Characterization of a neutron imaging setup at the INES facility

NASA Astrophysics Data System (ADS)

Durisi, E. A.; Visca, L.; Albertin, F.; Brancaccio, R.; Corsi, J.; Dughera, G.; Ferrarese, W.; Giovagnoli, A.; Grassi, N.; Grazzi, F.; Lo Giudice, A.; Mila, G.; Nervo, M.; Pastrone, N.; Prino, F.; Ramello, L.; Re, A.; Romero, A.; Sacchi, R.; Salvemini, F.; Scherillo, A.; Staiano, A.

2013-10-01

The Italian Neutron Experimental Station (INES) located at the ISIS pulsed neutron source (Didcot, United Kingdom) provides a thermal neutron beam mainly used for diffraction analysis. A neutron transmission imaging system was also developed for beam monitoring and for aligning the sample under investigation. Although the time-of-flight neutron diffraction is a consolidated technique, the neutron imaging setup is not yet completely characterized and optimized. In this paper the performance for neutron radiography and tomography at INES of two scintillator screens read out by two different commercial CCD cameras is compared in terms of linearity, signal-to-noise ratio, effective dynamic range and spatial resolution. In addition, the results of neutron radiographies and a tomography of metal alloy test structures are presented to better characterize the INES imaging capabilities of metal artifacts in the cultural heritage field.

Grating-based holographic diffraction methods for X-rays and neutrons: phase object approximation and dynamical theory

DOE PAGES

Feng, Hao; Ashkar, Rana; Steinke, Nina; ...

2018-02-01

A method dubbed grating-based holography was recently used to determine the structure of colloidal fluids in the rectangular grooves of a diffraction grating from X-ray scattering measurements. Similar grating-based measurements have also been recently made with neutrons using a technique called spin-echo small-angle neutron scattering. The analysis of the X-ray diffraction data was done using an approximation that treats the X-ray phase change caused by the colloidal structure as a small perturbation to the overall phase pattern generated by the grating. In this paper, the adequacy of this weak phase approximation is explored for both X-ray and neutron grating holography.more » Additionally, it is found that there are several approximations hidden within the weak phase approximation that can lead to incorrect conclusions from experiments. In particular, the phase contrast for the empty grating is a critical parameter. Finally, while the approximation is found to be perfectly adequate for X-ray grating holography experiments performed to date, it cannot be applied to similar neutron experiments because the latter technique requires much deeper grating channels.« less

Study of residual stresses in CT test specimens welded by electron beam

NASA Astrophysics Data System (ADS)

Papushkin, I. V.; Kaisheva, D.; Bokuchava, G. D.; Angelov, V.; Petrov, P.

2018-03-01

The paper reports result of residual stress distribution studies in CT specimens reconstituted by electron beam welding (EBW). The main aim of the study is evaluation of the applicability of the welding technique for CT specimens’ reconstitution. Thus, the temperature distribution during electron beam welding of a CT specimen was calculated using Green’s functions and the residual stress distribution was determined experimentally using neutron diffraction. Time-of-flight neutron diffraction experiments were performed on a Fourier stress diffractometer at the IBR-2 fast pulsed reactor in FLNP JINR (Dubna, Russia). The neutron diffraction data estimates yielded a maximal stress level of ±180 MPa in the welded joint.

Investigation of TbMn2O5 by polarized neutron diffraction

NASA Astrophysics Data System (ADS)

Zobkalo, I. A.; Gavrilov, S. V.; Sazonov, A.; Hutanu, V.

2018-05-01

In order to make a new approach to the elucidation of the microscopic mechanisms of multiferroicity in the RMn2O5 family, experiments with different methods of polarized neutrons scattering were performed on a TbMn2O5 single crystal. We employed three different techniques of polarized neutron diffraction without the analysis after scattering, the XYZ-polarization analysis, and technique of spherical neutron polarimetry (SNP). Measurements with SNP were undertaken both with and without external electric field. A characteristic difference in the population of ‘right’ and ‘left’ helix domains in all magnetically ordered phases of TbMn2O5, was observed. This difference can be controlled by an external electric field in the field-cooled mode. The analysis of the results gives an evidence that antisymmetric Dzyaloshinsky-Moria exchange is effective in all the magnetic phases in TbMn2O5.

Investigation of TbMn2O5 by polarized neutron diffraction.

PubMed

Zobkalo, I A; Gavrilov, S V; Sazonov, A; Hutanu, V

2018-05-23

In order to make a new approach to the elucidation of the microscopic mechanisms of multiferroicity in the RMn 2 O 5 family, experiments with different methods of polarized neutrons scattering were performed on a TbMn 2 O 5 single crystal. We employed three different techniques of polarized neutron diffraction without the analysis after scattering, the XYZ-polarization analysis, and technique of spherical neutron polarimetry (SNP). Measurements with SNP were undertaken both with and without external electric field. A characteristic difference in the population of 'right' and 'left' helix domains in all magnetically ordered phases of TbMn 2 O 5 , was observed. This difference can be controlled by an external electric field in the field-cooled mode. The analysis of the results gives an evidence that antisymmetric Dzyaloshinsky-Moria exchange is effective in all the magnetic phases in TbMn 2 O 5 .

Texture analysis of Napoleonic War Era copper bolts

NASA Astrophysics Data System (ADS)

Malamud, Florencia; Northover, Shirley; James, Jon; Northover, Peter; Kelleher, Joe

2016-04-01

Neutron diffraction techniques are suitable for volume texture analyses due to high penetration of thermal neutrons in most materials. We have implemented a new data analysis methodology that employed the spatial resolution achievable by a time-of-flight neutron strain scanner to non-destructively determine the crystallographic texture at selected locations within a macroscopic sample. The method is based on defining the orientation distribution function of the crystallites from several incomplete pole figures, and it has been implemented on ENGIN-X, a neutron strain scanner at the Isis Facility in the UK. Here, we demonstrate the application of this new texture analysis methodology in determining the crystallographic texture at selected locations within museum quality archaeological objects up to 1 m in length. The results were verified using samples of similar, but less valuable, objects by comparing the results of applying this method with those obtained using both electron backscatter diffraction and X-ray diffraction on their cross sections.

Characterisation of the incident beam and current diffraction capabilities on the VESUVIO spectrometer

NASA Astrophysics Data System (ADS)

Romanelli, G.; Krzystyniak, M.; Senesi, R.; Raspino, D.; Boxall, J.; Pooley, D.; Moorby, S.; Schooneveld, E.; Rhodes, N. J.; Andreani, C.; Fernandez-Alonso, F.

2017-09-01

The VESUVIO spectrometer at the ISIS pulsed neutron and muon source is a unique instrument amongst those available at neutron facilities. This is the only inverted-geometry neutron spectrometer accessing values of energy and wavevector transfer above tens of eV and {\\mathringA}-1 , respectively, and where deep inelastic neutron scattering experiments are routinely performed. As such, the procedure at the base of the technique has been previously described in an article published by this journal (Mayers and Reiter 2012 Meas. Sci. Technol. 23 045902). The instrument has recently witnessed an upsurge of interest due to a new trend to accommodate, within a single experiment, neutron diffraction and transmission measurements in addition to deep inelastic neutron scattering. This work presents a broader description of the instrument following these recent developments. In particular, we assess the absolute intensity and two-dimensional profile of the incident neutron beam and the capabilities of the backscattering diffraction banks. All results are discussed in the light of recent changes to the moderator viewed by the instrument. We find that VESUVIO has to be considered a high-resolution diffractometer as much as other diffractometers at ISIS, with a resolution as high as 2× 10-3 in backscattering. Also, we describe the extension of the wavelength range of the instrument to include lower neutron energies for diffraction measurements, an upgrade that could be readily applied to other neutron instruments as well.

Nuclear techniques in studies of condensed matter

NASA Technical Reports Server (NTRS)

Singh, Jag J.

1987-01-01

Nuclear techniques have played an important role in the studies of materials over the past several decades. For example, X-ray diffraction, neutron diffraction, neutron activation, and particle- or photon-induced X-ray emission techniques have been used extensively for the elucidation of structural and compositional details of materials. Several new techniques have been developed recently. Four such techniques are briefly reviewed which have great potential in the study and development of new materials. Of these four, Mossbauer spectroscopy, muon spin rotation, and positron annihilation spectroscopy techniques exploit their great sensitivity to the local atomic environments in the test materials. Interest in synchrotron radiation, on the other hand, stems from its special properties, such as high intensity, high degree of polarization, and high monochromaticity. It is hoped that this brief review will stimulate interest in the exploitation of these newer techniques for the development of improved materials.

Neutron and X-ray Microbeam Diffraction Studies around a Fatigue-Crack Tip after Overload

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

Lee, Sooyeol; Barabash, Rozaliya; Chung, Jin-Seok

2008-01-01

An in-situ neutron diffraction technique was used to investigate the lattice-strain distributions and plastic deformation around a crack tip after overload. The lattice-strain profiles around a crack tip were measured as a function of the applied load during the tensile loading cycles after overload. Dislocation densities calculated from the diffraction peak broadening were presented as a function of the distance from the crack tip. Furthermore, the crystallographic orientation variations were examined near a crack tip using polychromatic X-ray microdiffraction combined with differential aperture microscopy. Crystallographic tilts are considerably observed beneath the surface around a crack tip, and these are consistentmore » with the high dislocation densities near the crack tip measured by neutron peak broadening.« less

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

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

Balagurov, Anatoly M.; Bobrikov, Ivan A.; Bokuchava, Gizo D.

2015-11-15

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of themore » material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.« less

Investigating the Defect Structures in Transparent Conducting Oxides Using X-ray and Neutron Scattering Techniques

PubMed Central

González, Gabriela B.

2012-01-01

Transparent conducting oxide (TCO) materials are implemented into a wide variety of commercial devices because they possess a unique combination of high optical transparency and high electrical conductivity. Created during the processing of the TCOs, defects within the atomic-scale structure are responsible for their desirable optical and electrical properties. Therefore, studying the defect structure is essential to a better understanding of the behavior of transparent conductors. X-ray and neutron scattering techniques are powerful tools to investigate the atomic lattice structural defects in these materials. This review paper presents some of the current developments in the study of structural defects in n-type TCOs using x-ray diffraction (XRD), neutron diffraction, extended x-ray absorption fine structure (EXAFS), pair distribution functions (PDFs), and x-ray fluorescence (XRF). PMID:28817010

A Neutron Diffractometer for a Long Pulsed Neutron Source

NASA Astrophysics Data System (ADS)

Sokol, Paul; Wang, Cailin

Long pulsed neutron sources are being actively developed as small university based sources and are being considered for the next generation of high powered sources, such as the European Neutron Source (ESS) and the Spallation Neutron Source (SNS) second target station. New instrumentation concepts will be required to effectively utilize the full spectrum of neutrons generated by these sources. Neutron diffractometers, which utilize time-of-flight (TOF) techniques for wavelength resolution, are particularly problematic. We describe an instrument for a long pulsed source that provides resolution comparable to that obtained on short pulsed sources without the need of long incident flight paths. We accomplish this by utilizing high speed choppers to impose a time structure on the spectrum of incident neutrons. By strategically positioning these choppers the response matrix assumes a convenient form that can be deconvoluted from the measured TOF spectrum to produce the diffraction pattern of the sample. We compare the performance of this instrument to other possible diffraction instruments that could be utilized on a long pulsed source.

Investigation of the dependence of deformation mechanisms on solute content in polycrystalline Mg–Al magnesium alloys by neutron diffraction and acoustic emission

DOE PAGES

Mathis, Kristian; Capek, J.; Clausen, Bjorn; ...

2015-04-20

Influence of aluminium content on the deformation mechanisms in Mg–Al binary alloys has been studied using in-situ neutron diffraction and acoustic emission technique. Here, it is shown that the addition of the solute increases the critical resolved shear stress for twinning. Further, the role of aluminium on the solid solution hardening of the basal plane and softening of non-basal planes are discussed using results of the convolutional multiple peak profile analysis of diffraction patterns. In conclusion, the results indicate that the density of both prismatic and pyramidal dislocations increases with increasing alloying content.

Phase Transition and Texture Evolution in the Ni-Mn-Ga Ferromagnetic Shape-Memory Alloys Studied by a Neutron Diffraction Technique

NASA Astrophysics Data System (ADS)

Nie, Z. H.; Wang, Y. D.; Wang, G. Y.; Richardson, J. W.; Wang, G.; Liu, Y. D.; Liaw, P. K.; Zuo, L.

2008-12-01

The phase transition and influence of the applied stress on the texture evolution in the as-cast Ni-Mn-Ga ferromagnetic shape-memory alloys were studied by the time-of-flight (TOF) neutron diffraction technique. The neutron diffraction experiments were performed on the General Purpose Powder Diffractometer (Argonne National Laboratory). Inverse pole figures were determined from the neutron data for characterizing the orientation distributions and variant selections of polycrystalline Ni-Mn-Ga alloys subjected to different uniaxial compression deformations. Texture analyses reveal that the initial texture for the parent phase in the as-cast specimen was composed of {left\\{ {{text{001}}} right\\}}{left< {{text{100}}} rightrangle } , {left\\{ {{text{001}}} right\\}}{left< {{text{110}}} rightrangle } , {left\\{ {{text{011}}} right\\}}{left< {{text{100}}} rightrangle } , and {left\\{ {{text{011}}} right\\}}{left< {{text{110}}} rightrangle } , which was weakened after the compression deformation. Moreover, a strong preferred selection of martensitic-twin variants ( {left\\{ {{text{110}}} right\\}}{left< {{text{001}}} rightrangle } and {left\\{ {{text{100}}} right\\}}{left< {{text{001}}} rightrangle } ) was observed in the transformed martensite after a compression stress applied on the parent phase along the cyclindrical axis of the specimens. The preferred selection of variants can be well explained by considering the grain/variant-orientation-dependent Bain-distortion energy.

Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

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

Cummins, Dustin Ray; Vogel, Sven C.; Hollis, Kendall Jon

2016-10-18

This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffractionmore » data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to the process and analysis can be made, and neutron diffraction can become a viable and efficient technique for gamma/alpha phase composition determination for nuclear fuels.« less

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

2016-06-30

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.

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

Martensitic transformation in a B2-containing CuZr-based BMG composite revealed by in situ neutron diffraction

DOE PAGES

Song, Gian; Lee, Chanho; Hong, Sung Hwan; ...

2017-06-27

Here, CuZr-based bulk-metallic-glass (BMG) composites reinforced by a B2-type CuZr crystalline-phase (CP) have been widely studied, and exhibit that the plastic deformation of the CP induces martensitic transformation from the B2 to B19', which plays a dominant role in the deformation behavior and mechanical properties. In the present study, 2.0% Co containing CuZr-based BMG composites were investigated using in-situ neutron-diffraction technique. The in-situ neutron-diffraction results reveal the continuous load transfer from the glass matrix to B2 CP and martensitic transformation from the B2 CP to B19' during the deformation of the composite. Moreover, it was found that the martensitic transformationmore » is initiated at the applied stress higher than 1500 MPa, and is significantly suppressed during the deformation, as compared to other 0.5% Co-containing CuZr-based BMG composites. Based on these in-situ neutron-diffraction results, the martensitic transformation is strongly affected by the amount of the addition of Co, which determines the mechanical properties of CP-reinforced BMG composites, such as ductility and hardening capability.« less

Martensitic transformation in a B2-containing CuZr-based BMG composite revealed by in situ neutron diffraction

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

Song, Gian; Lee, Chanho; Hong, Sung Hwan

Here, CuZr-based bulk-metallic-glass (BMG) composites reinforced by a B2-type CuZr crystalline-phase (CP) have been widely studied, and exhibit that the plastic deformation of the CP induces martensitic transformation from the B2 to B19', which plays a dominant role in the deformation behavior and mechanical properties. In the present study, 2.0% Co containing CuZr-based BMG composites were investigated using in-situ neutron-diffraction technique. The in-situ neutron-diffraction results reveal the continuous load transfer from the glass matrix to B2 CP and martensitic transformation from the B2 CP to B19' during the deformation of the composite. Moreover, it was found that the martensitic transformationmore » is initiated at the applied stress higher than 1500 MPa, and is significantly suppressed during the deformation, as compared to other 0.5% Co-containing CuZr-based BMG composites. Based on these in-situ neutron-diffraction results, the martensitic transformation is strongly affected by the amount of the addition of Co, which determines the mechanical properties of CP-reinforced BMG composites, such as ductility and hardening capability.« less

In-situ neutron diffraction and crystal plasticity finite element modeling to study the kinematic stability of retained austenite in bearing steels

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

Voothaluru, Rohit; Bedekar, Vikram; Xie, Qingge

This work integrates in-situ neutron diffraction and crystal plasticity finite element modeling to study the kinematic stability of retained austenite in high carbon bearing steels. The presence of a kinematically metastable retained austenite in bearing steels can significantly affect the macro-mechanical and micro-mechanical material response. Mechanical characterization of metastable austenite is a critical component in accurately capturing the micro-mechanical behavior under typical application loads. Traditional mechanical characterization techniques are unable to discretely quantify the micro-mechanical response of the austenite, and as a result, the computational predictions rely heavily on trial and error or qualitative descriptions of the austenite phase. Inmore » order to overcome this, in the present work, we use in-situ neutron diffraction of a uniaxial tension test of an A485 Grade 1 bearing steel specimen. The mechanical response determined from the neutron diffraction analysis was incorporated into a hybrid crystal plasticity finite element model that accounts for the martensite's crystal plasticity and the stress-assisted transformation from austenite to martensite in bearing steels. Here, the modeling response was used to estimate the single crystal elastic constants of the austenite and martensite phases. Finally, the results show that using in-situ neutron diffraction, coupled with a crystal plasticity model, can successfully predict both the micro-mechanical and macro-mechanical responses of bearing steels while accounting for the martensitic transformation of the retained austenite.« less

In-situ neutron diffraction and crystal plasticity finite element modeling to study the kinematic stability of retained austenite in bearing steels

DOE PAGES

Voothaluru, Rohit; Bedekar, Vikram; Xie, Qingge; ...

2018-11-21

This work integrates in-situ neutron diffraction and crystal plasticity finite element modeling to study the kinematic stability of retained austenite in high carbon bearing steels. The presence of a kinematically metastable retained austenite in bearing steels can significantly affect the macro-mechanical and micro-mechanical material response. Mechanical characterization of metastable austenite is a critical component in accurately capturing the micro-mechanical behavior under typical application loads. Traditional mechanical characterization techniques are unable to discretely quantify the micro-mechanical response of the austenite, and as a result, the computational predictions rely heavily on trial and error or qualitative descriptions of the austenite phase. Inmore » order to overcome this, in the present work, we use in-situ neutron diffraction of a uniaxial tension test of an A485 Grade 1 bearing steel specimen. The mechanical response determined from the neutron diffraction analysis was incorporated into a hybrid crystal plasticity finite element model that accounts for the martensite's crystal plasticity and the stress-assisted transformation from austenite to martensite in bearing steels. Here, the modeling response was used to estimate the single crystal elastic constants of the austenite and martensite phases. Finally, the results show that using in-situ neutron diffraction, coupled with a crystal plasticity model, can successfully predict both the micro-mechanical and macro-mechanical responses of bearing steels while accounting for the martensitic transformation of the retained austenite.« less

Non-destructive diagnostics of irradiated materials using neutron scattering from pulsed neutron sources

NASA Astrophysics Data System (ADS)

Korenev, Sergey; Sikolenko, Vadim

2004-09-01

The advantage of neutron-scattering studies as compared to the standard X-ray technique is the high penetration of neutrons that allow us to study volume effects. The high resolution of instrumentation on the basis neutron scattering allows measurement of the parameters of lattice structure with high precision. We suggest the use of neutron scattering from pulsed neutron sources for analysis of materials irradiated with pulsed high current electron and ion beams. The results of preliminary tests using this method for Ni foils that have been studied by neutron diffraction at the IBR-2 (Pulsed Fast Reactor at Joint Institute for Nuclear Research) are presented.

Radiative neutron capture as a counting technique at pulsed spallation neutron sources: a review of current progress

NASA Astrophysics Data System (ADS)

Schooneveld, E. M.; Pietropaolo, A.; Andreani, C.; Perelli Cippo, E.; Rhodes, N. J.; Senesi, R.; Tardocchi, M.; Gorini, G.

2016-09-01

Neutron scattering techniques are attracting an increasing interest from scientists in various research fields, ranging from physics and chemistry to biology and archaeometry. The success of these neutron scattering applications is stimulated by the development of higher performance instrumentation. The development of new techniques and concepts, including radiative capture based neutron detection, is therefore a key issue to be addressed. Radiative capture based neutron detectors utilize the emission of prompt gamma rays after neutron absorption in a suitable isotope and the detection of those gammas by a photon counter. They can be used as simple counters in the thermal region and (simultaneously) as energy selector and counters for neutrons in the eV energy region. Several years of extensive development have made eV neutron spectrometers operating in the so-called resonance detector spectrometer (RDS) configuration outperform their conventional counterparts. In fact, the VESUVIO spectrometer, a flagship instrument at ISIS serving a continuous user programme for eV inelastic neutron spectroscopy measurements, is operating in the RDS configuration since 2007. In this review, we discuss the physical mechanism underlying the RDS configuration and the development of associated instrumentation. A few successful neutron scattering experiments that utilize the radiative capture counting techniques will be presented together with the potential of this technique for thermal neutron diffraction measurements. We also outline possible improvements and future perspectives for radiative capture based neutron detectors in neutron scattering application at pulsed neutron sources.

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

Feng, Hao; Ashkar, Rana; Steinke, Nina

A method dubbed grating-based holography was recently used to determine the structure of colloidal fluids in the rectangular grooves of a diffraction grating from X-ray scattering measurements. Similar grating-based measurements have also been recently made with neutrons using a technique called spin-echo small-angle neutron scattering. The analysis of the X-ray diffraction data was done using an approximation that treats the X-ray phase change caused by the colloidal structure as a small perturbation to the overall phase pattern generated by the grating. In this paper, the adequacy of this weak phase approximation is explored for both X-ray and neutron grating holography.more » Additionally, it is found that there are several approximations hidden within the weak phase approximation that can lead to incorrect conclusions from experiments. In particular, the phase contrast for the empty grating is a critical parameter. Finally, while the approximation is found to be perfectly adequate for X-ray grating holography experiments performed to date, it cannot be applied to similar neutron experiments because the latter technique requires much deeper grating channels.« less

First spin-resolved electron distributions in crystals from combined polarized neutron and X-ray diffraction experiments.

PubMed

Deutsch, Maxime; Gillon, Béatrice; Claiser, Nicolas; Gillet, Jean-Michel; Lecomte, Claude; Souhassou, Mohamed

2014-05-01

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.

Neutron and positron techniques for fluid transfer system analysis and remote temperature and stress measurement

NASA Astrophysics Data System (ADS)

Stewart, P. A. E.

1987-05-01

Present and projected applications of penetrating radiation techniques to gas turbine research and development are considered. Approaches discussed include the visualization and measurement of metal component movement using high energy X-rays, the measurement of metal temperatures using epithermal neutrons, the measurement of metal stresses using thermal neutron diffraction, and the visualization and measurement of oil and fuel systems using either cold neutron radiography or emitting isotope tomography. By selecting the radiation appropriate to the problem, the desired data can be probed for and obtained through imaging or signal acquisition, and the necessary information can then be extracted with digital image processing or knowledge based image manipulation and pattern recognition.

Clifford G. Shull, Neutron Diffraction, Hydrogen Atoms, and Neutron

Science.gov Websites

Analysis of NaH and NaD, DOE Technical Report, April 1947 The Diffraction of Neutrons by Crystalline Powders; DOE Technical Report; 1948 Neutron Diffraction Studies, DOE Technical Report, 1948 Laue Structure of Thorium and Zirconium Dihydrides by X-ray and Neutron Diffraction, DOE Technical Report, April

Asymmetric band flipping for time-of-flight neutron diffraction data

DOE PAGES

Whitfield, Pamela S.; Coelho, Alan A.

2016-08-24

Charge flipping with powder diffraction data is known to produce a result more reliably with high-resolution data,i.e.visible reflections at smalldspacings. This data are readily accessible with the neutron time-of-flight technique but the assumption that negative scattering density is nonphysical is no longer valid where elements with negative scattering lengths are present. The concept of band flipping was introduced in the literature, where a negative threshold is used in addition to a positive threshold during the flipping. But, it was not tested with experimental data at the time. Finallly, band flipping has been implemented inTOPAStogether with the band modification of low-densitymore » elimination and tested with experimental powder and Laue single-crystal neutron data.« less

Neutron Bragg-edge-imaging for strain mapping under in situ tensile loading

NASA Astrophysics Data System (ADS)

Woracek, R.; Penumadu, D.; Kardjilov, N.; Hilger, A.; Strobl, M.; Wimpory, R. C.; Manke, I.; Banhart, J.

2011-05-01

Wavelength selective neutron radiography at a cold neutron reactor source was used to measure strain and determine (residual) stresses in a steel sample under plane stress conditions. We present a new technique that uses an energy-resolved neutron imaging system based on a double crystal monochromator and is equipped with a specially developed (in situ) biaxial load frame to perform Bragg edge based transmission imaging. The neutron imaging technique provides a viewing area of 7 cm by 7 cm with a spatial resolution on the order of ˜ 100 μm. The stress-induced shifts of the Bragg edge corresponding to the (110) lattice plane were resolved spatially for a ferritic steel alloy A36 (ASTM international) sample. Furthermore it is demonstrated that results agree with comparative data obtained using neutron diffraction and resistance based strain-gauge rosettes.

Search for memory effects in methane hydrate: structure of water before hydrate formation and after hydrate decomposition.

PubMed

Buchanan, Piers; Soper, Alan K; Thompson, Helen; Westacott, Robin E; Creek, Jefferson L; Hobson, Greg; Koh, Carolyn A

2005-10-22

Neutron diffraction with HD isotope substitution has been used to study the formation and decomposition of the methane clathrate hydrate. Using this atomistic technique coupled with simultaneous gas consumption measurements, we have successfully tracked the formation of the sI methane hydrate from a water/gas mixture and then the subsequent decomposition of the hydrate from initiation to completion. These studies demonstrate that the application of neutron diffraction with simultaneous gas consumption measurements provides a powerful method for studying the clathrate hydrate crystal growth and decomposition. We have also used neutron diffraction to examine the water structure before the hydrate growth and after the hydrate decomposition. From the neutron-scattering curves and the empirical potential structure refinement analysis of the data, we find that there is no significant difference between the structure of water before the hydrate formation and the structure of water after the hydrate decomposition. Nor is there any significant change to the methane hydration shell. These results are discussed in the context of widely held views on the existence of memory effects after the hydrate decomposition.

In-Situ Neutron Diffraction Studies of Micromechanical Behavior in a Friction Stir Welded AA7475-T761

NASA Astrophysics Data System (ADS)

Liu, X. P.; Lin Peng, R.; Hofmann, M.; Johansson, S.; Wang, Y. D.

2011-01-01

An in-situ neutron diffraction technique was used to investigate the lattice strain distributions and micromechanical behavior in a friction stir welded (FSW) sheet of AA7475-T761. The neutron diffraction experiments were performed on the spectrometer for material research, STRESS-SPEC, at FRM II (Garching, Germany). The lattice strain profiles around the weld center were measured as a function of the applied strain during the tensile loading and unloading. The anisotropic elastic and plastic properties of the FSW aluminum alloy were simulated by elasto-plastic self-consistent (EPSC) model to predict the anisotropic deformation behaviors involving the grain-to-grain interactions. Material parameters used for describing the constitutive laws of each test position were determined from the measured lattice strain distributions for different diffraction hkl planes as well as the macroscopic stress-strain curve of the FSW aluminum alloy. A good agreement between experimental results and numerical simulations was obtained. The present investigations provided a reliable prediction of the anisotropic micromechanical behavior of the FSW aluminum alloy during tensile deformation.

X-ray absorption spectroscopy and neutron diffraction study of the perovskite-type rare-earth cobaltites

NASA Astrophysics Data System (ADS)

Sikolenko, V.; Efimova, E.; Franz, A.; Ritter, C.; Troyanchuk, I. O.; Karpinsky, D.; Zubavichus, Y.; Veligzhanin, A.; Tiutiunnikov, S. I.; Sazonov, A.; Efimov, V.

2018-05-01

Correlations between local and long-range structure distortions in the perovskite-type RE1-xSrxCoO3-δ (RE = La, Pr, Nd; x = 0.0 and 0.5) compounds have been studied at room temperature by extended X-ray absorption fine structure (EXAFS) at the Co K-edge and high-resolution neutron powder diffraction (NPD). The use of two complementary experimental techniques allowed us to explore the influence of the type of rare-earth element and strontium substitution on unusual behavior of static and dynamic features of both the Co-O bond lengths.

A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

NASA Astrophysics Data System (ADS)

Weber, J. K. R.; Benmore, C. J.; Tailor, A. N.; Tumber, S. K.; Neuefeind, J.; Cherry, B.; Yarger, J. L.; Mou, Q.; Weber, W.; Byrn, S. R.

2013-10-01

Acoustic levitation was used to trap 1-3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 °C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses.

Structure of Nano-sized CeO 2 Materials: Combined Scattering and Spectroscopic Investigations

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

Marchbank, Huw R.; Clark, Adam H.; Hyde, Timothy I.

Here, the nature of nano-sized ceria, CeO 2, systems were investigated using neutron and X-ray diffraction and X-ray absorption spectroscopy. Whilst both diffraction andtotal pair distribution functions (PDFs) revealed that in all the samples the occupancy of both Ce 4+ and O 2- are very close to the ideal stoichiometry, the analysis using reverse Monte Carlo technique revealedsignificant disorder around oxygen atoms in the nano sized ceria samples in comparison to the highly crystalline NIST standard.In addition, the analysis reveal that the main differences observed in the pair correlations from various X-ray and neutron diffraction techniques were attributed to themore » particle size of the CeO 2 prepared by the reported three methods. Furthermore, detailed analysis of the Ce L 3– and K-edge EXAFS data support this finding; in particular the decrease in higher shell coordination numbers with respect to the NIST standard, are attributed to differences in particle size.« less

Structure of Nano-sized CeO 2 Materials: Combined Scattering and Spectroscopic Investigations

DOE PAGES

Marchbank, Huw R.; Clark, Adam H.; Hyde, Timothy I.; ...

2016-08-29

Here, the nature of nano-sized ceria, CeO 2, systems were investigated using neutron and X-ray diffraction and X-ray absorption spectroscopy. Whilst both diffraction andtotal pair distribution functions (PDFs) revealed that in all the samples the occupancy of both Ce 4+ and O 2- are very close to the ideal stoichiometry, the analysis using reverse Monte Carlo technique revealedsignificant disorder around oxygen atoms in the nano sized ceria samples in comparison to the highly crystalline NIST standard.In addition, the analysis reveal that the main differences observed in the pair correlations from various X-ray and neutron diffraction techniques were attributed to themore » particle size of the CeO 2 prepared by the reported three methods. Furthermore, detailed analysis of the Ce L 3– and K-edge EXAFS data support this finding; in particular the decrease in higher shell coordination numbers with respect to the NIST standard, are attributed to differences in particle size.« less

Analysis of strain-induced crystallinity in neutron-irradiated amorphous PET fiber

NASA Astrophysics Data System (ADS)

Mallick, B.

2015-05-01

Polyethylene terephthalate (PET) fiber of 2.2 denier per filament has been irradiated with 4.44-MeV fast neutron beam at different low doses: 0.58-2,513.5 mGy. The variation of crystallinity because of neutron irradiation straining in PET filaments has been investigated. Study of the effects of irradiation by using X-ray diffraction and differential scanning calorimetry technique confirms the radiation-induced microstrain-dependent crystallinity of PET fiber.

