressures. The designed reactor enables the application to a sample of industrially-relevant reaction conditions, i.e., in a temperature range up to 330° C and 60 bar pressure, coupled with online gas-analysis. Application of the cell is demonstrated by ammonia synthesis over a commercial catalyst with diffraction data obtained from the high-resolution powder diffractometer, Echidna, at the Australian Nuclear Science and Technology Organisation, ANSTO.

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

    DOE PAGESBeta

    Mauro, N. A.; Vogt, A. J.; Derendorf, K. S.; Johnson, M. L.; Rustan, G. E.; Quirinale, D. G.; Kreyssig, A.; Lokshin, K. A.; Neuefeind, J. C.; An, Ke; et al

    2016-01-01

    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. But, 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 elasticmore » 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%. Furthermore, to demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr64Ni36 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).« less

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

    SciTech Connect

    Mauro, N. A.; Vogt, A. J.; Derendorf, K. S.; Johnson, M. L.; Rustan, G. E.; Quirinale, D. G.; Kreyssig, A.; Lokshin, K. A.; Neuefeind, J. C.; An, Ke; Wang, Xun-Li; Goldman, A. I.; Egami, T.; Kelton, K. F.

    2016-01-01

    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. But, 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%. Furthermore, to demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr64Ni36 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).

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

    NASA Astrophysics Data System (ADS)

    Mauro, N. A.; Vogt, A. J.; Derendorf, K. S.; Johnson, M. L.; Rustan, G. E.; Quirinale, D. G.; Kreyssig, A.; Lokshin, K. A.; Neuefeind, J. C.; An, Ke; Wang, Xun-Li; Goldman, A. I.; Egami, T.; Kelton, K. F.

    2016-01-01

    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 Zr64Ni36 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).

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

    PubMed

    Mauro, N A; Vogt, A J; Derendorf, K S; Johnson, M L; Rustan, G E; Quirinale, D G; Kreyssig, A; Lokshin, K A; Neuefeind, J C; An, Ke; Wang, Xun-Li; Goldman, A I; Egami, T; Kelton, K F

    2016-01-01

    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 Zr64Ni36 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). PMID:26827330

  9. Structural analysis of a completely amorphous {sup 238}Pu-doped zircon by neutron diffraction.

    SciTech Connect

    Fortner, J. A.; Badyal, Y.; Price, D. C.; Hanchar, J. M.; Weber, W. J.; Materials Science Division; PNNL

    1999-01-01

    The structure of a completely amorphous zircon was determined by time-of-flight neutron diffraction at Argonne's Intense Pulsed Neutron Source (IPNS). The sample of metamict zircon (ZrSiO{sub 4}), initially doped to 8.85 weight percent {sup 238}Pu, had been completely amorphized by alpha-recoil damage since its synthesis in 1981 at the Pacific Northwest National Laboratory (PNNL). The measured diffraction structure factor, S(Q), indicated a completely amorphous sample, with no signs of residual zircon microcrystallinity. The pair distribution function obtained indicated that the structure was that of an oxide glass, retaining the Si-0, Zr-0, and O-O bond lengths of crystalline zircon.

  10. Structural analysis of a completely amorphous {sup 238}Pu-doped zircon by neutron diffraction.

    SciTech Connect

    Fortner, J. A.

    1998-12-16

    The structure of a completely amorphous zircon was determined by time-of-flight neutron diffraction at Argonne's Intense Pulsed Neutron Source (IPNS). The sample of metamict zircon (ZrSiO{sub 4}),initially doped to 8.85 weight percent {sup 238}Pi, had been completely amorphized by alpha-recoil damage since its synthesis in 1981 at the Pacific Northwest National Laboratory (PNNL). The measured diffraction structure factor, S(Q), indicated a completely amorphous sample, with no signs of residual zircon microcrystallinity. The pair distribution function obtained indicated that the structure was that of an oxide glass, retaining the Si-0, Zr-0, and O-O bond lengths of crystalline zircon.

  11. X-ray and neutron diffraction study of nanocrystalline Ti-Ru-Fe-O compounds

    SciTech Connect

    Blouin, M.; Guay, D.; Huot, J.; Schulz, R.; Swainson, I.P.

    1998-11-01

    The effect of adding oxygen on the structure of nanocrystalline Ti-Ru-Fe compounds obtained by high-energy ball-milling has been studied by X-ray and neutron diffraction using a Rietveld refinement analysis. It is shown that oxygen atoms readily oxidize Ti to form various types of titanium oxides depending on the oxygen content. In each case, a simple cubic structure (cP2-CsCl) is also formed during milling but with a concentration higher than expected on the basis of various reaction schemes. Through a detailed analysis of the neutron and X-ray diffraction peaks, it is shown that the 1a site of the CsCl-type unit cell is depleted from Ti atoms by preferential substitution with Fe. At high oxygen concentration, the alloy is a multiphase material containing Ti{sub 2{minus}x}Ru{sub 1+y}Fe{sub 1+z}, Ti oxides, Ru, and Fe.

  12. Neutron diffraction measurements and modeling of residual strains in metal matrix composites

    NASA Technical Reports Server (NTRS)

    Saigal, A.; Leisk, G. G.; Hubbard, C. R.; Misture, S. T.; Wang, X. L.

    1996-01-01

    Neutron diffraction measurements at room temperature are used to characterize the residual strains in tungsten fiber-reinforced copper matrix, tungsten fiber-reinforced Kanthal matrix, and diamond particulate-reinforced copper matrix composites. Results of finite element modeling are compared with the neutron diffraction data. In tungsten/Kanthal composites, the fibers are in compression, the matrix is in tension, and the thermal residual strains are a strong function of the volume fraction of fibers. In copper matrix composites, the matrix is in tension and the stresses are independent of the volume fraction of tungsten fibers or diamond particles and the assumed stress free temperature because of the low yield strength of the matrix phase.

  13. α-Phase transformation kinetics of U - 8 wt% Mo established by in situ neutron diffraction

    NASA Astrophysics Data System (ADS)

    Steiner, M. A.; Calhoun, C. A.; Klein, R. W.; An, K.; Garlea, E.; Agnew, S. R.

    2016-08-01

    The α-phase transformation kinetics of as-cast U - 8 wt% Mo below the eutectoid temperature have been established by in situ neutron diffraction. α-phase weight fraction data acquired through Rietveld refinement at five different isothermal hold temperatures can be modeled accurately utilizing a simple Johnson-Mehl-Avrami-Kolmogorov impingement-based theory, and the results are validated by a corresponding evolution in the γ-phase lattice parameter during transformation that follows Vegard's law. Neutron diffraction data is used to produce a detailed Time-Temperature-Transformation diagram that improves upon inconsistencies in the current literature, exhibiting a minimum transformation start time of 40 min at temperatures between 500 °C and 510 °C. The transformation kinetics of U - 8 wt% Mo can vary significantly from as-cast conditions after extensive heat treatments, due to homogenization of the typical dendritic microstructure which possesses non-negligible solute segregation.

  14. Neutron diffraction measurements and modeling of residual strains in metal matrix composites

    SciTech Connect

    Saigal, A.; Leisk, G.G.; Hubbard, C.R.; Misture, S.T.; Wang, X.L.

    1996-04-01

    Neutron diffraction measurements at room temperature are used to characterize the residual strains in tungsten fiber-reinforced copper matrix, tungsten fiber-reinforced Kanthal matrix, and diamond particulate-reinforced copper matrix composites. Results of finite element modeling are compared with the neutron diffraction data. In tungsten/Kanthal composites, the fibers are in compression, the matrix is in tension, and the thermal residual strains are a strong function of the volume fraction of fibers. In copper matrix composites, the matrix is in tension and the stresses are independent of the volume fraction of tungsten fibers or diamond particles and the assumed stress free temperature because of the low yield strength of the matrix phase.

  15. Bauschinger Effect in an Austenitic Steel: Neutron Diffraction and a Multiscale Approach

    NASA Astrophysics Data System (ADS)

    Fajoui, Jamal; Gloaguen, David; Legrand, Vincent; Oum, Guy; Kelleher, Joe; Kockelmann, Winfried

    2016-05-01

    The generation of internal stresses/strains arising from mechanical deformations in single-phase engineering materials was studied. Neutron diffraction measurements were performed to study the evolution of intergranular strains in austenitic steel during sequential loadings. Intergranular strains expand due to incompatibilities between grains and also resulting from single-crystal elastic and plastic anisotropy. A two-level homogenization approach was adopted in order to predict the mechanical state of deformed polycrystals in relation to the microstructure during Bauschinger tests. A mechanical description of the grain was developed through a micro-meso transition based on the Kröner model. The meso-macro transition using a self-consistent approach was applied to deduce the global behavior. Mechanical tests and neutron diffraction measurements were used to validate and assess the model.

  16. In-Situ Studies of Intercritically Austempered Ductile Iron Using Neutron Diffraction

    SciTech Connect

    Druschitz, Alan; Aristizabal, Ricardo; Druschitz, Edward; Hubbard, Camden R; Watkins, Thomas R; Walker, Larry R; Ostrander, M

    2012-01-01

    Intercritically austempered ductile irons hold promise for applications requiring fatigue durability, excellent castability, low production energy requirements, reduced greenhouse gas emissions and excellent machinability. In the present study, four different ductile iron alloys, containing manganese and nickel as the primary austenite-stabilizing elements, were heat treated to obtain different quantities of austenite in the final microstructure. This paper reports the microstructures and phases present in these alloys. Further, lattice strains and diffraction elastic constants in various crystallographic directions and the transformation characteristics of the austenite as a function of applied stress were determined using in-situ loading with neutron diffraction at the second generation Neutron Residual Stress Facility (NRSF2) at the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL).

  17. Revealing cyclic hardening mechanism of a TRIP steel by real-time in situ neutron diffraction

    SciTech Connect

    Yu, Dunji; An, Ke; Chen, Yan; Chen, Xu

    2014-01-01

    Real-time in situ neutron diffraction was performed on a transformation-induced plasticity (TRIP) steel under cyclic loading at room temperature. By Rietveld refinement and single peak analysis, the volume fraction and average stress estimates as well as dislocation density of individual phases (austenite and martensite phase) were derived. The results reveal that the volume fraction of martensite phase, instead of individual phase strengthening, should be accounted for the remarkable secondary cyclic hardening.

  18. Texture analysis of bulk YBa sub 2 Cu sub 3 O sub x by neutron diffraction

    SciTech Connect

    Kallend, J.S. ); Biondo, A.C.; Schultz, A.J.; Goretta, K.C. )

    1990-09-01

    Neutron diffraction has been used to generate Orientation Distribution Functions for two sinter-forged YBa{sub 2}Cu{sub 3}O{sub x} specimens. Sinter forging imparted a strong texture, with c axes of crystals preferentially aligned parallel to the forging direction. The distribution of a and b axes was not uniform, which may have implications to critical current density. 14 refs., 6 figs.

  19. Monte-Carlo sorption and neutron diffraction study of the filling isotherm in clathrate hydrates

    SciTech Connect

    Klapproth, Alice; Kuhs, Werner F.; Chazallon, Bertrand

    1999-06-15

    We are interested in the thermodynamics of the gas filling of clathrate hydrates. In order to determine the pressure-dependent filling of the cages, neutron powder diffraction experiments on N{sub 2} and CO{sub 2} clathrates were performed. Interaction potentials were refined by comparing the experimentally determined fillings with those generated by MC-sorption calculations. Unsatisfactory agreement between experiment and simulation is observed when using the widely employed SPC water-water interaction potential.

  20. Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

    DOE PAGESBeta

    Wang, H.; Kirkham, M. J.; Watkins, T. R.; Payzant, E. A.; Salvador, J. R.; Thompson, A. J.; Sharp, J.; Brown, D.; Miller, D.

    2016-02-17

    N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

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

    SciTech Connect

    Todd, R.I.; Borsa, C.; Derby, B.; Bourke, M.A.M.

    1994-07-01

    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{sub 2}O{sub 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.

  2. Neutron diffraction and the electronic properties of BaFe2Se3

    NASA Astrophysics Data System (ADS)

    Lovesey, S. W.; Khalyavin, D. D.; van der Laan, G.

    2016-01-01

    It is argued on the basis of previously published experimental data that, the magnetic space-group Cac (#9.41) is the correct description of magnetically ordered BaFe2Se3. The corresponding crystal class m1‧ allows axial and polar dipoles and forbids bulk ferromagnetism. Magneto-electric multipoles that are both time-odd and parity-odd are allowed, e.g., a magnetic charge (monopole) and an anapole (magnetic toroidal dipole). The experimental observation of magneto-electric multipoles must shed light on valence electrons involved in bonding, including charge transfer using 3d(Fe) and p-states of ligand ions. We provide the appropriate structure factors for the Bragg diffraction neutrons, together with estimates of atomic form factors. Structure factors for resonant x-ray Bragg diffraction are also considered, because the analysis of successful experiments will yield complementary information about electronic properties. Magneto-electric multipoles, over and above those that contribute to magnetic neutron diffraction, include the magnetic monopole. A time-odd, parity-even monopole created from the magnetic dipole and an electric toroidal dipole, which is a manifestation of a structural rotation, is allowed in BaFe2Se3 but it is not visible in diffraction, nor is the corresponding dipole.

  3. In situ neutron diffraction under high pressure—Providing an insight into working catalysts

    NASA Astrophysics Data System (ADS)

    Kandemir, Timur; Wallacher, Dirk; Hansen, Thomas; Liss, Klaus-Dieter; Naumann d'Alnoncourt, Raoul; Schlögl, Robert; Behrens, Malte

    2012-05-01

    In the present work the construction and application of a continuous flow cell is presented, from which neutron diffraction data could be obtained during catalytic reactions at high pressure. By coupling an online gas detection system, parallel structure and activity investigations of working catalysts under industrial relevant conditions are possible. The flow cell can be operated with different feed gases in a wide range from room temperature to 603 K. Pressures from ambient up to 6 MPa are applicable. An exchangeable sample positioning system makes the flow cell suitable for several different goniomter types on a variety of instrument beam lines. Complementary operational test measurements were carried out monitoring reduction of and methanol synthesis over a Cu/ZnO/Al2O3 catalyst at the high-flux powder diffraction beamline D1B at ILL and high-resolution diffraction beamline Echidna at ANSTO.

  4. Investigation of the structure of multilayer lipid membranes by real-time neutron diffraction

    NASA Astrophysics Data System (ADS)

    Ryabova, N. Yu.; Kiselev, M. A.; Beskrovnyĭ, A. I.; Balagurov, A. M.

    2010-05-01

    This paper reports on the results of neutron diffraction experiments on the study of structural changes in multilayer lipid membranes as a function of the degree of hydration. The experiments have been performed on a time-of-flight diffractometer at the IBR-2 pulsed reactor (Joint Institute for Nuclear Research, Dubna, Russia) with a dipalmitoylphosphatidylcholine (DPPC) multilayer membrane oriented on a quartz plate. The structural parameters have been determined from the simultaneously measured several (up to five) diffraction orders of reflection, which has made it possible to calculate the profile of the DPPC bilayer structure. A high rate of the measurement of diffraction patterns has allowed one to trace the evolution the lamellar structure of the lipid bilayer in the course of its hydration and dehydration. The minimum time of accumulation of the necessary statistics is 3 min, which has made it possible to determine the characteristic times of transition processes in the membrane with a high accuracy.

  5. Magnetic symmetries in neutron and resonant x-ray Bragg diffraction patterns of four iridium oxides

    NASA Astrophysics Data System (ADS)

    Lovesey, S. W.; Khalyavin, D. D.; Manuel, P.; Chapon, L. C.; Cao, G.; Qi, T. F.

    2012-12-01

    The magnetic properties of Sr2IrO4, Na2IrO3, Sr3Ir2O7 and CaIrO3 are discussed, principally in the light of experimental data in recent literature for Bragg intensities measured in x-ray diffraction with enhancement at iridium L-absorption edges. The electronic structure factors we report, which incorporate parity-even and acentric entities, serve the immediate purpose of making full use of crystal and magnetic symmetry to refine our knowledge of the magnetic properties of the four iridates from resonant x-ray diffraction data. They also offer a platform on which to interpret future investigations, using dichroic signals, resonant x-ray diffraction and neutron diffraction, for example, as well as ab initio calculations of electronic structure. Unit-cell structure factors, suitable for x-ray Bragg diffraction enhanced by an electric dipole-electric dipole (E1-E1) event, reveal exactly which iridium multipoles are visible, e.g., a magnetic dipole parallel to the crystal c-axis (z-axis) and an electric quadrupole with yz-like symmetry in the specific case of CaIrO3. Magnetic space-groups are assigned to Sr2IrO4, Sr3Ir2O7 and CaIrO3, namely, PIcca, PAban and Cm‧cm‧, respectively, in the Belov-Neronova-Smirnova notation. The assignment for Sr2IrO4 is possible because of our new high-resolution neutron diffraction data, gathered on a powder sample. In addition, the new data are used to show that the ordered magnetic moment of an Ir4+ ion in Sr2IrO4 does not exceed 0.29(4) μB. Na2IrO3 has two candidate magnetic space-groups that are not resolved with currently available resonant x-ray data.

  6. The ferroelectric phase of CdTiO{sub 3}: A powder neutron diffraction study

    SciTech Connect

    Kennedy, Brendan J.; Zhou Qingdi; Avdeev, Maxim

    2011-11-15

    The synthesis of bulk samples of polycrystalline CdTiO{sub 3} in both the rhombohedral ilmenite and orthorhombic perovskite forms is described and the structures of these have been refined using powder neutron diffraction data. This involved the preparation of samples enriched in {sup 114}Cd. Cooling perovskite-type CdTiO{sub 3} to 4 K induces a ferroelectric phase transition, with the neutron data suggesting the low temperature structure is in Pna2{sub 1}. Mode analysis shows the polar mode to be dominant at low temperatures. The ilmenite-structure of CdTiO{sub 3} is compared with that of ZnTiO{sub 3}. The refined scattering length of the {sup 114}Cd is estimated to be 5.56 fm. Attempts to dope CdTiO{sub 3} with Ca and Sr are described. - Graphical abstract: The structure of three phases of CdTiO{sub 3} have been refined using high resolution powder neutron diffraction data. This involved the preparation of samples enriched in {sup 114}Cd. Cooling perovskite-type CdTiO{sub 3} to 4 K results in a ferroelectric phase in Pna2{sub 1}. Highlights: > Both the ilmenite and perovskite forms of CdTiO{sub 3} have been prepared using {sup 114}Cd. > Cooling the perovskite form results in a ferroelectric phase. > The structures of these are refined from powder neutron diffraction data. > Attempts to dope CdTiO{sub 3} are described.

  7. Neutron diffraction study of hydrogen-bond symmetrization in δ-AlOOD

    NASA Astrophysics Data System (ADS)

    Sano-Furukawa, A.; Hattori, T.; Kuribayashi, T.

    2013-12-01

    δ-AlOOH, a high-pressure polymorph of diaspore, is an important hydrous mineral in the deep earth that has the ability to transport hydrogen into the lower mantle. Theoretical studies have pointed out that hydrogen would locate at the center between two oxygen atoms at high pressure, which is so called hydrogen-bond symmetrization [1]. It was also suggested that the symmetrization would trigger the increase of bulk modulus, which is one of the important parameters of minerals at high pressure. The transition of δ-AlOOH(D) at high pressure has been suggested by X-ray and neutron diffraction [2, 3]. X-ray diffraction study found that the axes a and b where the hydrogen bond is oriented become less compressible above 12 GPa in δ-AlOOD. Neutron diffraction study on δ-AlOOD up to 9.2 GPa showed the increase of O-D bond distance, that is considered as a precousor phenomena of the symmetrization. However, the pressure was insufficient to observe the symmetrization. To investigate the symmetrization of hydrogen bond directly, we conducted neutron diffraction experiments to 16.7 GPa at PLANET, MLF in J-PARC. Powder sample of δ-AlOOD was loaded in Paris-Edinburgh press with double-toroid sintered diamond anvils with methanol-ethanol mixture of pressure medium. In the experiments, the disappearance of 120 refrection was observed at 12.1 GPa, indicating the transition from P21nm to Pnnm, which can be attributed to the disorder of hydrogen bond or the symmtrization. Results of Rietveld refienment will be shown in the presentation. [1] Tsuchiya et al., Geophys. Res. Lett., 29, 1909, 2002. [2] Sano-Furukawa et al., Am. Mineral., 93, 1558-1567, 2008. [3] Sano-Furukawa et al., Am. Mineral., 94, 1255-1261, 2009.

  8. Polarised light sheet tomography.

    PubMed

    Reidt, Sascha L; O'Brien, Daniel J; Wood, Kenneth; MacDonald, Michael P

    2016-05-16

    The various benefits of light sheet microscopy have made it a widely used modality for capturing three-dimensional images. It is mostly used for fluorescence imaging, but recently another technique called light sheet tomography solely relying on scattering was presented. The method was successfully applied to imaging of plant roots in transparent soil, but is limited when it comes to more turbid samples. This study presents a polarised light sheet tomography system and its advantages when imaging in highly scattering turbid media. The experimental configuration is guided by Monte Carlo radiation transfer methods, which model the propagation of a polarised light sheet in the sample. Images of both reflecting and absorbing phantoms in a complex collagenous matrix were acquired, and the results for different polarisation configurations are compared. Focus scanning methods were then used to reduce noise and produce three-dimensional reconstructions of absorbing targets. PMID:27409945

  9. Time-of-flight neutron diffraction study of bovine [gamma]-chymotrypsin at the Protein Crystallography Station

    SciTech Connect

    Lazar, Louis M.; Fisher, S. Zoe; Moulin, Aaron G.; Kovalevsky, Andrey; Novak, Walter R.P.; Langan, Paul; Petsko, Gregory A.; Ringe, Dagmar

    2012-02-06

    The overarching goal of this research project is to determine, for a subset of proteins, exact hydrogen positions using neutron diffraction, thereby improving H-atom placement in proteins so that they may be better used in various computational methods that are critically dependent upon said placement. In order to be considered applicable for neutron diffraction studies, the protein of choice must be amenable to ultrahigh-resolution X-ray crystallography, be able to form large crystals (1 mm{sup 3} or greater) and have a modestly sized unit cell (no dimension longer than 100 {angstrom}). As such, {gamma}-chymotrypsin is a perfect candidate for neutron diffraction. To understand and probe the role of specific active-site residues and hydrogen-bonding patterns in {gamma}-chymotrypsin, neutron diffraction studies were initiated at the Protein Crystallography Station (PCS) at Los Alamos Neutron Science Center (LANSCE). A large single crystal was subjected to H/D exchange prior to data collection. Time-of-flight neutron diffraction data were collected to 2.0 {angstrom} resolution at the PCS with 85% completeness. Here, the first time-of-flight neutron data collection from {gamma}-chymotrypsin is reported.

  10. Tau polarisation at LEP

    NASA Astrophysics Data System (ADS)

    Alemany, Ricard

    1999-04-01

    The measurements of the tau polarisation at LEP I are reviewed. Special emphasis is given to the new preliminary results presented at this conference. The ALEPH collaboration has studied the polarisation as a function of the polar angle using a new method based on the tau direction reconstruction and fully exploiting the angular correlations. A second traditional approach, based on the single tau decays has been also developed. The DELPHI collaboration has also studied the full data sample using an individual tau decay method and an inclusive hadronic selection. The results from the four experiments are presented with discussion of the compatibility among the methods and experiments.

  11. Preliminary neutron diffraction studies of Escherichia coli dihydrofolate reductase bound to the anticancer drug methotrexate

    SciTech Connect

    Bennett, Brad C.; Meilleur, Flora; Myles, Dean A A; Howell, Elizabeth E.; Dealwis, Chris G.

    2005-01-01

    The contribution of H atoms in noncovalent interactions and enzymatic reactions underlies virtually all aspects of biology at the molecular level, yet their 'visualization' is quite difficult. To better understand the catalytic mechanism of Escherichia coli dihydrofolate reductase (ecDHFR), a neutron diffraction study is under way to directly determine the accurate positions of H atoms within its active site. Despite exhaustive investigation of the catalytic mechanism of DHFR, controversy persists over the exact pathway associated with proton donation in reduction of the substrate, dihydrofolate. As the initial step in a proof-of-principle experiment which will identify ligand and residue protonation states as well as precise solvent structures, a neutron diffraction data set has been collected on a 0.3 mm{sup 3} D{sub 2}O-soaked crystal of ecDHFR bound to the anticancer drug methotrexate (MTX) using the LADI instrument at ILL. The completeness in individual resolution shells dropped to below 50% between 3.11 and 3.48 {angstrom} and the I/{sigma}(I) in individual shells dropped to below 2 at around 2.46 {angstrom}. However, reflections with I/{sigma}(I) greater than 2 were observed beyond these limits (as far out as 2.2 {angstrom}). To our knowledge, these crystals possess one of the largest primitive unit cells (P6{sub 1}, a = b = 92, c = 73 {angstrom}) and one of the smallest crystal volumes so far tested successfully with neutrons.

  12. Crystallization and preliminary neutron diffraction experiment of human farnesyl pyrophosphate synthase complexed with risedronate

    PubMed Central

    Yokoyama, Takeshi; Ostermann, Andreas; Mizuguchi, Mineyuki; Niimura, Nobuo; Schrader, Tobias E.; Tanaka, Ichiro

    2014-01-01

    Nitrogen-containing bisphosphonates (N-BPs), such as risedronate and zoledronate, are currently used as a clinical drug for bone-resorption diseases and are potent inhibitors of farnesyl pyrophosphate synthase (FPPS). X-ray crystallographic analyses of FPPS with N-BPs have revealed that N-BPs bind to FPPS with three magnesium ions and several water molecules. To understand the structural characteristics of N-BPs bound to FPPS, including H atoms and hydration by water, neutron diffraction studies were initiated using BIODIFF at the Heinz Maier-Leibnitz Zentrum (MLZ). FPPS–risedronate complex crystals of approximate dimensions 2.8 × 2.5 × 1.5 mm (∼3.5 mm3) were obtained by repeated macro-seeding. Monochromatic neutron diffraction data were collected to 2.4 Å resolution with 98.4% overall completeness. Here, the first successful neutron data collection from FPPS in complex with N-BPs is reported. PMID:24699741

  13. Structure of molten Al and eutectic Al-Si alloy studied by neutron diffraction

    SciTech Connect

    Dahlborg, U.; Kramer, Matthew J.; Besser, M.; Morris, J. R.; Calvo-Dahlborg, M.

    2012-11-24

    The structure of molten eutectic Al87.8Si12.2 alloy has been studied by neutron diffraction during a temperature cycle. For comparison measurements were performed on pure molten Al. The measurements show that the alloy after heating above the liquidus contains particles of two kinds, aluminum-rich and silicon-rich. The silicon-rich particles are partly dissolved after a further heating. Earlier published data obtained by the γ-ray absorption technique of the density of the molten eutectic Al–Si alloy had demonstrated the existence of two temperatures above the liquidus temperature: A dissolution temperature Td, at which the microstructure of the melt inherited from the ingot starts to dissolve and a branching temperature, Tb, at which the melt reaches a fully mixed state. The highest temperature that was possible to reach during the neutron experiments lies between Td and Tb. The obtained results support these conclusions that molten alloys after melting are inhomogeneous up to a temperature well above the liquidus. Moreover, the difference in shape between the static structure factors measured by neutron and X-ray diffraction on molten aluminum is observed and is found to be more accentuated and to extend to larger wavevectors than in earlier works.

  14. Characterisation of Residual Stresses Generated by Laser Shock Peening by Neutron and Synchrotron Diffraction

    NASA Astrophysics Data System (ADS)

    Evans, Alexander Dominic; King, Andrew; Pirling, Thilo; Peyre, Patrice; Withers, Phillip John

    The fatigue behaviour of engineering alloys can be significantly improved through the application of mechanical surface treatments. These processes generate significant compressive residual stresses near surface by inhomogeneous plastic deformation. In the case of mechanical surface treatments such as laser shock peening, certain burnishing and rolling techniques and ultrasonic impact treatment (UIT), the compressive residual stress layer can extend to a depth of the order of millimeters, with balancing tensile stresses located deeper. Techniques to characterise the residual stresses generated by such mechanical surface treatments non-destructively are mainly limited to diffraction methods using penetrating neutron and synchrotron X-ray radiations. The application of these radiation sources is illustrated here by the characterisation of residual strain distributions in a two types of specimens treated with laser shock peening (LSP). Analyses of diffraction peak broadening provide qualitative information concerning the depth to which the plastic deformation of the treatments extends. Two case studies of laser shock peening of titanium and aluminium alloys is presented to demonstrate the capabilities of neutron and synchrotron diffraction techniques in the field of residual stress characterisation of surface engineered material non-destructively.

  15. Neutron diffraction analysis of residual strain/stress distribution in the vicinity of high strength welds

    NASA Astrophysics Data System (ADS)

    Mráz, L.; Karlsson, L.; Hamák, I.; Vrána, M.; Mikula, P.

    2010-06-01

    Residual stresses resulting from non homogeneous heat distribution during welding process belong to most significant factor influencing behavior of welded structures. These stresses are responsible for defect occurrence during welding and they are also responsible for crack initiation and propagation at the either static or dynamic load. The significant effect of weld metal chemical composition as well as the effect of fatigue load and local plastic deformation on residual stress distribution and fatigue life have been recognized for high strength steels welds. The changes in residual stress distribution have then positive effect on cold cracking behavior and also on fatigue properties of the welds [1-3]. Several experimental methods, both destructive and non-destructive, such as hole drilling method, X-ray diffraction, neutron diffraction and others, have been used to examine residual stress distribution in all three significant orientations in the vicinity of the welds. The present contribution summarizes the results of neutron diffraction measurements of residual stress distribution in the vicinity of single-pass high-strength-steel welds having different chemical composition as well as the influence of fatigue load and local plastic deformation. It has been observed that the chemical composition of the weld metal has a significant influence on the stress distribution around the weld. Similarly, by aplying both cyclic load or pre-stress load on the specimens, stress relaxation was observed even in the region of approximately 40 mm far from the weld toe.

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

    NASA Astrophysics Data System (ADS)

    Roberts, Matthew; Biendicho, Jordi Jacas; Hull, Stephen; Beran, Premysl; Gustafsson, Torbjörn; Svensson, Gunnar; Edström, Kristina

    2013-03-01

    This paper introduces a new cell design for the construction of lithium ion batteries with conventional electrochemical performance whilst allowing in situ neutron diffraction measurement. A cell comprising of a wound cathode, electrolyte and anode stack has been prepared. The conventional hydrogen-containing components of the cell have been replaced by hydrogen-free equivalents. The electrodes are fabricated using a PTFE binder, the electrolyte consists of deuterated solvents which are supported in a quartz glass fibre separator. Typical battery performance is reported using the hydrogen-free components with a specific capacity of 140 mA h g-1 being observed for LiFePO4 at a rate of 0.2 C. Neutron diffraction patterns of full cells were recorded with phase change reactions monitored. When aluminium packaging was used a better signal to noise ratio was obtained. The obtained atomic positions and lattice parameters for all cells investigated were found to be consistent with parameters refined from the diffraction pattern of a powder of the pure electrode material. This paper highlights the pertinent points in designing cells for these measurements and addresses some of the problems.

  17. Neutron and X-ray diffraction of plasma-sprayed zirconia-yttria thermal barrier coatings

    NASA Technical Reports Server (NTRS)

    Shankar, N. R.; Herman, H.; Singhal, S. P.; Berndt, C. C.

    1984-01-01

    ZrO2-7.8mol. pct. YO1.5, a fused powder, and ZrO2-8.7mol. pct. YO1.5, a prereacted powder, were plasma-sprayed onto steel substrates. Neutron diffraction and X-ray diffraction of the as-received powder, the powder plasma sprayed into water, as-sprayed coatings, and coatings heat-treated for 10 and 100 h were carried out to study phase transformations and ordering of the oxygen ions on the oxygen sublattice. The as-received fused powder has a much lower monoclinic percentage than does the pre-reacted powder, this resulting in a much lower monoclinic percentage in the coating. Heat treatment increases the percentages of the cubic and monoclinic phases, while decreasing the tetragonal content. An ordered tetragonal phase is detected by the presence of extra neutron diffraction peaks. These phase transformations and ordering will result in volume changes. The implications of these transformations on the performance of partially stabilized zirconia thermal barrier coatings is discussed.

  18. Structure of deuterated liquid n-butanol by neutron diffraction and molecular dynamics simulations

    NASA Astrophysics Data System (ADS)

    Cristiglio, Viviana; Gonzalez, Miguel Angel; Cuello, Gabriel Julio; Cabrillo, Carlos; Pardo, Luis Carlos; Silva-Santisteban, Alvaro

    Aliphatic alcohols are the simpler molecular liquids possessing a polar hydroxylic group and a nonpolar alkyl tail. While the structure of the smallest alcohols has been relatively well studied, no much attention has been paid to the temperature dependence of the pre-peak observed before the main diffraction peak. The role of H-bonding in causing this feature and the direct relation between the number of C atoms and their distance were discovered very early, suggesting a liquid picture constituted of straight chains joined by H-bonds with the formation of mesoscopic size clusters. X-rays and neutron diffraction measurements showed that the height of the pre-peak associated with the formation of H-bonds increases with temperature. To explain this counterintuitive effect, a complete diffraction study using two neutron diffractometers D4 and D16 (ILL, Grenoble, France) allowing to cover the range 0.01-23 Å t1 and exploring a temperature range from 100 K (glassy butanol) to 400 K (moderately supercritical conditions) has been conducted. Molecular Dynamics simulations using the OPLS-AA potential were also carried out as a function of temperature and compared to experiment. Experimental and numerical results of liquid n-butanol and its glassy transition will be presented.

  19. Similar quartz crystallographic textures in rocks of continental earth's crust (by neutron diffraction data): I. Quartz textures in monomineral rocks

    NASA Astrophysics Data System (ADS)

    Nikitin, A. N.; Ivankina, T. I.; Ullemeyer, K.; Vasin, R. N.

    2008-09-01

    Quartz crystallographic textures in different rocks have been investigated by neutron diffraction. Various types of crystallographic textures of quartz-bearing mineral associations in monomineral and multiphase rocks from a representative collection of samples have been revealed and classified. Experimental investigations have been performed on special neutron texture diffractometers designed at the Frank Laboratory of Neutron Physics and mounted in the seventh channel of the IBR-2 reactor at the Joint Institute for Nuclear Research (Dubna).

  20. Similar quartz crystallographic textures in rocks of continental earth's crust (by neutron diffraction data): I. Quartz textures in monomineral rocks

    SciTech Connect

    Nikitin, A. N. Ivankina, T. I.; Ullemeyer, K.; Vasin, R. N.

    2008-09-15

    Quartz crystallographic textures in different rocks have been investigated by neutron diffraction. Various types of crystallographic textures of quartz-bearing mineral associations in monomineral and multiphase rocks from a representative collection of samples have been revealed and classified. Experimental investigations have been performed on special neutron texture diffractometers designed at the Frank Laboratory of Neutron Physics and mounted in the seventh channel of the IBR-2 reactor at the Joint Institute for Nuclear Research (Dubna).

  1. Hydrogen site analysis of hydrous ringwoodite in mantle transition zone by pulsed neutron diffraction

    NASA Astrophysics Data System (ADS)

    Purevjav, Narangoo; Okuchi, Takuo; Tomioka, Naotaka; Abe, Jun; Harjo, Stefanus

    2014-10-01

    Hydrogen site positions and occupancies in the crystal structure of synthetic hydrous ringwoodite have been determined for the first time by high-resolution neutron powder diffraction conducted at the pulsed neutron source at Japan Proton Accelerator Research Complex (J-PARC). It is demonstrated that hydrogen exchanges not only with Mg or Fe but also with Si cations to form hydroxyl and hydrogen bonding, both within the relevant octahedra or tetrahedra created by their surrounding oxygen anions. The hydrated octahedra shrink, whereas the hydrated tetrahedra expand. The occurrence of simultaneous hydration of octahedra and tetraheda is thus unambiguously confirmed, whereby the latter plays an especially unique role in reducing seismic velocity and for enhancing the electrical conductivity of ringwoodite at high pressures and temperatures. These results provide distinctive implications for discussing the physical properties of hydrous ringwoodite occurring in the mantle transition zone and evaluating the actual water content in the zone.

  2. Intergranular Strain Evolution in Titanium During Tensile Loading: Neutron Diffraction and Polycrystalline Model

    NASA Astrophysics Data System (ADS)

    Gloaguen, David; Oum, Guy; Legrand, Vincent; Fajoui, Jamal; Moya, Marie-José; Pirling, Thilo; Kockelmann, Winfried

    2015-11-01

    Intergranular strains due to tensile plastic deformation were investigated in a commercially pure Ti. Neutron diffraction has been used to characterize the evolution of residual elastic strain in grains with different crystallographic orientations. Experimental data have been obtained for the macroscopic stress-strain curve and the intergranular strain evolution in the longitudinal and transverse direction relative to the uniaxial loading axis. The elasto-plastic self-consistent (EPSC) approach was used to model the deformation behavior of the studied material. Comparison between the neutron measurements and the model predictions shows that in most cases the EPSC approach can predict the lattice strain evolution and capture the plastic anisotropy observed in the experiments.

  3. The Existence of Ferroelectric Ice on Icy Bodies in Space: a Neutron Diffraction Study

    NASA Astrophysics Data System (ADS)

    Fukazawa, Hiroshi

    The complex behavior of water and the unusual properties of ferroelectric ice XI continue to attract much interest. Whether ice in the space exists as ice XI, is an important question, because long range electrostatic forces caused by the ferroelectricity might be an important factor for planet formation. From neutron diffraction experiments, we found the temperature and pressure conditions for the transformation of the largest fraction of ice into ferroelectric ice. It suggests that myriad big icy-bodies, which exist as dwarf planets and Kuiper Belt Object, consist of thick ferroelectric-ice surface. Furthermore, we report spectral and vibrational properties of ferroelectric ice investigated by inelastic neutron scattering and infrared absorption measurements. Because the spectral properties of ferroelectric ice are clearly different from those of ordinary ice, the distinct ferroelectric ice in the universe is detectable using infrared telescopes and planetary exploration.

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

    NASA Astrophysics Data System (ADS)

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

    2008-01-01

    An austenitic-martensitic nitrogen steel 0Kh16N4AB has been studied under load using high-resolution neutron diffraction analysis on an FSD neutron diffractometer at an IBR-2 reactor (Dubna) and on a diffractometer with a focusing monochromator on a reactor of the Nuclear Physics Institute (Czech Republic). Young's moduli calculated from different reflections of the martensite and austenite phases have been obtained. It has been found that the yield strength σ0.2 corresponding to the slip plane (111) of the austenite phase is anomalously low and that with increasing degree of uniaxial tension the width of lines (111)γ strongly grows. In the steel under consideration the plane (111) of the austenite phase appears to be an easy-slip plane that ensures the enhanced properties of the steel, i.e., the combination of a high ultimate strength (1600 MPa) with a high plasticity (δ = 16%).

  5. Determination of the residual stress tensor in textured zirconium alloy by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Sumin, V. V.; Papushkin, I. V.; Vasin, R. N.; Venter, А. M.; Balagurov, А. М.

    2012-02-01

    Results of neutron diffraction studies of crystallographic texture and residual stress tensor components in cold-worked and annealed cylindrical components made from E-110 zirconium alloy are presented. Those components are used as plugs in the fuel elements of the VVER-type reactors; the resident residual stresses influence the durability and safety of the fuel elements. The experiments were carried out on the neutron diffractometers at Dubna (the IBR-2 pulsed reactor) and Berlin Helmholtz-Zentrum (the BER II research reactor). It is shown that the samples have fiber texture that is changed considerably with annealing. The type I residual stress tensors for both samples were calculated by the BulkPathGEO model. The cold worked component has 136-166 MPa tensile residual stress in the radial direction and zero stress along the axial direction. Residual stress values in the annealed component are close to zero.

  6. The magnetic structure of Co(NCNH)₂ as determined by (spin-polarized) neutron diffraction

    SciTech Connect

    Jacobs, Philipp; Houben, Andreas; Senyshyn, Anatoliy; Müller, Paul; Dronskowski, Richard

    2013-06-01

    The magnetic structure of Co(NCNH)₂ has been studied by neutron diffraction data below 10 K using the SPODI and DNS instruments at FRM II, Munich. There is an intensity change in the (1 1 0) and (0 2 0) reflections around 4 K, to be attributed to the onset of a magnetic ordering of the Co²⁺ spins. Four different spin orientations have been evaluated on the basis of Rietveld refinements, comprising antiferromagnetic as well as ferromagnetic ordering along all three crystallographic axes. Both residual values and supplementary susceptibility measurements evidence that only a ferromagnetic ordering with all Co²⁺ spins parallel to the c axis is a suitable description of the low-temperature magnetic ground state of Co(NCNH)₂. The deviation of the magnetic moment derived by the Rietveld refinement from the expectancy value may be explained either by an incomplete saturation of the moment at temperatures slightly below the Curie temperature or by a small Jahn–Teller distortion. - Graphical abstract: The magnetic ground state of Co(NCNH)₂ has been clarified by (spin-polarized) neutron diffraction data at low temperatures. Intensity changes below 4 K arise due to the onset of ferromagnetic ordering of the Co²⁺ spins parallel to the c axis, corroborated by various (magnetic) Rietveld refinements. Highlights: • Powderous Co(NCNH)₂ has been subjected to (spin-polarized) neutron diffraction. • Magnetic susceptibility data of Co(NCNH)₂ have been collected. • Below 4 K, the magnetic moments align ferromagnetically with all Co²⁺ spins parallel to the c axis. • The magnetic susceptibility data yield an effective magnetic moment of 4.68 and a Weiss constant of -13(2) K. • The ferromagnetic Rietveld refinement leads to a magnetic moment of 2.6 which is close to the expectancy value of 3.

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

    NASA Technical Reports Server (NTRS)

    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

  8. Insights into Analogue Perovskite Solid Solutions from High-Resolution Neutron Powder Diffraction

    NASA Astrophysics Data System (ADS)

    Redfern, S. A.; Chaddock, E. H.; Becerro, A. I.

    2002-12-01

    Neutron powder diffraction provides a powerful tool for the study of phase transitions as a function of pressure, temperature, or chemical composition. The structural information obtainable from powders using diffractometers such as HRPD (ISIS, UK) or D2B (ILL, France) rivals, and in some respects exceeds what may be possible using conventional crystallographic techniques reliant on single crystals. We have used both instruments to explore the subtle phase transitions observed in the (CaxSr1-x)TiO3 and (SrxBa1-x)SnO3 solid solutions. We have also used low resolution high flux instruments to explore the thermal dependence of the superlattice behavior below the cubic to tetragonal phase transition in (CaxSr1-x)TiO3. In each case a sequence of phase transitions from Pm-3m through I4/mcm to Pbnm is seen as a function of composition, and is driven by the change in average radius of the B-cation. This sequence of transitions is the same as expected for a magnesium silicate perovskite structure on increasing temperature. It is now recognised that lower mantle perovskite is likely aluminous, with solid solution towards either a stoichiometric or oxygen-defect end-member. The analogue systems we have characterised have been doped with trivalent cations on the B site to explore the effect of such substitution on the sequence of phase transitions. High-temperature neutron diffraction shows that oxygen defects stabilize the higher symmetry structures, lowering Tc for the transition to cubic. New developments in high-T high-P neutron diffraction techniques will allow the extension of these ambient pressure studies to the investigation of the influence of pressure as a variable, and hence the extension of such analogue studies to the whole range of variables experienced in the lower mantle. These will be briefly outlined.

  9. Neutron diffraction of hydrogenous materials: Measuring incoherent and coherent intensities separately

    NASA Astrophysics Data System (ADS)

    Temleitner, László; Stunault, Anne; Cuello, Gabriel J.; Pusztai, László

    2015-07-01

    Accurate determination of the coherent static structure factor of any disordered material containing substantial amounts of proton nuclei has proven to be rather problematic by neutron diffraction, due to the large incoherent cross section of 1H. This problem has continued to set severe obstacles to the reliable determination of liquid structures of hydrogenous materials up to this day, by introducing large uncertainties whenever a sample with a 1H content larger than about 20% had to be investigated by neutron diffraction. Huge theoretical efforts over the past 40 years which were aimed at estimating the incoherent background of such data did not result in any practical solution to the problem. Here, we present data for the coherent and incoherent contributions to the total static structure of mixtures of light and heavy water. The measurements were done using the polarized neutron diffraction technique, which uniquely allows determination of the two contributions separately. The data covers a wide range of momentum transfer (0.8-21 Å-1) and the entire composition range, i.e., light water contents between 0 and 100% at five different values. We show that the measured incoherent scattering can be approximated by a Gaussian function. The separately measured coherent intensities exhibit signs of small inelastic contributions. Out of several possible approaches, we have chosen to subtract a cubic background using the reverse Monte Carlo algorithm. This algorithm has the advantage of requiring an actual physical model with thousands of realistic water molecules at the correct density describing the corrected data. Finally, coherent static structure factors for five different compositions of liquid H2O and D2O mixtures are presented for which the huge incoherent background could actually be measured and separated, instead of being approximated as it has been done so far. These experimental results provide a strong hope that determining the structure of hydrogenous

  10. Pulsed neutron powder diffraction at high pressure by a capacity-increased sapphire anvil cell

    NASA Astrophysics Data System (ADS)

    Okuchi, Takuo; Yoshida, Masashi; Ohno, Yoshiki; Tomioka, Naotaka; Purevjav, Narangoo; Osakabe, Toyotaka; Harjo, Stefanus; Abe, Jun; Aizawa, Kazuya; Sasaki, Shigeo

    2013-12-01

    A new design of opposed anvil cell for time-of-flight neutron powder diffraction was prepared for use at advanced pulsed sources. A couple of single-crystal sapphire sphere anvils and a gasket of fully hardened Ti-Zr null alloy were combined to compress 35 mm3 of sample volume to 1 GPa and 11 mm3 to 2 GPa of pressures, respectively. A very high-quality powder diffraction pattern was obtained at Japan Proton Accelerator Research Complex for a controversial high pressure phase of methane hydrate. The counting statistics, resolution, absolute accuracy and d-value range of the pattern were all improved to be best suitable for precise structure refinement. The sample is optically accessible to be measured by Raman and fluorescence spectroscopy during and after compression. The current cell will be an alternative choice to study hydrogenous materials of complex structures that are stable at the described pressure regime.

  11. Localization of glycolipids in membranes by in vivo labeling and neutron diffraction.

    PubMed

    Weik, M; Patzelt, H; Zaccai, G; Oesterhelt, D

    1998-02-01

    Evidence is accumulating for the lateral organization of cell membrane lipids and proteins in the context of sorting or intracellular signaling. So far, however, information has been lacking on the details of protein-lipid interactions in such aggregates. Purple membranes are patches made up of lipids and the protein bacteriorhodopsin in the plasma membrane of certain Archaea. Naturally crystalline, they provide a unique opportunity to study the structure of a natural membrane at submolecular resolution by diffraction methods. We present a direct structural determination of the glycolipids with respect to bacteriorhodopsin in these membranes. Deuterium labels incorporated in vivo into the sugar moieties of the major glycolipid were localized by neutron diffraction. The data suggest a role for specific aromatic residue-carbohydrate stacking interactions in the formation of the purple membrane crystalline patches. PMID:9660925

  12. Real-time observations of lithium battery reactions-operando neutron diffraction analysis during practical operation.

    PubMed

    Taminato, Sou; Yonemura, Masao; Shiotani, Shinya; Kamiyama, Takashi; Torii, Shuki; Nagao, Miki; Ishikawa, Yoshihisa; Mori, Kazuhiro; Fukunaga, Toshiharu; Onodera, Yohei; Naka, Takahiro; Morishima, Makoto; Ukyo, Yoshio; Adipranoto, Dyah Sulistyanintyas; Arai, Hajime; Uchimoto, Yoshiharu; Ogumi, Zempachi; Suzuki, Kota; Hirayama, Masaaki; Kanno, Ryoji

    2016-01-01

    Among the energy storage devices for applications in electric vehicles and stationary uses, lithium batteries typically deliver high performance. However, there is still a missing link between the engineering developments for large-scale batteries and the fundamental science of each battery component. Elucidating reaction mechanisms under practical operation is crucial for future battery technology. Here, we report an operando diffraction technique that uses high-intensity neutrons to detect reactions in non-equilibrium states driven by high-current operation in commercial 18650 cells. The experimental system comprising a time-of-flight diffractometer with automated Rietveld analysis was developed to collect and analyse diffraction data produced by sequential charge and discharge processes. Furthermore, observations under high current drain revealed inhomogeneous reactions, a structural relaxation after discharge, and a shift in the lithium concentration ranges with cycling in the electrode matrix. The technique provides valuable information required for the development of advanced batteries. PMID:27357605

  13. Real-time observations of lithium battery reactions—operando neutron diffraction analysis during practical operation

    PubMed Central

    Taminato, Sou; Yonemura, Masao; Shiotani, Shinya; Kamiyama, Takashi; Torii, Shuki; Nagao, Miki; Ishikawa, Yoshihisa; Mori, Kazuhiro; Fukunaga, Toshiharu; Onodera, Yohei; Naka, Takahiro; Morishima, Makoto; Ukyo, Yoshio; Adipranoto, Dyah Sulistyanintyas; Arai, Hajime; Uchimoto, Yoshiharu; Ogumi, Zempachi; Suzuki, Kota; Hirayama, Masaaki; Kanno, Ryoji

    2016-01-01

    Among the energy storage devices for applications in electric vehicles and stationary uses, lithium batteries typically deliver high performance. However, there is still a missing link between the engineering developments for large-scale batteries and the fundamental science of each battery component. Elucidating reaction mechanisms under practical operation is crucial for future battery technology. Here, we report an operando diffraction technique that uses high-intensity neutrons to detect reactions in non-equilibrium states driven by high-current operation in commercial 18650 cells. The experimental system comprising a time-of-flight diffractometer with automated Rietveld analysis was developed to collect and analyse diffraction data produced by sequential charge and discharge processes. Furthermore, observations under high current drain revealed inhomogeneous reactions, a structural relaxation after discharge, and a shift in the lithium concentration ranges with cycling in the electrode matrix. The technique provides valuable information required for the development of advanced batteries. PMID:27357605

  14. Neutron diffraction study of NiTi during compressive deformation and after shape-memory recovery

    SciTech Connect

    Dunand, D.C.; Mari, D.; Bourke, M.A.M.; Goldstone, J.A.

    1995-09-01

    Neutron diffraction measurements of internal elastic strains and texture were performed during compressive deformation of martensitic NiTi deforming by twinning. Rietveld refinement of the diffraction spectrum was performed in order to obtain lattice parameter variations and preferred orientation of martensitic variants. The elastic internal strains, are proportional to the externally applied stress but strongly dependent on crystallographic orientation. Plastic deformation by matrix twinning is consistent with type I (1-1-1) twinning, whereby (100) and (011) planes tend to align perpendicular and parallel to the stress axis, respectively. The preferred orientation ratio r according to the model by March and Dollase is proportional to the macroscopic plastic strain for (100) and (011) planes for loading, unloading and shape-memory recovery. To the best of our knowledge, this is the first in situ bulk measurement of reversible twinning in NiTi. Finally, shape-memory recovery results in a marked change of NiTi cell parameters.

  15. Structure of liquid equiatomic potassium--lead alloy: A neutron diffraction experiment

    SciTech Connect

    Saboungi, M.; Blomquist, R.; Volin, K.J.; Price, D.L.

    1987-08-15

    Neutron diffraction measurements have been performed on liquid equiatomic potassium--lead alloy at T = 870, 900, and 930 K to determine the influence of temperature on the structure. A well-defined first sharp diffraction peak (FSDP) at Q = 0.96 A/sup -1/, similar to that found in glassy materials, was obtained in the total structure factors S(Q) at the three temperatures. While the position of the peak remained unaffected by temperature changes, its magnitude decreased with increasing temperature. The other features of S(Q) were almost unaltered by temperature, as expected. The FSDP can be related to the presence of chemical bonds or clusters whose stability decreases with increasing temperature. A molecular model based on the random packing of K/sub 4/Pb/sub 4/ structural units is shown to give a remarkable correspondence with the measured structure factors.

  16. REVIEW ARTICLE: Determination of residual stresses in materials and industrial components by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Albertini, Gianni; Bruno, Giovanni; Carradò, Adele; Fiori, Fabrizio; Rogante, Massimo; Rustichelli, Franco

    1999-03-01

    We present a review of the determination of residual stresses in materials and components of industrial interest by using the non-destructive technique of neutron diffraction. The fundamental aspects are discussed, together with a brief description of the experimental facilities. Several experimental results are then reported, particularly concerning applications to materials and components for power plants (CrMo steel, AISI304 stainless steel and 2.25Cr1Mo ferritic steel), aerospace and automotive technology (Al alloys, metal matrix composites, nickel superalloy gas-turbine components) and fusion-reactor technology (AISI316L for the first wall). A few thermomechanical treatments are considered, such as welding, cold-expanded holes, thermoelastic coupling and thermal and mechanical fatigue. Moreover, a few applications to general industrial problems are shown, namely brazed ceramic-steel components, coatings and fatigue-cracked samples. In some cases, experimental results are compared with numerical models or results from x-ray diffraction measurements.

  17. The Crystal Structure of Thorium and Zirconium Dihydrides by X-ray and Neutron Diffraction

    DOE R&D Accomplishments Database

    Rundle, R.E.; Shull, C.G.; Wollan, E.O.

    1951-04-20

    Thorium forms a tetragonal lower hydride of composition ThH{sub 2}. The hydrides ThH{sub 2}, ThD{sub 2}, and ZrD{sub 2} have been studied by neutron diffraction in order that hydrogen positions could be determined. The hydrides are isomorphous, and have a deformed fluorite structure. Metal-hydrogen distances in thorium hydride are unusually large, as in UH{sub 3}. Thorium and zirconium scattering amplitudes and a revised scattering amplitude for deuterium are reported.

  18. Structural Study of Liquid Se-Te Alloys by Neutron Diffraction

    NASA Astrophysics Data System (ADS)

    Takeda, Shin'ichi; Tamaki, Shigeru; Waseda, Yoshio

    1986-12-01

    The neutron diffraction study of liquid Se-Te system has been carried out to reveal the origin of characteristic temperature dependence of various properties related to the structural order in atomic scale. The temperature dependence of measured structural functions of liquid SexTe1-x system could be explained by a gradual transition from two-fold coordinated component (non-metallic) to the three-fold coordinated one (metallic). The partial structure factors of these two-fold and three-fold coordinations are separated with the help of the thermodynamic data. A configurational model satisfying these situations is also presented.