Instrument and method for focusing X-rays, gamma rays and neutrons

DOEpatents

Smither, Robert K.

1984-01-01

A crystal diffraction instrument or diffraction grating instrument with an improved crystalline structure or grating spacing structure having a face for receiving a beam of photons or neutrons and diffraction planar spacing or grating spacing along that face with the spacing increasing progressively along the face to provide a decreasing Bragg diffraction angle for a monochromatic radiation and thereby increasing the usable area and acceptance angle. The increased planar spacing for the diffraction crystal is provided by the use of a temperature differential across the crystalline structure, by assembling a plurality of crystalline structures with different compositions, by an individual crystalline structure with a varying composition and thereby a changing planar spacing along its face, and by combinations of these techniques. The increased diffraction grating element spacing is generated during the fabrication of the diffraction grating by controlling the cutting tool that is cutting the grooves or controlling the laser beam, electron beam or ion beam that is exposing the resist layer, etc. It is also possible to vary this variation in grating spacing by applying a thermal gradient to the diffraction grating in much the same manner as is done in the crystal diffraction case.

Instrument and method for focusing x rays, gamma rays, and neutrons

DOEpatents

Smither, R.K.

1982-03-25

A crystal-diffraction instrument or diffraction-grating instrument is described with an improved crystalline structure or grating spacing structure having a face for receiving a beam of photons or neutrons and diffraction planar spacing or grating spacing along that face with the spacing increasing progressively along the face to provide a decreasing Bragg diffraction angle for a monochromatic radiation and thereby increasing the usable area and acceptance angle. The increased planar spacing for the diffraction crystal is provided by the use of a temperature differential across the line structures with different compositions, by an individual crystalline structure with a varying composition and thereby a changing planar spacing along its face, and by combinations of these techniques. The increased diffraction grating element spacing is generated during the fabrication of the diffraction grating by controlling the cutting tool that is cutting the grooves or controlling the laser beam, electron beam, or ion beam that is exposing the resist layer, etc. It is also possible to vary this variation in grating spacing by applying a thermal gradient to the diffraction grating in much the same manner as is done in the crystal-diffraction case.

Aging behavior of lithium iron phosphate based 18650-type cells studied by in situ neutron diffraction

NASA Astrophysics Data System (ADS)

Paul, Neelima; Wandt, Johannes; Seidlmayer, Stefan; Schebesta, Sebastian; Mühlbauer, Martin J.; Dolotko, Oleksandr; Gasteiger, Hubert A.; Gilles, Ralph

2017-03-01

The aging behavior of commercially produced 18650-type Li-ion cells consisting of a lithium iron phosphate (LFP) based cathode and a graphite anode based on either mesocarbon microbeads (MCMB) or needle coke (NC) is studied by in situ neutron diffraction and standard electrochemical techniques. While the MCMB cells showed an excellent cycle life with only 8% relative capacity loss (i.e., referenced to the capacity after formation) after 4750 cycles and showed no capacity loss on storage for two years, the needle coke cells suffered a 23% relative capacity loss after cycling and a 11% loss after storage. Based on a combination of neutron diffraction and electrochemical characterization, it is shown that the entire capacity loss for both cell types is dominated by the loss of active lithium; no other aging mechanisms like structural degradation of anode or cathode active materials or deactivation of active material could be found, highlighting the high structural stability of the active material and the excellent quality of the investigated cells.

Diffraction des neutrons : principe, dispositifs expérimentaux et applications

NASA Astrophysics Data System (ADS)

Muller, C.

2003-02-01

La diffraction de neutrons, sur monocristal ou sur échantillon polycristallin (ou poudre), est une technique très largement utilisée, en science des matériaux comme en biologie, lorsque l'on souhaite déterminer la structure cristalline d'un composé ou d'une molécule. Toutefois, le degré de précision de la détermination structurale est très corrélé au choix de l'instrument utilisé. Il s'en suit que la question “comment choisir l'instrument le mieux adapté au composé et à la problématique ?" apparaît comme fondamentale. L'objectif de ce cours est de tenter de répondre à cette question en décrivant brièvement les caractéristiques instrumentales de différents diffractomètres, en exposant les avantages spécifiques des expériences de diffraction de neutrons et en donnant quelques exemples d'application.

A neutron diffraction and imaging study of ancient iron tie rods

NASA Astrophysics Data System (ADS)

Di Martino, D.; Bellanova, M.; Perelli Cippo, E.; Felicetti, R.; Scherillo, A.; Kelleher, J.; Kis, Z.; Gorini, G.

2018-05-01

Milan Cathedral is one of the biggest and widest churches ever built among the other coeval architectures. It had a very long and complex construction history, which started in 1386 and lasted more than four centuries. The dominant style is the European gothic but the lombard tradition has strongly influenced the composition. Gothic cathedrals were diffusely built in Europe during the Middle Age, and each region developed its own local interpretation. However, a common feature of the style was the presence of slender pillars and of many elements able to reduce the horizontal thrusts of the vaults, such as spires, buttresesses, flying buttresesses and tie rods. In Milan Cathedral, tie rods have a fundamental role due to the specific characteristics of the structural system and its complex history. In 2012, a broken tie rod was found and it was substituted with a new one. Therefore, a multidisciplinary research on these elements started, aiming at a deeper material characterization and an in-situ identification of local defects. Among non-destructive techniques, several neutron analyses were performed on different samples. We will report on neutron diffraction measurements and neutron resonant capture analysis on part of the original broken tie rod. Moreover, neutron imaging was recorded on other iron tie rods (from an external spire). Results will be useful for an independent assessment and validation of models and of new on-site monitoring techniques, since no other conventional non-destructive technique will allow the same characterization.

Monochromatic neutron beam production at Brazilian nuclear research reactors

NASA Astrophysics Data System (ADS)

Stasiulevicius, Roberto; Rodrigues, Claudio; Parente, Carlos B. R.; Voi, Dante L.; Rogers, John D.

2000-12-01

Monochomatic beams of neutrons are obtained form a nuclear reactor polychromatic beam by the diffraction process, suing a single crystal energy selector. In Brazil, two nuclear research reactors, the swimming pool model IEA-R1 and the Argonaut type IEN-R1 have been used to carry out measurements with this technique. Neutron spectra have been measured using crystal spectrometers installed on the main beam lines of each reactor. The performance of conventional- artificial and natural selected crystals has been verified by the multipurpose neutron diffractometers installed at IEA-R1 and simple crystal spectrometer in operator at IEN- R1. A practical figure of merit formula was introduced to evaluate the performance and relative reflectivity of the selected planes of a single crystal. The total of 16 natural crystals were selected for use in the neutron monochromator, including a total of 24 families of planes. Twelve of these natural crystal types and respective best family of planes were measured directly with the multipurpose neutron diffractometers. The neutron spectrometer installed at IEN- R1 was used to confirm test results of the better specimens. The usually conventional-artificial crystal spacing distance range is limited to 3.4 angstrom. The interplane distance range has now been increased to approximately 10 angstrom by use of naturally occurring crystals. The neutron diffraction technique with conventional and natural crystals for energy selection and filtering can be utilized to obtain monochromatic sub and thermal neutrons with energies in the range of 0.001 to 10 eV. The thermal neutron is considered a good tool or probe for general applications in various fields, such as condensed matter, chemistry, biology, industrial applications and others.

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

Neutron diffraction as a tool to monitor the establishment of the electro-osmotic flux during realkalisation of carbonated concrete

NASA Astrophysics Data System (ADS)

Castellote, Marta; Llorente, I.; Andrade, Carmen; Turrillas, X.; Alonso, Cruz; Campo, Javier

2006-11-01

Realkalisation is an electrochemical technique for repairing concrete structures damaged by rebar corrosion due to carbonation. The treatment aims at restoring alkalinity of the concrete by application of a continuous current between the rebar, acting as a cathode, and an external auxiliary electrode placed in a carbonate solution and connected to a positive pole of a power supply. Here we report the application of neutron diffraction in the in situ monitoring of a realkalisation treatment, analysing at the same time the development of the electro-osmotic flux and the microstructural variations in the surroundings of the rebar.

Instrument and method for focusing x rays, gamma rays, and neutrons

DOEpatents

Smither, R.K.

1981-04-20

A crystal diffraction instrument is described which has an improved crystalline structure having a face for receiving a beam of photons or neutrons and diffraction planar spacing along that face with the spacing increasing progressively along the face to provide a decreasing Bragg angle and thereby increasing the usable area and acceptance angle. The increased planar spacing is provided by the use of a temperature differential across the crystalline structure, by assembling a plurality of crystalline structure with different compositions, by an individual crystalline structure with a varying composition and thereby a changing planar spacing along its face, and by combinations of these techniques.

Spin-liquid ground state in the frustrated J 1 - J 2 zigzag chain system BaTb 2 O 4

DOE PAGES

Aczel, A. A.; Li, L.; Garlea, V. O.; ...

2015-07-13

We have investigated polycrystalline samples of the zigzag chain system BaTb 2O 4 with magnetic susceptibility, heat capacity, neutron powder diffraction, and muon spin relaxation measurements. No magnetic transitions are observed in the bulk measurements, while neutron diffraction reveals low-temperature, short-range, intrachain magnetic correlations between Tb 3+ ions. Muon spin relaxation measurements indicate that these correlations are dynamic, as the technique detects no signatures of static magnetism down to 0.095 K. Altogether these findings provide strong evidence for a spin liquid ground state in BaTb 2O 4.

The HB-2D Polarized Neutron Development Beamline at the High Flux Isotope Reactor

NASA Astrophysics Data System (ADS)

Crow, Lowell; Hamilton, WA; Zhao, JK; Robertson, JL

2016-09-01

The Polarized Neutron Development beamline, recently commissioned at the HB-2D position on the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory, provides a tool for development and testing of polarizers, polarized neutron devices, and prototyping of polarized neutron techniques. With available monochromators including pyrolytic graphite and polarizing enriched Fe-57 (Si), the instrument has operated at 4.25 and 2.6 Å wavelengths, using crystal, supermirror, or He-3 polarizers and analyzers in various configurations. The Neutron Optics and Development Team has used the beamline for testing of He-3 polarizers for use at other HFIR and Spallation Neutron Source (SNS) instruments, as well as a variety of flipper devices. Recently, we have acquired new supermirror polarizers which have improved the instrument performance. The team and collaborators also have continuing demonstration experiments of spin-echo focusing techniques, and plans to conduct polarized diffraction measurements. The beamline is also used to support a growing use of polarization techniques at present and future instruments at SNS and HFIR.

Inelastic neutron scattering

NASA Astrophysics Data System (ADS)

Petit, Sylvain

2017-10-01

The goal of the JDN22 school was to propose a progressive teaching eager to improve the expertise of students in neutron diffraction. Neutron-based techniques have indeed proved for decades to be essential tools in the investigation of condensed matter. This lecture is however concerned with inelastic neutron scattering and is thus somehow apart. In the context of this school, it should then only be considered as a brief introduction. We give simple examples along with the basics of the spectrometers, and finally useful formula for the inelastic cross sections in different situations. We strongly encourage interested readers to refer to the bibliography for more detailed information.

Monte Carlo analysis of neutron diffuse scattering data

NASA Astrophysics Data System (ADS)

Goossens, D. J.; Heerdegen, A. P.; Welberry, T. R.; Gutmann, M. J.

2006-11-01

This paper presents a discussion of a technique developed for the analysis of neutron diffuse scattering data. The technique involves processing the data into reciprocal space sections and modelling the diffuse scattering in these sections. A Monte Carlo modelling approach is used in which the crystal energy is a function of interatomic distances between molecules and torsional rotations within molecules. The parameters of the model are the spring constants governing the interactions, as they determine the correlations which evolve when the model crystal structure is relaxed at finite temperature. When the model crystal has reached equilibrium its diffraction pattern is calculated and a χ2 goodness-of-fit test between observed and calculated data slices is performed. This allows a least-squares refinement of the fit parameters and so automated refinement can proceed. The first application of this methodology to neutron, rather than X-ray, data is outlined. The sample studied was deuterated benzil, d-benzil, C14D10O2, for which data was collected using time-of-flight Laue diffraction on SXD at ISIS.

In situ neutron scattering study of nanoscale phase evolution in PbTe-PbS thermoelectric material

DOE PAGES

Ren, Fei; Schmidt, Robert; Keum, Jong K.; ...

2016-08-24

Introducing nanostructural second phases has been proved to be an effective approach to reduce the lattice thermal conductivity and thus enhance the figure of merit for many thermoelectric materials. Furthermore studies of the formation and evolution of these second phases are central to understanding temperature dependent material behavior, improving thermal stabilities, as well as designing new materials. We examined powder samples of PbTe-PbS thermoelectric material using in situ neutron diffraction and small angle neutron scattering (SANS) techniques from room temperature to elevated temperature up to 663 K, to explore quantitative information on the structure, weight fraction, and size of themore » second phase. Neutron diffraction data showed the as-milled powder was primarily solid solution before heat treatment. During heating, PbS second phase precipitated out of the PbTe matrix around 480 K, while re-dissolution started around 570 K. The second phase remained separated from the matrix upon cooling. Furthermore, SANS data indicated there are two populations of nanostructures. The size of the smaller nanostructure increased from initially 5 nm to approximately 25 nm after annealing at 650 K, while the size of the larger nanostructure remained unchanged. Our study demonstrated that in situ neutron techniques are effective means to obtain quantitative information to study temperature dependent nanostructural behavior of thermoelectrics and likely other high-temperature materials.« less

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

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

Mason, T. E., E-mail: masont@ornl.gov; Gawne, T. J.; Nagler, S. E.

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 quitemore » 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.« less

Wavelength resolved neutron transmission analysis to identify single crystal particles in historical metallurgy

NASA Astrophysics Data System (ADS)

Barzagli, E.; Grazzi, F.; Salvemini, F.; Scherillo, A.; Sato, H.; Shinohara, T.; Kamiyama, T.; Kiyanagi, Y.; Tremsin, A.; Zoppi, Marco

2014-07-01

The phase composition and the microstructure of four ferrous Japanese arrows of the Edo period (17th-19th century) has been determined through two complementary neutron techniques: Position-sensitive wavelength-resolved neutron transmission analysis (PS-WRNTA) and time-of-flight neutron diffraction (ToF-ND). Standard ToF-ND technique has been applied by using the INES diffractometer at the ISIS pulsed neutron source in the UK, while the innovative PS-WRNTA one has been performed at the J-PARC neutron source on the BL-10 NOBORU beam line using the high spatial high time resolution neutron imaging detector. With ToF-ND we were able to reach information about the quantitative distribution of the metal and non-metal phases, the texture level, the strain level and the domain size of each of the samples, which are important parameters to gain knowledge about the technological level of the Japanese weapon. Starting from this base of data, the more complex PS-WRNTA has been applied to the same samples. This experimental technique exploits the presence of the so-called Bragg edges, in the time-of-flight spectrum of neutrons transmitted through crystalline materials, to map the microstructural properties of samples. The two techniques are non-invasive and can be easily applied to archaeometry for an accurate microstructure mapping of metal and ceramic artifacts.

Neutron diffraction and ferromagnetic resonance studies on plasma-sprayed MnZn ferrite films

NASA Astrophysics Data System (ADS)

Yan, Q. Y.; Gambino, R. J.; Sampath, S.; Huang, Q.

2005-02-01

The magnetic properties of MnZn ferrites are affected by the plasma spray process. It is found that improvements can be made by annealing the ferrite films at 500°C-800°C. The annealing induced magnetic property changes are studied by neutron diffraction and ferromagnetic resonance techniques. The increase of the saturation magnetization is attributed to the cation ordering within the spinel lattice, which increases the magnetic moment per ferrite formula. The refinements on the neutron diffraction data suggest that the redistribution of the cation during annealing neither starts from a fully disordered state nor ends to a fully ordered state. The decrease of the coercivity is analyzed with the domain wall pinning model. The measurements on the magnetostriction and residual stress indicate that coercive mechanisms arising from the magnetoelastic energy term are not dominant in these ferrite films. The decrease of the coercivity for annealed ferrite films is mainly attributed to the decrease of the effective anisotropic field, which may result from the homogenization of the film composition and the reduction of the microstructural discontinuity (e.g., cracks, voids, and splat boundaries).

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

Song, Gian; Lee, Chanho; Hong, Sung Hwan

Here, CuZr-based bulk-metallic-glass (BMG) composites reinforced by a B2-type CuZr crystalline-phase (CP) have been widely studied, and exhibit that the plastic deformation of the CP induces martensitic transformation from the B2 to B19', which plays a dominant role in the deformation behavior and mechanical properties. In the present study, 2.0% Co containing CuZr-based BMG composites were investigated using in-situ neutron-diffraction technique. The in-situ neutron-diffraction results reveal the continuous load transfer from the glass matrix to B2 CP and martensitic transformation from the B2 CP to B19' during the deformation of the composite. Moreover, it was found that the martensitic transformationmore » is initiated at the applied stress higher than 1500 MPa, and is significantly suppressed during the deformation, as compared to other 0.5% Co-containing CuZr-based BMG composites. Based on these in-situ neutron-diffraction results, the martensitic transformation is strongly affected by the amount of the addition of Co, which determines the mechanical properties of CP-reinforced BMG composites, such as ductility and hardening capability.« less

Neutron and X-Ray Diffraction Studies of Advanced Materials

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

Barabash, Rozaliya; Tiley, Jaimie; Wang, Yandong

2010-01-01

The selection of articles in the special topic 'Neutron and X-Ray Studies of Advanced Materials' is based on the materials presented during the TMS 2009 annual meeting in San Francisco, CA, February 15-19, 2009. The development of ultrabrilliant third-generation synchrotron X-ray sources, together with advances in X-ray optics, has created intense X-ray microbeams, which provide the best opportunities for in-depth understanding of mechanical behavior in a broad spectrum of materials. Important applications include ultrasensitive elemental detection by X-ray fluorescence/absorption and microdiffraction to identify phase and strain with submicrometer spatial resolution. X-ray microdiffraction is a particularly exciting application compared with alternativemore » probes of crystalline structure, orientation, and strain. X-ray microdiffraction is nondestructive with good strain resolution, competitive or superior spatial resolution in thick samples, and with the ability to probe below the sample surface. Moreover, the high-energy X-ray diffraction technique provides an effective tool for characterizing the mechanical and functional behavior in various environments (temperature, stress, and magnetic field). At the same time, some neutron diffraction instruments constructed mainly for the purpose of engineering applications can be found at nearly all neutron facilities. The first generation-dedicated instruments designed for studying in-situ mechanical behavior have been commissioned and used, and industrial standards for reliable and repeatable measurements have been developed. Furthermore, higher penetration of neutron beams into most engineering materials provides direct measurements on the distribution of various stresses (i.e., types I, II, and III) beneath the surface up to several millimeters, even tens of millimeters for important industrial components. With X-ray and neutron measurements, it is possible to characterize material behavior at different length scales. It is predicted that the application of these techniques, in combination with theoretical simulations and numerical modeling, will lead to major breakthroughs in materials science in the foreseeable future, which will contribute to the development of materials technology and industrial innovation. Specifically, the use of these techniques provides bulk material properties that further augment new characterization tools including the increased use of atom probe tomography and high-resolution transmission electron microscopy systems. The combination of these techniques greatly assists the material property models that address multi-length-scale mechanisms. Different applications of diffuse scattering for understanding the fundamental materials properties are illustrated in the articles of Welberry et al., Goossens and Welberry, Campbell, Abe et al., Gilles et al., and Zhang et al. Analysis of thin films and two-dimensional structures is described in the articles of Gramlich et al., Brock et al., Vigliante et al., Kuzel et al., and Davydok et al. Recent advances in the line profile analysis are represented by the the articles of Scardi et al., Ungar et al., and Woo et al. Characterization of modern alloys is presented by the articles of Wollmershauser et al., Eidenberger et al., Garlea et al., Jia et al., Soulami et al., Wilson et al., and Wang et al. The collected articles are written by different scientific X-ray and neutron research groups. They represent a general trend in the development and application of diffraction techniques all over the world.« less

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.

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 subsequent shape recovery experiments. Neutron diffraction techniques are also being applied to the investigation of novel high temperature SMAs with the objective of designing alloys with better stability, higher transition temperatures and ultimately superior durability.

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

Unambiguous determination of H-atom positions: comparing results from neutron and high-resolution X-ray crystallography.

PubMed

Gardberg, Anna S; Del Castillo, Alexis Rae; Weiss, Kevin L; Meilleur, Flora; Blakeley, Matthew P; Myles, Dean A A

2010-05-01

The locations of H atoms in biological structures can be difficult to determine using X-ray diffraction methods. Neutron diffraction offers a relatively greater scattering magnitude from H and D atoms. Here, 1.65 A resolution neutron diffraction studies of fully perdeuterated and selectively CH(3)-protonated perdeuterated crystals of Pyrococcus furiosus rubredoxin (D-rubredoxin and HD-rubredoxin, respectively) at room temperature (RT) are described, as well as 1.1 A resolution X-ray diffraction studies of the same protein at both RT and 100 K. The two techniques are quantitatively compared in terms of their power to directly provide atomic positions for D atoms and analyze the role played by atomic thermal motion by computing the sigma level at the D-atom coordinate in simulated-annealing composite D-OMIT maps. It is shown that 1.65 A resolution RT neutron data for perdeuterated rubredoxin are approximately 8 times more likely overall to provide high-confidence positions for D atoms than 1.1 A resolution X-ray data at 100 K or RT. At or above the 1.0sigma level, the joint X-ray/neutron (XN) structures define 342/378 (90%) and 291/365 (80%) of the D-atom positions for D-rubredoxin and HD-rubredoxin, respectively. The X-ray-only 1.1 A resolution 100 K structures determine only 19/388 (5%) and 8/388 (2%) of the D-atom positions above the 1.0sigma level for D-rubredoxin and HD-rubredoxin, respectively. Furthermore, the improved model obtained from joint XN refinement yielded improved electron-density maps, permitting the location of more D atoms than electron-density maps from models refined against X-ray data only.

In situ neutron scattering study of nanoscale phase evolution in PbTe-PbS thermoelectric material

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

Ren, Fei, E-mail: renfei@temple.edu, E-mail: kean@ornl.gov; Qian, Bosen; Schmidt, Robert

2016-08-22

Introducing nanostructural second phases has proved to be an effective approach to reduce the lattice thermal conductivity and thus enhances the figure of merit for many thermoelectric materials. Studies of the formation and evolution of these second phases are essential to understanding material temperature dependent behaviors, improving thermal stabilities, as well as designing new materials. In this study, powder samples of the PbTe-PbS thermoelectric material were examined using in situ neutron diffraction and small angle neutron scattering (SANS) techniques between room temperature and elevated temperature up to 663 K, to explore quantitative information on the structure, weight fraction, and size ofmore » the second phase. Neutron diffraction data showed that the as-milled powder was primarily a solid solution prior to heat treatment. During heating, a PbS second phase precipitated out of the PbTe matrix around 500 K, while re-dissolution started around 600 K. The second phase remained separated from the matrix upon cooling. Furthermore, SANS data indicated that there are two populations of nanostructures. The size of the smaller nanostructure increased from initially 5 nm to approximately 25 nm after annealing at 650 K, while the size of the larger one remained unchanged. This study demonstrated that in situ neutron techniques are effective means to obtain quantitative information on temperature-dependent nanostructural behavior of thermoelectrics and likely other high-temperature materials.« less

Thermal neutron radiative capture on cadmium as a counting technique at the INES beam line at ISIS: A preliminary investigation of detector cross-talk.

PubMed

Festa, G; Grazzi, F; Pietropaolo, A; Scherillo, A; Schooneveld, E M

2017-12-01

Experimental tests are presented that assess the cross-talk level among three scintillation detectors used as neutron counters exploiting the thermal neutron radiative capture on Cd. The measurements were done at the INES diffractometer operating at the ISIS spallation neutron source (Rutherford Appleton Laboratory, UK). These tests follow a preliminary set of measurements performed on the same instrument to study the effectiveness of this thermal neutron counting strategy in neutron diffraction measurements, typically performed on INES using squashed 3 He filled gas tubes. The experimental data were collected in two different geometrical configurations of the detectors and compared to results of Monte Carlo simulations, performed using the MCNP code. Copyright © 2017 Elsevier Ltd. All rights reserved.

Neutron absorption of Al-Si-Mg-B{sub 4}C composite

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

Abdullah, Yusof, E-mail: yusofabd@nuclearmalaysia.gov.my; Yusof, Mohd Reusmaazran; Ibrahim, Anis Syukriah

2016-01-22

Al-Si-Mg-B{sub 4}C composites containing 2-8 wt% of B{sub 4}C were prepared by stir casting technique. Homogenization treatment was carried out at temperatures of 540°C for 4 houra and followed by ageing at 180°C for 2 houra. Microstructure and phase identification were studied by scanning electron microscopy (SEM) and X-ray diffraction (XRD) respectively. Neutron absorption study was investigated using neutron source Am/Be{sup 241}. The result indicated that higher B{sub 4}C content improved the neutron absorption property. Meanwhile homogeneity of the composite was increased by ageing processes. This composite is potential to be used as neutron shielding material especially for nuclear reactormore » application.« less

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.

The magnetic order of GdMn₂Ge₂ studied by neutron diffraction and x-ray resonant magnetic scattering.

PubMed

Granovsky, S A; Kreyssig, A; Doerr, M; Ritter, C; Dudzik, E; Feyerherm, R; Canfield, P C; Loewenhaupt, M

2010-06-09

The magnetic structure of GdMn₂Ge₂ (tetragonal I4/mmm) has been studied by hot neutron powder diffraction and x-ray resonant magnetic scattering techniques. These measurements, along with the results of bulk experiments, confirm the collinear ferrimagnetic structure with moment direction parallel to the c-axis below T(C) = 96 K and the collinear antiferromagnetic phase in the temperature region T(C) < T < T(N) = 365 K. In the antiferromagnetic phase, x-ray resonant magnetic scattering has been detected at Mn K and Gd L₂ absorption edges. The Gd contribution is a result of an induced Gd 5d electron polarization caused by the antiferromagnetic order of Mn-moments.

Radiation damage induced in Al2O3 single crystal sequentially irradiated with reactor neutrons and 90 MeV Xe ions

NASA Astrophysics Data System (ADS)

Zirour, H.; Izerrouken, M.; Sari, A.

2016-06-01

The present investigation reports the effect of 90 MeV Xe ion irradiation on neutron irradiated Al2O3 single crystals. Three irradiation experiments were performed, with neutrons only, 90 MeV Xe ions only and with neutrons followed by 90 MeV Xe ions. Neutron and 90 MeV Xe ion irradiations were performed at NUR research reactor, Algiers, Algeria and at GANIL accelerator, Caen, France respectively. After irradiation, the radiation damage was investigated by Raman spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR), optical absorption measurements, and X-ray diffraction (XRD) techniques. Raman technique revealed that the concentration of the defects formed in Al2O3 samples subsequently irradiated with neutrons and 90 MeV Xe ions is lower than that formed in Al2O3 samples which were irradiated only with neutrons. This reveals the occurrence of ionization-induced recovery of the neutron damage. Furthermore, as revealed by XRD analysis, a new peak is appeared at about 2θ = 38.03° after irradiation at high fluence (>3 × 1013 Xe/cm2). It can be assigned to the formation of new lattice plane.

Hirshfeld atom refinement for modelling strong hydrogen bonds.

PubMed

Woińska, Magdalena; Jayatilaka, Dylan; Spackman, Mark A; Edwards, Alison J; Dominiak, Paulina M; Woźniak, Krzysztof; Nishibori, Eiji; Sugimoto, Kunihisa; Grabowsky, Simon

2014-09-01

High-resolution low-temperature synchrotron X-ray diffraction data of the salt L-phenylalaninium hydrogen maleate are used to test the new automated iterative Hirshfeld atom refinement (HAR) procedure for the modelling of strong hydrogen bonds. The HAR models used present the first examples of Z' > 1 treatments in the framework of wavefunction-based refinement methods. L-Phenylalaninium hydrogen maleate exhibits several hydrogen bonds in its crystal structure, of which the shortest and the most challenging to model is the O-H...O intramolecular hydrogen bond present in the hydrogen maleate anion (O...O distance is about 2.41 Å). In particular, the reconstruction of the electron density in the hydrogen maleate moiety and the determination of hydrogen-atom properties [positions, bond distances and anisotropic displacement parameters (ADPs)] are the focus of the study. For comparison to the HAR results, different spherical (independent atom model, IAM) and aspherical (free multipole model, MM; transferable aspherical atom model, TAAM) X-ray refinement techniques as well as results from a low-temperature neutron-diffraction experiment are employed. Hydrogen-atom ADPs are furthermore compared to those derived from a TLS/rigid-body (SHADE) treatment of the X-ray structures. The reference neutron-diffraction experiment reveals a truly symmetric hydrogen bond in the hydrogen maleate anion. Only with HAR is it possible to freely refine hydrogen-atom positions and ADPs from the X-ray data, which leads to the best electron-density model and the closest agreement with the structural parameters derived from the neutron-diffraction experiment, e.g. the symmetric hydrogen position can be reproduced. The multipole-based refinement techniques (MM and TAAM) yield slightly asymmetric positions, whereas the IAM yields a significantly asymmetric position.

Nondestructive evaluation of loading and fatigue effects in Haynes(R) 230(R) alloy

NASA Astrophysics Data System (ADS)

Saleh, Tarik Adel

Nondestructive evaluation is a useful method for studying the effects of deformation and fatigue. In this dissertation I employed neutron and X-ray diffraction, nonlinear resonant ultrasound spectroscopy (NRUS), and infrared thermography to study the effects of deformation and fatigue on two different nickel based superalloys. The alloys studied were HAYNES 230, a solid solution strengthened alloy with 4% M6C carbides, and secondarily HASTELLOY C-2000 a similar single phase alloy. Using neutron and X-ray diffraction, the deformation behavior of HAYNES 230 was revealed to be composite-like during compression, but unusual in tension, where the carbides provide strengthening until just after the macroscopic yield strength and then they begin to debond and crack, creating a tension-compression asymmetry that is revealed clearly by in situ diffraction. In fatigue of HAYNES 230, the hkl elastic strains changed very little in tension-tension fatigue. However, in situ tension-compression studies showed large changes over the initial stages of fatigue. The HAYNES 230 samples studies had two distinct starting textures, measured by neutron diffraction. Some samples were texture free initially and deformed in tension and compression to fiber textures. Other samples started with a bimodal texture due to cross-rolling and incomplete annealing. The final texture of these bimodal samples is shown through modeling to be a superposition of the initial texture and typical FCC deformation mechanisms. The texture-free samples deformed significantly more macroscopically and in internal elastic strains than the samples with the cross-rolled texture. In contrast to the relative insensitivity of neutron diffraction to the effects of tension-tension fatigue, NRUS revealed large differences between as-received and progressively fatigued samples. This showed that microcracking and void formation are the primary mechanisms responsible for fatigue damage in tension-tension fatigue. NRUS is shown to be a useful complimentary technique to neutron diffraction to evaluate fatigue damage. Finally, infrared thermography is used to show temperature changes over the course of fatigue in HASTELLOY C-2000. Four stages of temperature are shown over the course of a single fatigue test. Both empirical and theoretical relationships between steady state temperature and fatigue life are developed and presented.

New neutron imaging techniques to close the gap to scattering applications

NASA Astrophysics Data System (ADS)

Lehmann, Eberhard H.; Peetermans, S.; Trtik, P.; Betz, B.; Grünzweig, C.

2017-01-01

Neutron scattering and neutron imaging are activities at the strong neutron sources which have been developed rather independently. However, there are similarities and overlaps in the research topics to which both methods can contribute and thus useful synergies can be found. In particular, the spatial resolution of neutron imaging has improved recently, which - together with the enhancement of the efficiency in data acquisition- can be exploited to narrow the energy band and to implement more sophisticated methods like neutron grating interferometry. This paper provides a report about the current options in neutron imaging and describes how the gap to neutron scattering data can be closed in the future, e.g. by diffractive imaging, the use of polarized neutrons and the dark-field imagining of relevant materials. This overview is focused onto the interaction between neutron imaging and neutron scattering with the aim of synergy. It reflects mainly the authors’ experiences at their PSI facilities without ignoring the activities at the different other labs world-wide.

Neutron diffraction of acetazolamide-bound human carbonic anhydrase II reveals atomic details of drug binding

PubMed Central

Fisher, S. Zoë; Aggarwal, Mayank; Kovalevsky, Andrey Y.; Silverman, David N.; McKenna, Robert

2012-01-01

Carbonic anhydrases (CAs) catalyze the hydration of CO2 forming HCO3− and a proton, an important reaction for many physiological processes including respiration, fluid secretion, and pH regulation. As such, CA isoforms are prominent clinical targets for treating various diseases. The clinically used acetazolamide (AZM) is a sulfonamide that binds with high affinity to human CA isoform II (HCA II). There are several X-ray structures available of AZM bound to various CA isoforms, but these complexes do not show the charged state of AZM, or hydrogen (H) atom positions of the protein and solvent. Neutron diffraction is a useful technique for directly observing H atoms and the mapping of H-bonding networks that can greatly contribute to rational drug design. To this end the neutron structure of H/D exchanged HCA II crystals in complex with AZM was determined. The structure reveals the molecular details of AZM binding and the charged state of the bound drug. This represents the first determined neutron structure of a clinically used drug bound to its target. PMID:22928733

The structure of liquid water by polarized neutron diffraction and reverse Monte Carlo modelling.

PubMed

Temleitner, László; Pusztai, László; Schweika, Werner

2007-08-22

The coherent static structure factor of water has been investigated by polarized neutron diffraction. Polarization analysis allows us to separate the huge incoherent scattering background from hydrogen and to obtain high quality data of the coherent scattering from four different mixtures of liquid H(2)O and D(2)O. The information obtained by the variation of the scattering contrast confines the configurational space of water and is used by the reverse Monte Carlo technique to model the total structure factors. Structural characteristics have been calculated directly from the resulting sets of particle coordinates. Consistency with existing partial pair correlation functions, derived without the application of polarized neutrons, was checked by incorporating them into our reverse Monte Carlo calculations. We also performed Monte Carlo simulations of a hard sphere system, which provides an accurate estimate of the information content of the measured data. It is shown that the present combination of polarized neutron scattering and reverse Monte Carlo structural modelling is a promising approach towards a detailed understanding of the microscopic structure of water.

Applying neutron transmission physics and 3D statistical full-field model to understand 2D Bragg-edge imaging

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

Xie, Qingge; Song, Gian; Gorti, Sarma B.

Bragg-edge imaging, which is also known as neutron radiography, has recently emerged as a novel crystalline characterization technique. Modelling of this novel technique by incorporating various features of the underlying microstructure (including the crystallographic texture, the morphological texture, and the grain size) of the material remains a subject of considerable research and development. In this paper, Inconel 718 samples made by additive manufacturing were investigated by neutron diffraction and neutron radiography techniques. The specimen features strong morphological and crystallographic textures and a highly heterogeneous microstructure. A 3D statistical full-field model is introduced by taking details of the microstructure into accountmore » to understand the experimental neutron radiography results. The Bragg-edge imaging and the total cross section were calculated based on the neutron transmission physics. A good match was obtained between the model predictions and experimental results at different incident beam angles with respect to the sample build direction. The current theoretical approach has the ability to incorporate 3D spatially resolved microstructural heterogeneity information and shows promise in understanding the 2D neutron radiography of bulk samples. With further development to incorporate the heterogeneity in lattice strain in the model, it can be used as a powerful tool in the future to better understand the neutron radiography data.« less

Applying neutron transmission physics and 3D statistical full-field model to understand 2D Bragg-edge imaging

DOE PAGES

Xie, Qingge; Song, Gian; Gorti, Sarma B.; ...

2018-02-21

Bragg-edge imaging, which is also known as neutron radiography, has recently emerged as a novel crystalline characterization technique. Modelling of this novel technique by incorporating various features of the underlying microstructure (including the crystallographic texture, the morphological texture, and the grain size) of the material remains a subject of considerable research and development. In this paper, Inconel 718 samples made by additive manufacturing were investigated by neutron diffraction and neutron radiography techniques. The specimen features strong morphological and crystallographic textures and a highly heterogeneous microstructure. A 3D statistical full-field model is introduced by taking details of the microstructure into accountmore » to understand the experimental neutron radiography results. The Bragg-edge imaging and the total cross section were calculated based on the neutron transmission physics. A good match was obtained between the model predictions and experimental results at different incident beam angles with respect to the sample build direction. The current theoretical approach has the ability to incorporate 3D spatially resolved microstructural heterogeneity information and shows promise in understanding the 2D neutron radiography of bulk samples. With further development to incorporate the heterogeneity in lattice strain in the model, it can be used as a powerful tool in the future to better understand the neutron radiography data.« less

Large-volume protein crystal growth for neutron macromolecular crystallography.

PubMed

Ng, Joseph D; Baird, James K; Coates, Leighton; Garcia-Ruiz, Juan M; Hodge, Teresa A; Huang, Sijay

2015-04-01

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for the growth of crystals to significant dimensions that are now relevant to NMC are revisited. These include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.

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

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

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

A history of neutrons in biology: the development of neutron protein crystallography at BNL and LANL.

PubMed

Schoenborn, Benno P

2010-11-01

The first neutron diffraction data were collected from crystals of myoglobin almost 42 years ago using a step-scan diffractometer with a single detector. Since then, major advances have been made in neutron sources, instrumentation and data collection and analysis, and in biochemistry. Fundamental discoveries about enzyme mechanisms, biological complex structures, protein hydration and H-atom positions have been and continue to be made using neutron diffraction. The promise of neutrons has not changed since the first crystal diffraction data were collected. Today, with the developments of beamlines at spallation neutron sources and the use of the Laue method for data collection, the field of neutrons in structural biology has renewed vitality.

PREFACE: Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques

NASA Astrophysics Data System (ADS)

Sakurai, Kenji

2010-12-01

This special issue is devoted to describing recent applications of x-ray and neutron scattering techniques to the exploration of surfaces and buried interfaces of various functional materials. Unlike many other surface-sensitive methods, these techniques do not require ultra high vacuum, and therefore, a variety of real and complicated surfaces fall within the scope of analysis. It must be particularly emphasized that the techniques are capable of seeing even buried function interfaces as well as the surface. Furthermore, the information, which ranges from the atomic to mesoscopic scale, is highly quantitative and reproducible. The non-destructive nature of the techniques is another important advantage of using x-rays and neutrons, when compared with other atomic-scale analyses. This ensures that the same specimen can be measured by other techniques. Such features are fairly attractive when exploring multilayered materials with nanostructures (dots, tubes, wires, etc), which are finding applications in electronic, magnetic, optical and other devices. The Japan Applied Physics Society has established a group to develop the research field of studying buried function interfaces with x-rays and neutrons. As the methods can be applied to almost all types of materials, from semiconductor and electronic devices to soft materials, participants have fairly different backgrounds but share a common interest in state-of-the-art x-ray and neutron techniques and sophisticated applications. A series of workshops has been organized almost every year since 2001. Some international interactions have been continued intensively, although the community is part of a Japanese society. This special issue does not report the proceedings of the recent workshop, although all the authors are in some way involved in the activities of the above society. Initially, we intended to collect quite long overview papers, including the authors' latest and most important original results, as well as updates on recent progress and global trends in the field. We planned to cover quite a wide area of surface and buried interface science with x-rays and neutrons. Following a great deal of discussion during the editing process, we have decided to change direction. As we intend to publish similar special issues on a frequent basis, we will not insist on editing this issue as systematic and complete collections of research. Many authors decided to write an ordinary research paper rather than an article including systematic accounts. Due to this change in policy, some authors declined to contribute, and the number of papers is now just 12. However, readers will find that the special issue gives an interesting collection of new original research in surface and buried interface studies with x-rays and neutrons. The 12 papers cover the following research topics: (1) polymer analysis by diffuse scattering; (2) discussion of the electrochemical solid--liquid interface by synchrotron x-ray diffraction; (3) analysis of capped nanodots by grazing incidence small-angle x-ray scattering (GISAXS); (4) discussion of the strain distribution in silicon by high-resolution x-ray diffraction; (5) study of mesoporous structures by a combination of x-ray reflectivity and GISAXS; (6) discussion of energy-dispersive x-ray reflectometry and its applications; (7) neutron reflectivity studies on hydrogen terminated silicon interface; (8) the fabrication and performance of a special mirror for water windows; (9) depth selective analysis by total-reflection x-ray diffraction; (10) nanoparticle thin films prepared by a gas deposition technique; (11) discussion of crystal truncation rod (CTR) scattering of semiconductor nanostructures; (12) magnetic structure analysis of thin films by polarized neutron reflectivity. While not discussed in the present special issue, x-ray and neutron techniques have made great progress. The most important steps forward have been in 2D/3D real-space imaging, and realtime measurement. Advances in such technologies are bringing with them new opportunities in surface and buried interface science. In the not too distant future, we will publish a special issue or a book detailing such progress. Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques contents Lateral uniformity in chemical composition along a buried reaction front in polymers using off-specular reflectivity Kristopher A Lavery, Vivek M Prabhu, Sushil Satija and Wen-li Wu Orientation dependence of Pd growth on Au electrode surfaces M Takahasi, K Tamura, J Mizuki, T Kondo and K Uosaki A grazing incidence small-angle x-ray scattering analysis on capped Ge nanodots in layer structures Hiroshi Okuda, Masayuki Kato, Keiji Kuno, Shojiro Ochiai, Noritaka Usami, Kazuo Nakajima and Osami Sakata High resolution grazing-incidence in-plane x-ray diffraction for measuring the strain of a Si thin layer Kazuhiko Omote X-ray analysis of mesoporous silica thin films templated by Brij58 surfactant S Fall, M Kulij and A Gibaud Review of the applications of x-ray refraction and the x-ray waveguide phenomenon to estimation of film structures Kouichi Hayashi Epitaxial growth of largely mismatched crystals on H-terminated Si(111) surfaces Hidehito Asaoka Novel TiO2/ZnO multilayer mirrors at 'water-window' wavelengths fabricated by atomic layer epitaxy H Kumagai, Y Tanaka, M Murata, Y Masuda and T Shinagawa Depth-selective structural analysis of thin films using total-external-reflection x-ray diffraction Tomoaki Kawamura and Hiroo Omi Structures of Yb nanoparticle thin films grown by deposition in He and N2 gas atmospheres: AFM and x-ray reflectivity studies Martin Jerab and Kenji Sakurai Ga and As composition profiles in InP/GaInAs/InP heterostructures—x-ray CTR scattering and cross-sectional STM measurements Yoshikazu Takeda, Masao Tabuchi and Arao Nakamura Polarized neutron reflectivity study of a thermally treated MnIr/CoFe exchange bias system Naoki Awaji, Toyoo Miyajima, Shuuichi Doi and Kenji Nomura

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

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

Mason, Thom; Gawne, Timothy J; Nagler, Stephen E

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,more » 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.« less

Advanced setup for high-pressure and low-temperature neutron diffraction at hydrostatic conditions

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

Lokshin, Konstantin A.; Zhao Yusheng

2005-06-15

We describe a design of the experimental setup for neutron diffraction studies at low temperatures and hydrostatic pressure. The significant benefit of the setup, compared to the previous methods, is that it makes possible the simultaneous collection of neutrons diffracted at the 30 deg. -150 deg. range with no contamination by the primary scattering from the sample surroundings and without cutting out the incident and diffracted beams. The suggested design is most useful for third-generation time-of-flight diffractometers and constant wavelength instruments. Application of the setup expands the capabilities of high-pressure neutron diffraction, allowing time-resolved kinetics and structural studies, multihistogram Rietveld,more » and pair distribution function and texture analyses. The high efficiency of the setup was proven for the HIPPO diffractometer at Los Alamos Neutron Science Center under pressures up to 10 kbar and temperatures from 4 to 300 K.« less

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

A Review of Significant Advances in Neutron Imaging from Conception to the Present

NASA Astrophysics Data System (ADS)

Brenizer, J. S.

This review summarizes the history of neutron imaging with a focus on the significant events and technical advancements in neutron imaging methods, from the first radiograph to more recent imaging methods. A timeline is presented to illustrate the key accomplishments that advanced the neutron imaging technique. Only three years after the discovery of the neutron by English physicist James Chadwick in 1932, neutron imaging began with the work of Hartmut Kallmann and Ernst Kuhn in Berlin, Germany, from 1935-1944. Kallmann and Kuhn were awarded a joint US Patent issued in January 1940. Little progress was made until the mid-1950's when Thewlis utilized a neutron beam from the BEPO reactor at Harwell, marking the beginning of the application of neutron imaging to practical applications. As the film method was improved, imaging moved from a qualitative to a quantitative technique, with applications in industry and in nuclear fuels. Standards were developed to aid in the quantification of the neutron images and the facility's capabilities. The introduction of dynamic neutron imaging (initially called real-time neutron radiography and neutron television) in the late 1970's opened the door to new opportunities and new challenges. As the electronic imaging matured, the introduction of the CCD imaging devices and solid-state light intensifiers helped address some of these challenges. Development of improved imaging devices for the medical community has had a major impact on neutron imaging. Additionally, amorphous silicon sensors provided improvements in temporal resolution, while providing a reasonably large imaging area. The development of new neutron imaging sensors and the development of new neutron imaging techniques in the past decade has advanced the technique's ability to provide insight and understanding of problems that other non-destructive techniques could not provide. This rapid increase in capability and application would not have been possible without the advances in computer processing speed and increased memory storage. For example, images with enhanced contrast are created by using the reflection, refraction, diffraction and ultra small angle scattering interactions. It is somewhat ironic that, like the first development of neutron images, the technique remains limited by the availability of high-intensity neutron sources, both in the facility cost and portability.

Large-volume protein crystal growth for neutron macromolecular crystallography

DOE PAGES

Ng, Joseph D.; Baird, James K.; Coates, Leighton; ...

2015-03-30

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for themore » growth of crystals to significant dimensions that are now relevant to NMC are revisited. We report that these include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.« less

Large-volume protein crystal growth for neutron macromolecular crystallography

PubMed Central

Ng, Joseph D.; Baird, James K.; Coates, Leighton; Garcia-Ruiz, Juan M.; Hodge, Teresa A.; Huang, Sijay

2015-01-01

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for the growth of crystals to significant dimensions that are now relevant to NMC are revisited. These include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations. PMID:25849493

Large-volume protein crystal growth for neutron macromolecular crystallography

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

Ng, Joseph D.; Baird, James K.; Coates, Leighton

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for themore » growth of crystals to significant dimensions that are now relevant to NMC are revisited. We report that these include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.« less

Analysis of the applicability of the modified kinematic approximation to describe the off-specular neutron scattering from the surface of micro- and nanostructured objects

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

Belushkin, A. V., E-mail: belushk@nf.jinr.ru; Manoshin, S. A., E-mail: manoshin@nf.jinr.ru; Rikhvitskiy, V. S.

2016-09-15

The applicability of the modified kinematic approximation to describe the off-specular neutron scattering from interfaces between media is analyzed. It is demonstrated that in some cases one can expect not only a qualitative but also a quantitative agreement between the data and the results of experiments and calculations based on more accurate techniques. Diffuse scattering from rough surfaces and thin films with correlated and noncorrelated roughness of the upper and lower interfaces and the neutron diffraction by stripe magnetic domains and magnetic domains with a random size distribution (magnetic roughness) are considered as examples.

Neutron and X-ray single-crystal diffraction from protein microcrystals via magnetically oriented microcrystal arrays in gels.

PubMed

Tsukui, Shu; Kimura, Fumiko; Kusaka, Katsuhiro; Baba, Seiki; Mizuno, Nobuhiro; Kimura, Tsunehisa

2016-07-01

Protein microcrystals magnetically aligned in D2O hydrogels were subjected to neutron diffraction measurements, and reflections were observed for the first time to a resolution of 3.4 Å from lysozyme microcrystals (∼10 × 10 × 50 µm). This result demonstrated the possibility that magnetically oriented microcrystals consolidated in D2O gels may provide a promising means to obtain single-crystal neutron diffraction from proteins that do not crystallize at the sizes required for neutron diffraction structure determination. In addition, lysozyme microcrystals aligned in H2O hydrogels allowed structure determination at a resolution of 1.76 Å at room temperature by X-ray diffraction. The use of gels has advantages since the microcrystals are measured under hydrated conditions.

Characterization of deformation mechanisms in zirconium alloys: effect of temperature and irradiation

NASA Astrophysics Data System (ADS)

Long, Fei

Zirconium alloys have been widely used in the CANDU (CANada Deuterium Uranium) reactor as core structural materials. Alloy such as Zircaloy-2 has been used for calandria tubes; fuel cladding; the pressure tube is manufactured from alloy Zr-2.5Nb. During in-reactor service, these alloys are exposed to a high flux of fast neutron at elevated temperatures. It is important to understand the effect of temperature and irradiation on the deformation mechanism of zirconium alloys. Aiming to provide experimental guidance for future modeling predictions on the properties of zirconium alloys this thesis describes the result of an investigation of the change of slip and twinning modes in Zircaloy-2 and Zr-2.5Nb as a function of temperature and irradiation. The aim is to provide scientific fundamentals and experimental evidences for future industry modeling in processing technique design, and in-reactor property change prediction of zirconium components. In situ neutron diffraction mechanical tests carried out on alloy Zircaloy-2 at three temperatures: 100¢ªC, 300¢ªC, and 500¢ªC, and described in Chapter 3. The evolution of the lattice strain of individual grain families in the loading and Poisson's directions during deformation, which probes the operation of slip and twinning modes at different stress levels, are described. By using the same type of in situ neutron diffraction technique, tests on Zr-2.5Nb pressure tube material samples, in either the fast-neutron irradiated or un-irradiated condition, are reported in Chapter 4. In Chapter 5, the measurement of dislocation density by means of line profile analysis of neutron diffraction patterns, as well as TEM observations of the dislocation microstructural evolution, is described. In Chapter 6 a hot-rolled Zr-2.5Nb with a larger grain size compared with the pressure tubing was used to study the development of dislocation microstructures with increasing plastic strain. In Chapter 7, in situ loading of heavy ion irradiated hot-rolled Zr-2.5Nb alloy is described, providing evidence for the interaction between moving dislocations and irradiation induced loops. Chapter 8 gives the effect on the dislocation structure of different levels of compressive strains along two directions in the hot-rolled Zr-2.5Nb alloy. By using high resolution neutron diffraction and TEM observations, the evolution of type and dislocation densities, as well as changes of dislocation microstructure with plastic strain were characterized.

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

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

Budayova-Spano, Monika, E-mail: spano@embl-grenoble.fr; Institut Laue-Langevin, 6 Rue Jules Horowitz, BP 156, 38042 Grenoble; Bonneté, Françoise

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 (grownmore » 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.« less

Reentrant cluster glass and stability of ferromagnetism in the Ga2MnCo Heusler alloy

NASA Astrophysics Data System (ADS)

Samanta, Tamalika; Bhobe, P. A.; Das, A.; Kumar, A.; Nigam, A. K.

2018-05-01

We present here a detailed investigation into the magnetic ordering of a full Heusler alloy Ga2MnCo using dc and ac magnetization measurements, neutron diffraction, and neutron depolarization experiments. The crystal structure at room temperature was first confirmed to be L 21 using the highly intense synchrotron x-ray diffraction technique. Temperature-dependent magnetization reveals that Ga2MnCo enters a ferromagnetic (FM) state at TC=154 K, characterized by a sharp increase in magnetization and a plateaulike region hereafter. As the temperature is decreased further, a sharp drop in magnetization is observed at Tf=50 K, hinting toward an antiferromagnetic (AFM) phase change. Neutron diffraction (ND) recorded over the range of temperature from 6 to 300 K provides combined information regarding crystal as well as magnetic structure. Accordingly, an increase in the intensity of the ND pattern is seen at 150 K, signaling the onset of long-range FM order. However, there is no sign of the appearance of superlattice reflections corresponding to the AFM phase in the patterns recorded below 50 K. An unusual discontinuity in the unit-cell volume is seen around Tf, indicating a coupling of this second transition with the contraction of the lattice. Attempts to unravel this interesting magnetic behavior using ac susceptibility measurements led to the existence of glassy magnetism below Tf. Systematic analysis of the susceptibility results along with neutron depolarization measurement identifies the low-temperature phase as a reentrant cluster glass.

Comparative study of the magnetic properties of La3Ni2B‧O9 for B‧ = Nb, Taor Sb

NASA Astrophysics Data System (ADS)

Chin, Chun-Mann; Battle, Peter D.; Blundell, Stephen J.; Hunter, Emily; Lang, Franz; Hendrickx, Mylène; Paria Sena, Robert; Hadermann, Joke

2018-02-01

Polycrystalline samples of La3Ni2NbO9 and La3Ni2TaO9 have been characterised by X-ray and neutron diffraction, electron microscopy, magnetometry and muon spin relaxation (μSR); the latter technique was also applied to La3Ni2SbO9. On the length scale of a neutron diffraction experiment, the six-coordinate sites of the monoclinic perovskite structure are occupied in a 1:1 ordered manner by Ni and a random ⅓Ni/⅔B‧ mixture. Electron microscopy demonstrated that this 1:1 ordering is maintained over microscopic distances, although diffuse scattering indicative of short-range ordering on the mixed site was observed. No magnetic Bragg scattering was observed in neutron diffraction patterns collected from La3Ni2B‧O9 (B‧ = Nb or Ta) at 5 K although in each case μSR identified the presence of static spins below 30 K. Magnetometry showed that La3Ni2NbO9 behaves as a spin glass below 29 K but significant short-range interactions are present in La3Ni2TaO9 below 85 K. The contrasting properties of these compounds are discussed in terms of their microstructure.

Studies of cavitation and ice nucleation in 'doubly-metastable' water: time-lapse photography and neutron diffraction.

PubMed

Barrow, Matthew S; Williams, P Rhodri; Chan, Hoi-Houng; Dore, John C; Bellissent-Funel, Marie-Claire

2012-10-14

High-speed photographic studies and neutron diffraction measurements have been made of water under tension in a Berthelot tube. Liquid water was cooled below the normal ice-nucleation temperature and was in a doubly-metastable state prior to a collapse of the liquid state. This transition was accompanied by an exothermic heat release corresponding with the rapid production of a solid phase nucleated by cavitation. Photographic techniques have been used to observe the phase transition over short time scales in which a solidification front is observed to propagate through the sample. Significantly, other images at a shorter time interval reveal the prior formation of cavitation bubbles at the beginning of the process. The ice-nucleation process is explained in terms of a mechanism involving hydrodynamically-induced changes in tension in supercooled water in the near vicinity of an expanding cavitation bubble. Previous explanations have attributed the nucleation of the solid phase to the production of high positive pressures. Corresponding results are presented which show the initial neutron diffraction pattern after ice-nucleation. The observed pattern does not exhibit the usual crystalline pattern of hexagonal ice [I(h)] that is formed under ambient conditions, but indicates the presence of other ice forms. The composite features can be attributed to a mixture of amorphous ice, ice-I(h)/I(c) and the high-pressure form, ice-III, and the diffraction pattern continues to evolve over a time period of about an hour.

Synthesis and characterization of Ca-doped LaMnAsO

NASA Astrophysics Data System (ADS)

Liu, Yong; Straszheim, Warren E.; Das, Pinaki; Islam, Farhan; Heitmann, Thomas W.; McQueeney, Robert J.; Vaknin, David

2018-05-01

We report on our attempt to hole-dope the antiferromagnetic semiconductor LaMnAsO by substitution of the La3 + site by Ca2 +. We use neutron and x-ray diffraction, magnetic susceptibility, and transport techniques to characterize polycrystalline (La1 -xCax)MnAsO samples prepared by solid-state reaction and find that the parent compound is highly resistant to substitution with an upper limit x ≤0.01 . Magnetic susceptibility of the parent and the x =0.002 (xnom=0.04 ) compounds indicate a negligible presence of magnetic impurities (i.e., MnO or MnAs). Rietveld analysis of neutron and x-ray diffraction data shows the preservation of both the tetragonal (P 4 /n m m ) structure upon doping and the antiferromagnetic ordering temperature, TN=355 ±5 K.

Precision determination of absolute neutron flux

DOE PAGES

Yue, A. T.; Anderson, E. S.; Dewey, M. S.; ...

2018-06-08

A technique for establishing the total neutron rate of a highly-collimated monochromatic cold neutron beam was demonstrated using an alpha–gamma counter. The method involves only the counting of measured rates and is independent of neutron cross sections, decay chain branching ratios, and neutron beam energy. For the measurement, a target of 10B-enriched boron carbide totally absorbed the neutrons in a monochromatic beam, and the rate of absorbed neutrons was determined by counting 478 keV gamma rays from neutron capture on 10B with calibrated high-purity germanium detectors. A second measurement based on Bragg diffraction from a perfect silicon crystal was performedmore » to determine the mean de Broglie wavelength of the beam to a precision of 0.024%. With these measurements, the detection efficiency of a neutron monitor based on neutron absorption on 6Li was determined to an overall uncertainty of 0.058%. We discuss the principle of the alpha–gamma method and present details of how the measurement was performed including the systematic effects. We further describe how this method may be used for applications in neutron dosimetry and metrology, fundamental neutron physics, and neutron cross section measurements.« less

Precision determination of absolute neutron flux

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

Yue, A. T.; Anderson, E. S.; Dewey, M. S.

A technique for establishing the total neutron rate of a highly-collimated monochromatic cold neutron beam was demonstrated using an alpha–gamma counter. The method involves only the counting of measured rates and is independent of neutron cross sections, decay chain branching ratios, and neutron beam energy. For the measurement, a target of 10B-enriched boron carbide totally absorbed the neutrons in a monochromatic beam, and the rate of absorbed neutrons was determined by counting 478 keV gamma rays from neutron capture on 10B with calibrated high-purity germanium detectors. A second measurement based on Bragg diffraction from a perfect silicon crystal was performedmore » to determine the mean de Broglie wavelength of the beam to a precision of 0.024%. With these measurements, the detection efficiency of a neutron monitor based on neutron absorption on 6Li was determined to an overall uncertainty of 0.058%. We discuss the principle of the alpha–gamma method and present details of how the measurement was performed including the systematic effects. We further describe how this method may be used for applications in neutron dosimetry and metrology, fundamental neutron physics, and neutron cross section measurements.« less

Microstructural and micromechanical characterization of IN718 theta shaped specimens built with electron beam melting

DOE PAGES

Cakmak, Ercan; Kirka, Michael M.; Watkins, Thomas R.; ...

2016-02-23

Theta-shaped specimens were additively manufactured out of Inconel 718 powders using an electron beam melting technique, as a model complex load bearing structure. We employed two different build strategies; producing two sets of specimens. Microstructural and micro-mechanical characterizations were performed using electron back-scatter, synchrotron x-ray and in-situ neutron diffraction techniques. In particular, the cross-members of the specimens were the focus of the synchrotron x-ray and in-situ neutron diffraction measurements. The build strategies employed resulted in the formation of distinct microstructures and crystallographic textures, signifying the importance of build-parameter manipulation for microstructural optimization. Large strain anisotropy of the different lattice planesmore » was observed during in-situ loading. Texture was concluded to have a distinct effect upon both the axial and transverse strain responses of the cross-members. In particular, the (200), (220) and (420) transverse lattice strains all showed unexpected overlapping trends in both builds. This was related to the strong {200} textures along the build/loading direction, providing agreement between the experimental and calculated results.« less

Neutron protein crystallography: A complementary tool for locating hydrogens in proteins.

PubMed

O'Dell, William B; Bodenheimer, Annette M; Meilleur, Flora

2016-07-15

Neutron protein crystallography is a powerful tool for investigating protein chemistry because it directly locates hydrogen atom positions in a protein structure. The visibility of hydrogen and deuterium atoms arises from the strong interaction of neutrons with the nuclei of these isotopes. Positions can be unambiguously assigned from diffraction at resolutions typical of protein crystals. Neutrons have the additional benefit to structural biology of not inducing radiation damage in protein crystals. The same crystal could be measured multiple times for parametric studies. Here, we review the basic principles of neutron protein crystallography. The information that can be gained from a neutron structure is presented in balance with practical considerations. Methods to produce isotopically-substituted proteins and to grow large crystals are provided in the context of neutron structures reported in the literature. Available instruments for data collection and software for data processing and structure refinement are described along with technique-specific strategies including joint X-ray/neutron structure refinement. Examples are given to illustrate, ultimately, the unique scientific value of neutron protein crystal structures. Copyright © 2015 Elsevier Inc. All rights reserved.

Investigation of Renal Stones by X-ray and Neutron Diffraction

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

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

2007-04-23

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

Investigation of microstructure in additive manufactured Inconel 625 by spatially resolved neutron transmission spectroscopy

DOE PAGES

Tremsin, Anton S.; Gao, Yan; Dial, Laura C.; ...

2016-07-08

Non-destructive testing techniques based on neutron imaging and diffraction can provide information on the internal structure of relatively thick metal samples (up to several cm), which are opaque to other conventional non-destructive methods. Spatially resolved neutron transmission spectroscopy is an extension of traditional neutron radiography, where multiple images are acquired simultaneously, each corresponding to a narrow range of energy. The analysis of transmission spectra enables studies of bulk microstructures at the spatial resolution comparable to the detector pixel. In this study we demonstrate the possibility of imaging (with ~100 μm resolution) distribution of some microstructure properties, such as residual strain,more » texture, voids and impurities in Inconel 625 samples manufactured with an additive manufacturing method called direct metal laser melting (DMLM). Although this imaging technique can be implemented only in a few large-scale facilities, it can be a valuable tool for optimization of additive manufacturing techniques and materials and for correlating bulk microstructure properties to manufacturing process parameters. Additionally, the experimental strain distribution can help validate finite element models which many industries use to predict the residual stress distributions in additive manufactured components.« less

Investigation of microstructure in additive manufactured Inconel 625 by spatially resolved neutron transmission spectroscopy.

PubMed

Tremsin, Anton S; Gao, Yan; Dial, Laura C; Grazzi, Francesco; Shinohara, Takenao

2016-01-01

Non-destructive testing techniques based on neutron imaging and diffraction can provide information on the internal structure of relatively thick metal samples (up to several cm), which are opaque to other conventional non-destructive methods. Spatially resolved neutron transmission spectroscopy is an extension of traditional neutron radiography, where multiple images are acquired simultaneously, each corresponding to a narrow range of energy. The analysis of transmission spectra enables studies of bulk microstructures at the spatial resolution comparable to the detector pixel. In this study we demonstrate the possibility of imaging (with ~100 μm resolution) distribution of some microstructure properties, such as residual strain, texture, voids and impurities in Inconel 625 samples manufactured with an additive manufacturing method called direct metal laser melting (DMLM). Although this imaging technique can be implemented only in a few large-scale facilities, it can be a valuable tool for optimization of additive manufacturing techniques and materials and for correlating bulk microstructure properties to manufacturing process parameters. In addition, the experimental strain distribution can help validate finite element models which many industries use to predict the residual stress distributions in additive manufactured components.