  19. Neutron powder diffraction studies as a function of temperature of structure II hydrate formed from propane

    USGS Publications Warehouse

    Rawn, C.J.; Rondinone, A.J.; Chakoumakos, B.C.; Circone, S.; Stern, L.A.; Kirby, S.H.; Ishii, Y.

    2003-01-01

    Neutron powder diffraction data confirm that hydrate samples synthesized with propane crystallize as structure type II hydrate. The structure has been modeled using rigid-body constraints to describe C3H8 molecules located in the eight larger polyhedral cavities of a deuterated host lattice. Data were collected at 12, 40, 100, 130, 160, 190, 220, and 250 K and used to calculate the thermal expansivity from the temperature dependence of the lattice parameters. The data collected allowed for full structural refinement of atomic coordinates and the atomic-displacement parameters.

  20. Structure and dynamics of hydrogen molecules in the novel clathrate hydrate by high pressure neutron diffraction.

    PubMed

    Lokshin, Konstantin A; Zhao, Yusheng; He, Duanwei; Mao, Wendy L; Mao, Ho-Kwang; Hemley, Russell J; Lobanov, Maxim V; Greenblatt, Martha

    2004-09-17

    The D2 clathrate hydrate crystal structure was determined as a function of temperature and pressure by neutron diffraction for the first time. The hydrogen occupancy in the (32+X)H2.136H(2)O, x=0-16 clathrate can be reversibly varied by changing the large (hexakaidecahedral) cage occupancy between two and four molecules, while remaining single occupancy of the small (dodecahedral) cage. Above 130-160 K, the guest D2 molecules were found in the delocalized state, rotating around the centers of the cages. Decrease of temperature results in rotation freezing followed by a complete localization below 50 K. PMID:15447276

  1. Anomalous structural feature of LiNbO{sub 3} observed using neutron diffraction

    SciTech Connect

    Fernandez-Ruiz, R.; Bermudez, V.; Martin y Marero, D.

    2005-11-01

    An anomalous structural effect has been observed and analyzed on LiNbO{sub 3} at low temperature by neutron-diffraction experiments. Two minima in the unit-cell volume at 55 and 100 K related with maxima and minima in the volume vibrational isotropic factors of Li and Nb atoms, respectively, and a change in the curve slope of the spontaneous stress at 55 K have been identified. This fact, together with the shortening in distance of the Li and O layers at 55 K, has been related with variations in the Ps factor through the secondary pyroelectric effect.

  2. Neutron diffraction method for stored energy measurement in interstitial free steel

    SciTech Connect

    Rajmohan, N.; Hayakawa, Y.; Szpunar, J.A.; Root, J.H.

    1997-06-01

    Part of the energy acquired by polycrystalline metals during plastic deformation is stored in the form of dislocations and other crystal defects. A method is described for the measurement of the orientation dependence of the stored energy of cold work, using neutron diffraction line broadening. To illustrate the method, the measured stored energy values for 80% cold rolled interstitial free (IF) steel are compared with the stored energy in a stress relieved specimen. The correlation between the Taylor factor and the stored energy for an 80% cold rolled specimen is discussed.

  3. Residual stress measurements in a zircaloy-4 weld by neutron diffraction

    SciTech Connect

    Carr, D.G.; Ripley, M.I.; Holden, T.M.; Brown, D.W.; Vogel, S.C

    2004-08-16

    The macroscopic stress distribution across a Zircaloy-4 gas tungsten arc weld was measured by time-of-flight neutron diffraction at the SMARTS diffractometer at Los Alamos National Laboratory. The method enabled the measurement of strain for all the available reflections permitted by the rolling texture of the plate and the modified texture in the weld-metal and heat affected zone. A maximum longitudinal stress of 220 {+-} 40 MPa was observed in the weld compared with the 0.2% yield stress of 390 MPa of the plate. A maximum transverse stress of 60 {+-} 40 MPa was observed in the weld. Textures were measured at the HIPPO diffractometer.

  4. In situ observation of ErD2 formation during D-2 loading via neutron diffraction

    SciTech Connect

    Browning, Jim; Snow, Clark; Wixom, Ryan R; Llobet, Anna; Rodriguez, Mark

    2011-01-01

    In an effort to better understand the structural changes occurring during hydrogen loading of erbium target materials, we have performed in situ D{sub 2} loading of erbium metal (powder) at temperature (450 C) with simultaneous neutron diffraction analysis. This experiment tracked the conversion of Er metal to the {alpha} erbium deuteride (solid-solution) phase and then into the {beta} (fluorite) phase. Complete conversion to ErD{sub 2.0} was accomplished at 10 Torr D{sub 2} pressure with deuterium fully occupying the tetrahedral sites in the fluorite lattice.

  5. Non-contact measurement of the stress within granular materials via neutron diffraction

    NASA Astrophysics Data System (ADS)

    Wensrich, C. M.; Kisi, E. H.; Luzin, V.; Kirstein, O.

    2013-06-01

    For some time neutron diffraction approaches have provided the ability to look within solid materials in order to make accurate measurements of stress and strain. More recently this technique has been applied to granular materials with some very promising results. Measurements of this type provide detailed information on the distribution of the full triaxial stress state at all points within a sample; something that is not yet achievable using any other method. In this paper we outline the basic principles behind the method and provide an example of the type of data that it can provide.

  6. Molecular-dynamics modelling and neutron diffraction study of the site disorder in air clathrate hydrates

    SciTech Connect

    Chazallon, Bertrand; Klapproth, Alice; Kuhs, Werner F.

    1999-06-15

    We present the results of MD-simulation runs with subsequent quenches for clathrate hydrates using SPC water in order to model properly the crystallographic site disorder of the guest molecules in the water cages. A procedure is described to transform the results of the quench (symmetry P1) into the proper space-time averaged space group (Fd3-bar m) of the clathrate hydrate. The resulting disorder models are compared with the outcome of crystallographic structure refinements (R-factors, Fourier maps) from our neutron powder diffraction data. A correct description of the disorder is important for a reliable determination of the pressure-dependent cage filling.

  7. The chemical reactivity and structure of collagen studied by neutron diffraction

    SciTech Connect

    Wess, T.J.; Wess, L.; Miller, A.

    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.

  8. Existence of ferroelectric ice on planets—A neutron diffraction study

    NASA Astrophysics Data System (ADS)

    Fukazawa, Hiroshi; Hoshikawa, Akinori; Chakoumakos, Bryan C.; Fernandez-Baca, Jaime A.

    2009-02-01

    From neutron powder-diffraction experiments, we have studied the growth process of ferroelectric ice XI (eleven) with deuteron-ordered arrangements. We measured time-resolved neutron diffraction of 0.001-M KOD-doped D2O ice. We observed the growth of ice XI at 72-74 K. The mass fraction f (the ratio of mass of ice XI to that of the doped ice) linearly increased with time for about 2 days. The de-transformed ice Ih, obtained after warming above the transition temperature of 76 K, retransformed to ice XI at 66 K. The observed increase of f with time is in good agreement with the nucleation process of the ordering and the constant growth of the ordered domain. A large fraction of ice Ih sample doped with sodium hydroxide changed to ice XI at 68 K. The results suggest that large quantities of ice on cold icy bodies in our solar system are able to transform to ice XI, which may be detectable by space telescope and planetary exploration.

  9. Unraveling cyclic deformation mechanisms of a rolled magnesium alloy using in situ neutron diffraction

    SciTech Connect

    Wu, Wei; An, Ke; Liaw, Peter K.

    2014-12-23

    In the current study, the deformation mechanisms of a rolled magnesium alloy were investigated under cyclic loading using real-time in situ neutron diffraction under a continuous-loading condition. The relationship between the macroscopic cyclic deformation behavior and the microscopic response at the grain level was established. The neutron diffraction results indicate that more and more grains are involved in the twinning and detwinning deformation process with the increase of fatigue cycles. The residual twins appear in the early fatigue life, which is responsible for the cyclic hardening behavior. The asymmetric shape of the hysteresis loop is attributed to the early exhaustion of the detwinning process during compression, which leads to the activation of dislocation slips and rapid strain-hardening. The critical resolved shear stress for the activation of tensile twinning closely depends on the residual strain developed during cyclic loading. In the cycle before the sample fractured, the dislocation slips became active in tension, although the sample was not fully twinned. The increased dislocation density leads to the rise of the stress concentration at weak spots, which is believed to be the main reason for the fatigue failure. Furthermore, the deformation history greatly influences the deformation mechanisms of hexagonal-close-packed-structured magnesium alloy during cyclic loading.

  10. Cage occupancies in the high pressure structure H methane hydrate: A neutron diffraction study

    SciTech Connect

    Tulk, Christopher A; Klug, Dennis D; Moreira Dos Santos, Antonio F; Karotsis, Georgios; Guthrie, Malcolm; Molaison, Jamie J; Pradhan, Neelam

    2012-01-01

    A neutron diffraction study was performed on the CD{sub 4}: D{sub 2}O structure H clathrate hydrate to refine its CD{sub 4} fractional cage occupancies. Samples of ice VII and hexagonal (sH) methane hydrate were produced in a Paris-Edinburgh press and in situ neutron diffraction data collected. The data were analyzed with the Rietveld method and yielded average cage occupancies of 3.1 CD{sub 4} molecules in the large 20-hedron (5{sup 12}6{sup 8}) cages of the hydrate unit cell. Each of the pentagonal dodecahedron (5{sup 12}) and 12-hedron (4{sup 3}5{sup 6}6{sup 3}) cages in the sH unit cell are occupied with on average 0.89 and 0.90 CD{sub 4} molecules, respectively. This experiment avoided the co-formation of Ice VI and sH hydrate, this mixture is more difficult to analyze due to the proclivity of ice VI to form highly textured crystals, and overlapping Bragg peaks of the two phases. These results provide essential information for the refinement of intermolecular potential parameters for the water methane hydrophobic interaction in clathrate hydrates and related dense structures.

  11. Pressure dependence of the magnetic order in CrAs: a neutron diffraction investigation

    DOE PAGESBeta

    Keller, L.; White, J. S.; Babkevich, P.; Susner, Michael A.; Sims, Zachary C; Safa-Sefat, Athena; Ronnow, H. M.; Ruegg, Ch.

    2015-01-29

    The suppression of magnetic order with pressure concomitant with the appearance of pressure-induced superconductivity was recently discovered in CrAs. Here we present a neutron diffraction study of the pressure evolution of the helimagnetic ground-state towards and in the vicinity of the superconducting phase. Neutron diffraction on polycrystalline CrAs was employed from zero pressure to 0.65 GPa and at various temperatures. The helimagnetic long-range order is sustained under pressure and the magnetic propagation vector does not show any considerable change. The average ordered magnetic moment is reduced from 1.73(2) μB at ambient pressure to 0.4(1) μB close to the critical pressuremore » Pc ≈ 0.7 GPa, at which magnetic order is completely suppressed. The width of the magnetic Bragg peaks strongly depends on temperature and pressure, showing a maximum in the region of the onset of superconductivity. In conclusion, we interpret this as associated with competing ground-states in the vicinity of the superconducting phase.« less

  12. In situ synthesis and characterization of uranium carbide using high temperature neutron diffraction

    NASA Astrophysics Data System (ADS)

    Reiche, H. Matthias; Vogel, Sven C.; Tang, Ming

    2016-04-01

    We investigated the formation of UCx from UO2+x and graphite in situ using neutron diffraction at high temperatures with particular focus on resolving the conflicting reports on the crystal structure of non-quenchable cubic UC2. The agents were UO2 nanopowder, which closely imitates nano grains observed in spent reactor fuels, and graphite powder. In situ neutron diffraction revealed the onset of the UO2 + 2C → UC + CO2 reaction at 1440 °C, with its completion at 1500 °C. Upon further heating, carbon diffuses into the uranium carbide forming C2 groups at the octahedral sites. This resulting high temperature cubic UC2 phase is similar to the NaCl-type structure as proposed by Bowman et al. Our novel experimental data provide insights into the mechanism and kinetics of formation of UC as well as characteristics of the high temperature cubic UC2 phase which agree with proposed rotational rehybridization found from simulations by Wen et al.

  13. The hydration structure of a Z-DNA hexameric duplex determined by a neutron diffraction technique.

    PubMed

    Chatake, Toshiyuki; Tanaka, Ichiro; Umino, Hisao; Arai, Shigeki; Niimura, Nobuo

    2005-08-01

    In order to reveal the hydration structure of Z-DNA, a neutron diffraction study has been carried out at 1.8 A resolution on a Z-DNA hexamer d(CGCGCG). Neutron diffraction data were collected with the BIX-3 single-crystal diffractometer at the JRR-3 reactor in the Japan Atomic Energy Research Institute (JAERI) using a large crystal (1.6 mm3) obtained from D2O solution. It has been found that almost all the guanine bases have participated in H/D exchange at the C8-H8 group, consistent with the acidic nature of this bond. 44 water molecules were found in the nuclear density maps, of which 29 showed the entire contour of all three atoms (D-O-D). The remaining 15 water molecules had a simple spherical shape, indicating that they were rotationally disordered. An interesting relationship was found between the orientational disorder of the water molecules and their locations. Almost all water molecules in the minor groove were well ordered in the crystal, while 40% of the water molecules in the major groove were rotationally disordered. The hydrogen-bonding networks in the hydration shells have two structural aspects: flexibility and regularity. PMID:16041074

  14. Magnetic Structure of Goethite α-FeOOH: A Neutron Diffraction Study

    NASA Astrophysics Data System (ADS)

    Zepeda-Alarcon, E.; Nakotte, H.; Vogel, S. C.; Wenk, H.

    2013-12-01

    Goethite (α-FeOOH) is found in diverse natural ecosystems, it is by far the most common oxyhydroxide in terrestrial soils, sediments and clays and an important mineral in the biogeochemical cycle of iron at the Earth's surface. Neutron diffraction studies have found that the iron magnetic moments are collinear in a two sublattice antiferromagnetic structure, aligned parallel to the c axis in space group Pbnm (Forsyth et. al. 1968). However, goethite shows superparamagnetic behavior and also a weak ferromagnetic component that has been attributed to the presence of lattice distortions. It is thought that these changes in magnetic ordering could be due to a 13° canting of the magnetic moment with respect to the c-axis, which enables the flipping of the spins due to small perturbations in the lattice (Coey et. al. 1995). In this study we used neutron diffraction at HIPPO and NPDF beamlines at LANSCE of Los Alamos National Laboratory on a powder of natural goethite provided by A. Gualtieri. The nuclear and magnetic structures were determined by means of a Rietveld refinement with GSAS and it was found that the spins of the iron atoms are aligned parallel to the c-axis, with no evidence of spin canting. The net magnetic moment is lower than what has previously been found. These results provide further insight into the magnetic ordering of this mineral and can be important in understanding the physical processes responsible for goethite's intriguing magnetic behavior.

  15. Unraveling cyclic deformation mechanisms of a rolled magnesium alloy using in situ neutron diffraction

    DOE PAGESBeta

    Wu, Wei; An, Ke; Liaw, Peter K.

    2014-12-23

    In the current study, the deformation mechanisms of a rolled magnesium alloy were investigated under cyclic loading using real-time in situ neutron diffraction under a continuous-loading condition. The relationship between the macroscopic cyclic deformation behavior and the microscopic response at the grain level was established. The neutron diffraction results indicate that more and more grains are involved in the twinning and detwinning deformation process with the increase of fatigue cycles. The residual twins appear in the early fatigue life, which is responsible for the cyclic hardening behavior. The asymmetric shape of the hysteresis loop is attributed to the early exhaustionmore » of the detwinning process during compression, which leads to the activation of dislocation slips and rapid strain-hardening. The critical resolved shear stress for the activation of tensile twinning closely depends on the residual strain developed during cyclic loading. In the cycle before the sample fractured, the dislocation slips became active in tension, although the sample was not fully twinned. The increased dislocation density leads to the rise of the stress concentration at weak spots, which is believed to be the main reason for the fatigue failure. Furthermore, the deformation history greatly influences the deformation mechanisms of hexagonal-close-packed-structured magnesium alloy during cyclic loading.« less

  16. Pressure dependence of the magnetic order in CrAs: a neutron diffraction investigation

    SciTech Connect

    Keller, L.; White, J. S.; Babkevich, P.; Susner, Michael A.; Sims, Zachary C; Safa-Sefat, Athena; Ronnow, H. M.; Ruegg, Ch.

    2015-01-29

    The suppression of magnetic order with pressure concomitant with the appearance of pressure-induced superconductivity was recently discovered in CrAs. Here we present a neutron diffraction study of the pressure evolution of the helimagnetic ground-state towards and in the vicinity of the superconducting phase. Neutron diffraction on polycrystalline CrAs was employed from zero pressure to 0.65 GPa and at various temperatures. The helimagnetic long-range order is sustained under pressure and the magnetic propagation vector does not show any considerable change. The average ordered magnetic moment is reduced from 1.73(2) μB at ambient pressure to 0.4(1) μB close to the critical pressure Pc ≈ 0.7 GPa, at which magnetic order is completely suppressed. The width of the magnetic Bragg peaks strongly depends on temperature and pressure, showing a maximum in the region of the onset of superconductivity. In conclusion, we interpret this as associated with competing ground-states in the vicinity of the superconducting phase.

  17. Neutron diffraction study of water freezing on aircraft engine combustor soot.

    PubMed

    Tishkova, V; Demirdjian, B; Ferry, D; Johnson, M

    2011-12-14

    The study of the formation of condensation trails and cirrus clouds on aircraft emitted soot particles is important because of its possible effects on climate. In the present work we studied the freezing of water on aircraft engine combustor (AEC) soot particles under conditions of pressure and temperature similar to the upper troposphere. The microstructure of the AEC soot was found to be heterogeneous containing both primary particles of soot and metallic impurities (Fe, Cu, and Al). We also observed various surface functional groups such as oxygen-containing groups, including sulfate ions, that can act as active sites for water adsorption. Here we studied the formation of ice on the AEC soot particles by using neutron diffraction. We found that for low amount of adsorbed water, cooling even up to 215 K did not lead to the formation of hexagonal ice. Whereas, larger amount of adsorbed water led to the coexistence of liquid water (or amorphous ice) and hexagonal ice (I(h)); 60% of the adsorbed water was in the form of ice I(h) at 255 K. Annealing of the system led to the improvement of the crystal quality of hexagonal ice crystals as demonstrated from neutron diffraction. PMID:21996755

  18. Malayaite ceramic pigments: A combined optical spectroscopy and neutron/X-ray diffraction study

    SciTech Connect

    Cruciani, Giuseppe; Dondi, Michele; Ardit, Matteo; Lyubenova, Teodora Stoyanova; Carda, Juan B.; Matteucci, Francesco; Costa, Anna L.

    2009-08-05

    Ceramic pigments based on the Cr-doped malayaite structure were synthesized by solid state reaction and characterized by optical spectroscopy and combined X-ray and neutron powder diffraction in order to elucidate the still unclear chromium substitution mechanisms. The results show that coloration is actually due to simultaneous occurrence of Cr{sup 4+} and Cr{sup 3+} ions in the crystal lattice. Spectroscopy data confirm that Cr{sup 4+} is replacing Sn{sup 4+} in the octahedral site and, in minor amount, Si{sup 4+} in the tetrahedral site. In addition, neutron powder diffraction data suggest that Cr{sup 3+} substitution for octahedral Sn{sup 4+} is charge balanced by the formation of oxygen vacancies with no preference over the different oxygen sites. Upon incorporation of Cr ion, the SnO{sub 6} octahedra exhibit an off-centre displacement of central cation which in turn induces a rearrangement of both the octahedral and tetrahedral coordination shells.

  19. Preparation and neutron diffraction study of polycrystalline Cu-Zn-Fe materials

    NASA Astrophysics Data System (ADS)

    Darul, J.; Nowicki, W.

    2009-10-01

    Polycrystalline oxides Cu1-xZnxFe2O4 (0.0≤x≤0.05) have been successfully prepared by a simple combustion method using citrate-nitrate precursors. The nature of structural transition in inverse spinels and ferrimagnetic behavior of the materials have been investigated by the neutron diffraction technique. At room temperature neutron diffraction study confirms the presence of a single-phase structure, where tetragonal unit cell with c/a>1 is observed. In these distorted spinel ferrites it is found that tetragonal → cubic transformation is attributed to the decrease of the concentration of Jahn-Teller ions Cu2+ (d9) in the host structure at the octahedral sites as a result of zinc substitution. The introduction of non-magnetic ion in place of Cu2+ in the spinel unit cell results in the reduction of intersublattice contributions, this in turn decreases temperature of the magnetic ordering (Curie point) in these diluted ferrimagnets.

  20. Dynamical Theory of Neutron Diffraction for Perfect Crystals with and Without Strain Gradients

    NASA Astrophysics Data System (ADS)

    Maheswaran, Saravanamuthu

    The dynamical theory of neutron diffraction is studied for perfect crystals and crystals with strain gradients. In the case of parallel-sided slab crystals, it is customary to distinguish the Bragg case where the beam enters and exits on the same side of the slab and the Laue case where the beam enters on one side and exits on the other. The symmetric Bragg case has the angle of incidence equal to the angle of diffraction with respect to the surface, that is the scattering vector is perpendicular to the surface. In the symmetric Laue case the scattering vector is parallel to the surface. In extreme cases either the incoming or exiting beam is close to being parallel to the surface. Schrodinger's equation for the perfect slab crystal with a periodic potential is solved by two methods which can give similar results. In the first method, which is known as the eikonal approach, a quartic dispersion relation is obtained and solved for all possible internal wave vectors. A given incident plane wave generates four pairs of internal waves. Each pair is coupled together by the periodic potential. Four waves, in addition to the incident wave, appear outside the crystal as a result of the interaction with the crystal slab. All the unknown internal and external amplitudes are found from the boundary conditions. In non-extreme cases, two pairs of internal waves suffice to describe the propagation of neutrons in the crystal. In the second approach, commonly referred to as the Takagi-Taupin method, one assumes that the wave amplitudes are position dependent solutions of coupled differential equations. We have measured the dependence of the diffracted beam intensity as a function of thickness of Si wafers and found good agreement with the theory. The theory has applications in the design of elements for neutron optics, particularly monochromating and analyzing crystals. In the extreme cases, all four pairs of internal waves are considered. It is shown that three pairs are

  1. Probing the Hydrogen Sublattice of FeHx with High-Pressure Neutron Diffraction

    NASA Astrophysics Data System (ADS)

    Murphy, C. A.; Guthrie, M.; Boehler, R.; Somayazulu, M.; Fei, Y.; Molaison, J.; dos Santos, A. M.

    2013-12-01

    The combination of seismic, cosmochemical, and mineral physics observations have revealed that Earth's iron-rich core must contain some light elements, such as hydrogen, carbon, oxygen, silicon, and/or sulfur. Therefore, understanding the influence of these light elements on the structural, thermoelastic, and electronic properties of iron is important for constraining the composition of this remote layer of the Earth and, in turn, providing constraints on planetary differentiation and core formation models. The high-pressure structural and magnetic properties of iron hydride (FeHx) have previously been studied using synchrotron x-ray diffraction and Mössbauer spectroscopy. Such experiments revealed that the double hexagonal close-packed (dhcp) structure of FeHx is stable above a pressure of ~5 GPa and up to at least 80 GPa at 300 K [1]. In addition, dhcp-FeHx is ferromagnetic at low-pressures, but undergoes a magnetic collapse around 22 GPa [2]. X-ray experiments provide valuable insight into the properties of FeHx, but such techniques are largely sensitive to the iron component because it is difficult to detect the hydrogen sublattice with x-rays. Therefore, neutron diffraction has been used to investigate metastable FeHx, which is formed by quenching the high-pressure phase to liquid nitrogen temperatures and probing the sample at ambient pressure [3]. However, such neutron experiments have been limited to formation pressures below 10 GPa, and cannot be performed at ambient temperature. Here we present the first in-situ investigation of FeHx at 300 K using high-pressure neutron diffraction experiments performed at the Spallation Neutrons and Pressure Diffractometer (SNAP) instrument at the Spallation Neutron Source, Oak Ridge National Laboratory. In order to achieve pressures of ~50 GPa, we loaded iron samples with a hydrogen gas pressure medium into newly designed large-volume panoramic diamond-anvil cells (DACs) for neutron diffraction experiments [4; 5]. We

  2. Texture and anisotropy analysis of a laminated lower crust: a neutron diffraction study of felsic granulites

    NASA Astrophysics Data System (ADS)

    Benitez Perez, J.; Gomez Barreiro, J.; Martinez-Catalan, J. R.; Castiñeiras Garcia, P.; Vogel, S. C.; Wenk, H.; Alvarez Valero, A.

    2013-12-01

    Quantitative fabric analyses of high-P and high-T tectonites were done with HIPPO, a Time-Of-Flight (TOF) neutron diffractometer at Los Alamos National Lab. Samples were collected in the Sobrado unit (NW Spain), a tectonic stack of highly deformed slices of metabasites, paragneisses and ultramafic rocks. Metamorphism ranges from granulites on top, to eclogites at the bottom of the unit. The ensemble represents and excellent example of laminated lower crust. The alternation of mechanically contrasted lithologies and/or the development of crystal preferred orientation might result into anisotropy. We explore the contribution of crystallographic preferred orientation or texture to the seismic anisotropy of the lower crust. Since strain partitioning occurred between mechanically strong and weak lithologies, a higher crystal preferred orientation is expected along the weak levels: the metasediments. TOF neutron diffraction experiments were conducted in HIPPO (LANSCE) with high-P and high-T mylonitic felsic paragneisses. Quantitative texture analysis of neutron data was accomplished by using the Rietveld method, with E-WIMW algorithm, implemented in the program package MAUD (Material Analysis Using Diffraction; Lutterotti, 1999). The orientation distribution function (ODF) for each mineral was calculated in MAUD and then processed in BEARTEX (Wenk et al. 1998). Selected pole figures were plotted for major components, quartz, plagioclase and biotite (first setting in monoclinic crystals). Texture patterns are compatible with non-coaxial progressive deformation and discussed accordingly in terms of dislocation activity. Besides, seismic waves velocities were computed from the texture data in BEARTEX. Calculated velocities and anisotropy were based on ODF, volume fraction of each mineral and their single-crystal elastic constant. Kinematic and mechanical implications are discussed in terms of the regional geology. The correlation of texture, mineral composition and seismic

  3. A revised structure and hydrogen bonding system in cellulose II from a neutron fiber diffraction analysis

    SciTech Connect

    Langan, P.; Nishiyama, Y.; Chanzy, H.

    1999-11-03

    The crystal and molecular structure and hydrogen bonding system in cellulose II have been revised using new neutron diffraction data extending to 1.2 {angstrom} resolution collected from two highly crystalline fiber samples of mercerized flax. Mercerization was achieved in NaOH/H{sub 2}O for one sample and in NaOD/D{sub 2}O for the other, corresponding to the labile hydroxymethyl moieties being hydrogenated and deuterated, respectively. Fourier difference maps were calculated in which neutron difference amplitudes were combined with phases calculated from two revised X-ray models of cellulose II. The revised phasing models were determined by refinement against the X-ray data set of Kolpak and Blackwell, using the LALS methodology. Both models have two antiparallel chains organized in a P2{sub 1} space group and unit cell parameters: a = 8.01 {angstrom}, b = 9.04 {angstrom}, c = 10.36 {angstrom}, and {gamma} = 117.1{degree}. One has equivalent backbone conformations for both chains but different conformations for the hydroxymethyl moieties: gt for the origin chain and tg for the center chain. The second model based on the recent crystal structures of cellotetraose, has different conformations for the two chains but nearly equivalent conformations for the hydroxymethyl moieties. On the basis of the X-ray data alone, the models could not be differentiated. From the neutron Fourier difference maps, possible labile hydrogen atom positions were identified for each model and refined using LALS. The second model is significantly different from previous proposals based on the crystal structures of cellotetraose, MD simulations of cellulose II, and any potential hydrogen-bonding network in the structure of cellulose II determined in earlier X-ray fiber diffraction studies. The exact localization of the labile hydrogen atoms involved in this bonding, together with their donor and acceptor characteristics, is presented and discussed. This study provides, for the first time

  4. Neutron diffraction studies of a four-coordinated hydride in near square-planar geometry.

    PubMed

    Liao, Jian-Hong; Dhayal, Rajendra Singh; Wang, Xiaoping; Kahlal, Samia; Saillard, Jean-Yves; Liu, C W

    2014-10-20

    The structure of a nanospheric polyhydrido copper cluster, [Cu20(H)11{S2P(O(i)Pr)2}9], was determined by single-crystal neutron diffraction. The Cu20 cluster consists of an elongated triangular orthobicupola constructed from 18 Cu atoms that encapsulate a [Cu2H5](3-) ion with an exceptionally short Cu-Cu distance. The 11 hydrides in the cluster display three different coordination modes to the Cu atoms: six μ3-hydrides in a pyramidal geometry, two μ4-hydrides in a tetrahedral cavity, and three μ4-hydrides in an unprecedented near square-planar geometry. The neutron data set was collected for 7 days on a small crystal with dimensions of 0.20 mm × 0.50 mm × 0.65 mm using the Spallation Neutron Source TOPAZ single-crystal time-of-flight Laue diffractometer at Oak Ridge National Laboratory. The final R-factor was 8.63% for 16,014 reflections. PMID:25290745

  5. Neutron diffraction studies of a four-coordinated hydride in near square-planar geometry

    DOE PAGESBeta

    Liao, Jian -Hong; Dhayal, Rajendra Singh; Wang, Xiaoping; Kahlal, Samia; Saillard, Jean -Yves; Liu, C. W.

    2014-10-07

    The structure of a nanospheric polyhydrido copper cluster, [Cu20(H)11{S2P(OiPr)2}9], was determined by single-crystal neutron diffraction. Cu20 cluster consists of an elongated triangular orthobicupola constructed from 18 Cu atoms that encapsulate a [Cu2H5}3- ion in the center with an exceptionally short Cu-Cu distance. The eleven hydrides in the cluster display three different coordination modes to the Cu atoms: Six μ3-hydrides in pyramidal geometry, two μ4-hydrides in tetrahedral cavity, and three μ4-hydrides in an unprecedented near square-planar geometry. The neutron data set was collected on a small crystal of the size 0.20 mm x 0.50 mm x 0.65 mm for seven daysmore » using the Spallation Neutron Source TOPAZ single-crystal time-of-flight Laue diffractometer at the Oak Ridge National Laboratory. Furthermore, the final R-factor is 8.64% for 16014 reflections.« less

  6. Neutron diffraction studies of a four-coordinated hydride in near square-planar geometry

    SciTech Connect

    Liao, Jian -Hong; Dhayal, Rajendra Singh; Wang, Xiaoping; Kahlal, Samia; Saillard, Jean -Yves; Liu, C. W.

    2014-10-07

    The structure of a nanospheric polyhydrido copper cluster, [Cu20(H)11{S2P(OiPr)2}9], was determined by single-crystal neutron diffraction. Cu20 cluster consists of an elongated triangular orthobicupola constructed from 18 Cu atoms that encapsulate a [Cu2H5}3- ion in the center with an exceptionally short Cu-Cu distance. The eleven hydrides in the cluster display three different coordination modes to the Cu atoms: Six μ3-hydrides in pyramidal geometry, two μ4-hydrides in tetrahedral cavity, and three μ4-hydrides in an unprecedented near square-planar geometry. The neutron data set was collected on a small crystal of the size 0.20 mm x 0.50 mm x 0.65 mm for seven days using the Spallation Neutron Source TOPAZ single-crystal time-of-flight Laue diffractometer at the Oak Ridge National Laboratory. Furthermore, the final R-factor is 8.64% for 16014 reflections.

  7. A Rietveld refinement method for angular- and wavelength-dispersive neutron time-of-flight powder diffraction data

    PubMed Central

    Jacobs, Philipp; Houben, Andreas; Schweika, Werner; Tchougréeff, Andrei L.; Dronskowski, Richard

    2015-01-01

    This paper introduces a two-dimensional extension of the well established Rietveld refinement method for modeling neutron time-of-flight powder diffraction data. The novel approach takes into account the variation of two parameters, diffraction angle 2θ and wavelength λ, to optimally adapt to the varying resolution function in diffraction experiments. By doing so, the refinement against angular- and wavelength-dispersive data gets rid of common data-reduction steps and also avoids the loss of high-resolution information typically introduced by integration. In a case study using a numerically simulated diffraction pattern of Rh0.81Fe3.19N taking into account the layout of the future POWTEX instrument, the profile function as parameterized in 2θ and λ is extracted. As a proof-of-concept, the resulting instrument parameterization is then utilized to perform a typical refinement of the angular- and wavelength-dispersive diffraction pattern of CuNCN, yielding excellent residuals within feasible computational efforts. Another proof-of-concept is carried out by applying the same approach to a real neutron diffraction data set of CuNCN obtained from the POWGEN instrument at the Spallation Neutron Source in Oak Ridge. The paper highlights the general importance of the novel approach for data analysis at neutron time-of-flight diffractometers and its possible inclusion within existing Rietveld software packages. PMID:26664340

  8. Neutron powder-diffraction studies of lithium, sodium, and potassium metal

    SciTech Connect

    Berliner, R.; Fajen, O. ); Smith, H.G. ); Hitterman, R.L. )

    1989-12-15

    Neutron powder-diffraction measurements have been performed on polycrystalline lithium and sodium specimens at 80 and 20 K and on potassium metal at 80 and 10 K. Lithium is bcc (body-centered cubic) at room temperature and undergoes a martensitic structural phase transformation to a 9{ital R} (samarium-type) form at low temperature. This experiment presents evidence that the 9{ital R} phase is present in sodium as well as lithium. No evidence of a transformation was observed in potassium at 10 K. The diffraction lines for both lithium and sodium after the phase transformation exhibit position shifts and broadening characteristic of stacking-fault defects. The line shifts, line broadening, and transformed fraction for the low-temperature phase of lithium and sodium metal are reported. The diffraction peak position shifts are, however, different from those predicted for deformation-type stacking faults alone. Qualitative agreement of the experimental results with stacking-fault-model calculations was obtained for a double-twin'' type of layer defect.

  9. Measuring strain and stress distributions along rebar embedded in concrete using time-of-flight neutron diffraction

    NASA Astrophysics Data System (ADS)

    Suzuki, H.; Kusunoki, K.; Hatanaka, Y.; Mukai, T.; Tasai, A.; Kanematsu, M.; Kabayama, K.; Harjo, S.

    2014-02-01

    In modern society, architectural and civil engineering structures such as reinforced concrete buildings require high seismic performance to minimize the ‘megarisk’ exposed from urban earthquake hazards. In the reinforced concrete structures, the bond resistance between rebar and concrete is one important parameter for discussing its performance and it has been typically evaluated by measuring the strain distribution along the embedded rebar. Here, we present in-situ strain and stress measurements for the rebar in reinforced concrete using time-of-flight neutron diffraction as a novel alternative technique to typical strain gauges. It was demonstrated in this study that the three-dimensional deformation behavior of the embedded rebar in normal-strength concrete, cured in air, can be accurately measured under pull-out loading using time-of-flight neutron diffraction. Wider applications of neutron diffraction in the structural engineering field are expected for advanced understanding of actual phenomena on reinforced concrete structures.

  10. Neutron diffraction studies of molecular liquids using the new detector system of the PSD diffractometer at the Budapest Research Reactor

    NASA Astrophysics Data System (ADS)

    Temleitner, László; Mészáros, György; Pusztai, László; Sváb, Erzsébet

    2004-07-01

    Neutron diffraction experiments on several molecular liquids have been performed using the PSD neutron diffractometer (Budapest Research Reactor) which has recently been equipped with a new detector system. Raw data are presented for liquid carbon-tetrachloride which served as a `calibration standard' for molecular liquids. Detailed comparison with data taken on the previous detector system, for several stages of the correction/evaluation process, validates results obtained by using the new detectors.

  11. Thermal neutron diffraction determination of the magnetic structure of EuCu{sub 2}Ge{sub 2}

    SciTech Connect

    Rowan-Weetaluktuk, W. N.; Ryan, D. H.; Lemoine, P.; Cadogan, J. M.

    2014-05-07

    The magnetic structure of EuCu{sub 2}Ge{sub 2} has been determined by flat-plate neutron powder diffraction. Two magnetic phases are present in the neutron diffraction pattern at 3.5 K. They have the same moment, within error, and a common transition temperature. Both {sup 151}Eu and {sup 153}Eu Mössbauer spectroscopy show that the two magnetic phases belong to the same crystallographic phase. Both phases can be modelled by planar helimagnetic structures: one with a propagation vector of [0.654(1), 0, 0], the other with a propagation vector of [0.410(1), 0.225(1), 0].

  12. Analysis of the Tensile Behavior of 12 pct Mn Multi-phase ( α + γ) TWIP + TRIP Steel by Neutron Diffraction

    NASA Astrophysics Data System (ADS)

    Lee, Sangwon; Woo, Wanchuck; de Cooman, Bruno C.

    2016-05-01

    The tensile behavior of intercritically annealed Fe-12 pctMn-0.3 pctC-2 pctAl and Fe-12 pctMn-0.3 pctC-3 pctAl steel was studied by means of in situ neutron diffraction and microstructural analysis. The in situ neutron diffraction measurements showed that the ferrite had a much higher yield strength and lower work hardening rate as compared to the austenite. The strain hardening of the austenite was controlled by deformation twinning and strain-induced transformation, occurring in succession. This TWIP + TRIP effect acted as an effective plasticity-enhancing mechanism which increased the work hardening rate.

  13. Degradation analysis of 18650-type lithium-ion cells by operando neutron diffraction

    NASA Astrophysics Data System (ADS)

    Shiotani, Shinya; Naka, Takahiro; Morishima, Makoto; Yonemura, Masao; Kamiyama, Takashi; Ishikawa, Yoshihisa; Ukyo, Yoshio; Uchimoto, Yoshiharu; Ogumi, Zempachi

    2016-09-01

    In-situ and operando neutron diffraction are used to analyze the degradation of 18650-type Li-ion cells. Structural characterization of the electrode materials is performed by applying the Rietveld refinement technique to the in-situ data. The structural refinement of both electrodes in the degraded cells indicates that the amount of active Li-ions is reduced by 14.4% and 13.7% in the cathode and anode, respectively. This reduction is good in agreement with the capacity loss determined electrochemically. The results suggest that capacity loss might be mainly caused by loss of active Li-ions due to side reactions such as solid electrolyte interface (SEI) growth. Furthermore, operando measurements are performed to examine the deterioration of the electrode and active materials. Because the structural evolution depending on capacity is increased in the cathode of degraded cells, it is presumed that the cathode active material has deteriorated due to phase transitions.

  14. Tensile behavior of TRIP-aided multi-phase steels studied by in situ neutron diffraction

    SciTech Connect

    Tomota, Y. . E-mail: tomota@mx.ibaraki.ac.jp; Tokuda, H.; Adachi, Y.; Wakita, M.; Minakawa, N.; Moriai, A.; Morii, Y.

    2004-12-01

    TRIP-aided multi-phase steels were made by thermo-mechanically controlled process, where the ferrite grain size and the amount of the retained austenite were changed by controlling process conditions. The tensile behavior of four steels was studied by in situ neutron diffraction. It is found that the retained austenite bearing about 1.0 wt% C is plastically harder than the ferrite matrix. The steel with a ferrite grain size of {approx}2.0 {mu}m showed tensile strength of 1.1 GPa and a uniform elongation of 18.4%, in which stress-induced martensitic transformation occurs during plastic deformation but a considerable amount of austenite remains even after the onset of necking. It is concluded that the enhancement of uniform elongation is caused mainly by the work-hardening due to the hard austenite and martensite, where the contribution of the transformation strain is negligible.

  15. Experimental determination of residual stress by neutron diffraction in a boiling water reactor core shroud

    SciTech Connect

    Payzant, A.; Spooner, S.; Zhu, Xiaojing; Hubbard, C.R.

    1996-06-01

    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.

  16. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    NASA Astrophysics Data System (ADS)

    Cui, J.; Choi, J. P.; Li, G.; Polikarpov, E.; Darsell, J.; Kramer, M. J.; Zarkevich, N. A.; Wang, L. L.; Johnson, D. D.; Marinescu, M.; Huang, Q. Z.; Wu, H.; Vuong, N. V.; Liu, J. P.

    2014-05-01

    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 μB at 50 K and 300 K, respectively.

  17. Experimental setup for simultaneous measurements of neutron diffraction and dielectric spectroscopy during crystallization of liquids

    NASA Astrophysics Data System (ADS)

    Jiménez-Ruiz, M.; Sanz, A.; Nogales, A.; Ezquerra, T. A.

    2005-04-01

    Here we present an experimental setup to obtain information on structural and dynamical changes in liquids during crystallization. This setup consists in a sample cell that allows performing simultaneous measurements of neutron diffraction and dielectric spectroscopy experiments. The capabilities of the technique have been probed by following in real time the crystallization process of a model liquid: the isopropanol. By performing the simultaneous experiment information can be obtained from both phases, amorphous and crystalline, and therefore it can provide a complete description of the changes occurring during a crystallization process. The use of this setup allowed us to demonstrate that a breakage of the hydrogen-bond network is a precursor step for the crystallization of isopropanol.

  18. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    SciTech Connect

    Cui, J. Choi, J. P.; Li, G.; Polikarpov, E.; Darsell, J.; Kramer, M. J.; Zarkevich, N. A.; Wang, L. L.; Johnson, D. D.; Marinescu, M.; Huang, Q. Z.; Wu, H.; Vuong, N. V.; Liu, J. P.

    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.

  19. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    SciTech Connect

    Cui, J.; Choi, J. P.; Li, G.; Polikarpov, E.; Darsell, J.; Kramer, M. J.; Zarkevich, N. A.; Wang, L. L.; Johnson, D. D.; Marinescu, M.; Huang, Q. Z.; Wu, H.; Vuong, N. V.; Liu, J. P.

    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 μB at 50 K and 300 K, respectively.

  20. Applications of pulsed neutron powder diffraction to actinide elements. [Pu-Al

    SciTech Connect

    Lawson, A.C.; Richardson, J.W.; Mueller, M.H.; Lander, G.H.; Goldstone, J.A.; Williams, A.; Kwei, G.H.; Von Dreele, R.B.; Faber, J. Jr.; Hitterman, R.L.

    1987-11-01

    We have been using the technique of pulsed neutron powder diffraction to study several problems in the physics and chemistry of the actinide elements. In these elements one often encounters very complex structures resulting from polymorphic transformations presumably induced by the presence of 5f-electrons. For example, at least five distinct structures of plutonium metal are found between room temperature and its melting point of 640/sup 0/C, and two of the structures are monoclinc. The determination of the crystal structure of beta-uranium (tetragonal, 30 atoms per unit cell) which has finnaly been shown to be centrosymmetric, after decades of uncertainty is discussed. Some preliminary results on the structure of alpha-plutonium (which confirm Zachariasen's original determination of the monoclinic structure) are presented. Pu-Al alloys were also studied. 12 refs., 18 figs.

  1. A neutron diffraction study of local stress concentrations surrounding defects in pipeline steel

    NASA Astrophysics Data System (ADS)

    Clapham, L.; Sabet-Sharghi, R.; Holden, T.; Atherton, D. L.

    Magnetic flux leakage (MFL) is the most commonly used technique for the in-service inspection of both gas and oil pipelines. However, MFL is sensitive to the stress state of the pipe wall and the area surrounding defects. MFL tools are often calibrated using pipe sections with defects artificially introduced into the pipe wall prior to the pipe being pressurized. Naturally occurring defects, however, occur while the pipe wall is under stress due to line pressure. In this study, neutron diffraction is used to map the strain surrounding the two defects that have been introduced into plates of pipeline grade steel, one into a plate prior to uniaxial loading, the second into a plate held at a constant background load high enough to ensure that stress at the edge of the defect exceeds the elastic limit of the material.

  2. SURFING: A Program for Precise Determination of Sample Position in Stress Measurements Via Neutron Diffraction

    SciTech Connect

    Wang, D.-Q.

    2000-08-08

    Precise determination of the specimen position relative to the sampling volume for texture and stress measurements by neutron diffraction is difficult or sometimes impossible using only optical devices due to large or irregular sample dimensions and/or complicated shape of the sampling volume. The knowledge of the shape and size of the sampling volume allows development of a general mathematical model for the intensity variation with a parallelogram-shape sampling volume moving from outside to inside the specimen for both transmission and reflection geometric set-ups. Both fixed slits and radial collimators are options in defining the geometrical setup. The attenuation by the sample also has been taken into account in this model. Experimental results agree well with the model calculations. The program SURFING is based on the model calculation and was written in Labwindows/CVI{copyright}.

  3. Magnetostructural transition in Fe5SiB2 observed with neutron diffraction

    NASA Astrophysics Data System (ADS)

    Cedervall, Johan; Kontos, Sofia; Hansen, Thomas C.; Balmes, Olivier; Martinez-Casado, Francisco Javier; Matej, Zdenek; Beran, Premysl; Svedlindh, Peter; Gunnarsson, Klas; Sahlberg, Martin

    2016-03-01

    The crystal and magnetic structure of Fe5SiB2 has been studied by a combination of X-ray and neutron diffraction. Also, the magnetocrystalline anisotropy energy constant has been estimated from magnetisation measurements. High quality samples have been prepared using high temperature synthesis and subsequent heat treatment protocols. The crystal structure is tetragonal within the space group I4/mcm and the compound behaves ferromagnetically with a Curie temperature of 760 K. At 172 K a spin reorientation occurs in the compound and the magnetic moments go from aligning along the c-axis (high T) down to the ab-plane (low T). The magnetocrystalline anisotropy energy constant has been estimated to 0.3 MJ/m3 at 300 K.

  4. Neutron diffraction determination of the residual stress redistribution in cracked autofrettaged tubing

    SciTech Connect

    Bourke, M.A. ); McGillivray, H.J.; Webster, G.A. . Dept. of Mechanical Engineering); Webster, P.J. . Dept. of Civil Engineering)

    1991-01-01

    Neutron diffraction has been used to measure the residual stress distributions in uncracked and fatigue cracked rings taken from a high strength, low alloy steel autofrettage tube with a bore diameter of 60mm and a wall thickness of 32mm. Stresses were determined to a precision of {plus minus} 10MPa. Three crack sixes were examines. No appreciable stress redistribution was observed until the crack was grown into a region which originally contained tensile residual hoop stress. When this occurred an increase in residual hoop tension was observed ahead of the crick tip. Qualitative agreement was achieved between the measured hoop stress distribution and values predicted using a boundary element method. 9 refs., 12 figs.

  5. Neutron Diffraction Characterization of Residual Strain in Welded Inconel 718 for NASA Space Shuttle Flow Liners

    SciTech Connect

    Rathod, C.R.; Vaidyanathan, R.; Livescu, V.; Clausen, B.; Bourke, M. A. M.; Notardonato, W.U.; Femminineo, M.

    2004-06-28

    This work quantitatively assesses residual strains and stresses associated with the weld repair process used to repair cracks on NASA's space shuttle flow liners. The coupons used in this investigation were made of the same INCONEL 718 alloy used for the flow liners. They were subjected to identical welding and certification procedures that were carried out on the space shuttle. Neutron diffraction measurements at Los Alamos National Laboratory determined residual strains at selected locations in a welded coupon at 293 K and 135 K. The weld repair process introduced Mises effective residual stresses of up to 555 MPa. On comparing the measurements at 293 K and 135 K, no significant change to the residual strain profile was noted at the low temperature. This indicated minimal mismatch in the coefficients of thermal expansion between the base metal and the weld.

  6. Determination of the residual stress in a centrifuge bowl by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Albertini, G.; Giuliani, A.; Lin Peng, R.; Manescu, A.; Ponzetti, A.

    An experimental study of the stress field in centrifuges for food processing and for agricultural applications was undertaken. The model, the dimensions and the material of the sample are those of the most recent line of production of the Nuova M.A.I.P. company. The rotor is also one of the largest rotors produced by that firm. The residual strains and stresses were determined by using neutron-diffraction techniques before centrifugation and after centrifugation, to evaluate the evolution of stress induced by centrifuging. The upper part of the rotating bowl is investigated, where the highest stress field during centrifugation is theoretically forecast to occur. A data elaboration aiming at avoiding systematic errors leads to the conclusion that no appreciable residual stress is induced by centrifugation.

  7. A study of internal damage of metal matrix composites by neutron diffraction

    SciTech Connect

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

    1994-12-31

    Using neutron diffraction, we have measured the elastic phase strains of Al/TiC and Al/SiC composites under uniaxial tensile loading. The phase strains were used to reconstruct the global elastic strain. It has been found that, above macroscopic yield, the global elastic strain response is not linear. A theoretical model shows that the nonlinearity is dictated by changes in the ratio of longitudinal phase stresses. Furthermore, the changes in this ratio resulting from matrix plasticity and reinforcement fracture are different which leads to distinct slope changes in the global elastic strain response that can be used to distinguish the onset of these two processes on the global elastic strain loading curve.

  8. A neutron diffraction and computer modeling study of the interatomic structure of phosphoric acid

    NASA Astrophysics Data System (ADS)

    Tromp, R. Hans; Spieser, Stephane H.; Neilson, George W.

    1999-01-01

    Wide angle neutron diffraction in combination with H/D substitution was used to determine the inter- and intramolecular structure of 100% phosphoric acid (H3PO4, PA). From radial distribution functions gHH(r), gHX(r), and gXX(r) (where X is either O or P) the hydrogen bonds were found to be characterized by a very short O…H distance (1.54 Å). Within a molecule, the orientation of an OH group was found to be preferably in one of the three O-P-O planes. In the interpretation of the radial distribution functions, use was made of preliminary results of molecular dynamics simulations. Temperature effects on the structure of PA were only found in the hydrogen bond structure, which becomes somewhat less well defined when heating up from room temperature to 60 °C. Polyphosphates could not be detected, probably due to the small degree of polymerization.

  9. Structure of aqueous ammonium calcium nitrate glass former studied by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Ansell, S.; Neilson, G. W.

    1999-09-01

    A neutron diffraction experiment was carried out on the glass-forming aqueous system of ammonium calcium nitrate tetrahydrate, ACN (NH4NO3.Ca(NO3)2.4H2O). The method of isotopic substitution was used to determine the local structure round the NO-3 ion, the hydrogen-hydrogen (gHH(r)), the hydrogen-oxygen (gOH(r)), and the nitrogen-hydrogen (gN2H(r)) radial pair distribution functions, in both the glassy (153 K) and liquid (303 K) states. The results show that significant changes occur on glassification. In particular, the nitrate ion exhibits an increase in the number of close hydrogen contacts and enhancement of its local structure. A microstructural model is proposed to explain the strong glass-forming ability of ACN.

  10. Study of tempering behavior of lath martensite using in situ neutron diffraction

    SciTech Connect

    Shi, Z.M.; Gong, W.; Tomota, Y.; Harjo, S.; Li, J.; Chi, B.; Pu, J.

    2015-09-15

    To elucidate changes in the density and substructure of dislocations during tempering of lath martensite steel, a convolutional multiple whole-profile fitting method was applied to in situ neutron diffraction profiles. With increasing tempering temperature, the dislocation density scarcely changed in the beginning and then decreased at temperatures above 473 K, whereas the dislocation arrangement drastically changed at temperatures above 673 K. The strength of the steel is speculated to depend on the density and arrangement of dislocations. - Highlights: • A convolutional multiple whole-profile fitting method was applied. • Dislocation density and dislocation arrangement changing with tempering were discussed. • Dislocation density scarcely changed in the beginning. • And then dislocation density decreased at temperatures above 473 K. • The dislocation arrangement drastically changed at temperatures above 673 K.

  11. Neutron diffraction measurement of internal strain in the first Japanese ITER CS conductor sample

    NASA Astrophysics Data System (ADS)

    Hemmi, T.; Harjo, S.; Nunoya, Y.; Kajitani, H.; Koizumi, N.; Aizawa, K.; Machiya, S.; Osamura, K.

    2013-08-01

    Several conductor samples were fabricated and tested in the SULTAN facility at CRPP for ITER Central Solenoid (CS) conductor qualification. From the result of the cyclic testing on the first and second conductor samples named CSJA01 and CSJA02, continuous linear degradation of the current sharing temperature (Tcs) was found. From the result of the visual inspection, a large deflection on the lower loading side (LLS) in the high field zone (HFZ) was observed. The bending strain of the strands cannot be evaluated from only the deflection obtained visually. To evaluate the strain of strands in CSJA01 quantitatively, a neutron diffraction measurement of the CSJA01 left leg was performed using the engineering materials diffractometer ‘Takumi’ in J-PARC. From the result, the large bending strain at the LLS in the HFZ was found. Therefore, the Tcs degraded position in the conductor sample due to the cyclic testing can be determined.

  12. Uranium Hydridoborates: Synthesis, Magnetism, and X-ray/Neutron Diffraction Structures.

    PubMed

    Braunschweig, H; Gackstatter, A; Kupfer, T; Radacki, K; Franke, S; Meyer, K; Fucke, K; Lemée-Cailleau, M-H

    2015-08-17

    While uranium hydridoborate complexes containing the [BH4](-) moiety have been well-known in the literature for many years, species with functionalized borate centers remained considerably rare. We were now able to prepare several uranium hydridoborates (1-4) with amino-substituted borate moieties with high selectivity by smooth reaction of [Cp*2UMe2] (Cp* = C5Me5) and [Cp'2UMe2] (Cp' = 1,2,4-tBu3C5H2) with the aminoborane H2BN(SiMe3)2. A combination of nuclear magnetic resonance spectroscopy, deuteration experiments, magnetic SQUID measurements, and X-ray/neutron diffraction studies was used to verify the anticipated molecular structures and oxidation states of 1-4 and helped to establish a linear tridentate coordination mode of the borate anions. PMID:26247295

  13. Neutron-diffraction study of Ho/sub 2/C at 4--296 K

    SciTech Connect

    Atoji, M.