Investigation of microstructure in additive manufactured Inconel 625 by spatially resolved neutron transmission spectroscopy

NASA Astrophysics Data System (ADS)

Tremsin, Anton S.; Gao, Yan; Dial, Laura C.; Grazzi, Francesco; Shinohara, Takenao

2016-01-01

Non-destructive testing techniques based on neutron imaging and diffraction can provide information on the internal structure of relatively thick metal samples (up to several cm), which are opaque to other conventional non-destructive methods. Spatially resolved neutron transmission spectroscopy is an extension of traditional neutron radiography, where multiple images are acquired simultaneously, each corresponding to a narrow range of energy. The analysis of transmission spectra enables studies of bulk microstructures at the spatial resolution comparable to the detector pixel. In this study we demonstrate the possibility of imaging (with 100 μm resolution) distribution of some microstructure properties, such as residual strain, texture, voids and impurities in Inconel 625 samples manufactured with an additive manufacturing method called direct metal laser melting (DMLM). Although this imaging technique can be implemented only in a few large-scale facilities, it can be a valuable tool for optimization of additive manufacturing techniques and materials and for correlating bulk microstructure properties to manufacturing process parameters. In addition, the experimental strain distribution can help validate finite element models which many industries use to predict the residual stress distributions in additive manufactured components.

Investigation of microstructure in additive manufactured Inconel 625 by spatially resolved neutron transmission spectroscopy

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

Tremsin, Anton S.; Gao, Yan; Dial, Laura C.

Non-destructive testing techniques based on neutron imaging and diffraction can provide information on the internal structure of relatively thick metal samples (up to several cm), which are opaque to other conventional non-destructive methods. Spatially resolved neutron transmission spectroscopy is an extension of traditional neutron radiography, where multiple images are acquired simultaneously, each corresponding to a narrow range of energy. The analysis of transmission spectra enables studies of bulk microstructures at the spatial resolution comparable to the detector pixel. In this study we demonstrate the possibility of imaging (with ~100 μm resolution) distribution of some microstructure properties, such as residual strain,more » texture, voids and impurities in Inconel 625 samples manufactured with an additive manufacturing method called direct metal laser melting (DMLM). Although this imaging technique can be implemented only in a few large-scale facilities, it can be a valuable tool for optimization of additive manufacturing techniques and materials and for correlating bulk microstructure properties to manufacturing process parameters. Additionally, the experimental strain distribution can help validate finite element models which many industries use to predict the residual stress distributions in additive manufactured components.« less

Investigation of microstructure in additive manufactured Inconel 625 by spatially resolved neutron transmission spectroscopy

PubMed Central

Tremsin, Anton S.; Gao, Yan; Dial, Laura C.; Grazzi, Francesco; Shinohara, Takenao

2016-01-01

Abstract Non-destructive testing techniques based on neutron imaging and diffraction can provide information on the internal structure of relatively thick metal samples (up to several cm), which are opaque to other conventional non-destructive methods. Spatially resolved neutron transmission spectroscopy is an extension of traditional neutron radiography, where multiple images are acquired simultaneously, each corresponding to a narrow range of energy. The analysis of transmission spectra enables studies of bulk microstructures at the spatial resolution comparable to the detector pixel. In this study we demonstrate the possibility of imaging (with ~100 μm resolution) distribution of some microstructure properties, such as residual strain, texture, voids and impurities in Inconel 625 samples manufactured with an additive manufacturing method called direct metal laser melting (DMLM). Although this imaging technique can be implemented only in a few large-scale facilities, it can be a valuable tool for optimization of additive manufacturing techniques and materials and for correlating bulk microstructure properties to manufacturing process parameters. In addition, the experimental strain distribution can help validate finite element models which many industries use to predict the residual stress distributions in additive manufactured components. PMID:27877885

Infrastructure development for radioactive materials at the NSLS-II

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

Sprouster, D. J.; Weidner, R.; Ghose, S. K.

2018-02-01

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this article, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. We describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Infrastructure development for radioactive materials at the NSLS-II

DOE PAGES

Sprouster, David J.; Weidner, R.; Ghose, S. K.; ...

2017-11-04

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this paper, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. Finally, we describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Flexible sample environment for high resolution neutron imaging at high temperatures in controlled atmosphere

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

Makowska, Małgorzata G.; Theil Kuhn, Luise; Cleemann, Lars N.

In high material penetration by neutrons allows for experiments using sophisticated sample environments providing complex conditions. Thus, neutron imaging holds potential for performing in situ nondestructive measurements on large samples or even full technological systems, which are not possible with any other technique. Our paper presents a new sample environment for in situ high resolution neutron imaging experiments at temperatures from room temperature up to 1100 degrees C and/or using controllable flow of reactive atmospheres. The design also offers the possibility to directly combine imaging with diffraction measurements. Design, special features, and specification of the furnace are described. In addition,more » examples of experiments successfully performed at various neutron facilities with the furnace, as well as examples of possible applications are presented. Our work covers a broad field of research from fundamental to technological investigations of various types of materials and components.« less

Flexible sample environment for high resolution neutron imaging at high temperatures in controlled atmosphere

DOE PAGES

Makowska, Małgorzata G.; Theil Kuhn, Luise; Cleemann, Lars N.; ...

2015-12-17

In high material penetration by neutrons allows for experiments using sophisticated sample environments providing complex conditions. Thus, neutron imaging holds potential for performing in situ nondestructive measurements on large samples or even full technological systems, which are not possible with any other technique. Our paper presents a new sample environment for in situ high resolution neutron imaging experiments at temperatures from room temperature up to 1100 degrees C and/or using controllable flow of reactive atmospheres. The design also offers the possibility to directly combine imaging with diffraction measurements. Design, special features, and specification of the furnace are described. In addition,more » examples of experiments successfully performed at various neutron facilities with the furnace, as well as examples of possible applications are presented. Our work covers a broad field of research from fundamental to technological investigations of various types of materials and components.« less

Direct evidence of detwinning in polycrystalline Ni-Mn-Ga ferromagnetic shape memory alloys during deformation.

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

Nie, Z. H.; Lin Peng, R.; Johansson, S.

2008-01-01

In situ time-of-flight neutron diffraction and high-energy x-ray diffraction techniques were used to reveal the preferred reselection of martensite variants through a detwinning process in polycrystalline Ni-Mn-Ga ferromagnetic shape memory alloys under uniaxial compressive stress. The variant reorientation via detwinning during loading can be explained by considering the influence of external stress on the grain/variant orientation-dependent distortion energy. These direct observations of detwinning provide a good understanding of the deformation mechanisms in shape memory alloys.

Magnetic properties of tapiolite (FeTa2O6); a quasi two-dimensional (2D) antiferromagnet

NASA Astrophysics Data System (ADS)

Chung, E. M. L.; Lees, M. R.; McIntyre, G. J.; Wilkinson, C.; Balakrishnan, G.; Hague, J. P.; Visser, D.; McK Paul, D.

2004-11-01

The possibilities of two-dimensional (2D) short-range magnetic correlations and frustration effects in the mineral tapiolite are investigated using bulk-property measurements and neutron Laue diffraction. In this study of the magnetic properties of synthetic single-crystals of tapiolite, we find that single crystals of FeTa2O6 order antiferromagnetically at TN = 7.95 ± 0.05 K, with extensive two-dimensional correlations existing up to at least 40 K. Although we find no evidence that FeTa2O6 is magnetically frustrated, hallmarks of two-dimensional magnetism observed in our single-crystal data include: (i) broadening of the susceptibility maximum due to short-range correlations, (ii) a spin-flop transition and (iii) lambda anomalies in the heat capacity and d(χT)/dT. Complementary neutron Laue diffraction measurements reveal 1D magnetic diffuse scattering extending along the c* direction perpendicular to the magnetic planes. This magnetic diffuse scattering, observed for the first time using the neutron Laue technique by VIVALDI, arises directly as a result of 2D short-range spin correlations.

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

NASA Astrophysics Data System (ADS)

Sediako, Dimitry G.; Kasprzak, Wojciech

2015-09-01

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

High-pressure cells for study of condensed matter by diffraction and inelastic neutron scattering at low temperatures and in strong magnetic fields

NASA Astrophysics Data System (ADS)

Sadykov, R. A.; Strassle, Th; Podlesnyak, A.; Keller, L.; Fak, B.; Mesot, J.

2017-12-01

We have developed and implemented series of new original clamp high-pressure cells for neutron diffraction and inelastic neutron scattering at low temperatures. The cells design allows one to place them in the standard cryostats or cryomagnets used on neutron sources. Some results obtained for ZnCr2Se4 are demonstrated as an example.

Synthesis and characterization of Ca-doped LaMnAsO

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

Liu, Yong; Straszheim, Warren E.; Das, Pinaki

Here, we report on our attempt to hole-dope the antiferromagnetic semiconductor LaMnAsO by substitution of the La 3+ site by Ca 2+. We use neutron and x-ray diffraction, magnetic susceptibility, and transport techniques to characterize polycrystalline (La 1–xCa x)MnAsO samples prepared by solid-state reaction and find that the parent compound is highly resistant to substitution with an upper limit x ≤ 0.01. Magnetic susceptibility of the parent and the x = 0.002(x nom = 0.04) compounds indicate a negligible presence of magnetic impurities (i.e., MnO or MnAs). Rietveld analysis of neutron and x-ray diffraction data shows the preservation of bothmore » the tetragonal (P4/nmm) structure upon doping and the antiferromagnetic ordering temperature, T N = 355 ± 5 K.« less

Neutron diffraction studies of amphipathic helices in phospholipid bilayers

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

Bradshaw, J.P.; Gilchrist, P.J.; Duff, K.C.

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 tomore » 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.« less

Synthesis and characterization of Ca-doped LaMnAsO

DOE PAGES

Liu, Yong; Straszheim, Warren E.; Das, Pinaki; ...

2018-05-18

Here, we report on our attempt to hole-dope the antiferromagnetic semiconductor LaMnAsO by substitution of the La 3+ site by Ca 2+. We use neutron and x-ray diffraction, magnetic susceptibility, and transport techniques to characterize polycrystalline (La 1–xCa x)MnAsO samples prepared by solid-state reaction and find that the parent compound is highly resistant to substitution with an upper limit x ≤ 0.01. Magnetic susceptibility of the parent and the x = 0.002(x nom = 0.04) compounds indicate a negligible presence of magnetic impurities (i.e., MnO or MnAs). Rietveld analysis of neutron and x-ray diffraction data shows the preservation of bothmore » the tetragonal (P4/nmm) structure upon doping and the antiferromagnetic ordering temperature, T N = 355 ± 5 K.« less

Synthesis and study on the luminescence properties of cadmium borate phosphors

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

Annalakshmi, O.; Jose, M.T., E-mail: mtjosein@yahoo.co.in; Venkatraman, B.

2014-02-01

Highlights: • Cadmium borate synthesized by solid state sintering technique. • Neutron sensitivity of the material ten times that of TLD-600. • Gamma sensitivity is found to be twice that of TLD-100. • Gamma response is linear from 0.1 to 10{sup 3} mGy. - Abstract: Cadmium borate compound prepared through wet chemical reaction from the starting chemicals followed by high temperature solid state synthesis below the melting point to get the final TL phosphor powder. Phase purity and bond details of cadmium borate crystals are characterized using X-ray diffraction technique and infrared spectroscopy. Feasibility of these materials for radiation dosimetrymore » applications was studied after gamma and neutron irradiation. Gamma irradiation of undoped phosphors show a single peak around 185 °C whereas doping with gadolinium and silver, new more intense peak observed at 290 °C. Irradiation to thermal neutrons revealed single peak around 170 °C for all the phosphors. TL emission spectra and photoluminescence (PL) studies were also carried out on the phosphors. These borate materials are found to be highly sensitive to neutrons and hence can be used for neutron detection. Neutron sensitivity of the material is about ten times that of TLD-600.« less

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

Makowska, Małgorzata G., E-mail: malg@dtu.dk; European Spallation Source ESS AB, P.O. Box 176, SE-221 00 Lund; Theil Kuhn, Luise

High material penetration by neutrons allows for experiments using sophisticated sample environments providing complex conditions. Thus, neutron imaging holds potential for performing in situ nondestructive measurements on large samples or even full technological systems, which are not possible with any other technique. This paper presents a new sample environment for in situ high resolution neutron imaging experiments at temperatures from room temperature up to 1100 °C and/or using controllable flow of reactive atmospheres. The design also offers the possibility to directly combine imaging with diffraction measurements. Design, special features, and specification of the furnace are described. In addition, examples of experimentsmore » successfully performed at various neutron facilities with the furnace, as well as examples of possible applications are presented. This covers a broad field of research from fundamental to technological investigations of various types of materials and components.« less

CO 2 Sorption to Subsingle Hydration Layer Montmorillonite Clay Studied by Excess Sorption and Neutron Diffraction Measurements

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

Rother, Gernot; Ilton, Eugene S.; Wallacher, Dirk

2013-01-02

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 CO2 densities of ≈0.15 g/cm 3, followed by an approximately linear decrease of excess sorption to zero and negativemore » 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. Finally, at the excess sorption maximum, increasing CO 2 sorption with decreasing temperature is observed while the high-pressure sorption properties exhibit weak temperature dependence.« less

In situ neutron diffraction study of twin reorientation and pseudoplastic strain in Ni-Mn-Ga single crystals

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

Stoica, Alexandru Dan

2011-01-01

Twin variant reorientation in single-crystal Ni-Mn-Ga during quasi-static mechanical compression was studied using in situ neutron diffraction. The volume fraction of reoriented twin variants for different stress amplitudes were obtained from the changes in integrated intensities of high-order neutron diffraction peaks. It is shown that, during compressive loading, {approx}85% of the twins were reoriented parallel to the loading direction resulting in a maximum pseudoplasticstrain of {approx}5.5%, which is in agreement with measured macroscopic strain.

A pseudo-tetragonal tungsten bronze superstructure: a combined solution of the crystal structure of K6.4(Nb,Ta)(36.3)O94 with advanced transmission electron microscopy and neutron diffraction.

PubMed

Paria Sena, Robert; Babaryk, Artem A; Khainakov, Sergiy; Garcia-Granda, Santiago; Slobodyanik, Nikolay S; Van Tendeloo, Gustaaf; Abakumov, Artem M; Hadermann, Joke

2016-01-21

The crystal structure of the K6.4Nb28.2Ta8.1O94 pseudo-tetragonal tungsten bronze-type oxide was determined using a combination of X-ray powder diffraction, neutron diffraction and transmission electron microscopy techniques, including electron diffraction, high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), annular bright field STEM (ABF-STEM) and energy-dispersive X-ray compositional mapping (STEM-EDX). The compound crystallizes in the space group Pbam with unit cell parameters a = 37.468(9) Å, b = 12.493(3) Å, c = 3.95333(15) Å. The structure consists of corner sharing (Nb,Ta)O6 octahedra forming trigonal, tetragonal and pentagonal tunnels. All tetragonal tunnels are occupied by K(+) ions, while 1/3 of the pentagonal tunnels are preferentially occupied by Nb(5+)/Ta(5+) and 2/3 are occupied by K(+) in a regular pattern. A fractional substitution of K(+) in the pentagonal tunnels by Nb(5+)/Ta(5+) is suggested by the analysis of the HAADF-STEM images. In contrast to similar structures, such as K2Nb8O21, also parts of the trigonal tunnels are fractionally occupied by K(+) cations.

High-resolution 2-D Bragg diffraction reveal heterogeneous domain transformation behavior in a bulk relaxor ferroelectric

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

Pramanick, Abhijit, E-mail: apramani@cityu.edu.hk; Stoica, Alexandru D.; An, Ke

2016-08-29

In-situ measurement of fine-structure of neutron Bragg diffraction peaks from a relaxor single-crystal using a time-of-flight instrument reveals highly heterogeneous mesoscale domain transformation behavior under applied electric fields. It is observed that only ∼25% of domains undergo reorientation or phase transition contributing to large average strains, while at least 40% remain invariant and exhibit microstrains. Such insights could be central for designing new relaxor materials with better performance and longevity. The current experimental technique can also be applied to resolve complex mesoscale phenomena in other functional materials.

High-resolution 2-D Bragg diffraction reveal heterogeneous domain transformation behavior in a bulk relaxor ferroelectric

DOE PAGES

Pramanick, Abhijit; Stoica, Alexandru D.; An, Ke

2016-09-02

In-situ measurement of fine-structure of neutron Bragg diffraction peaks from a relaxor single-crystal using a time-of-flight instrument reveals highly heterogeneous mesoscale domain transformation behavior under applied electric fields. We observed that only 25% of domains undergo reorienta- tion or phase transition contributing to large average strains, while at least 40% remain invariant and exhibit microstrains. Such insights could be central for designing new relaxor materials with better performance and longevity. The current experimental technique can also be applied to resolve com- plex mesoscale phenomena in other functional materials.

Diffraction Techniques in Structural Biology

PubMed Central

Egli, Martin

2016-01-01

A detailed understanding of chemical and biological function and the mechanisms underlying the molecular activities ultimately requires atomic-resolution structural data. Diffraction-based techniques such as single-crystal X-ray crystallography, electron microscopy, and neutron diffraction are well established and they have paved the road to the stunning successes of modern-day structural biology. The major advances achieved in the last 20 years in all aspects of structural research, including sample preparation, crystallization, the construction of synchrotron and spallation sources, phasing approaches, and high-speed computing and visualization, now provide specialists and nonspecialists alike with a steady flow of molecular images of unprecedented detail. The present unit combines a general overview of diffraction methods with a detailed description of the process of a single-crystal X-ray structure determination experiment, from chemical synthesis or expression to phasing and refinement, analysis, and quality control. For novices it may serve as a stepping-stone to more in-depth treatises of the individual topics. Readers relying on structural information for interpreting functional data may find it a useful consumer guide. PMID:27248784

Diffraction Techniques in Structural Biology

PubMed Central

Egli, Martin

2010-01-01

A detailed understanding of chemical and biological function and the mechanisms underlying the activities ultimately requires atomic-resolution structural data. Diffraction-based techniques such as single-crystal X-ray crystallography, electron microscopy and neutron diffraction are well established and have paved the road to the stunning successes of modern-day structural biology. The major advances achieved in the last 20 years in all aspects of structural research, including sample preparation, crystallization, the construction of synchrotron and spallation sources, phasing approaches and high-speed computing and visualization, now provide specialists and non-specialists alike with a steady flow of molecular images of unprecedented detail. The present chapter combines a general overview of diffraction methods with a step-by-step description of the process of a single-crystal X-ray structure determination experiment, from chemical synthesis or expression to phasing and refinement, analysis and quality control. For novices it may serve as a stepping-stone to more in-depth treatises of the individual topics. Readers relying on structural information for interpreting functional data may find it a useful consumer guide. PMID:20517991

Diffraction Techniques in Structural Biology.

PubMed

Egli, Martin

2016-06-01

A detailed understanding of chemical and biological function and the mechanisms underlying the molecular activities ultimately requires atomic-resolution structural data. Diffraction-based techniques such as single-crystal X-ray crystallography, electron microscopy, and neutron diffraction are well established and they have paved the road to the stunning successes of modern-day structural biology. The major advances achieved in the last twenty years in all aspects of structural research, including sample preparation, crystallization, the construction of synchrotron and spallation sources, phasing approaches, and high-speed computing and visualization, now provide specialists and nonspecialists alike with a steady flow of molecular images of unprecedented detail. The present unit combines a general overview of diffraction methods with a detailed description of the process of a single-crystal X-ray structure determination experiment, from chemical synthesis or expression to phasing and refinement, analysis, and quality control. For novices it may serve as a stepping-stone to more in-depth treatises of the individual topics. Readers relying on structural information for interpreting functional data may find it a useful consumer guide. © 2016 by John Wiley & Sons, Inc. Copyright © 2016 John Wiley & Sons, Inc.

Neutron diffraction studies for realtime leaching of catalytic Ni

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

Iles, Gail N., E-mail: gail.iles@helmholtz-berlin.de; Reinhart, Guillaume, E-mail: guillaume.reinhart@im2np.fr; Institut Laue-Langevin, 6 rue Jules Horowitz, BP 156, 38042 Grenoble

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 processingmore » 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.« less

Mechanical characterization of an additively manufactured Inconel 718 theta-shaped specimen

DOE PAGES

Cakmak, Ercan; Watkins, Thomas R.; Bunn, Jeffrey R.; ...

2015-11-20

Two sets of “theta”-shaped specimens were additively manufactured with Inconel 718 powders using an electron beam melting technique with two distinct scan strategies. Light optical microscopy, mechanical testing coupled with a digital image correlation (DIC) technique, finite element modeling, and neutron diffraction with in situ loading characterizations were conducted. The cross-members of the specimens were the focus. Light optical micrographs revealed that different microstructures were formed with different scan strategies. Ex situ mechanical testing revealed each build to be stable under load until ductility was observed on the cross-members before failure. The elastic moduli were determined by forming a correlationmore » between the elastic tensile stresses determined from FEM, and the elastic strains obtained from DIC. The lattice strains were mapped with neutron diffraction during in situ elastic loading; and a good correlation between the average axial lattice strains on the cross-member and those determined from the DIC analysis was found. Lastly, the spatially resolved stresses in the elastic deformation regime are derived from the lattice strains and increased with applied load, showing a consistent distribution along the cross-member.« less

Mechanical characterization of an additively manufactured Inconel 718 theta-shaped specimen

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

Cakmak, Ercan; Watkins, Thomas R.; Bunn, Jeffrey R.

Two sets of “theta”-shaped specimens were additively manufactured with Inconel 718 powders using an electron beam melting technique with two distinct scan strategies. Light optical microscopy, mechanical testing coupled with a digital image correlation (DIC) technique, finite element modeling, and neutron diffraction with in situ loading characterizations were conducted. The cross-members of the specimens were the focus. Light optical micrographs revealed that different microstructures were formed with different scan strategies. Ex situ mechanical testing revealed each build to be stable under load until ductility was observed on the cross-members before failure. The elastic moduli were determined by forming a correlationmore » between the elastic tensile stresses determined from FEM, and the elastic strains obtained from DIC. The lattice strains were mapped with neutron diffraction during in situ elastic loading; and a good correlation between the average axial lattice strains on the cross-member and those determined from the DIC analysis was found. Lastly, the spatially resolved stresses in the elastic deformation regime are derived from the lattice strains and increased with applied load, showing a consistent distribution along the cross-member.« less

An Experimental Investigation into Additive Manufacturing-Induced Residual Stresses in 316L Stainless Steel

NASA Astrophysics Data System (ADS)

Wu, Amanda S.; Brown, Donald W.; Kumar, Mukul; Gallegos, Gilbert F.; King, Wayne E.

2014-12-01

Additive manufacturing (AM) technology provides unique opportunities for producing net-shape geometries at the macroscale through microscale processing. This level of control presents inherent trade-offs necessitating the establishment of quality controls aimed at minimizing undesirable properties, such as porosity and residual stresses. Here, we perform a parametric study into the effects of laser scanning pattern, power, speed, and build direction in powder bed fusion AM on residual stress. In an effort to better understand the factors influencing macroscale residual stresses, a destructive surface residual stress measurement technique (digital image correlation in conjunction with build plate removal and sectioning) has been coupled with a nondestructive volumetric evaluation method ( i.e., neutron diffraction). Good agreement between the two measurement techniques is observed. Furthermore, a reduction in residual stress is obtained by decreasing scan island size, increasing island to wall rotation to 45 deg, and increasing applied energy per unit length (laser power/speed). Neutron diffraction measurements reveal that, while in-plane residual stresses are affected by scan island rotation, axial residual stresses are unchanged. We attribute this in-plane behavior to misalignment between the greatest thermal stresses (scan direction) and largest part dimension.

2011 U.S. National School on Neutron and X-ray Scattering

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

Lang, Jonathan; te Vethuis, Suzanne; Ekkebus, Allen E

The 13th annual U.S. National School on Neutron and X-ray Scattering was held June 11 to 25, 2011, at both Oak Ridge and Argonne National Laboratories. This school brought together 65 early career graduate students from 56 different universities in the US and provided them with a broad introduction to the techniques available at the major large-scale neutron and synchrotron x-ray facilities. This school is focused primarily on techniques relevant to the physical sciences, but also touches on cross-disciplinary bio-related scattering measurements. During the school, students received lectures by over 30 researchers from academia, industry, and national laboratories and participatedmore » in a number of short demonstration experiments at Argonne's Advanced Photon Source (APS) and Oak Ridge's Spallation neutron Source (SNS) and High Flux Isotope Reactor (HFIR) facilities to get hands-on experience in using neutron and synchrotron sources. The first week of this year's school was held at Oak Ridge National Lab, where Lab director Thom Mason welcomed the students and provided a shitorical perspective of the neutron and x-ray facilities both at Oak Ridge and Argonne. The first few days of the school were dedicated to lectures laying out the basics of scattering theory and the differences and complementarity between the neutron and x-ray probes given by Sunil Sinha. Jack Carpenter provided an introduction into how neutrons are generated and detected. After this basic introduction, the students received lectures each morning on specific techniques and conducted demonstration experiments each afternoon on one of 15 different instruments at either the SNS or HFIR. Some of the topics covered during this week of the school included inelastic neutron scattering by Bruce Gaulin, x-ray and neutron reflectivity by Chuck Majkrazak, small-angle scattering by Volker Urban, powder diffraction by Ashfia Huq and diffuse scattering by Gene Ice.« less

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

NASA Astrophysics Data System (ADS)

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

2005-08-01

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

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

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

Chakoumakos, Bryan C.; Pracheil, Brenda M.; Koenigs, Ryan

Otoliths, calcium carbonate (CaCO 3) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3. Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed ofmore » vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 522 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.« less

Energy research with neutrons (ErwiN) and installation of a fast neutron powder diffraction option at the MLZ, Germany1

PubMed Central

Mühlbauer, Martin J.

2018-01-01

The need for rapid data collection and studies of small sample volumes in the range of cubic millimetres are the main driving forces for the concept of a new high-throughput monochromatic diffraction instrument at the Heinz Maier-Leibnitz Zentrum (MLZ), Germany. A large region of reciprocal space will be accessed by a detector with sufficient dynamic range and microsecond time resolution, while allowing for a variety of complementary sample environments. The medium-resolution neutron powder diffraction option for ‘energy research with neutrons’ (ErwiN) at the high-flux FRM II neutron source at the MLZ is foreseen to meet future demand. ErwiN will address studies of energy-related systems and materials with respect to their structure and uniformity by means of bulk and spatially resolved neutron powder diffraction. A set of experimental options will be implemented, enabling time-resolved studies, rapid parametric measurements as a function of external parameters and studies of small samples using an adapted radial collimator. The proposed powder diffraction option ErwiN will bridge the gap in functionality between the high-resolution powder diffractometer SPODI and the time-of-flight diffractometers POWTEX and SAPHiR at the MLZ. PMID:29896055

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

DOE PAGES

Chakoumakos, Bryan C.; Pracheil, Brenda M.; Koenigs, Ryan; ...

2016-11-18

Otoliths, calcium carbonate (CaCO 3) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3. Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed ofmore » vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 522 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.« less

New test of the dynamic theory of neutron diffraction by a moving grating

NASA Astrophysics Data System (ADS)

Zakharov, Maxim; Frank, Alexander; Kulin, German; Goryunov, Semyon

2018-04-01

Recently, multiwave dynamical theory of neutron diffraction by a moving grating was developed. The theory predicts that at a certain height of the grating profile a significant suppression of the zero-order diffraction may occur. The experiment to confirm predictions of this theory was performed. The resulting diffracted UCNs spectra were measured using time-of-flight Fourier diffractometer. The experimental data were compared with the results of numerical simulation and were found in a good agreement with theoretical predictions.

Neutron Radiography, Tomography, and Diffraction of Commercial Lithium-ion Polymer Batteries

NASA Astrophysics Data System (ADS)

Butler, Leslie G.; Lehmann, Eberhard H.; Schillinger, Burkhard

Imaging an intact, commercial battery as it cycles and wears is proved possible with neutron imaging. The wavelength range of imaging neutrons corresponds nicely with crystallographic dimensions of the electrochemically active species and the metal elec- trodes are relatively transparent. The time scale of charge/discharge cycling is well matched to dynamic tomography as performed with a golden ratio based projection angle ordering. The hydrogen content does create scatter which tends to blur internal struc- ture. In this report, three neutron experiments will be described: 3D images of charged and discharged batteries were obtained with monochromatic neutrons at the FRM II reactor. 2D images (PSI) of fresh and worn batteries as a function of charge state may show a new wear pattern. In situ neutron diffraction (SNS) of the intact battery provides more information about the concentrations of electrochemical species within the battery as a function of charge state and wear. The combination of 2D imaging, 3D imaging, and diffraction data show how neutron imaging can contribute to battery development and wear monitoring.

Neutron Nucleic Acid Crystallography.

PubMed

Chatake, Toshiyuki

2016-01-01

The hydration shells surrounding nucleic acids and hydrogen-bonding networks involving water molecules and nucleic acids are essential interactions for the structural stability and function of nucleic acids. Water molecules in the hydration shells influence various conformations of DNA and RNA by specific hydrogen-bonding networks, which often contribute to the chemical reactivity and molecular recognition of nucleic acids. However, X-ray crystallography could not provide a complete description of structural information with respect to hydrogen bonds. Indeed, X-ray crystallography is a powerful tool for determining the locations of water molecules, i.e., the location of the oxygen atom of H2O; however, it is very difficult to determine the orientation of the water molecules, i.e., the orientation of the two hydrogen atoms of H2O, because X-ray scattering from the hydrogen atom is very small.Neutron crystallography is a specialized tool for determining the positions of hydrogen atoms. Neutrons are not diffracted by electrons, but are diffracted by atomic nuclei; accordingly, neutron scattering lengths of hydrogen and its isotopes are comparable to those of non-hydrogen atoms. Therefore, neutron crystallography can determine both of the locations and orientations of water molecules. This chapter describes the current status of neutron nucleic acid crystallographic research as well as the basic principles of neutron diffraction experiments performed on nucleic acid crystals: materials, crystallization, diffraction experiments, and structure determination.

Orthodontic archwire composition and phase analyses by neutron spectroscopy.

PubMed

Tian, Kun V; Festa, Giulia; Basoli, Francesco; Laganà, Giuseppina; Scherillo, Antonella; Andreani, Carla; Bollero, Patrizio; Licoccia, Silvia; Senesi, Roberto; Cozza, Paola

2017-05-31

Quantitative metallurgical and phase analyses employing neutron diffraction technique were conducted on two as-received commercial rectangular austenitic stainless steel orthodontic archwires, G&H and Azdent, 0.43×0.64 mm (0.017×0.025 inch). Results showed a bi-phase structure containing martensitic phase (45.67% for G&H and 6.62% for Azdent) in addition to the expected metastable austenite. The former may be a strain-induced phase-transformation arising during the cold working process of wire fabrication. Further neutron resonance capture analysis determinations provided atomic and isotopic compositions, including alloying elements in each sample, complementary to the results of traditional energy dispersive X-ray spectroscopy. Together, these results assist in relating commercial alloying recipes and processing histories with mechanical performance, strength and ductility in particular.