    1981-02-01

    By neutron powder diffraction, trigonal Ho/sub 2/C has been shown to become ferromagnetic below 100 K. The paramagnetic scattering indicates the free Ho/sup 3 +/-ion moment, while the saturation moment in the ferromagnetic phase is 7.16 Bohr magnetons (72% of the free-ion moment), showing a sizeable crystal-field effect. The preferential crystallite orientation induced by the applied magnetic field has shown that the ordered moments are aligned parallel to the (104) axis which corresponds to the (100) axis of the high-temperature cubic modification. The previously proposed HoN-type magnetic ordering is not compatible with our results. The residual, disordered moments exhibit a ferromagnetic short-range order superposing on the ferromagnetic long-range order. Crystallographic-structure data at 296 and 4 K are also presented.

  14. Accelerated carbonation of cement pastes in situ monitored by neutron diffraction

    SciTech Connect

    Castellote, M. Andrade, C.; Turrillas, X.; Campo, J.; Cuello, G.J.

    2008-12-15

    In-situ monitoring of the changes that take place in the phase composition of cement pastes during accelerated carbonation (100% CO{sub 2}) for different binders, has been carried out, by taking Neutron Diffraction patterns in parallel with the carbonation experiments. The variation of the intensity of chosen reflections for each phase along the experiment has been used to monitor concentration changes and has supplied data, in real time, for fractional conversion of different phases (Portlandite, Ettringite and CSH gel) of the hydrated cement pastes. Fitting of these results has allowed to make a qualitative approach to the kinetics of the carbonation of the different phases and extracting conclusions on the microstructural changes that takes place during the carbonation of cement pastes.

  15. In-situ monitoring the realkalisation process by neutron diffraction: Electroosmotic flux and portlandite formation

    SciTech Connect

    Castellote, Marta . E-mail: martaca@ietcc.csic.es; Llorente, Irene; Andrade, Carmen; Turrillas, Xavier; Alonso, Cruz; Campo, Javier

    2006-05-15

    Even though the electroosmotic flux through hardened cementitious materials during laboratory realkalisation trials had been previously noticed, it has never been in-situ monitored, analysing at the same time the establishment of the electroosmotic flux and the microstructure changes in the surroundings of the rebar. In this paper, two series of cement pastes, cast with CEM I and CEM I substituted in a 35% by fly ash, previously carbonated at 100% CO{sub 2}, were submitted to realkalisation treatments followed on line by simultaneous acquisition of neutron diffraction data. As a result, it has been possible to confirm the electroosmosis as the driving force of carbonates towards the rebar and to determine the range of pH in the anolyte in which most of the relevant electroosmotic phenomena takes place. On the other hand, the behaviour of the main crystalline phases involved in the process has been monitored during the treatment, with the precipitation of portlandite as main result.

  16. Complex magnetic ordering in CeFe1.76 studied by neutron diffraction

    SciTech Connect

    Jayasekara, Wageesha T; Tian, W; Hodovanets, Halyna; Canfield, Paul C; Bud'ko, Serguei L; Kreyssig, Andreas; Goldman, Alan I

    2014-10-01

    Neutron diffraction measurements on a single crystal of CeGe1.76 reveal a complex series of magnetic transitions at low temperature. At TN≈7 K, there is a transition from a paramagnetic state at higher temperature to an incommensurate magnetic structure characterized by a magnetic propagation vector (0 0 τ) with τ≈1/4 and the magnetic moment along the a axis of the orthorhombic unit cell. Below TLI≈5 K, the magnetic structure locks in to a commensurate structure with τ=1/4 and the magnetic moment remains along the a axis. Below T≈4 K, we find additional half-integer and integer indexed magnetic Bragg peaks consistent with a second commensurately ordered antiferromagnetic state.

  17. Texture Evolution and Phase Transformation in Titanium Investigated by In-Situ Neutron Diffraction

    SciTech Connect

    Ma, Dong; Stoica, Alexandru Dan; An, Ke; Yang, Ling; Bei, Hongbin; Mills, Rebecca A; Skorpenske, Harley David; Wang, Xun-Li

    2011-01-01

    We report in-situ neutron diffraction studies of texture evolution and the (hcp) (bcc) phase transformation in commercially pure cold-drawn titanium upon continuous heating and cooling, complemented by differential scanning calorimetry (DSC) measurements. We show that the recrystallization of the phase at elevated temperature enhanced the preexisting fiber texture, which eventually facilitated the nucleation and growth of the phase favored by the Burgers orientation relationship, i.e., {0001} //{110} . More strikingly, upon completion of the transformation, the {110} texture (or preferred orientation) in was eliminated immediately by the rapid grain growth of intergranular allotriomorphs. This resulted in the loss of the original -texture when Ti was transformed back to from to upon subsequent cooling, distinct from the known texture memory effect for rolling textures in titanium. Our present work provides useful experimental results for understanding the mechanisms of texture evolution and phase transformation in titanium and its alloys and, by and large, low-symmetry alloys such as zirconium.

  18. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    SciTech Connect

    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. Development of MnBi permanent magnet: neutron diffraction of MnBi powder

    SciTech Connect

    Cui, Jun; Choi, Jung-Pyung; Li, Guosheng; Polikarpov, Evgueni; Darsell, Jens T.; Kramer, Matthew J.; Zarkevich, Nikolai; Wang, L. L.; Johnson, D. D.; Marinescu, Melania; Huang, Qingzhen; Wu, Hui; Vuong, Nguyen V.; Liu, J.Ping

    2014-03-05

    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 power. The result shows that the purity of the obtained powder is about 91wt.% at 300K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 μB at 50 K and 300 K respectively.

  20. Spin distribution in the diphenylpicrylhydrazyl (DPPH) radical measured by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Boucherle, J. X.; Gillon, B.; Maruani, J.; Schweizer, J.

    A complete experimental determination of the spin density has been performed on a DPPH : C6H6 single crystal using the polarized neutron diffraction technique. A parametric description of the spin density has been used, this being necessary for non-centrosymmetrical crystals. A large amount of the spin density (61 per cent) remains localized on the central hydrazyl group, in accordance with magnetic resonance data, with a slight excess of Nβ over Nα. The remaining part of the spin density (39 per cent) is delocalized on the three aromatic rings of DPPH, the amount of spin transferred on to a ring depending on the twist angle of the ring with respect to the hydrazyl backbone. On every ring the spin density changes its sign from carbon to carbon atom, in accordance with magnetic resonance and quantum theory. The spin populations measured for the carbons of the rings compare well with the hyperfine coupling constants of the adjacent protons, which permits a direct experimental verification of McConnell's first relation. These neutron diffraction results are compared with two quantum-mechanical calculations performed for the isolated DPPH radical, using the experimental geometry measured in the crystal. Both calculations reproduce fairly well the details of the spin density observed on the rings. The experimental spin distribution on the central nitrogen atoms is better reproduced by the local spin density (LSD) method than by the unrestricted Hartree-Fock (UHF) method, which overlocalizes the spin density on atom Nβ. None of these calculations predicts accurately the amount of delocalization on the rings.

  1. Rearrangement of twin variants in ferromagnetic shape memory alloy polyurethane composites studied by stroboscopic neutron diffraction

    NASA Astrophysics Data System (ADS)

    Feuchtwanger, J.; Lázpita, P.; Vidal, N.; Barandiaran, J. M.; Gutiérrez, J.; Hansen, T.; Peel, M.; Mondelli, C.; O'Handley, R. C.; Allen, S. M.

    2008-03-01

    The use of ferromagnetic shape memory alloy (FSMA) particles as fillers in polymeric matrix composites has been proposed for vibration damping. The large pseudo-plastic recoverable deformation of the FSMA particles due to the rearrangement of twin variants can dissipate a large amount of energy, both under compression and tension. The composites studied are made by mixing particles of NiMnGa with a polyurethane matrix. A magnetic field is applied to the composite while the matrix sets, to achieve a strong [112] texture in the field direction. In situ strobed neutron diffraction measurements were carried out while the composites were subjected to a cyclic deformation. They show that the intensity of certain peaks varies during the deformation cycle. All the peaks that show this behavior can be grouped into pairs that stem from a single austenitic peak. The (020) and (112) martensite peaks correspond to the splitting of the (220) austenite peak, and the intensity of one increases as that of the other decreases. The neutron measurements show directly that there is a change in the texture of the composite during the stress cycle applied to the composite and confirm that the large mechanical loss observed in the stress-strain cycles is in good part due to the rearrangement of twin variants in the FSMA filler used in the composites.

  2. Polymorphism in Photoluminescent KNdW2O8: Synthesis, Neutron Diffraction, and Raman Study

    SciTech Connect

    S. M. Bhat, Swetha; Swain, Diptikanta; Feygenson, Mikhail; Neuefeind, Joerg C; Sundaram, Nalini

    2014-01-01

    Polymorphs of KNdW2O8 ( -KNdW2O8 and -KNdW2O8) phosphors were synthesized by an efficient solution combustion technique for the first time. The crystal structure of the polymorphs analyzed from Rietveld refinement of neutron diffraction data confirms that -KNdW2O8 crystallizes in the tetragonal system (space group I4 ), and -KNdW2O8 crystallizes in the monoclinic system (space group C2/m). The local structure of both polymorphs was elucidated using combined neutron pair distribution function (PDF) and Raman scattering techniques. Photoluminescence measurements of the polymorphs showed broadened emission line width and increased intensity for -KNdW2O8 in the visible region compared to -KNdW2O8. This phenomenon is attributed to the increased distortion in the coordination environment of the luminescing Nd3+ ion. Combined PDF, Rietveld, and Raman measurements reveal distortions of the WO6 octahedra and NdO8 polyhedra in -KNdW2O8. This crystal structure photoluminescence study suggests that this class of tungstates can be exploited for visible light emitting devices by tuning the crystal symmetry.

  3. Residual stresses in a shape welded steel tube by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Taran, Yu V.; Balagurov, A. M.; Schreiber, J.; Stuhr, U.

    2008-03-01

    Measurements of the triaxial residual strains in a composite tube from an austenitic stainless steel as a parent material and a shape welded ferritic steel were carried out by the time-of-flight neutron diffraction method on the POLDI instrument at the PSI SINQ neutron pulsed facility. The shape weld is used to build compressive stresses and, as a result, to suppress stress corrosion. Investigations of the residual stresses in such composite tubes are important for developing optimal welding techniques. Calculation of the residual stresses was performed using measurement results with a comb-sample, machined from the tube by the electro-discharge method, as the stress free reference sample. The results of the POLDI measurements of the stress state in the composite tube are presented and compared to the results of the destructive turning out method and theoretical predictions of calculations by the finite element method. Semiquantitative agreement between all the used methods was only observed for the tangential component of the stress tensor. In this case, the ferrite cladding produced a tangential compressive stress of about 800 MPa on the austenitic tube.

  4. Neutron diffraction measurement of residual stresses in Al-clad U-10Mo fuel plates

    NASA Astrophysics Data System (ADS)

    Brown, D. W.; Okuniewski, M. A.; Clausen, B.; Moore, G. A.; Sisneros, T. A.

    2016-06-01

    Neutron diffraction was used to determine residual stress in monolithic two Al-clad U 10 weight percent Mo mini-fuel plates and a full sized fuel plate. One mini-plate was cooled following hot isostatic pressing at a rate of 6.75 °C/min, the second at 0.675 °C/min. A non-traditional method of calibrating the neutron diffractometer at each measurement point was necessitated by the thin nature of the sample. The in-plane stresses in the U-10Mo foils are relatively large, -250 MPa in the U-10Mo foil of the fast cooled mini-plate,-150 MPa in the slow cooled mini-plate and -275 MPa in the full-sized plate. Likewise, the in-plane stresses in the Al-cladding of the fast-cooled mini-plate and full-sized plate were determined to reach ∼50 MPa, while in the slow-cooled sample the stresses in the Al cladding were on the level of the measurement uncertainty. The in-plane stresses in the Zr diffusion barrier were estimated to be as large as -300 MPa.

  5. Temperature effects on the structure of liquid D-methanol through neutron diffraction

    NASA Astrophysics Data System (ADS)

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

    2004-08-01

    The study of changes in the structure (H-bonded) of liquid alcohols at elevated temperatures is rare probably due to low flash points of these liquids. An indigenously devised special quartz cell is now used to carry out the structural studies of these liquids at elevated temperatures through neutron diffraction. Here, the liquid consists of deuterated methanol and neutron data was collected on the high-Q diffractometer at Dhruva, BARC. The corrected data at elevated temperatures (BP (boiling point) and double the BP) show that there is a large change in the H-bonded structure of this liquid. The pre-peak or hump, known to be signature of H-bonded clusters appears to be present at all the three temperatures studied. In the low-Q (scattering vector) data Ornstein--Zernike (OZ) behaviour is also observed. It is, however, seen that the intramolecular structure does not change very much at higher temperatures. A detailed model analysis is in progress and would be reported later.

  6. Neutron-diffraction study up to 1600 °C of 3:2 mullite

    NASA Astrophysics Data System (ADS)

    Brunauer, G.; Frey, F.; Boysen, H.; Schneider, H.; Fischer, P.; Hansen, Th.; Többens, D.; Ehrenberg, H.

    Neutron-diffraction studies were carried out on pure and Cr-doped 3:2 (`sinter') mullite. To learn about structure-property relationships of this refractory material, thermal expansion coefficients and structural parameters were determined by in situ high-temperature investigations. Neutron experiments were performed at the powder diffractometers D2B/ILL, E9/HMI, and HRPT/PSI. All data gave a rather uniform picture of the thermal expansion coefficients: a linear behaviour below 1000 °C and significantly increased (mean) expansion between 1000 and 1600 °C. There is a marked anisotropy of the highest values along the b-axis of the orthorhombic mullite structure. Concerning the structural parameters and the derived bond lengths, there is an expansion of the Al1O6 octahedra, whereas the cross-linking Al2SiO4 tetrahedra stay more or less rigid, but may slightly rotate. Thus a major expansion along the b direction may be qualitatively understood. A structural discussion, however, is affected by the presence of disorder in mullite, in particular in Cr-doped mullite, as it is also reflected by the presence of a modulated diffuse background in the powder patterns.

  7. The magnetic and crystal structures of Sr2IrO4: A neutron diffraction study

    SciTech Connect

    Ye, Feng; Chi, Songxue; Chakoumakos, Bryan C; Fernandez-Baca, Jaime A; Qi, Tongfei; Cao, Gang

    2013-01-01

    We report a single-crystal neutron diffraction study of the layered Sr2IrO4. This work unambigu- ously determines the magnetic and crystal structures, and reveals that the spin orientation rigidly tracks the staggered rotation of the IrO6 octahedra in Sr2IrO4. The long-range antiferromagnetic order has a canted spin configuration with an ordered moment of 0.208(3) B/Ir site within the basal plane; a detailed examination of the spin canting yields 0.202(3) and 0.049(2) B/site for the a-axis and the b-axis, respectively. It is intriguing that forbidden nuclear reflections of space group I41/acd are also observed in a wide temperature range from 4 K to 600 K, which suggests a reduced crystal structure symmetry. This neutron scattering work provides a direct, well-refined experimen- tal characterization of the magnetic and crystal structures that are crucial to the understanding of the unconventional magnetism existent in this unusual magnetic insulator.

  8. Diffraction limit of the theory of multiple small-angle neutron scattering by a dense system of scatterers

    NASA Astrophysics Data System (ADS)

    Dzheparov, F. S.; Lvov, D. V.

    2016-02-01

    Multiple small-angle neutron scattering by a high-density system of inhomogeneities has been considered. A combined approach to the analysis of multiple small-angle neutron scattering has been proposed on the basis of the synthesis of the Zernike-Prince and Moliére formulas. This approach has been compared to the existing multiple small-angle neutron scattering theory based on the eikonal approximation. This comparison has shown that the results in the diffraction limit coincide, whereas differences exist in the refraction limit because the latter theory includes correlations between successive scattering events. It has been shown analytically that the existence of correlations in the spatial position of scatterers results in an increase in the number of unscattered neutrons. Thus, the narrowing of spectra of multiple small-angle neutron scattering observed experimentally and in numerical simulation has been explained.

  9. A large volume cell for in situ neutron diffraction studies of hydrothermal crystallizations

    NASA Astrophysics Data System (ADS)

    Xia, Fang; Qian, Gujie; Brugger, Joël; Studer, Andrew; Olsen, Scott; Pring, Allan

    2010-10-01

    A hydrothermal cell with 320 ml internal volume has been designed and constructed for in situ neutron diffraction studies of hydrothermal crystallizations. The cell design adopts a dumbbell configuration assembled with standard commercial stainless steel components and a zero-scattering Ti-Zr alloy sample compartment. The fluid movement and heat transfer are simply driven by natural convection due to the natural temperature gradient along the fluid path, so that the temperature at the sample compartment can be stably sustained by heating the fluid in the bottom fluid reservoir. The cell can operate at temperatures up to 300 °C and pressures up to 90 bars and is suitable for studying reactions requiring a large volume of hydrothermal fluid to damp out the negative effect from the change of fluid composition during the course of the reactions. The capability of the cell was demonstrated by a hydrothermal phase transformation investigation from leucite (KAlSi2O6) to analcime (NaAlSi2O6ṡH2O) at 210 °C on the high intensity powder diffractometer Wombat in ANSTO. The kinetics of the transformation has been resolved by collecting diffraction patterns every 10 min followed by Rietveld quantitative phase analysis. The classical Avrami/Arrhenius analysis gives an activation energy of 82.3±1.1 kJ mol-1. Estimations of the reaction rate under natural environments by extrapolations agree well with petrological observations.

  10. Neutron diffraction studies of nickel-containing perovskite oxide catalysts exposed to autothermal reforming environments.

    SciTech Connect

    Mawdsley, J. R.; Vaughey, J. T.; Krause, T. R.; Chemical Sciences and Engineering Division

    2009-10-27

    Six nickel-containing perovskite oxides (La{sub 1-x}Sr{sub x})M{sub 0.9}Ni{sub 0.1}O{sub 3{+-}{delta}}, where x = 0 or 0.2 and M = Cr, Fe, or Mn were used to catalyze the autothermal reforming of isooctane (C{sub 8}H{sub 18}) into a hydrogen-rich gas during short-term tests at 700 C. To determine the phase stability of the samples in the reducing environment of the reforming reactor, characterization studies of the as-prepared and tested perovskite samples were conducted using powder X-ray diffraction, powder neutron diffraction, transmission electron microscopy, and scanning electron microscopy. We determined that the reducing conditions of the microreactor caused metallic nickel to form in all six compositions. However, the extent of the nickel loss from the perovskite lattices varied: the chromium-containing compositions lost the least nickel, compared to the manganese- and iron-containing compositions, and the strontium-free compositions lost more nickel than their strontium-containing analogs. Five of the six perovskite compositions tested showed no breakdown of the perovskite lattice despite the loss of nickel from the B-sites, producing only the third example of a B-cation-deficient, 3d transition-metal-containing perovskite.

  11. Optimizations in angular dispersive neutron powder diffraction using divergent beam geometries

    NASA Astrophysics Data System (ADS)

    Buchsteiner, Alexandra; Stüßer, Norbert

    2009-01-01

    Angular dispersive neutron powder diffractometers are usually built using beam divergencies defined by Soller type collimators. To account for the needs of resolution for crystal structure refinement a good in-pile collimation α1, a high take-off angle above 90∘ at the monochromator and a good collimation α3 in front of the detector bank are chosen whereas the value of α2 for the collimation between monochromator and sample is less crucial. During the last years new strategies were developed at our institute using wide divergent beam geometries defined by fan collimators or slit-type diaphragms which correlate ray direction and wavelength within the beam. Here we present the performance of a newly developed fan collimator, which enables one to adjust the opening of the collimator channels on both sides independently. This fan collimator is positioned in front of the monochromator at the instrument E6 at the Helmholtz Centre Berlin (formerly Hahn-Meitner-Institut Berlin). It will be shown that control of the beam divergency allows optimization of the resolution in a large angular diffraction range. Hence the resolution and intensity can be adapted to the needs of powder diffraction. Monte Carlo simulations using McStas are used to check and prove the optimal setting of the instrument. We obtain a very good agreement between experimental and simulated data and demonstrate the superior outcome of the new instrument configuration with respect to Soller type instruments.

  12. Lamellar spacing of photosystem II membrane fragments upon dehydration studied by neutron membrane diffraction

    NASA Astrophysics Data System (ADS)

    Pieper, Jörg; Rusevich, Leonid; Hauß, Thomas; Renger, Gernot

    2016-02-01

    The effect of dehydration on the lamellar spacing of photosystem II (PS II) membrane fragments from spinach has been investigated using neutron membrane diffraction at room temperature. The diffraction data reveal a major peak at a scattering vector Q of 0.049 Å-1 at a relative humidity (r.h.) of 90% corresponding to a repeat distance D of about 129 Å. Upon dehydration to 44% r.h., this peak shifts to about 0.060 Å-1 corresponding to a distance of 104.7±2.5 Å. Within experimental error, the latter repeat distance remains almost the same at hydration levels below 44% r.h. indicating that most of the hydration water is removed. This result is consistent with the earlier finding that hydration-induced conformational protein motions in PS II membrane fragments are observed above 44% r.h. and correlated with the onset electron transfer in PS II (Pieper et al. 2008, Eur. Biophys. J. 37: 657-663).

  13. Lamellar spacing of photosystem II membrane fragments upon dehydration studied by neutron membrane diffraction

    NASA Astrophysics Data System (ADS)

    Pieper, Jörg; Rusevich, Leonid; Hauß, Thomas; Renger, Gernot

    2015-12-01

    The effect of dehydration on the lamellar spacing of photosystem II (PS II) membrane fragments from spinach has been investigated using neutron membrane diffraction at room temperature. The diffraction data reveal a major peak at a scattering vector Q of 0.049 Å-1 at a relative humidity (r.h.) of 90% corresponding to a repeat distance D of about 129 Å. Upon dehydration to 44% r.h., this peak shifts to about 0.060 Å-1 corresponding to a distance of 104.7±2.5 Å. Within experimental error, the latter repeat distance remains almost the same at hydration levels below 44% r.h. indicating that most of the hydration water is removed. This result is consistent with the earlier finding that hydration-induced conformational protein motions in PS II membrane fragments are observed above 44% r.h. and correlated with the onset electron transfer in PS II (Pieper et al. 2008, Eur. Biophys. J. 37: 657-663).

  14. Determination and mitigation of the uncertainty of neutron diffraction measurements of residual strain in large-grained polycrystalline material

    PubMed Central

    Holden, Tom M.; Traore, Yeli; James, Jon; Kelleher, Joe; Bouchard, P. John

    2015-01-01

    For large-grained samples it is advantageous to perform pairs of neutron diffraction measurements at the same spatial location but rotated 180° around the geometric centre of the gauge volume as a means of minimizing the scatter coming from the random positioning of grains within the gauge volume. PMID:25844082

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

    SciTech Connect

    Christien, F.; Telling, M.T.F.; Knight, K.S.

    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)

  16. In-Situ Neutron Diffraction Studies of Complex Hydrogen Storage Materials

    SciTech Connect

    Yelon, William B.

    2013-05-13

    The thrust of this project was to investigate the structures of important materials with potential application to hydrogen storage, in an effort to meet the DOE goals for 2010 and 2015, namely 9% (wt) and 15% (wt) respectively. Unfortunately, no material has been found, despite the efforts of many laboratories, including our own, that achieves these goals in a reversible complex hydride such as ammonia borane (NH{sub 4}BH{sub 4}), and other ammonia based compounds, or with light hydrides such as LiBH{sub 4}, due either to their irreversibility or to the high decomposition temperatures and residual simple hydrides such as LiH from the decomposition of the last named compound. Nevertheless, several important technical goals have been accomplished that could be valuable to other DOE programs and would be available for collaborative research. These include the development of a high quality glove box with controlled (low) oxygen and water content, which we continue to employ for the synthesis of potential new materials (unfunded research) and the development of a high quality neutron diffraction furnace with controlled gas environment for studies of hydrogen uptake and loss as well as for studies with other gasses. This furnace was initially constructed with an alumina (Al{sub 2}O{sub 3}) center tube to contain the sample and the flowing gas. The heaters are located in the vacuum space outside the tube and it was found that, for the low temperatures required for the study of hydrogen storage materials, the heat transfer was too poor to allow good control. At temperatures in excess of about 400C (and up to more than 1200C) the heat transfer and control are excellent. For the lower temperatures, however, the center tube was replaced by stainless steel and temperature control to 1C became possible. The paired heaters, above and below the neutron beam window allowed control of the temperature gradient to a similar precision. The high temperature capability of the furnace

  17. Feasibility Study on Neutron Diffraction Method for Evaluation of Residual Strain Distribution of Regenerative Cooled Combustion Chamber

    NASA Astrophysics Data System (ADS)

    Masuoka, Tadashi; Moriya, Shin-Ichi; Sato, Masaki; Yoshida, Makoto; Tsuchiya, Yoshinori; Suzuki, Hiroshi

    The regenerative cooled combustion chamber of a cryogenic liquid rocket engine is exposed to a large temperature difference between the hot gas (about 3500K) and the liquid hydrogen (about 20K). This induces thermal stress, and strain is accumulated in the chamber wall throughout the cyclic firing tests. Evaluation of the stress and the strain distribution in a chamber wall is essential since chamber life is usually related to such stress and strain. In this study, the residual strain in a regenerative cooled combustion chamber wall was measured by applying the neutron diffraction method and the X-ray diffraction method. The measured data were compared with the numerical data by finite element analysis, and the feasibility of the neutron diffraction method for the regenerative cooled combustion chamber of a cryogenic liquid rocket engine was evaluated.

  18. Neutron diffraction of alpha, beta and gamma cyclodextrins: Hydrogen bonding patterns

    SciTech Connect

    Hingerty, B.; Klar, B.; Hardgrove, G.L.; Betzel, C.; Saenger, W. )

    1984-08-01

    Cyclodextrins (CD's) have proved useful as model systems for the study of hydrogen bonding. They are torus-shaped molecules composed of six(alpha), seven(beta) or eight(gamma) (1----4) linked glucoses. Because of their particular geometry, they are able to act as a host to form inclusion complexes with guest molecules very much like enzymes. Cyclodextrins have been shown to exert catalytic activity on suitable included-substrate molecules; they catalyze the hydrolysis of phenylacetates, of organic pyrophosphates and of penicillin derivatives. They also accelerate aromatic chlorinations and diazo coupling by means of their primary and/or secondary hydroxyl groups, so that the rates of hydrolysis are enhanced by up to a factor of 400. In order to understand the hydrogen bonding in these enzyme models, neutron diffraction data were collected to unambiguously determine the hydrogen atom positions, which could not be done from the x-ray diffraction data. alpha-CD has been shown to have two different structures with well-defined hydrogen bonds, one tense and the other relaxed. An induced-fit-like mechanism for alpha-CD complex formation has been proposed. Circular hydrogen bond networks have also been found for alpha-CD due to the energetically favored cooperative effect. beta-CD with a disordered water structure possesses an unusual flip-flop hydrogen bonding system of the type O-H...H-O representing an equilibrium between two states: O-H...O in equilibrium O...H-O. gamma-CD with a disordered water structure similar to beta-CD also possesses the flip-flop hydrogen bond. This study demonstrates that hydrogen bonds are operative in disordered systems and display dynamics even in the solid state. 33 references.

  19. Neutron diffraction measurements and micromechanical modelling of temperature-dependent variations in TATB lattice parameters

    DOE PAGESBeta

    Yeager, John D.; Luscher, Darby J.; Vogel, Sven C.; Clausen, Bjorn; Brown, Donald W.

    2016-06-01

    Triaminotrinitrobenzene (TATB) is a highly anisotropic molecular crystal used in several plastic-bonded explosive (PBX) formulations. TATB-based explosives exhibit irreversible volume expansion (“ratchet growth”) when thermally cycled. A theoretical understanding of the relationship between anisotropy of the crystal, crystal orientation distribution (texture) of polycrystalline aggregates, and the intergranular interactions leading to this irreversible growth is necessary to accurately develop physics-based predictive models for TATB-based PBXs under various thermal environments. In this work, TATB lattice parameters were measured using neutron diffraction during thermal cycling of loose powder and a pressed pellet. The measured lattice parameters help clarify conflicting reports in the literaturemore » as these new results are more consistent with one set of previous results than another. The lattice parameters of pressed TATB were also measured as a function of temperature, showing some differences from the powder. This data is used along with anisotropic single-crystal stiffness moduli reported in the literature to model the nominal stresses associated with intergranular constraints during thermal expansion. The texture of both specimens were characterized and the pressed pellet exhibits preferential orientation of (001) poles along the pressing direction, whereas no preferred orientation was found for the loose powder. Lastly, thermal strains for single-crystal TATB computed from lattice parameter data for the powder is input to a self-consistent micromechanical model, which predicts the lattice parameters of the constrained TATB crystals within the pellet. The agreement of these model results with the diffraction data obtained from the pellet is discussed along with future directions of research.« less

  20. Phase transitions and hydrogen bonding in deuterated calcium hydroxide: High-pressure and high-temperature neutron diffraction measurements

    SciTech Connect

    Iizuka, Riko; Komatsu, Kazuki; Kagi, Hiroyuki; Nagai, Takaya; Sano-Furukawa, Asami; Hattori, Takanori; Gotou, Hirotada; Yagi, Takehiko

    2014-10-15

    In situ neutron diffraction measurements combined with the pulsed neutron source at the Japan Proton Accelerator Research Complex (J-PARC) were conducted on high-pressure polymorphs of deuterated portlandite (Ca(OD){sub 2}) using a Paris–Edinburgh cell and a multi-anvil press. The atomic positions including hydrogen for the unquenchable high-pressure phase at room temperature (phase II′) were first clarified. The bent hydrogen bonds under high pressure were consistent with results from Raman spectroscopy. The structure of the high-pressure and high-temperature phase (Phase II) was concordant with that observed previously by another group for a recovered sample. The observations elucidate the phase transition mechanism among the polymorphs, which involves the sliding of CaO polyhedral layers, position modulations of Ca atoms, and recombination of Ca–O bonds accompanied by the reorientation of hydrogen to form more stable hydrogen bonds. - Graphical abstract: Crystal structures of high-pressure polymorphs of Ca(OD){sub 2}, (a) at room temperature (phase II′) and (b) at high temperature (phase II), were obtained from in situ neutron diffraction measurements. - Highlights: • We measured in situ neutron diffraction of high-pressure polymorphs of Ca(OD){sub 2}. • Hydrogen positions of the high-pressure phase are first determined. • The obtained hydrogen bonds reasonably explain Raman peaks of OH stretching modes. • A phase transition mechanism among the polymorphs is proposed.

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

    PubMed

    Sano-Furukawa, A; Hattori, T; Arima, H; Yamada, A; Tabata, S; Kondo, M; Nakamura, A; Kagi, H; Yagi, T

    2014-11-01

    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(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. PMID:25430122

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

    SciTech Connect

    Sano-Furukawa, A. Hattori, T.; Arima, H.; Yamada, A.; Tabata, S.; Kondo, M.; Nakamura, A.; Kagi, H.; Yagi, T.

    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.

  3. Tensile deformation behaviors of Zircaloy-4 alloy at ambient and elevated temperatures: In situ neutron diffraction and simulation study

    NASA Astrophysics Data System (ADS)

    Li, Hongjia; Sun, Guangai; Woo, Wanchuck; Gong, Jian; Chen, Bo; Wang, Yandong; Fu, Yong Qing; Huang, Chaoqiang; Xie, Lei; Peng, Shuming

    2014-03-01

    Tensile stress-strain relationship of a rolled Zircaloy-4 (Zr-4) plate was examined in situ using a neutron diffraction method at room temperature (RT, 25 °C) and an elevated temperature (250 °C). Variations of lattice strains were obtained as a function of macroscopic bulk strains along prismatic (101¯0), basal (0 0 0 2) and pyramidal (101¯1) planes in the hexagonal close-packed structure of the Zr-4. The mechanisms of strain responses in these three major planes were simulated using elastic-plastic self-consistent (EPSC) model based on Hill-Hutchinson method, thus the inter-granular stresses and deformation systems of each individual grain under loading were obtained. Results show that there is a good agreement between the EPSC modeling and neutron diffraction measurements in terms of macroscopic stress-strain relationship and lattice strain evolutions of the planes at RT. However, there is a slight discrepancy in the lattice strains obtained from the EPSC modeling and neutron diffraction when the specimen was deformed at 250 °C. Analysis of grain structure and texture obtained using electron back-scattered diffraction suggests that dynamic recovery process is significant during the tensile deformation at the elevated temperature, which was not considered in the simulation.

  4. Crystal structure and thermal vibrations of cholesteryl acetate from neutron diffraction at 123 and 20 K.

    PubMed

    Weber, H P; Craven, B M; Sawzik, P; McMullan, R K

    1991-02-01

    Cholesteryl acetate (C29H48O2) at 20 K is monoclinic, space group P2(1) with a = 16,521 (4), b = 9,220 (2), c = 17,620 (5) A, beta = 107.18 (2) degrees and Z = 4 (two molecules in the asymmetric unit). The crystal structure, earlier determined by X-ray diffraction at 123 K, has been redetermined at 123 and 20 K by neutron diffraction (7447 reflections at 123 K, 7281 at 20 K; sin theta/lambda less than 0.69 A-1) and refined by full-matrix least squares with 1423 variables to give R(F2) = 0.10 at 123 K, 0.06 at 20 K. Results at 20 K are more accurate not only because nuclear thermal vibrations have reduced amplitudes but also because a larger crystal was used for data collection. At 20 K, the average of 44 methylene C-H bond lengths is 1,102 (8) A (sigma from the observed distribution) and 1.103 (6) A for 16 methine groups. The 22 methylene H-C-H angles [106.2 (9) degrees] all fall within a narrow range. Analysis of nuclear anisotropic thermal parameters shows that intramolecular vibrations of the H nuclei are highly significant with similar mean-square amplitudes at 123 and 20 K. Torsional vibrations around the C-CH3 bonds of the C18 and C19 methyl groups have r.m.s. amplitudes of about 7 degrees. For methylene groups, mean-square amplitudes are a minimum for C-H bond stretching (0.006 A2) and a maximum for CH2 in-plane vibrations (0.024 A2). Values of Beq for the H-atom intramolecular vibrations are 0.8, 1.2 and 1.6 A2 for methine, methylene and methyl H atoms respectively. These results can be used to estimate Beq for H atoms in crystal structure determinations carried out by X-ray diffraction. The anisotropic intramolecular vibrations of the H nuclei contribute to the effective shape of the H atoms which, from the observed anisotropy in the distribution of intermolecular H...H distances, appears to be flattened along the direction of the C-H bond. PMID:2025409

  5. Microstructural Investigation of Fe-Ni-Mn-Mo-V-C-N Ferritic Steels by Neutron Diffraction

    NASA Astrophysics Data System (ADS)

    Baeva, M.; Beskrovnyi, A. I.; Parshorov, I.; Vassilovskii, S. G.

    2010-01-01

    The design of alloys, that economize strategic element as chromium requires detailed physical investigations of their structure and phase composition. In the search for new materials in the last two decades a new class of Fe alloys was composed—the so-called nitrogen steels. The contemporary achievements in the casting technology—the use of nitrogen under high preasure above the melt—made possible the production of Fe alloys with nitrogen concentration even above 0.4 wt%. The wide application of investigated alloy system is connected with creation of alloys without presence of strong carbides-forming elements. The microstructure and phase formation of these new materials are insufficiently studied. The aim of this work is to characterize the microstructure and phase composition of two series Fe-alloys casted with and without nitrogen pressure above the melt. The so cast steels appear as experimental ones and they are directed to demonstrate the possibility for nitrogen doping of steels without presence of Chromium in them. The latter is technologically difficult to fulfil at usual conditions. Six samples [with lower nitrogen, N = 0.0111 wt%] are cast at normal pressure, and six samples [with higher nitrogen, N0.2121 wt%] are cast at pressure of 10.106 Pa. The results of Rietveld structure analysis of Time-Of-Flight neutron diffraction data show that studied steels consist of purely ferritic crystal phase (Body Centered Cubic crystal lattice).

  6. Neutron diffraction study of MnNiGa{sub 2}—Structural and magnetic behaviour

    SciTech Connect

    Wang, J. L.; Ma, L.; Wu, G. H.; Hofmann, M.; Avdeev, M.; Kennedy, S. J.; Campbell, S. J.; Md Din, M. F.; Dou, S. X.; Hoelzel, M.

    2014-05-07

    MnNiGa{sub 2} crystallizes in the L21 (Heusler) structure and has a ferromagnetic ordering temperature T{sub C} ∼ 192 K. Rietveld refinement of the neutron diffraction patterns indicates that the Ga atoms occupy the equivalent 8c position, while Mn and Ni share the 4a (0, 0, 0) and 4b (0.5, 0.5, 0.5) sites with a mixed occupancy of Mn and Ni atoms. It is found that that ∼83% of Mn and ∼17% Ni are located at the 4a site while ∼83% of Ni and ∼17% Mn occupy the 4b site. There is no evidence of a magneto-volume effect around T{sub C}. In agreement with this finding, our detailed critical exponent analyses of isothermal magnetization curves and the related Arrott plots confirm that the magnetic phase transition at T{sub C} is second order.

  7. Residual Stresses in DC cast Aluminum Billet: Neutron Diffraction Measurements and Thermomechanical Modeling

    SciTech Connect

    Drezet, J.-M.; Evans, A.; Pirling, T.

    2011-05-04

    Thermally-induced residual stresses, generated during the industrial Direct Chill casting process of aluminum alloys, can cause both significant safety concerns as well as the formation of defects during down-stream processing. Although these thermally induced strains can be partially relieved by permanent deformation, cracks will be generated either during solidification (hot tears) or post-solidification cooling (cold cracks) when stresses exceed the deformation limit of the alloy. Furthermore, the thermally induced strains result in the presence of large internal stresses within the billet before further processing steps. Although numerical models have been previously developed to compute these residual stresses, most of the computations have been validated only against measured surface distortions. In the present work, the variation in residual elastic strains and stresses in the steady state regime of casting has been measured as a function of radial position using neutron diffraction in an AA6063 grain-refined cylindrical billet. These measurements have been carried out on the same billet section at Poldi at PSI-Villigen and at Salsa at ILL-Grenoble and compare favorably. The results are used to validate a thermo-mechanical finite element casting model and to assess the level of stored elastic energy within the billet.

  8. Residual Stresses in DC cast Aluminum Billet: Neutron Diffraction Measurements and Thermomechanical Modeling

    NASA Astrophysics Data System (ADS)

    Drezet, J.-M.; Evans, A.; Pirling, T.

    2011-05-01

    Thermally-induced residual stresses, generated during the industrial Direct Chill casting process of aluminum alloys, can cause both significant safety concerns as well as the formation of defects during down-stream processing. Although these thermally induced strains can be partially relieved by permanent deformation, cracks will be generated either during solidification (hot tears) or post-solidification cooling (cold cracks) when stresses exceed the deformation limit of the alloy. Furthermore, the thermally induced strains result in the presence of large internal stresses within the billet before further processing steps. Although numerical models have been previously developed to compute these residual stresses, most of the computations have been validated only against measured surface distortions. In the present work, the variation in residual elastic strains and stresses in the steady state regime of casting has been measured as a function of radial position using neutron diffraction in an AA6063 grain-refined cylindrical billet. These measurements have been carried out on the same billet section at Poldi at PSI-Villigen and at Salsa at ILL-Grenoble and compare favorably. The results are used to validate a thermo-mechanical finite element casting model and to assess the level of stored elastic energy within the billet.

  9. Neutron diffraction of titanium aluminides formed by continuous electron-beam treatment

    NASA Astrophysics Data System (ADS)

    Valkov, S.; Neov, D.; Luytov, D.; Petrov, P.

    2016-03-01

    Ti-Al-based alloys were produced by hybrid electron-beam technologies. A composite Ti-Al film was deposited on a Ti substrate by electron-beam evaporation (EBE), followed by electron-beam treatment (EBT) by a continuously scanned electron beam. The speed of the specimens motion during the EBT were V 1 = 1 cm/sec and V 2 = 5 cm/sec, in order to realize two different alloying mechanisms -- by surface melting and by electron-beam irradiation without melting the surface. The samples prepared were characterized by XRD and neutron diffraction to study the crystal structure on the surface and in depth. SEM/EDX analysis was conducted to explore the surface structure and analyze the chemical composition. Nanoindentation measurements were also carried out. No intermetallic phases were registered in the sample treated at velocity V 1, while the sample treated at V 2 exhibited a Ti3Al/TiAl structure on the surface, transformed to Ti/TiAl in depth. The nanoindentation test demonstrated a significant negative hardness gradient from the surface to the depth of the sample.

  10. NEUTRON DIFFRACTION MEASUREMENT OF RESIDUAL STRESSES IN FRICTION STIR PROCESSED NANOCOMPOSITE SURFACE LAYER

    SciTech Connect

    Xu, Hanbing; Hubbard, Camden R; An, Ke; Wang, Xun-Li; Feng, Zhili; Qu, Jun

    2009-01-01

    Friction stir processing (FSP) was successfully used to stir and mix nano-sized Al2O3 particles into a Al6061-T6 aluminum plate to form a nanocomposite layer up to 3 mm thick. This nanocomposite surface has demonstrated significantly improved surface hardness, yield strength, and wear-resistance without sacrificing the substrate ductility and conductivity. Neutron diffraction analysis was conducted to determine the residual stress distribution in the nanocomposite surface layer. For comparison, the residual stress of the aluminum surface that was processed similarly but had no particle involved was also measured. Results showed that the macro-level residual stresses in the FSP zone without particles are low due to the annealing effect induced by the long heating time and large heat input. The macro-level residual stresses in the FSP-processed Al-Al2O3 nanocomposite zone are tensile up to 100 MPa in all three directions. The details of the results will be further discussed in the paper.

  11. Characterization of the Structure of LaD 2.50by Neutron Powder Diffraction

    NASA Astrophysics Data System (ADS)

    Udovic, T. J.; Huang, Q.; Rush, JJ

    1996-02-01

    Neutron powder diffraction (NPD) measurements of the rare-earth deuteride LaD2.50were undertaken between 10 and 430 K. Rietveld refinements indicated that, above ∼385 K, the LaD2.50structure is cubic (Fm3m) with deuterium fully occupying the tetrahedral (t) interstices of the fcc La lattice and the excess deuterium occupying a portion of the octahedral (o) interstices with full statistical disorder. As the temperature is decreased below ∼385 K, the LaD2.50structure undergoes a tetragonal distortion concomitant with the onset of deuterium long-range order (I41/amd) in the o sublattice, similar to previous structural results for the light-rare-earth deuteridesRD2+xfor 0.3

  12. In Situ Neutron Diffraction Studies of Large Monotonic Deformations of Superelastic Nitinol

    NASA Astrophysics Data System (ADS)

    Stebner, Aaron P.; Paranjape, Harshad M.; Clausen, Bjørn; Brinson, L. Catherine; Pelton, Alan R.

    2015-06-01

    Superelastic Nitinol micromechanics are studied well into plastic deformation regimes using neutron diffraction. Insights are made into the nature of initial transformation, bulk transformation, plastic deformation, and unloading. Schmid factor predictions based on habit plane variants are found to best describe the very first grains that transform, prior to the transformation plateaus. However, the bulk transformation behavior that gives rise to transformation plateaus violates single crystal Schmid factor analyses, indicating that in bulk polycrystals, it is the effect of grain neighborhoods, not the orientations of individual grains, that drives transformation behaviors. Beyond the plateaus, a sudden shift in micromechanical deformation mechanisms is observed at ~8.50 %/4.75 % tension/compression engineering strain. This mechanism results in reverse-phase transformation in both cases, indicating a strong relaxation in internal stresses of the samples. It is inferred that this mechanism is most likely initial bulk plastic flow, and postulated that it is the reason for a transition from fatigue life enhancement to detriment when pre-straining superelastic Nitinol. The data presented in this work provide critical datasets for development and verification of both phenomenological internal variable-driven and micromechanical theories of transformation-plasticity coupling in shape memory alloys.

  13. Collinear antiferromagnetism in trigonal SrMn2As2 revealed by single crystal neutron diffraction

    NASA Astrophysics Data System (ADS)

    Kreyssig, A.; Das, P.; Sangeetha, N. S.; Benson, Z. A.; Heitman, T.; Johnston, D. C.; Goldman, A. I.

    FeAs-based compounds and related materials have been an area of intense research in understanding the complex interplay between magnetism and superconductivity. Here we report on the magnetic structure of SrMn2As2 that crystallizes in a trigonal structure (P 3 m1) and undergoes an antiferromagnetic (AFM) transition at TN ~ 120 K. The temperature dependence of the magnetic susceptibility remains nearly constant below TN with H ∥ c while it decreases significantly with H ∥ ab . This shows that the local Mn moments order and lie in the ab plane instead of aligning along the c axis as in BaMn2As2. Single crystal neutron diffraction measurements on SrMn2As2 determined that the Mn moments are collinearly aligned in a G-type AFM order with AFM alignments between a moment and all nearest neighbors in the basal plane and also perpendicular to it. This manifests that G-type AFM order is robust for Mn122 systems despite different symmetries, i.e. tetragonal for BaMn2As2 and trigonal for SrMn2As2.Work at Ames Laboratory was supported by the DOE, BES, Division of Materials Sciences & Engineering, through DE-AC02-07CH11358. This research used resources at University of Missouri Research Reactor.

  14. Neutron diffraction studies of the interaction between amphotericin B and lipid-sterol model membranes

    NASA Astrophysics Data System (ADS)

    Foglia, Fabrizia; Lawrence, M. Jayne; Demeė, Bruno; Fragneto, Giovanna; Barlow, David

    2012-10-01

    Over the last 50 years or so, amphotericin has been widely employed in treating life-threatening systemic fungal infections. Its usefulness in the clinic, however, has always been circumscribed by its dose-limiting side-effects, and it is also now compromised by an increasing incidence of pathogen resistance. Combating these problems through development of new anti-fungal agents requires detailed knowledge of the drug's molecular mechanism, but unfortunately this is far from clear. Neutron diffraction studies of the drug's incorporation within lipid-sterol membranes have here been performed to shed light on this problem. The drug is shown to disturb the structures of both fungal and mammalian membranes, and co-localises with the membrane sterols in a manner consistent with trans-membrane pore formation. The differences seen in the membrane lipid ordering and in the distributions of the drug-ergosterol and drug-cholesterol complexes within the membranes are consistent with the drug's selectivity for fungal vs. human cells.

  15. Characterization of the intercalate C60(CO2)x by powder neutron diffraction

    NASA Astrophysics Data System (ADS)

    James, M.; Kennedy, S. J.; Elcombe, M. M.; Gadd, G. E.

    1998-12-01

    The intercalate compound C60(CO2)x has been synthesized by hot isostatically pressing C60 under 170 MPa of CO2 and 350 °C. Neutron powder diffraction studies conducted on C60(CO2)x between room temperature and 5 K have been analyzed using Rietveld techniques and reveal a structural transition between a high-temperature (>~250 K) face-centered cubic phase [Fm3¯m, a=14.224(2) Å (293 K)] and a low-temperature (<~150 K) monoclinic phase [P21/n, a=9.7438(9) Å, b=9.7473(9) Å, c=14.6121(11) Å, β=90.390(6)° (5 K)]. The CO2 molecules occupy the octahedral interstices between the C60 molecules and are oriented along the body diagonal of the high-temperature phase. In the low-temperature phase they are tilted slightly away from the c axis so as to place the oxygen atoms adjacent to the center of a pentagonal face on the C60 molecules.

  16. Thermal expansion and decomposition of jarosite: a high-temperature neutron diffraction study

    SciTech Connect

    Xu, Hongwu; Zhao, Yusheng; Vogel, Sven C; Hickmott, Donald D; Daemen, Luke L; Hartl, Monika A

    2009-01-01

    The structure of deuterated jarosite, KFe{sub 3}(SO{sub 4}){sub 2}(OD){sub 6}, was investigated using time-of-flight neutron diffraction up to its dehydroxylation temperature. Rietveld analysis reveals that with increasing temperature, its c dimension expands at a rate {approx}10 times greater than that for a. This anisotropy of thermal expansion is due to rapid increase in the thickness of the (001) sheet of [Fe(O,OH){sub 6}] octahedra and [SO{sub 4}] tetrahedra with increasing temperature. Fitting of the measured cell volumes yields a coefficient of thermal expansion, a = a{sub 0} + a{sub 1} T, where a{sub 0} = 1.01 x 10{sup -4} K{sup -1} and a{sub 1} = -1.15 x 10{sup -7} K{sup -2}. On heating, the hydrogen bonds, O1{hor_ellipsis}D-O3, through which the (001) octahedral-tetrahedral sheets are held together, become weakened, as reflected by an increase in the D{hor_ellipsis}O1 distance and a concomitant decrease in the O3-D distance with increasing temperature. On further heating to 575 K, jarosite starts to decompose into nanocrystalline yavapaiite and hematite (as well as water vapor), a direct result of the breaking of the hydrogen bonds that hold the jarosite structure together.

  17. Structure Determination and Refinement of Acid Strontium Oxalate from X-Ray and Neutron Powder Diffraction

    NASA Astrophysics Data System (ADS)

    Vanhoyland, G.; Bourée, F.; Van Bael, M. K.; Mullens, J.; Van Poucke, L. C.

    2001-03-01

    The structure of acid strontium oxalate Sr(HC2O4)·{1}/{2}(C2O4)·H2O has been determined by conventional X-ray powder diffractometry. The diffraction pattern was indexed from a monoclinic unit cell with cell parameters a=6.341(1) Å, b=16.880(2) Å, c=5.7798(8) Å, and β=97.60(1)°; space group, P21/n (No. 14) with Z=4. Final (isotropic) Rietveld refinement of the neutron powder data yielded RB=4.57%, RF=2.87%, and Rwp=7.87% as conventional Rietveld parameters. Strontium is eight-fold coordinated and can be described as a distorted bicapped trigonal prism. The SrO8 polyhedra form one-dimensional chains along the c-axis by sharing edges. In contrast to all other known strontium oxalates, in this compound H2O acts as bridging ligand between two Sr atoms. SDPD-D classification (1): Sr(HC2O4)-{1}/{2}(C2O4)-H2O, P21/n, C1=14, Nc=42, C2=11, XC1+N/TREOR-97 & DICVOL-91, EXTRA, EQUI, SIRPOW-92 (DM), GFOURIER, FULLPROF.

  18. Neutron diffraction study of 154SmFeAsO1-xDx

    NASA Astrophysics Data System (ADS)

    Iimura, Soshi; Okanishi, Hiroshi; Matsuishi, Satoru; Hiraka, Haruhiro; Ikeda, Kazutaka; Hansen, Thomas; Otomo, Toshiya; Hosono, Hideo

    Hot issue in unconventional superconductors (SC) is why the 2nd highest-Tc of 56 K after cuprates is accomplished in the 1111-type iron-oxyarsenides LnFeAsO1-xFx (Ln = lanthanide). Recently, utilizing a hydride-substitution-method (O2- = H- + e-) in the LnFeAsO1 -xHx, we found a second SC phase in 0.18 <= x <= 0.45 at Ln = La in addition to the first one adjacent to the antiferromagnetic (AFM) order, and another AFM order accompanying a unique structural transition in over-doped region x >0.4. However, since the Tc of La-system is lower than the other systems, i.e., Ln = Ce, Sm and so on, it is still unclear whether the second AFM phase is essential for their high-Tc or not. Thus, we synthesized the isotope-substituted 154SmFeAsO1-xDx and performed neutron powder diffraction (NPD) to examine the structural and magnetic properties of the high-Tc 1111 system. In this talk, we show the results of NPD data and discuss the relation between the superconducting, magnetic, and structural properties of the 154SmFeAsO1-xDx and electron-doping-effect on it.

  19. Location of chlorhexidine in DMPC model membranes: a neutron diffraction study.

    PubMed

    Komljenović, Ivana; Marquardt, Drew; Harroun, Thad A; Sternin, Edward

    2010-06-01

    Chlorhexidine (CHX) is an effective anti-bacterial agent whose mode of action is thought to be the disruption of the cell membrane. It is known to partition into phospholipid bilayers of aqueous model-membrane preparations. Neutron diffraction data taken at 36 degrees C on the location of CHX in phosphatidylcholine (PC) bilayers is presented. The center of mass of the deuterated hydrocarbon chain of CHX is found to reside 16A from the center of the bilayer in 1,2-dimyristoyl-sn-glycero-3-phosphatidylcholine (14:0-14:0PC). This places the drug near the glycerol backbone of the lipid, and suggests a mode of action whereby the molecule is bent in half and inserts wedge-like into the lipid matrix. This mechanism is distinct from detergent-like mechanisms of membrane disruption and more similar to some anti-microbial peptide action, where peptides insert obliquely into the bilayer headgroup region to disrupt its structure. PMID:20359468

  20. High-temperature single-crystal neutron diffraction study of natural chondrodite

    NASA Astrophysics Data System (ADS)

    Kunz, Martin; Lager, George A.; Bürgi, Hans-Beat; Fernandez-Diaz, Maria Teresa

    2006-03-01

    The H-atom environment in a Tilly Foster chondrodite was analyzed using single-crystal neutron-diffraction data collected at 500, 700 and 900 K and previously published low temperature data collected at 10, 100 and 300 K on the same crystal (Mg4.64Fe0.28Mn0.014Ti0.023(Si1.01O4)2F1.16(OH)0.84; Friedrich et al. in Am Mineral 86:981-989, 2001). The full mean square displacement matrix Σ of the O-H pair was determined from the temperature dependence of the anisotropic displacement parameters, enabling a proper correction of the O-H bond for thermal vibration without assumptions about the correlation of O and H movements. The results show that the perpendicular O-H motions in chondrodite are intermediate between the riding and the independent motion models. The corrected O-H bond lengths do not change with temperature whereas the corrected H···F distances show an increase of ~0.02 Å with temperature, as do the Mg-O distances. This result shows that spectroscopic observations on the strength of the covalent O-H bond cannot be interpreted unambiguously in terms of a corresponding behaviour of the associated H···O/F hydrogen bond.

  1. Neutron diffraction study of the magnetic structure of Na2 RuO 4

    NASA Astrophysics Data System (ADS)

    Mogare, K. M.; Sheptyakov, D. V.; Bircher, R.; Güdel, H.-U.; Jansen, M.

    2006-08-01

    Nuclear and magnetic structures of sodium ruthenate (VI) have been studied by neutron powder diffraction in the temperature range 1.5 200 K. Na2RuO4 crystallizes in the monoclinic structure, with space group P 21/c. The structure consists of apical corner sharing RuO5 trigonal bipyramids forming infinite chains running along the b axis. These infinite [ RuO3O2/2] chains form a pseudo hexagonal close packing of rods with Ru Ru distances of 3.51 Å within the chains and 5.30 5.47 Å between the chains. At TN=37.2 K a magnetic transition leads to an antiferromagnetic state. The Ru6+ magnetic moments are ordered antiferromagnetically along the chains (b-axis), while the inter-chain interaction is ferromagnetic. A classical infinite chain model was fitted to the magnetic susceptibility data in order to estimate the strength of the nearest-neighbor exchange interactions along and between the chains, resulting in an intrachain coupling parameter of 2J=-86 K, and an interchain parameter J⊥ with \\vert 2J⊥ \\vert = 3 K.

  2. Determination of the location of hydrogen in the CuTi amorphous alloys by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Rodmacq, B.; Billard, L.; Chamberod, A.; Mangin, Ph.

    1986-02-01

    Neutron diffraction experiments have been performed on hydrogenated and deuterated Cu xTi 1- x amorphous alloys ( x = 0.67, 0.50, 0.35). The evolution of the interference functions as a function of hydrogen and deuterium concentration has shown that the hydrogen atoms have no copper atoms as first neighbours but are surrounded only by titanium atoms. The metal-hydrogen first distances compare well to those found in the corresponding crystalline hydrides. A model for the Cu 50Ti 50 amorphous alloy has been built up. The introduction of hydrogen or deuterium atoms in Ti 4 tetrahedra leads to calculated pair correlation functions very close to the experimental ones. Finally, the thermal evolution of CuTiH and CuTiD samples as been studied. Increasing the temperature leads to the precipitation of TiH 2 particles in the amorphous matrix. This is followed by the crystallization of the matrix and by the desorption of hydrogen at still higher temperature.

  3. Verification of residual stresses in flash-butt-weld rails using neutron diffraction

    NASA Astrophysics Data System (ADS)

    Tawfik, David; Kirstein, Oliver; Mutton, Peter John; Chiu, Wing Kong

    2006-11-01

    Residual stresses developed during flash-butt welding may play a crucial role in prolonging the fatigue life of the welded tracks under service loading conditions. The finished welds typically exhibit high levels of tensile residual stresses in the web region of the weld. Moreover, the surface condition of the web may contain shear drag or other defects resulting from the shearing process which may lead to the initiation and propagation of fatigue cracks in a horizontal split web failure mode under high axle loads. However, a comprehensive understanding into the residual stress behaviour throughout the complex weld geometry remains unclear and is considered necessary to establish the correct localised post-weld heat treatment modifications intended to lower tensile residual stresses. This investigation used the neutron diffraction technique to analyse residual stresses in an AS60 flash-butt-welded rail cooled under normal operating conditions. The findings will ultimately contribute to developing modifications to the flash-butt-welding procedure to lower tensile residual stresses which may then improve rail performance under high axle load.

  4. Distribution of Drug Molecules in Lipid Membranes: Neutron Diffraction and MD Simulations.

    NASA Astrophysics Data System (ADS)

    Boggara, Mohan; Mihailescu, Ella; Krishnamoorti, Ramanan

    2009-03-01

    Non-steroidal anti-inflammatory drugs (NSAIDs) e.g. Aspirin and Ibuprofen, with chronic usage cause gastro intestinal (GI) toxicity. It has been shown experimentally that NSAIDs pre-associated with phospholipids reduce the GI toxicity and also increase the therapeutic activity of these drugs compared to the unmodified ones. In this study, using neutron diffraction, the DOPC lipid bilayer structure (with and without drug) as well as the distribution of a model NSAID (Ibuprofen) as a function of its position along the membrane normal was obtained at sub-nanometer resolution. It was found that the bilayer thickness reduces as the drug is added. Further, the results are successfully compared with atomistic Molecular Dynamics simulations. Based on this successful comparison and motivated by atomic details from MD, quasi-molecular modeling of the lipid membrane is being carried out and will be presented. The above study is expected to provide an effective methodology to design drug delivery nanoparticles based on a variety of soft condensed matter such as lipids or polymers.

  5. Residual stress measurements in forced convective quenched steel bars by means of neutron diffraction

    SciTech Connect

    Hernandez-Morales, B.; Hawbolt, B.E.; Brimacombe, J.K.

    1996-12-31

    The residual stress distributions in 38.1 mm-dia., forced convective quenched bars of interstitial-free (IF), 1045 carbon, and alloyed steels were determined by neutron diffraction. The IF and 1045 carbon steel quenched bars exhibited compressive axial and circumferential (hoop) residual stresses near the surface and tensile values at the center. The radial residual stresses were tensile at all radial positions, decreasing towards zero near the surface. In contrast, the measured axial and circumferential components of the residual stress tensor in the alloyed eutectoid steel quenched bar were tensile near the surface and decreased to compressive values at the center. The radial component showed a maximum compressive value at the center and approached zero close to the surface. Metallographic analysis and hardness testing of the three steel specimens, revealed that the IF steel had transformed completely to ferrite, while the 1045 carbon steel bar transformed to martensite near the surface and a mixture of pearlite, ferrite and martensite at the center. On the other hand, the alloyed eutectoid steel specimen transformed entirely to martensite with small amounts of bainite near the center of the rod. The observed differences in the residual stress distributions in the three steels were explained based on the sequence of phase transformations that took place during quenching.

  6. A Powder Neutron Diffraction Study of Structure and Magnetism in NiCr 2S 4

    NASA Astrophysics Data System (ADS)

    Powell, Anthony V.; Colgan, Douglas C.; Ritter, Clemens

    1997-11-01

    Powder neutron diffraction data for NiCr 2S 4have been collected over the temperature range 1.8≤ T≤286 K. The Cr 3S 4structure (space group I2/ m) is adopted at all temperatures. Refinement of 286 K data ( a=5.8954(14) Å, b=3.4066(8) Å, c=11.0589(22) Å, β=91.362(4)°) demonstrates that the distribution of nickel and chromium cations between sites in a fully occupied metal layer and sites in an ordered vacancy layer is close to that expected for the normal structure type. Data collected at 1.8 K ( a=5.8621(5) Å, b=3.4051(2) Å, c=11.0297(9) Å, β=91.607(6)°) reveal the presence of long-range magnetic order, involving a doubling of the unit cell in both the aand cdirections. Cations in the fully occupied metal layer possess an ordered magnetic moment of 1.57(6) μBwhich is directed parallel to the cation layers. Cations in the vacancy layer have a moment of 1.36(8) μBwhich is directed toward the anion layers. The magnetic ordering temperature was determined as 180(5) K. These results are correlated with magnetic susceptibility and electrical conductivity data.

  7. Advanced sample environments for in situ neutron diffraction studies of nuclear materials

    NASA Astrophysics Data System (ADS)

    Reiche, Helmut Matthias

    Generation IV nuclear reactor concepts, such as the supercritical-water-cooled nuclear reactor (SCWR), are actively researched internationally. Operating conditions above the critical point of water (374°C, 22.1 MPa) and fuel core temperature that potentially exceed 1850°C put a high demand on the surrounding materials. For their safe application, it is essential to characterize and understand the material properties on an atomic scale such as crystal structure and grain orientation (texture) changes as a function of temperature and stress. This permits the refinement of models predicting the macroscopic behavior of the material. Neutron diffraction is a powerful tool in characterizing such crystallographic properties due to their deep penetration depth into condensed matter. This leads to the ability to study bulk material properties, as opposed to surface effects, and allows for complex sample environments to study e.g. the individual contributions of thermo-mechanical processing steps during manufacturing, operating or accident scenarios. I present three sample environments for in situ neutron diffraction studies that provide such crystallographic information and have been successfully commissioned and integrated into the user program of the High Pressure -- Preferred Orientation (HIPPO) diffractometer at the Los Alamos Neutron Science Center (LANSCE) user facility. I adapted a sample changer for reliable and fast automated texture measurements of multiple specimens. I built a creep furnace combining a 2700 N load frame with a resistive vanadium furnace, capable of temperatures up to 1000°C, and manipulated by a pair of synchronized rotation stages. This combination allows following deformation and temperature dependent texture and strain evolutions in situ. Utilizing the presented sample changer and creep furnace we studied pressure tubes made of Zr-2.5wt%Nb currently employed in CANDURTM nuclear reactors and proposed for future SCWRs, acting as the primary

  8. Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction.

    PubMed

    Binns, Jack; Kamenev, Konstantin V; McIntyre, Garry J; Moggach, Stephen A; Parsons, Simon

    2016-05-01

    The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions. PMID:27158503

  9. Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction

    PubMed Central

    Binns, Jack; Kamenev, Konstantin V.; McIntyre, Garry J.; Moggach, Stephen A.; Parsons, Simon

    2016-01-01

    The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions. PMID:27158503

  10. High pressure neutron diffraction to beyond 20 GPa and below 1.8 K using Paris-Edinburgh load frames

    NASA Astrophysics Data System (ADS)

    Klotz, S.; Strässle, Th.; Lebert, B.; d'Astuto, M.; Hansen, Th.

    2016-01-01

    We describe a method for collecting neutron diffraction patterns simultaneously at high pressure (>22 GPa) and low temperature (<1.8 K). The system uses ∼5-10 mm3 samples compressed by double-toroidal sintered diamond anvils, with the required forces generated by a Paris-Edinburgh press of 30 kg mass. Technical details are given and diffraction data of ε-iron at 22.6 GPa and 1.79 K are presented.

  11. Effect of microstructure anisotropy on the deformation of MAX polycrystals studied by in-situ compression combined with neutron diffraction

    SciTech Connect

    Guitton, A.; Joulain, A.; Thilly, L.; Van Petegem, S.; Tromas, C.; Van Swygenhoven, H.

    2014-06-16

    In situ compression tests combined with neutron diffraction were performed on Ti{sub 2}AlN MAX polycrystals with lamellar anisotropic microstructure: the diffraction peak evolution (position and profile) with applied stress reveals that lamellar grains parallel to compression axis remain elastic while lamellar grains perpendicular to compression plastify, both families being subjected to strong variations of heterogeneous strains (types II and III). We demonstrate that this behavior originates from the complex response of the very anisotropic lamellar microstructure and explains the observation of reversible hysteretic loops when cycling MAX polycrystals even in the elastic regime.

  12. Neutron diffraction study of Bi doped cubic spinel Co{sub 2}MnO{sub 4}

    SciTech Connect

    Rajeevan, N. E.; Kaushik, S. D.; Kumar, Ravi

    2015-06-24

    Polycrystalline Bi doped spinel Bi{sub x}Co{sub 2-x}MnO{sub 4} compounds were prepared by solid state reaction route. Room temperature neutron diffraction study reveals that all the compounds are formed in cubic phase and there is no change in the crystal structure due to Bi doping and the compound has cubic structure with Fd-3m space group. Cell parameter found to increase with respect to Bi doping and ferrimagnetic nature is established through magnetization. Low temperature neutron diffraction is carried out and emphasis the ferrimagnetic ordering in the samples of Bi{sub x}Co{sub 2-x}MnO{sub 4} series.

  13. Long-range magnetic ordering in Ba{sub 2}CoS{sub 3}: A neutron diffraction study

    SciTech Connect

    Headspith, D.A.; Battle, P.D.; Francesconi, M.G.

    2007-10-15

    Neutron powder diffraction has been used to determine the magnetic structure of the quasi-one-dimensional compound Ba{sub 2}CoS{sub 3}, which contains linear [001] chains of vertex-sharing CoS{sub 4} tetrahedra, spaced apart by Ba{sup 2+} cations. At 1.5 K the Co{sup 2+} cations in the chains are antiferromagnetically ordered with an ordered magnetic moment of 1.97(4) {mu}{sub B} per cation aligned along [100]. Each Co{sup 2+} cation is ferromagnetically aligned with four cation in neighbouring chains and antiferromagnetically aligned with two others. - Graphical abstract: Neutron powder diffraction has been used to prove that Ba{sub 2}CoS{sub 3} shows long-range antiferromagnetic order at low temperatures, despite the quasi-one-dimensional arrangement of the CoS{sub 4} tetrahedra in the crystal structure.

  14. Neutron and electron diffraction studies of La(Zn1/2Ti1/2)O3 perovskite.

    PubMed

    Ubic, Rick; Hu, Yi; Abrahams, Isaac

    2006-08-01

    The crystallography and microwave dielectric properties of La(Zn(1/2)Ti(1/2))O(3) (LZT) ceramics prepared via the mixed-oxide route were investigated in this study. While samples were largely single phase, small amounts of ZnO impurity were detected in sintered pellets. Observed reflections in electron and neutron diffraction patterns indicate that the symmetry of LZT is P2(1)/n. The B site is ordered on {110} or pseudocubic {111}, but the presence of the pseudocubic 1/2(111) reflection is in itself insufficient to indicate the existence of such order. Rietveld refinements of the neutron diffraction data yield an excellent fit for such a model. The structure is highly twinned, with variants related through common {211} composition planes and 90 degrees rotations about <011>. The microwave dielectric properties measured were epsilon(r) = 34, Qf = 36,090 and tau(f) = -70 MK(-1). PMID:16840801

  15. Neutron diffraction and electrical transport studies on the incommensurate magnetic phase transition in holmium at high pressures

    SciTech Connect

    Thomas, Sarah; Uhoya, Walter; Tsoi, Georgiy; Wenger, Lowell E; Vohra, Yogesh; Chesnut, Gary Neal; Weir, S. T.; Tulk, Christopher A; Moreira Dos Santos, Antonio F

    2012-01-01

    Neutron diffraction and electrical transport measurements have been made on the heavy rare earth metal holmium at high pressures and low temperatures in order to elucidate its transition from a paramagnetic (PM) to a helical antiferromagnetic (AFM) ordered phase as a function of pressure. The electrical resistance measurements show a change in the resistance slope as the temperature is lowered through the antiferromagnetic Neel temperature. The temperature of this antiferromagnetic transition decreases from approximately 122 K at ambient pressure at a rate of -4.9 K GPa(-1) up to a pressure of 9 GPa, whereupon the PM-to-AFM transition vanishes for higher pressures. Neutron diffraction measurements as a function of pressure at 89 and 110 K confirm the incommensurate nature of the phase transition associated with the antiferromagnetic ordering of the magnetic moments in a helical arrangement and that the ordering occurs at similar pressures as determined from the resistance results for these temperatures.

  16. Neutron diffraction study on the two-dimensional Ising system KEr(MoO{sub 4}){sub 2}

    SciTech Connect

    Mat'as, Slavomir; Dudzik, Esther; Feyerherm, Ralf; Gerischer, Sebastian; Klemke, Sebastian; Prokes, Karel; Orendacova, Alzbeta

    2010-11-01

    The magnetic properties of the two-dimensional Ising antiferromagnet KEr(MoO{sub 4}){sub 2} have been investigated below and above transition temperature T{sub N}{approx}0.95 K in zero field and in fields up to 6.5 T by means of elastic neutron-diffraction, heat-capacity, and magnetization measurements. The low-temperature signal recorded at 0.34 K by neutron diffraction is explained within a noncollinear magnetic structure model. However, additional contribution is also present when applying the external magnetic field along the c axis even at temperatures well above the magnetic transition temperature T{sub N}. Various explanations are discussed.

  17. High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal-organic framework material HKUST-1

    NASA Astrophysics Data System (ADS)

    Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I. F.; Millange, Franck; Walton, Richard I.

    2013-12-01

    We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal-organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal-organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host.

  18. Neutron Diffraction Residual Strain Tensor Measurements Within The Phase IA Weld Mock-up Plate P-5

    SciTech Connect

    Hubbard, Camden R

    2011-09-01

    Oak Ridge National Laboratory (ORNL) has worked with NRC and EPRI to apply neutron and X-ray diffraction methods to characterize the residual stresses in a number of dissimilar metal weld mockups and samples. The design of the Phase IA specimens aimed to enable stress measurements by several methods and computational modeling of the weld residual stresses. The partial groove in the 304L stainless steel plate was filled with weld beads of Alloy 82. A summary of the weld conditions for each plate is provided in Table 1. The plates were constrained along the long edges during and after welding by bolts with spring-loaded washers attached to the 1-inch thick Al backing plate. The purpose was to avoid stress relief due to bending of the welded stainless steel plate. The neutron diffraction method was one of the methods selected by EPRI for non-destructive through thickness strain and stress measurement. Four different plates (P-3 to P-6) were studied by neutron diffraction strain mapping, representing four different welding conditions. Through thickness neutron diffraction strain mappings at NRSF2 for the four plates and associated strain-free d-zero specimens involved measurement along seven lines across the weld and at six to seven depths. The mountings of each plate for neutron diffraction measurements were such that the diffraction vector was parallel to each of the three primary orthogonal directions of the plate: two in-plane directions, longitudinal and transverse, and the direction normal to the plate (shown in left figure within Table 1). From the three orthogonal strains for each location, the residual stresses along the three plate directions were calculated. The principal axes of the strain and stress tensors, however, need not necessarily align with the plate coordinate system. To explore this, plate P-5 was selected for examination of the possibility that the principal axes of strain are not along the sample coordinate system axes. If adequate data could

  19. Baromagnetic Effect in Antiperovskite Mn3 Ga0.95 N0.94 by Neutron Powder Diffraction Analysis.

    PubMed

    Shi, Kewen; Sun, Ying; Yan, Jun; Deng, Sihao; Wang, Lei; Wu, Hui; Hu, Pengwei; Lu, Huiqing; Malik, Muhammad Imran; Huang, Qingzhen; Wang, Cong

    2016-05-01

    A baromagnetic effect in a novel tetragonal magnetic structure is introduced by vacancies in Mn3 Ga0.95 N0.94 , due to the change of the Mn-Mn distance and their spin re-orientation induced by a pressure field. This effect is proven for the first time in antiperovskite compounds by neutron powder diffraction analysis. This feature will enable wide applications in magnetoelectric devices and intelligent instruments. PMID:27007214

  20. Fluid bilayer structure determination: Joint refinement in composition space using X-ray and neutron diffraction data

    SciTech Connect

    White, S.H.; Wiener, M.C.

    1994-12-31

    Experimentally-determined structural models of fluid lipid bilayers are essential for verifying molecular dynamics simulations of bilayers and for understanding the structural consequences of peptide interactions. The extreme thermal motion of bilayers precludes the possibility of atomic-level structural models. Defining {open_quote}the structure{close_quote} of a bilayer as the time-averaged transbilayer distribution of the water and the principal lipid structural groups such as the carbonyls and double-bonds (quasimolecular fragments), one can represent the bilayer structure as a sum of Gaussian functions referred to collectively as the quasimolecular structure. One method of determining the structure is by neutron diffraction combined with exhaustive specific deuteration. This method is impractical because of the expense of the chemical syntheses and the limited amount of neutron beam time currently available. We have therefore developed the composition space refinement method for combining X-ray and minimal neutron diffraction data to arrive at remarkably detailed and accurate structures of fluid bilayers. The composition space representation of the bilayer describes the probability of occupancy per unit length across the width of the bilayer of each quasimolecular component and permits the joint refinement of X-ray and neutron lamellar diffraction data by means of a single quasimolecular structure that is fitted simultaneously to both data sets. Scaling of each component by the appropriate neutron or X-ray scattering length maps the composition-space profile to the appropriate scattering length space for comparison to experimental data. The difficulty with the method is that fluid bilayer structures are generally only marginally determined by the experimental data. This means that the space of possible solutions must be extensively explored in conjunction with a thorough analysis of errors.

  1. Observation of long-range magnetic ordering in pyrohafnate Nd2Hf2O7 : A neutron diffraction study

    NASA Astrophysics Data System (ADS)

    Anand, V. K.; Bera, A. K.; Xu, J.; Herrmannsdörfer, T.; Ritter, C.; Lake, B.

    2015-11-01

    We have investigated the physical properties of a pyrochlore hafnate Nd2Hf2O7 using ac magnetic susceptibility χac(T ) , dc magnetic susceptibility χ (T ) , isothermal magnetization M (H ) , and heat capacity Cp(T ) measurements, and determined the magnetic ground state by neutron powder diffraction. An upturn is observed below 6 K in Cp(T ) /T , however both Cp(T ) and χ (T ) do not show any clear anomaly down to 2 K. The χac(T ) shows a well-pronounced anomaly indicating an antiferromagnetic transition at TN=0.55 K. The long-range antiferromagnetic ordering is confirmed by neutron diffraction. The refinement of the neutron diffraction pattern reveals an all-in/all-out antiferromagnetic structure, where for successive tetrahedra the four Nd3 + magnetic moments point alternatively all-into or all-out-of the tetrahedron, with an ordering wave vector k = (0, 0, 0) and an ordered state magnetic moment of m =0.62 (1 ) μB /Nd at 0.1 K. The ordered moment is strongly reduced, reflecting strong quantum fluctuations in ordered state.

  2. Quasi-steady state principle and in-situ real-time investigation of transient strains in 6061-T6 Al alloy using neutron diffraction

    SciTech Connect

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

    2007-01-01

    Neutron diffraction research has been limited to the "static" behavior of materials since the number of collected neutrons is insufficient to reach the adequate neutron counts in rapid changes of material state. In order to achieve the desired precision for the study of the transient material behavior, we propose an in-situ neutron-diffraction measurement method based on the quasi-steady state (QSS) phenomenon. The QSS principle was applied for the measurement of transient lattice spacing changes in a 6061-T6 aluminum alloy plate during thermo-mechanical processing.

  3. Elucidating High Field Phases of the Multiferroic MnWO4 with a Pulsed Magnetic Field and Time of Flight Neutron Laue Diffraction

    SciTech Connect

    Nojiri, H; Yoshii, Shunsuke; Yasui, Motoyoshi; Okada, Kyoko; Matsuda, M.; Santodonato, Louis J; Granroth, Garrett E; Ross, Kathyrn; Carlo, Jeremy P; Gaulin, Bruce D.

    2011-01-01

    We have combined time-of-flight neutron Laue diffraction and pulsed high magnetic fields at the Spallation Neutron Source to study the phase diagram of the multiferroic material MnWO4. The control of the field-pulse timing enabled an exploration of magnetic Bragg scattering through the time dependence of both the neutron wavelength and the pulsed magnetic field. This allowed us to observe several magnetic Bragg peaks in different field-induced phases of MnWO4 with a single instrument configuration. These phases were not previously amenable to neutron diffraction studies due to the large fields involved.

  4. Investigation of an unusual low-temperature phase transformation in RbBH{sub 4} by neutron diffraction

    SciTech Connect

    Kitchen, Brian B.; Verdal, Nina; Udovic, Terrence J.; Rush, John J.; Hartman, Michael R.; DeVries, Daniel J.

    2013-07-15

    To investigate the previously reported low-temperature phase transition in rubidium borohydride (RbBH{sub 4}) near 48.5 K, we carried out neutron powder diffraction and vibrational spectroscopy measurements both above and below this temperature on an isotopically-enriched sample of Rb{sup 11}BD{sub 4}. Our diffraction data reflected an average cubic Fm3{sup ¯}m structure with BD{sub 4}{sup −} anion orientational disorder at all temperatures, with no hint of extra Bragg peaks due to long-range orientational order below the transition temperature as reported by others. These structural results and careful analysis of torsional vibrations in RbBD{sub 4} corroborate the results of prior neutron vibrational spectroscopy measurements suggesting that the low-temperature RbBH{sub 4} structure indeed possesses some orientational ordering of the BH{sub 4}{sup −} anions, but of a shorter-ranged nature insensitive to powder diffraction methods. - The neutron powder diffraction pattern of RbBD{sub 4} below the phase transition temperature (shown here in black) is indistinguishable from that collected above the phase transition temperature. The inset depicts the cubic structure that fits the data at both temperatures. - Highlights: • We investigated the nature of the RbBD{sub 4} phase transition using NVS and NPD. • A change in shape of the RbBD{sub 4} torsion mode was observed across the transition. • The RbBD{sub 4} diffraction pattern across this phase transition was unchanged. • The phase transition in RbBD{sub 4} appears to produce only short-range ordering of BD{sub 4}{sup −}.

  5. Neutron Diffraction Study Oxygen Dissolution Alpha(sub 2)-Ti3Al

    NASA Technical Reports Server (NTRS)

    Jones, Camille Y.; Luecke, William E.; Copland, Evan

    2005-01-01

    Rietveld refinements of neutron powder diffraction data on alpha(sub 2)-Ti3Al have been performed to determine the crystal structure as a function of interstitial oxygen (O) concentration for three alloys with a Ti/Al ratio of approximately equal to 2.34 and O concentrations of 0.25%, 3.99% and 7.71%. The structures of the allows are hexagonal in space group P6(sub 3)/mmc where Ti and Al atoms populate unique sites with excess Al at the Ti site and O atoms occupy octahedral interstitial sites surrounded by six Ti sites. The length of the c-axis was found to increase linearly as the O occupancy of the interstitial sites increased; this lattice lengthening effect was much less pronounced along the alpha axis. Correspondingly, the increases in the lengths of Ti-Al and Ti-Ti bonds with a major component of their direction parallel to the c-axis were roughly an order of magnitude greater than the increases in the lengths of Ti-al and Ti-Ti bonds more closely aligned with the alpha-axis. Densities calculated form the lattice parameters and occupancy factors fall in the range (4.118 plus or minus 0.004) grams per cubic centimeter to (4.194 plus or minus 0.004) grams per cubic centimeter, and exhibit a nearly linear increase with oxygen concentration. Measured densities of (4.113 plus or minus 0.001) grams per cubic centimeter, (4.146 plus or minus 0.009) grams per cubic centimeter, and (4.191 plus or minus 0.002) grams per cubic centimeter for these alloys agree with the results of the refinements.

  6. Oxygen transport pathways in Ruddlesden–Popper structured oxides revealed via in situ neutron diffraction

    DOE PAGESBeta

    Tomkiewicz, Alex C.; Tamimi, Mazin; Huq, Ashfia; McIntosh, Steven

    2015-09-21

    Ruddlesden-Popper structured oxides, general form An+1BnO3n+1, consist of n-layers of the perovskite structure stacked in between rock-salt layers, and have potential application in solid oxide electrochemical cells and ion transport membrane reactors. Three materials with constant Co/Fe ratio, LaSrCo0.5Fe0.5O4-δ (n = 1), La0.3Sr2.7CoFeO7-δ (n = 2), and LaSr3Co1.5Fe1.5O10-δ (n = 3) were synthesized and studied via in situ neutron powder diffraction between 765 K and 1070 K at a pO2 of 10-1 atm. Then, the structures were fit to a tetragonal I4/mmm space group, and were found to have increased total oxygen vacancy concentration in the order La0.3Sr2.7CoFeO7-δ > LaSr3Co1.5Fe1.5O10-δmore » > LaSrCo0.5Fe0.5O4-δ, following the trend predicted for charge compensation upon increasing Sr2+/La3+ ratio. The oxygen vacancies within the material were almost exclusively located within the perovskite layers for all of the crystal structures with only minimal vacancy formation in the rock-salt layer. Finally, analysis of the concentration of these vacancies at each distinct crystallographic site and the anisotropic atomic displacement parameters for the oxygen sites reveals potential preferred oxygen transport pathways through the perovskite layers.« less

  7. High-temperature structural phase transitions in neighborite: a high-resolution neutron powder diffraction investigation

    NASA Astrophysics Data System (ADS)

    Knight, Kevin S.; Price, G. David; Stuart, John A.; Wood, Ian G.

    2015-01-01

    The nature of the apparently continuous structural phase transition at 1,049 K in the perovskite-structured, MgSiO3 isomorph, neighborite (NaMgF3), from the orthorhombic ( Pbnm) hettotype phase to the cubic () aristotype structure, has been re-investigated using high-resolution, time-of-flight neutron powder diffraction. Using data collected at 1 K intervals close to the nominal phase transition temperature, the temperature dependence of the intensities of superlattice reflections at the M point and the R point of the pseudocubic Brillouin zone indicate the existence of a new intermediate tetragonal phase in space group P4/ mbm, with a narrow phase field extending from ~1,046.5 to ~1,048.5 K, at ambient pressure. Group theoretical analysis shows that the structural transitions identified in this study, Pbnm- P4/ mbm, and P4/ mbm-, are permitted to be second order. The observation of the tetragonal phase resolves the longstanding issue of why the high-temperature phase transition, previously identified as Pbnm-, and which would be expected to be first order under Landau theory, is in fact found to be continuous. Analysis of the pseudocubic shear strain shows it to vary with a critical exponent of 0.5 implying that the phase transition from Pbnm to P4/ mbm is tricritical in character. The large librational modes that exist in the MgF6 octahedron at high temperature, and the use of Gaussian probability density functions to describe atomic displacements, result in apparent bond shortening in the Mg-F distances, making mode amplitude determination an unreliable method for determination of the critical exponent from internal coordinates. Crystal structures are reported for the three phases of NaMgF3 at 1,033 K ( Pbnm), 1,047 K ( P4/ mbm) and 1,049 K ().

  8. Neutron Diffraction of Aqueous Tetramethylammonium Chloride (TMA) Solutions and TMA Intercalated Swelling Clays Under Burial Conditions

    NASA Astrophysics Data System (ADS)

    Patel, R.; Howard, C. A.; Greenwell, C.; Youngs, T.; Soper, A. K.; Skipper, N. T.

    2014-12-01

    There is a need for the improvement and optimisation of clay swelling inhibitors for the enhancement of oil and gas exploration. The hydration region of both ions and the possibility of ion pairing in 1 molar aqueous solution of clay swelling inhibitor, tetramethylammonium chloride (TMACl), in D2O, under elevated hydrostatic-pressures and temperatures has been determined with unprecedented detail using a combination of neutron diffraction and small-angle scattering in conjunction with hydrogen/deuterium isotopic labeling. The O-H correlation function (H-bonds) for the water in the 1.0M solution is measured and compared with that for pure D2O. Also investigated is the effect of burial conditions on the d-spacing of TMA-intercalated vermiculite. Contrary to expectations, no aggregation of TMA ions due to hydrophobic interactions is observed, nor are any ionic pairs of TMA+ and Cl- at these burial conditions. The data revealed a more ordered water-water structure with the addition of TMACl from bulk D2O. There is no change in the hydration structure measured at the applied elevated conditions. This is in remarkable contrast to pure water at the same conditions which is well known to be compressible. The dry d-spacing of the TMA-exchanged Eucatex vermiculite is measured at 13.66 Å which increases to 14.03 Å with the addition of D2O. Beyond this, there is no change in d-spacing with increasing pressure and temperature indicating the strength of the TMA ions binding to the clay interlayers and therefore its performance as a clay-swelling inhibitor.

  9. Structure and Dynamics of Cholesterol-Containing Polyunsaturated Lipid Membranes Studied by Neutron Diffraction and NMR

    PubMed Central

    Mihailescu, Mihaela; Soubias, Olivier; Worcester, David; White, Stephen H.

    2010-01-01

    A direct and quantitative analysis of the internal structure and dynamics of a polyunsaturated lipid bilayer composed of 1-stearoyl-2-docosahexaenoyl-sn-glycero-3-phosphocholine (18:0-22:6n3-PC) containing 29 mol% cholesterol was carried out by neutron diffraction, 2H-NMR and 13C-MAS NMR. Scattering length distribution functions of cholesterol segments as well as of the sn-1 and sn-2 hydrocarbon chains of 18:0-22:6n3-PC were obtained by conducting experiments with specifically deuterated cholesterol and lipids. Cholesterol orients parallel to the phospholipids, with the A-ring near the lipid glycerol and the terminal methyl groups 3 Å away from the bilayer center. Previously, we reported that the density of polyunsaturated docosahexaenoic acid (DHA, 22:6n3) chains was higher near the lipid–water interface. Addition of cholesterol partially redistributes DHA density from near the lipid–water interface to the center of the hydrocarbon region. Cholesterol raises chain-order parameters of both stearic acid and DHA chains. The fractional order increase for stearic acid methylene carbons C8–C18 is larger, reflecting the redistribution of DHA chain density toward the bilayer center. The correlation times of DHA chain isomerization are short and mostly unperturbed by the presence of cholesterol. The uneven distribution of saturated and polyunsaturated chain densities and the cholesterol-induced balancing of chain distributions may have important implications for the function and integrity of membrane receptors, such as rhodopsin. PMID:21161517

  10. Neutron diffraction study of the beta' and gamma phases of LiFeO{sub 2}

    SciTech Connect

    Barre, Maud; Catti, Michele

    2009-09-15

    The beta, beta', gamma and alpha phases of LiFeO{sub 2}, synthesized as powders, were annealed at different temperatures and characterized by X-ray measurements. The beta' and gamma modifications were also studied by time-of-flight neutron diffraction (ISIS Facility, UK). The structure of the beta' phase was refined in the monoclinic C2/c space group (a=8.566(1), b=11.574(2), c=5.1970(5) A, beta=146.064(5){sup o}) to wR{sub p}=0.071-0.080 (data from four counter banks). Fe and Li atoms are ordered over two of the four independent sites, and partially disordered over the other two. The ordered Li has a distorted tetrahedral coordination. The gamma structure was refined at RT (a=4.047(1), c=8.746(2) A) and at 570 deg. C (a=4.082(3), c=8.822(6) A) in the I4{sub 1}/amd symmetry, showing full order with Li in octahedral coordination at RT, and in a split-atom configuration at high temperature. On annealing, the beta' polymorph was found to transform to gamma at 550 deg. C, thus suggesting that it is a metastable phase. Electrostatics is discussed as the driving force for the alpha->beta'->gamma ordering process of LiFeO{sub 2}. - Graphical abstract: Crystal structure of beta'-LiFeO{sub 2} (monoclinic C2/c). Lithium and iron atoms are both ordered (blue and yellow balls) and partially disordered (green balls) over four independent sites. The beta' phase transforms to fully ordered gamma (tetragonal I4{sub 1}/amd) at 550 deg. C.

  11. Operando Lithium Dynamics in the Li-Rich Layered Oxide Cathode Material via Neutron Diffraction

    DOE PAGESBeta

    Liu, Haodong; An, Ke; Venkatachalam, Subramanian; Qian, Danna; Zhang, Minghao; Meng, Ying Shirley

    2016-04-06

    Neutron diffraction under operando battery cycling is used to study the lithium and oxygen dynamics of high Li-rich Li(Lix/3Ni(3/8-3x/8)Co(1/4-x/4)Mn(3/8+7x/24)O2 (x = 0.6, HLR) and low Li-rich Li(Lix/3Ni(1/3-x/3)Co(1/3-x/3)Mn(1/3+x/3)O2 (x = 0.24, LLR) compounds that exhibit different degrees of oxygen activation at high voltage. The measured lattice parameter changes and oxygen position show largely contrasting changes for the two cathodes where the LLR exhibits larger movement of oxygen and lattice contractions in comparison to the HLR that maintains relatively constant lattice parameters and oxygen position during the high voltage plateau until the end of charge. Density functional theory calculations show the presencemore » of oxygen vacancy during the high voltage plateau; changes in the lattice parameters and oxygen position are consistent with experimental observations. Lithium migration kinetics for the Li-rich material is observed under operando conditions for the first time to reveal the rate of lithium extraction from the lithium layer, and transition metal layer is related to the different charge and discharge characteristics. At the beginning of charging, the lithium extraction predominately occurs within the lithium layer. The lithium extraction from the lithium layer slows down and extraction from the transition metal layer evolves at a faster rate once the high voltage plateau is reached.« less

  12. X-ray and neutron diffraction measurements of dislocation density and subgrain size in a friction stir welded aluminum alloy

    SciTech Connect

    Claussen, Bjorn; Woo, Wanchuck; Zhili, Feng; Edward, Kenik; Ungar, Tamas

    2009-01-01

    The dislocation density and subgrain size were determined in the base material and friction-stir welds of 6061-T6 aluminum alloy. High-resolution X-ray diffraction measurement was performed in the base material. The result of the line profile analysis of the X-ray diffraction peak shows that the dislocation density is about 4.5 x 10{sup 14} m{sup 02} and the subgrain size is about 200 nm. Meanwhile, neutron diffraction measurements have been performed to observe the diffraction peaks during friction-stir welding (FSW). The deep penetration capability of the neutron enables us to measure the peaks from the midplane of the Al plate underneath the tool shoulder of the friction-stir welds. The peak broadening analysis result using the Williamson-Hall method shows the dislocation density of about 3.2 x 10{sup 15} m{sup -2} and subgrain size of about 160 nm. The significant increase of the dislocation density is likely due to the severe plastic deformation during FSW. This study provides an insight into understanding the transient behavior of the microstructure under severe thermomechanical deformation.

  13. Spinel materials for Li-ion batteries: new insights obtained by operando neutron and synchrotron X-ray diffraction.

    PubMed

    Bianchini, Matteo; Fauth, François; Suard, Emmanuelle; Leriche, Jean Bernard; Masquelier, Christian; Croguennec, Laurence

    2015-12-01

    In the last few decades Li-ion batteries changed the way we store energy, becoming a key element of our everyday life. Their continuous improvement is tightly bound to the understanding of lithium (de)intercalation phenomena in electrode materials. Here we address the use of operando diffraction techniques to understand these mechanisms. We focus on powerful probes such as neutrons and synchrotron X-ray radiation, which have become increasingly familiar to the electrochemical community. After discussing the general benefits (and drawbacks) of these characterization techniques and the work of customization required to adapt standard electrochemical cells to an operando diffraction experiment, we highlight several very recent results. We concentrate on important electrode materials such as the spinels Li1 + xMn2 - xO4 (0 ≤ x ≤ 0.10) and LiNi0.4Mn1.6O4. Thorough investigations led by operando neutron powder diffraction demonstrated that neutrons are highly sensitive to structural parameters that cannot be captured by other means (for example, atomic Debye-Waller factors and lithium site occupancy). Synchrotron radiation X-ray powder diffraction reveals how LiMn2O4 is subject to irreversibility upon the first electrochemical cycle, resulting in severe Bragg peak broadening. Even more interestingly, we show for the first time an ordering scheme of the elusive composition Li0.5Mn2O4, through the coexistence of Mn(3+):Mn(4+) 1:3 cation ordering and lithium/vacancy ordering. More accurately written as Li0.5Mn(3+)0.5Mn(4+)1.5O4, this intermediate phase loses the Fd\\overline 3m symmetry, to be correctly described in the P213 space group. PMID:26634725

  14. High pressure behavior of phlogopite using neutron diffraction and first principle simulations

    NASA Astrophysics Data System (ADS)

    Chheda, T. D.; Mookherjee, M.; dos Santos, A. M.; Molaison, J.; Manthilake, G. M.; Chantel, J.; Mainprice, D.

    2013-12-01

    Hydrous phases play an important role in the deep water cycle by transporting water into the Earth's interior. Upon, reaching their thermodynamic stability, these hydrous phases decompose and release the water. A part of the water is cycled back to the arc, thus completing the deep water cycle, the remaining water is partitioned into dense hydrous phases and nominally anhydrous phases. Hence, in order to understand the role the hydrous phases in the deep water cycle, it is important to constrain the effect of pressure, temperature, and chemistry on the thermodynamic stability of the hydrous phases. In addition, it is important to constrain the elasticity of these hydrous phases to test whether they can explain the distinct geophysical observations such as lower bulk sound velocities and elastic anisotropy. Phlogopite is a potassium bearing mica that is stable in the hydrated crust and metasomatized mantle up to pressures of ~9 GPa, i.e., base of the upper mantle. We investigated the response of the crystal structure, lattice parameters and unit-cell volume of a natural phlogopite upon compression. We conducted in situ neutron diffraction studies at high-pressures using Paris-Edinburgh press at the Spallation Neutrons and Pressure Diffractometer (SNAP), Oak Ridge National Laboratory. All the experiments were conducted at room temperatures and pressures up to 10 GPa were explored. The equation of state parameters from our experiments could be explained by a finite strain formulation with V0= 487 Å3, K0 = 49 GPa, K' = 4.1. In addition, we have used first principle simulations based on density functional theory to calculate the equation of state and elasticity. The predicted equation of state is in good agreement with the experiments, with V0= 519 Å3, K0 = 45.8 GPa and K'= 6.9. The full elastic constant tensor shows significant anisotropy with the principal elastic constants at theoretical V0: C11= 181 GPa, C22= 185 GPa, C33= 62 GPa, the shear elastic constants- C44

  15. Oxygen transport pathways in Ruddlesden–Popper structured oxides revealed via in situ neutron diffraction

    SciTech Connect

    Tomkiewicz, Alex C.; Tamimi, Mazin; Huq, Ashfia; McIntosh, Steven

    2015-09-21

    Ruddlesden-Popper structured oxides, general form An+1BnO3n+1, consist of n-layers of the perovskite structure stacked in between rock-salt layers, and have potential application in solid oxide electrochemical cells and ion transport membrane reactors. Three materials with constant Co/Fe ratio, LaSrCo0.5Fe0.5O4-δ (n = 1), La0.3Sr2.7CoFeO7-δ (n = 2), and LaSr3Co1.5Fe1.5O10-δ (n = 3) were synthesized and studied via in situ neutron powder diffraction between 765 K and 1070 K at a pO2 of 10-1 atm. Then, the structures were fit to a tetragonal I4/mmm space group, and were found to have increased total oxygen vacancy concentration in the order La0.3Sr2.7CoFeO7-δ > LaSr3Co1.5Fe1.5O10-δ > LaSrCo0.5Fe0.5O4-δ, following the trend predicted for charge compensation upon increasing Sr2+/La3+ ratio. The oxygen vacancies within the material were almost exclusively located within the perovskite layers for all of the crystal structures with only minimal vacancy formation in the rock-salt layer. Finally, analysis of the concentration of these vacancies at each distinct crystallographic site and the anisotropic atomic displacement parameters for the oxygen sites reveals potential preferred oxygen transport pathways through the perovskite layers.

  16. Neutron diffraction analysis of transition metal hydrides: Terminal, bridging, and agostic interactions

    SciTech Connect

    Stevens, R.C.

    1988-01-01

    The High Flux Beam Reactor at Brookhaven National Laboratory located in Upton, New York, was used in all experiments described in this thesis. Two main types of problems were tackled with this technique: (i) the structures of transition metal hydrido complexes and (ii) the determination of the absolute configuration of chiral CHD groups generated via biochemical processes. Transition metal hydrido complexes have been studies extensively due to several reasons: (i) their potential for catalysis in organic synthetic reactions such as hydrogenation, hydroformulation, and olefin isomerization; (ii) their unconventional bonding mode in metal clusters; and (iii) their potential as hydrogen storage materials. Six transition metal hydride complexes have been studied in this work which fall into this category. The compounds studies include: (i) a transition metal dimer containing bridging hydrides, ((C{sub 5}(CH{sub 3}){sub 5}Ir){sub 2} ({mu}-H){sub 3}){sup +}(ClO{sub 4}){sup {minus}}2C{sub 6}H{sub 6}; (ii) compounds suspected to have agostic hydride interactions, (cis-IrH(OH)(PMe{sub 3}){sub 4}){sup +}(PF{sub 6}){sup {minus}}, Cp{sub 3}U = CHPMe{sup 3}, and (C{sub 5}Me{sub 5}){sub 2}Th({mu}-CH{sub 2})({mu}-1-3,4-Me{sub 2}C{sub 5}H{sub 2}) ZrMe(C{sub 5}H{sub 5}); (iii) a metal cluster containing face-bridging hydrogen atoms H{sub 6}Cu{sub 6}(P(p-toyl){sub 3}){sub 6}; and (iv) the complex HRh(P(C{sub 6}H{sub 5}){sub 3}){sub 4}, in which the shortest hydrogen-metal bond distance (1.31(8){angstrom}) was discovered. The appendix section is concerned with the powerful, yet presently under-utilized application of neutron diffraction in the determination of absolute configurations of molecules bearing chiral methylene groups. Here, the systems malate/succinate and acetaldehyde/alcohol have been studied and confirmed to be consistent with previous (non-crystallographic) studies.

  17. Hemoglobin redux: combining neutron and X-ray diffraction with mass spectrometry to analyse the quaternary state of oxidized hemoglobins

    SciTech Connect

    Mueser, Timothy C. Griffith, Wendell P.; Kovalevsky, Andrey Y.; Guo, Jingshu; Seaver, Sean; Langan, Paul; Hanson, B. Leif

    2010-11-01

    X-ray and neutron diffraction studies of cyanomethemoglobin are being used to evaluate the structural waters within the dimer–dimer interface involved in quaternary-state transitions. Improvements in neutron diffraction instrumentation are affording the opportunity to re-examine the structures of vertebrate hemoglobins and to interrogate proton and solvent position changes between the different quaternary states of the protein. For hemoglobins of unknown primary sequence, structural studies of cyanomethemoglobin (CNmetHb) are being used to help to resolve sequence ambiguity in the mass spectra. These studies have also provided additional structural evidence for the involvement of oxidized hemoglobin in the process of erythrocyte senescence. X-ray crystal studies of Tibetan snow leopard CNmetHb have shown that this protein crystallizes in the B state, a structure with a more open dyad, which possibly has relevance to RBC band 3 protein binding and erythrocyte senescence. R-state equine CNmetHb crystal studies elaborate the solvent differences in the switch and hinge region compared with a human deoxyhemoglobin T-state neutron structure. Lastly, comparison of histidine protonation between the T and R state should enumerate the Bohr-effect protons.

  18. In Situ Tensile Deformation and Residual Stress Measurement by Neutron Diffraction in Modified 9Cr-1Mo Steel

    NASA Astrophysics Data System (ADS)

    Shrestha, Triratna; Charit, Indrajit; Potirniche, Gabriel

    2015-12-01

    The deformation behavior of monolithic modified 9Cr-1Mo (Grade 91) steel during uniaxial tensile loading was studied using the in situ neutron diffraction technique. The residual stress distribution across gas tungsten arc welds in the Grade 91 steel was measured by the time-of-flight neutron diffraction method using the SMARTS diffractometer at Lujan Neutron Scattering Center, Los Alamos National Laboratory. Grade 91 plates were welded using the gas tungsten arc welding (GTAW) technique. The load sharing by different grain orientations was observed during the tensile loading. The residual stresses along three orthogonal directions were determined at the mid-thickness, 4.35 and 2.35 mm below the surface of both the as-welded and post-weld heat-treated plates. The residual stresses of the as-welded plates were compared with those of the post-weld heat-treated plates. The post-weld heat treatment significantly reduced the residual stress level in the base metal, the heat-affected zone, and the weld zone. Vickers microhardness across the weld zone of the as-welded and post-weld heat-treated specimens was evaluated and correlated with the observed residual stress profile and microstructure.

  19. Characterization of neutron-irradiated HT-UPS steel by high-energy X-ray diffraction microscopy

    NASA Astrophysics Data System (ADS)

    Zhang, Xuan; Park, Jun-Sang; Almer, Jonathan; Li, Meimei

    2016-04-01

    This paper presents the first measurement of neutron-irradiated microstructure using far-field high-energy X-ray diffraction microscopy (FF-HEDM) in a high-temperature ultrafine-precipitate-strengthened (HT-UPS) austenitic stainless steel. Grain center of mass, grain size distribution, crystallographic orientation (texture), diffraction spot broadening and lattice constant distributions of individual grains were obtained for samples in three different conditions: non-irradiated, neutron-irradiated (3dpa/500 °C), and irradiated + annealed (3dpa/500 °C + 600 °C/1 h). It was found that irradiation caused significant increase in grain-level diffraction spot broadening, modified the texture, reduced the grain-averaged lattice constant, but had nearly no effect on the average grain size and grain size distribution, as well as the grain size-dependent lattice constant variations. Post-irradiation annealing largely reversed the irradiation effects on texture and average lattice constant, but inadequately restored the microstrain.

  20. Locating active-site hydrogen atoms in d-xylose isomerase: Time-of-flight neutron diffraction

    PubMed Central

    Katz, Amy K.; Li, Xinmin; Carrell, H. L.; Hanson, B. Leif; Langan, Paul; Coates, Leighton; Schoenborn, Benno P.; Glusker, Jenny P.; Bunick, Gerard J.

    2006-01-01

    Time-of-flight neutron diffraction has been used to locate hydrogen atoms that define the ionization states of amino acids in crystals of d-xylose isomerase. This enzyme, from Streptomyces rubiginosus, is one of the largest enzymes studied to date at high resolution (1.8 Å) by this method. We have determined the position and orientation of a metal ion-bound water molecule that is located in the active site of the enzyme; this water has been thought to be involved in the isomerization step in which d-xylose is converted to d-xylulose or d-glucose to d-fructose. It is shown to be water (rather than a hydroxyl group) under the conditions of measurement (pH 8.0). Our analyses also reveal that one lysine probably has an −NH2-terminal group (rather than NH3+). The ionization state of each histidine residue also was determined. High-resolution x-ray studies (at 0.94 Å) indicate disorder in some side chains when a truncated substrate is bound and suggest how some side chains might move during catalysis. This combination of time-of-flight neutron diffraction and x-ray diffraction can contribute greatly to the elucidation of enzyme mechanisms. PMID:16707576

  1. Diffraction pattern from thermal neutron incoherent elastic scattering and the holographic reconstruction of the coherent scattering length distribution

    SciTech Connect

    Sur, B.; Anghel, V.N.P.; Rogge, R.B.; Katsaras, J.

    2005-01-01

    The diffraction of spherical waves (S waves) interacting with a periodic scattering length distribution produces characteristic intensity patterns known as Kossel and Kikuchi lines (collectively called K lines). The K-line signal can be inverted to give the three-dimensional structure of the coherent scattering length distribution surrounding the source of S waves - a process known as 'Gabor holography' or, simply, 'holography'. This paper outlines a kinematical formulation for the diffraction pattern of monochromatic plane waves scattering from a mixed incoherent and coherent S-wave scattering length distribution. The formulation demonstrates that the diffraction pattern of plane waves incident on a sample with a uniformly random distribution of incoherent scatterers is the same as that from a sample with a single incoherent scatterer per unit cell. In practice, one can therefore reconstruct the holographic data from samples with numerous incoherent S-wave scatterers per unit cell. Thus atomic resolution thermal neutron holography is possible for materials naturally rich in incoherent thermal neutron scatterers, such as hydrogen (e.g., biological and polymeric materials). Additionally, holographic inversions from single-wavelength data have suffered from the so-called conjugate or twin-image problem. The formulation presented for holographic inversion - different from those used previously [e.g., T. Gog et al., Phys. Rev. Lett. 76, 3132 (1996)] - eliminates the twin-image problem for single-wavelength data.

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

    NASA Astrophysics Data System (ADS)

    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.

  3. The structure of molten CaSiO3: A neutron diffraction isotope substitution and aerodynamic levitation study.

    SciTech Connect

    Skinner, Lawrie; Benmore, Chris J; Weber, Richard; Santodonato, Louis J; Tumber, Sonia; Neuefeind, Joerg C; Lazareva, Lena; Du, Jincheng; Parise, John B

    2012-01-01

    We have performed neutron diffraction isotopic substitution experiments on aerodynamically levitated droplets of CaSiO3, to directly extract intermediate and local structural information on the Ca environment. The results show a substantial broadening of the Ca-O peak in the pair distribution function of the melt compared to the glass, which comprises primarily of 6- and 7-fold coordinated Ca-polyhedra. The broadening can be explained by a re-distribution of Ca-O bond lengths, especially towards longer distances in the liquid. The first order neutron difference function provides a rigorous test of recent molecular dynamics simulations and supports the model of the presence of short chains or channels of edge shared Ca-octahedra in the liquid state. It is suggested that the polymerization of Ca-polyhedra is responsible for the fragile viscosity behavior of the melt and the glass forming ability in CaSiO3.

  4. Extracting grain-orientation-dependent data from in situ time-of-flight neutron diffraction. I. Inverse pole figures

    DOE PAGESBeta

    Stoica, Grigoreta M.; Stoica, Alexandru Dan; An, Ke; Ma, Dong; Vogel, S. C.; Carpenter, J. S.; Wang, Xun-Li

    2014-11-28

    The problem of calculating the inverse pole figure (IPF) is analyzed from the perspective of the application of time-of flight neutron diffraction toin situmonitoring of the thermomechanical behavior of engineering materials. On the basis of a quasi-Monte Carlo (QMC) method, a consistent set of grain orientations is generated and used to compute the weighting factors for IPF normalization. The weighting factors are instrument dependent and were calculated for the engineering materials diffractometer VULCAN (Spallation Neutron Source, Oak Ridge National Laboratory). The QMC method is applied to face-centered cubic structures and can be easily extended to other crystallographic symmetries. Examples includemore » 316LN stainless steelin situloaded in tension at room temperature and an Al–2%Mg alloy, substantially deformed by cold rolling and in situannealed up to 653 K.« less

  5. Neutron diffraction of p-hydroxyacetanilide (Paracetamol): libration or disorder of the methyl group at 100 K

    NASA Astrophysics Data System (ADS)

    Wilson, C. C.

    1997-03-01

    A single-crystal pulsed neutron diffraction study of p-hydroxyacetanilide (the analgesic Paracetamol, C 8H 9NO 2) was carried out at 100 K. The structure, in good agreement with previous X-ray determination, is monoclinic, space group {P2 1}/{a}, a = 12.763(6), b = 9.250(4), c = 7.082(2) Å, β = 115.52(3)°, Dx = 1.34 g cm -3, Z = 4. The present neutron data allowed full anisotropic refinement of all atoms including the hydrogens, yielding an agreement factor wR( F) = 0.063, for 2882 unique reflections and 181 refined parameters. Large, very anisotropic thermal ellipsoids are found on the methyl group hydrogen atoms; librational analysis was carried out along with attempts to model possible disorder associated with these large thermal vibrations.

  6. CONDENSED MATTER: STRUCTURE, MECHANICAL AND THERMAL PROPERTIES: Neutron Diffraction Measurements of a Thermally Fatigued Single Crystal Superalloy

    NASA Astrophysics Data System (ADS)

    Sun, Guang-Ai; Chen, Bo; Wu, Er-Dong; Li, Jin-Chao; Pirling, T.; Hughes, D.