Single phase Pb0.7Bi0.3Fe0.65Nb0.35O3 multiferroic: Neutron diffraction, impedance and modulus studies

NASA Astrophysics Data System (ADS)

Dadami, Sunanda T.; Matteppanvar, Shidaling; Shivaraja, I.; Rayaprol, Sudhindra; Deshpande, S. K.; Angadi, Basavaraj

2018-04-01

The Pb0.7Bi0.3Fe0.65Nb0.35O3 (PBFNO) multiferroic solid solution was synthesized by using single step solid state reaction method. Single phase formation was confirmed through room temperature (RT) X Ray Diffraction (XRD) and Neutron Diffraction (ND). Rietveld refinement was used to perform the structural analysis using FullProf Suite program. RT XRD and ND patterns well fitted with monoclinic structure (Cm space group) and cell parameters from the ND data are found to be a = 5.6474(4) Å, b = 5.6415(3) Å, c = 3.9992(3) Å and β = 89.95(2)°. ND data at RT exhibits G-type antiferromagnetic structure. The electrical properties (impedance and modulus) of PBFNO were studied as a function of frequency (100 Hz - 5 MHz) and temperature (133 K - 293 K) by Impedance spectroscopy technique. Impedance and modulus spectroscopy studies confirm the contribution to the conductivity is from grains only and the relaxation is of non-Debye type. The PBFNO sample exhibits negative temperature coefficient of resistance (NTCR) behaviour. PBFNO is found be a potential candidate for RT applications.

High temperature phase stability in Li{sub 0.12}Na{sub 0.88}NbO{sub 3}: A combined powder X-ray and neutron diffraction study

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

Mishra, S. K.; Krishna, P. S. R.; Shinde, A. B.

2015-09-07

The phase stabilities of ecofriendly piezoelectric material of lithium doped sodium niobate for composition Li{sub 0.12}Na{sub 0.88}NbO{sub 3} (LNN12) have been investigated by a combination of powder X-ray and neutron diffraction techniques in the temperature range of 300–1100 K. We observed interesting changes with appearance or disappearance of the super-lattice reflections in the powder diffraction patterns. Unambiguous experimental evidence is shown for coexistence of paraelectric and ferroelectric orthorhombic phases in the temperature range of 525 K to 675 K. We identified the correct crystal structure of LNN12 with temperature and correlated it with observed anomaly in the physical properties. Identification of crystal structuremore » also helps in the mode assignments in Raman and infrared spectroscopies. We argued that application of chemical pressure as a result of Li substitution in NaNbO{sub 3} matrix favors the freezing of zone centre phonons in contrast to the freezing of zone boundary phonons in pure NaNbO{sub 3} with the variation of temperature.« less

On the novel double perovskites A2Fe(Mn0.5W0.5)O6 (A= Ca, Sr, Ba). Structural evolution and magnetism from neutron diffraction data

NASA Astrophysics Data System (ADS)

García-Ramos, Crisanto A.; Larrégola, Sebastián; Retuerto, María; Fernández-Díaz, María Teresa; Krezhov, Kiril; Alonso, José Antonio

2018-06-01

New A2Fe(Mn0.5W0.5)O6 (A = Ca, Sr, Ba) double perovskite oxides have been prepared by ceramic techniques. X-ray diffraction (XRD) complemented with neutron powder diffraction (NPD) indicate a structural evolution from monoclinic (space group P21/n) for A = Ca to cubic (Fm-3m) for A = Sr and finally to hexagonal (P63/mmc) for A = Ba as the perovskite tolerance factor increases with the A2+ ionic size. The three oxides present different tilting schemes of the FeO6 and (Mn,W)O6 octahedra. NPD data also show evidence in all cases of a considerable anti-site disordering, involving the partial occupancy of Fe positions by Mn atoms, and vice-versa. Magnetic susceptibility data show magnetic transitions below 50 K characterized by a strong irreversibility between ZFC and FC susceptibility curves. The A = Ca perovskite shows a G-type magnetic structure, with weak ordered magnetic moments due to the mentioned antisite disordering. Interesting magnetostrictive effects are observed for the Sr perovskite below 10 K.

In situ investigation of deformation mechanisms in magnesium-based metal matrix composites

NASA Astrophysics Data System (ADS)

Farkas, Gergely; Choe, Heeman; Máthis, Kristián; Száraz, Zoltán; Noh, Yoonsook; Trojanová, Zuzanka; Minárik, Peter

2015-07-01

We studied the effect of short fibers on the mechanical properties of a magnesium alloy. In particular, deformation mechanisms in a Mg-Al-Sr alloy reinforced with short alumina fibers were studied in situ using neutron diffraction and acoustic emission methods. The fibers' plane orientation with respect to the loading axis was found to be a key parameter, which influences the acting deformation processes, such as twinning or dislocation slip. Furthermore, the twinning activity was much more significant in samples with parallel fiber plane orientation, which was confirmed by both acoustic emission and electron backscattering diffraction results. Neutron diffraction was also used to assist in analyzing the acoustic emission and electron backscattering diffraction results. The simultaneous application of the two in situ methods, neutron diffraction and acoustic emission, was found to be beneficial for obtaining complementary datasets about the twinning and dislocation slip in the magnesium alloys and composites used in this study.

Determination of atomic site susceptibility tensors from neutron diffraction data on polycrystalline samples.

PubMed

Gukasov, A; Brown, P J

2010-12-22

Polarized neutron diffraction can provide information about the atomic site susceptibility tensor χ(ij) 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 Tb(2)Sn(2)O(7).

Quantum model of catalysis based on a mobile proton revealed by subatomic x-ray and neutron diffraction studies of h-aldose reductase

PubMed Central

Blakeley, Matthew P.; Ruiz, Federico; Cachau, Raul; Hazemann, Isabelle; Meilleur, Flora; Mitschler, Andre; Ginell, Stephan; Afonine, Pavel; Ventura, Oscar N.; Cousido-Siah, Alexandra; Haertlein, Michael; Joachimiak, Andrzej; Myles, Dean; Podjarny, Alberto

2008-01-01

We present results of combined studies of the enzyme human aldose reductase (h-AR, 36 kDa) using single-crystal x-ray data (0.66 Å, 100K; 0.80 Å, 15K; 1.75 Å, 293K), neutron Laue data (2.2 Å, 293K), and quantum mechanical modeling. These complementary techniques unveil the internal organization and mobility of the hydrogen bond network that defines the properties of the catalytic engine, explaining how this promiscuous enzyme overcomes the simultaneous requirements of efficiency and promiscuity offering a general mechanistic view for this class of enzymes. PMID:18250329

Quantum model of catalysis based on a mobile proton revealed by subatomic x-ray and neutron diffraction studies of h-aldose reductase.

PubMed

Blakeley, Matthew P; Ruiz, Federico; Cachau, Raul; Hazemann, Isabelle; Meilleur, Flora; Mitschler, Andre; Ginell, Stephan; Afonine, Pavel; Ventura, Oscar N; Cousido-Siah, Alexandra; Haertlein, Michael; Joachimiak, Andrzej; Myles, Dean; Podjarny, Alberto

2008-02-12

We present results of combined studies of the enzyme human aldose reductase (h-AR, 36 kDa) using single-crystal x-ray data (0.66 A, 100K; 0.80 A, 15K; 1.75 A, 293K), neutron Laue data (2.2 A, 293K), and quantum mechanical modeling. These complementary techniques unveil the internal organization and mobility of the hydrogen bond network that defines the properties of the catalytic engine, explaining how this promiscuous enzyme overcomes the simultaneous requirements of efficiency and promiscuity offering a general mechanistic view for this class of enzymes.

Quantum Model of Catalysis Based on a Mobile Proton Revealed by Subatomic X-ray and Neutron Diffraction Studies of h-aldose Reductase

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

Blakeley, M. P.; Ruiz, Fredrico; Cachau, Raul

2008-01-01

We present results of combined studies of the enzyme human aldose reductase (h-AR, 36 kDa) using single-crystal x-ray data (0.66 Angstroms, 100K; 0.80 Angstroms, 15K; 1.75 Angstroms, 293K), neutron Laue data (2.2 Angstroms, 293K), and quantum mechanical modeling. These complementary techniques unveil the internal organization and mobility of the hydrogen bond network that defines the properties of the catalytic engine, explaining how this promiscuous enzyme overcomes the simultaneous requirements of efficiency and promiscuity offering a general mechanistic view for this class of enzymes.

Neutron diffraction study of Tb0.5Ho0.5Mn2Si2

NASA Astrophysics Data System (ADS)

Pandey, Swati; Siruguri, Vasudeva; Rawat, Rajeev

2018-02-01

The magnetic properties of tetragonal polycrystalline intermetallic compound Tb0.5Ho0.5Mn2Si2 have been investigated using temperature dependent dc magnetic susceptibility and neutron powder diffraction studies. Results of high temperature susceptibility data shows anomaly at TN = 510 K while low temperature susceptibility data indicate two successive anomalies at T1 = 11 K and T2 = 25 K. Metamagnetic transition is observed in magnetization versus field curves. Our neutron diffraction results indicate three different magnetic regions with different magnetic structures. Neutron diffraction data shows that below T2, the intensities of some of the nuclear peaks get enhanced indicating ferromagnetic ordering, while additional magnetic reflections are observed below T1, indicating antiferromagnetic order. Ordering of rare earth sublattice at low temperature rearranges the ordering of Mn sublattice and results in reorientation of Mn spins at T1. At 2 K Tb/Ho moments are aligned along c-axis while Mn moments are aligned perpendicular to c-axis.

Compositional Tuning, Crystal Growth, and Magnetic Properties of Iron Phosphate Oxide

NASA Astrophysics Data System (ADS)

Tarne, Michael

Iron phosphate oxide, Fe3PO4O 3, is a crystalline solid featuring magnetic Fe3+ ions on a complex lattice composed of closely-spaced triangles. Previous work from our research group on this compound has proposed a helical magnetic structure below T = 163 K attributed to J1 - J2 competing interactions between nearest-neighbor and next-nearest-neighbor iron atoms. This was based on neutron powder diffraction featuring unique broad, flat-topped magnetic reflections due to needle-like magnetic domains. In order to confirm the magnetic structure and origins of frustration, this thesis will expand upon the research focused on this compound. The first chapter focuses on single crystal growth of Fe3PO 4O3. While neutron powder diffraction provides insight to the magnetic structure, powder and domain averaging obfuscate a conclusive structure for Fe3PO4O3 and single crystal neutron scattering is necessary. Due to the incongruency of melting, single crystal growth has proven challenging. A number of techniques including flux growth, slow cooling, and optical floating zone growth were attempted and success has been achieved via heterogenous chemical vapor transport from FePO 4 using ZrCl4 as a transport agent. These crystals are of sufficient size for single crystal measurements on modern neutron diffractometers. Dilution of the magnetic sublattice in frustrated magnets can also provide insight into the nature of competing spin interactions. Dilution of the Fe 3+ lattice in Fe3PO4O3 is accomplished by substituting non-magnetic Ga3+ to form the solid solution series Fe3-xGaxPO4O3 with x = 0, 0.012, 0.06, 0.25, 0.5, 1.0, 1.5. The magnetic susceptibility and neutron powder diffraction data of these compounds are presented. A dramatic decrease of the both the helical pitch length and the domain size is observed with increasing x; for x > 0.5, the compounds lack long range magnetic order. The phases that do exhibit magnetic order show a decrease in helical pitch with increasing x as determined from the magnitude of the magnetic propagation vector. This trend can be qualitatively reproduced by increasing the ratio of J2/ J1 in the Heisenberg model. Intriguingly, the domain size extracted from peak broadening of the magnetic reflections is nearly equal to the pitch length for each value of x, which suggests that the two qualities are linked in this unusual antiferromagnet. The last chapter focuses on the oxyfluoride Fe3PO7-x Fx. Through fluorination using low-temperature chimie douce reactions with polytetrafluoroethylene, the magnetic properties show changes in the magnetic susceptibility, isothermal magnetization, and neutron powder diffraction. The magnetic susceptibility shows a peak near T = 13 K and a zero field cooled/field cooled splitting at T = 78 K. The broad, flat-topped magnetic reflections in the powder neutron diffraction exhibit a decrease in width and increase in intensity. The changes in the neutron powder diffraction suggest an increase in correlation length in the ab plane of the fluorinated compound. Iron phosphate oxide is a unique lattice showing a rich magnetic phase diagram in both the gallium-substituted and fluorinated species. While mean-field interactions are sufficient to describe interactions in the solid solution series Fe3-xGaxPO4O3, the additional magnetic transitions in Fe3PO7-xFx suggest a more complicated set of interactions.

Dynamic theory of neutron diffraction from a moving grating

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

Bushuev, V. A., E-mail: vabushuev@yandex.ru; Frank, A. I.; Kulin, G. V.

2016-01-15

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

New in-situ neutron diffraction cell for electrode materials

NASA Astrophysics Data System (ADS)

Biendicho, Jordi Jacas; Roberts, Matthew; Offer, Colin; Noréus, Dag; Widenkvist, Erika; Smith, Ronald I.; Svensson, Gunnar; Edström, Kristina; Norberg, Stefan T.; Eriksson, Sten G.; Hull, Stephen

2014-02-01

A novel neutron diffraction cell has been constructed to allow in-situ studies of the structural changes in materials of relevance to battery applications during charge/discharge cycling. The new design is based on the coin cell geometry, but has larger dimensions compared to typical commercial batteries in order to maximize the amount of electrode material and thus, collect diffraction data of good statistical quality within the shortest possible time. An important aspect of the design is its modular nature, allowing flexibility in both the materials studied and the battery configuration. This paper reports electrochemical tests using a Nickel-metal-hydride battery (Ni-MH), which show that the cell is able to deliver 90% of its theoretical capacity when using deuterated components. Neutron diffraction studies performed on the Polaris diffractometer using nickel metal and a hydrogen-absorbing alloy (MH) clearly show observable changes in the neutron diffraction patterns as a function of the discharge state. Due to the high quality of the diffraction patterns collected in-situ (i.e. good peak-to-background ratio), phase analysis and peak indexing can be performed successfully using data collected in around 30 min. In addition to this, structural parameters for the β-phase (charged) MH electrode obtained by Rietveld refinement are presented.

Neutron diffraction measurements on a reference metallic sample with a high-efficiency GEM side-on 10B-based thermal neutron detector

NASA Astrophysics Data System (ADS)

Pietropaolo, A.; Claps, G.; Fedrigo, A.; Grazzi, F.; Höglund, C.; Murtas, F.; Scherillo, A.; Schmidt, S.; Schooneveld, E. M.

2018-03-01

The upgraded version of the GEM side-on thermal neutron detector was successfully tested in a neutron diffraction experiment on a reference sample using the INES diffractometer at the ISIS spallation neutron source, UK. The performance of the new 10B4C-based detector is compared to that of a standard 3He tube, operating at the instrument as a part of the detectors assembly. The results show that the upgraded detector has a better resolution and an efficiency of the same order of magnitude of a 3He-based detector.

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl(6) and other alloys are twinned cubic crystals.

PubMed

Pauling, L

1987-06-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl(6) and Mg(32)(Al,Zn)(49) and the neutron powder diffraction pattern of MnAl(6) are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl(6) and 24.313 A (x-ray) for Mg(32)(Al,Zn)(49).

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl6 and other alloys are twinned cubic crystals

PubMed Central

Pauling, Linus

1987-01-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl6 and Mg32(Al,Zn)49 and the neutron powder diffraction pattern of MnAl6 are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 Å (x-ray) and 23.416 Å (neutron) for MnAl6 and 24.313 Å (x-ray) for Mg32(Al,Zn)49. PMID:16593841

Examination of Short- and Long-Range Atomic Order Nanocrystalline SiC and Diamond by Powder Diffraction Methods

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Gierlotka, S.; Weber, H.-P.; Proffen, T.; Palosz, W.

2002-01-01

The real atomic structure of nanocrystals determines unique, key properties of the materials. Determination of the structure presents a challenge due to inherent limitations of standard powder diffraction techniques when applied to nanocrystals. Alternate methodology of the structural analysis of nanocrystals (several nanometers in size) based on Bragg-like scattering and called the "apparent lattice parameter" (alp) is proposed. Application of the alp methodology to examination of the core-shell model of nanocrystals will be presented. The results of application of the alp method to structural analysis of several nanopowders were complemented by those obtained by determination of the Atomic Pair Distribution Function, PDF. Based on synchrotron and neutron diffraction data measured in a large diffraction vector of up to Q = 25 Angstroms(exp -1), the surface stresses in nanocrystalline diamond and SiC were evaluated.

Residual strain mapping of Roman styli from Iulia Concordia, Italy

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

Salvemini, Filomena, E-mail: floriana.salvemini@fi.isc.cnr.it; Università degli Studi di Firenze, Dipartimento di Scienze della Terra; Grazzi, Francesco

Iulia Concordia is an important Roman settlement known for the production of iron objects and weapons during the Roman Empire. A huge number of well-preserved styli were found in the past century in the bed of an old channel. In order to shed light about the production processes used by Roman for stylus manufacturing, a neutron diffraction residual strain analysis was performed on the POLDI materials science diffractometer at the Paul Scherrer Institut in Switzerland. Here, we present results from our investigation conducted on 11 samples, allowing to define, in a non-invasive way, the residual strain map related to themore » ancient Roman working techniques. - Highlights: • We examined 11 Roman styli from the settlement of Iulia Concordia, Italy. • We performed a neutron diffraction residual strain analysis on POLDI at PSI (CH). • We identified the production processes used by Roman for stylus manufacturing. • We clarified the way and direction of working applied for different classes of styli.« less

Residual Stress Analysis in Girth-welded Ferritic and Austenitic Steel Pipes Using Neutron and X-Ray Diffraction

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

Hempel, Nico; Bunn, Jeffrey R; Nitschke-Pagel, Thomas

This paper is dedicated to the thorough experimental analysis of the residual stresses in the vicinity of tubular welds and the mechanisms involved in their formation. Pipes made of a ferritic-pearlitic structural steel and an austenitic stainless steel are investigated in this study. The pipes feature a similar geometry and are MAG welded with two passes and comparable parameters. Residual strain mappings are carried out using X-ray and neutron diffraction. The combined use of both techniques permits both near-surface and through-wall analyses of the residual stresses. The findings allow for a consistent interpretation of the mechanisms accounting for the formationmore » of the residual stress fields due to the welding process. Since the results are similar for both materials, it can be concluded that residual stresses induced by phase transformations, which can occur in the structural steel, play a minor role in this regard.« less

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 will present the details of our DAC preparations and results of our in-situ structural refinements of dhcp-FeHx up to ~50 GPa. Together with previous investigations of the thermoelastic and electronic properties of FeHx [2; 6], we will discuss implications for the composition of Earth's iron-rich core. References: 1. N. Hirao et al. (2004), Geophys. Res. Lett., 31, L06616, doi:10.1029/2003GL019380. 2. W.L. Mao et al. (2004), Geophys. Res. Lett., 31, L15618, doi:10.1029/2004GL020541. 3. V.E. Antonov et al. (2002), J. Phys.: Condens. Matter, 14, 6427-6445, doi:10.1088/0953-8984/14/25/311. 4. M. Guthrie et al. (2013), ACA Transactions, 44, in press. 5. R. Boehler et al. (2013), High Press. Res., in press, doi:10.1080/08957959.2013.823197. 6. Y. Shibazaki et al. (2012), Earth Planet. Sci. Lett., 313-314, 79-85, doi:10.1016/j.epsl.2011.11.002.

Lattice strain measurements on sandstones under load using neutron diffraction

NASA Astrophysics Data System (ADS)

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

2000-11-01

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

The use of neutron scattering to determine the functional structure of glycoside hydrolase.

PubMed

Nakamura, Akihiko; Ishida, Takuya; Samejima, Masahiro; Igarashi, Kiyohiko

2016-10-01

Neutron diffraction provides different information from X-ray diffraction, because neutrons are scattered by atomic nuclei, whereas X-rays are scattered by electrons. One of the key advantages of neutron crystallography is the ability to visualize hydrogen and deuterium atoms, making it possible to observe the protonation state of amino acid residues, hydrogen bonds, networks of water molecules and proton relay pathways in enzymes. But, because of technical difficulties, less than 100 enzyme structures have been evaluated by neutron crystallography to date. In this review, we discuss the advantages and disadvantages of neutron crystallography as a tool to investigate the functional structure of glycoside hydrolases, with some examples. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

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

Sano-Furukawa, A., E-mail: sano.asami@jaea.go.jp; Hattori, T.; J-PARC Center, Japan Atomic Energy Agency, Ibaraki 319-1195

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 themore » 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.« less

A Novel In-situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes of Li-ion Batteries

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

Vadlamani, Bhaskar S; An, Ke; Jagannathan, M.

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 hasmore » 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.« less

Time-resolved in situ neutron diffraction under supercritical hydrothermal conditions: a study of the synthesis of KTiOPO4.

PubMed

Ok, Kang Min; Lee, Dong Woo; Smith, Ronald I; O'Hare, Dermot

2012-10-31

In the first in situ neutron powder diffraction study of a supercritical hydrothermal synthesis, the crystallization of KTiOPO(4) (KTP) at 450 °C and 380 bar has been investigated. The time-resolved diffraction data suggest that the crystallization of KTP occurs by the reaction between dissolved K(+)(aq), PO(4)(3-)(aq), and [Ti(OH)(x)]((4-x)+)(aq) species.

Interpretation of small-angle diffraction experiments on opal-like photonic crystals

NASA Astrophysics Data System (ADS)

Marlow, F.; Muldarisnur, M.; Sharifi, P.; Zabel, H.

2011-08-01

Comprehensive structural information on artificial opals involving the deviations from the strongly dominating face-centered cubic structure is still missing. Recent structure investigations with neutrons and synchrotron sources have shown a high degree of order but also a number of unexpected scattering features. Here, we point out that the exclusion of the allowed 002-type diffraction peaks by a small atomic form factor is not obvious and that surface scattering has to be included as a possible source for the diffraction peaks. Our neutron diffraction data indicate that surface scattering is the main reason for the smallest-angle peaks in the diffraction patterns.

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.

Absolute configuration of a chiral CHD group via neutron diffraction: confirmation of the absolute stereochemistry of the enzymatic formation of malic acid

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

Bau, R.; Brewer, I.; Chiang, M.Y.

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.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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.

Defect ordering in YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6: Synthesis and characterization by neutron and electron diffraction

NASA Astrophysics Data System (ADS)

Lin, Y. P.; Greedan, J. E.; O'Reilly, A. H.; Reimers, J. N.; Stager, C. V.; Post, M. L.

1990-02-01

Polycrystalline samples of YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6 were prepared by oxygen titration of YBa 2 Cu 3O 6.0 at 450°C followed by slow cooling to room temperature. Both samples showed evidence for the a' = 2a supercell in individual grains by electron diffraction as reported previously. In addition the superlattice was observed in neutron powder diffraction indicating that the bulk material is also well ordered. In this study the YBa 2Cu 3O 6.6 phase showed longer correlation lengths for ordering along both a* and b* than YBa 2Cu 3O 6.5. For the former compound the powder-averaged, sample-averaged a* correlation distance is 26A˚from neutron diffraction. Analysis of electron diffraction profiles on selected single crystals give correlation lengths along a*, b*, and c* of 100, 200, and 50A˚, respectively. Dark field imaging discloses the presence of striped, ordered domains elongated along b* with a distribution of sizes. Both neutron diffraction and dark field imaging indicate that the volume fraction of the ordered domains is about 50%. A correlation is noted between the Meissner Effect and the extent of defect ordering in the bulk samples of the two phases.

Neutron detection by scintillation of noble-gas excimers

NASA Astrophysics Data System (ADS)

McComb, Jacob Collin

Neutron detection is a technique essential to homeland security, nuclear reactor instrumentation, neutron diffraction science, oil-well logging, particle physics and radiation safety. The current shortage of helium-3, the neutron absorber used in most gas-filled proportional counters, has created a strong incentive to develop alternate methods of neutron detection. Excimer-based neutron detection (END) provides an alternative with many attractive properties. Like proportional counters, END relies on the conversion of a neutron into energetic charged particles, through an exothermic capture reaction with a neutron absorbing nucleus (10B, 6Li, 3He). As charged particles from these reactions lose energy in a surrounding gas, they cause electron excitation and ionization. Whereas most gas-filled detectors collect ionized charge to form a signal, END depends on the formation of diatomic noble-gas excimers (Ar*2, Kr*2,Xe* 2) . Upon decaying, excimers emit far-ultraviolet (FUV) photons, which may be collected by a photomultiplier tube or other photon detector. This phenomenon provides a means of neutron detection with a number of advantages over traditional methods. This thesis investigates excimer scintillation yield from the heavy noble gases following the boron-neutron capture reaction in 10B thin-film targets. Additionally, the thesis examines noble-gas excimer lifetimes with relationship to gas type and gas pressure. Experimental data were collected both at the National Institute of Standards and Technology (NIST) Center for Neutron Research, and on a newly developed neutron beamline at the Maryland University Training Reactor. The components of the experiment were calibrated at NIST and the University of Maryland, using FUV synchrotron radiation, neutron imaging, and foil activation techniques, among others. Computer modeling was employed to simulate charged-particle transport and excimer photon emission within the experimental apparatus. The observed excimer scintillation yields from the 10B( n, alpha)7Li reaction are comparable to the yields of many liquid and solid neutron scintillators. Additionally, the observed slow triplet-state decay of neutron-capture-induced excimers may be used in a practical detector to discriminate neutron interactions from gamma-ray interactions. The results of these measurements and simulations will contribute to the development and optimization of a deployable neutron detector based on noble-gas excimer scintillation.

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Phase Concentration Determination of Fe 16N 2 Using State of the Art Neutron Scattering Techniques

DOE PAGES

Bennett, S. P.; Feygenson, M.; Jiang, Y.; ...

2016-03-25

Limitation on the availability of rare earth elements have made it imperative that new high energy product rare earth free permanent magnet materials are developed for the next generation of energy systems. One promising low cost permanent magnet candidate for a high energy magnet is -Fe 16N 2, whose giant magnetic moment has been predicted to be well above any other from conventional first principles calculations. Despite its great promise, the phase is metastable; making synthesis of the pure phase difficult, resulting in less than ideal magnetic characteristics. This instability gives way to a slew of possible secondary phases (i.e.more » -Fe, Fe 2O 3, Fe 8N, Fe 4N ) whose concentrations are difficult to detect by conventional x-ray diffraction. Moreover, we show how high resolution neutron diffraction and polarized neutron reflectometry can be used to extract the phase concentration ratio of the giant magnetic phase from ultra-small powder sample sizes (~0.1g) and thin films. These studies have led to the discovery of promising fabrication methods for both homogeneous thin films, and nanopowders containing the highest reported to date (>95%) phase concentrations of room temperature stable -Fe 16N 2.« less

Polarized single crystal neutron diffraction study of the zero-magnetization ferromagnet Sm1 -xGdxAl2 (x =0.024 )

NASA Astrophysics Data System (ADS)

Chatterji, T.; Stunault, A.; Brown, P. J.

2018-02-01

We have determined the temperature evolution of the spin and orbital moments in the zero-magnetization ferromagnet Sm1 -xGdxAl2 (x = 0.024) by combining polarized and unpolarized single crystal neutron diffraction data. The sensitivity of the polarized neutron technique has allowed the moment values to be determined with a precision of ≈0.1 μB . Our results clearly demonstrate that, when magnetized by a field of 8 T, the spin and orbital moments in Sm1 -xGdxAl2 are oppositely directed, so that the net magnetization is very small. Below 60 K the contributions from spin and orbital motions are both about 2 μB , with that due to orbital motion being slightly larger than that due to spin. Between 60 and 65 K the contributions of each to the magnetization fall rapidly and change sign at Tcomp ≈67 K , above which the aligned moments recover but with the orbital magnetization still slightly higher than the spin one. These results imply that above Tcomp the small resultant magnetization of the Sm3 + ion is oppositely directed to the magnetizing field. It is suggested that this anomaly is due to polarization of conduction electron spin associated with the doping Gd3 + ions.

Performance improvements of wavelength-shifting-fiber neutron detectors using high-resolution positioning algorithms

DOE PAGES

Wang, C. L.

2016-05-17

On the basis of FluoroBancroft linear-algebraic method [S.B. Andersson, Opt. Exp. 16, 18714 (2008)] three highly-resolved positioning methods were proposed for wavelength-shifting fiber (WLSF) neutron detectors. Using a Gaussian or exponential-decay light-response function (LRF), the non-linear relation of photon-number profiles vs. x-pixels was linearized and neutron positions were determined. The proposed algorithms give an average 0.03-0.08 pixel position error, much smaller than that (0.29 pixel) from a traditional maximum photon algorithm (MPA). The new algorithms result in better detector uniformity, less position misassignment (ghosting), better spatial resolution, and an equivalent or better instrument resolution in powder diffraction than the MPA.more » Moreover, these characters will facilitate broader applications of WLSF detectors at time-of-flight neutron powder diffraction beamlines, including single-crystal diffraction and texture analysis.« less

New large volume hydrothermal reaction cell for studying chemical processes under supercritical hydrothermal conditions using time-resolved in situ neutron diffraction.

PubMed

Ok, Kang Min; O'Hare, Dermot; Smith, Ronald I; Chowdhury, Mohammed; Fikremariam, Hanna

2010-12-01

The design and testing of a new large volume Inconel pressure cell for the in situ study of supercritical hydrothermal syntheses using time-resolved neutron diffraction is introduced for the first time. The commissioning of this new cell is demonstrated by the measurement of the time-of-flight neutron diffraction pattern for TiO(2) (Anatase) in supercritical D(2)O on the POLARIS diffractometer at the United Kingdom's pulsed spallation neutron source, ISIS, Rutherford Appleton Laboratory. The sample can be studied over a wide range of temperatures (25-450 °C) and pressures (1-355 bar). This novel apparatus will now enable us to study the kinetics and mechanisms of chemical syntheses under extreme environments such as supercritical water, and in particular to study the crystallization of a variety of technologically important inorganic materials.

Neutron residual stress measurements on rail sections for different production conditions

DOT National Transportation Integrated Search

2004-11-13

Rail sectioning with subsequent neutron diffraction experiments has been used to assess residual stresses in the rails. In this study we present the results of neutron stress : measurements performed at the NIST Center for Neutron Research (NCNR) on ...

Aging effects in bulk and fiber TlBr-TlI

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

Wysocki, J.A.; Wilson, R.G.; Standlee, A.G.

1988-05-01

A study of optical aging in bulk and extruded fibers of thallium bromo-iodide (TlBr-TlI) is presented. A variety of techniques including secondary ion mass spectrometry (SIMS), powder neutron and x-ray diffraction, infrared spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy are used to probe the chemical and structural properties of both pristine and aged material. High concentration levels of a hydrogen bearing impurity have been detected by SIMS and neutron scattering in aged TlBr-TlI, and have been shown to be localized in the surface layers of fibers as well as bulk samples. We present EPR evidence which indicates that the hydrogenmore » bearing impurity is water.« less

Liquid Alumina: Detailed Atomic Coordination Determined from Neutron Diffraction Data Using Empirical Potential Structure Refinement

NASA Astrophysics Data System (ADS)

Landron, C.; Hennet, L.; Jenkins, T. E.; Greaves, G. N.; Coutures, J. P.; Soper, A. K.

2001-05-01

The neutron scattering structure factor SN\\(Q\\) for a 40 mg drop of molten alumina ( Al2O3) held at 2500 K, using a laser-heated aerodynamic levitation furnace, is measured for the first time. A 1700 atom model of liquid alumina is generated from these data using the technique of empirical potential structural refinement. About 62% of the aluminum sites are 4-fold coordinated, matching the mostly triply coordinated oxygen sites, but some 24% of the aluminum sites are 5-fold coordinated. The octahedral aluminum sites found in crystalline α-Al2O3 occur only at the 2% level in liquid alumina.

Spatially resolved texture and microstructure evolution of additively manufactured and gas gun deformed 304L stainless steel investigated by neutron diffraction and electron backscatter diffraction

DOE PAGES

Takajo, Shigehiro; Brown, Donald William; Clausen, Bjorn; ...

2018-04-30

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residualmore » strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. We found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. In conclusion, knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.« less

Spatially resolved texture and microstructure evolution of additively manufactured and gas gun deformed 304L stainless steel investigated by neutron diffraction and electron backscatter diffraction

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

Takajo, Shigehiro; Brown, Donald William; Clausen, Bjorn

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residualmore » strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. We found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. In conclusion, knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.« less

Magnetic ground state of the multiferroic hexagonal LuFe O3

NASA Astrophysics Data System (ADS)

Suresh, Pittala; Vijaya Laxmi, K.; Bera, A. K.; Yusuf, S. M.; Chittari, Bheema Lingam; Jung, Jeil; Anil Kumar, P. S.

2018-05-01

The structural, electric, and magnetic properties of bulk hexagonal LuFe O3 are investigated. Single phase hexagonal LuFe O3 has been successfully stabilized in the bulk form without any doping by sol-gel method. The hexagonal crystal structure with P 63c m space group has been confirmed by x-ray-diffraction, neutron-diffraction, and Raman spectroscopy study at room temperature. Neutron diffraction confirms the hexagonal phase of LuFe O3 persists down to 6 K. Further, the x-ray photoelectron spectroscopy established the 3+ oxidation state of Fe ions. The temperature-dependent magnetic dc susceptibility, specific heat, and neutron-diffraction studies confirm an antiferromagnetic ordering below the Néel temperature (TN)˜130 K . Analysis of magnetic neutron-diffraction patterns reveals an in-plane (a b -plane) 120∘ antiferromagnetic structure, characterized by a propagation vector k =(0 0 0 ) with an ordered moment of 2.84 μB/F e3 + at 6 K. The 120∘ antifferomagnetic ordering is further confirmed by spin-orbit coupling density functional theory calculations. The on-site coulomb interaction (U ) and Hund's parameter (JH) on Fe atoms reproduced the neutron-diffraction Γ1 spin pattern among the Fe atoms. P -E loop measurements at room temperature confirm an intrinsic ferroelectricity of the sample with remnant polarization Pr˜0.18 μ C /c m2 . A clear anomaly in the dielectric data is observed at ˜TN revealing the presence of magnetoelectric coupling. A change in the lattice constants at TN has also been found, indicating the presence of a strong magnetoelastic coupling. Thus a coupling between lattice, electric, and magnetic degrees of freedom is established in bulk hexagonal LuFe O3 .

Structural and physical property study of sol-gel synthesized CoFe2-xHoxO4 nano ferrites

NASA Astrophysics Data System (ADS)

Patankar, K. K.; Ghone, D. M.; Mathe, V. L.; Kaushik, S. D.

2018-05-01

CoFe2-xHoxO4 (x = 0.00, 0.05, 0.10, 0.15, 0.20) ferrites were prepared by the suitably modified Sol-Gel technique. X-ray diffraction (XRD) analysis revealed that the substituted samples show phase pure formation till 10% substitution, which is far higher phase pure than the earlier reports. Upon further substitution an inevitable secondary phase of HoFeO3 along with the spinel phase despite regulating synthesis parameters in the sol-gel reaction route. These results are further corroborated more convincingly by room temperature neutron diffraction. Morphological features of the ferrites were studied by Scanning Electron Microscopy (SEM). The magnetic parameters viz. the saturation magnetization (Ms), coercivity (Hc) and remanence (Mr) were determined from room temperature isothermal magnetization. These parameters were found to decrease with increase in Ho substitution. The decrease in magnetization is analyzed in the light of exchange interactions between rare earth and transition metal ions. Magnetostriction measurements revealed interesting results and the presence of a secondary phase was found to be responsible for decreased measu-red magnetostriction values. The solubility limit of Ho in CoFe2O4 lattice is also reflected from the X-ray and neutron diffraction analysis and magnetostriction studies.

Structural characterization and aging of glassy pharmaceuticals made using acoustic levitation.

PubMed

Benmore, Chris J; Weber, J K R; Tailor, Amit N; Cherry, Brian R; Yarger, Jeffery L; Mou, Qiushi; Weber, Warner; Neuefeind, Joerg; Byrn, Stephen R

2013-04-01

Here, we report the structural characterization of several amorphous drugs made using the method of quenching molten droplets suspended in an acoustic levitator. (13) C NMR, X-ray, and neutron diffraction results are discussed for glassy cinnarizine, carbamazepine, miconazole nitrate, probucol, and clotrimazole. The (13) C NMR results did not find any change in chemical bonding induced by the amorphization process. High-energy X-ray diffraction results were used to characterize the ratio of crystalline to amorphous material present in the glasses over a period of 8 months. All the glasses were stable for at least 6 months except carbamazepine, which has a strong tendency to crystallize within a few months. Neutron and X-ray pair distribution function analyses were applied to the glassy materials, and the results were compared with their crystalline counterparts. The two diffraction techniques yielded similar results in most cases and identified distinct intramolecular and intermolecular correlations. The intramolecular scattering was calculated based on the crystal structure and fit to the measured X-ray structure factor. The resulting intermolecular pair distribution functions revealed broad-nearest and next-nearest neighbor molecule-molecule correlations. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:1290-1300, 2013. Copyright © 2013 Wiley Periodicals, Inc.

In Situ Powder Diffraction Studies of Electrode Materials in Rechargeable Batteries.

PubMed

Sharma, Neeraj; Pang, Wei Kong; Guo, Zaiping; Peterson, Vanessa K

2015-09-07

The ability to directly track the charge carrier in a battery as it inserts/extracts from an electrode during charge/discharge provides unparalleled insight for researchers into the working mechanism of the device. This crystallographic-electrochemical information can be used to design new materials or modify electrochemical conditions to improve battery performance characteristics, such as lifetime. Critical to collecting operando data used to obtain such information in situ while a battery functions are X-ray and neutron diffractometers with sufficient spatial and temporal resolution to capture complex and subtle structural changes. The number of operando battery experiments has dramatically increased in recent years, particularly those involving neutron powder diffraction. Herein, the importance of structure-property relationships to understanding battery function, why in situ experimentation is critical to this, and the types of experiments and electrochemical cells required to obtain such information are described. For each battery type, selected research that showcases the power of in situ and operando diffraction experiments to understand battery function is highlighted and future opportunities for such experiments are discussed. The intention is to encourage researchers to use in situ and operando techniques and to provide a concise overview of this area of research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Shining a light on Jarosite: formation, alteration and stability studies using in situ experimental synchrotron and neutron techniques.

NASA Astrophysics Data System (ADS)

Brand, H. E. A.; Scarlett, N. V. Y.; Wilson, S. A.; Frierdich, A. J.; Grey, I. E.

2016-12-01

Jarosites and related minerals are critical to a range of mineral processing and research applications. They are used in the removal of iron species from smelting processes; they occur in metal bioleaching systems, and they are present in acid mine drainage environments. There has been a recent resurgence in interest in jarosites since their detection on Mars. In this context, the presence of jarosite has been recognised as a likely indicator of liquid water at the surface of Mars in the past & it is thought that their study will provide insight into the environmental history of Mars. Acid sulfate soils cover large areas of the Australian coastline and are likely to be a major constituent of the Martian environment. The oxidation of acid sulfate soils, coupled with potential release of heavy metals and acidic groundwaters, can have serious consequences for fragile ecosystems. Understanding these sediments will provide insight into the biogeochemical processes that affect the lifetimes of transient mineral species on Earth, and may be used to better understand soil acidification, contaminant mobility at sites affected by acid and metalliferous drainage, and even constrain past weathering and putative biosignatures on Mars. Knowledge of the behaviour of jarosite minerals under the actual conditions that they are found in is crucial to understanding their potential environmental impacts on both Earth and Mars. To this end, we are engaged in a program to study the formation, stability and alteration of natural and synthetic jarosite minerals using a complementary suite of in situ synchrotron and neutron techniques. There are 3 sections to this work that will introduce the experimental techniques and sample environments that make these measurements possible: Studying the nucleation and growth of jarosites under laboratory conditions. The experimentation consisted of time-resolved synchrotron small angle X-ray scattering and X-ray diffraction. Studying the stability of natural & synthetic jarosites with temperature and pressure using synchrotron and neutron diffraction. Parallel neutron and X-ray imaging at OPAL and the Australian Synchrotron, combined with synchrotron pseudo-microdiffraction to map the mineralogy and structural relationships within naturally occurring jarosite nodules.

In-situ neutron diffraction study on the tension-compression fatigue behavior of a twinning induced plasticity steel

DOE PAGES

Xie, Qingge; Liang, Jiangtao; Stoica, Alexandru Dan; ...

2017-05-17

Grain orientation dependent behavior during tension-compression type of fatigue loading in a TWIP steel was studied using in-situ neutron diffraction. Orientation zones with dominant behavior of (1) twinning-de-twinning, (2) twinning-re-twinning followed by twinning-de-twinning, (3) twinning followed by dislocation slip and (4) dislocation slip were identified. Jumps of the orientation density were evidenced in neutron diffraction peaks which explains the macroscopic asymmetric behavior. The asymmetric behavior in early stage of fatigue loading is mainly due to small volume fraction of twins in comparison with that at later stage. As a result, easy activation of the de-twin makes the macroscopically unloading behaviormore » nonlinear.« less

In-situ neutron diffraction study on the tension-compression fatigue behavior of a twinning induced plasticity steel

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

Xie, Qingge; Liang, Jiangtao; Stoica, Alexandru Dan

Grain orientation dependent behavior during tension-compression type of fatigue loading in a TWIP steel was studied using in-situ neutron diffraction. Orientation zones with dominant behavior of (1) twinning-de-twinning, (2) twinning-re-twinning followed by twinning-de-twinning, (3) twinning followed by dislocation slip and (4) dislocation slip were identified. Jumps of the orientation density were evidenced in neutron diffraction peaks which explains the macroscopic asymmetric behavior. The asymmetric behavior in early stage of fatigue loading is mainly due to small volume fraction of twins in comparison with that at later stage. As a result, easy activation of the de-twin makes the macroscopically unloading behaviormore » nonlinear.« less

Neutron and high-resolution room-temperature X-ray data collection from crystallized lytic polysaccharide monooxygenase

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

Bacik, John -Paul; Mekasha, Sophanit; Forsberg, Zarah

Bacteria and fungi express lytic polysaccharide monooxgyenase (LPMO) enzymes that act in conjunction with canonical hydrolytic sugar-processing enzymes to rapidly convert polysaccharides such as chitin, cellulose and starch to single monosaccharide products. In order to gain a better understanding of the structure and oxidative mechanism of these enzymes, large crystals (1–3 mm 3) of a chitin-processing LPMO from the Gram-positive soil bacterium Jonesia denitrificans were grown and screened for their ability to diffract neutrons. In addition to the collection of neutron diffraction data, which were processed to 2.1 Å resolution, a high-resolution room-temperature X-ray diffraction data set was collected andmore » processed to 1.1 Å resolution in space group P2 12 12 1. To our knowledge, this work marks the first successful neutron crystallographic experiment on an LPMO. As a result, joint X-ray/neutron refinement of the resulting data will reveal new details of the structure and mechanism of this recently discovered class of enzymes.« less

Neutron and high-resolution room-temperature X-ray data collection from crystallized lytic polysaccharide monooxygenase

DOE PAGES

Bacik, John -Paul; Mekasha, Sophanit; Forsberg, Zarah; ...

2015-01-01

Bacteria and fungi express lytic polysaccharide monooxgyenase (LPMO) enzymes that act in conjunction with canonical hydrolytic sugar-processing enzymes to rapidly convert polysaccharides such as chitin, cellulose and starch to single monosaccharide products. In order to gain a better understanding of the structure and oxidative mechanism of these enzymes, large crystals (1–3 mm 3) of a chitin-processing LPMO from the Gram-positive soil bacterium Jonesia denitrificans were grown and screened for their ability to diffract neutrons. In addition to the collection of neutron diffraction data, which were processed to 2.1 Å resolution, a high-resolution room-temperature X-ray diffraction data set was collected andmore » processed to 1.1 Å resolution in space group P2 12 12 1. To our knowledge, this work marks the first successful neutron crystallographic experiment on an LPMO. As a result, joint X-ray/neutron refinement of the resulting data will reveal new details of the structure and mechanism of this recently discovered class of enzymes.« less

Structure determination of Ba5AlF13 by coupling electron, synchrotron and neutron powder diffraction, solid-state NMR and ab initio calculations.

PubMed

Martineau, Charlotte; Allix, Mathieu; Suchomel, Matthew R; Porcher, Florence; Vivet, François; Legein, Christophe; Body, Monique; Massiot, Dominique; Taulelle, Francis; Fayon, Franck

2016-10-04

The room temperature structure of Ba 5 AlF 13 has been investigated by coupling electron, synchrotron and neutron powder diffraction, solid-state high-resolution NMR ( 19 F and 27 Al) and first principles calculations. An initial structural model has been obtained from electron and synchrotron powder diffraction data, and its main features have been confirmed by one- and two-dimensional NMR measurements. However, DFT GIPAW calculations of the 19 F isotropic shieldings revealed an inaccurate location of one fluorine site (F3, site 8a), which exhibited unusual long F-Ba distances. The atomic arrangement was reinvestigated using neutron powder diffraction data. Subsequent Fourier maps showed that this fluorine atom occupies a crystallographic site of lower symmetry (32e) with partial occupancy (25%). GIPAW computations of the NMR parameters validate the refined structural model, ruling out the presence of local static disorder and indicating that the partial occupancy of this F site reflects a local motional process. Visualisation of the dynamic process was then obtained from the Rietveld refinement of neutron diffraction data using an anharmonic description of the displacement parameters to account for the thermal motion of the mobile fluorine. The whole ensemble of powder diffraction and NMR data, coupled with first principles calculations, allowed drawing an accurate structural model of Ba 5 AlF 13 , including site-specific dynamical disorder in the fluorine sub-network.

Probing the accuracy and precision of Hirshfeld atom refinement with HARt interfaced with Olex2.

PubMed

Fugel, Malte; Jayatilaka, Dylan; Hupf, Emanuel; Overgaard, Jacob; Hathwar, Venkatesha R; Macchi, Piero; Turner, Michael J; Howard, Judith A K; Dolomanov, Oleg V; Puschmann, Horst; Iversen, Bo B; Bürgi, Hans-Beat; Grabowsky, Simon

2018-01-01

Hirshfeld atom refinement (HAR) is a novel X-ray structure refinement technique that employs aspherical atomic scattering factors obtained from stockholder partitioning of a theoretically determined tailor-made static electron density. HAR overcomes many of the known limitations of independent atom modelling (IAM), such as too short element-hydrogen distances, r ( X -H), or too large atomic displacement parameters (ADPs). This study probes the accuracy and precision of anisotropic hydrogen and non-hydrogen ADPs and of r ( X -H) values obtained from HAR. These quantities are compared and found to agree with those obtained from (i) accurate neutron diffraction data measured at the same temperatures as the X-ray data and (ii) multipole modelling (MM), an established alternative method for interpreting X-ray diffraction data with the help of aspherical atomic scattering factors. Results are presented for three chemically different systems: the aromatic hydro-carbon rubrene (orthorhombic 5,6,11,12-tetra-phenyl-tetracene), a co-crystal of zwitterionic betaine, imidazolium cations and picrate anions (BIPa), and the salt potassium hydrogen oxalate (KHOx). The non-hydrogen HAR-ADPs are as accurate and precise as the MM-ADPs. Both show excellent agreement with the neutron-based values and are superior to IAM-ADPs. The anisotropic hydrogen HAR-ADPs show a somewhat larger deviation from neutron-based values than the hydrogen SHADE-ADPs used in MM. Element-hydrogen bond lengths from HAR are in excellent agreement with those obtained from neutron diffraction experiments, although they are somewhat less precise. The residual density contour maps after HAR show fewer features than those after MM. Calculating the static electron density with the def2-TZVP basis set instead of the simpler def2-SVP one does not improve the refinement results significantly. All HARs were performed within the recently introduced HARt option implemented in the Olex2 program. They are easily launched inside its graphical user interface following a conventional IAM.

Probing the accuracy and precision of Hirshfeld atom refinement with HARt interfaced with Olex2

PubMed Central

Fugel, Malte; Hathwar, Venkatesha R.; Turner, Michael J.; Howard, Judith A. K.

2018-01-01

Hirshfeld atom refinement (HAR) is a novel X-ray structure refinement technique that employs aspherical atomic scattering factors obtained from stockholder partitioning of a theoretically determined tailor-made static electron density. HAR overcomes many of the known limitations of independent atom modelling (IAM), such as too short element–hydrogen distances, r(X—H), or too large atomic displacement parameters (ADPs). This study probes the accuracy and precision of anisotropic hydrogen and non-hydrogen ADPs and of r(X—H) values obtained from HAR. These quantities are compared and found to agree with those obtained from (i) accurate neutron diffraction data measured at the same temperatures as the X-ray data and (ii) multipole modelling (MM), an established alternative method for interpreting X-ray diffraction data with the help of aspherical atomic scattering factors. Results are presented for three chemically different systems: the aromatic hydro­carbon rubrene (orthorhombic 5,6,11,12-tetra­phenyl­tetracene), a co-crystal of zwitterionic betaine, imidazolium cations and picrate anions (BIPa), and the salt potassium hydrogen oxalate (KHOx). The non-hydrogen HAR-ADPs are as accurate and precise as the MM-ADPs. Both show excellent agreement with the neutron-based values and are superior to IAM-ADPs. The anisotropic hydrogen HAR-ADPs show a somewhat larger deviation from neutron-based values than the hydrogen SHADE-ADPs used in MM. Element–hydrogen bond lengths from HAR are in excellent agreement with those obtained from neutron diffraction experiments, although they are somewhat less precise. The residual density contour maps after HAR show fewer features than those after MM. Calculating the static electron density with the def2-TZVP basis set instead of the simpler def2-SVP one does not improve the refinement results significantly. All HARs were performed within the recently introduced HARt option implemented in the Olex2 program. They are easily launched inside its graphical user interface following a conventional IAM. PMID:29354269

Inorganic pyrophosphatase crystals from Thermococcus thioreducens for X-ray and neutron diffraction.

PubMed

Hughes, Ronny C; Coates, Leighton; Blakeley, Matthew P; Tomanicek, Steve J; Langan, Paul; Kovalevsky, Andrey Y; García-Ruiz, Juan M; Ng, Joseph D

2012-12-01

Inorganic pyrophosphatase (IPPase) from the archaeon Thermococcus thioreducens was cloned, overexpressed in Escherichia coli, purified and crystallized in restricted geometry, resulting in large crystal volumes exceeding 5 mm3. IPPase is thermally stable and is able to resist denaturation at temperatures above 348 K. Owing to the high temperature tolerance of the enzyme, the protein was amenable to room-temperature manipulation at the level of protein preparation, crystallization and X-ray and neutron diffraction analyses. A complete synchrotron X-ray diffraction data set to 1.85 Å resolution was collected at room temperature from a single crystal of IPPase (monoclinic space group C2, unit-cell parameters a=106.11, b=95.46, c=113.68 Å, α=γ=90.0, β=98.12°). As large-volume crystals of IPPase can be obtained, preliminary neutron diffraction tests were undertaken. Consequently, Laue diffraction images were obtained, with reflections observed to 2.1 Å resolution with I/σ(I) greater than 2.5. The preliminary crystallographic results reported here set in place future structure-function and mechanism studies of IPPase.

Effect of different annealing condition on the structural and magnetic properties of Mn2NiGa Heusler alloys

NASA Astrophysics Data System (ADS)

Vagadia, Megha; Hester, James; Nigam, A. K.

2018-04-01

We studied the effect of different annealing conditions on structural and magnetic properties of Mn2NiGa Heusler alloys. Reitveld refinement of neutron diffraction pattern at RT confirms the tetragonal structure with cubic phase for I-W quenched alloy whereas Le Bail fitting trials performed on neutron diffraction pattern collected for other three alloys confirm 7M monoclinic structure with cubic phase. It is found that starting and finish temperatures associated with martensite and austenite phase transformation depends strongly on the cooling rate corresponding to different cooling techniques. Slow furnace cooled sample possesses the highest martensite start temperature above room temperature ˜ 326K which decreases to ˜ 198K for ice -water quenched sample. Variation in the drop in the magnetization around MS obtained upon warming from martensite to austenite phase under ZFC cycle suggests that change in the cooling condition strongly affects the magnetization in the low temperature martensite phase. Present results suggest that by varying the cooling rate, martensite transformation as well as the martensite structure can be tuned.

Absence of bacterial imprints on struvite-containing kidney stones: a structural investigation at the mesoscopic and atomic scale.

PubMed

Bazin, Dominique; André, Gilles; Weil, Raphael; Matzen, Guy; Emmanuel, Veron; Carpentier, Xavier; Daudon, M

2012-04-01

Bacterial imprints are always observed on highly carbonated apatite kidney stones but not struvite kidney stones. Struvite and carbonated apatite stones with a high CO(3)(2-)/PO(4)(3-) rate are believed to develop from infections, but their structural differences at the mesoscopic scale lack explanation. We investigated 17 urinary calculi composed mainly of struvite or carbonated apatite by Fourier transform infrared, scanning electron microscopy, and powder neutron diffraction techniques. Carbonated apatite but not struvite stones showed bacterial imprints. If the same stone contained both carbonated apatite and struvite components, bacterial imprints were observed on the carbonated apatite but not the struvite part. Moreover, neutron powder diffraction experiments revealed the crystal size of struvite stones were larger than that of carbonated apatite stones (250 ± 50 vs 50 nm). Bacterial imprints may appear more easily on kidney stones with small nanocrystals, such as carbonated apatite than with large nanocrystals, such as struvite. This approach may help identify bacteria contributing to stone formation, perhaps with negative results of urine culture. Copyright © 2012 Elsevier Inc. All rights reserved.

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.

Evaluation between residual stresses obtained by neutron diffraction and simulation for dual phase steel welded by laser process

NASA Astrophysics Data System (ADS)

Kouadri-Henni, Afia; Malard, Benoit

2018-05-01

This study aimed at characterizing the residual stresses (RS) distribution of a Dual Phase Steel (DP600) undergoing a Laser Beam Welding (LBW) with two different laser parameters. The RS in the ferritic phase have been experimentally determined by the use of the neutrons diffraction technique. The results confirmed a gradient of RS among different zones both on the top and below surfaces but also through the thickness of the fusion zone. Low compressive stresses were observed in the Base Metal (BM) close to the Heat Affected Zone (HAZ) whereas high tensile stresses were observed in the Fusion Zone (FZ). Numerical results showed a difference in the RS distribution depending on the model used. In the end, it appears that the high temperature gradient, specific to the laser beam, is the main factor governing the RS. Our results suggest as well that the approach regarding the RS should consider not only the temperature but also process parameters. When comparing simulation results with experimental data, the values converge well in some zones, in particular the FZ and the others less.

The structural phase diagram and oxygen equilibrium partial pressure of YBa 2Cu 3O 6+ x studied by neutron powder diffraction and gas volumetry

NASA Astrophysics Data System (ADS)

Andersen, N. H.; Lebech, B.; Poulsen, H. F.

1990-12-01

An experimental technique based on neutron powder diffraction and gas volumetry is presented and used to study the structural phase diagram of YBa 2Cu 3O 6+ x under equilibrium conditions in an extended part of ( x, T)-phase (0.15< x<0.92 and 25° C< T<725°C). Our experimental observations lend strong support to a recent two-dimensional anisotropic next-nearest-neighbour Ising model calculation (the ASYNNNI model) of the basal plane oxygen ordering based of first principle interaction parameters. Simultaneous measurements of the oxygen equilibrium partial pressure show anomalies, one of which proves the thermodynamic stability of the orthorhombic OII double cell structure. Striking similarity with predictions of recent model calculations support that another anomaly may be interpreted to result from local one-dimensional fluctuations in the distribution of oxygen atoms in the basal plane of tetragonal YBCO. Our pressure data also indicate that x=0.92 is a maximum obtainable oxygen concentration for oxygen pressures below 760 Torr.

Combined elemental and microstructural analysis of genuine and fake copper-alloy coins

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

Bartoli, L; Agresti, J; Mascalchi, M

2011-07-31

Innovative noninvasive material analysis techniques are applied to determine archaeometallurgical characteristics of copper-alloy coins from Florence's National Museum of Archaeology. Three supposedly authentic Roman coins and three hypothetically fraudolent imitations are thoroughly investigated using laser-induced plasma spectroscopy and time of flight neutron diffraction along with 3D videomicroscopy and electron microscopy. Material analyses are aimed at collecting data allowing for objective discrimination between genuine Roman productions and late fakes. The results show the mentioned techniques provide quantitative compositional and textural data, which are strictly related to the manufacturing processes and aging of copper alloys. (laser applications)

The Morphology of Titanium Dioxide Aerogels

NASA Astrophysics Data System (ADS)

Zhu, Zhu

The morphology of titanium dioxide TiO _2 aerogels has been characterized by four major techniques. This work will discuss these complementary techniques such as nitrogen adsorption, X-ray powder diffraction (XRD), electron microscopies (EM- TEM, SEM), and small angle neutron scattering (SANS). The results of these characterizations have shown that the morphology of titanium dioxide TiO_2 aerogels can be characterized in terms of two length scales: 5 nm diameter, crystalline nanoparticles of anatase closely packed into mesoaggregates about 50 nm in size. The mesoaggregates are, in turn, packed into a loosely linked structure with an overall porosity of 80%.

Structure of Aqueous Trehalose Solution by Neutron Diffraction and Structural Modeling.

PubMed

Olsson, Christoffer; Jansson, Helén; Youngs, Tristan; Swenson, Jan

2016-12-15

The molecular structure of an aqueous solution of the disaccharide trehalose (C 12 H 22 O 11 ) has been studied by neutron diffraction and empirical potential structure refinement modeling. Six different isotope compositions with 33 wt % trehalose (corresponding to 38 water molecules per trehalose molecule) were measured to ensure that water-water, trehalose-water, and trehalose-trehalose correlations were accurately determined. In fact, this is the first neutron diffraction study of an aqueous trehalose solution in which also the nonexchangeable hydrogen atoms in trehalose are deuterated. With this approach, it was possible to determine that (1) there is a substantial hydrogen bonding between trehalose and water (∼11 hydrogen bonds per trehalose molecule), which is in contrast to previous neutron diffraction studies, and (2) there is no tendency of clustering of trehalose, in contrast to what is generally observed by molecular dynamics simulations and experimentally found for other disaccharides. Thus, the results give the structural picture that trehalose prefers to interact with water and participate in a hydrogen-bonded network. This strong network character of the solution might be one of the key reasons for its extraordinary stabilization effect on biological materials.

Neutron Diffraction Studies of the Atomic Vibrations of Bulk and Surface Atoms of Nanocrystalline SiC

NASA Technical Reports Server (NTRS)

Stelmakh, S.; Grzanka, E.; Zhao, Y.; Palosz, W.; Palosz, B.

2004-01-01

Thermal atomic motions of nanocrystalline Sic were characterized by two temperature atomic factors B(sub core), and B(sub shell). With the use of wide angle neutron diffraction data it was shown that at the diffraction vector above 15A(exp -1) the Wilson plots gives directly the temperature factor of the grain interior (B(sub core)). At lower Q values the slope of the Wilson plot provides information on the relative amplitudes of vibrations of the core and shell atoms.

Holographic Gratings for Slow-Neutron Optics

PubMed Central

Klepp, Juergen; Pruner, Christian; Tomita, Yasuo; Geltenbort, Peter; Drevenšek-Olenik, Irena; Gyergyek, Saso; Kohlbrecher, Joachim; Fally, Martin

2012-01-01

Recent progress in the development of holographic gratings for neutron-optics applications is reviewed. We summarize the properties of gratings recorded in deuterated (poly)methylmethacrylate, holographic polymer-dispersed liquid crystals and nanoparticle-polymer composites revealed by diffraction experiments with slow neutrons. Existing and anticipated neutron-optical instrumentations based on holographic gratings are discussed.

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.

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

NASA Astrophysics Data System (ADS)

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

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

Structural phase transition in d-benzil characterised by capacitance measurements and neutron powder diffraction

NASA Astrophysics Data System (ADS)

Goossens, D. J.; Wu, Xiaodong; Prior, M.

2005-12-01

The ferroelectric phase transition in deuterated benzil, C 14H 10O 2, has been studied using capacitance measurements and neutron powder diffraction. Hydrogenous benzil shows a phase transition at 83.5 K from a high temperature P3 121 phase to a cell-doubled P2 1 phase. The phase transition in d-benzil occurs at 88.1 K, a small isotope effect. Neutron powder diffraction was consistent with a low temperature phase of space group P2 1. Upon deuteration the transition remained first-order and the dynamics of the phenyl ring dominated the behaviour. The isotope effect can be attributed to the difference in mass and moment of inertia between C 6H 5 and C 6D 5.

Hippo/crates-in-situ deformation strain and testure studies using neutron time-of-flight diffraction.

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

Vogel, S. C.; Hartig, C.; Brissier, T. D.

2005-01-01

In situ deformation studies by diffraction allow studying of deformation mechanisms and provide valuable data to validate and improve deformation models. In particular, deformation studies using time-of-flight neutrons provide averages over large numbers of grains and allow to probing the response of lattice planes parallel and perpendicular to the applied load simultaneously. In this paper we describe the load-frame CRATES, designed for the HIPPO neutron time-of-flight diffractometer at LANSCE. The HIPPO/CRATES combination allows probing up to 20 diffraction vectors simultaneously and provides rotation of the sample in the beam while under load. With this, deformation texture, i.e. the change ofmore » grain orientation due to plastic deformation, or strain pole figures may be measured. We report initial results of a validation experiment, comparing deformation of a Zircaloy specimen measured using the NPD neutron diffractometer with results obtained for the same material using HIPPO/CRATES.« less

High-level expression and deuteration of sperm whale myoglobin: A study of its solvent structure by X-ray and neutron diffraction methods

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

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 modifiedmore » 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%.« less

Magnetic behaviour of synthetic Co(2)SiO(4).

PubMed

Sazonov, Andrew; Meven, Martin; Hutanu, Vladimir; Heger, Gernot; Hansen, Thomas; Gukasov, Arsen

2009-12-01

Synthetic Co(2)SiO(4) crystallizes in the olivine structure (space group Pnma) with two crystallographically non-equivalent Co positions and shows antiferromagnetic ordering below 50 K. We have investigated the temperature variation of the Co(2)SiO(4) magnetic structure by means of non-polarized and polarized neutron diffraction for single crystals. Measurements with non-polarized neutrons were made at 2.5 K (below T(N)), whereas polarized neutron diffraction experiments were carried out at 70 and 150 K (above T(N)) in an external magnetic field of 7 T parallel to the b axis. Additional accurate non-polarized powder diffraction studies were performed in a broad temperature range from 5 to 500 K with small temperature increments. Detailed symmetry analysis of the Co(2)SiO(4) magnetic structure shows that it corresponds to the magnetic (Shubnikov) group Pnma, which allows the antiferromagnetic configuration (G(x), C(y), A(z)) for the 4a site with inversion symmetry 1 (Co1 position) and (0,C(y),0) for the 4c site with mirror symmetry m (Co2 position). The temperature dependence of the Co1 and Co2 magnetic moments obtained from neutron diffraction experiments was fitted in a modified molecular-field model. The polarized neutron study of the magnetization induced by an applied field shows a non-negligible amount of magnetic moment on the oxygen positions, indicating a delocalization of the magnetic moment from Co towards neighbouring O owing to superexchange coupling. The relative strength of the exchange interactions is discussed based on the non-polarized and polarized neutron data.

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.

Path length dependent neutron diffraction peak shifts observed during residual strain measurements in U–8 wt% Mo castings

DOE PAGES

Steiner, M. A.; Bunn, J. R.; Einhorn, J. R.; ...