    2009-08-01

    The thermally fatigued single crystal superalloy DZ125L is investigated by neutron diffraction measurements. The measurements, made using the phi angle oscillating method, provide more detailed and reliable data than those with the phi angle fixed. Diffraction studies show that the influence of thermal fatigue on the lattice parameters of the alloy is very limited. The stress analysis reveals that triaxial elastic hydrostatic stress plays a major role during thermal fatigue. The magnitude of the macrostress increases with the fatigue cycles, with the stress of the γ phase increasing more significantly than that of the γ' phase, and becoming fragile after many cycles. The changes in the microstrain are dependent on the reflection planes. The microstrains at the center of the sample are released by the thermal fatigue in comparison with those at the outlying locations, which has been attributed to the advance of the dislocation slips.

  7. Investigation of the reduction of NiAl{sub 2}O{sub 4}. 1: Neutron diffraction studies

    SciTech Connect

    Uestuendag, E.; Hanan, J.C.; Clausen, B.; Bourke, M.A.M.; Sass, S.L.; Barbieri, T.J.

    1998-09-01

    In-situ metal-ceramic composites consisting of Ni particles embedded in alumina matrices were obtained by the partial reduction of NiAl{sub 2}O{sub 4}. The volume shrinkage that accompanies the reduction reaction generates residual stresses. Neutron diffraction studies were performed for the first time at various temperatures to study the evolution of phases in situ during reduction and to determine their stress state. It was determined that compressive stresses of several hundred MPa in magnitude can be generated inside the unreduced part of spinel. It was also found that the stress generation is strongly influenced by material and processing variables such as reduction temperature and the initial density of spinel. The diffraction results were then compared to finite element calculations and a reasonable agreement was obtained.

  8. Magnetic Barkhausen Noise and Neutron Diffraction Techniques for the Study of Intergranular Residual Strains in Mild Steel

    SciTech Connect

    Hutanu, Roxana; Clapham, Lynann; Rogge, Ronald

    2004-02-26

    Intergranular residual stresses (IS) are microscopic residual stresses which have been found to accumulate along the <100> direction in steels. The <100> direction is also the magnetic easy axis direction in steel. This work involved Magnetic Barkhausen Noise (MBN) studies on steel samples, deformed uniaxially to increasing levels of strain. The MBN results indicated that a bulk magnetic easy axis was produced by the deformation process, and neutron diffraction experiments showed that this easy axis was correlated with the tensile strain in grains oriented in the <100> direction.

  9. Neutron-Diffraction Evidence for the Ferrimagnetic Ground State of a Molecule-Based Magnet with Weakly Coupled Sublattices

    SciTech Connect

    Fishman, Randy Scott; Campo, Javier; Vos, Thomas E.; Miller, Joel S.

    2012-01-01

    The diruthenium compound [Ru2(O2CMe)4]3[Cr(CN)6] contains two weakly coupled, ferrimag- netically ordered sublattices occupying the same volume. The magnetic field Hc 800 Oe required to align the two sublattice moments is proportional to the antiferromagnetic dipolar interaction Kc B Hc 5 10 3 meV between sublattices. Powder neutron-diffraction measurements on a deuterated sample reveal that the sublattice moments are restricted by the anisotropy of the diruthenium paddle-wheel complexes to the cubic diagonals. Those measurements also suggest that the quantum corrections to the ground state are significant.

  10. In situ x-ray and neutron powder diffraction study of LaNi5-xSnx-H systems

    NASA Technical Reports Server (NTRS)

    Bowman, Robert C., Jr.; Nakamara, Yumiko; Akiba, Etsuo

    2004-01-01

    This paper will present results of in situ XRD measurements of LaNi4.75Sn0.25 .during the initial absorption-desorption cycle, These measurements were performed under a similar condition to that for LaNi4.75Al0.25 previously reported [1]. The data were analyzed by the Rietveld method. Lattice parameter change and strain formation accompanying hydride phase formation and decomposition will be discussed. In addition, results of in situ neutron diffraction of LaNi4.78Sn0.22, focusing on hydrogen occupation in the hydride phase, will be presented.

  11. In-situ observation of ErD2 formation during D2 loading via neutron diffraction.

    SciTech Connect

    Browning, James Frederick; Llobet, Anna; Snow, Clark Sheldon; Rodriguez, Mark Andrew; Wixom, Ryan R.

    2010-09-01

    In an effort to better understand the structural changes occurring during hydrogen loading of erbium target materials, we have performed in situ D{sub 2} loading of erbium metal (powder) at temperature (450 C) with simultaneous neutron diffraction analysis. This experiment tracked the conversion of Er metal to the {alpha} erbium deuteride (solid-solution) phase and then into the {beta} (fluorite) phase. Complete conversion to ErD{sub 2.0} was accomplished at 10 Torr D{sub 2} pressure with deuterium fully occupying the tetrahedral sites in the fluorite lattice.

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

    SciTech Connect

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

    1998-12-31

    Superelastic NiTi (51.0 at% Ni) with 0, 10 and 20 vol% TiC particles were deformed under uniaxial compression as neutron diffraction spectra were simultaneously obtained. The experiments yielded in-situ measurements of the thermoelastic stress-induced transformation. A detailed Rietveld determination is made of the phase fractions and the evolving strains in the reinforcing TiC particles and the austenite as it transforms to martensite on loading (and its subsequent back transformation on unloading). These strains are used to shed light on the phenomenon of load transfer in composites where the matrix undergoes a stress-induced phase transformation.

  13. Nanostructures of Mg0.65Ti0.35Dx studied with x-ray diffraction, neutron diffraction, and magic-angle-spinning H2 NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Srinivasan, S.; Magusin, P. C. M. M.; Kalisvaart, W. P.; Notten, P. H. L.; Cuevas, F.; Latroche, M.; van Santen, R. A.

    2010-02-01

    Magnesium transition-metal alloys have a high hydrogen-storage capacity and show improved hydrogen-uptake and -release kinetics compared to magnesium alone. In the present study we have investigated the structure of bulk magnesium-titanium deuteride Mg0.65Ti0.35Dx prepared via mechanical alloying and gas-phase deuterium absorption by combined use of x-ray diffraction (XRD), neutron diffraction, and magic-angle-spinning H2 nuclear magnetic resonance (NMR). The initial ball-milled alloy has two XRD-distinct Mg and Ti fcc phases. Even after prolonged exposure to deuterium gas at 75 bar and 175°C the materials with and without palladium catalyst are only partly deuterated. Deuterium loading causes the formation of, on the one hand, bct (rutile) MgD2 nanodomains with interdispersed TiDy layers and, on the other hand, a separate fcc (fluorite) TiDz phase. The TiDy phase is XRD invisible, but shows clearly up at a H2 NMR shift of -43ppm between the shift of MgD2 (3 ppm) and the Knight shift of the TiDz phase (-143ppm) . Exchange NMR indicates complete deuterium exchange at 25°C between the MgD2 and TiDy phase within 1 s, as consistent with intimate contacts between these phases. Combined analysis of the XRD and NMR peak areas suggests that the deuterium concentrations y and z in the TiDy and TiDz domains are about 1.5 and 2.0, respectively. Comparing the intrinsic cell parameters of rutile MgH2 and fluorite TiH2 , we propose that stabilization of the mixed nanocomposite may arise from a coherent coupling between the crystal structures of the rutile MgD2 nanodomains and the thin layers of fcc TiDy .

  14. Neutron diffraction study and superparamagnetic behavior of ZnFe 2O 4 nanoparticles obtained with different conditions

    NASA Astrophysics Data System (ADS)

    Blanco-Gutierrez, V.; Climent-Pascual, E.; Torralvo-Fernandez, M. J.; Saez-Puche, R.; Fernandez-Diaz, M. T.

    2011-07-01

    Spinel-type (S.G.= Fd3¯ m) ZnFe 2O 4 fine particles with sizes from 4 to 19 nm prepared by solvothermal and microwave-assisted solvothermal methods have been studied by neutron powder diffraction at room temperature. The cation distribution corresponding to mixed spinel structure (Zn 2+1- xFe 3+x)[Fe 3+2- xZn 2+x]O 4 along with the unit cell parameter has been estimated after Rietveld refinement of the obtained neutron diffraction data for all the samples. It has been found that the inversion degree parameter ( x) takes values between 0.11 and 0.20 depending not only on the particle size but also on the synthesis conditions as well. All the samples behave as superparamagnetic with an effective magnetic moment per particle ( μSP) from 7.0×10 2 to 7.7×10 3 μ B. The sample obtained by microwave assistance displays a different magnetic behavior as the ZFC and FC magnetic susceptibility and the magnetization versus applied field hysteresis loop measured at 5 K suggest. This is related with the dipole interactions that are a consequence of the higher inversion degree and μSP.

  15. In Situ Neutron and Synchrotron X-ray Diffraction Studies of Jarosite at High-Temperature High-Pressure Conditions

    NASA Astrophysics Data System (ADS)

    Xu, H.; Zhao, Y.; Hickmott, D.; Zhang, J.; Vogel, S.; Daemen, L.; Hartl, M.

    2011-03-01

    Jarosite (KFe 3 (SO4)2 (OH)6) occurs in acid mine drainage and epithermal environments and hot springs associated with volcanic activity. Jarosite is also of industrial interest as an iron-impurity extractor from zinc sulfide ores. In 2004, jarosite was detected by the Mars Exploration Rover Mössbauer spectrometer, which has been interpreted as a strong evidence for the existence of water (and possibly life) on ancient Mars. This discovery has spurred considerable interests in stability and structural behavior of jarosite and related phases at various temperature, pressure, and aqueous conditions. In this work, we have investigated the crystal structure and phase stability of jarosite at temperatures up to 900 K and/or pressures up to 9 GPa using in situ neutron and synchrotron X-ray diffraction. To avoid the large incoherent scattering of neutrons by hydrogen, a deuterated sample was synthesized and characterized. Rietveld analysis of the obtained diffraction data allowed determination of unit-cell parameters, atomic positions and atomic displacement parameters as a function of temperature and pressure. In addition, the coefficients of thermal expansion, bulk moduli and pressure-temperature stability regions of jarosite were determined.

  16. Neutron diffraction and electrical transport studies on magnetic ordering in terbium at high pressures and low temperatures

    SciTech Connect

    Thomas, Sarah; Montgomery, Jeffrey M; Tsoi, Georgiy; Vohra, Yogesh; Chesnut, Gary Neal; Weir, S. T.; Tulk, Christopher A; Moreira Dos Santos, Antonio F

    2013-01-01

    Neutron diffraction and electrical transport measurements have been carried out on the heavy rare-earth metal terbium at high pressures and low temperatures in order to elucidate the onset of ferromagnetic (FM) order as a function of pressure. The electrical resistance measurements show a change in slope as the temperature is lowered through the FM Curie temperature. The temperature of this FM transition decreases at a rate of-16.7 K/GPa up to a pressure of 3.6 GPa, at which point the onset of FM order is suppressed. The neutron diffraction measurements as a function of pressure at temperatures ranging from 90 to 290 K confirm that the change of slope in the resistance is associated with the FM ordering, since this occurs at pressures similar to those determined from the resistance results at these temperatures. A disappearance of FM ordering was observed as the pressure is increased above 3.6 GPa and is correlated with the phase transition from the ambient hexagonal close packed structure to an -Sm-type structure at high pressures.

  17. CO2 Adsorption to Sub-Single Hydration Layer Montmorillonite Clay Studied by Excess Sorption and Neutron Diffraction

    SciTech Connect

    Rother, Gernot; Ilton, Eugene; Wallacher, Dirk; Hauss, Thomas; Schaef, Herbert; Qafoku, Odeta; Rosso, Kevin M.; Felmy, Andrew; Krukowski, Elizabeth G; Stack, Andrew G; Bodnar, Robert J

    2013-01-01

    Geologic storage of CO2 requires that the caprock sealing the storage rock is highly impermeable by CO2. Swelling clays, which are important components of caprocks, may react with CO2 under volume change, potentially impacting the seal quality. The interactions of scCO2 with Na saturated montmorillonite clay containing a sub-single layer of water in the interlayer region have been studied by sorption and neutron diffraction techniques. The excess sorption isotherms show maxima at bulk CO2 densities of 0.15 g/cm3, followed by an approximately linear decrease of excess sorption to zero and negative values with increasing CO2 bulk density. Neutron diffraction experiments on the same clay sample measured interlayer spacing and composition. The results show that limited amounts of CO2 are sorbed into the interlayer region, leading to depression of the interlayer peak intensity and an increase of the d(001) spacing by ca. 0.5 . The density of CO2 in the clay pores is relatively stable over a wide range of CO2 pressures at a given temperature, indicating the formation of a clay-CO2 phase. At low pressure increasing CO2 adsorption with decreasing temperature is observed while the high-pressure sorption properties exhibit weak or no temperature dependence. Supercritical fluids, sorption phenomena, carbon dioxide, carbon sequestration, caprock integrity

  18. CO2 Sorption to Subsingle Hydration Layer Montmorillonite Clay Studied by Excess Sorption and Neutron Diffraction Measurements

    SciTech Connect

    Rother, Gernot; Ilton, Eugene S.; Wallacher, Dirk; Hauβ, Thomas; Schaef, Herbert T.; Qafoku, Odeta; Rosso, Kevin M.; Felmy, Andrew R.; Krukowski, Elizabeth G.; Stack, Andrew G.; Grimm, Nico; Bodnar, Robert J.

    2013-01-02

    Geologic storage of CO2 requires that the caprock sealing the storage rock is highly impermeable to CO2. Swelling clays, which are important components of caprocks, may interact with CO2 leading to volume change and potentially impacting the seal quality. The interactions of supercritical (sc) CO2 with Na saturated montmorillonite clay containing a subsingle layer of water in the interlayer region have been studied by sorption and neutron diffraction techniques. The excess sorption isotherms show maxima at bulk CO2 densities of ≈0.15 g/cm3, followed by an approximately linear decrease of excess sorption to zero and negative values with increasing CO2 bulk density. Neutron diffraction experiments on the same clay sample measured interlayer spacing and composition. The results show that limited amounts of CO2 are sorbed into the interlayer region, leading to depression of the interlayer peak intensity and an increase of the d(001) spacing by ca. 0.5 Å. The density of CO2 in the clay pores is relatively stable over a wide range of CO2 pressures at a given temperature, indicating the formation of a clay-CO2 phase. Finally, at the excess sorption maximum, increasing CO2 sorption with decreasing temperature is observed while the high-pressure sorption properties exhibit weak temperature dependence.

  19. Temperature-dependent neutron diffraction measurements from D2O hydrating single-supported lipid bilayers of DMPC

    NASA Astrophysics Data System (ADS)

    Buck, Z. N.; Torres, J.; Mazza, A.; Kaiser, H.; Taub, H.; Hansen, F. Y.; Miskowiec, A.; Tyagi, M.

    The freezing point depression of water associated with biological membranes, studied principally by NMR, has been of interest for decades. Here we have used neutron diffraction measurements at the University of Missouri Research Reactor (MURR) to investigate the freezing behavior of water associated with single-supported zwitterionic lipid bilayers composed of DMPC. Diffraction patterns obtained as a function of temperature reveal that water freezes abruptly into its hexagonal phase at 270 K with no evidence of amorphous ice. Following the initial crystallization of the membrane-associated water there is a region of continuous hexagonal crystal growth, which is believed to occur in the interfacial water closest to the membrane. The temperature-dependent intensity of the observed Bragg peaks have been compared with that of incoherently elastically-scattered neutrons collected on the High-Flux Backscattering Spectrometer at NIST from an identical sample hydrated with H2O [2]. We find excellent agreement between the two data sets, suggesting the absence of amorphous solid water and that all the water hydrating a DMPC membrane eventually freezes into the hexagonal crystalline phase. 2 M. Bai et al., Europhys. Lett. 98, 48006 (2012). Supported by NSF Grant Nos. DMR-0944772 and DGE-1069091.

  20. Neutron diffraction and electrical transport studies on magnetic ordering in terbium at high pressures and low temperatures

    SciTech Connect

    Thomas, Sarah A.; Montgomery, Jeffrey M.; Tsoi, Georgiy M.; Vohra, Yogesh K.; Chesnut, Gary N.; Weir, Samuel T.; Tulk, Christopher A.; dos Santos, Antonio M.

    2013-06-11

    Neutron diffraction and electrical transport measurements have been carried out on the heavy rare earth metal terbium at high pressures and low temperatures in order to elucidate the onset of ferromagnetic order as a function of pressure. The electrical resistance measurements show a change in slope as the temperature is lowered through the ferromagnetic Curie temperature. The temperature of this ferromagnetic transition decreases from approximately 240 K at ambient pressure at a rate of –16.7 K/GPa up to a pressure of 3.6 GPa, at which point the onset of ferromagnetic order is suppressed. Neutron diffraction measurements as a function of pressure at temperatures ranging from 90 K to 290 K confirm that the change of slope in the resistance is associated with the ferromagnetic ordering, since this occurs at pressures similar to those determined from the resistance results at these temperatures. Furthermore, a change in ferromagnetic ordering as the pressure is increased above 3.6 GPa is correlated with the phase transition from the ambient hexagonal close packed (hcp) structure to an α-Sm type structure at high pressures.

  1. Lithium plating in lithium-ion batteries at sub-ambient temperatures investigated by in situ neutron diffraction

    NASA Astrophysics Data System (ADS)

    Zinth, Veronika; von Lüders, Christian; Hofmann, Michael; Hattendorff, Johannes; Buchberger, Irmgard; Erhard, Simon; Rebelo-Kornmeier, Joana; Jossen, Andreas; Gilles, Ralph

    2014-12-01

    Lithium plating in commercial LiNi1/3Mn1/3Co1/3O2/graphite cells at sub-ambient temperatures is studied by neutron diffraction at Stress-Spec, MLZ. Li plating uses part of the active lithium in the cell and competes with the intercalation of lithium into graphite. As a result, the degree of graphite lithiation during and after charge is lower. Comparison of graphite lithiation after a C/5 charging cycle fast enough to expect a considerable amount of Li plating with a much slower C/30 reference cycle reveals a lower degree of graphite lithiation in the first case; neutron diffraction shows less LiC6 and more LiC12 is present. If the cell is subjected to a 20 h rest period after charge, a gradual transformation of remaining LiC12 to LiC6 can be observed, indicating Li diffusion into the graphite. During the rest period after the C/5 charging cycle, the degree of graphite lithiation can be estimated to increase by 17%, indicating at least 17% of the active lithium is plated. Data collected during discharge immediately after C/5 charging give further evidence of the presence and amount of metallic lithium: in this case 19% of discharge capacity originates from the oxidation of metallic lithium. Also, lithium oxidation can be directly related to the high voltage plateau observed during discharge in case of lithium plating.

  2. Structure of 2 molar NaOH in aqueous solution from neutron diffraction and empirical potential structure refinement

    SciTech Connect

    McLain, Sylvia E.; Imberti, Silvia; Soper, Alan K.; Botti, Alberto; Bruni, Fabio; Ricci, Maria Antonietta

    2006-09-01

    Neutron diffraction with isotopic substitution has been used to investigate aqueous solutions of 2M NaOH in the liquid state. The data were modeled using empirical potential structure refinement which allows for the extraction of the ion-water and water-water correlations. The data show that the ion-water radial distribution functions are in accordance with those found by previous studies on NaOH solutions and follow a trend which is dependent on the concentration of the solute. In particular, the shape of the hydroxide hydration shell is found to be concentration independent, but the number of water molecules occupying this shell increases with dilution. Additionally, the water-water correlations show that there is still a measurable effect on water structure with the addition of ions at this concentration, as the second shell in the water oxygen radial distribution function is compressed relative to the first shell. The data are also used to discuss the recent claims that the published radial distribution functions of water are unreliable, showing that data taken at different neutron sources, with different diffraction geometry and systematic errors lead to the same structural information when analyzed via a realistic modeling regime.

  3. Visualizing the chemistry and structure dynamics in lithium-ion batteries by in-situ neutron diffraction

    PubMed Central

    Wang, Xun-Li; An, Ke; Cai, Lu; Feng, Zhili; Nagler, Stephen E.; Daniel, Claus; Rhodes, Kevin J.; Stoica, Alexandru D.; Skorpenske, Harley D.; Liang, Chengdu; Zhang, Wei; Kim, Joon; Qi, Yue; Harris, Stephen J.

    2012-01-01

    We report an in-situ neutron diffraction study of a large format pouch battery cell. The succession of Li-Graphite intercalation phases was fully captured under an 1C charge-discharge condition (i.e., charge to full capacity in 1 hour). However, the lithiation and dilithiation pathways are distinctively different and, unlike in slowing charging experiments with which the Li-Graphite phase diagram was established, no LiC24 phase was found during charge at 1C rate. Approximately 75 mol. % of the graphite converts to LiC6 at full charge, and a lattice dilation as large as 4% was observed during a charge-discharge cycle. Our work demonstrates the potential of in-situ, time and spatially resolved neutron diffraction study of the dynamic chemical and structural changes in “real-world” batteries under realistic cycling conditions, which should provide microscopic insights on degradation and the important role of diffusion kinetics in energy storage materials. PMID:23087812

  4. CO2 sorption to subsingle hydration layer montmorillonite clay studied by excess sorption and neutron diffraction measurements.

    PubMed

    Rother, Gernot; Ilton, Eugene S; Wallacher, Dirk; Hauβ, Thomas; Schaef, Herbert T; Qafoku, Odeta; Rosso, Kevin M; Felmy, Andrew R; Krukowski, Elizabeth G; Stack, Andrew G; Grimm, Nico; Bodnar, Robert J

    2013-01-01

    Geologic storage of CO(2) requires that the caprock sealing the storage rock is highly impermeable to CO(2). Swelling clays, which are important components of caprocks, may interact with CO(2) leading to volume change and potentially impacting the seal quality. The interactions of supercritical (sc) CO(2) with Na saturated montmorillonite clay containing a subsingle layer of water in the interlayer region have been studied by sorption and neutron diffraction techniques. The excess sorption isotherms show maxima at bulk CO(2) densities of ≈ 0.15 g/cm(3), followed by an approximately linear decrease of excess sorption to zero and negative values with increasing CO(2) bulk density. Neutron diffraction experiments on the same clay sample measured interlayer spacing and composition. The results show that limited amounts of CO(2) are sorbed into the interlayer region, leading to depression of the interlayer peak intensity and an increase of the d(001) spacing by ca. 0.5 Å. The density of CO(2) in the clay pores is relatively stable over a wide range of CO(2) pressures at a given temperature, indicating the formation of a clay-CO(2) phase. At the excess sorption maximum, increasing CO(2) sorption with decreasing temperature is observed while the high-pressure sorption properties exhibit weak temperature dependence. PMID:22917276

  5. Procedure for Computing Residual Stresses from Neutron Diffraction Data and its Application to Multi-Pass Dissimilar Weld

    SciTech Connect

    Zhang, Wei; Feng, Zhili; Crooker, Paul

    2011-01-01

    Neutron diffraction is a powerful tool for non-destructive measurement of internal residual stresses of welded structures. The conventional approach for determination of residual stresses requires the knowledge of stress-free lattice spacing a priori. For multiple-pass dissimilar metal welds common to nuclear reactor pipeline systems, the stress-free lattice parameter is a complex function of position due to the chemistry inhomogeneity in the weld region and can be challenging to determine experimentally. This paper presents a new approach to calculate the residual stress field in dissimilar welds without the use of stress-free lattice parameter. The theoretical basis takes advantage of the fact that the normal component of welding residual stresses is typically small for thin plate or pipe welds. The applicability of the new approach is examined and justified in a multi-pass dissimilar metal weld consisting of a stainless steel plate and a nickel alloy filler metal. The level of uncertainties associated with this new approach is assessed. Neutron diffraction experiment is carried out to measure the lattice spacing at various locations in the dissimilar weld. A comb-shaped specimen, electro-discharge machined from a companion weld, is used to determine the stress-free lattice spacing. The calculated results from the new approach are consistent with those from the conventional approach. The new approach is found to be a practical method for determining the two in-plane residual stress components in thin plate or pipe dissimilar metal welds.

  6. Mechanochemical synthesis in the Li-Mg-N-D system under deuterium gas: a neutron diffraction study.

    PubMed

    Li, Z; Zhang, J; Latroche, M; Wang, S; Jiang, L; Du, J; Cuevas, F

    2016-09-14

    The Mg(NH2)2/2LiH mixture is considered as one of the most valuable reversible hydrogen storage systems for feeding PEM fuel cells. In this paper, we investigate the mechanochemical synthesis in the Li-Mg-N-H system under deuterium gas, using Li3N and Mg as reactants, and the structural and sorption properties of the intermediate and final products mainly by means of neutron powder diffraction. Mechanochemistry leads to the end formation of amorphous Mg(ND2)2, which crystallizes upon heating above 425 K. During synthesis, a novel cation-mixed nitride/imide phase of simplified composition Li3MgN2D has been unveiled as the intermediate phase. It crystallizes in the cubic disordered anti-fluorite type structure (S.G. Fm3[combining macron]m) with a lattice parameter of 4.996 Å at room temperature. Deuterium absorption in this compound occurs through an original solid solution type mechanism ending with the imide compound β-Li2MgN2D2. The conjoint use of mechanochemistry under deuterium gas and in situ neutron diffraction techniques offers new avenues for better characterization of the efficient hydrogen storage materials. In particular, this work highlights the unexpected role of intermediate nitride/imide phases in the Li-Mg-N-H system. PMID:27523164

  7. Visualizing the Structural Evolution of LSM/xYSZ Composite Cathodes for SOFC by in-situ Neutron Diffraction

    SciTech Connect

    Chen, Yan; Yang, Ling; Ren, Fei; An, Ke

    2014-01-01

    Composite cathodes for solid oxide fuel cells, the mixtures of (La0.8Sr0.2)0.95MnO3- (LSM) and (Y2O3)x(ZrO2)1-x (xYSZ, x = 3, 6, 8 and 10), have the thermal stability unraveled at elevated temperatures by using in-situ neutron diffraction. The Rietveld refinement analysis of neutron diffraction visualizes the phase evolutions and the ion activities in the material systems. The phase transition of tetragonal YSZ at T > 900 C leads to a heterogeneous redistribution of Mn ions. The reaction of LSM and YSZ occurring at T > 1100 C was revealed as a three-stage process, yielding La2Zr2O7, SrZrO3 and MnO. The activities of Y, Mn and La ions at elevated temperatures are derived by the structural analysis, and the three-stage reaction of YSZ and LSM was found strongly correlated to ions behaviors.

  8. Visualizing the chemistry and structure dynamics in lithium-ion batteries by in-situ neutron diffraction

    SciTech Connect

    Wang, Xun-Li; An, Ke; Cai, Lu; Feng, Zhili; Nagler, Stephen E.; Daniel, Claus; Rhodes, Kevin J.; Stoica, Alexandru D.; Skorpenske, Harley D.; Liang, Chengdu; Zhang, Wei; Kim, Joon; Qi, Yue; Harris, Stephen J.

    2012-10-19

    We report an in-situ neutron diffraction study of a large format pouch battery cell. The succession of Li-Graphite intercalation phases was fully captured under an 1C charge-discharge condition (i.e., charge to full capacity in 1 hour). However, the lithiation and dilithiation pathways are distinctively different and, unlike in slowing charging experiments with which the Li-Graphite phase diagram was established, no LiC24 phase was found during charge at 1C rate. Approximately 75 mol. % of the graphite converts to LiC6 at full charge, and a lattice dilation as large as 4% was observed during a charge-discharge cycle. Our work demonstrates the potential of in-situ, time and spatially resolved neutron diffraction study of the dynamic chemical and structural changes in “real-world” batteries under realistic cycling conditions, which should provide microscopic insights on degradation and the important role of diffusion kinetics in energy storage materials.

  9. α-Phase transformation kinetics of U – 8 wt% Mo established by in situ neutron diffraction

    DOE PAGESBeta

    Garlea, Elena; Steiner, M. A.; Calhoun, C. A.; Klein, R. W.; An, K.; Agnew, S. R.

    2016-05-08

    The α-phase transformation kinetics of as-cast U - 8 wt% Mo below the eutectoid temperature have been established by in situ neutron diffraction. α-phase weight fraction data acquired through Rietveld refinement at five different isothermal hold temperatures can be modeled accurately utilizing a simple Johnson-Mehl-Avrami-Kolmogorov impingement-based theory, and the results are validated by a corresponding evolution in the γ-phase lattice parameter during transformation that follows Vegard’s law. Neutron diffraction data is used to produce a detailed Time-Temperature-Transformation diagram that improves upon inconsistencies in the current literature, exhibiting a minimum transformation start time of 40 min at temperatures between 500 °Cmore » and 510 °C. Lastly, the transformation kinetics of U – 8 wt% Mo can vary significantly from as-cast conditions after extensive heat treatments, due to homogenization of the typical dendritic microstructure which possesses non-negligible solute segregation.« less

  10. Neutron diffraction and electrical transport studies on magnetic ordering in terbium at high pressures and low temperatures

    DOE PAGESBeta

    Thomas, Sarah A.; Montgomery, Jeffrey M.; Tsoi, Georgiy M.; Vohra, Yogesh K.; Chesnut, Gary N.; Weir, Samuel T.; Tulk, Christopher A.; dos Santos, Antonio M.

    2013-06-11

    Neutron diffraction and electrical transport measurements have been carried out on the heavy rare earth metal terbium at high pressures and low temperatures in order to elucidate the onset of ferromagnetic order as a function of pressure. The electrical resistance measurements show a change in slope as the temperature is lowered through the ferromagnetic Curie temperature. The temperature of this ferromagnetic transition decreases from approximately 240 K at ambient pressure at a rate of –16.7 K/GPa up to a pressure of 3.6 GPa, at which point the onset of ferromagnetic order is suppressed. Neutron diffraction measurements as a function ofmore » pressure at temperatures ranging from 90 K to 290 K confirm that the change of slope in the resistance is associated with the ferromagnetic ordering, since this occurs at pressures similar to those determined from the resistance results at these temperatures. Furthermore, a change in ferromagnetic ordering as the pressure is increased above 3.6 GPa is correlated with the phase transition from the ambient hexagonal close packed (hcp) structure to an α-Sm type structure at high pressures.« less

  11. Structural and magnetic behavior of the cubic oxyfluoride SrFeO{sub 2}F studied by neutron diffraction

    SciTech Connect

    Thompson, Corey M.; Blakely, Colin K.; Flacau, Roxana; Greedan, John E.; Poltavets, Viktor V.

    2014-11-15

    The oxyfluoride SrFeO{sub 2}F has been prepared via a low temperature route involving the infinite-layer SrFeO{sub 2} and XeF{sub 2}. SrFeO{sub 2}F crystallizes in the cubic space group Pm-3m with disordered oxygen and fluorine atoms on the anion site. Recent reports demonstrated that SrFeO{sub 2}F is antiferromagnetic at room temperature and the zero field cooled and field cooled curves diverge at ∼150 K and ∼60 K, suggesting that the material has a spin glassy magnetic state at low temperatures. In this article, variable-temperature neutron diffraction (4–723 K) was performed to clarify the magnetic behavior observed in this material. Neutron powder diffraction measurements confirmed the antiferromagnetic (AFM) ordering of the system at room temperature. Below 710(1) K, the magnetic structure is a G-type AFM structure characterized by a propagation vector k=(1/2 , 1/2 , 1/2 ). The ordered moments on Fe{sup 3+} are 4.35(6)µ{sub B} at 4 K and 4.04(5)µ{sub B} at 290 K. Our results indicate that the cubic structure is retained all the way to base temperature (4 K) in contrast to PbFeO{sub 2}F. These results are compared with those of Pb and Ba analogs which exhibit very similar magnetic behavior. Furthermore, the observation of magnetic reflections at 4 K in the diffraction pattern shows the absence of the previously proposed spin glassy behavior at low temperatures. Previous proposals to explain the ZFC/FC divergences are examined. - Graphical abstract: Variable temperature powder neutron diffraction was employed to follow the evolution of the long range antiferromagnetic state in SrFeO{sub 2}F. - Highlights: • SrFeO{sub 2}F prepared via low temperature route involving SrFeO{sub 2} and XeF{sub 2}. • The cubic structure, Pm-3m, is retained at low temperatures, 4 K. • The magnetic structure is G-type AFM with T{sub N}=710 K and Fe{sup 3+} moment of 4.35µ{sub B}. • A small volume, bulk decoupled, spin glassy domain/cluster mechanism is proposed.

  12. Enhanced crystal fabric analysis of a lava flow sample by neutron texture diffraction: A case study from the Castello d'Ischia dome

    NASA Astrophysics Data System (ADS)

    Walter, Jens M.; Iezzi, Gianluca; Albertini, Gianni; Gunter, Mickey E.; Piochi, Monica; Ventura, Guido; Jansen, Ekkehard; Fiori, Fabrizio

    2013-01-01

    The crystal fabric of a lava has been analyzed for the first time by neutron texture diffraction. In this study we quantitatively investigate the crystallographic preferred orientation of feldspars in the Castello d'Ischia (Ischia Island, Italy) trachytic exogenous dome. The crystallographic preferred orientation was measured with the monochromatic neutron texture diffractometer SV7 at the Forschungszentrum Jülich in Germany and a Rietveld refinement was applied to the sum diffraction pattern. The complementary thin section analysis showed that the three-dimensional crystal shape and the corresponding shape preferred orientation are in agreement with the quantitative orientation distributions of the neutron texture data. The (0k0) crystallographic planes of the feldspars are roughly parallel to the local flow bands, whereas the other corresponding pole figures show that a pivotal rotation of the anorthoclase and sanidine crystals was active during the emplacement of this lava dome. In combination with scanning electron microscopy investigations, electron probe microanalysis, XRF, and X-ray diffraction, the Rietveld refinement of the neutron diffraction data indicates a slow cooling dynamic on the order of several months during their crystallization under subaerial conditions. Results attained here demonstrate that neutron texture diffraction is a powerful tool that can be applied to lava flows.

  13. Nucleon polarisabilities at and beyond physical pion masses

    NASA Astrophysics Data System (ADS)

    Grießhammer, Harald W.; McGovern, Judith A.; Phillips, Daniel R.

    2016-05-01

    We examine the results of Chiral Effective Field Theory ( χ EFT) for the scalar- and spin-dipole polarisabilities of the proton and neutron, both for the physical pion mass and as a function of {m_{π}}. This provides chiral extrapolations for lattice QCD polarisability computations. We include both the leading and subleading effects of the nucleon's pion cloud, as well as the leading ones of the Δ(1232)-resonance and its pion cloud. The analytic results are complete at N2LO in the δ counting for pion masses close to the physical value, and at leading order for pion masses similar to the Delta-nucleon mass splitting. In order to quantify the truncation error of our predictions and fits as 68% degree-of-belief intervals, we use a Bayesian procedure recently adapted to EFT expansions. At the physical point, our predictions for the spin polarisabilities are, within respective errors, in good agreement with alternative extractions using experiments and dispersion-relation theory. At larger pion masses we find that the chiral expansion of all polarisabilities becomes intrinsically unreliable as {m_{π}} approaches about 300 MeV -as has already been seen in other observables. χ EFT also predicts a substantial isospin splitting above the physical point for both the electric and magnetic scalar polarisabilities; and we speculate on the impact this has on the stability of nucleons. Our results agree very well with emerging lattice computations in the realm where χ EFT converges. Curiously, for the central values of some of our predictions, this agreement persists to much higher pion masses. We speculate on whether this might be more than a fortuitous coincidence.

  14. First spin-resolved electron distributions in crystals from combined polarized neutron and X-ray diffraction experiments

    PubMed Central

    Deutsch, Maxime; Gillon, Béatrice; Claiser, Nicolas; Gillet, Jean-Michel; Lecomte, Claude; Souhassou, Mohamed

    2014-01-01

    Since the 1980s it has been possible to probe crystallized matter, thanks to X-ray or neutron scattering techniques, to obtain an accurate charge density or spin distribution at the atomic scale. Despite the description of the same physical quantity (electron density) and tremendous development of sources, detectors, data treatment software etc., these different techniques evolved separately with one model per experiment. However, a breakthrough was recently made by the development of a common model in order to combine information coming from all these different experiments. Here we report the first experimental determination of spin-resolved electron density obtained by a combined treatment of X-ray, neutron and polarized neutron diffraction data. These experimental spin up and spin down densities compare very well with density functional theory (DFT) calculations and also confirm a theoretical prediction made in 1985 which claims that majority spin electrons should have a more contracted distribution around the nucleus than minority spin electrons. Topological analysis of the resulting experimental spin-resolved electron density is also briefly discussed. PMID:25075338

  15. Ancient and historic steel in Japan, India and Europe, a non-invasive comparative study using thermal neutron diffraction.

    PubMed

    Grazzi, F; Civita, F; Williams, A; Scherillo, A; Barzagli, E; Bartoli, L; Edge, D; Zoppi, M

    2011-05-01

    The production and refinement of steel has followed very different paths in different parts of the Eurasian continent. In aiming to characterize the similarities and differences between various smelting and smithing methods, we have analysed steel samples from four different areas and historic periods: the Kotō Age in Japan (twelfth-sixteenth century), the Moghul Empire in India (seventeenth-nineteenth century), the Ottoman Turkish Empire (seventeenth century) and the late Middle Ages (fifteenth century) in Italy. The best quality steel was employed for forging arms and armour of high quality, so that we have selected samples from Japan, India, the Middle East and Italy belonging to such a category. Traditional methods, such as metallography, used to characterize different steels in terms of their carbon contents, microconstituents and slag inclusions, entailed an invasive approach. Since many of the selected artefacts are in a very good state of conservation, a different and non-invasive approach was desirable. To this aim, we have used time of flight neutron diffraction on the Italian Neutron Experimental Station diffractometer, located at the pulsed neutron source ISIS in the United Kingdom. By this technique, we were able to quantify the phase distribution of the metal phases, the slag inclusion content, and the oxidation state of the samples, both as average concentration on the whole artefact and in selected gauge volumes. The results of the present investigation offer an interesting picture of the steel metallurgy in different areas of the world. PMID:21400072

  16. Combined high-pressure neutron and X-ray diffraction study of H-D substitution effects on brucite

    SciTech Connect

    dos Santos, Antonio M.; Horita, Juske; Tulk, Christopher A; Chakoumakos, Bryan C; Polyakov, Dr. Veniamin B

    2010-01-01

    The high-pressure behavior of the mineral brucite, Mg(OH)2, is of great geochemical and geophysical interest, because brucite-type minerals serve as a simple analog for more complex, hydrogen-bearing oxide and silicate minerals in the deep-earth. A combined neutron and synchrotron x-ray powder diffraction study of hydrogenated and deuterated brucite was conducted at ambient temperature and at pressures to 9 and 20 GPa, using a Paris-Edinburgh (neutron diffraction) and a diamond anvil cell (synchrotron x-ray radiation), respectively. The two materials were synthesized by the same method and companion diffraction measurements of the two materials were conducted under the same conditions. Our experimental results show that the lattice-parameters of the a axis, parallel to the sheets of Mg-O octahedra, decrease only slightly with pressure with no effect of H-D substitution. However, the c axis of Mg (OD)2 is shorter and may exhibit greater compressibility with pressure than that of Mg (OH)2. Consequently, the unit-cell volume of deuterated brucite is slightly, but systematically smaller than that of hydrogenated brucite. Fitting to a third-order Birch-Murnaghan equation shows that values of the bulk modulus for hydrogenated and deuterated brucite are indistinguishable from each other within the experimental errors. The measured effect of H-D substitution on the unit-cell volume demonstrates that brucite (and other hydrous minerals) preferentially incorporate deuterium over hydrogen under pressure, suggesting that the distribution of hydrogen isotopes in deep-earth conditions may differ significantly from that in near-surface environments.

  17. A structural investigation of the alkali metal site distribution within bioactive glass using neutron diffraction and multinuclear solid state NMR.

    PubMed

    Martin, Richard A; Twyman, Helen L; Rees, Gregory J; Smith, Jodie M; Barney, Emma R; Smith, Mark E; Hanna, John V; Newport, Robert J

    2012-09-21

    The atomic-scale structure of Bioglass and the effect of substituting lithium for sodium within these glasses have been investigated using neutron diffraction and solid state magic angle spinning (MAS) NMR. Applying an effective isomorphic substitution difference function to the neutron diffraction data has enabled the Na-O and Li-O nearest-neighbour correlations to be isolated from the overlapping Ca-O, O-(P)-O and O-(Si)-O correlations. These results reveal that Na and Li behave in a similar manner within the glassy matrix and do not disrupt the short range order of the network former. Residual differences are attributed solely to the variation in ionic radius between the two species. Successful simplification of the 2 < r (Å) < 3 region via the difference method has enabled all the nearest neighbour correlations to be deconvolved. The diffraction data provides the first direct experimental evidence of split Na-O nearest-neighbour correlations in these melt quench bioactive glasses, and an analogous splitting of the Li-O correlations. The observed correlations are attributed to the metal ions bonded either to bridging or to non-bridging oxygen atoms. (23)Na triple quantum MAS (3QMAS) NMR data corroborates the split Na-O correlations. The structural sites present will be intimately related to the release properties of the glass system in physiological fluids such as plasma and saliva, and hence to the bioactivity of the material. Detailed structural knowledge is therefore a prerequisite for optimizing material design. PMID:22868255

  18. Combined high-pressure neutron and X-ray diffraction study of H-D substitution effects on brucite

    SciTech Connect

    Moreira Dos Santos, Antonio F; Horita, Juske; Tulk, Christopher A; Chakoumakos, Bryan C; Polyakov, Dr. V. B.

    2010-01-01

    The high-pressure behavior of the mineral brucite, Mg(OH){sub 2}, is of great geochemical and geophysical interest, because brucite-type minerals serve as a simple analog for more complex, hydrogen-bearing oxide and silicate minerals in the deep-earth. A combined neutron and synchrotron x-ray powder diffraction study of hydrogenated and deuterated brucite was conducted at ambient temperature and at pressures to 9 and 20 GPa, using a Paris-Edinburgh (neutron diffraction) and a diamond anvil cell (synchrotron x-ray radiation), respectively. The two materials were synthesized by the same method and companion diffraction measurements of the two materials were conducted under the same conditions. Our experimental results show that the lattice-parameters of the a axis, parallel to the sheets of Mg-O octahedra, decrease only slightly with pressure with no effect of H-D substitution. However, the c axis of Mg (OD){sub 2} is shorter and may exhibit greater compressibility with pressure than that of Mg (OH){sub 2}. Consequently, the unit-cell volume of deuterated brucite is slightly, but systematically smaller than that of hydrogenated brucite. Fitting to a third-order Birch-Murnaghan equation shows that values of the bulk modulus for hydrogenated and deuterated brucite are indistinguishable from each other within the experimental errors. The measured effect of H-D substitution on the unit-cell volume demonstrates that brucite (and other hydrous minerals) preferentially incorporate deuterium over hydrogen under pressure, suggesting that the distribution of hydrogen isotopes in deep-earth conditions may differ significantly from that in near-surface environments.

  19. Neutron diffraction as a precise and reliable method for obtaining structural properties of bulk quantities of graphene

    NASA Astrophysics Data System (ADS)

    Sofer, Zdeněk; Šimek, Petr; Jankovský, Ondřej; Sedmidubský, David; Beran, Přemysl; Pumera, Martin

    2014-10-01

    Graphene based carbon materials have attracted a great deal of attention in the last decade; nowadays tons of graphene are produced yearly. However, there is lack of precise and reliable techniques for the determination of structural properties of graphene on the bulk scale. The analytical methods being routinely applied for graphene characterization, including TEM and AFM, can be only used for the study of scant amounts of graphene samples and do not give general information on the average number of layers and the structure of the prepared graphenes. On the other hand, diffraction methods can be advantageously used to obtain information on the average thickness of the produced graphene as well as on the average sheets lateral dimensions, without the necessity of sample dispersion in solvents. We present a study of the structural properties of graphene prepared by chemical and thermal reduction of graphite oxide, comparing SEM, STEM, AFM, Raman spectroscopy, BET, X-ray and neutron diffraction methods. Our study brings new deep insights into the basic structural properties of graphene in a bulk form. Given the importance of a suitable characterization technique on the bulk materials, we wish to highlight the importance of these diffraction techniques for accurate determination of the graphene thickness and lateral parameters.

  20. Structure refinement of sub-cubic-mm volume sample at high pressures by pulsed neutron powder diffraction: application to brucite in an opposed anvil cell

    NASA Astrophysics Data System (ADS)

    Okuchi, Takuo; Tomioka, Naotaka; Purevjav, Narangoo; Abe, Jun; Harjo, Stefanus; Gong, Wu

    2014-04-01

    Neutron powder diffraction measurements of 0.9 mm3 of mixture of deuterated brucite and pressure medium were conducted at pressures to 2.8 GPa, using an opposed anvil cell and a medium-resolution diffractometer at Japan Proton Accelerator Research Complex pulsed neutron source. Spurious-free diffraction patterns were successfully obtained and refined to provide all structural parameters including Debye-Waller factors. Tilting of hydroxyl dipoles of brucite toward one of the three nearest-neighbor oxygen anions was confirmed to be substantial at pressure as low as 1.5 GPa. By this application, technical feasibility to analyze such a small sample has been newly established, which would be useful to extend the applications of neutron diffraction at high pressures.

  1. High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures

    NASA Astrophysics Data System (ADS)

    Jacobsen, Matthew K.; Ridley, Christopher J.; Bocian, Artur; Kirichek, Oleg; Manuel, Pascal; Khalyavin, Dmitry; Azuma, Masaki; Attfield, J. Paul; Kamenev, Konstantin V.

    2014-04-01

    Pressure generation at cryogenic temperatures presents a problem for a wide array of experimental techniques, particularly neutron studies due to the volume of sample required. We present a novel, compact pressure cell with a large sample volume in which load is generated by a bellow. Using a supply of helium gas up to a pressure of 350 bar, a load of up to 78 kN is generated with leak-free operation. In addition, special fiber ports added to the cryogenic center stick allow for in situ pressure determination using the ruby pressure standard. Mechanical stability was assessed using finite element analysis and the dimensions of the cell have been optimized for use with standard cryogenic equipment. Load testing and on-line experiments using NaCl and BiNiO3 have been done at the WISH instrument of the ISIS pulsed neutron source to verify performance.

  2. High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures

    SciTech Connect

    Jacobsen, Matthew K.; Ridley, Christopher J.; Bocian, Artur; Kamenev, Konstantin V.; Kirichek, Oleg; Manuel, Pascal; Khalyavin, Dmitry; Azuma, Masaki; Attfield, J. Paul

    2014-04-15

    Pressure generation at cryogenic temperatures presents a problem for a wide array of experimental techniques, particularly neutron studies due to the volume of sample required. We present a novel, compact pressure cell with a large sample volume in which load is generated by a bellow. Using a supply of helium gas up to a pressure of 350 bar, a load of up to 78 kN is generated with leak-free operation. In addition, special fiber ports added to the cryogenic center stick allow for in situ pressure determination using the ruby pressure standard. Mechanical stability was assessed using finite element analysis and the dimensions of the cell have been optimized for use with standard cryogenic equipment. Load testing and on-line experiments using NaCl and BiNiO{sub 3} have been done at the WISH instrument of the ISIS pulsed neutron source to verify performance.

  3. Absolute configuration of a chiral CHD group via neutron diffraction: confirmation of the absolute stereochemistry of the enzymatic formation of malic acid

    SciTech Connect

    Bau, R.; Brewer, I.; Chiang, M.Y.; Fujita, S.; Hoffman, J.; Watkins, M.I.; Koetzle, T.F.

    1983-09-30

    Neutron diffraction has been used to monitor the absolute stereochemistry of an enzymatic reaction. (-)(2S)malic-3-d acid was prepared by the action of fumarase on fumaric acid in D/sub 2/O. After a large number of cations were screened, it was found that (+)(R)..cap alpha..-phenylethylamine forms the large crystals necessary for a neutron diffraction analysis. The subsequent structure determination showed that (+)(R)..cap alpha..-phenylethylammonium (-)(2S)malate-3-d has an absolute configuration of R at the CHD site. This result confirms the absolute stereochemistry of fumarate-to-malate transformation as catalyzed by the enzyme fumarase.

  4. Single phase synthesis and room temperature neutron diffraction studies on multiferroic PbFe{sub 0.5}Nb{sub 0.5}O{sub 3}

    SciTech Connect

    Matteppanavar, Shidaling; Angadi, Basavaraj; Rayaprol, Sudhindra

    2013-02-05

    The lead-iron-niobate, (PbFe{sub 0.5}Nb{sub 0.5}O{sub 3} or PFN) was synthesized by low temperature sintering Single Step / Solid State Reaction Method. The 700 Degree-Sign C/2 hrs. calcined powder was sintered at 1050 Degree-Sign C/1 hr. The sintered pellets were characterized through X-Ray Diffraction and Neutron Diffraction at room temperature. It is found from the XRD pattern that the materials is in single phase with no traces of pyrochlore phase. It was also confirmed from the neutron diffraction pattern, the structure of PFN to be monoclinic, space group Cm. Structural studies has been carried out by refining the obtained neutron diffraction data by Rietveld refinement method using Fullprof program. The neutron diffraction pattern at 300 K (room temperature) was selected to refine the structure. The lattice parameters obtained are; a = 5.6709 A, b = 5.6732 A, c = 4.0136 A, and {alpha}= 90, {beta}= 89.881, {gamma}= 90. The P-E measurements showed hysteretic behavior with high remnant polarization.

  5. Neutron diffraction study of the magnetic-field-induced transition in Mn{sub 3}GaC

    SciTech Connect

    Çakir, Ö.; Acet, M.; Farle, M.; Senyshyn, A.

    2014-01-28

    The antiperovskite Mn{sub 3}GaC undergoes an isostructural cubic–cubic first order transition from a low-temperature, large-cell-volume antiferromagnetic state to a high-temperature, small-cell-volume ferromagnetic state at around 160 K. The transition can also be induced by applying a magnetic field. We study here the isothermal magnetic-field-evolution of the transition as ferromagnetism is stabilized at the expense of antiferromagnetism. We make use of the presence of the two distinct cell volumes of the two magnetic states as a probe to observe by neutron diffraction the evolution of the transition, as the external magnetic field carries the system from the antiferromagnetic to the ferromagnetic state. We show that the large-volume antiferromagnetic and the small-volume ferromagnetic states coexist in the temperature range of the transition. The ferromagnetic state is progressively stabilized as the field increases.

  6. Equilibrium properties of the fluxoid lattice in single-crystal niobium. II. Small-angle neutron-diffraction measurements

    SciTech Connect

    Christen, D.K.; Kerchner, H.R.; Sekula, S.T.; Thorel, P.

    1980-01-01

    A small-angle neutron-diffraction technique has been used to measure several properties of the flux-line lattice (FLL) in a single-crystal sphere of pure niobium. For applied fields parallel to several crystallographic directions in the (100) and (110) planes, the low-field mixed state and intermediate mixed state were investigated. From these results, the orientation dependence of the low-field critical parameters H/sub c/1 and B/sub 0/ are deduced. The consistency of these results is verified by comparison with direct measurements of the equilibrium misalignment angle between the applied-field direction and the fluxoid axes. In addition, results are reported which extend the available information concerning correlations between the FLL and crystal lattice (CL) symmetry properties.

  7. In-situ neutron diffraction of LaCoO{sub 3} perovskite under uniaxial compression. II. Elastic properties

    SciTech Connect

    Lugovy, Mykola; Aman, Amjad; Orlovskaya, Nina; Chen, Yan; Kuebler, Jakob; Graule, Thomas; Reece, Michael J.; Ma, Dong; Stoica, Alexandru D.; An, Ke

    2014-07-07

    Calculations of elastic constants and development of elastic anisotropy under uniaxial compression in originally isotropic polycrystalline LaCoO{sub 3} perovskite are reported. The lattice strains in individual (hkl) planes as well as average lattice strain were determined both for planes oriented perpendicular and parallel to the loading direction using in-situ neutron diffraction. Utilizing average lattice strains as well as lattice strains along the a and c crystallographic directions, an attempt was made to determine Poisson's ratio of LaCoO{sub 3}, which was then compared with that measured using an impulse excitation technique. The elastic constants were calculated and Young's moduli of LaCoO{sub 3} single crystal in different crystallographic directions were estimated.

  8. Polarized Neutron Diffraction to Probe Local Magnetic Anisotropy of a Low-Spin Fe(III) Complex.

    PubMed

    Ridier, Karl; Mondal, Abhishake; Boilleau, Corentin; Cador, Olivier; Gillon, Béatrice; Chaboussant, Grégory; Le Guennic, Boris; Costuas, Karine; Lescouëzec, Rodrigue

    2016-03-14

    We have determined by polarized neutron diffraction (PND) the low-temperature molecular magnetic susceptibility tensor of the anisotropic low-spin complex PPh4 [Fe(III) (Tp)(CN)3 ]⋅H2 O. We found the existence of a pronounced molecular easy magnetization axis, almost parallel to the C3 pseudo-axis of the molecule, which also corresponds to a trigonal elongation direction of the octahedral coordination sphere of the Fe(III) ion. The PND results are coherent with electron paramagnetic resonance (EPR) spectroscopy, magnetometry, and ab initio investigations. Through this particular example, we demonstrate the capabilities of PND to provide a unique, direct, and straightforward picture of the magnetic anisotropy and susceptibility tensors, offering a clear-cut way to establish magneto-structural correlations in paramagnetic molecular complexes. PMID:26890339

  9. Studies of V, Nb, Cr, and Zr substituted 2:17 compounds and their carbides using neutron diffraction

    SciTech Connect

    Luo, H.; Hu, Z.; Chen, M.; Yelon, W.B.; Marasinghe, G.K.; Ezekwenna, P.C.; James, W.J.; Chang, W.C.; Tsai, S.H.

    1997-04-01

    Samples of Nd{sub 2}Fe{sub 17{minus}x}T{sub x}C{sub y} with T=V, Nb, Cr, and Zr were prepared by melting of the constituent elements including C and studied by neutron diffraction. Comparing with their uncarbided counterparts, we found that the substituents transfer, more or less, from the {ital 6c} site to the {ital 18f} and {ital 18h} sites with the introduction of C atoms. This behavior appears to relate to the electronegativities between the C atoms and the early transition series elements because the {ital 18f} and {ital 18h} sites are near neighbors of the interstitial C site. However, the C effects in the V, Nb, Cr, and Zr samples are not as strong as those in Ti samples. SQUID measurements show that the Curie temperatures of these samples depend on both the interstitial C atoms and the substituents. {copyright} {ital 1997 American Institute of Physics.}

  10. Neutron diffraction study of the formation kinetics of ordered antiphase domains in titanium carbohydride TiC x H y

    NASA Astrophysics Data System (ADS)

    Khidirov, I.