2017-05-16

This study reports an angular diffraction peak shift that scales linearly with the neutron beam path length traveled through a diffracting sample. This shift was observed in the context of mapping the residual stress state of a large U–8 wt% Mo casting, as well as during complementary measurements on a smaller casting of the same material. If uncorrected, this peak shift implies a non-physical level of residual stress. A hypothesis for the origin of this shift is presented, based upon non-ideal focusing of the neutron monochromator in combination with changes to the wavelength distribution reaching the detector due to factorsmore » such as attenuation. The magnitude of the shift is observed to vary linearly with the width of the diffraction peak reaching the detector. Consideration of this shift will be important for strain measurements requiring long path lengths through samples with significant attenuation. This effect can probably be reduced by selecting smaller voxel slit widths.« less

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.

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

Lewis, Randolph

Spider silks have the potential to provide new bio-inspired materials for numerous applications in bioenergetics and products ranging from protective clothing to artificial ligaments and tendons. A number of spider silk genes have been cloned and sequenced by the Lewis laboratory revealing the basis for understanding the key elements of spider silk proteins with respect to their materials performance. In particular, specific amino acid motifs have been identified which have been conserved for over 125 million years in all spiders that use their silk to physically trap prey. The key element in taking the next step toward generating bio-based materialsmore » from spider silks will be to move from the current descriptive data to predictive knowledge. Current efforts are focused on mimicking spider silk through synthetic proteins. In developing synthetic silk fibers, we first need to understand the complete secondary and tertiary structure of natural silk so that we can compare synthetic constructs to the natural material. Being able to compare the structure on a single fiber level is critical to the future of molecular directed mimic development because we can vary mechanical properties by different spinning methods. The new generation of synchrotron x-ray diffraction and neutron beamlines will allow, for the first time, determination of the molecular structure of silk fibers and synthetic mimics. We propose an exciting new collaborative research team working jointly between Argonne National Laboratory, Arizona State U. and the University of Wyoming to address the ?characterization of synthetic and natural spider silk fibers using x-ray and neutron diffraction.? Thus these new methodologies will provide understanding of current fibers and determine changes needed to produce fibers with specific properties. The following specific aims are proposed: ? Synthesize spider silk fibers with molecular structures mimicking that of natural silks. Test the mechanic properties of these materials and compare them to natural silk fibers. ? Develop x-ray and neutron diffraction techniques to better determine the structure in amorphous and semicrystalline biopolymers, such as spider silk fibers. ? Combine mechanical testing and structural x-ray and neutron diffraction data to develop a molecular understanding of the structure-function relationship in spider silk materials. ? Elucidate the role water plays in spider silk fiber formation and structure. Emphasis will be placed on combined neutron and NMR studies. ? Use solid-state Nuclear Magnetic Resonance (NMR) to characterize synthetic and natural spider silk materials that show potential as a biomimetic material or bio-inspired polymer architecture. ? Develop EPSCoR student and postdoctoral training and exposure to national laboratory facilities. ? Further develop scientific outreach and chemical education programs and research.« less

Probing multiscale transport and inhomogeneity in a lithium-ion cells using in-situ neutron methods

DOE PAGES

Zhou, Hui; An, Ke; Allu, Srikanth; ...

2016-01-01

Here, we demonstrate for the first time the lithiation process in graphitic anodes using insitu neutron radiography in a pouch cell format. The neutron absorption contrast shows a direct correlation between degree of lithiation and the discharge voltage plateau. Furthermore, we provide a semi-quantitative comparison between the observed spatial variations of neutron attenuation line profile across the graphite electrode and the calculated lithium concentration profiles computed under similar electrochemical discharge conditions. In conjunction, in situ neutron diffraction of a similar pouch cell under identical test protocol was carried to obtain information about the local phase changes upon lithiation. Combined in-situmore » radiography and diffraction opens up a powerful nondestructive method to understand the multi-scale nature of lithium transport and degradation in practical lithium-ion cells.« less

Electron-volt neutron spectroscopy: beyond fundamental systems

NASA Astrophysics Data System (ADS)

Andreani, Carla; Krzystyniak, Maciej; Romanelli, Giovanni; Senesi, Roberto; Fernandez-Alonso, Felix

2017-01-01

This work provides an up-to-date account of the use of electron-volt neutron spectroscopy in materials research. This is a growing area of neutron science, capitalising upon the unique insights provided by epithermal neutrons on the behaviour and properties of an increasing number of complex materials. As such, the present work builds upon the aims and scope of a previous contribution to this journal back in 2005, whose primary focus was on a detailed description of the theoretical foundations of the technique and their application to fundamental systems [see Andreani et al., Adv. Phys. 54 (2005) p.377] A lot has happened since then, and this review intends to capture such progress in the field. With both expert and novice in mind, we start by presenting the general principles underpinning the technique and discuss recent conceptual and methodological developments. We emphasise the increasing use of the technique as a non-invasive spectroscopic probe with intrinsic mass selectivity, as well as the concurrent use of neutron diffraction and first-principles computational materials modelling to guide and interpret experiments. To illustrate the state of the art, we discuss in detail a number of recent exemplars, chosen to highlight the use of electron-volt neutron spectroscopy across physics, chemistry, biology, and materials science. These include: hydrides and proton conductors for energy applications; protons, deuterons, and oxygen atoms in bulk water; aqueous protons confined in nanoporous silicas, carbon nanotubes, and graphene-related materials; hydrated water in proteins and DNA; and the uptake of molecular hydrogen by soft nanostructured media, promising materials for energy-storage applications. For the primary benefit of the novice, this last case study is presented in a pedagogical and question-driven fashion, in the hope that it will stimulate further work into uncharted territory by newcomers to the field. All along, we emphasise the increasing (and much-needed) synergy between experiments using electron-volt neutrons and contemporary condensed matter theory and materials modelling to compute and ultimately understand neutron-scattering observables, as well as their relation to materials properties not amenable to scrutiny using other experimental probes.

Neutron diffraction studies of some rare earth-transition metal deuterides

NASA Astrophysics Data System (ADS)

James, W. J.

1984-04-01

Neutron diffraction studies of the ternary alloy system Y6(Fel-xMnx)23 reveal that the unusual magnetic behavior upon substitution of Mn or Fe into the end members, is a consequence of atomic ordering wherein there is strong site preference of Mn for the f sub 2 sites and of Fe for the f sub 1 sites. In the Mn-rich compositions, Fe is found to have no spontaneous moments. Therefore, the long range magnetic ordering arises solely from Mn-Mn interactions. Upon substitution of Mn into the Fe-rich ternaries, the Fe moments are considerably reduced. Neutron diffraction studies of Y6Mn23D23 show that a transition occurs below 180K from a fcc structure to a primitive tetragonal structure, space group P4/mmm with the onset of antiferromagnetic ordering. The Mn moments are directed along the c-axis. The transition probably results from atomic ordering of the D atoms at low temperature which induces c axis magnetic ordering. The question of the appropriate space group of LaNi4.5Al0.5D4.5, P6/mmm or P3/m has been resolved by a careful refinement and analysis of neutron diffraction data. The preferred space group is P6/mmm. Neutron powder diffraction and thermal magnetization measurements on small single crystals of ErNi3, ErCo3, and ErFe3 (space group R3m) show that the magnetocrystalline properties are a consequence of competing local site anisotropies between the two non-equivalent crystallographic sites of Er and two of the three non-equivalent sites of the 3d-transition metal.

Low Temperature and Neutron Physics Studies: Final Progress Report, March 1, 1986--May 31, 1987

DOE R&D Accomplishments Database

Shull, C.G.

1989-07-27

A search for a novel coupling interaction between the Pendelloesung periodicity which is formed in a diffracting crystal and the Larmor precession of neutrons in a magnetic field has been carried out. This interaction is expected to exhibit a resonant behavior when the two spatial periodicities become matched upon scanning the magnetic field being applied to the crystal. Observations on a diffracting, perfect crystal of silicon with neutrons of wavelength 1 Angstrom show the expected resonant action but some discrepancy between the observed magnitude of the resonance effects remains for interpretation.

High-resolution neutron-diffraction measurements to 8 kbar

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

Structural characterization of nanoscale intermetallic precipitates in highly neutron irradiated reactor pressure vessel steels

DOE PAGES

Sprouster, D. J.; Sinsheimer, J.; Dooryhee, E.; ...

2015-10-21

Here, massive, thick-walled pressure vessels are permanent nuclear reactor structures that are exposed to a damaging flux of neutrons from the adjacent core. The neutrons cause embrittlement of the vessel steel that increases with dose (fluence or service time), as manifested by an increasing temperature transition from ductile-to-brittle fracture. Moreover, extending reactor life requires demonstrating that large safety margins against brittle fracture are maintained at the higher neutron fluence associated with 60 to 80 years of service. Here synchrotron-based x-ray diffraction and small angle x-ray scattering measurements are used to characterize a new class of highly embrittling nm-scale Mn-Ni-Si precipitatesmore » that develop in the irradiated steels at high fluence. Furthermore, these precipitates can lead to severe embrittlement that is not accounted for in current regulatory models. Application of the complementarity techniques has, for the very first time, successfully characterized the crystal structures of the nanoprecipitates, while also yielding self-consistent compositions, volume fractions and size distributions.« less

Neutron diffraction from aligned stacks of lipid bilayers using the WAND instrument

DOE PAGES

Marquardt, Drew; Frontzek, Matthias D.; Zhao, Yu; ...

2018-02-06

Neutron diffraction from aligned stacks of lipid bilayers is examined using the Wide-Angle Neutron Diffractometer (WAND), located at the High Flux Isotope Reactor, Oak Ridge, Tennessee, USA. Data were collected at different levels of hydration and neutron contrast by varying the relative humidity (RH) and H 2O/D 2O ratio from multi-bilayers of dioleoylphosphatidylcholine and sunflower phosphatidylcholine extract aligned on single-crystal silicon substrates. This work highlights the capabilites of a newly fabricated sample hydration cell, which allows the lipid bilayers to be hydrated with varying H/D ratios from the RH generated by saturated salt solutions, and also demonstrates WAND's capability asmore » an instrument suitable for the study of aligned lipid multi-bilayers.« less

Neutron diffraction from aligned stacks of lipid bilayers using the WAND instrument

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

Marquardt, Drew; Frontzek, Matthias D.; Zhao, Yu

Neutron diffraction from aligned stacks of lipid bilayers is examined using the Wide-Angle Neutron Diffractometer (WAND), located at the High Flux Isotope Reactor, Oak Ridge, Tennessee, USA. Data were collected at different levels of hydration and neutron contrast by varying the relative humidity (RH) and H 2O/D 2O ratio from multi-bilayers of dioleoylphosphatidylcholine and sunflower phosphatidylcholine extract aligned on single-crystal silicon substrates. This work highlights the capabilites of a newly fabricated sample hydration cell, which allows the lipid bilayers to be hydrated with varying H/D ratios from the RH generated by saturated salt solutions, and also demonstrates WAND's capability asmore » an instrument suitable for the study of aligned lipid multi-bilayers.« less

Evidence for weak ferromagnetism, isostructural phase transition, and linear magnetoelectric coupling in the multiferroic Bi0.8Pb0.2Fe0.9Nb0.1O3 solid solution

NASA Astrophysics Data System (ADS)

Patel, Jay Prakash; Senyshyn, Anatoliy; Fuess, Hartmut; Pandey, Dhananjai

2013-09-01

Magnetization, dielectric, and calorimetric studies on Bi0.8 Pb0.2 Fe0.9 Nb0.1O3 (BF-0.2PFN) reveal very weak ferromagnetism but strong dielectric anomaly at the antiferromagnetic transition temperature (TN) characteristic of magnetoelectric coupling. We correlate these results with nuclear and magnetic structure studies using x-ray and neutron powder diffraction techniques, respectively. Rietveld refinements using x-ray powder diffraction data in the temperature range 300 to 673 K reveal pronounced anomalies in the unit cell parameters at TN, indicating strong magnetoelastic coupling. The nuclear and magnetic structures of BF-0.2PFN were determined from neutron powder diffraction data using a representation theory approach. They show the occurrence of a first-order isostructural phase transition (IPT) accompanying the magnetic ordering below TN˜566 K, leading to significant discontinuous change in the ionic polarization (ΔPz˜1.6(3) μC/cm2) and octahedral tilt angle (˜0.3°) at TN. The ionic polarization obtained from refined positional coordinates of the nuclear structure and Born effective charges is shown to scale linearly with sublattice magnetization, confirming the presence of linear magnetoelectric coupling in BF-0.2PFN at the atomic level, despite the very low value of remanent magnetization (Mr).

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Influence of ceramide on the internal structure and hydration of the phospholipid bilayer studied by neutron and X-ray scattering

NASA Astrophysics Data System (ADS)

Kiselev, M. A.; Zemlyanaya, E. V.; Ryabova, N. Y.; Hauss, T.; Almasy, L.; Funari, S. S.; Zbytovska, J.; Lombardo, D.

2014-07-01

Small angle neutron scattering (SANS), neutron diffraction and X-ray powder diffraction were used to investigate influence of N-stearoyl phytosphingosine (CER[NP]) and α-hydroxy- N-stearoyl phytosphingosine (CER[AP]) on the internal structure and hydration of DMPC membrane in fully and partly hydrated states at T = 30 °C. Application of Fourier analysis for diffraction data and model calculations for the SANS data evidence that addition of both CER[NP] and CER[AP] in small concentrations promotes significant changes in the organization of DMPC bilayers, such as the increase of the hydrophobic core region. SANS data evidence a decrease in the average radius and polydispersity of the vesicles that can be ascribed to hydrogen bonds interactions that favor tight lipid packing with a compact, more rigid character.

Neutron scattering study on cathode LiMn2O4 and solid electrolyte 5(Li2O)(P2O5)

NASA Astrophysics Data System (ADS)

Kartini, E.; Putra, Teguh P.; Jahya, A. K.; Insani, A.; Adams, S.

2014-09-01

Neutron scattering is very important technique in order to investigate the energy storage materials such as lithium-ion battery. The unique advantages, neutron can see the light atoms such as Hydrogen, Lithium, and Oxygen, where those elements are negligible by other corresponding X-ray method. On the other hand, the energy storage materials, such as lithium ion battery is very important for the application in the electric vehicles, electronic devices or home appliances. The battery contains electrodes (anode and cathode), and the electrolyte materials. There are many challenging to improve the existing lithium ion battery materials, in order to increase their life time, cyclic ability and also its stability. One of the most scientific challenging is to investigate the crystal structure of both electrode and electrolyte, such as cathodes LiCoO2, LiMn2O4 and LiFePO4, and solid electrolyte Li3PO4. Since all those battery materials contain Lithium ions and Oxygen, the used of neutron scattering techniques to study their structure and related properties are very important and indispensable. This article will review some works of investigating electrodes and electrolytes, LiMn2O4 and 5(Li2O)(P2O5), by using a high resolution powder diffraction (HRPD) at the multipurpose research reactor, RSG-Sywabessy of the National Nuclear Energy Agency (BATAN), Indonesia.

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

Zarkevich, Nikolai A; Johnson, Duane D

Nitinol (NiTi), the most widely used shape-memory alloy, exhibits an austenite phase that has yet to be identified. The usually assumed austenitic structure is cubic B2, which has imaginary phonon modes, hence it is unstable. We suggest a stable austenitic structure that “on average” has B2 symmetry (observed by x-ray and neutron diffraction), but it exhibits finite atomic displacements from the ideal B2 sites. The proposed structure has a phonon spectrum that agrees with that from neutron scattering, has diffraction spectra in agreement with x-ray diffraction, and has an energy relative to the ground state that agrees with calorimetry data.

Magnetic topology of Co-based inverse opal-like structures

NASA Astrophysics Data System (ADS)

Grigoryeva, N. A.; Mistonov, A. A.; Napolskii, K. S.; Sapoletova, N. A.; Eliseev, A. A.; Bouwman, W.; Byelov, D. V.; Petukhov, A. V.; Chernyshov, D. Yu.; Eckerlebe, H.; Vasilieva, A. V.; Grigoriev, S. V.

2011-08-01

The magnetic and structural properties of a cobalt inverse opal-like crystal have been studied by a combination of complementary techniques ranging from polarized neutron scattering and superconducting quantum interference device (SQUID) magnetometry to x-ray diffraction. Microradian small-angle x-ray diffraction shows that the inverse opal-like structure (OLS) synthesized by the electrochemical method fully duplicates the three-dimensional net of voids of the template artificial opal. The inverse OLS has a face-centered cubic (fcc) structure with a lattice constant of 640±10 nm and with a clear tendency to a random hexagonal close-packed structure along the [111] axes. Wide-angle x-ray powder diffraction shows that the atomic cobalt structure is described by coexistence of 95% hexagonal close-packed and 5% fcc phases. The SQUID measurements demonstrate that the inverse OLS film possesses easy-plane magnetization geometry with a coercive field of 14.0 ± 0.5 mT at room temperature. The detailed picture of the transformation of the magnetic structure under an in-plane applied field was detected with the help of small-angle diffraction of polarized neutrons. In the demagnetized state the magnetic system consists of randomly oriented magnetic domains. A complex magnetic structure appears upon application of the magnetic field, with nonhomogeneous distribution of magnetization density within the unit element of the OLS. This distribution is determined by the combined effect of the easy-plane geometry of the film and the crystallographic geometry of the opal-like structure with respect to the applied field direction.

Polarized neutron scattering on HYSPEC: the HYbrid SPECtrometer at SNS

DOE PAGES

Zaliznyak, Igor A.; Savici, Andrei T.; Ovidiu Garlea, V.; ...

2017-06-20

Here, we describe some of the first polarized neutron scattering measurements performed at HYSPEC [1-4] spectrometer at the Spallation Neutron Source, Oak Ridge National Laboratory. Furthermore, we discuss details of the instrument setup and the experimental procedures in the mode with full polarization analysis. Examples of polarized neutron diffraction and polarized inelastic neutron data obtained on single crystal samples are presented.

Neutron diffraction investigation of γ manganese hydride

NASA Astrophysics Data System (ADS)

Fedotov, V. K.; Antonov, V. E.; Kolesnikov, A. I.; Beskrovnyi, A. I.; Grosse, G.; Wagner, F. E.

1998-08-01

A profile analysis of the neutron diffraction spectrum of the fcc high pressure hydride λ-MnH 0.41 measured under ambient conditions showed that hydrogen is randomly distributed over the octahedral interstices of the fcc metal lattice and that the hydride is an antiferromagnet with the same collinear spin structure as pure λ-Mn, but with a smaller magnetic moment of about 1.9 Bohr magnetons per Mn atom.

STRUCTURE OF POTASSIUM HYDROGEN MALEATE BY NEUTRON DIFFRACTION

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

Peterson, S.W.; Levy, H.A.

1958-10-01

The preliminary results of a neutron diffraction study are presented which confirm the existence in potassium hydrogen maleate of a short, strong, hydrogen bond and show the ion to be at least statistically symmetrical. The hydrogen is strongly linked to both neighboring oxygen atoms, and there is an existing mode of correlated motion of considerable amplitude in which the oxygen atoms are displaced but hydrogen is not. (J.R.D.)

Neutron Diffraction and Electrical Transport Studies on Magnetic Transition in Terbium at High Pressures and Low Temperatures

NASA Astrophysics Data System (ADS)

Thomas, Sarah; Montgomery, Jeffrey; Tsoi, Georgiy; Vohra, Yogesh; Weir, Samuel; Tulk, Christopher; Moreira Dos Santos, Antonio

2013-06-01

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 its transition from a helical antiferromagnetic to a ferromagnetic ordered phase as a function of pressure. The electrical resistance measurements using designer diamonds show a change in slope as the temperature is lowered through the ferromagnetic Curie temperature. The temperature of the ferromagnetic transition decreases at a rate of -16.7 K/GPa till 3.6 GPa, where terbium undergoes a structural transition from hexagonal close packed (hcp) to an α-Sm phase. Above this pressure, the electrical resistance measurements no longer exhibit a change in slope. In order to confirm the change in magnetic phase suggested by the electrical resistance measurements, neutron diffraction measurements were conducted at the SNAP beamline at the Oak Ridge National Laboratory. Measurements were made at pressures to 5.3 GPa and temperatures as low as 90 K. An abrupt increase in peak intensity in the neutron diffraction spectra signaled the onset of magnetic order below the Curie temperature. A magnetic phase diagram of rare earth metal terbium will be presented to 5.3 GPa and 90 K based on these studies.

Structural properties of barium stannate

NASA Astrophysics Data System (ADS)

Phelan, D.; Han, F.; Lopez-Bezanilla, A.; Krogstad, M. J.; Gim, Y.; Rong, Y.; Zhang, Junjie; Parshall, D.; Zheng, H.; Cooper, S. L.; Feygenson, M.; Yang, Wenge; Chen, Yu-Sheng

2018-06-01

BaSnO3 has attracted attention as a transparent conducting oxide with high room temperature carrier mobility. We report a series of measurements that were carried out to assess the structure of BaSnO3 over a variety of length scales. Measurements included single crystal neutron and x-ray diffraction, Rietveld and pair distribution analysis of neutron powder diffraction, Raman scattering, and high-pressure x-ray diffraction. Results from the various diffraction probes indicate that both the long-range and local structures are consistent with the cubic symmetry. The diffraction data under pressure was consistent with a robustly cubic phase up to 48.9 GPa, which is supported by density functional calculations. Additionally, transverse phonon velocities were determined from measured dispersion of the transverse acoustic phonon branches, the results of which are in good agreement with previous theoretical estimates and ultrasound measurements.

Quantitative phase analysis of challenging samples using neutron powder diffraction. Sample #4 from the CPD QPA round robin revisited

DOE PAGES

Whitfield, Pamela S.

2016-04-29

Here, quantitative phase analysis (QPA) using neutron powder diffraction more often than not involves non-ambient studies where no sample preparation is possible. The larger samples and penetration of neutrons versus X-rays makes neutron diffraction less susceptible to inhomogeneity and large grain sizes, but most well-characterized QPA standard samples do not have these characteristics. Sample #4 from the International Union of Crystallography Commission on Powder Diffraction QPA round robin was one such sample. Data were collected using the POWGEN time-of-flight (TOF) neutron powder diffractometer and analysed together with historical data from the C2 diffractometer at Chalk River. The presence of magneticmore » reflections from Fe 3O 4 (magnetite) in the sample was an additional consideration, and given the frequency at which iron-containing and other magnetic compounds are present during in-operando studies their possible impact on the accuracy of QPA is of interest. Additionally, scattering from thermal diffuse scattering in the high-Qregion (<0.6 Å) accessible with TOF data could impact QPA results during least-squares because of the extreme peak overlaps present in this region. Refinement of POWGEN data was largely insensitive to the modification of longer d-spacing reflections by magnetic contributions, but the constant-wavelength data were adversely impacted if the magnetic structure was not included. A robust refinement weighting was found to be effective in reducing quantification errors using the constant-wavelength neutron data both where intensities from magnetic reflections were ignored and included. Results from the TOF data were very sensitive to inadequate modelling of the high- Q (low d-spacing) background using simple polynomials.« less

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr4S8

NASA Astrophysics Data System (ADS)

Pokharel, G.; May, A. F.; Parker, D. S.; Calder, S.; Ehlers, G.; Huq, A.; Kimber, S. A. J.; Arachchige, H. Suriya; Poudel, L.; McGuire, M. A.; Mandrus, D.; Christianson, A. D.

2018-04-01

The physical properties of the spinel LiGaCr4S8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. These results indicate strong magnetoelastic coupling in LiGaCr4S8 .

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

Vogel, Sven C.; Losko, Adrian Simon; Pokharel, Reeju

The goal of the Advanced Non-destructive Fuel Examination (ANDE) work package is the development and application of non-destructive neutron imaging and scattering techniques to ceramic and metallic nuclear fuels, ultimately also to irradiated fuels. The results of these characterizations provide complete pre- and post-irradiation on length scales ranging from mm to nm, guide destructive examination, and inform modelling efforts. Besides technique development and application to samples to be irradiated, the ANDE work package also examines possible technologies to provide these characterization techniques pool-side, e.g. at the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) using laser-driven intense pulsed neutronmore » and gamma sources. Neutron tomography and neutron diffraction characterizations were performed on nine pellets; four UN/ U-Si composite formulations (two enrichment levels), three pure U 3Si 5 reference formulations (two enrichment levels), and two reject pellets with visible flaws (to qualify the technique). The 235U enrichments ranged from 0.2 to 8.8 wt. %. The nitride/silicide composites are candidate compositions for use as Accident Tolerant Fuel (ATF). The monophase U 3Si 5 material was included as a reference. Pellets from the same fabrication batches will be inserted in the Advanced Test Reactor at Idaho during 2016. We have also proposed a data format to build a database for characterization results of individual pellets. Neutron data reported in this report were collected in the LANSCE run cycle that started in September 2015 and ended in March 2016. This report provides the results for the characterized samples and discussion in the context of ANDE and APIE. We quantified the gamma spectra of several samples in their received state as well as after neutron irradiation to ensure that the neutron irradiation does not add significant activation that would complicate shipment and handling. We demonstrated synchrotron-based 3D X-ray microscopy on the composite fuel materials, providing unparalleled level of detail on the 3D microstructure. Furthermore, we initiated development of shielding containers allowing the characterizations presented herein while allowing handling of irradiated samples.« less

Comparison between different techniques applied to quartz CPO determination in granitoid mylonites

NASA Astrophysics Data System (ADS)

Fazio, Eugenio; Punturo, Rosalda; Cirrincione, Rosolino; Kern, Hartmut; Wenk, Hans-Rudolph; Pezzino, Antonino; Goswami, Shalini; Mamtani, Manish

2016-04-01

Since the second half of the last century, several techniques have been adopted to resolve the crystallographic preferred orientation (CPO) of major minerals constituting crustal and mantle rocks. To this aim, many efforts have been made to increase the accuracy of such analytical devices as well as to progressively reduce the time needed to perform microstructural analysis. It is worth noting that many of these microstructural studies deal with quartz CPO because of the wide occurrence of this mineral phase in crustal rocks as well as its quite simple chemical composition. In the present work, four different techniques were applied to define CPOs of dynamically recrystallized quartz domains from naturally deformed rocks collected from a ductile crustal scale shear zone in order to compare their advantages and limitation. The selected Alpine shear zone is located in the Aspromonte Massif (Calabrian Peloritani Orogen, southern Italy) representing granitoid lithotypes. The adopted methods span from "classical" universal stage (US), to image analysis technique (CIP), electron back-scattered diffraction (EBSD), and time of flight neutron diffraction (TOF). When compared, bulk texture pole figures obtained by means of these different techniques show a good correlation. Advances in analytical techniques used for microstructural investigations are outlined by discussing results of quartz CPO that are presented in this study.

Magnetic and Structural Characterization of Fe-Ga Using Kerr Microscopy and Neutron Scattering

DTIC Science & Technology

2010-01-01

117 4.6 Schematic of triple axes single crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right...Therefore, USANS data is one-dimensional. 4.3.3 Single Crystal Neutron Diffraction The single crystal neutron diffractometer, TriCS at Paul Scherrer...crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right) [106] 4.4 Unpolarized SANS In this section, SANS

Morin-like spin canting in the magnetic CaFe5O7 ferrite: A combined neutron and Mössbauer study

NASA Astrophysics Data System (ADS)

Delacotte, C.; Bréard, Y.; Caignaert, V.; Hardy, V.; Greneche, J. M.; Hébert, S.; Suard, E.; Pelloquin, D.

2017-03-01

Magnetic structure of CaFe5O7 ferrite has been studied jointly from neutron powder diffraction data and spectroscopic Mössbauer measurements in the thermal range from 5 to 500 K. This coupled work highlights three distinct magnetic domains around two specific temperatures: TM=125 K and TN=360 K. The latter corroborates the structural monoclinic-orthorhombic transition previously reported by transmission electron microscopy techniques and X-ray thermodiffractometry. Complementary heat capacity measurements have confirmed this first order transition with a sharp peak at 360 K. Interestingly, this large study has revealed a second magnetic transition associated to a spin rotation at 125 K similar to this one reported by Morin in α-Fe2O3 hematite at TM=260 K.

Pressure-Induced Structural Phase Transition in CeNi: X-ray and Neutron Scattering Studies and First-Principles Calculations

DOE PAGES

Mirmelstein, A.; Podlesnyak, Andrey A.; dos Santos, Antonio M.; ...

2015-08-03

The pressure-induced structural phase transition in the intermediate-valence compound CeNi has been investigated by x-ray and neutron powder diffraction techniques. It is shown that the structure of the pressure-induced CeNi phase (phases) can be described in terms of the Pnma space group. Equations of state for CeNi on both sides of the phase transition are derived and an approximate P-T phase diagram is suggested for P<8 GPa and T<300 K. The observed Cmcm→Pnma structural transition is then analyzed using density functional theory calculations, which successfully reproduce the ground state volume, the phase transition pressure, and the volume collapse associated withmore » the phase transition.« less

Neutron powder diffraction and high-pressure synchrotron x-ray diffraction study of tantalum nitrides

NASA Astrophysics Data System (ADS)

Feng, Lei-hao; Hu, Qi-wei; Lei, Li; Fang, Lei-ming; Qi, Lei; Zhang, Lei-lei; Pu, Mei-fang; Kou, Zi-li; Peng, Fang; Chen, Xi-ping; Xia, Yuan-hua; Kojima, Yohei; Ohfuji, Hiroaki; He, Duan-wei; Chen, Bo; Irifune, Tetsuo

2018-02-01

Not Available Project supported by the Research Foundation of Key Laboratory of Neutron Physics (Grant No. 2015BB03), the National Natural Science Foundation of China (Grant Nos. 11774247), the Science Foundation for Excellent Youth Scholars of Sichuan University (Grant No. 2015SCU04A04), and the Joint Usage/Research Center PRIUS (Ehime University, Japan) and Chinese Academy of Sciences (Grant No. 2017-BEPC-PT-000568).

The structural and magnetic phase transitions in a ``parent'' Fe pnictide compound

NASA Astrophysics Data System (ADS)

Ni, Ni; Allred, Jared; Cao, Huibo; Tian, Wei; Liu, Lian; Cho, Kyuil; Krogstad, Matthew; Ma, Jie; Taddei, Keith; Tanatar, Makariy; Prozorov, Ruslan; Matsuda, Masaaki; Rosenkranz, Stephan; Uemura, Yasutomo; Jiang, Shan

2015-03-01

We will present transport, thermodynamic, synchrotron X-ray, neutron diffraction, μSR, ARPES and polarized optical image measurements on the ``parent'' compound of the 112 high Tc superconducting Fe pnictide family. Structural and magnetic phase transitions are revealed. Detailed magnetic structure was solved by single crystal neutron diffraction. We will discuss the similarity and difference of these transitions comparing to the parent compounds of other Fe pnictide superconductors.

Neutron diffraction studies of laser welding residual stresses

NASA Astrophysics Data System (ADS)

Petrov, Peter I.; Bokuchava, Gizo D.; Papushkin, Igor V.; Genchev, Gancho; Doynov, Nikolay; Michailov, Vesselin G.; Ormanova, Maria A.

2016-01-01

The residual stress and microstrain distribution induced by laser beam welding of the low-alloyed C45 steel plate was investigated using high-resolution time-of-flight (TOF) neutron diffraction. The neutron diffraction experiments were performed on FSD diffractometer at the IBR-2 pulsed reactor in FLNP JINR (Dubna, Russia). The experiments have shown that the residual stress distribution across weld seam exhibit typical alternating sign character as it was observed in our previous studies. The residual stress level is varying in the range from -60 MPa to 450 MPa. At the same time, the microstrain level exhibits sharp maxima at weld seam position with maximal level of 4.8·10-3. The obtained experimental results are in good agreement with FEM calculations according to the STAAZ model. The provided numerical model validated with measured data enables to study the influence of different conditions and process parameters on the development of residual welding stresses.