    2015-09-01

    The kinetics of formation and growth of ordered antiphase domains (APDs) in titanium carbohydride TiC0.50H0.21 has been investigated by neutron diffraction. A model of ordered APDs is proposed. It is established that the pronounced ordering of interstitial atoms and APDs begin at 450°C. It is shown that the period of ordered APDs ( Р ≈ 10-12) is independent of the exposure time at a constant temperature. It is found that the temperature of ordered APDs, T OAPD, increases nonlinearly with an increase in the carbon concentration in the range 0.50 ≤ C/Ti ≤ 0.70. The formation temperature of ordered APDs is found to correlate with the concentration dependence of the order-disorder transition temperature and be 0.60 of the order-disorder transition temperature: T APD = 0.60 Т С.

  11. In situ neutron diffraction study of the low cycle fatigue of the α-γ duplex stainless steel

    NASA Astrophysics Data System (ADS)

    Jenčuš, Peter; Polák, Jaroslav; Lukáš, Petr; Muránsky, Ondrej

    2006-11-01

    In duplex stainless steels, significant thermal stresses are generated during the cooling from the homogenization temperature due to different thermal expansion coefficients of the austenitic and ferritic phases. The results of the in situ neutron diffraction examination of the evolution of the internal stresses during the low cycle fatigue in the SAF 2507 duplex stainless steel are reported. Stress response of both constituent components resulting from the load sharing between austenitic and ferritic grains was measured. It was found that the initial thermal residual stresses were relaxed rapidly at the beginning of the cyclic loading. Whereas initial hardening was identified in both phases, the subsequent fatigue softening was fully attributed to the austenitic phase.

  12. Neutron Powder Diffraction and Molecular Simulation Study of the Structural Evolution of Ammonia Borane from 15 to 340 K

    SciTech Connect

    Hess, Nancy J.; Schenter, Gregory K.; Hartman, Michael R.; Daemen, Luke L.; Proffen, Thomas E.; Kathmann, Shawn M.; Mundy, Christopher J.; Hartl, Monika A.; Heldebrant, David J.; Stowe, Ashley C.; Autrey, Thomas

    2009-04-17

    The structural behavior of perdeuterated, 11B-enriched ammonia borane, ND311BD3, was investigated by neutron powder diffraction measurements collected over the temperature range from 15 to 340 K and by molecular dynamics simulation. In the low temperature orthorhombic phase, the progressive displacement of the borane group under the amine group was observed leading to the rotation of the B-N bond parallel to the c-axis. The structural phase transition at 225 K is marked by dramatic change in the dynamics of both the amine and borane group that is problematic to extract from the metrics provided by Rietveld analysis of the NPD data alone but is evident in the molecular dynamics simulation and other spectroscopic evidence. This study highlights the valued added by complimentary experimental approaches and coupled computational studies.

  13. Studies of V, Nb, Cr, and Zr substituted 2:17 compounds and their carbides using neutron diffraction

    NASA Astrophysics Data System (ADS)

    Luo, H.; Hu, Z.; Chen, M.; Yelon, W. B.; Marasinghe, G. K.; Ezekwenna, P. C.; James, W. J.; Chang, W. C.; Tsai, S. H.

    1997-04-01

    Samples of Nd2Fe17-xTxCy with T=V, Nb, Cr, and Zr were prepared by melting of the constituent elements including C and studied by neutron diffraction. Comparing with their uncarbided counterparts, we found that the substituents transfer, more or less, from the 6c site to the 18f and 18h sites with the introduction of C atoms. This behavior appears to relate to the electronegativities between the C atoms and the early transition series elements because the 18f and 18h sites are near neighbors of the interstitial C site. However, the C effects in the V, Nb, Cr, and Zr samples are not as strong as those in Ti samples. SQUID measurements show that the Curie temperatures of these samples depend on both the interstitial C atoms and the substituents.

  14. Neutron Powder Diffraction study of the Magnetic Ionic Liquid Emim[FeCL4] and its deuterated phase

    NASA Astrophysics Data System (ADS)

    García-Saiz, A.; de Pedro, I.; Fernández Barquín, L.; Fernández-Díaz, M. T.; Blanco, J. A.; Rodríguez Fernández, J.

    2015-11-01

    A magnetic ionic liquid comprising 1-ethyl-3 methylimidazolium (Emim) cations and tetraclhoroferrate(III) (FeCl4) anions and its deuterated phase were synthetized and characterized magnetically. In both materials, the low temperature dependence of the magnetic susceptibility presents a maximum (around 4 K) related to an antiferromagnetic ordering, but the ordering temperatures are slightly shifted and the curves display different shapes. In addition, the magnetization of the deuterated phase tends to saturate at higher values than that corresponding to the non-deuterated analogue. A comparison of the neutron diffraction patterns above and below the magnetic transition clearly shows that the crystal and magnetic structures of these materials are different. Therefore, the present findings clearly prove that the magnetic exchange interactions that induce three-dimensional magnetic ordering are modified after the deuteration process.

  15. FEA predictions of residual stress in stainless steel compared to neutron and x-ray diffraction measurements. [Finite element analysis

    SciTech Connect

    Flower, E.C.; MacEwen, S.R.; Holden, T.M.

    1987-05-01

    Residual stresses in a body arise from nonuniform plastic deformation and continue to be an important consideration in the design and the fabrication of metal components. The finite element method offers a potentially powerful tool for predicting these stresses. However, it is important to first verify this method through careful analysis and experimentation. This paper describes experiments using neutron and x-ray diffraction to provide quantitative data to compare to finite element analysis predictions of deformation induced residual stress in a plane stress austenitic stainless steel ring. Good agreement was found between the experimental results and the numerical predictions. Effects of the formulation of the finite element model on the analysis, constitutive parameters and effects of machining damage in the experiments are addressed.

  16. Neutron-diffraction study of CD 3ND 3SnBr 3: Semiconductor-insulator transition with orientational ordering

    NASA Astrophysics Data System (ADS)

    Onoda-Yamamuro, N.; Yamamuro, O.; Matsuo, T.; Suga, H.; Oikawa, K.; Tsuchiya, N.; Kamiyama, T.; Asano, H.

    1995-02-01

    Neutron-diffraction experiments were performed on the semiconductor (room-temperature) and insulator (195 K) phases of CD 3ND 3SnBr 3 using a powder diffractometer at KENS. Rietveld refinement revealed fully disordered CD 3ND 3+ ions (rotating like a spherical shell) in the semiconductor phase (Pm3m, Z = 1, a = 5.899Å). The insulator phase has a rhombohedral structure with cell doubling in three directions (R3c or R3¯c, Z = 8, a = 11.767Å, α = 88.997 o) suggesting that the C sbnd N axis of the CD 3ND 3+ ion is ordered along the crystallographic C 3 or 3¯ axis and the SnBr 6 octahedron is distorted from the regular O h symmetry.

  17. Thermodynamic, structural, and dynamic properties of supercooled water confined in mesoporous MCM-41 studied with calorimetric, neutron diffraction, and neutron spin echo measurements

    NASA Astrophysics Data System (ADS)

    Yoshida, Koji; Yamaguchi, Toshio; Kittaka, Shigeharu; Bellissent-Funel, Marie-Claire; Fouquet, Peter

    2008-08-01

    Thermodynamic, structural, and dynamic properties of heavy water (D2O) confined in mesoporous silica glass MCM-41 C10, C12, and C14 were investigated by differential scanning calorimetry, neutron diffraction, and neutron spin echo (NSE) measurements, respectively. The DSC data showed that no crystallization of D2O confined in C10 occurs in a temperature range between 298 and 180 K, and that crystalline ice is formed at 204 and 221 K for C12 and C14, respectively. For C10, the neutron radial distribution functions of confined D2O suggested a structural change in the supercooled state between 223 and 173 K. For C10 sample, it has been found that the tetrahedral-like water structure is partially enhanced in the central part of pores at 173 K. For all the samples, the intermediate scattering functions from the NSE measurements are fitted by the Kohlrausch-Williams-Watts stretched exponential function which implies that confined supercooled D2O exhibits a wide distribution of relaxation times. For C10, C12, and C14 samples, between 298 and 240 K, the relaxation times of supercooled D2O follow remarkably well the Vogel-Fulcher-Tamman equation; for C10 sample, below 240 K, the relaxation times of nonfreezing D2O show an Arrhenius type behavior. From the present experimental results on calorimetric, structural, and dynamic properties, it has been concluded that supercooled D2O confined in MCM-41 C10 experiences a transition from high-density to low-density hydrogen-bonded structure at around 229 K.

  18. Determination of the plane specific elastic constants of Waspaloy using neutron diffraction

    SciTech Connect

    Stone, H.J.; Reed, R.C.; Holden, T.M.

    1999-01-08

    In the present paper, the plane specific elastic constants for Waspaloy, a high strength nickel-base superalloy, have been determined with a considerable degree of precision. For this purpose, in-situ tensile tests have been carried out in a neutron diffractometer. The data which are reported are of considerable significance, since they allow an accurate determination of the residual stress slate from an estimate of the local d-spacing from the hkl lattice reflection. Thus, the data should be of interest to those interested in the determination of the residual stress state in components which are fabricated from Waspaloy, and nickel-base superalloys in general.

  19. A neutron diffraction study of hydrogen positions at 13 K, domain model, and chemical composition of staurolite

    NASA Astrophysics Data System (ADS)

    Ståhl, K.; Kvick, Å.; Smith, J. V.

    1988-04-01

    Comparison of new neutron and old X-ray diffraction data for single crystals of staurolite from Pizzo Forno yielded unique answers to some, but not all, outstanding structural questions. Neutron data were collected at 13(1) K for a crystal with assumed composition Li 0.07Mg 0.87Ti 0.14V 0.01Cr 0.01Mn 0.04Fe 2+3.00 Fe 3+0.06Co 0.01Zn 0.05Al 17.69Si 7.67O 48H 3.41F 0.01, Mw = 1671, a = 7.8639(10), b = 16.625(2), c = 5.651(2) Å, β = 90.015(14)°, {C2}/{m}, Z = 1, D x = 3.75 g cm-3; 1874 (1024 unique) reflections, λ = 1.1598(1) Å, R( F) = 3.3%. The diffraction evidence is consistent with full occupancy of the Si, Al(1), Al(2), and Al(3) sites, but not of the other ones. Detailed assignment of atoms is based on diffraction evidence and crystal-chemical arguments, but some uncertainties remain; thus exchange of (Li + Fe) by two Mg would have little effect on diffraction data. A structural model with three types of domains is proposed: ˜63% type 1, (Fe, etc.) + H(1); ˜22% type 2, (Mg, etc.) + H(2); ˜15% type 3, (Fe, etc.) without hydrogen. For the orthorhombic pseudostructure, the occupancies of the two hydrogen sites place strong restrictions on the other site occupancies. The 25(4)% observed occupancy of H(2) limits the occupancy of the nearby (Fe, etc.) site to a maximum of 75(4)%. To explain the neutron scattering, the Fe site must be occupied mainly by Fe; Li, Mn, Zn, and Mg may also occupy this site. A good ionic balance is attained for the type 2 domain if the U site from the old X-ray work is occupied simultaneously with H(2). To match the neutron data, assignment of 21(2)% Mg to the U site is plausible, but other substituents are possible. H(2) lies directly between two O(1) atoms at ˜0.9 and 2.3 Å, and H(1) is displaced away from the Fe site so that it is bonded to one O(1) at 1.01 Å and one O(3) at 2.07 Å. Four-fifths of the Fe atoms should be displaced from z = 0.25 because of electrostatic repulsion from H(1), and one-fifth should not be. This is

  20. Visualizing the Structural Evolution of LSM/xYSZ Composite Cathodes for SOFC by in-situ Neutron Diffraction

    PubMed Central

    Chen, Yan; Yang, Ling; Ren, Fei; An, Ke

    2014-01-01

    Thermal stability of composite cathodes for solid oxide fuel cells, the mixtures of (La0.8Sr0.2)0.95MnO3−δ (LSM) and (Y2O3)x(ZrO2)1−x (xYSZ, x = 3, 6, 8 and 10), is determined using in-situ neutron diffraction. Thanks to the most advanced high flux neutron source, our work highlights the visualization of the phase evolutions in heterogeneous material systems at high temperatures, along with the analysis of the diffusion activities of transition metal ions that reveal the reaction mechanism and kinetics. It is found that the tetragonal-to-cubic phase transition in YSZ at T > 900°C leads to a heterogeneous redistribution of Mn ions. The subsequent reaction of LSM and YSZ occurring at T > 1100°C is revealed as a three-stage kinetic process, yielding La2Zr2O7, SrZrO3 and MnO. The diffusion activities of Y, Mn and La ions in the heterogeneous systems at elevated temperatures are derived by the structural analysis, and the three-stage reaction of YSZ and LSM is found strongly correlated to ions' behaviors as functions of temperature. PMID:24899139

  1. Hemoglobin redux: combining neutron and X-ray diffraction with mass spectrometry to analyse the quaternary state of oxidized hemoglobins

    PubMed Central

    Mueser, Timothy C.; Griffith, Wendell P.; Kovalevsky, Andrey Y.; Guo, Jingshu; Seaver, Sean; Langan, Paul; Hanson, B. Leif

    2010-01-01

    Improvements in neutron diffraction instrumentation are affording the opportunity to re-examine the structures of vertebrate hemoglobins and to interrogate proton and solvent position changes between the different quaternary states of the protein. For hemoglobins of unknown primary sequence, structural studies of cyanomethemoglobin (CNmetHb) are being used to help to resolve sequence ambiguity in the mass spectra. These studies have also provided additional structural evidence for the involvement of oxidized hemoglobin in the process of erythrocyte senescence. X-ray crystal studies of Tibetan snow leopard CNmetHb have shown that this protein crystallizes in the B state, a structure with a more open dyad, which possibly has relevance to RBC band 3 protein binding and erythrocyte senescence. R-state equine CNmetHb crystal studies elaborate the solvent differences in the switch and hinge region compared with a human deoxyhemoglobin T-­state neutron structure. Lastly, comparison of histidine protonation between the T and R state should enumerate the Bohr-effect protons. PMID:21041946

  2. Hemoglobin redux: combining neutron and X-ray diffraction with mass spectrometry to analyse the quaternary state of oxidized hemoglobins.

    PubMed

    Mueser, Timothy C; Griffith, Wendell P; Kovalevsky, Andrey Y; Guo, Jingshu; Seaver, Sean; Langan, Paul; Hanson, B Leif

    2010-11-01

    Improvements in neutron diffraction instrumentation are affording the opportunity to re-examine the structures of vertebrate hemoglobins and to interrogate proton and solvent position changes between the different quaternary states of the protein. For hemoglobins of unknown primary sequence, structural studies of cyanomethemoglobin (CNmetHb) are being used to help to resolve sequence ambiguity in the mass spectra. These studies have also provided additional structural evidence for the involvement of oxidized hemoglobin in the process of erythrocyte senescence. X-ray crystal studies of Tibetan snow leopard CNmetHb have shown that this protein crystallizes in the B state, a structure with a more open dyad, which possibly has relevance to RBC band 3 protein binding and erythrocyte senescence. R-state equine CNmetHb crystal studies elaborate the solvent differences in the switch and hinge region compared with a human deoxyhemoglobin T-state neutron structure. Lastly, comparison of histidine protonation between the T and R state should enumerate the Bohr-effect protons. PMID:21041946

  3. Neutron Diffraction on NaNi2 BiO6 : Complex Interactions on a Honeycomb Lattice

    NASA Astrophysics Data System (ADS)

    Scheie, Allen; Ross, Kate; Seibel, Elizabeth; Rodriguez-Rivera, Jose; Broholm, Collin; Cava, Robert; Institute for Quantum Matter Collaboration

    Magnetic crystals with a honeycomb lattice can have a very high degree of frustration when next-nearest neighbor interactions are strong. Such complex interactions can lead to Kitaev model physics, including a proposed spin liquid phase. Using neutron scattering, we studied the magnetic properties of a new spin-1/2 honeycomb compound, NaNi2BiO6, which was known to have heat capacity peaks indicative of a phase transition at 5 K. The magnetic order indicates beyond nearest-neighbor exchange as well as significant inter-plane interaction, which allows for a study of rich and complex structure. In this talk I report the magnetic structure of the compound as found with neutron powder diffraction, and discuss the exchanges necessary to lead to such a complex order. The work at IQM was supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Division of Material Sciences and Engineering, under Grant No. DEFG02-08ER46544.

  4. Strain and texture measurements on geological samples using neutron diffraction at IBR-2, Joint Institute for Nuclear Research, Dubna (Russia)

    NASA Astrophysics Data System (ADS)

    Frischbutter, A.; Janssen, Ch.; Scheffzük, Ch.; Walther, K.; Ullemeyer, K.; Behrmann, J. H.; Nikitin, A. N.; Ivankina, T. I.; Kern, H.; Leiss, B.

    2006-12-01

    Information on texture and residual stress in geological samples is very important for the calculation of physical properties connected with the evaluation of the geomechanical behavior of parts of the earths’s crust in connection with processes from human activities (mining, tunnelling) and natural processes of deformation (seismicity, earthquakes). Texture and stress are not independent of each other and in the general case should be analyzed together. Complications arise because geological samples are generally composed of several phases (minerals) whose elastic constants may be significantly different. Nevertheless, modern neutron diffractometers such as SKAT and EPSILON-MDS at the fast pulsed reactor IBR-2 at the FLNP of the JINR make it possible to obtain the needed diffraction patterns. This was shown especially for texture measurements on samples with quartz as the main component as well as for mica, feldspar, amphibole, and several other minerals. In order to extend strain measurements beyond samples composed of quartz, dolomite, and/or anhydrite to such frequently occurring minerals as feldspars and mica it would be necessary on the one hand to use Rietveld refinement with corrections due to texture and anisotropic peak broadening. With an increase in the number of mineral phases suitable for these diffractometers, it is in general necessary to improve the experimental conditions for SKAT and EPSILON-MDS, especially to significantly raise the flux of incident neutrons on the sample.

  5. In situ stress measurement of fiber reinforced composite in low temperature state by neutron diffraction

    NASA Astrophysics Data System (ADS)

    Nishida, Masayuki; Jing, Tian; Muslih, M. Refai; Doi, Taisei; Matsue, Tatsuya; Hanabusa, Takao

    2015-03-01

    The tungsten fiber reinforced titanium composite (W/Ti) was produced by the spot welding method. The internal stress alteration of the W/Ti composite was measured by the neutron diffractometer, DN1, which had been installed at beam port #6 in National Nuclear Energy Agency Indonesia. The two-dimensional detector and cryostat system were mounted on the DN1 diffractometer, and the residual stress alterations were measured by the in situ neutron stress measurement technique under the cooling cycles from 300 K to 10 K. Residual stresses in tungsten fiber were investigated at several temperatures. In the longitudinal fiber direction, the thermal residual stresses of tungsten fiber became a large compressive state and represented the maximum value is about -950 MPa. The calculated results of the simple elastic model agreed with the experimental results of the in situ thermal stress measurement qualitatively. It is assumed that the stresses in the fiber longitudinal direction are the dominant stresses in the W/Ti composite.

  6. Residual stress measurements of welded components using synchrotron and neutron diffraction.

    SciTech Connect

    Paradowska, A. M.; Price, J. W .H; Finlayson, T. R.; Lienert, U.; Ibrahim, R.; Monash Univ.; Univ. of Melbourne

    2007-01-01

    Residual stress remains the single largest unknown in industrial damage situations. Residual stresses have a significant effect on corrosion, fracture resistance, creep and corrosion/fatigue performance and a reduction of these stresses is normally desirable. In this research high energy synchrotron (70 keV) radiation (at the Advanced Photon Source) and thermal neutrons (at the Lucas Heights Research Reactor) have been employed to investigate and compare the residual stress characteristics in fully restrained samples with different numbers of weld beads. The aim of the research was to characterize the residual stress distribution which arises in a welded component with increasing number of beads. The number and resolution of the measurements carried out in this work reveal significant features of the residual stress pattern in single bead in the as-welded condition and after post-weld heat treatment. The intention is to provide key data for the validation of design, fitness-for-purpose methodologies and finite-element tools. In this presentation the details of the synchrotron X-ray and neutron techniques will be compared and contrasted, utilizing results from a number of weldment samples.

  7. Measurement of residual stress fields in FHPP welding: a comparison between DSPI combined with hole-drilling and neutron diffraction

    NASA Astrophysics Data System (ADS)

    Viotti, Matias R.; Albertazzi, Armando; Staron, Peter; Pisa, Marcelo

    2013-04-01

    This paper shows a portable device to measure mainly residual stress fields outside the optical bench. This system combines the traditional hole drilling technique with Digital Speckle Pattern Interferometry. The novel feature of this device is the high degree of compaction since only one base supports simultaneously the measurement module and the hole-drilling device. The portable device allows the measurement of non-uniform residual stresses in accordance with the ASTM standard. In oil and gas offshore industries, alternative welding procedures among them, the friction hydro pillar processing (FHPP) is highlighted and nowadays is an important maintenance tool since it has the capability to produce structure repairs without risk of explosions. In this process a hole is drilled and filled with a consumable rod of the same material. The rod, which could be cylindrical or conical, is rotated and pressed against the hole, leading to frictional heating. In order to assess features about the residual stress distribution generated by the weld into the rod as well as into the base material around the rod, welded samples were evaluated by neutron diffraction and by the hole drilling technique having a comparison between them. For the hole drilling technique some layers were removed by using electrical discharge machining (EDM) after diffraction measurements in order to assess the bulk stress distribution. Results have shown a good agreement between techniques.

  8. Local order and orientational correlations in liquid and crystalline phases of carbon tetrabromide from neutron powder diffraction measurements

    NASA Astrophysics Data System (ADS)

    Temleitner, L.; Pusztai, L.

    2010-04-01

    The liquid, plastic crystalline and ordered crystalline phases of CBr4 were studied using neutron-powder diffraction. The measured total scattering differential cross sections were modeled by reverse Monte Carlo simulation techniques ( RMC++ and RMCPOW). Following successful simulations, the single-crystal-diffraction pattern of the plastic phase as well as partial radial distribution functions and orientational correlations for all the three phases have been calculated from the atomic coordinates (particle configurations). The single-crystal pattern, calculated from a configuration that had been obtained from modeling the powder pattern, shows identical behavior to the recent single-crystal data of Folmer [Phys. Rev. B 77, 144205 (2008)]. The BrBr partial radial-distribution functions of the liquid and plastic crystalline phases are almost the same while CC correlations clearly display long-range ordering in the latter phase. Orientational correlations also suggest strong similarities between liquid and plastic crystalline phases whereas the monoclinic phase behaves very differently. Orientations of the molecules are distinct in the ordered phase whereas in the plastic crystal their distribution seems to be isotropic.

  9. Micromechanical Behavior of Solid-Solution-Strengthened Mg-1wt.%Al Alloy Investigated by In-Situ Neutron Diffraction

    SciTech Connect

    Lee, Sooyeol; Woo, Wanchuck; Gharghouri, Michael; Yoon, Cheol; An, Ke

    2014-01-01

    In-situ neutron-diffraction experiments were employed to investigate the micromechanical behavior of solid-solution-strengthened Mg-1wt.%Al alloy. Two starting textures were used: 1) as-extruded then solutionized texture, T1, in which the basal poles of most grains are tilted around 70~85 from the extrusion axis, and 2) a reoriented texture, T2, in which the basal poles of most grains are tilted around 10~20 from the extrusion axis. Lattice strains and diffraction peak intensity variations were measured in situ during loading-unloading cycles in uniaxial tension. Twinning activities and stress states for various grain orientations were revealed. The results show that the soft grain orientations, favorably oriented for either extension twinning or basal slip, exhibit the stress relaxation, resulting in the compressive residual strain after unloading. On the other hand, the hard grain orientations, unfavorably oriented for both extension twinning and basal slip, carry more applied load, leading to much higher lattice strains during loading followed by tensile residual strains upon unloading.

  10. Single crystal neutron diffraction study of the magnetic structure of TmNi{sub 2}B{sub 2}C

    SciTech Connect

    Sternlieb, B.; Shapiro, S.; Stassis, C.; Goldman, A.I.; Canfield, P.

    1997-02-01

    Neutron diffraction techniques have been used to study the magnetic structure of single crystals of the magnetic superconductor (T{sub c} {congruent} 11K) TmNi{sub 2}B{sub 2}C. We find that below approximately 1.5K the magnetic moments order in an incommensurate spin wave with propagation vector q{sub m} = q{sub m} (a* +b*) (or q{sub m} = q{sub m} (a* + b*)) with q{sub m} = 0.094 {+-} 0.001. The spin wave is transverse with the moments aligned along the c-axis, and the observation of relatively intense higher order harmonics shows that the modulation is not purely sinusoidal but considerably squared. This incommensurate magnetic structure, which coexists with superconductivity below T{sub N} {congruent} 1.5K, is quite different from those observed in the magnetic superconductors HoNi{sub 2}B{sub 2}C and ErNi{sub 2}B{sub 2}C. The origin of diffraction peaks observed in scans parallel to a* is briefly discussed.

  11. Polarised antibranes from Smarr relations

    NASA Astrophysics Data System (ADS)

    Cohen-Maldonado, Diego; Diaz, Juan; Gautason, Fridrik Freyr

    2016-05-01

    We study the backreaction of smeared and localised anti M2-branes placed at the tip of the CGLP background. To this end we derive a Smarr relation for backreacted antibranes at zero and finite temperature. For extremal antibranes we show that if smeared they cannot have regular horizons, whereas localised M2-branes can potentially be regular when polarised into M5-branes, in agreement with the probe result of Klebanov and Pufu. We further discuss antibranes at finite temperature and argue that localised antibrane solutions with regular horizons are not excluded.

  12. Synthesis, x-ray, and low-temperature neutron diffraction study of a rhodium (V) complex: dihydridobis(triethylsilyl)-pentamethylcyclopentadienylrhodium

    SciTech Connect

    Fernandez, M.J.; Bailey, P.M.; Bentz, P.O.; Ricci, J.S.; Koetzle, T.F.; Maitlis, P.M.

    1984-09-19

    Reaction of (C/sub 5/ qentamethyl Rh)/sub 2/Cl/sub 4/) (1) with triethylsilane leads to the novel rhodium(V) complex (eta/sup 5/-C/sub 5/Me/sub 5/Rh(H)/sub 2/(SiE-triethyl/sub 3/)/sub 2/) (2) characterized by NMR spectra (/sup 1/H, /sup 13/C, /sup 29/Si, and /sup 103/Rh), X-ray diffraction, and neutron diffraction at 20 K. The complex shows a four-legged piano stool geometry with the pentamethylcyclopentadienyl eta/sub 5/-bonded to the rhodium (average Rh-C, 2.283 (9) A) on top and the two triethylsilyl ligands trans in the basal plane (Rh-Si, 2.379 (2) A). The neutron diffraction analysis located the two hydrides, which are trans to each other and cis to the triethylsilyls in the basal plane. The mean Rh-H distance is 1.581 (3) A, and the H-Rh-H angle is 94.8 (2)/sup 0/. Complex 2 is rather stable, but it reacts under forcing conditions with neutral ligands (triphenylphosphine, CO, or maleic anhydride) to give (C/sub 5/Me/sub 5/Rh(PPh/sub 3/)H(SiEt/sub 3/)), (C/sub 5/Me/sub 5/Rh(CO)/sub 2/), or (C/sub 5/M3/5Rh(maleic anhydride)/sup 2/). It reacts more easily with electrophiles such as HBF/sub 4/ to give (C/sub 5/Me/sub 5/Rh)/sub 4/H/sub 4/)/sup 2 +/, with HCl to give 1, with AgBF/sub 4/ in MeCN to give (C/sub 5/Me/sub 5/Rh(MeCN)/sub 3/)/sup 2 +/, and with I/sub 2/ to give ((C/sub 5/Me/sub 5/Rh)/sub 2/I/sub 4/). The predominant mode of reaction involves reductive elimination of Et/sub 3/Si-H, which can be strongly promoted by an electrophile. 43 references, 3 figures, 3 tables.

  13. Study of clathrate hydrates via equilibrium molecular-dynamics simulation employing polarisable and non-polarisable, rigid and flexible water models.

    PubMed

    Burnham, Christian J; English, Niall J

    2016-04-28

    Equilibrium molecular-dynamics (MD) simulations have been performed on metastable sI and sII polymorphs of empty hydrate lattices, in addition to liquid water and ice Ih. The non-polarisable TIP4P-2005, simple point charge model (SPC), and polarisable Thole-type models (TTM): TTM2, TTM3, and TTM4 water models were used in order to survey the differences between models and to see what differences can be expected when polarisability is incorporated. Rigid and flexible variants were used of each model to gauge the effects of flexibility. Power spectra are calculated and compared to density-of-states spectra inferred from inelastic neutron scattering (INS) measurements. Thermodynamic properties were also calculated, as well as molecular-dipole distributions. It was concluded that TTM models offer optimal fidelity vis-à-vis INS spectra, together with thermodynamic properties, with the flexible TTM2 model offering optimal placement of vibrational modes. PMID:27131553

  14. Study of clathrate hydrates via equilibrium molecular-dynamics simulation employing polarisable and non-polarisable, rigid and flexible water models

    NASA Astrophysics Data System (ADS)

    Burnham, Christian J.; English, Niall J.

    2016-04-01

    Equilibrium molecular-dynamics (MD) simulations have been performed on metastable sI and sII polymorphs of empty hydrate lattices, in addition to liquid water and ice Ih. The non-polarisable TIP4P-2005, simple point charge model (SPC), and polarisable Thole-type models (TTM): TTM2, TTM3, and TTM4 water models were used in order to survey the differences between models and to see what differences can be expected when polarisability is incorporated. Rigid and flexible variants were used of each model to gauge the effects of flexibility. Power spectra are calculated and compared to density-of-states spectra inferred from inelastic neutron scattering (INS) measurements. Thermodynamic properties were also calculated, as well as molecular-dipole distributions. It was concluded that TTM models offer optimal fidelity vis-à-vis INS spectra, together with thermodynamic properties, with the flexible TTM2 model offering optimal placement of vibrational modes.

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

    SciTech Connect

    Fujiwara, Satoru; Mendelson, R.A.

    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.

  16. Ferroelastic phase transition in Cs3Bi2I9: A neutron diffraction study

    NASA Astrophysics Data System (ADS)

    Jorio, A.; Currat, R.; Myles, D. A. A.; McIntyre, G. J.; Aleksandrova, I. P.; Kiat, J. M.; Saint-Grégoire, P.

    2000-02-01

    Crystalline Cs3Bi2I9, with the P63/mmc symmetry at room temperature was studied by Laue and four-circle neutron diffractometry from room temperature down to 50 K. At T0=220 K the crystal undergoes a second-order proper ferroelastic phase transition to a polydomain structure with a nonprimitive monoclinic C12/m1 space group. Satellites were not found below T0, indicating that the continuous distribution of sites observed in previous 127I nuclear quadrupole resonance experiments is due either to an undetected incommensurate phase characterized by a very small displacement amplitude, or due to the fraction of the crystal volume occupied by domain walls. We argue that thick domain walls are expected in the present structure due to the absence of mechanical compatibility between domains.

  17. Neutron-diffraction study of PuAs and PuSb

    NASA Astrophysics Data System (ADS)

    Burlet, P.; Quezel, S.; Rossat-Mignod, J.; Spirlet, J. C.; Rebizant, J.; Müller, W.; Vogt, O.

    1984-12-01

    The first neutron scattering experiments on PuAs and PuSb single crystals are reported. PuAs is found to be a ferromagnet below Tc=123+/-1 K. PuSb develops below TN=85+/-1 K an incommensurate ordering and undergoes, at TIC=67 K, a first-order transition to a commensurate phase, ferromagnetic in nature. In both compounds, moments are perpendicular to the ferromagnetic (001) planes, their low-temperature value is μ=(0.75+/-0.1)μB, indicating a Γ8-type ground state within the Russell-Saunders level scheme. The magnetic phase diagram of PuSb has been determined. The incommensurate phase is suppressed by a small field of 8.5 kOe.

  18. Neutron powder diffraction study of the layer organic-inorganic hybrid iron(II) methylphosphonate-hydrate, Fe[(CD 3PO 3)(D 2O)

    NASA Astrophysics Data System (ADS)

    Léone, Philippe; Bellitto, Carlo; Bauer, Elvira M.; Righini, Guido; André, Gilles; Bourée, Françoise

    2008-11-01

    The crystal and magnetic structures of the hybrid organic-inorganic layer compound Fe[(CD 3PO 3)(D 2O)] have been studied by neutron powder diffraction as a function of temperature down to 1.5 K. The neutron diffraction pattern recorded at 200 K shows that the fully deuterated compound crystallizes in one of the two known forms of the undeuterated Fe[(CH 3PO 3)(H 2O)]. The crystal structure is orthorhombic, space group Pmn2 1, with the following unit-cell parameters: a=5.7095(1) Å, b=8.8053(3) Å and c=4.7987(1) Å; Z=2. The crystal structure remains unchanged on cooling from 200 to 1.5 K. Moreover, at low temperature, Fe[(CD 3PO 3)(D 2O)] shows a commensurate magnetic structure ( k=(0,0,0)). As revealed by bulk susceptibility measurements on Fe[(CH 3PO 3)(H 2O)], the magnetic structure corresponds to a canted antiferromagnet with a critical temperature TN=25 K. Neutron powder diffraction reveals that below TN=23.5 K the iron magnetic moments in Fe[(CD 3PO 3)(D 2O)] are antiferromagnetically coupled and oriented along the b-axis, perpendicular to the inorganic layers. No ferromagnetic component is observable in the neutron powder diffraction experiment, due to its too small value (<0.1 μB).

  19. A simple homemade polarised sunglasses test card

    NASA Astrophysics Data System (ADS)

    Bamdad, Farzad

    2016-05-01

    In this article construction of a simple and inexpensive test card which can be used to demonstrate the polarisation ability of sunglasses is described. The card was fabricated simply by using a piece of polariser sheet with one to three layers of cellophane tape fixed on it.

  20. A Simple Homemade Polarised Sunglasses Test Card

    ERIC Educational Resources Information Center

    Bamdad, Farzad

    2016-01-01

    In this article construction of a simple and inexpensive test card which can be used to demonstrate the polarisation ability of sunglasses is described. The card was fabricated simply by using a piece of polariser sheet with one to three layers of cellophane tape fixed on it.

  1. Polarisation of Social Studies Textbooks in Pakistan

    ERIC Educational Resources Information Center

    Zaidi, Syed Manzar Abbas

    2011-01-01

    This article looks at the evolution of the social studies curricula in Pakistan, which are of critical importance in shaping the outlook of many young Pakistanis, who are affected by this polarised discourse. The author argues that this trend of polarisation springing from dynamics of education also effectively contributes to a widening social…

  2. Determination of the temperature dependence of the lattice parameters of cementite by neutron diffraction

    SciTech Connect

    Reed, R.C.; Root, J.H.

    1997-12-18

    The structure and behavior of the cementite phase has a profound effect on the properties of steels and cast irons. For example, the size and distribution of cementite particles is known to influence the fracture and fatigue behavior of steels. Cementite plays a critical role in various phase transformations in the system, for example the pearlite and bainite reactions. Recently, it has been shown that cementite plays an important role in the process of austenite formation which occurs when the eutectoid temperature is exceeded. Despite the importance of the cementite phase in the context of ferrous metallurgy, it appears that little emphasis has been placed on determining the dependence of the lattice parameters on temperature. The results which are available have been determined using X-ray diffractometry, which can be subject to systematic errors arising from (i) specimen height misalignments, and (ii) temperature inhomogeneities. The purpose of the present paper is to report data from a high purity Fe-C hypereutectoid steel, which were obtained using high-resolution neutron diffractometry. The cementite is thus in equilibrium with the matrix phase, even above the eutectoid temperature, and this allows measurements to be obtained with a considerable degree of precision.

  3. Laue diffraction: The key to neutron crystallography from submillimetric-volume single crystals

    NASA Astrophysics Data System (ADS)

    Lemée-Cailleau, M.-H.; McIntyre, G. J.; Wilkinson, C.

    2005-12-01

    For several decades, chemists and physicists have been fascinated by molecular compounds rich in delocalized electrons. In the solid state these compounds may offer a very rich fan of properties: optical, conduction and dielectric, magneticldots Each state is the result of a delicate balance amongst intra- and/or intermolecular interactions which can be controlled, not just by direct chemical substitution, but also by external parameters such as temperature, pressure, continuous electric or magnetic fields, or by light. The recent evolution of this field of science towards more and more sophisticated materials makes also more and more difficult their crystal growth. While neutron scattering is an extremely powerful technique to get precise structural information, it is also often disregarded in this field because usually large single crystals are required. With the recent renaissance of Laue techniques using the very intense flux provided by the reactor of the Institut Laue-Langevin (ILL), accurate structural and/or magnetic information can be now extracted routinely from molecular crystals of volume 0.1 mm3 or smaller, with easy possibilities of high pressure (up to 3 GPa) down to 0.2 K. A general survey of these new possibilities is illustrated by an example taken from the field of low-dimensional organic complexes.

  4. Crystal structures of deuterated sodium molybdate dihydrate and sodium tungstate dihydrate from time-of-flight neutron powder diffraction.

    PubMed

    Fortes, A Dominic

    2015-07-01

    Time-of-flight neutron powder diffraction data have been measured from ∼90 mol% deuterated isotopologues of Na2MoO4·2H2O and Na2WO4·2H2O at 295 K to a resolution of sin (θ)/λ = 0.77 Å(-1). The use of neutrons has allowed refinement of structural parameters with a precision that varies by a factor of two from the heaviest to the lightest atoms; this contrasts with the X-ray based refinements where precision may be > 20× poorer for O atoms in the presence of atoms such as Mo and W. The accuracy and precision of inter-atomic distances and angles are in excellent agreement with recent X-ray single-crystal structure refinements whilst also completing our view of the hydrogen-bond geometry to the same degree of statistical certainty. The two structures are isotypic, space-group Pbca, with all atoms occupying general positions, being comprised of edge- and corner-sharing NaO5 and NaO6 polyhedra that form layers parallel with (010) inter-leaved with planes of XO4 (X = Mo, W) tetra-hedra that are linked by chains of water mol-ecules along [100] and [001]. The complete structure is identical with the previously described molybdate [Capitelli et al. (2006 ▸). Asian J. Chem. 18, 2856-2860] but shows that the purported three-centred inter-action involving one of the water mol-ecules in the tungstate [Farrugia (2007 ▸). Acta Cryst. E63, i142] is in fact an ordinary two-centred 'linear' hydrogen bond. PMID:26279871

  5. A high-temperature neutron diffraction study of Nb2AlC and TiNbAlC

    DOE PAGESBeta

    Bentzel, Grady W.; Lane, Nina J.; Vogel, Sven C.; An, Ke; Barsoum, Michel W.; Caspi, El'ad N.

    2014-12-16

    In this paper, we report on the crystal structures of Nb2AlC and TiNbAlC actual composition (Ti0.45,Nb0.55)2AlC compounds determined from Rietveld analysis of neutron diffraction patterns in the 300-1173 K temperature range. The average linear thermal expansion coefficients of a Nb2AlC sample in the a and c directions are, respectively, 7.9(5)x10-6 K-1 and 7.7(5)x10-6 K-1 on one neutron diffractometer and 7.3(3)x10-6 K-1 and 7.0(2)x10-6 K-1 on a second diffractometer. The respective values for the (Ti0.45,Nb0.55)2AlC composition - only tested on one diffractometer - are 8.5(3)x10-6 K-1 and 7.5(5)x10-6 K-1. These values are relatively low compared to other MAX phases. Like othermore » MAX phases, however, the atomic displacement parameters show that the Al atoms vibrate with higher amplitudes than the Ti and C atoms, and 1 more along the basal planes than normal to them. In addition, when the predictions of the atomic displacement parameters obtained from density functional theory are compared to the experimental results, good quantitative agreement is found for the Al atoms. In case of the Nb and C atoms, the agreement was more qualitative.« less

  6. Crystal structures of deuterated sodium molybdate dihydrate and sodium tungstate dihydrate from time-of-flight neutron powder diffraction

    PubMed Central

    Fortes, A. Dominic

    2015-01-01

    Time-of-flight neutron powder diffraction data have been measured from ∼90 mol% deuterated isotopologues of Na2MoO4·2H2O and Na2WO4·2H2O at 295 K to a resolution of sin (θ)/λ = 0.77 Å−1. The use of neutrons has allowed refinement of structural parameters with a precision that varies by a factor of two from the heaviest to the lightest atoms; this contrasts with the X-ray based refinements where precision may be > 20× poorer for O atoms in the presence of atoms such as Mo and W. The accuracy and precision of inter­atomic distances and angles are in excellent agreement with recent X-ray single-crystal structure refinements whilst also completing our view of the hydrogen-bond geometry to the same degree of statistical certainty. The two structures are isotypic, space-group Pbca, with all atoms occupying general positions, being comprised of edge- and corner-sharing NaO5 and NaO6 polyhedra that form layers parallel with (010) inter­leaved with planes of XO4 (X = Mo, W) tetra­hedra that are linked by chains of water mol­ecules along [100] and [001]. The complete structure is identical with the previously described molybdate [Capitelli et al. (2006 ▸). Asian J. Chem. 18, 2856–2860] but shows that the purported three-centred inter­action involving one of the water mol­ecules in the tungstate [Farrugia (2007 ▸). Acta Cryst. E63, i142] is in fact an ordinary two-centred ‘linear’ hydrogen bond. PMID:26279871

  7. Neutron diffraction study of monoclinic brannerite-type CoV{sub 2}O{sub 6}

    SciTech Connect

    Markkula, Mikael; Arevalo-Lopez, Angel M.; Paul Attfield, J.

    2012-08-15

    A variable-temperature powder neutron diffraction study of the monoclinic brannerite-type CoV{sub 2}O{sub 6} (space group C2/m, a=9.2531(2), b=3.5040(1), c=6.6201(1) A and {beta}=111.617(1) Degree-Sign at 300 K) is reported. No structural transition is observed down to 4 K, but a magnetostriction accompanying antiferromagnetic order at T{sub N}=15 K is discovered. Antiferromagnetic order observed below T{sub N} has an a Multiplication-Sign b Multiplication-Sign 2c supercell in which Co{sup 2+} moments of magnitude 4.77(4) {mu}{sub B} at 4 K lie in the ac plane and are ferromagnetically coupled within chains of edge-sharing CoO{sub 6} octahedra parallel to b. Ferromagnetic chains are coupled antiferromagnetically to neighbouring chains in the a and c directions, and a model for the interchain order in the reported 1/3 magnetization plateau region is proposed. - Graphical abstract: Antiferromagnetic order of Co{sup 2+} moments in monoclinic brannerite type CoV2O6 results in a magnetostriction at the 15 K Neel transition. An alternative coupling between ferromagnetic chains is proposed to account for a 1/3 magnetization plateau in this material. Highlights: Black-Right-Pointing-Pointer Variable-temperature powder neutron diffraction study of the monoclinic brannerite-type CoV{sub 2}O{sub 6} is reported. Black-Right-Pointing-Pointer Magnetostriction accompanying antiferromagnetic order at T{sub N}=15 K in monoclinic CoV{sub 2}O{sub 6} is discovered. Black-Right-Pointing-Pointer Antiferromagnetic order in a Multiplication-Sign b Multiplication-Sign 2c supercell of CoV{sub 2}O{sub 6} is determined. Black-Right-Pointing-Pointer Model for spin order in the reported 1/3 magnetization plateau of CoV{sub 2}O{sub 6} is proposed.

  8. Powder Neutron Diffraction Study of the Thermal Expansion of Mirabilite, Na2SO4.10H2O

    NASA Astrophysics Data System (ADS)

    Brand, H. E.; Fortes, A. D.; Wood, I. G.; Knight, K. S.; Vocadlo, L.

    2006-12-01

    The presence of salts such as MgSO4 and Na2SO4 in chondritic meteorites has led to the suggestion that the water-rich icy moons of the Gas Giant planets are likely to be dominated by multiply hydrated salts such as Fritzsche's salt (MgSO4.11H2O), epsomite (MgSO4.7H2O) and mirabilite (Na2SO4.10H2O). Moreover, hydrated sulfates are likely to be important rock-forming minerals and water storage reservoirs on Mars. When constructing models of icy moons to explore their structure and evolution, it is therefore extremely important to know the phase behaviour and physical properties of the constituent materials under the appropriate pressure and temperature regimes (0 < P < 5 GPa, and 100 < T < 300 K). We are therefore engaged in a programme of study to measure the physical characteristics of candidate materials using a combination of neutron diffraction and computational chemistry. Neutrons are powerful probes of low molecular-weight solids, hydrogen-bearing species in particular, and their penetrative power allows one to study materials even in complex sample environments, such as pressure cells and cryostats. In practice, we measure the variation in molar volume of a solid as a function of pressure and temperature; this leads to derivatives in P and T, such as thermal expansivity and compressibility. Furthermore, we can observe phase transitions in situ, and collect diffraction data which may lead to a successful solution of the new polymorph's structure. In this contribution, we present the results of work to investigate the structure and thermoelastic properties of mirabilite. We have determined the ambient pressure thermal expansion tensor and investigated the low- temperature structural disorder of deuterated mirabilite from 4 - 300K. The volume expansion is positive and this is echoed by the expansion of the a and c axes. However, the b axis shows a small negative thermal expansion below 50K. Very similar behaviour is seen in MgSO4.7H2O and MgSO4.11H2O (Fortes et

  9. Development of a Neutron Diffraction Based Experiemental Capability for Investigating Hydraulic Fracturing for EGS-like Conditions

    SciTech Connect

    Polsky, Yarom; Anovitz, Lawrence {Larry} M; An, Ke; Carmichael, Justin R; Bingham, Philip R; Dessieux Jr, Luc Lucius

    2013-01-01

    Hydraulic fracturing to enhance formation permeability is an established practice in the Oil & Gas (O&G) industry and is expected to be an enabler for EGS. However, it is rarely employed in conventional geothermal systems and there are significant questions regarding the translation of practice from O&G to both conventional geothermal and EGS applications. Lithological differences(sedimentary versus crystalline rocks, significantly greater formation temperatures and different desired fracture characteristics are among a number of factors that are likely to result in a gap of understanding of how to manage hydraulic fracturing practice for geothermal. Whereas the O&G community has had both the capital and the opportunity to develop its understanding of hydraulic fracturing operations empirically in the field as well through extensive R&D efforts, field testing opportunities for EGS are likely to be minimal due to the high expense of hydraulic fracturing field trials. A significant portion of the knowledge needed to guide the management of geothermal/EGS hydraulic fracturing operations will therefore likely have to come from experimental efforts and simulation. This paper describes ongoing efforts at Oak Ridge National Laboratory (ORNL) to develop an experimental capability to map the internal stresses/strains in core samples subjected to triaxial stress states and temperatures representative of EGS-like conditions using neutron diffraction based strain mapping techniques. This capability is being developed at ORNL\\'s Spallation Neutron Source, the world\\'s most powerful pulsed neutron source and is still in a proof of concept phase. A specialized pressure cell has been developed that permits independent radial and axial fluid pressurization of core samples, with axial flow through capability and a temperature rating up to 300 degrees C. This cell will ultimately be used to hydraulically pressurize EGS-representative core samples to conditions of imminent fracture

  10. In-situ Time-Resolved Neutron Diffraction Measurements of Microstructure Variations during Friction Stir Welding in a 6061-T6 Aluminum Alloy

    SciTech Connect

    Woo, Wan Chuck; Wang, Xun-Li; Ungar, Prof Tomas; Feng, Zhili; David, Stan A; Clausen, B; Hubbard, Camden R

    2008-01-01

    The microstructure change is one of the most important research areas in the friction stir welding (FSW). However, direct observation of microstructure changes during FSW has been extremely challenging because many measurement techniques are inapplicable. Recently developed in-situ time-resolved neutron diffraction methodology, which drastically improves the temporal resolution of neutron diffraction, enables to observe the transient microstructure changes during FSW. We installed a portable FSW system in the Spectrometer for MAterials Research at Temperature and Stress (SMARTS) at Los Alamos Neutron Science Center and the FSW was made on 6.35mm-thickness 6061-T6 Al alloy plate. At the same time, the neutron beam was centered on the mid-plane of the Al plate at 8 mm from the tool center (underneath the tool shoulder) and the diffraction peak was continuously measured during welding. The peak broadening analysis has been performed using the Williamson-Hall Method. The result shows that the dislocation density of about 3.2 x 10^15 m-2 duing FSW, which is the significant increse compared to the before (4.5 x 10^14 m-2) and after (4.0 x 10^14 m-2) the FSW. The quantitatively analysis of the grain structure can provide an insight to understand the transient variation of the microstructure during FSW.

  11. A Novel In-situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes of Li-ion Batteries

    SciTech Connect

    Vadlamani, Bhaskar S; An, Ke; Jagannathan, M.; Ravi Chandran, K.

    2014-01-01

    The design and performance of a novel in-situ electrochemical cell that greatly facilitates the neutron diffraction study of complex phase transitions in small volume electrodes of Li-ion cells, is presented in this work. Diffraction patterns that are Rietveld-refinable could be obtained simultaneously for all the electrodes, which demonstrates that the cell is best suited to explore electrode phase transitions driven by the lithiation and delithiation processes. This has been facilitated by the use of single crystal (100) Si sheets as casing material and the planar cell configuration, giving improved signal-to-noise ratio relative to other casing materials. The in-situ cell has also been designed for easy assembly and to facilitate rapid experiments. The effectiveness of cell is demonstrated by tracking the neutron diffraction patterns during the charging of graphite/LiCoO2 and graphite/LiMn2O4 cells. It is shown that good quality neutron diffraction data can be obtained and that most of the finer details of the phase transitions, and the associated changes in crystallographic parameters in these electrodes, can be captured.

  12. Probing ferroic transitions in a multiferroic framework family: a neutron diffraction study of the ammonium transition metal formates.

    PubMed

    Lawler, James M M; Manuel, Pascal; Thompson, Amber L; Saines, Paul J

    2015-07-01

    This study probes the magnetic and ferroelectric ordering of the NH4M(HCO2)3 (M = Mn(2+), Fe(2+), Co(2+) and Ni(2+)) frameworks using neutron diffraction, improving the understanding of the origins of the properties of these fascinating multiferroics. This rare study of the magnetic structure of a family of metal-organic frameworks shows that all four compounds exhibit antiferromagnetic coupling between neighbouring cations bridged by formate ligands. The orientation of the spin, however, changes in a highly unusual way across the series with the spins aligned along the c-axis for the Fe(2+) and Ni(2+) frameworks but lying in the ab plane for the other members of the series. This work also sheds new light on the nature of the ferroelectric order-disorder transition in these materials; probing changes in the ammonium cation across the transition and also shows that the Ni(2+) framework does not undergo a transition to the polar P63 phase due to the smaller size of the Ni(2+) cation. Finally trends in their anisotropic negative thermal expansion, which potentially enhances their ferroic behaviour, are quantified. PMID:26040906

  13. Single Crystal Neutron Diffraction Study of Organic Multiferroic (ND4)2[FeCl5(D2O)

    NASA Astrophysics Data System (ADS)

    Tian, Wei; Cao, Huibo; Yan, Jiaqiang; Chakoumakos, Bryan; Sales, Brian; Fernandez-Baca, Jaime

    2015-03-01

    (NH4)2 [FeCl5(H2O)] is a new organic multiferroic that exhibits intriguing magnetic/multiferroic behavior as a function of temperature and applied magnetic field. Unlike its counterpart compounds where NH4 group is replaced by K, Cs, and Rb, (NH4)2 [FeCl5(H2O)] is the only system that undergoes two successive magnetic transitions accompanied by pronounced spontaneous electric polarization. Large deuterated (ND4)2 [FeCl5(D2O)] single crystals were grown and characterized by specific heat and magnetization measurements showing no significant effects due to deuteration. Here we report single crystal neutron diffraction results that reveal an incommensurate antiferromagnetic order below TN ~ 7.3 K with a propagation vector of (0 0 ~ 0.77). Higher harmonic Bragg peaks were observed indicate ``squaring up'' behavior upon further cooling. At 1.5 K, a field induced incommensurate-to-commensurate transition was also observed by applying magnetic field along the a-axis. Research conducted at ORNL's High Flux Isotope Reactor was sponsored by the Scientific User Facilities Division, Office of Basic Energy Sciences, U. S. Department of Energy.

  14. Thermal-expansion behavior of a directionally solidified NiAl-Mo composite investigated by neutron diffraction and dilatometry

    SciTech Connect

    Bei, H.; George, E.P.; Brown, D.W.; Pharr, G.M.; Choo, H.; Porter, W.D.; Bourke, M.A.M.

    2005-06-15

    The thermal expansion of directionally solidified NiAl-Mo eutectic alloys consisting of nanoscale Mo fibers embedded in a NiAl matrix was analyzed by neutron diffraction and dilatometry. From room temperature to 800 deg. C, perpendicular to the fiber direction, the NiAl and Mo phases expand independently with average coefficients of thermal expansion (CTEs) of 16.0x10{sup -6} deg. C{sup -1} and 5.8x10{sup -6} deg. C{sup -1}, respectively. Parallel to the fiber direction, they coexpand up to 650 deg. C with an average CTE of 12.8x10{sup -6} deg. C{sup -1}, but above this temperature the Mo fibers expand more than the NiAl matrix. This anomalous behavior is the result of the load transfer to the Mo fibers when the NiAl matrix softens. The average CTE of the composite parallel to the fiber direction was determined by dilatometry to be 13.0x10{sup -6} deg. C{sup -1}, which is approximately 11% lower than the value predicted by a simple rule of mixtures using the CTEs of the constituent phases.

  15. Deformation mechanisms in a precipitation-strengthened ferritic superalloy revealed by in situ neutron diffraction studies at elevated temperatures

    DOE PAGESBeta

    Huang, Shenyan; Gao, Yanfei; An, Ke; Zheng, Lili; Wu, Wei; Teng, Zhenke; Liaw, Peter K

    2014-10-22

    In this study, the ferritic superalloy Fe–10Ni–6.5Al–10Cr–3.4Mo strengthened by ordered (Ni,Fe)Al B2-type precipitates is a candidate material for ultra-supercritical steam turbine applications above 923 K. Despite earlier success in improving its room-temperature ductility, the creep resistance of this material at high temperatures needs to be further improved, which requires a fundamental understanding of the high-temperature deformation mechanisms at the scales of individual phases and grains. In situ neutron diffraction has been utilized to investigate the lattice strain evolution and the microscopic load-sharing mechanisms during tensile deformation of this ferritic superalloy at elevated temperatures. Finite-element simulations based on the crystal plasticitymore » theory are employed and compared with the experimental results, both qualitatively and quantitatively. Based on these interphase and intergranular load-partitioning studies, it is found that the deformation mechanisms change from dislocation slip to those related to dislocation climb, diffusional flow and possibly grain boundary sliding, below and above 873 K, respectively. Insights into microstructural design for enhancing creep resistance are also discussed.« less

  16. Phase coexistence in NaTaO3 at room temperature; a high resolution neutron powder diffraction study

    NASA Astrophysics Data System (ADS)

    Knight, Kevin S.; Kennedy, Brendan J.

    2015-05-01

    Room temperature high resolution neutron powder diffraction data, measured in time-of-flight, from two independent samples of NaTaO3 shows the presence of phase coexistence of two orthorhombic structures with space groups Pbnm, and Cmcm. The failure of earlier work to recognise the extent of the hysteresis associated with the high temperature (∼763 K on heating) Cmcm - Pbnm phase transition, that extends down to room temperature, and probably to 0 K, is due to data having been collected at too low a real-space resolution to characterise the diagnostic pseudocubic fundamental and superlattice reflection multiplicities. The phase fraction of the Cmcm phase increases with increasing temperature from 45 weight % at 298 K, to 74 weight % at 758 K. Throughout the whole temperature interval 298 K-758 K, the volume per formula unit of the Cmcm phase exceeds that of the Pbnm phase by an almost constant ∼0.01 Å3 suggesting the addition of pressure would supress the volume fraction of the higher temperature phase. The crystal structure of both phases, determined from data collected at 298 K, are reported, with the atomic displacement parameters of the Cmcm phase being significantly larger than those associated with the Pbnm phase, probably reflecting a high degree of thermal and static disorder.

  17. Polarized Neutron Diffraction as a Tool for Mapping Molecular Magnetic Anisotropy: Local Susceptibility Tensors in Co(II) Complexes.

    PubMed

    Ridier, Karl; Gillon, Béatrice; Gukasov, Arsen; Chaboussant, Grégory; Cousson, Alain; Luneau, Dominique; Borta, Ana; Jacquot, Jean-François; Checa, Ruben; Chiba, Yukako; Sakiyama, Hiroshi; Mikuriya, Masahiro

    2016-01-11

    Polarized neutron diffraction (PND) experiments were carried out at low temperature to characterize with high precision the local magnetic anisotropy in two paramagnetic high-spin cobalt(II) complexes, namely [Co(II) (dmf)6 ](BPh4 )2 (1) and [Co(II) 2 (sym-hmp)2 ](BPh4 )2 (2), in which dmf=N,N-dimethylformamide; sym-hmp=2,6-bis[(2-hydroxyethyl)methylaminomethyl]-4-methylphenolate, and BPh4 (-) =tetraphenylborate. This allowed a unique and direct determination of the local magnetic susceptibility tensor on each individual Co(II) site. In compound 1, this approach reveals the correlation between the single-ion easy magnetization direction and a trigonal elongation axis of the Co(II) coordination octahedron. In exchange-coupled dimer 2, the determination of the individual Co(II) magnetic susceptibility tensors provides a clear outlook of how the local magnetic properties on both Co(II) sites deviate from the single-ion behavior because of antiferromagnetic exchange coupling. PMID:26728231

  18. In situ neutron powder diffraction investigation of the hydration of tricalcium aluminate in the presence of gypsum

    SciTech Connect

    Hartman, M.R. . E-mail: michael.hartman@nist.gov; Berliner, R.

    2005-11-15

    The hydration of a 1:3 molar ratio of tricalcium aluminate, Ca{sub 3}Al{sub 2}O{sub 6}, to gypsum, CaSO{sub 4}.2D{sub 2}O, was investigated at temperatures of 25, 50, and 80 deg. C using time-of-flight powder neutron diffraction combined with multiphase Rietveld structural refinement. It was shown that ettringite, Ca{sub 6}[Al(OD){sub 6}]{sub 2}(SO{sub 4}){sub 3}.{approx}26D{sub 2}O, was the first and only hydration product of the system, in contrast to a prior investigation which suggested the occurrence of a precursor phase prior to the formation of ettringite. Kinetics data showed that the hydration reaction is very sensitive to temperature: hydration at 25 deg. C was characterized by a single kinetic regime while hydration at higher temperatures consisted of two distinct kinetic regimes. The presence of two kinetic regimes was attributed to a change in either the dimensionality of the growth process or a change in the rate controlling mechanism in the hydration reaction.

  19. Lithium insertion properties of LixTiNb2O7 investigated by neutron diffraction and first-principles modelling

    NASA Astrophysics Data System (ADS)

    Catti, Michele; Pinus, Ilya; Knight, Kevin

    2015-09-01

    TiNb2O7, a good candidate as anode in lithium batteries, was treated with n-butyllithium to synthesize LixTiNb2O7 phases similar to those formed during electrochemical reactions. The Li2.67TiNb2O7 and Li3.33TiNb2O7 compounds, monoclinic C2/m, were studied by time-of-flight powder neutron diffraction. Their crystal structures, containing 3×3 blocks of (Ti,Nb)O6 octahedra, were Rietveld refined including Li positions. The Li atoms are distributed in similar amounts over sites with (Li-O) Coordination Numbers 5 and 4, although CN=5 should be preferred for having lower energy. Quantum-mechanical calculations were also performed, determining the average charge-discharge voltages to be 1.415 and 1.571 V for Li3.33TiNb2O7 and Li2.67TiNb2O7, respectively, in good agreement with experimental results. An analysis of the theoretical charge distribution shows that, on lithiation, the chemical reduction of Ti and Nb atoms concentrates in the more condensed peripheral octahedra of the 3×3 block. This corresponds to electrons moving into a partly spin-polarized small band which gives rise to semi-metallic conductivity.

  20. As-Cast Residual Stresses in an Aluminum Alloy AA6063 Billet: Neutron Diffraction Measurements and Finite Element Modeling

    NASA Astrophysics Data System (ADS)

    Drezet, J.-M.; Phillion, A. B.

    2010-12-01

    The presence of thermally induced residual stresses, created during the industrial direct chill (DC) casting process of aluminum alloys, can cause both significant safety concerns and the formation of defects during downstream processing. Although numerical models have been previously developed to compute these residual stresses, most of the computations have been validated only against measured surface distortions. Recently, the variation in residual elastic strains in the steady-state regime of casting has been measured as a function of radial position using neutron diffraction (ND) in an AA6063 grain-refined cylindrical billet. In the present study, these measurements are used to show that a well-designed thermomechanical finite element (FE) process model can reproduce relatively well the experimental results. A sensitivity analysis is then carried out to determine the relative effect of the various mechanical parameters when computing the as-cast residual stresses in a cylindrical billet. Two model parameters have been investigated: the temperature when the alloy starts to thermally contract and the plasticity behavior. It is shown that the mechanical properties at low temperatures have a much larger influence on the residual stresses than those at high temperatures.

  1. Using neutron powder diffraction and first-principles calculations to understand the working mechanisms of porous coordination polymer sorbents.

    PubMed

    Chevreau, Hubert; Duyker, Samuel G; Peterson, Vanessa K

    2015-12-01

    Metal-organic frameworks (MOFs) are promising solid sorbents, showing gas selectivity and uptake capacities relevant to many important applications, notably in the energy sector. To improve and tailor the sorption properties of these materials for such applications, it is necessary to gain an understanding of their working mechanisms at the atomic and molecular scale. Specifically, it is important to understand how features such as framework porosity, topology, chemical functionality and flexibility underpin sorbent behaviour and performance. Such information is obtained through interrogation of structure-function relationships, with neutron powder diffraction (NPD) being a particularly powerful characterization tool. The combination of NPD with first-principles density functional theory (DFT) calculations enables a deep understanding of the sorption mechanisms, and the resulting insights can direct the future development of MOF sorbents. In this paper, experimental approaches and investigations of two example MOFs are summarized, which demonstrate the type of information and the understanding into their functional mechanisms that can be gained. Such information is critical to the strategic design of new materials with targeted gas-sorption properties. PMID:26634721

  2. In-Situ Neutron Diffraction Study of the Bauschinger Effect in B2 Structured CoZr

    NASA Astrophysics Data System (ADS)

    Mulay, R. P.; Clausen, B.; Agnew, S. R.

    2011-01-01

    A combination of in-situ neutron diffraction and elastoplastic self-consistent (EPSC) modeling have been used to elucidate the role played by intergranular stresses in the Bauschinger effect in B2 structured CoZr at room temperature and 423 K (150 °C). It is shown that, when insufficient slip modes are present to accommodate arbitrary strains, the large intergranular stresses built up due to inhomogeneous plastic deformation are responsible for the observed Bauschinger effect. Upon the onset of secondary deformation mechanism(s), the stresses are more uniformly distributed among the grains and the influence of intergranular stresses on the Bauschinger effect diminishes. On the other hand, it is speculated that the contribution of intragranular (dislocation-based) stresses is responsible for the persistent Bauschinger effect past the transition point. Similar results are obtained at both room temperature and 423 K (150 °C), and while the yield strength decreases with temperature, the high-temperature stress-strain curve progressively becomes harder than the room temperature one. In light of this, the previously characterized yield strength anomaly in CoZr has been re-examined.

  3. In situ neutron-diffraction study of the Ti38V30Cr14Mn18 structure during hydrogenation

    NASA Astrophysics Data System (ADS)

    Fei, Yang; Kong, Xiangcheng; Wu, Zhu; Li, Huanhuan; Peterson, V. K.

    2013-11-01

    The phase transformations of the Ti38V30Cr14Mn18 alloy during hydrogenation and dehydrogenation using deuterium (D2) were investigated using in situ neutron powder diffraction (NPD) at various D2 pressures up to 2 MPa. Initially, the first hydride that formed, Ti38V30Cr14Mn18D15, had the same body centered cubic (BCC) crystal structure as the starting alloy. Upon further hydrogenation, the system displays a distinct two-phase mixture of the intermediate BCC and body-centered tetragonal (BCT) phases, that exist in a ration of 1.38:1.42, respectively. At the end of the deuterium absorption, the phase pure Ti38V30Cr14Mn18D183 material forms, with a face-centered cubic (FCC) structure. Upon dehydrogenation, all hydride phases eventually returned to the initial alloy phase without any amorphization or disproportionation. Using standard Rietveld refinement, information on the variation of the deuterium site occupancy, the lattice symmetry, and the cell volume were determined during these phase changes and are presented.

  4. A neutron powder diffraction study of ND 3 intercalated titanium disulfide, 3 R-TiS 2ND 3

    NASA Astrophysics Data System (ADS)

    Bouwmeester, H. J. M.; Wiegers, G. A.

    1988-10-01

    Neutron powder diffraction of rhombohedral 3 R-TiS 2ND 3 ( a = 3.419 Å, c = 27.03 Å at 300 K, space group R overline3m ) has shown that ND 3 molecules and ND +4 ions, present in a ratio of about 5 to 1 from chemical and physical evidence, occupy statistically the trigonal-prismatic holes between TiS 2 sandwiches. One cannot distinguish between ND 3 and ND +4. Powder intensities calculated for a model with spherically symmetric ND 3 molecules (corresponding to isotropically rotating ND 3 and ND +4) in the trigonal-prismatic holes were in reasonable agreement with the observed intensities. Attempts to obtain information on the precise orientation of ND 3 and ND +4 in the TiS 2 lattice using refinements with structure factors were not successful; the reliability R factor was 0.093 for spherical symmetric ND 3 molecules with nitrogen in the center of the trigonal-prismatic holes.

  5. Refinement of atomic and magnetic structures using neutron diffraction for synthesized bulk and nano-nickel zinc gallate ferrite

    NASA Astrophysics Data System (ADS)

    Ata-Allah, S. S.; Balagurov, A. M.; Hashhash, A.; Bobrikov, I. A.; Hamdy, Sh.

    2016-01-01

    The parent NiFe2O4 and Zn/Ga substituted spinel ferrite powders have been prepared by solid state reaction technique. As a typical example, the Ni0.7Zn0.3Fe1.5Ga0.5O4 sample has been prepared by sol-gel auto combustion method with the nano-scale crystallites size. X-ray and Mössbauer studies were carried out for the prepared samples. Structure and microstructure properties were investigated using the time-of-flight HRFD instrument at the IBR-2 pulsed reactor, at a temperatures range 15-473 K. The Rietveld refinement of the neutron diffraction data revealed that all samples possess cubic symmetry corresponding to the space group Fd3m. Cations distribution show that Ni2+ is a complete inverse spinel ion, while Ga3+ equally distributed between the two A and B-sublattices. The level of microstrains in bulk samples was estimated as very small while the size of coherently scattered domains is quite large. For nano-structured sample the domain size is around 120 Å.

  6. The application of neutron diffraction to a study of phases in type 316 stainless steel weld metals

    NASA Astrophysics Data System (ADS)

    Slattery, G. F.; Windsor, C. G.

    1983-10-01

    Neutron diffraction techniques have been utilised to study the phases in type 316 austenitic stainless steel weld metal, both in the as-welded condition and after stress-relieving and ageing heat-treatments. The amounts of the principal crystallographic phases present in bulk specimens have been measured. Two compositions of weld metal were selected to provide a "low" (6%) and "high" (16%) initial ferrite level and the subsequent volume fractions of transformation products were measured after heat-treatment. Some retained ferrite was observed in all the heat-treated specimens, ranging from 4% for specimens of both initial ferrite levels treated at 625°C for 1000 h, to around 1% for the specimens treated at 850°C for 6 h. The high initial ferrite specimen produced 0.9% of sigma phase after the 850°C treatment and 0.2% sigma after the 625°C treatment. The low initial ferrite specimen produced 1.5% M 23C 6 carbide after both heat-treatments. The results compare well with previous findings on similar samples of weld metal using optical and electron microscopy.

  7. Neutron diffraction study on very high elastic strain of 6% in an Fe{sub 3}Pt under compressive stress

    SciTech Connect

    Yamaguchi, Takashi; Fukuda, Takashi Kakeshita, Tomoyuki; Harjo, Stefanus; Nakamoto, Tatsushi

    2014-06-09

    An Fe{sub 3}Pt alloy with degree of order 0.75 exhibits a second-order-like martensitic transformation from a cubic structure to a tetragonal one at about 90 K; its tetragonality c/a changes nearly continuously from 1 to 0.945 on cooling from 90 K to 14 K. We have investigated the change in lattice parameters in a single crystal of the Fe{sub 3}Pt alloy at 93 K under compressive stresses, σ, applied in the [001] direction by neutron diffraction. The tetragonality c/a has decreased continuously from 1 to 0.907 with an increase in |σ| up to |σ| = 280 MPa; the corresponding lattice strain in the [001] direction, due to the continuous structure change, increases from 0% to 6.1%. When the stress of 300 MPa is reached, c/a has changed abruptly from 0.907 to 0.789 due to a first-order martensitic transformation.

  8. Deformation mechanisms in a precipitation-strengthened ferritic superalloy revealed by in situ neutron diffraction studies at elevated temperatures

    SciTech Connect

    Huang, Shenyan; Gao, Yanfei; An, Ke; Zheng, Lili; Wu, Wei; Teng, Zhenke; Liaw, Peter K

    2014-10-22

    In this study, the ferritic superalloy Fe–10Ni–6.5Al–10Cr–3.4Mo strengthened by ordered (Ni,Fe)Al B2-type precipitates is a candidate material for ultra-supercritical steam turbine applications above 923 K. Despite earlier success in improving its room-temperature ductility, the creep resistance of this material at high temperatures needs to be further improved, which requires a fundamental understanding of the high-temperature deformation mechanisms at the scales of individual phases and grains. In situ neutron diffraction has been utilized to investigate the lattice strain evolution and the microscopic load-sharing mechanisms during tensile deformation of this ferritic superalloy at elevated temperatures. Finite-element simulations based on the crystal plasticity theory are employed and compared with the experimental results, both qualitatively and quantitatively. Based on these interphase and intergranular load-partitioning studies, it is found that the deformation mechanisms change from dislocation slip to those related to dislocation climb, diffusional flow and possibly grain boundary sliding, below and above 873 K, respectively. Insights into microstructural design for enhancing creep resistance are also discussed.

  9. Quantum entanglement in manganese(II) hexakisimidazole nitrate: on electronic structure imaging - A polarized neutron diffraction and DFT study

    NASA Astrophysics Data System (ADS)

    Wallace, Warren A.

    2016-04-01

    Quantum entanglement has been visualized for the first time, in view of the spin density distribution and electronic structure for manganese in manganese(II)hexakisimidazole nitrate. Using polarized neutron diffraction and density functional theory modelling we have found for the complex, which crystallizes in the R3¯ spacegroup, a = b = 12.4898(3) Å, c = 14.5526(4) Å, α = γ = 90°, β = 120°, Z = 3, that spatially antisymmetric and spatially symmetric shaped regions of negative spin density, in the spin density map for manganese, are a result of quantum entanglement of the high spin d5 configuration due to dative imidazole- manganese π- donation and σ-bonding interactions respectively. We have found leakage of the entangled states for manganese observed as regions of positive spin density with spherical (3.758(2) μB) and non-spherical (1.242(3) μB) contributions. Our results, which are supportive of Einstein's theory of general relativity, provide evidence for the existence of a black hole spin density distribution at the origin of an electronic structure and also address the paradoxical views of entanglement and quantum mechanics. We have also found the complex, which is an insulator, to be suitable for spintronic studies.

  10. Computation of diffuse scattering arising from one-phonon excitations in a neutron time-of-flight single-crystal Laue diffraction experiment

    PubMed Central

    Gutmann, Matthias J.; Graziano, Gabriella; Mukhopadhyay, Sanghamitra; Refson, Keith; von Zimmerman, Martin

    2015-01-01

    Direct phonon excitation in a neutron time-of-flight single-crystal Laue diffraction experiment has been observed in a single crystal of NaCl. At room temperature both phonon emission and excitation leave characteristic features in the diffuse scattering and these are well reproduced using ab initio phonons from density functional theory (DFT). A measurement at 20 K illustrates the effect of thermal population of the phonons, leaving the features corresponding to phonon excitation and strongly suppressing the phonon annihilation. A recipe is given to compute these effects combining DFT results with the geometry of the neutron experiment. PMID:26306090

  11. Influence of Cr doping on the magnetic structure of the FeAs-strips compound CaFe4As3: A single-crystal neutron diffraction study

    NASA Astrophysics Data System (ADS)

    Manuel, P.; Chapon, L. C.; Trimarchi, G.; Todorov, I. S.; Chung, D. Y.; Ouladdiaf, B.; Gutmann, M. J.; Freeman, A. J.; Kanatzidis, M. G.

    2013-09-01

    We have studied the magnetic structure of a Cr-doped iron-arsenide compound CaFe4As3 by means of single crystal neutron diffraction. The neutron data reveal that below 90 K, an antiferromagnetic structure with propagation vector k=0 is adopted. Refinement of the magnetic structure using one of the modes allowed by symmetry analysis indicates that two of the four Fe sites, including the one where the selective substitution Fe/Cr happens, bear reduced magnetic moments. Density functional theory calculations confirm the stability of such a magnetic arrangement.

  12. Non destructive neutron diffraction measurements of cavities, inhomogeneities, and residual strain in bronzes of Ghiberti's relief from the Gates of Paradise

    SciTech Connect

    Festa, G.; Senesi, R.; Alessandroni, M.; Andreani, C.; Vitali, G.; Porcinai, S.; Giusti, A. M.; Materna, T.; Paradowska, A. M.

    2011-03-15

    Quantitative neutron studies of cultural heritage objects provide access to microscopic, mesoscopic, and macroscopic structures in a nondestructive manner. In this paper we present a neutron diffraction investigation of a Ghiberti Renaissance gilded bronze relief devoted to the measurement of cavities and inhomogeneities in the bulk of the sample, along with the bulk phase composition and residual strain distribution. The quantitative measurements allowed the determination of the re-melting parts extension, as well as improving current knowledge about the manufacturing process. The study provides significant and unique information to conservators and restorators about the history of the relief.

  13. Vector solitons with a uniform polarisation state induced by polarisation filtering in a fibre laser

    SciTech Connect

    Chen Weicheng; Chen Guojie; Han Dingan; Xie Jianing

    2013-06-30

    A fibre laser with a SESAM as a passive mode-locker is constructed for obtaining a vector soliton with the Kelly sidebands. The analysis of the peculiarities of the sidebands shows that the polarisation states are nonuniform across the entire pulse spectral profile from the leading edge to the trailing edge. Polarisation filtering effect is proposed to obtain a vector soliton with a uniform polarisation state. It is shown that during the polarisation filtering by a polariser incorporated into the laser cavity, the spectral width of the vector solitons gradually broadens and the pulse power decreases. It is found that at a maximum spectral width and a minimum pulse power, vector solitons with a uniform polarisation state are generated. (nonlinear optical phenomena)

  14. New insights into the compressibility and high-pressure stability of Ni(CN)2: a combined study of neutron diffraction, Raman spectroscopy, and inelastic neutron scattering.

    PubMed

    Mishra, Sanjay K; Mittal, Ranjan; Zbiri, Mohamed; Rao, Rekha; Goel, Prabhatasree; Hibble, Simon J; Chippindale, Ann M; Hansen, Thomas; Schober, Helmut; Chaplot, Samrath L

    2016-02-01

    Nickel cyanide is a layered material showing markedly anisotropic behaviour. High-pressure neutron diffraction measurements show that at pressures up to 20.1 kbar, compressibility is much higher in the direction perpendicular to the layers, c, than in the plane of the strongly chemically bonded metal-cyanide sheets. Detailed examination of the behaviour of the tetragonal lattice parameters, a and c, as a function of pressure reveal regions in which large changes in slope occur, for example, in c(P) at 1 kbar. The experimental pressure dependence of the volume data is fitted to a bulk modulus, B0, of 1050 (20) kbar over the pressure range 0-1 kbar, and to 124 (2) kbar over the range 1-20.1 kbar. Raman spectroscopy measurements yield additional information on how the structure and bonding in the Ni(CN)2 layers change with pressure and show that a phase change occurs at about 1 kbar. The new high-pressure phase, (Phase PII), has ordered cyanide groups with sheets of D4h symmetry containing Ni(CN)4 and Ni(NC)4 groups. The Raman spectrum of phase PII closely resembles that of the related layered compound, Cu1/2Ni1/2(CN)2, which has previously been shown to contain ordered C≡N groups. The phase change, PI to PII, is also observed in inelastic neutron scattering studies which show significant changes occurring in the phonon spectra as the pressure is raised from 0.3 to 1.5 kbar. These changes reflect the large reduction in the interlayer spacing which occurs as Phase PI transforms to Phase PII and the consequent increase in difficulty for out-of-plane atomic motions. Unlike other cyanide materials e.g. Zn(CN)2 and Ag3Co(CN)6, which show an amorphization and/or a decomposition at much lower pressures (~100 kbar), Ni(CN)2 can be recovered after pressurising to 200 kbar, albeit in a more ordered form. PMID:26751175

  15. Neutron Diffraction Study on Plastic behavior of a Nickel-Based Alloy Under the Monotonic-Tension and the Low-Cyclic-Fatigue Experiments

    SciTech Connect

    Huang, E.-W.; Barabash, R.; Clausen, B.; Wang, Y.; Yang, R.; Li, L.; Choo, H.; Liaw, P.K.

    2007-11-02

    The plastic behavior of an annealed HASTELLOY C-22HS alloy, a face-centered cubic (FCC), nickel-based superalloy, was examined by in-situ neutron-diffraction measurements at room temperature. Both monotonic-tension and low-cycle-fatigue experiments were conducted. Monotonic-tension straining and cyclic-loading deformation were studied as a function of stress. The plastic behavior during deformation is discussed in light of the relationship between the stress and dislocation-density evolution. The calculated dislocation-density evolution within the alloy reflects the strain hardening and cyclic hardening/softening. Experimentally determined lattice strains are compared to verify the hardening mechanism at selected stress levels for tension and cyclic loadings. Combined with calculations of the dislocation densities, the neutron-diffraction experiments provide direct information about the strain and cyclic hardening of the alloy.

  16. A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

    SciTech Connect

    Christien, F. Le Gall, R.; Telling, M. T. F.; Knight, K. S.

    2015-05-15

    A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

  17. Neutron diffraction study of the formation of ordered antiphase domains in cubic titanium carbide TiC{sub 0.60}

    SciTech Connect

    Khidirov, I. Parpiev, A. S.

    2013-05-15

    A series of superstructural reflections (described within the sp. gr. Fd3m) are found to be split into three symmetric parts in the neutron powder diffraction pattern of titanium carbide TiC{sub 0.60} annealed at a temperature of 600 Degree-Sign C. No splitting of superstructural reflections is observed in the neutron diffraction pattern of TiC{sub 0.60} annealed at relatively high temperatures (780 Degree-Sign C). This phenomenon can be explained by that fact that the ordering of carbon atoms at relatively high temperatures (780 Degree-Sign C) is accompanied by the formation of randomly oriented rather large antiphase domains (APDs) (450 A). At relatively low temperatures (600 Degree-Sign C), stacking faults arise in the arrangement of partially ordered carbon atoms. In this case, relatively small ordered APDs (290 A) are formed, along with disordered ones.

  18. A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

    NASA Astrophysics Data System (ADS)

    Christien, F.; Telling, M. T. F.; Knight, K. S.; Le Gall, R.

    2015-05-01

    A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

  19. Local magnetic moments in a dinuclear Co{sup 2+} complex as seen by polarized neutron diffraction:Beyond the effective spin-(1/2) model

    SciTech Connect

    Borta, Ana; Luneau, Dominique; Jeanneau, Erwann; Gillon, Beatrice; Gukasov, Arsen; Cousson, Alain; Ciumacov, Iurii; Sakiyama, Hiroshi; Tone, Katsuya; Mikuriya, Masahiro

    2011-05-01

    Polarized neutron diffraction investigations of a paramagnetic molecular dinuclear Co{sup 2+} complex, using the local site susceptibility method, show that the Co{sup 2+} ions carry opposite magnetic moments of 3.1(1) and 3.2(1) {mu}{sub B}, making an angle of 37(1) deg. which is in agreement with the value (39 deg.) provided by the theoretical analysis of the magnetic susceptibility using the model of effective spin 1/2. Polarized neutron diffraction (PND) shows that this dinuclear Co{sup 2+} complex behaves more like a system of two antiferromagnetically coupled ions with spin 3/2, the directions of which are imposed by the distortion axis of the octahedra around each Co{sup 2+} ion due to ligand field. This first application of the local susceptibility tensor method to a molecular compound demonstrates the efficiency of the PND method as a tool for exploring magnetic anisotropy in molecular paramagnets.

  20. First Polarised Light with the NIKA Camera

    NASA Astrophysics Data System (ADS)

    Ritacco, A.; Adam, R.; Adane, A.; Ade, P.; André, P.; Beelen, A.; Belier, B.; Benoît, A.; Bideaud, A.; Billot, N.; Bourrion, O.; Calvo, M.; Catalano, A.; Coiffard, G.; Comis, B.; D'Addabbo, A.; Désert, F.-X.; Doyle, S.; Goupy, J.; Kramer, C.; Leclercq, S.; Macías-Pérez, J. F.; Martino, J.; Mauskopf, P.; Maury, A.; Mayet, F.; Monfardini, A.; Pajot, F.; Pascale, E.; Perotto, L.; Pisano, G.; Ponthieu, N.; Rebolo-Iglesias, M.; Revéret, V.; Rodriguez, L.; Savini, G.; Schuster, K.; Sievers, A.; Thum, C.; Triqueneaux, S.; Tucker, C.; Zylka, R.

    2015-10-01

    NIKA is a dual-band camera operating with 315 frequency multiplexed LEKIDs cooled at 100 mK. NIKA is designed to observe the sky in intensity and polarisation at 150 and 260 GHz from the IRAM 30-m telescope. It is a test-bench for the final NIKA2 camera. The incoming linear polarisation is modulated at four times the mechanical rotation frequency by a warm rotating multi-layer half- wave plate. Then, the signal is analyzed by a wire grid and finally absorbed by the lumped element kinetic inductance detectors (LEKIDs). The small time constant (< 1 ms ) of the LEKIDs combined with the modulation of the HWP enables the quasi-simultaneous measurement of the three Stokes parameters I, Q, U, representing linear polarisation. In this paper, we present the results of recent observational campaigns demonstrating the good performance of NIKA in detecting polarisation at millimeter wavelength.

  1. First Polarised Light with the NIKA Camera

    NASA Astrophysics Data System (ADS)

    Ritacco, A.; Adam, R.; Adane, A.; Ade, P.; André, P.; Beelen, A.; Belier, B.; Benoît, A.; Bideaud, A.; Billot, N.; Bourrion, O.; Calvo, M.; Catalano, A.; Coiffard, G.; Comis, B.; D'Addabbo, A.; Désert, F.-X.; Doyle, S.; Goupy, J.; Kramer, C.; Leclercq, S.; Macías-Pérez, J. F.; Martino, J.; Mauskopf, P.; Maury, A.; Mayet, F.; Monfardini, A.; Pajot, F.; Pascale, E.; Perotto, L.; Pisano, G.; Ponthieu, N.; Rebolo-Iglesias, M.; Revéret, V.; Rodriguez, L.; Savini, G.; Schuster, K.; Sievers, A.; Thum, C.; Triqueneaux, S.; Tucker, C.; Zylka, R.

    2016-08-01

    NIKA is a dual-band camera operating with 315 frequency multiplexed LEKIDs cooled at 100 mK. NIKA is designed to observe the sky in intensity and polarisation at 150 and 260 GHz from the IRAM 30-m telescope. It is a test-bench for the final NIKA2 camera. The incoming linear polarisation is modulated at four times the mechanical rotation frequency by a warm rotating multi-layer half- wave plate. Then, the signal is analyzed by a wire grid and finally absorbed by the lumped element kinetic inductance detectors (LEKIDs). The small time constant (<1 ms ) of the LEKIDs combined with the modulation of the HWP enables the quasi-simultaneous measurement of the three Stokes parameters I, Q, U, representing linear polarisation. In this paper, we present the results of recent observational campaigns demonstrating the good performance of NIKA in detecting polarisation at millimeter wavelength.

  2. Polarisation losses in a ring prism cavity

    SciTech Connect

    Kuryatov, V N; Sokolov, A L

    2000-02-28

    The polarisation losses in a ring cavity, formed by total-internal-reflection prisms, were analysed. All the sources of the polarisation losses are indicated and expressions for their calculation are presented. The limit to loss reduction in cavities of this kind, set by the difference between the radii of curvature of the radiation wavefront and of the refracting prism faces, was determined. (laser gyroscopes)

  3. An ultrafast carbon nanotube terahertz polarisation modulator

    SciTech Connect

    Docherty, Callum J.; Stranks, Samuel D.; Habisreutinger, Severin N.; Joyce, Hannah J.; Herz, Laura M.; Nicholas, Robin J.; Johnston, Michael B.

    2014-05-28

    We demonstrate ultrafast modulation of terahertz radiation by unaligned optically pumped single-walled carbon nanotubes. Photoexcitation by an ultrafast optical pump pulse induces transient terahertz absorption in nanowires aligned parallel to the optical pump. By controlling the polarisation of the optical pump, we show that terahertz polarisation and modulation can be tuned, allowing sub-picosecond modulation of terahertz radiation. Such speeds suggest potential for semiconductor nanowire devices in terahertz communication technologies.

  4. An ultrafast carbon nanotube terahertz polarisation modulator

    NASA Astrophysics Data System (ADS)

    Docherty, Callum J.; Stranks, Samuel D.; Habisreutinger, Severin N.; Joyce, Hannah J.; Herz, Laura M.; Nicholas, Robin J.; Johnston, Michael B.

    2014-05-01

    We demonstrate ultrafast modulation of terahertz radiation by unaligned optically pumped single-walled carbon nanotubes. Photoexcitation by an ultrafast optical pump pulse induces transient terahertz absorption in nanowires aligned parallel to the optical pump. By controlling the polarisation of the optical pump, we show that terahertz polarisation and modulation can be tuned, allowing sub-picosecond modulation of terahertz radiation. Such speeds suggest potential for semiconductor nanowire devices in terahertz communication technologies.

  5. A short note on physical properties to irradiated nuclear fuel by means of X-ray diffraction and neutron scattering techniques

    SciTech Connect

    Abdullah, Yusof Husain, Hishamuddin; Hak, Cik Rohaida Che; Alias, Nor Hayati; Yusof, Mohd Reusmaazran; Kasim, Norasiah Ab; Zali, Nurazila Mat; Mohamed, Abdul Aziz

    2015-04-29

    For nuclear reactor applications, understanding the evolution of the fuel materials microstructure during irradiation are of great importance. This paper reviews the physical properties of irradiated nuclear fuel analysis which are considered to be of most importance in determining the performance behavior of fuel. X-rays diffraction was recognize as important tool to investigate the phase identification while neutron scattering analyses the interaction between uranium and other materials and also investigation of the defect structure.

  6. Dynamic nuclear polarisation of diamond

    NASA Astrophysics Data System (ADS)

    High, Grant Lysle

    Chapter one reviews the reported literature on the NMR of diamond. This signal consists of a single line at 39 ppm from TMS and two hyperfine lines due to 13C interactions. The second chapter introduces the apparatus used in this study. The availability of this excellently equipped laboratory presented a unique opportunity to perform this investigation. Chapter three outlines the experimental techniques used as well as the manner in which the acquired data was processed. The fourth chapter presents an overview of the most common defects found in diamond. Proposed models of these defects are presented and the EPR spectra displayed. The methods developed to determine the paramagnetic impurity concentration, from the EPR line width and the spin-spin relaxation times are presented in the fifth chapter. The line width gives the total paramagnetic impurity concentration to about 10 ppm. The spin-spin relaxation time allows the determination of paramagnetic impurity concentrations, to much lower levels. This information was used in the explanation of the relaxation behaviour for the diamonds investigated. The temperature dependence of the paramagnetic electron relaxation times is reported in the sixth chapter. The results obtained are consistent with the findings in prior work that P1 impurities are typical, Jahn Teller centres. Two diamonds, however, display trends that depart from this theory. It was found in these experiments that, bar thermal expansion effects, the spin-spin relaxation time is independent of temperature. The seventh chapter deals with the solid state and thermal mixing effects. The relevant theory, results obtained and a discussion of these results, are presented. The effect of various parameters on the polarisation rates and the 13C signal enhancement are investigated. Finally the effect of applying the DNP treatment on the central and hyperfine lines is discussed. The pulsed DNP process is presented in the eighth chapter. The relevant theory, the

  7. High-level expression and deuteration of sperm whale myoglobin: A study of its solvent structure by X-ray and neutron diffraction methods

    SciTech Connect

    Shu, F.; Ramakrishnan, V.; Schoenborn, B.P.

    1994-12-31

    Neutron diffraction has become one of the best ways to study light atoms, such as hydrogens. Hydrogen however has a negative coherent scattering factor, and a large incoherent scattering factor, while deuterium has virtually no incoherent scattering, but a large positive coherent scattering factor. Beside causing high background due to its incoherent scattering, the negative coherent scattering of hydrogen tends to cancel out the positive contribution from other atoms in a neutron density map. Therefore a fully deuterated sample will yield better diffraction data with stronger density in the hydrogen position. On this basis, a sperm whale myoglobin gene modified to include part of the A cII protein gene has been cloned into the T7 expression system. Milligram amounts of fully deuterated holo-myoglobin have been obtained and used for crystallization. The synthetic sperm whale myoglobin crystallized in P2{sub 1} space group isomorphous with the native protein crystal. A complete X-ray diffraction dataset at 1.5{Angstrom} has been collected. This X-ray dataset, and a neutron data set collected previously on a protonated carbon-monoxymyoglobin crystal have been used for solvent structure studies. Both X-ray and neutron data have shown that there are ordered hydration layers around the protein surface. Solvent shell analysis on the neutron data further has shown that the first hydration layer behaves differently around polar and apolar regions of the protein surface. Finally, the structure of per-deuterated myoglobin has been refined using all reflections to a R factor of 17%.

  8. A new polarisation amplitude bias reduction method.

    NASA Astrophysics Data System (ADS)

    Vidal, M.; Leahy, J. P.; Dickinson, C.

    2016-06-01

    Polarisation amplitude estimation is affected by a positive noise bias, particularly important in regions with low signal-to-noise ratio (SNR). We present a new approach to correct for this bias in the case there is additional information about the polarisation angle. We develop the `known-angle estimator' that works in the special case when there is an independent and high signal-to-noise ratio (≳ 2σ) measurement of the polarisation angle. It is derived for the general case where the uncertainties in the Q, U Stokes parameters are not symmetric. This estimator completely corrects for the polarisation bias if the polarisation angle is perfectly known. In the realistic case, where the angle template has uncertainties, a small residual bias remains, but that is shown to be much smaller that the one left by other classical estimators. We also test our method with more realistic data, using the noise properties of the three lower frequency maps of WMAP. In this case, the known-angle estimator also produces better results than methods that do not include the angle information. This estimator is therefore useful in the case where the polarisation angle is expected to be constant over different data sets with different SNR.

  9. Deformation Behavior of Solid-Solution-Strengthened Mg-9wt%Al Alloy: In-Situ Neutron Diffraction and Elastic-Viscoplastic Self-Consistent Modeling

    SciTech Connect

    Lee, Sooyeol; Wang, H; Gharghouri, Michael; Nayyeri, G.; Woo, Wan; Shin, E; Wu, Peidong; Poole, W. J.; Wu, Wei; An, Ke

    2014-01-01

    In situ neutron diffraction and elastic viscoplastic self-consistent (EVPSC) modeling have been employed to understand the deformation mechanisms of the loading unloading process under uniaxial tension in a solid-solution-strengthened extruded Mg 9 wt.% Al alloy. The initial texture measured by neutron diffraction shows that the {00.2} basal planes in most grains are tilted around 20 30 from the extrusion axis, indicating that basal slip should be easily activated in a majority of grains under tension. Non-linear stress strain responses are observed during unloading and reloading after the material is fully plastically deformed under tension. In situ neutron diffraction measurements have also demonstrated the non-linear behavior of lattice strains during unloading and reloading, revealing that load redistribution continuously occurs between soft and hard grain orientations. The predicted macroscopic stress strain curve and the lattice strain evolution by the EVPSC model are in good agreement with the experimental data. The EVPSC model provides the relative activities of the available slip and twinning modes, as well as the elastic and plastic strains of the various grain families. It is suggested that the non-linear phenomena in the macroscopic stress strain responses and microscopic lattice strains during unloading and reloading are due to plastic deformation by the operation of basal a slip in the soft grain orientations (e.g. {10.1}, {11.2} and {10.2} grain families).

  10. Neutron and X-Ray Powder Diffraction Study of RBa 2Fe 3O 8+ wPhases

    NASA Astrophysics Data System (ADS)

    Karen, P.; Kjekshus, A.; Huang, Q.; Lynn, J. W.; Rosov, N.; Natali Sora, I.; Karen, V. L.; Mighell, A. D.; Santoro, A.

    1998-02-01

    Compounds of composition RBa 2Fe 3O 8+ w( R=La, Nd, Sm, Gd, Dy, Er, Yb, Lu, and Y) with variable oxygen content have been synthesized using the liquid mixing technique and have been analyzed by powder X-ray and neutron diffraction methods. A triple perovskite-type structure with ordered Ba and Rcations and having the symmetry of space group P4/ mmmwas obtained only for R=Y, Dy, and Er, whereas the larger Ratoms gave the atomic arrangement of disordered, defective perovskites with average symmetry Pmoverline3m. No perovskite-type phases were obtained when Yb and Lu were tried. The oxygen content of the oxygen-saturated phases was found to increase with increasing size of the cation Rfrom w=0.07 for Er to w=0.83 for La. The Néel temperature (˜650 K) and the magnitude of the Fe magnetic moment (˜3.3 μBat room temperature) are highest when trivalent iron is involved ( w=0), but these quantities are rather insensitive to the nature of Rand to slight variations of oxygen content in the triple perovskite-type structure of the Y, Dy, and Er compounds. In the case of the cubic structures, however, both quantities depend strongly on the oxygen stoichiometry. In the magnetically ordered state, nearest-neighbor iron moments are coupled antiferromagnetically along the three crystallographic directions in all samples, resulting in magnetic structures with symmetry Imm' mand magnetic unit cells related to those of the corresponding nuclear structures by the transformation matrix (1 overline10/110/002).

  11. Anharmonic Computations Meet Experiments (IR, Raman, Neutron Diffraction) for Explaining the Behavior of 1,3,5-Tribromo-2,4,6-trimethylbenzene.

    PubMed

    Meinnel, Jean; Latouche, Camille; Ghanemi, Soumia; Boucekkine, Abdou; Barone, Vincenzo; Moréac, Alain; Boudjada, Ali

    2016-02-25

    In the present paper we first show the experimental Raman, infrared, and neutron INS spectra of tribromomesitylene (TBM) measured in the range 50-3200 cm(-1) using crystalline powders at 6 or 4 K. Then, the bond lengths and angles determined by neutron diffraction using a TBM single crystal at 14 K are compared to the computed ones at different levels of theory. Anharmonic computations were then performed on the relaxed structure using the VPT2 approach, and for the lowest normal modes, the HRAO model has led to a remarkable agreement for the assignment of the experimental signatures. A particularity appears for frequencies below 150 cm(-1), and in particular for those concerning the energy levels of "hindered rotation" of the three methyl groups, they must be calculated for one-dimensional symmetrical tops independent of the frame vibrations. This fact is consistent with the structure established by neutron diffraction: the protons of the methyl groups undergoing huge "libration" motions are widely spread in space. The values of the transitions between the librational levels determined by inelastic neutron scattering indicate that the hindering potentials are mainly due to intermolecular interactions different for each methyl group in the triclinic cell. PMID:26836589

  12. X-Ray and Neutron Diffraction Measurements of Dislocation Density and Subgrain Size in a Friction-Stir-Welded Aluminum Alloy

    SciTech Connect

    Woo, Wan Chuck; Ungar, Prof Tomas; Feng, Zhili; Kenik, Edward A; Clausen, B

    2009-01-01

    The dislocation density and subgrain size were determined in the base material and friction-stir welds of 6061-T6 aluminum alloy. High-resolution X-ray diffraction measurement was performed in the base material. The result of the line profile analysis of the X-ray diffraction peak shows that the dislocation density is about 4.5 x 10{sup 14} m{sup -2} and the subgrain size is about 200 nm. Meanwhile, neutron diffraction measurements have been performed to observe the diffraction peaks during friction-stir welding (FSW). The deep penetration capability of the neutron enables us to measure the peaks from the midplane of the Al plate underneath the tool shoulder of the friction-stir welds. The peak broadening analysis result using the Williamson-Hall method shows the dislocation density of about 3.2 x 10{sup 15} m{sup -2} and subgrain size of about 160 nm. The significant increase of the dislocation density is likely due to the severe plastic deformation during FSW. This study provides an insight into understanding the transient behavior of the microstructure under severe thermomechanical deformation.

  13. Neutron diffraction and electrochemical studies of Na0.79(Co,Mn)O2 cathodes for sodium-ion batteries

    SciTech Connect

    Beck, Faith R; Cheng, Yongqiang; Feygenson, Mikhail; Bridges, Craig A; Moorhead-Rosenberg, Z; Manthiram, Arumugam; Goodenough, J. B.; Paranthaman, Mariappan Parans; Manivannan, A.

    2014-01-01

    Na0.79CoO2 and Na0.79Co0.7Mn0.3O2 with a layered hexagonal structure (P2-type) were synthesized by the Pechini process followed by heat treatment at elevated temperatures in order to achieve the crystalline phases. The samples were characterized with x-ray diffraction, neutron diffraction, magnetic measurements and electrochemical charge-discharge cycling. X-ray diffraction confirmed the P2 layered hexagonal structure after heat treatment at 900 C in air. Neutron diffraction patterns confirm Mn doping on Co sites without forming pronounced Mn-Co ordering. Cyclic voltammetry showed the oxidation and reduction peaks of Co and Mn, indicating the intercalation and de-intercalation behavior of the Na ions. A discharge capacity of 60 mAh/g was achieved for both the compositions, with the Na0.79Co0.70Mn0.3O2 composition showing a more stable discharge capacity up to 60 cycles.

  14. X-Ray and Neutron Diffraction Measurements of Dislocation Density and Subgrain Size in a Friction-Stir-Welded Aluminum Alloy

    NASA Astrophysics Data System (ADS)

    Woo, Wanchuck; Ungár, Tamás; Feng, Zhili; Kenik, Edward; Clausen, Bjørn

    2010-05-01

    The dislocation density and subgrain size were determined in the base material and friction-stir welds of 6061-T6 aluminum alloy. High-resolution X-ray diffraction measurement was performed in the base material. The result of the line profile analysis of the X-ray diffraction peak shows that the dislocation density is about 4.5 × 1014 m-2 and the subgrain size is about 200 nm. Meanwhile, neutron diffraction measurements have been performed to observe the diffraction peaks during friction-stir welding (FSW). The deep penetration capability of the neutron enables us to measure the peaks from the midplane of the Al plate underneath the tool shoulder of the friction-stir welds. The peak broadening analysis result using the Williamson-Hall method shows the dislocation density of about 3.2 × 1015 m-2 and subgrain size of about 160 nm. The significant increase of the dislocation density is likely due to the severe plastic deformation during FSW. This study provides an insight into understanding the transient behavior of the microstructure under severe thermomechanical deformation.

  15. New Measurements of Polarised Light from Exoplanets

    NASA Astrophysics Data System (ADS)

    Bott, Kimberly Marie; Cotton, Daniel; Kedziora-Chudczer, Lucyna; Bailey, Jeremy

    2015-08-01

    Detections of polarised light from exoplanets are an important expansion of exoplanet studies, as they provide a complimentary and advantageous diagnostic to the other characterisation methods. However some of the earliest claimed detections of polarised light from exoplanets are disputed.The High Precision Polarimetric Instrument (HIPPI) is currently the highest sensitivity astronomical polarimeter (Bailey 2015) in the world at 4.3 ppm or better precision, and has been used to observe exoplanet systems including the disputed first detection source (Berdyugina 2008, Wiktorowicz 2009, Berdyugina 2011), HD189733b. HIPPI is designed for best sensitivity in blue light where Rayleigh scattering would produce a strong signal for hot Jupiter planets (Burrows 2008). These observations, taken at the Anglo-Australian Telescope in 2014 and 2015, are compared to models from a polarised light adaptation of the Versatile Software for the Transfer of Atmospheric Radiation (VSTAR).Our new, independent Hot Jupiter polarised light detections are discussed, including the physical sources of the detected polarised light, as well as additional contributing factors (e.g. debris, ISM anomalies). For HD 189733b we use available visible and near infrared transit and polarimetric data to create and interpret a planetary portrait using VSTAR.

  16. Crystal structure and magnetism of YbFeMnO 5: A neutron diffraction and Mössbauer spectroscopy study

    NASA Astrophysics Data System (ADS)

    Martínez-Lope, M. J.; Retuerto, M.; Alonso, J. A.; García-Hernández, M.; Krezhov, K.; Spirov, I.; Ruskov, T.; Fernández-Díaz, M. T.

    2009-04-01

    We have studied the crystal structure and magnetic properties of Y bFeMnO 5 obtained by substituting Fe 3+ for Mn 3+ in the parent Y bMn 2O 5 compound, through x-ray (XRD) and neutron (NPD) powder diffraction, magnetometry and Mössbauer spectroscopy. The samples were prepared in polycrystalline form by a soft chemistry route, followed by thermal treatments under high-oxygen pressure. The Rietveld analysis of diffraction data shows that Y bFeMnO 5 is isostructural with the oxides of stoichiometry RMn 2O 5 (R=rare earth, Y or Bi); the crystal structure is orthorhombic, Pbam space group, formed by chains of edge-sharing Mn 4+O 6 octahedra linked together by dimer groups of square pyramids Fe 3+O 5 and Y b 3+O 8 scalenohedra. A low level of disorder was established between the two transition metal positions 4 f and 4 h, occupied ideally by Mn 4+ and by Fe 3+: about 6% of Mn cations is replaced by Fe and 16% of Fe by Mn. Mössbauer spectroscopy data confirm the existence of two distinct crystallographic sites for Fe 3+. One of them corresponds to almost regular octahedra (at 4 f positions), characterized by nearly equal Mn/Fe-O distances of 1.890 Å at RT (from NPD data), giving a quadrupole doublet in the Mössbauer spectra at RT, broadened by the Fe/Mn disorder over this site. The second environment for Fe 3+ contributes to a less broadened, but more intensive doublet in the Mössbauer spectra, which corresponds to a distorted square pyramid Fe 3+O 5 (at 4h sites), for which NPD data demonstrates an axial distortion with three sets of Fe-O distances at 2.010(2) Å, 1.859(5) Å and 1.925(3) Å. Magnetic studies and the thermal evolution of the NPD patterns show that below a transition temperature Tc˜178 K a long-range magnetic order is developed, resolved from NPD data as a ferrimagnetic structure with propagation vector k=0. The spin arrangements for the Mn 4+ ions ( 4f site) and Fe 3+ ions ( 4h site) are given by the basis vectors ( 0,0,Fz) and ( 0,0,Fz

  17. High temperature neutron diffraction studies of PrInO3 and the measures of perovskite structure distortion.

    PubMed

    Baszczuk, A; Dabrowski, B; Avdeev, M

    2015-06-21

    The crystal structure of PrInO(3) was investigated in the temperature range 303-1123 K by high-resolution neutron-powder diffraction. The PrInO(3) adopts a highly distorted variant of the perovskite structure with the orthorhombic Pnma space group in the whole temperature range investigated. The bond length and bond-angle analysis revealed a very slow tendency to decrease structural distortion with increasing temperature. Comparison of different parameters quantifying perovskite structure distortion calculated for PrInO(3) and the similar PrAlO(3) and PrGaO(3) shows the advantage of using the tolerance factor t12 calculated for the 12-fold coordinated Pr by geometrical averaging of the individual interatomic distances. An additional advantage of the tolerance factor method results from the possibility of extending it to predict the average structural distortion and the geometrical stability of the perovskites at various temperatures once the accurate dependence of t(x,T,d) on the composition, temperature and oxygen content is found. By comparing PrInO(3) with several AMO(3) perovskites containing ions in the fixed oxidation state on the A and M crystal sites it was found that structural distortion and the tolerance factor t12 for PrInO(3) are consistent with the empirical thermal expansion coefficient based on the bond strength calculation [R. M. Hazen, and C. T. Prewitt, Am. Mineral., 1977, 62(3-4), 309]. In contrast to perovskites AMO(3-d) containing mixed-valent M ions, which allow for a wide range of changes of the tolerance factor t(12)(T,d) as a function of oxygen content, perovskites AMO(3) with M ions in the fixed oxidation state show much less flexibility. This flexibility is further reduced for the A(3+)M(3+)O(3) perovskites like PrInO(3) for which even a large change of the synthesis temperature has a minor effect on controlling the resulting t(12)(T) and the structural phase in comparison with A(2+)M(4+)O3 perovskites. The only parameter left for A(3+)M

  18. Quantum interferences revealed by neutron diffraction accord with a macroscopic-scale quantum-theory of ferroelectrics KH2(1- ρ)D2 ρ PO4

    NASA Astrophysics Data System (ADS)

    Fillaux, François; Cousson, Alain

    2016-03-01

    Neutron diffraction by single-crystals KH2(1- ρ)D2 ρ PO4 at 293 K reveal quantum interferences consistent with a static lattice of entangled proton-deuteron scatterers. These crystals are represented by a macroscopic-scale condensate of phonons with continuous space-time-translation symmetry and zero-entropy. This state is energetically favored and decoherence-free over a wide temperature-range. Projection of the crystal state onto a basis of four electrically- and isotopically-distinct state-vectors accounts for isotope and pressure effects on the temperature of the ferroelectric-dielectric transition, as well as for the latent heat. At the microscopic level, an incoming wave realizes a transitory state either in the space of static positional parameters (elastic scattering) or in that of the symmetry species (energy transfer). Neutron diffraction, vibrational spectroscopy, relaxometry and neutron Compton scattering support the conclusion that proton and deuteron scatterers are separable exclusively through resonant energy-transfer.

  19. Superstructure of a phosphor material Ba{sub 3}MgSi{sub 2}O{sub 8} determined by neutron diffraction data

    SciTech Connect

    Park, Cheol-Hee Hong, Seung-Tae; Keszler, Douglas A.

    2009-03-15

    Ba{sub 3}MgSi{sub 2}O{sub 8}, a phosphor host examined for use in white-light devices and plant-growth lamps, was synthesized at 1225 deg. C in air. Its crystal structure has been determined and refined by a combined powder X-ray and neutron Rietveld method (P3-bar, Z=3, a=9.72411(3) A, c=7.27647(3) A, V=595.870(5) A{sup 3}; R{sub p}/R{sub wp}=3.79%/5.03%, {chi}{sup 2}=4.20). Superstructure reflections, observed only in the neutron diffraction data, provided the means to establish the true unit cell and a chemically reasonable structure. The structure contains three crystallographically distinct Ba atoms-Ba1 resides in a distorted octahedral site with S{sub 6} (3-bar) symmetry, Ba2 in a nine-coordinate site with C{sub 3} (3) symmetry, and Ba3 in a ten-coordinate site with C{sub 1} (1) symmetry. The Mg atoms occupy distorted octahedral sites, and the Si atom occupies a distorted tetrahedral site. - Graphical Abstract: Crystal structure of Ba{sub 3}MgSi{sub 2}O{sub 8} viewed along the c direction. Superstructure reflections, observed only in the neutron diffraction data, provided the means to establish the true unit cell and a chemically reasonable structure.

  20. Neutron diffraction study of the martensitic transformation and chemical order in Heusler alloy Ni1.91Mn1.29Ga0.8

    DOE PAGESBeta

    Ari-Gur, Pnina; Garlea, Vasile O.; Cao, Huibo; Ge, Y.; Aaltio, I.; Hannula, S. P.; Koledov, V.

    2015-11-05

    In this study, Heusler alloys of Ni-Mn-Ga compositions demonstrate ferromagnetic shape memory effect in the martensitic state. The transformation temperature and the chemical order depend strongly on the composition. In the current work, the structure and chemical order of the martensitic phase of Ni1.91Mn1.29Ga0.8 were studied using neutron diffraction; the diffraction pattern was refined using the FullProf software. It was determined that the structural transition occurs around 330 K. At room temperature, 300 K, which is below the martensite transformation temperature, all the Bragg reflections can be described by a monoclinic lattice with a symmetry of space group P 1more » 2/m 1 and lattice constants of a = 4.23047(7) [Å], b = 5.58333(6) [Å], c = 21.0179(2) [Å], beta = 90.328(1). The chemical order is of critical importance in these alloys, and it was previously studied at 363 K. Analysis of the neutron diffraction in the monoclinic phase shows that the chemical order is maintained during the martensitic transformation.« less

  1. Neutron diffraction studies of RSn{sub 1+x}Ge{sub 1-x} (R=Tb-Er) compounds

    SciTech Connect

    Gil, A.; Hoser, A.; Szytula, A.

    2011-07-15

    The magnetic structures of RSn{sub 1+x}Ge{sub 1-x} (R=Tb, Dy, Ho and Er, x{approx}0.1) compounds have been determined by neutron diffraction studies on polycrystalline samples. The data recorded in a paramagnetic state confirmed the orthorhombic crystal structure described by the space group Cmcm. These compounds are antiferromagnets at low temperatures. The magnetic ordering in TbSn{sub 1.12}Ge{sub 0.88} is sine-modulated described by the propagation vector k=(0.4257(2), 0, 0.5880(3)). Tb magnetic moment equals 9.0(1) {mu}{sub B} at 1.62 K. It lies in the b-c plane and form an angle {theta}=17.4(2) deg. with the c-axis. This structure is stable up to the Neel temperature equal to 31 K. The magnetic structures of RSn{sub 1+x}Ge{sub 1-x}, where R are Dy, Ho and Er at low temperatures are described by the propagation vector k=(1/2, 1/2, 0) with the sequence (++-+) of magnetic moments in the crystal unit cell. In DySn{sub 1.09}Ge{sub 0.91} and HoSn{sub 1.1}Ge{sub 0.9} magnetic moments equal 7.25(15) and 8.60(6) {mu}{sub B} at 1.55 K, respectively. The moments are parallel to the c-axis. For Ho-compound this ordering is stable up to T{sub N}=10.7 K. For ErSn{sub 1.08}Ge{sub 0.92}, the Er magnetic moment equals 7.76(7) {mu}{sub B} at T=1.5 K and it is parallel to the b-axis. At T{sub t}=3.5 K it tunes into the modulated structure described by the k=(0.496(1), 0.446(4), 0). With the increase of temperature there is a slow decrease of k{sub x} component and a quick decrease of k{sub y} component. The Er magnetic moment is parallel to the b-axis up to 3.9 K while at 4 K and above it lies in the b-c plane and form an angle 48(3) deg. with the c-axis. In compounds with R=Tb, Ho and Er the magnetostriction effect at the Neel temperature is observed. - Graphical abstract: The magnetic structures of RSn{sub 1+x}Ge{sub 1-x} (R=Tb, Dy, Ho and Er, x{approx}0.1) compounds have been determined by neutron diffraction studies on polycrystalline samples. The magnetic ordering in Tb

  2. Extracting grain-orientation-dependent data from in situ time-of-flight neutron diffraction. I. Inverse pole figures

    SciTech Connect

    Stoica, Grigoreta M.; Stoica, Alexandru Dan; An, Ke; Ma, Dong; Vogel, S. C.; Carpenter, J. S.; Wang, Xun-Li

    2014-11-28

    The problem of calculating the inverse pole figure (IPF) is analyzed from the perspective of the application of time-of flight neutron diffraction toin situmonitoring of the thermomechanical behavior of engineering materials. On the basis of a quasi-Monte Carlo (QMC) method, a consistent set of grain orientations is generated and used to compute the weighting factors for IPF normalization. The weighting factors are instrument dependent and were calculated for the engineering materials diffractometer VULCAN (Spallation Neutron Source, Oak Ridge National Laboratory). The QMC method is applied to face-centered cubic structures and can be easily extended to other crystallographic symmetries. Examples include 316LN stainless steelin situloaded in tension at room temperature and an Al–2%Mg alloy, substantially deformed by cold rolling and in situannealed up to 653 K.

  3. Preliminary time-of-flight neutron diffraction studies of Escherichia coli ABC transport receptor phosphate-binding protein at the Protein Crystallography Station

    PubMed Central

    Sippel, K. H.; Bacik, J.; Quiocho, F. A.; Fisher, S. Z.

    2014-01-01

    Inorganic phosphate is an essential molecule for all known life. Organisms have developed many mechanisms to ensure an adequate supply, even in low-phosphate conditions. In prokaryotes phosphate transport is instigated by the phosphate-binding protein (PBP), the initial receptor for the ATP-binding cassette (ABC) phosphate transporter. In the crystal structure of the PBP–phosphate complex, the phosphate is completely desolvated and sequestered in a deep cleft and is bound by 13 hydrogen bonds: 12 to protein NH and OH donor groups and one to a carboxylate acceptor group. The carboxylate plays a key recognition role by accepting a phosphate hydrogen. PBP phosphate affinity is relatively consistent across a broad pH range, indicating the capacity to bind monobasic (H2PO4 −) and dibasic (HPO4 2−) phosphate; however, the mechanism by which it might accommodate the second hydrogen of monobasic phosphate is unclear. To answer this question, neutron diffraction studies were initiated. Large single crystals with a volume of 8 mm3 were grown and subjected to hydrogen/deuterium exchange. A 2.5 Å resolution data set was collected on the Protein Crystallography Station at the Los Alamos Neutron Science Center. Initial refinement of the neutron data shows significant nuclear density, and refinement is ongoing. This is the first report of a neutron study from this superfamily. PMID:24915101

  4. The magnetic and neutron diffraction studies of La{sub 1−x}Sr{sub x}MnO{sub 3} nanoparticles prepared via molten salt synthesis

    SciTech Connect

    Kačenka, M.; Kaman, O.; Jirák, Z.; Maryško, M.; Veverka, P.; Veverka, M.; Vratislav, S.

    2015-01-15

    Series of single-phase La{sub 1−x}Sr{sub x}MnO{sub 3} nanoparticles (x=0.25−0.47) with the size of about 50 nm was prepared in molten NaNO{sub 2}. TEM evidenced well dispersed particles that are not interconnected by sintering bridges in contrast to traditional products. Interestingly, some reduction of the perovskite cell volume, particularly at higher Sr-contents, was detected by XRD. Moreover, reduced magnetization and decreased Curie temperature in comparison to sol–gel samples were observed. Neutron diffraction analysis of the as-prepared nanoparticles and several comparative samples with x=0.37 indicated that the anomalous behavior of studied particles probably originate in the overdoped outer shell. The overdoping might result from both the surface oxygen chemisorption and from an increased Sr concentration in the shell. By all means, the overdoping would lead to compressive surface stress, driving the x=0.37 ground state toward a mixture of FM and A-type AFM ordering as observed by neutron diffraction. - Graphical abstract: La{sub 1−x}Sr{sub x}MnO{sub 3} nanoparticles with the size of about 50 nm were prepared by newly established method in molten NaNO{sub 2}. TEM proved the formation of well-separated particles without sintering bridges, the major advantage over traditional preparation methods. - Highlights: • Series of La{sub 1−x}Sr{sub x}MnO{sub 3} nanoparticles was prepared by novel method in NaNO{sub 2} melt. • Lower magnetization and Curie temperature in comparison to sol–gel nanoparticles was observed. • Overdoping of outer shell was indicated by neutron diffraction and cerimetric titration. • Overdoping shifts La{sub 0.37}Sr{sub 0.63}MnO{sub 3} ground state to a mixture of FM and A-type AFM ordering.

  5. Magnetic structures and magnetic phase transitions in the Mn-doped orthoferrite TbFeO3 studied by neutron powder diffraction

    NASA Astrophysics Data System (ADS)

    Nair, Harikrishnan S.; Chatterji, Tapan; Kumar, C. M. N.; Hansen, Thomas; Nhalil, Hariharan; Elizabeth, Suja; Strydom, André M.

    2016-02-01

    The magnetic structures and the magnetic phase transitions in the Mn-doped orthoferrite TbFeO3 studied using neutron powder diffraction are reported. Magnetic phase transitions are identified at TN Fe / Mn ≈ 295 K where a paramagnetic-to-antiferromagnetic transition occurs in the Fe/Mn sublattice, TS R Fe / Mn ≈ 26 K where a spin-reorientation transition occurs in the Fe/Mn sublattice and TN R ≈ 2 K where Tb-ordering starts to manifest. At 295 K, the magnetic structure of the Fe/Mn sublattice in TbFe 0.5 Mn 0.5 O3 belongs to the irreducible representation Γ 4 ( G x A y F z or P b ' n ' m ). A mixed-domain structure of ( Γ 1 + Γ 4 ) is found at 250 K which remains stable down to the spin re-orientation transition at TS R Fe / Mn ≈ 26 K. Below 26 K and above 250 K, the majority phase ( > 80 % ) is that of Γ 4 . Below 10 K the high-temperature phase Γ 4 remains stable till 2 K. At 2 K, Tb develops a magnetic moment value of 0.6(2) μ B / f.u. and orders long-range in Fz compatible with the Γ 4 representation. Our study confirms the magnetic phase transitions reported already in a single crystal of TbFe 0.5 Mn 0.5 O3 and, in addition, reveals the presence of mixed magnetic domains. The ratio of these magnetic domains as a function of temperature is estimated from Rietveld refinement of neutron diffraction data. Indications of short-range magnetic correlations are present in the low-Q region of the neutron diffraction patterns at T < TS R Fe / Mn . These results should motivate further experimental work devoted to measure electric polarization and magnetocapacitance of TbFe 0.5 Mn 0.5 O3.

  6. A multisectional annular thermal-neutron detector for the study of diffraction on microsamples in axial geometry

    NASA Astrophysics Data System (ADS)

    Belushkin, A. V.; Bogdzel', A. A.; Buzdavin, A. P.; Veleshki, S. I.; Zhuravlev, A. I.; Zhuravlev, V. V.; Kichanov, S. E.; Kozlenko, D. P.; Kulikov, S. A.; Levchanovskii, F. V.; Lukin, E. V.; Milkov, V. M.; Murashkevich, S. M.; Panteleev, Ts. Ts.; Prikhod'ko, V. I.; Savenko, B. N.; Tsankov, L. T.

    2013-09-01

    A new gaseous annular sectional thermal-neutron detector for the new neutron diffractometer at the IBR-2 reactor has been designed and manufactured at the Frank Laboratory of Neutron Physics of the Joint Institute for Nuclear Research (JINR). The detector is designed to study small-volume samples at high pressure and consists of 16 sections, each one of which is divided into six independent detector elements. We present the main design features of the detector, detecting electronics, data-acquisition and visualization software, and software system for experiment management. The results of the first neutronographic experiments that were carried out with the use of the detector are also presented.

  7. Simultaneous neutron diffraction and microwave dielectric characterisation of ammine materials - a non-destructive, non-contact characterisation tool for determining ammonia content in solids.

    PubMed

    Jones, Martin Owen; Hartley, Jon; Porch, Adrian

    2016-08-17

    We have investigated ammonia adsorption in group two halides (MgI2 and CaBr2) using custom-built apparatus that permits simultaneous neutron diffraction, microwave dielectric characterisation and out-gas mass spectroscopy of solid state materials during ammonia adsorption. Deuterated ammonia was flowed over the sample and the uptake - as measured by mass flow meters, mass spectroscopy and structure - compared with the change in dielectric constant. An excellent correlation between ammonia content and dielectric property was observed and, when linked to diffraction, mass flow and mass spectroscopy data, could be used to determine the amount of ammonia present within the solid. The combination of these techniques could also be used to differentiate physisorbed and metal-coordinated ammonia and explain subtleties in the observed structural transformations. PMID:27498837

  8. X-ray and Neutron Diffraction Studies of Rb{sub 4}LiH{sub 3}(XO{sub 4}){sub 4} (X = S, Se) Single Crystals

    SciTech Connect

    Troyanov, S.I.; Snigireva, E.M.; Ling, C.D.

    2004-11-01

    Rb{sub 4}LiH{sub 3}(SeO{sub 4}){sub 4} single crystals (1) are studied by the X-ray diffraction method at 180 K and Rb{sub 4}LiH{sub 3}(SO{sub 4}){sub 4} single crystals (2a-2c) are studied by the neutron diffraction method at 298 K (2a and 2b) and 480 K (2c). It is established that isostructural single crystals 1 and 2 (sp. gr. P4{sub 1}) have analogous systems of hydrogen bonds: chains of four XO{sub 4} tetrahedra linked by three H bonds with the central bond (2.49 A) being somewhat shorter than the terminal ones (2.52-2.54 A). In the high-temperature 2c phase, the amplitudes of atomic thermal vibrations and the degree of proton disorder in the central hydrogen bond have somewhat elevated values.

  9. In-situ neutron diffraction study of martensitic variant redistribution in polycrystalline Ni-Mn-Ga alloy under cyclic thermo-mechanical treatment

    SciTech Connect

    Li, Zongbin; Zou, Naifu; Zhao, Xiang; Zuo, Liang E-mail: yudong.zhang@univ-lorraine.fr; Zhang, Yudong E-mail: yudong.zhang@univ-lorraine.fr; Esling, Claude; Gan, Weimin

    2014-07-14

    The influences of uniaxial compressive stress on martensitic transformation were studied on a polycrystalline Ni-Mn-Ga bulk alloy prepared by directional solidification. Based upon the integrated in-situ neutron diffraction measurements, direct experimental evidence was obtained on the variant redistribution of seven-layered modulated (7M) martensite, triggered by external uniaxial compression during martensitic transformation. Large anisotropic lattice strain, induced by the cyclic thermo-mechanical treatment, has led to the microstructure modification by forming martensitic variants with a strong 〈0 1 0〉{sub 7M} preferential orientation along the loading axis. As a result, the saturation of magnetization became easier to be reached.

  10. Anomalous Depletion of Pore-Confined Carbon Dioxide upon Cooling below the Bulk Triple Point: An In Situ Neutron Diffraction Study.

    PubMed

    Stefanopoulos, K L; Katsaros, F K; Steriotis, Th A; Sapalidis, A A; Thommes, M; Bowron, D T; Youngs, T G A

    2016-01-15

    The phase behavior of sorbed CO{2} in an ordered mesoporous silica sample (SBA-15) was studied by neutron diffraction. Surprisingly, upon cooling our sample below the bulk critical point, confined CO{2} molecules neither freeze nor remain liquid as expected, but escape from the pores. The phenomenon has additionally been confirmed gravimetrically. The process is reversible and during heating CO{2} refills the pores, albeit with hysteresis. This depletion was for the first time observed in an ordered mesoporous molecular sieve and provides new insight on the phase behavior of nanoconfined fluids. PMID:26824548

  11. Change in the magnetic structure of (Bi,Sm)FeO{sub 3} thin films at the morphotropic phase boundary probed by neutron diffraction

    SciTech Connect

    Maruyama, Shingo; Anbusathaiah, Varatharajan; Takeuchi, Ichiro; Fennell, Amy; Enderle, Mechthild; Ratcliff, William D.

    2014-11-01

    We report on the evolution of the magnetic structure of BiFeO{sub 3} thin films grown on SrTiO{sub 3} substrates as a function of Sm doping. We determined the magnetic structure using neutron diffraction. We found that as Sm increases, the magnetic structure evolves from a cycloid to a G-type antiferromagnet at the morphotropic phase boundary, where there is a large piezoelectric response due to an electric-field induced structural transition. The occurrence of the magnetic structural transition at the morphotropic phase boundary offers another route towards room temperature multiferroic devices.

  12. Neutron powder diffraction study of Ba3ZnRu2-xIrxO9 (x = 0, 1, 2) with 6H-type perovskite structure

    NASA Astrophysics Data System (ADS)

    Beran, P.; Ivanov, S. A.; Nordblad, P.; Middey, S.; Nag, A.; Sarma, D. D.; Ray, S.; Mathieu, R.

    2015-12-01

    The triple perovskites Ba3ZnRu2-xIrxO9 with x = 0, 1, and 2 are insulating compounds in which Ru(Ir) cations form a dimer state. Polycrystalline samples of these materials were studied using neutron powder diffraction (NPD) at 10 and 295 K. No structural transition nor evidence of long range magnetic order was observed within the investigated temperature range. The results from structural refinements of the NPD data and its polyhedral analysis are presented, and discussed as a function of Ru/Ir content.

  13. Analysis of the Plasticity-Enhancing Mechanisms in 12 pctMn Austeno-ferritic Steel by In Situ Neutron Diffraction

    NASA Astrophysics Data System (ADS)

    Lee, Sangwon; Woo, Wanchuck; De Cooman, Bruno C.

    2014-12-01

    The tensile behavior of ductile ultra-high strength Fe-12 pctMn-0.3 pctC-2 pctAl austeno-ferritic steel was studied by in situ neutron diffraction measurement of the elastic lattice strains, dislocation density, stacking fault probability, and strain-induced transformation kinetics. Micro-yielding was observed in austenite, and the plastic deformation of ferrite remained very limited throughout the deformation. The analysis identified three contributions to the strain hardening: twinning-induced plasticity, transformation-induced plasticity, and the accumulation of a high density of geometrically necessary dislocations accommodating the strain mismatch at the phase boundaries.

  14. Dimethylamine borane dehydrogenation chemistry: syntheses, X-ray and neutron diffraction studies of 18-electron aminoborane and 14-electron aminoboryl complexes.

    PubMed

    Tang, Christina Y; Phillips, Nicholas; Bates, Joshua I; Thompson, Amber L; Gutmann, Matthias J; Aldridge, Simon

    2012-08-21

    The reactions of Me(2)NH·BH(3) with cationic Rh(III) and Ir(III) complexes have been shown to generate the 18-electron aminoborane adduct [Ir(IMes)(2)(H)(2){κ(2)-H(2)BNMe(2))](+) and the remarkable 14-electron aminoboryl complex [Rh(IMes)(2)(H)-{B(H)NMe(2))](+). Neutron diffraction studies have been used for the first time to define H-atom locations in metal complexes of this type formed under catalytic conditions. PMID:22781307

  15. Neutron diffraction study of magnetic field induced behavior in the heavy Fermion Ce3Co4Sn13

    SciTech Connect

    Christianson, Andrew D; Goremychkin, E. A.; Gardner, J. S.; Kang, H. J.; Chung, J.-H.; Manuel, P.; Thompson, J. D.; Sarrao, J. L.; Lawrence, J. M.

    2008-01-01

    The specific heat of Ce3Co4Sn13 exhibits a crossover from heavy Fermion behavior with antiferromagnetic correlations at low field to single impurity Kondo behavior above 2 T. We have performed neutron diffraction measurements in magnetic fields up to 6 Tesla on single crystal samples. The (001) position shows a dramatic increase in intensity in field which appears to arise from static polarization of the 4f level and which at 0.14 K also exhibits an anomaly near 2T reflecting the crossover to single impurity behavior.

  16. Neutron and X-ray diffraction analysis of the effect of irradiation dose and temperature on microstructure of irradiated HT-9 steel

    NASA Astrophysics Data System (ADS)

    Mosbrucker, P. L.; Brown, D. W.; Anderoglu, O.; Balogh, L.; Maloy, S. A.; Sisneros, T. A.; Almer, J.; Tulk, E. F.; Morgenroth, W.; Dippel, A. C.

    2013-11-01

    Material harvested from several positions within a nuclear fuel duct (the ACO-3 duct) used in a 6-year irradiation of a fuel assembly in the Fast Flux Test Reactor Facility (FFTF) was examined using neutron and high-energy X-ray diffraction. Samples with a wide range of irradiation dose and irradiation temperature history, reaching doses of up to 147 dpa and temperatures of up to 777 K, were examined. The response of various microstructural characteristics such as the weight fraction of M23C6 carbides, the dislocation density and character, and the crystallographic texture were determined using whole profile analysis of the diffraction data and related to the macroscopic mechanical behavior. For instance, the dislocation density was observed to be intimately linked with observed flow strength of the irradiated materials, following the Taylor law. In general, at the high doses studied in this work, the irradiation temperature is the predominant controlling factor of the dislocation density and, thus, the flow strength of the irradiated material. The results, representing some of the first diffraction work done on samples exposed to such a high received dose, demonstrate how non-destructive and stand-off diffraction techniques can be used to characterize irradiation induced microstructure and at least estimate mechanical properties in irradiated materials without exposing workers to radiation hazards.

  17. A Hybrid Reflective/Refractive/Diffractive Achromatic Fiber-Coupled Radiation Resistant Imaging System for Use in the Spallation Neutron Source (SNS)

    SciTech Connect

    Maxey, L Curt; Ally, Tanya R; Brunson, Aly; Garcia, Frances; Goetz, Kathleen C; Hasse, Katelyn E; McManamy, Thomas J; Shea, Thomas J; Simpson, Marc Livingstone

    2011-01-01

    A fiber-coupled imaging system for monitoring the proton beam profile on the target of the Spallation Neutron Source was developed using reflective, refractive and diffractive optics to focus an image onto a fiber optic imaging bundle. The imaging system monitors the light output from a chromium-doped aluminum oxide (Al{sub 2}0{sub 3}:Cr) scintillator on the nose of the target. Metal optics are used to relay the image to the lenses that focus the image onto the fiber. The material choices for the lenses and fiber were limited to high-purity fused silica, due to the anticipated radiation dose of 10{sup 8} R. In the first generation system (which had no diffractive elements), radiation damage to the scintillator on the nose of the target significantly broadened the normally monochromatic (694 nm) spectrum. This created the need for an achromatic design in the second generation system. This was achieved through the addition of a diffractive optic for chromatic correction. An overview of the target imaging system and its performance, with particular emphasis on the design and testing of a hybrid refractive/diffractive high-purity fused silica imaging triplet, is presented.

  18. Neutron-diffraction studies of the crystal structure and the color enhancement in γ-irradiated tourmaline

    NASA Astrophysics Data System (ADS)

    Maneewong, Apichate; Seong, Baek Seok; Shin, Eun Joo; Kim, Jeong Seog; Kajornrith, Varavuth

    2016-01-01

    Tourmaline gemstones have an extremely complex composition and show great variety in color. Most color centers are related to transition-metal ions. Oxidation/reduction of these ions is known to be related with the color enhancement of tourmaline caused by gamma-ray ( γ)-irradiation and/or thermal treatment. However, the current understanding of the microscopic structure of the color centers remains weak. In this work, γ-irradiation was performed on three types of tourmaline gemstones to enhance the colors of the gemstones: two pink from Afghanistan and one green from Nigeria. All three samples were irradiated at 600 and 800 kGy. Their crystal structural and chemical behaviors have been investigated by using a Rietveld refinement analysis of neutron diffraction data, Energy Dispersive X-ray Fluorescence (EDXRF), Ultraviolet-visible Spectroscopy (UV-Vis) and X-ray Photoelectron Spectroscopy (XPS), and the results were compared with data obtained for samples in the natural state. Pink tourmaline of a high number of Mn ions (T2, 0.24 wt%) showed significant improvement in the quality of the pink color (rubellite) after irradiation of 800 kGy while the pink tourmaline of low MnO content (T1, 0.08 wt%) showed color adulteration. Pink color enhancement in T2, responding to darker pink, was associated with increases in the two absorption bands, one peaking at 396 and the other at 522 nm, after irradiation. These absorption bands are ascribed to d-d transitions of divalent manganese. T1 with color enhancement due to oxidation of Mn2+ showed a slightly larger < Y- O> distance. The green tourmaline containing much higher amounts of both Mn (T3) and Fe ions, 2.59 wt% and 5.7 wt%, respectively, changed to a yellow color after irradiation at 800 kGy. The refined structural parameters of this sample revealed distortions in the Z site. The < Z- O> distance decreased from 2.033 to 2.0192 Å. In addition, the unit-cell parameter was decreased after irradiation. The color change

  19. Polarisation modulation in X-ray binaries

    NASA Astrophysics Data System (ADS)

    Ingram, Adam; Maccarone, Thomas

    2016-07-01

    X-ray polarimetry promises to provide a powerful new lever arm for studying accretion onto black holes with the next generation of X-ray telescopes. I will discuss how polarisation can be used to help constrain the physical origin of quasi-periodic oscillations (QPOs) observed in the X-ray light curves of accreting black holes. QPOs may be signatures of the frame dragging effect: in General Relativity, a spinning black hole twists up the surrounding space-time, causing vertical precession of nearby orbits. In the truncated disc / precessing inner flow model, the entire inner accretion flow precesses as a solid body causing a modulation in the X-ray flux through solid angle and Doppler effects. This model also predicts the observed polarisation of the X-ray signal to vary quasi-periodically. I will summarise our work to model the polarisation signal from a precessing accretion flow, starting with simple assumptions about the emission mechanism but taking General Relativity fully into account. We find that it should be possible to measure the predicted modulation in polarisation degree for a reasonable region of parameter space with a polarimeter capable of detecting ~60 counts per second from a bright black hole binary. I will also show that sensitivity can be greatly improved by correlating the signal with a high count rate reference band signal.

  20. Optimal polarisation equations in FLRW universes

    SciTech Connect

    Tram, Thomas; Lesgourgues, Julien E-mail: Julien.Lesgourgues@cern.ch

    2013-10-01

    This paper presents the linearised Boltzmann equation for photons for scalar, vector and tensor perturbations in flat, open and closed FLRW cosmologies. We show that E- and B-mode polarisation for all types can be computed using only a single hierarchy. This was previously shown explicitly for tensor modes in flat cosmologies but not for vectors, and not for non-flat cosmologies.

  1. Polarisation of electroweak gauge bosons at the LHC

    NASA Astrophysics Data System (ADS)

    Stirling, James; Vryonidou, Eleni

    2013-05-01

    We present results for the polarisation of gauge bosons produced at the LHC. Polarisation effects for W bosons manifest themselves in the angular distributions of the lepton and in the distributions of lepton transverse momentum and missing transverse energy. The polarisation is discussed for a range of different processes producing W bosons such as W+jets and W from top production. The relative contributions of the different polarisation states vary from process to process, reflecting the dynamics of the underlying hardscattering process. We also calculate the polarisation of the Z boson produced in association with QCD jets at the LHC.

  2. Muon Spin Relaxation and Neutron Diffraction Studies of Cluster-Glass States in Sr1‑xLaxRuO3

    NASA Astrophysics Data System (ADS)

    Kawasaki, Ikuto; Fujimura, Kenji; Watanabe, Isao; Avdeev, Maxim; Tenya, Kenichi; Yokoyama, Makoto

    2016-05-01

    To clarify the magnetic properties of cluster-glass states in Sr1-xLaxRuO3 (0.3 <= x <= 0.5), we report herein the results of muon spin relaxation (muSR) and neutron powder diffraction measurements. The muSR experiments showed that magnetic clusters start developing well above the peak temperature T^* in the ac susceptibility. The volume fraction of the magnetically ordered region increases continuously with decreasing temperature, showing no anomaly at T^*, and reaches nearly 100% at the lowest temperature. The temperature variation of the volume fraction is essentially independent of the La concentration in the x range presently investigated, although the dc magnetization is significantly suppressed with increasing x. Neutron powder diffraction experiments revealed that the ground state for x = 0.3 is a long-range ferromagnetic ordered state. These results indicate that, with decreasing temperature, cluster-glass states in Sr1-xLaxRuO3 gradually develop into long-range ferromagnetic ordered states with decreasing temperature, and that the magnetic ordering process differs strikingly from that expected for a conventional second-order ferromagnetic transition.

  3. Combined X-Ray and Neutron Powder Diffraction Studies of Nanoscale Ca5-xFex(PO4)3OH Systems

    NASA Astrophysics Data System (ADS)

    Kyriacou, A.; Leventouri, Th.; Chakoumakos, B. C.; Garlea, V. O.; Cruz, C. D.; Rondinone, A. J.; Sorge, K. D.

    2012-02-01

    Multi-substituted hydroxyapatite (HAp) with crystallite size 4-130 nm is the major mineral phase in physiological apatites. Substitutions at all ionic sites affect their physicochemical properties. Fe is one of the minor substitutions at the Ca sites of HAp. It is important because it reduces the solubility of HAp, functioning as a cavities preventive agent, whereas Fe overload leads to a decreased mechanical strength and osteoporosis. Powder x-ray and neutron diffraction methods as well as energy-filtered transmission electron microscopy were used to study the effect of Fe substitution on the crystal structure properties of the Ca(5-x)Fex(PO4)3OH systems. Single phase HAp is identified in systems with x <= 0.1. Hematite is formed for higher x. Simultaneous Rietveld refinement of the x-ray and neutron diffraction patterns reveals an unexpected increase of the a-lattice constant. It is attributed to the increase of the Ca1-O3 and Ca2-O1 interatomic distances indicating a local lattice relaxation. Fe substitutes in both Ca1 and Ca2 sites with a preference to the Ca2 site and an occupancy up to 0.05 for x=0.3. Magnetic measurements reveal a transition from the diamagnetic state of the HAp to the paramagnetic of the Fe-doped systems.

  4. A high temperature neutron diffraction study of the double perovskite Ba{sub 2}{sup 154}SmMoO{sub 6}

    SciTech Connect

    Wallace, Thomas K.; Ritter, Clemens; Mclaughlin, Abbie C.

    2012-12-15

    Ba{sub 2}LnMoO{sub 6} double perovskites have been recently shown to display a wide range of interesting magnetic and structural properties; Ba{sub 2}{sup 154}SmMoO{sub 6} exhibits simultaneous antiferromagnetic order and a Jahn-Teller distortion. Here we report a high temperature neutron diffraction study of Ba{sub 2}{sup 154}SmMoO{sub 6} from 353 to 877 K. The results evidence a tetragonal to cubic phase transition at 423 K. Above this temperature the thermal displacement parameters of the oxygen atoms are modelled anisotropically as a result of a transverse vibration of the bridging oxygen. A smooth increase in the cell parameter a is observed with temperature for Ba{sub 2}{sup 154}SmMoO{sub 6}. - Graphical abstract: The high temperature crystal structure of Ba{sub 2}{sup 154}SmMoO{sub 6} evidencing a transverse oxygen vibration. Highlights: Black-Right-Pointing-Pointer A high temperature neutron diffraction study has been performed on an isotopically enriched sample of Ba{sub 2}{sup 154}SmMoO{sub 6}. Black-Right-Pointing-Pointer A cubic-tetragonal phase transition occurs below 423 K. Black-Right-Pointing-Pointer The thermal displacement parameters of the bridging oxygens are modelled anisotropically. Black-Right-Pointing-Pointer There is a transverse vibration of the bridging oxygen.

  5. The magnetic and neutron diffraction studies of La1-xSrxMnO3 nanoparticles prepared via molten salt synthesis

    NASA Astrophysics Data System (ADS)

    Kačenka, M.; Kaman, O.; Jirák, Z.; Maryško, M.; Veverka, P.; Veverka, M.; Vratislav, S.

    2015-01-01

    Series of single-phase La1-xSrxMnO3 nanoparticles (x=0.25-0.47) with the size of about 50 nm was prepared in molten NaNO2. TEM evidenced well dispersed particles that are not interconnected by sintering bridges in contrast to traditional products. Interestingly, some reduction of the perovskite cell volume, particularly at higher Sr-contents, was detected by XRD. Moreover, reduced magnetization and decreased Curie temperature in comparison to sol-gel samples were observed. Neutron diffraction analysis of the as-prepared nanoparticles and several comparative samples with x=0.37 indicated that the anomalous behavior of studied particles probably originate in the overdoped outer shell. The overdoping might result from both the surface oxygen chemisorption and from an increased Sr concentration in the shell. By all means, the overdoping would lead to compressive surface stress, driving the x=0.37 ground state toward a mixture of FM and A-type AFM ordering as observed by neutron diffraction.

  6. Exploring the complex magnetic phase diagram of Ce2PdGe3 : A neutron powder diffraction and μ SR study

    NASA Astrophysics Data System (ADS)

    Bhattacharyya, A.; Ritter, C.; Adroja, D. T.; Coomer, F. C.; Strydom, A. M.

    2016-07-01

    The magnetic state of the tetragonal compound Ce2PdGe3 , which crystallizes in the space group P 42/m m c , a derivative of the α -ThSi2 structure, has been investigated by magnetic susceptibility, heat capacity, muon spin relaxation (μ SR ), and neutron diffraction measurements. Heat capacity data indicate two separate magnetic phase transitions at TN1=10.7 K and TN 2=2.3 K. The presence of bulk long-range magnetic order is confirmed by our μ SR study below 11 K, where a drop of nearly 2/3 in the muon initial asymmetry and a sharp increase in the muon depolarization rate were observed. Neutron powder diffraction reveals that only one out of two Ce sites becomes magnetically ordered with magnetic propagation vector κ =(0 ) at TN1,adopting an antiferromagnetic arrangement of magnetic moments μCe3+=1.78 (1 ) μB along the c axis. At TN 2 the second Ce site orders similarly, following the same magnetic propagation vector κ =(0 ) , showing, however, at the same time a significant ferromagnetic component within the tetragonal basal plane. A second propagation vector, κ =(1/2 ,0 ,1/2 ) , appears concomitantly at TN 2.

  7. Neutron diffraction measurements and first-principles study of thermal motion of atoms in select Mn+1AXn and binary MX transition-metal carbide phases

    NASA Astrophysics Data System (ADS)

    Lane, Nina J.; Vogel, Sven C.; Hug, Gilles; Togo, Atsushi; Chaput, Laurent; Hultman, Lars; Barsoum, Michel W.

    2012-12-01

    Herein, we compare the thermal vibrations of atoms in select ternary carbides with the formula Mn+1AXn (“MAX phases,” M = Ti, Cr; A = Al, Si, Ge; X = C, N) as determined from first-principles phonon calculations to those obtained from high-temperature neutron powder diffraction studies. The transition metal carbides TiC, TaC, and WC are also studied to test our methodology on simpler carbides. Good qualitative and quantitative agreement is found between predicted and experimental values for the binary carbides. For all the MAX phases studied—Ti3SiC2, Ti3GeC2, Ti2AlN, Cr2GeC and Ti4AlN3—density functional theory calculations predict that the A element vibrates with the highest amplitude and does so anisotropically with a higher amplitude within the basal plane, which is in line with earlier results from high-temperature neutron diffraction studies. In some cases, there are quantitative differences in the absolute values between the theoretical and experimental atomic displacement parameters (ADPs), such as reversal of anisotropy or a systematic offset of temperature-dependent ADPs. The mode-dependent Grüneisen parameters are also computed to explore the anharmonicity in the system.

  8. In-situ neutron diffraction of LaCoO3 perovskite under uniaxial compression. I. Crystal structure analysis and texture development

    SciTech Connect

    Aman, Amjad; Chen, Yan; Lugovy, Mykola; Orlovskaya, Nina; Reece, Michael John; Ma, Dong; Stoica, Alexandru Dan; An, Ke

    2014-01-01

    The dynamics of texture formation, changes in crystal structure and stress accommodation mechanisms are studied in R3c rhombohedral LaCoO3 perovskite during in-situ uniaxial compression experiment by neutron diffraction. The neutron diffraction revealed the complex crystallographic changes causing the texture formation and significant straining along certain crystallographic directions during in-situ compression, which are responsible for the appearance of hysteresis and non-linear ferroelastic deformation in LaCoO3 perovskite. The irreversible strain after the first loading was connected with the appearance of non-recoverable changes in the intensity ratio of certain crystallographic peaks, causing non-reversible texture formation. However in the second loading/unloading cycle the hysteresis loop was closed and no irreversible strain appears after deformation. The significant texture formation is responsible for increase in the Young s modulus of LaCoO3 at high compressive loads, where the reported values of Young s modulus increase from 76 GPa measured at the very beginning of the loading to 194 GPa at 900 MPa applied compressive stress measured at the beginning of the unloading curve.

  9. In-situ neutron diffraction of LaCoO3 perovskite under uniaxial compression. I. Crystal structure analysis and texture development

    NASA Astrophysics Data System (ADS)

    Aman, Amjad; Chen, Yan; Lugovy, Mykola; Orlovskaya, Nina; Reece, Michael J.; Ma, Dong; Stoica, Alexandru D.; An, Ke

    2014-07-01

    The dynamics of texture formation, changes in crystal structure, and stress accommodation mechanisms have been studied in perovskite-type R3¯c rhombohedral LaCoO3 during uniaxial compression using in-situ neutron diffraction. The in-situ neutron diffraction revealed the complex crystallographic changes causing the texture formation and significant straining along certain crystallographic directions during compression, which are responsible for the appearance of hysteresis and non-linear ferroelastic deformation in the LaCoO3 perovskite. The irreversible strain after the first loading was connected with the appearance of non-recoverable changes in the intensity ratio of certain crystallographic peaks, causing non-reversible texture formation. However, in the second loading/unloading cycle, the hysteresis loop was closed and no further irrecoverable strain appeared after deformation. The significant texture formation is responsible for an increase in the Young's modulus of LaCoO3 at high compressive stresses, ranging from 76 GPa at the very beginning of the loading to 194 GPa at 900 MPa at the beginning of the unloading curve.

  10. In-situ neutron diffraction of LaCoO₃ perovskite under uniaxial compression. I. Crystal structure analysis and texture development

    SciTech Connect

    Aman, Amjad; Orlovskaya, Nina; Chen, Yan; Lugovy, Mykola; Reece, Michael J.; Ma, Dong; Stoica, Alexandru D.; An, Ke

    2014-07-07

    The dynamics of texture formation, changes in crystal structure, and stress accommodation mechanisms have been studied in perovskite-type R3⁻c rhombohedral LaCoO₃ during uniaxial compression using in-situ neutron diffraction. The in-situ neutron diffraction revealed the complex crystallographic changes causing the texture formation and significant straining along certain crystallographic directions during compression, which are responsible for the appearance of hysteresis and non-linear ferroelastic deformation in the LaCoO₃ perovskite. The irreversible strain after the first loading was connected with the appearance of non-recoverable changes in the intensity ratio of certain crystallographic peaks, causing non-reversible texture formation. However, in the second loading/unloading cycle, the hysteresis loop was closed and no further irrecoverable strain appeared after deformation. The significant texture formation is responsible for an increase in the Young's modulus of LaCoO₃ at high compressive stresses, ranging from 76 GPa at the very beginning of the loading to 194 GPa at 900 MPa at the beginning of the unloading curve.

  11. Structural, thermodynamic, and transport properties of Laves-phase ZrMn2 from x-ray and neutron diffraction and first principles

    NASA Astrophysics Data System (ADS)

    Rotter, M.; Grytsiv, A.; Chen, Xing-Qiu; Rogl, P.; Podloucky, R.; Wolf, W.; Witusiewicz, V. T.; Saccone, A.; Noel, H.; Doerr, M.; Lindbaum, A.; Michor, H.; Bauer, E.; Heathman, S.; Kockelmann, W.; Taylor, J.

    2006-12-01

    Recently, the prediction of structural degeneracy for the ground state of ZrMn2 by ab initio methods has stimulated research on this system. We investigated the structural and thermodynamic properties by single crystal and powder x-ray diffraction (at zero and high pressure) as well as by neutron powder diffraction, demonstrating that the C14 Laves phase structure is stable down to a temperature of 4.2K and up to applied pressure of 56GPa . The bulk modulus and enthalpy of formation (measured by high-temperature drop calorimetric experiments) of ZrMn2 are found to be 150GPa and -66.6kJ(moloff.u.)-1 , respectively, in nice agreement with the ab initio calculated results. The experimental bulk thermal-expansion data of ZrMn2 resembles that of a typical metal. However, the temperature-dependent electrical resisitivity shows that there is a power law with n≈1.1 at low temperature quite different from simple metals which originates probably from scattering of the charge carriers on the frustrated Mn moments. The phonons have been investigated in detail by comparing results of ab initio calculations with neutron spectra and experimental specific-heat data.

  12. Low temperature neutron diffraction study of Nd1-xSrxCrO3 (0.05≤x≤0.15)

    NASA Astrophysics Data System (ADS)

    Chakraborty, Keka R.; Mukherjee, S.; Kaushik, S. D.; Rayaprol, S.; Prajapat, C. L.; Singh, M. R.; Siruguri, V.; Tyagi, A. K.; Yusuf, S. M.

    2014-06-01

    Low temperature magnetic structure of Sr substituted NdCrO3 has been investigated using neutron diffraction in the temperature range of 2-300 K. We carried out a low temperature magnetization study in the temperature range 5-300 K. The Rietveld analysis of neutron diffraction patterns led us to conclude that the Cr moments have a Gy type of alignment of spins while the Nd moments align in a -Cz type fashion for all three samples. The weighted average Cr3+/4+ ions moments were 3.19(7), 2.77(3) and 2.57(7) μB close to its theoretical Cr3+ moment value namely 3 μB at 2 K for the x=0.05, 0.1 and 0.15 samples respectively. While the Nd3+ moments for the three samples at 2 K were 3.0(1), 2.39(8) and 2.2(2), respectively.

  13. Application of neutron diffraction in characterization of texture evolution during high-temperature creep in magnesium alloys

    SciTech Connect

    Vogel, Sven C; Sediako, Dimitry; Shook, S; Sediako, A

    2010-01-01

    A good combination of room-temperature and elevated temperature strength and ductility, good salt-spray corrosion resistance and exceUent diecastability are frequently among the main considerations in development of a new alloy. 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 becomes an important factor 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. These studies were performed using E3 neutron spectrometer of the Canadian Neutron Beam Centre in Chalk River, ON, and HIPPO time-of-flight (TOF) spectrometer at Los Alamos Neutron Science Center, NM.

  14. X-ray diffraction analysis of secondary phases in zirconium alloys before and after neutron irradiation at the MARS synchrotron radiation beamline

    NASA Astrophysics Data System (ADS)

    Béchade, J.-L.; Menut, D.; Doriot, S.; Schlutig, S.; Sitaud, B.

    2013-06-01

    To further advance understanding of microstructural evolution in zirconium alloys for high burnup applications in PWR, it is important to obtain precise characterizations of second-phase particles present in the bulk alloys as a function of the neutron-irradiation fluence. X-ray diffraction from a synchrotron radiation source (SOLEIL) was used to identify and follow the evolution of second-phase particles that are in very small volume fractions in two zirconium alloys: Zy-4 in stress-relieved metallurgical state before irradiation and Zr-1%Nb (M5®) in recrystallized metallurgical state before and after neutron irradiation. Despite the fact the neutron irradiated sample is not in the as-irradiated state due to a thermal treatment and creep test performed after irradiation, interesting results have been obtained on secondary phases using XRD techniques. Analyses have been performed at the MARS beamline, fully dedicated to advanced structural and chemical characterizations of radioactive matter. A first proof of the improvement brought by these new analyses performed at the MARS beamline is given with Zr(Fe, Cr)2 precipitates found in unirradiated Zy-4 alloy in stress relieved metallurgical state, highly textured and displaying significant residual stresses and numerous dislocations: lattice parameters, crystallite size and microstrains (line profile analysis using the Williamson-Hall method after correction for instrumental broadening) have been estimated with very good accuracy. Then, second phase particles of the Zr-1%Nb alloy (M5®) have been analyzed before and after irradiation. For the Zr(Fe, Nb)2 Laves phase, the diffraction line disappeared after neutron irradiation. For β-Nb phases, the evolution of diffraction peaks clearly show the convolution of two phenomena: in one hand slight decreases in Nb content for native β-Nb particles and on the other hand irradiation-enhanced precipitation of nano-sized needle-like β-Nb particles. To our knowledge, this is

  15. Neutron diffraction study and superparamagnetic behavior of ZnFe{sub 2}O{sub 4} nanoparticles obtained with different conditions

    SciTech Connect

    Blanco-Gutierrez, V.; Climent-Pascual, E.; Torralvo-Fernandez, M.J.; Saez-Puche, R.; Fernandez-Diaz, M.T.

    2011-07-15

    Spinel-type (S.G.= Fd3-bar m) ZnFe{sub 2}O{sub 4} fine particles with sizes from 4 to 19 nm prepared by solvothermal and microwave-assisted solvothermal methods have been studied by neutron powder diffraction at room temperature. The cation distribution corresponding to mixed spinel structure (Zn{sup 2+}{sub 1-x}Fe{sup 3+}{sub x})[Fe{sup 3+}{sub 2-x}Zn{sup 2+}{sub x}]O{sub 4} along with the unit cell parameter has been estimated after Rietveld refinement of the obtained neutron diffraction data for all the samples. It has been found that the inversion degree parameter (x) takes values between 0.11 and 0.20 depending not only on the particle size but also on the synthesis conditions as well. All the samples behave as superparamagnetic with an effective magnetic moment per particle ({mu}{sub SP}) from 7.0x10{sup 2} to 7.7x10{sup 3} {mu}{sub B}. The sample obtained by microwave assistance displays a different magnetic behavior as the ZFC and FC magnetic susceptibility and the magnetization versus applied field hysteresis loop measured at 5 K suggest. This is related with the dipole interactions that are a consequence of the higher inversion degree and {mu}{sub SP}. - Graphical abstract: ZnFe{sub 2}O{sub 4} nanoparticles of 19 nm obtained by the solvotermal method together with its Rietveld refined pattern. Highlights: > Solvothermally prepared ZnFe{sub 2}O{sub 4} nanoparticles.{yields} Inversion degree obtained after Rietveld refinement of neutron data.{yields} Superparamagnetic behavior.{yields} Dependence with the synthesis conditions.

  16. Symmetry lowering in crystalline solid solutions: A study of cinnamamide-thienylacrylamide by x-ray and neutron diffraction and solid-state photochemistry

    SciTech Connect

    Shimon, L.J.W.; Weissinger-Lewin, Y.; McMullan, R.K. ); Vaida, M.; Frolow, F.; Lahav, M.; Leiserowitz, L. . Dept. of Materials and Interfaces)

    1993-01-01

    Principles are outlined for symmetry lowering of a mixed crystal. A survey is given of methods used to detect reduced symmetry: changes in crystal morphology, detection of enantiomeric segregation of chiral additives in centrosymmetric'' crystals, generation of second harmonic optical signals, optical birefringence, asymmetric photoreactions in the crystalline state and X-ray and neutron diffraction. The last two methods are applied to mixed crystals of cinnamamide host and thienylacrylamide. Diffraction demonstrated that the mixed crystals are composed of six sectors of reduced symmetry, from monoclinic centrosymmetric P2[sub 1]/c to triclinic P1 in four sectors and possibly Pc in the remaining two. The X-ray diffraction data were not sufficiently accurate for assigning the absolute structures of the PI sectors of anomalous X-ray scattering. Thus, by this method one could not ascertain the absolute orientation of the guest molecules on the surface sites through which they were selectively occluded. This ambiguity was resolved by assignment of the absolute configuration of the chiral heterophotodimers, between host and guest, in enantiomeric excess in the PI sectors, after irradiation with UV light. This leads to the conclusion that the selective occlusion of thienylacrylamide arises from replacement of attractive C-H[pi] (electron) interactions between host molecules by a repulsive sulfur (lone pair electron)[pi](electron) interactions between guest and host at the crystal surfaces.

  17. Symmetry lowering in crystalline solid solutions: A study of cinnamamide-thienylacrylamide by x-ray and neutron diffraction and solid-state photochemistry

    SciTech Connect

    Shimon, L.J.W.; Weissinger-Lewin, Y.; McMullan, R.K.; Vaida, M.; Frolow, F.; Lahav, M.; Leiserowitz, L.

    1993-04-01

    Principles are outlined for symmetry lowering of a mixed crystal. A survey is given of methods used to detect reduced symmetry: changes in crystal morphology, detection of enantiomeric segregation of chiral additives in ``centrosymmetric`` crystals, generation of second harmonic optical signals, optical birefringence, asymmetric photoreactions in the crystalline state and X-ray and neutron diffraction. The last two methods are applied to mixed crystals of cinnamamide host and thienylacrylamide. Diffraction demonstrated that the mixed crystals are composed of six sectors of reduced symmetry, from monoclinic centrosymmetric P2{sub 1}/c to triclinic P1 in four sectors and possibly Pc in the remaining two. The X-ray diffraction data were not sufficiently accurate for assigning the absolute structures of the PI sectors of anomalous X-ray scattering. Thus, by this method one could not ascertain the absolute orientation of the guest molecules on the surface sites through which they were selectively occluded. This ambiguity was resolved by assignment of the absolute configuration of the chiral heterophotodimers, between host and guest, in enantiomeric excess in the PI sectors, after irradiation with UV light. This leads to the conclusion that the selective occlusion of thienylacrylamide arises from replacement of attractive C-H{pi} (electron) interactions between host molecules by a repulsive sulfur (lone pair electron){pi}(electron) interactions between guest and host at the crystal surfaces.

  18. Modelling elliptically polarised free electron lasers

    NASA Astrophysics Data System (ADS)

    Henderson, J. R.; Campbell, L. T.; Freund, H. P.; McNeil, B. W. J.

    2016-06-01

    A model of a free electron laser (FEL) operating with an elliptically polarised undulator is presented. The equations describing the FEL interaction, including resonant harmonic radiation fields, are averaged over an undulator period and generate a generalised Bessel function scaling factor, similar to that of planar undulator FEL theory. Comparison between simulations of the averaged model with those of an unaveraged model show very good agreement in the linear regime. Two unexpected results were found. Firstly, an increased coupling to harmonics for elliptical rather than planar polarisarised undulators. Secondly, and thought to be unrelated to the undulator polarisation, a significantly different evolution between the averaged and unaveraged simulations of the harmonic radiation evolution approaching FEL saturation.

  19. Crystal structure of α- and β-Na{sub 2}U{sub 2}O{sub 7}: From Rietveld refinement using powder neutron diffraction data

    SciTech Connect

    IJdo, D.J.W. Akerboom, S.; Bontenbal, A.

    2015-01-15

    The crystal structures of α- and β-Na{sub 2}U{sub 2}O{sub 7} have been determined from neutron powder diffraction. At 293 K, the compound α-Na{sub 2}U{sub 2}O{sub 7} has a monoclinic unit cell, space group P2{sub 1}/a, with a=12.7617(14) Å, b=7.8384(10) Å, c=6.8962(9) Å, β=111.285(9)°, and Z=4. At 773 K, β-Na{sub 2}U{sub 2}O{sub 7} is also monoclinic, space group C2/m, with a=12.933(1) Å, b=7.887(1) Å, c=6.9086(8) Å, β=110.816(10)°, and Z=4. The structures can be described by layers U{sub 2}O{sub 7}{sup 2−} built from corner linked deformed UO{sub 6} octahedra with pentagonal UO{sub 7} bipyramids in between linked with common edges to each other and to the octahedra. The Na atoms occupy the interlayer space. The Na{sub 2}U{sub 2}O{sub 7} layers are similar as in K{sub 2}U{sub 2}O{sub 7}, but with a different stacking sequence of the layers. The layers in β-Na{sub 2}U{sub 2}O{sub 7} are more symmetric. The relationship with the compounds A{sub 2}U{sub 2}O{sub 7} (A=K, Rb, and Cs) is discussed. - Graphical abstract: The U{sub 2}O{sub 7} layer of α-Na{sub 2}U{sub 2}O{sub 7} (left) at 293 K and of β-Na{sub 2}U{sub 2}O{sub 7} (right) at 773 K determined by neutron diffraction. Some Na atoms between the layers are visible. - Highlights: • Na{sub 2}U{sub 2}O{sub 7} has been prepared by means of a solid state reaction. • The structure has been determined using neutron diffraction. • At 293 K, the compound adopts a monoclinic structure with space group P2{sub 1}/a. • The structure at 773 K is closely related, and is described in the space group C2/m.

  20. Electronically- and crystal-structure-driven magnetic structures and physical properties of RScSb (R = rare earth) compounds. A neutron diffraction, magnetization and heat capacity study

    SciTech Connect

    Ritter, C; Dhar, S K; Kulkarni, R; Provino, A; Paudyal, Durga; Manfrinetti, Pietro; Gschneidner, Karl A

    2014-08-14

    The synthesis of the new equiatomic RScSb ( R = La-Nd, Sm, Gd-Tm, Lu, Y) compounds has been recently reported. These rare earth compounds crystallize in two different crystal structures, adopting the CeScSi-type ( I 4/ mmm) for the lighter R (La-Nd, Sm) and the CeFeSi-type (P4 /nmm) structure for the heavier R ( R = Gd-Tm, Lu, Y). Here we report the results of neutron diffraction, magnetization and heat capacity measurements on some of these compounds ( R = Ce, Pr, Nd, Gd and Tb). Band structure calculations have also been performed on CeScSb and GdScGe (CeScSi-type), and on GdScSb and TbScSb (CeFeSi-type) to compare and understand the exchange interactions in CeScSi and CeFeSi structure types. The neutron diffraction investigation shows that all five compounds order magnetically, with the highest transition temperature of 66 K in TbScSb and the lowest of about 9 K in CeScSb. The magnetic ground state is simple ferromagnetic (τ = [0 0 0]) in CeScSb, as well in NdScSb for 32 >T > 22 K. Below 22 K a second magnetic transition, with propagation vector τ = [¼ ¼ 0], appears in NdScSb. PrScSb has a magnetic structure within, determined by mostly ferromagnetic interactions and antiferromagnetic alignment of the Pr-sites connected through the I-centering ( τ = [1 0 0]). A cycloidal spiral structure with a temperature dependent propagation vector τ = [δ δ ½] is found in TbScSb. The results of magnetization and heat capacity lend support to the main conclusions derived from neutron diffraction. As inferred from a sharp peak in magnetization, GdScSb orders antiferromagnetically at 56 K. First principles calculations show lateral shift of spin split bands towards lower energy from the Fermi level as the CeScSi-type structure changes to the CeFeSi-type structure. This rigid shift may force the system to transform from exchange split ferromagnetic state to the antiferromagnetic state in RScSb compounds (as seen for example in GdScSb and TbScSb) and is proposed to