Neutron diffraction study of the formation of ordered antiphase domains in cubic titanium carbide TiC{sub 0.60}

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

Khidirov, I., E-mail: khidirov@inp.uz; 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 relativelymore » 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.« less

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).

Numerical and neutron diffraction measurement of residual stress distribution in dissimilar weld

DOE PAGES

Eisazadeh, Hamid; Bunn, Jeffrey R.; Aidun, Daryush K.

2017-01-01

In this study, a model considering an asymmetric power heat distribution, temperature-dependent material properties, strain hardening and phase transformation was developed to predict temperature field and residual stress distribution in GTA dissimilar weld between austenitic stainless steel (304) and low carbon steel (1018). The effect of martensite formation on longitudinal and transverse residual stress distributions were investigated using both FE model and neutron diffraction measurement. The results indicate that martensitic phase has a significant influence on both residual stress components, i.e., transverse and longitudinal, and it not only can change the distribution shape of residual stress near the weld centermore » line but, also, can alter the peak value of the residual stresses. The calculated temperature and weld zone profile were in agreement with the experimental results. Favorable general agreement was also found between the calculated residual stress distribution and residual stress measurements by the neutron diffraction method.« less

Numerical and neutron diffraction measurement of residual stress distribution in dissimilar weld

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

Eisazadeh, Hamid; Bunn, Jeffrey R.; Aidun, Daryush K.

In this study, a model considering an asymmetric power heat distribution, temperature-dependent material properties, strain hardening and phase transformation was developed to predict temperature field and residual stress distribution in GTA dissimilar weld between austenitic stainless steel (304) and low carbon steel (1018). The effect of martensite formation on longitudinal and transverse residual stress distributions were investigated using both FE model and neutron diffraction measurement. The results indicate that martensitic phase has a significant influence on both residual stress components, i.e., transverse and longitudinal, and it not only can change the distribution shape of residual stress near the weld centermore » line but, also, can alter the peak value of the residual stresses. The calculated temperature and weld zone profile were in agreement with the experimental results. Favorable general agreement was also found between the calculated residual stress distribution and residual stress measurements by the neutron diffraction method.« less

Crystallographic texture of straight-rolled ?-uranium foils via neutron and X-ray diffraction

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

Einhorn, J. R.; Steiner, M. A.; Vogel, S. C.

The texture of recrystallized straight-rolled ?-uranium foils, a component in prospective irradiation target designs for medical isotope production, has been measured by neutron diffraction, as well as X-ray diffraction using both Cu and Mo sources. Variations in the penetration depth of neutron and X-ray radiation allow for determination of both the bulk and surface textures. The bulk ?-uranium foil texture is similar to the warm straight-rolled plate texture, with the addition of a notable splitting of the (001) poles along the transverse direction. The surface texture of the foils is similar to the bulk, with an additional (001) texture componentmore » that is oriented between the rolling and normal directions. Differences between the surface and bulk textures are expected to arise from shear forces during the rolling process and the influence that distinct strain histories have on subsequent texture evolution during recrystallization.« less

Crystallographic texture of straight-rolled ?-uranium foils via neutron and X-ray diffraction

DOE PAGES

Einhorn, J. R.; Steiner, M. A.; Vogel, S. C.; ...

2017-05-25

The texture of recrystallized straight-rolled ?-uranium foils, a component in prospective irradiation target designs for medical isotope production, has been measured by neutron diffraction, as well as X-ray diffraction using both Cu and Mo sources. Variations in the penetration depth of neutron and X-ray radiation allow for determination of both the bulk and surface textures. The bulk ?-uranium foil texture is similar to the warm straight-rolled plate texture, with the addition of a notable splitting of the (001) poles along the transverse direction. The surface texture of the foils is similar to the bulk, with an additional (001) texture componentmore » that is oriented between the rolling and normal directions. Differences between the surface and bulk textures are expected to arise from shear forces during the rolling process and the influence that distinct strain histories have on subsequent texture evolution during recrystallization.« less

High-resolution neutron diffraction study of CuNCN: New evidence of structure anomalies at low temperature

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

Jacobs, Philipp; Houben, Andreas; Dronskowski, Richard, E-mail: drons@HAL9000.ac.rwth-aachen.de

Copper carbodiimide (CuNCN) is the nitrogen-containing analogue of cupric oxide. Based on high-resolution neutron-diffraction data, CuNCN's lattice parameters are derived as a function of the temperature. In accordance with a recent synchrotron study, a clear trend in the cell parameter a is observed accompanying the changing magnetic behavior. With decreasing temperature, a slowly decreases to a minimum at ∼100 K after which it rises again. The same trend—albeit more pronounced—is observed for the c lattice parameter at ∼35 K. The herein presented neutron powder-diffraction data also support the conjectured sequence of transitions from the high-temperature one-dimensional resonating valence-bond (RVB) statemore » to a transient two-dimensional RVB state and eventually, at lowest temperatures, into another two-dimensional RVB state, presumably the ground state.« less

Probing hydrogen positions in hydrous compounds: information from parametric neutron powder diffraction studies.

PubMed

Ting, Valeska P; Henry, Paul F; Schmidtmann, Marc; Wilson, Chick C; Weller, Mark T

2012-05-21

We demonstrate the extent to which modern detector technology, coupled with a high flux constant wavelength neutron source, can be used to obtain high quality diffraction data from short data collections, allowing the refinement of the full structures (including hydrogen positions) of hydrous compounds from in situ neutron powder diffraction measurements. The in situ thermodiffractometry and controlled humidity studies reported here reveal that important information on the reorientations of structural water molecules with changing conditions can be easily extracted, providing insight into the effects of hydrogen bonding on bulk physical properties. Using crystalline BaCl2·2H2O as an example system, we analyse the structural changes in the compound and its dehydration intermediates with changing temperature and humidity levels to demonstrate the quality of the dynamic structural information on the hydrogen atoms and associated hydrogen bonding that can be obtained without resorting to sample deuteration.

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction.

PubMed

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.

Non destructive neutron diffraction measurements of cavities, inhomogeneities, and residual strain in bronzes of Ghiberti's relief from the Gates of Paradise

NASA Astrophysics Data System (ADS)

Festa, G.; Senesi, R.; Alessandroni, M.; Andreani, C.; Vitali, G.; Porcinai, S.; Giusti, A. M.; Materna, T.; Paradowska, A. M.

2011-03-01

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.

Design and implementation of a multiaxial loading capability during heating on an engineering neutron diffractometer

DOE PAGES

Benafan, O.; Padula, S. A.; Skorpenske, H. D.; ...

2014-10-02

Here we discuss a gripping capability that was designed, implemented, and tested for in situ neutron diffraction measurements during multiaxial loading and heating on the VULCAN engineering materials diffractometer at the spallation neutron source at Oak Ridge National Laboratory.

Functional properties of poly(tetrafluoroethylene) (PTFE) gasket working in nuclear reactor conditions

NASA Astrophysics Data System (ADS)

Wyszkowska, Edyta; Leśniak, Magdalena; Kurpaska, Lukasz; Prokopowicz, Rafal; Jozwik, Iwona; Sitarz, Maciej; Jagielski, Jacek

2018-04-01

In this study structural and nanomechanical properties of polytetrafluoroethylene (PTFE) used as a gasket in the nuclear reactor have been deeply investigated. In order to reveal structural changes caused by long-term pressure, temperature and irradiation (possibly neutron and gamma), methods such as SEM, X-ray diffraction and Raman Spectroscopy have been used. Nanomechanical properties such as Young Modulus and hardness were investigated by means of the nanoindentation technique. Presented study confirmed the influence of working (radiative) environment on the functional properties of PTFE. The results of Raman spectroscopy and X-ray diffraction techniques revealed shift of the major band positions and band intensities increase. Moreover, changes of hardness and Young Modulus values of the irradiated material with respect to the virgin specimen have been recorded. This phenomenon can be attributed to the modifications in crystallinity of the material. Presented work suggest that morphology of the irradiated material altered from well-ordered parallel fibers to more dense and thicker ones.

Structural Properties of Barium Stannate.

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

Phelan, D.; Han, F.; Lopez-Bezanilla, A.

2018-06-01

BaSnO3 has attracted attention as a transparent conducting oxide with high room temperature carrier mobility. We report a series of measurements that were carried out to assess the structure of BaSnO3 over a variety of length scales. Measurements included single crystal neutron and x-ray diffraction, Rietveld and pair distribution analysis of neutron powder diffraction, Raman scattering, and high-pressure x-ray diffraction. Results from the various diffraction probes indicate that both the long-range and local structures are consistent with the cubic symmetry. The diffraction data under pressure was consistent with a robustly cubic phase up to 48.9 GPa, which is supported bymore » density functional calculations. Additionally, transverse phonon velocities were determined from measured dispersion of the transverse acoustic phonon branches, the results of which are in good agreement with previous theoretical estimates and ultrasound measurements.« less

Neutron Diffraction Structure of Melampodin: Its Role in the Reclassification of the Germacranolides

PubMed Central

Watkins, Steven F.; Fischer, Nikolaus H.; Bernal, Ivan

1973-01-01

The precise crystal and molecular structure of melampodin, C21H24O9, was determined from three-dimensional neutron diffraction data collected by counter techniques and phases by direct statistical methods. Crystals are orthorhombic, P212121, a = 8,990(9), b = 14.352(14), c = 16.294(16) Å, V = 2102 Å3, d(calc.) = 1.328 g·cm-3, Z = 4 molecules per unit cell. The structural model was refined by full matrix least-squares of 2303 observed independent reflections, with all 54 atoms treated anisotropically, to R(F) = 5.0%. Hydrogen bonds link melampodin molecules together in the solid state. The conformation of the cyclodeca-1,5-diene ring is such that one intraannular hydrogen atom interacts strongly with one double bond, but there is little or no transannular interaction between double bonds. Strain in the ten-membered ring and in the trans-fused lactone ring is discussed, as are chemical implications of the unsymmetric epoxide in the epoxyangelic acid side chain. The previously suggested reclassification of germacranolide sesquiterpene lactones into four subgroups is supported, and a new convention for configurational representations of the four subgroups is proposed. PMID:16592106

Unified structure theory of icosahedral quasicrystals: Evidence from neutron powder diffraction patterns that AlCrFeMnSi, AlCuLiMg, and TiNiFeSi icosahedral quasicrystals are twins of cubic crystals containing about 820 or 1012 atoms in a primitive unit cube

PubMed Central

Pauling, Linus

1988-01-01

A unified structure theory of icosahedral quasicrystals, combining the twinned-cubic-crystal theory and the Penrose-tiling-six-dimensional-projection theory, is described. Values of the primitive-cubic lattice constant for several quasicrystals are evaluated from x-ray and neutron diffraction data. The fact that the low-angle diffraction maxima can be indexed with cubic unit cells provides additional support for the twinned-cubic-crystal theory of icosahedral quasicrystals. PMID:16593990

The sciences and applications of the Electron LINAC-driven neutron source in Argentina

NASA Astrophysics Data System (ADS)

Granada, J. R.; Mayer, R. E.; Dawidowski, J.; Santisteban, J. R.; Cantargi, F.; Blostein, J. J.; Rodríguez Palomino, L. A.; Tartaglione, A.

2016-06-01

The Neutron Physics group at Centro Atómico Bariloche (CNEA, Argentina) has evolved for more than forty five years around a small 25MeV linear electron accelerator. It constitutes our compact accelerator-driven neutron source (CANS), which is dedicated to the use and development of neutronic methods to tackle problems of basic sciences and technological applications. Its historical first commitment has been the determination of the total cross sections of materials as a function of neutron energy by means of transmission experiments for thermal and sub-thermal neutrons. This also allowed testing theoretical models for the generation of scattering kernels and cross sections. Through the years, our interests moved from classic pulsed neutron diffraction, which included the development of high-precision methods for the determination of very low hydrogen content in metals, towards deep inelastic neutron scattering (DINS), a powerful tool for the determination of atomic momentum distribution in condensed matter. More recently non-intrusive techniques aimed at the scanning of large cargo containers have started to be developed with our CANS, testing the capacity and limitations to detect special nuclear material and dangerous substances. Also, the ever-present "bremsstrahlung" radiation has been recognized and tested as a useful complement to instrumental neutron activation, as it permits to detect other nuclear species through high-energy photon activation. The facility is also used for graduate and undergraduate students' experimental work within the frame of Instituto Balseiro Physics and Nuclear Engineering courses of study, and also MSc and PhD theses work.

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr 4 S 8

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

Pokharel, G.; May, A. F.; Parker, D. S.

In this paper, the physical properties of the spinel LiGaCr 4S 8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. Finally, these results indicate strong magnetoelastic coupling in LiGaCrmore » 4S 8.« less

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr 4 S 8

DOE PAGES

Pokharel, G.; May, A. F.; Parker, D. S.; ...

2018-04-30

In this paper, the physical properties of the spinel LiGaCr 4S 8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. Finally, these results indicate strong magnetoelastic coupling in LiGaCrmore » 4S 8.« less

Sensitivity Analysis and Simulation of Theoretical Response of Ceramics to Strong Magnetic Fields

DTIC Science & Technology

2016-09-01

Weapons and Materials Research Directorate, ARL Approved for public release; distribution is unlimited. FOR OFFICIAL USE ONLY...Compounds. 2013;551:568–577. 4. Terada N, Suzuki HS, Suzuki TS, Kitazawa H, Sakka Y, Kaneko K, Metoki N. In situ neutron diffraction study of...TS, Kitazawa H, Sakka Y, Kaneko K, Metoki N. Neutron diffraction texture analysis for alpha-Al2O3 oriented by a high magnetic field and sintering

Neutron diffraction studies on cobalt substituted BiFeO3

NASA Astrophysics Data System (ADS)

Ray, J.; Biswal, A. K.; Acharya, S.; Babu, P. D.; Siruguri, V.; Vishwakarma, P. N.

2013-02-01

A dilute concentration of single phase Cobalt substituted Bismuth ferrite, BiFe1-XCoXO3; (x=0, 0.02) is prepared by sol-gel auto combustion method. Room temperature neutron diffraction patterns show no change in the crystal and magnetic structure upon cobalt doping. The calculation of magnetic moments shows 3.848 μB for Fe+ and 2.85 μB for Co3+. The cobalt is found to be in intermediate spin state.

Neutron Diffraction Studies of Some Rare Earth-Transition Metal Deuterides.

DTIC Science & Technology

1986-05-01

RD-A168 M NEUTRON DIFFRACTION STUDIES OF SONE RARE EARTH-TRANSITION METAL DEUTERIDES(U) MISSOURI UNIV-ROLLR MATERIALS RESEARCH CENTER N J JAMES MY 86...REPORT William J. James OTtO -il May 1986 ZLECTEJU U. S. Army Research Office DAAG29-83-K-01 59 ".;’ Graduate Center for Materials Research ...9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT, PROJECT. TASK AREA & WORK UNIT NUMBERS 2* Graduate Center for Materials Research

Morin-like spin canting in the magnetic CaFe{sub 5}O{sub 7} ferrite: A combined neutron and Mössbauer study

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

Delacotte, C.; Bréard, Y.; Caignaert, V.

2017-03-15

Magnetic structure of CaFe{sub 5}O{sub 7} ferrite has been studied jointly from neutron powder diffraction data and spectroscopic Mössbauer measurements in the thermal range from 5 to 500 K. This coupled work highlights three distinct magnetic domains around two specific temperatures: T{sub M}=125 K and T{sub N}=360 K. The latter corroborates the structural monoclinic-orthorhombic transition previously reported by transmission electron microscopy techniques and X-ray thermodiffractometry. Complementary heat capacity measurements have confirmed this first order transition with a sharp peak at 360 K. Interestingly, this large study has revealed a second magnetic transition associated to a spin rotation at 125 Kmore » similar to this one reported by Morin in α-Fe{sub 2}O{sub 3} hematite at T{sub M}=260 K. - Graphical abstract: Magnetic structure of CaFe{sub 5}O{sub 7} ferrite has been studied jointly from neutron powder diffraction data and spectroscopic Mössbauer measurements in the thermal range from 5 to 500 K. This coupled work highlights three distinct magnetic domains around two specific temperatures: T{sub M}=125 K and T{sub N}=360 K. Interestingly, this large study has revealed a magnetic transition associated to a spin rotation at 125 K similar to this one reported by Morin in α-Fe{sub 2}O{sub 3} hematite at T{sub M}=260 K.« less

Beam modulation: A novel ToF-technique for high resolution diffraction at the Beamline for European Materials Engineering Research (BEER)

NASA Astrophysics Data System (ADS)

Rouijaa, M.; Kampmann, R.; Šaroun, J.; Fenske, J.; Beran, P.; Müller, M.; Lukáš, P.; Schreyer, A.

2018-05-01

The Beamline for European Materials Engineering Research (BEER) is under construction at the European Spallation Source (ESS) in Lund, Sweden. A basic requirement on BEER is to make best use of the long ESS pulse (2.86 ms) for engineering investigations. High-resolution diffraction, however, demands timing resolution up to 0.1% corresponding to a pulse length down to about 70 μs for the case of thermal neutrons (λ ∼ 1.8 Å). Such timing resolution can be achieved by pulse shaping techniques cutting a short section out of the long pulse, and thus paying for resolution by strong loss of intensity. In contrast to this, BEER proposes a novel operation mode called pulse modulation technique based on a new chopper design, which extracts several short pulses out of the long ESS pulse, and hence leads to a remarkable gain of intensity compared to nowadays existing conventional pulse shaping techniques. The potential of the new technique can be used with full advantage for investigating strains and textures of highly symmetric materials. Due to its instrument design and the high brilliance of the ESS pulse, BEER is expected to become the European flagship for engineering research for strain mapping and texture analysis.

POWTEX Neutron Diffractometer at FRM II - New Perspectives in Rock Deformation and Recrystallisation Analysis

NASA Astrophysics Data System (ADS)

Walter, J. M.; Stipp, M.; Ullemeyer, K.; Klein, H.; Leiss, B.; Hansen, B.; Kuhs, W. F.

2011-12-01

Neutron diffraction has become a routine method in Geoscience for the quantitative analysis of crystallographic preferred orientations (CPOs) and for (experimental) powder diffraction. Quantitative texture analysis is a common tool for the investigation of fabric development in mono- and polyphase rocks, their deformation histories and kinematics. Furthermore the quantitative characterization of anisotropic physical properties by bulk texture measurements can be achieved due to the high penetration capabilities of neutrons. To cope with increasing needs for beam time at neutron diffraction facilities with the corresponding technical characteristics and equipment, POWTEX (POWder and TEXture Diffractometer) is designed as a high-intensity diffractometer at the neutron research reactor FRM II in Garching, Germany by groups from the RWTH Aachen, Forschungszentrum Jülich and the University of Göttingen. Complementary to existing neutron diffractometers (SKAT at Dubna, Russia; GEM at ISIS, UK; HIPPO at Los Alamos, USA; D20 at ILL, France; and the local STRESS-SPEC and SPODI at FRM II) the layout of POWTEX is focused on fast (texture) measurements for either time-resolved experiments or the measurement of larger sample series as necessary for the study of large scale geological structures. By utilizing a range of neutron wavelengths simultaneously (TOF-technique), a high flux (~1 x 107 n/cm2s) and a high detector coverage ( 9.8 sr) effective texture measurements without sample tilting and rotation are possible. Furthermore the instrument and the angular detector resolution is sufficient for strong recrystallisation textures as well as weak textures of polyphase rocks. Thereby large sample environments will be implemented at POWTEX allowing in-situ time-resolved texture measurements during deformation experiments on rocksalt, ice and other materials. Furthermore a furnace for 3D-recrystallisation analysis of single grains will be realized complementary to the furnace that already exists for fine grained materials at the synchrotron beamline BW5 at HASYLAB, Germany (e.g. Klein et al. 2009). The in-situ triaxial deformation apparatus is operated by a uniaxial spindle drive with a maximum axial load of 200 kN, which will be redesigned to minimize shadowing effects on the detector. The HT experiments will be carried out in uniaxial compression or extension and an upgrade to triaxial deformation conditions is envisaged. The load frame can alternatively be used for ice deformation by inserting a cryostat cell for temperatures down to 77 K with a triaxial apparatus allowing also simple shear experiments on ice. Strain rates range between 10-8 and 10-3 s-1 reaching to at least 50 % axial strain. The furnace for the recrystallization analysis will be a mirror furnace with temperatures up to 1500° C, which will be rotatable around a vertical axis to obtain the required stereologic orientation information.

High-pressure studies on Ba-doped cobalt perovskites by neutron diffraction

NASA Astrophysics Data System (ADS)

Cao, Huibo; Garlea, Vasile; Wang, Fangwei; Dos Santos, Antonio; Cheng, Zhaohua

2012-02-01

Cobalt perovskite possess rich structural, magnetic and electrical properties depending on the subtle balance of the interactions among the spin, charge, and orbital degrees of freedom. Divalent hole-doped cobalt perovskites LaA^2+CoO3 exhibit structural phase transitions, metal-insulator transitions, and multi-magnetic phase transitions. High-pressure measurement is believed to mimic the size effects of the doped ions. We performed neutron diffraction experiments on selected Ba-doped LaCoO3 under pressures up to 6.3 GPa at SNAP at Spallation Neutron Source of ORNL. This work focuses on the high-pressure effects of the selected Ba-doped samples and the change of the phase diagram with pressure.

Quantum correlations and Bell’s inequality violation in a Heisenberg spin dimer via neutron scattering

NASA Astrophysics Data System (ADS)

Cruz, C.

The characterization of quantum information quantifiers has attracted a considerable attention of the scientific community, since they are a useful tool to verify the presence of quantum correlations in a quantum system. In this context, in the present work we show a theoretical study of some quantifiers, such as entanglement witness, entanglement of formation, Bell’s inequality violation and geometric quantum discord as a function of the diffractive properties of neutron scattering. We provide one path toward identifying the presence of quantum correlations and quantum nonlocality in a molecular magnet as a Heisenberg spin-1/2 dimer, by diffractive properties typically obtained via neutron scattering experiments.

The Macromolecular Neutron Diffractometer MaNDi at the Spallation Neutron Source

DOE PAGES

Coates, Leighton; Cuneo, Matthew J.; Frost, Matthew J.; ...

2015-07-18

The Macromolecular Neutron Diffractometer (MaNDi) is located on beamline 11B of the Spallation Neutron Source at Oak Ridge National Laboratory. Moreover, the instrument is a neutron time-of-flight wavelength-resolved Laue diffractometer optimized to collect diffraction data from single crystals. Finally, the instrument has been designed to provide flexibility in several instrumental parameters, such as beam divergence and wavelength bandwidth, to allow data collection from a range of macromolecular systems.

Preferred Orientation of Rare Earth (RE)-Doped Alumina Crystallites by an Applied Magnetic Field

DTIC Science & Technology

2016-06-01

Magnetic Field by Victoria L Blair, Raymond E Brennan, and Jane W Adams Weapons and Materials Research Directorate, ARL Carli A Moorehead...public release; distribution is unlimited. 16 13. Terada N, Suzuki HS, Suzuki TS, Kitazawa H, Sakka Y, Kaneko K, Metok N. In situ neutron diffraction...HS, Suzuki TS, Kitazawa H, Sakka Y, Kaneko K, Metoki N. Neutron diffraction texture analysis for alpha-Al2O3 oriented by high magnetic field and

Residual-stress measurement in socket welded joints by neutron diffraction

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

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

1994-12-31

Neutron diffraction measurements of lattice strains provide spatial maps of residual stress near welds in ferritic steel socket joints. The highest tensile stresses in the welds are found in axial, radial and hoop direction at the weld root. However, the highest tensile stress in the axial direction is about 110MPa. Balancing compressive stresses are found near the surface of the socket weld fusion zone. Heat treatment at 600 C for 2 hours is sufficient to relieve residual stress in socket welds.

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.

Magnetic structure of the swedenborgite CaBa (Co3Fe ) O7 derived by unpolarized neutron diffraction and spherical neutron polarimetry

NASA Astrophysics Data System (ADS)

Qureshi, N.; Díaz, M. T. Fernández; Chapon, L. C.; Senyshyn, A.; Schweika, W.; Valldor, M.

2018-02-01

We present a study that combines polarized and unpolarized neutrons to derive the magnetic structure of the swedenborgite compound CaBa (Co3Fe ) O7. Integrated intensities from a standard neutron diffraction experiment and polarization matrices from spherical neutron polarimetry have been simultaneously analyzed revealing a complex order, which differs from the usual spin configurations on a kagome lattice. We find that the magnetic structure is well described by a combination of two one-dimensional representations corresponding to the magnetic superspace symmetry P 21' , and it consists of spins rotating around an axis close to the [110] direction. Due to the propagation vector q =(1/3 00 ) , this modulation has cycloidal and helicoidal character rendering this system a potential multiferroic. The resulting spin configuration can be mapped onto the classical √{3 }×√{3 } structure of a kagome lattice, and it indicates an important interplay between the kagome and the triangular layers of the crystal structure.

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.

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

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

Mueser, Timothy C., E-mail: timothy.mueser@utoledo.edu; Griffith, Wendell P.; Kovalevsky, Andrey Y.

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-raymore » 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.« less

Evolution in boron-based GEM detectors for diffraction measurements: from planar to 3D converters

NASA Astrophysics Data System (ADS)

Albani, Giorgia; Perelli Cippo, Enrico; Croci, Gabriele; Muraro, Andrea; Schooneveld, Erik; Scherillo, Antonella; Hall-Wilton, Richard; Kanaki, Kalliopi; Höglund, Carina; Hultman, Lars; Birch, Jens; Claps, Gerardo; Murtas, Fabrizio; Rebai, Marica; Tardocchi, Marco; Gorini, Giuseppe

2016-11-01

The so-called ‘3He-crisis’ has motivated the neutron detector community to undertake an intense R&D programme in order to develop technologies alternative to standard 3He tubes and suitable for neutron detection systems in future spallation sources such as the European spallation source (ESS). Boron-based GEM (gas electron multiplier) detectors are a promising ‘3He-free’ technology for thermal neutron detection in neutron scattering experiments. In this paper the evolution of boron-based GEM detectors from planar to 3D converters with an application in diffraction measurements is presented. The use of 3D converters coupled with GEMs allows for an optimization of the detector performances. Three different detectors were used for diffraction measurements on the INES instrument at the ISIS spallation source. The performances of the GEM-detectors are compared with those of conventional 3He tubes installed on the INES instrument. The conceptual detector with the 3D converter used in this paper reached a count rate per unit area of about 25% relative to the currently installed 3He tube. Its timing resolution is similar and the signal-to-background ratio (S/B) is 2 times lower.

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.

Structure and texture analysis of PVC foils by neutron diffraction.

PubMed

Kalvoda, L; Dlouhá, M; Vratislav, S

2010-01-01

Crystalline order of molded and then bi-axially stretched foils prepared from atactic PVC resin is investigated by means of wide-angle neutron diffraction (WAND). The observed high-resolution WAND patterns of all samples are dominated by a sharp maximum corresponding to the inter-planar distance 0.52 nm. Two weaker maxima are also resolved at 0.62 and 0.78 nm. Intensities of the peaks vary with deformation ratios of the samples and their diffraction position. Average size of the coherently scattering domains is estimated as approximately 4-8 nm. Based on the experimental data, a novel model of crystalline order of atactic PVC is proposed. Copyright 2009 Elsevier Ltd. All rights reserved.

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

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

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

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

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

DOE PAGES

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

2017-04-28

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

Influence of neutron irradiation on the microstructure of nuclear graphite: An X-ray diffraction study

NASA Astrophysics Data System (ADS)

Zhou, Z.; Bouwman, W. G.; Schut, H.; van Staveren, T. O.; Heijna, M. C. R.; Pappas, C.

2017-04-01

Neutron irradiation effects on the microstructure of nuclear graphite have been investigated by X-ray diffraction on virgin and low doses (∼ 1.3 and ∼ 2.2 dpa), high temperature (750° C) irradiated samples. The diffraction patterns were interpreted using a model, which takes into account the turbostratic disorder. Besides the lattice constants, the model introduces two distinct coherent lengths in the c-axis and the basal plane, that characterise the volumes from which X-rays are scattered coherently. The methodology used in this work allows to quantify the effect of irradiation damage on the microstructure of nuclear graphite seen by X-ray diffraction. The results show that the changes of the deduced structural parameters are in agreement with previous observations from electron microscopy, but not directly related to macroscopic changes.

Analytical solutions for determining residual stresses in two-dimensional domains using the contour method

PubMed Central

Kartal, Mehmet E.

2013-01-01

The contour method is one of the most prevalent destructive techniques for residual stress measurement. Up to now, the method has involved the use of the finite-element (FE) method to determine the residual stresses from the experimental measurements. This paper presents analytical solutions, obtained for a semi-infinite strip and a finite rectangle, which can be used to calculate the residual stresses directly from the measured data; thereby, eliminating the need for an FE approach. The technique is then used to determine the residual stresses in a variable-polarity plasma-arc welded plate and the results show good agreement with independent neutron diffraction measurements. PMID:24204187

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

PubMed

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

2010-01-14

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

Phase diagram of the relaxor ferroelectric (1- x )Pb(Mg 1/3Nb 2/3)O 3+ x PbTiO 3 revisited: a neutron powder diffraction study of the relaxor skin effect

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

Phelan, D.; Rodriguez, E. E.; Gao, J.

2014-11-17

We revisit the phase diagram of the relaxor ferroelectric PMN- xPT using neutron powder diffraction to test suggestions that residual oxygen vacancies and/or strain affect the ground state crystal structure. Powdered samples of PMN- xPT were prepared with nominal compositions of x = 0:10, 0.20, 0.30, and 0.40 and divided into two identical sets, one of which was annealed in air to relieve grinding-induced strain and to promote an ideal oxygen stoichiometry. For a given composition and temperature the same structural phase is observed for each specimen. However, the distortions in all of the annealed samples are smaller than thosemore » in the as-grown samples. Further, the diffraction patterns for x = 0:10, 0.20, and 0.30 are best refined using the monoclinic Cm space group. By comparing our neutron diffraction results to those obtained on single crystals having similar compositions, we conclude that the relaxor skin effect in PMN- xPT vanishes on the Ti-rich side of the morphotropic phase boundary.« less

Neutron diffraction study of the martensitic transformation and chemical order in Heusler alloy Ni 1.91Mn 1.29Ga 0.8

DOE PAGES

Ari-Gur, Pnina; Garlea, Vasile O.; Cao, Huibo; ...

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 Ni 1.91Mn 1.29Ga 0.8 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 spacemore » group P 1 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

Magnetic moment distribution modeling in non stoichiometric Ni-Mn-Ga ferromagnetic shape memory alloys

NASA Astrophysics Data System (ADS)

Lázpita, P.; Gutiérrez, J.; Barandiarán, J. M.; Chernenko, V. A.; Mondelli, C.; Chapon, L.

2014-11-01

Neutron polarized diffraction technique has been used to elucidate the magnetic moment distribution density in non stoichiometric Ni—Mn—Ga single crystals. These experiments allow us to determine a localized magnetic moment in the Mn position in the austenitic phase, and to validity qualitatively previous models of magnetic distributions where there are antiferromagnetic and ferromagnetic coupling for Mn atoms that are sited out of their properly positions. This measurements show the deep dependence of the magnetic moment with the composition and the atomic order.

Short-range order of undercooled melts of PdZr2 intermetallic compound studied by X-ray and neutron scattering experiments

NASA Astrophysics Data System (ADS)

Klein, S.; Holland-Moritz, D.; Herlach, D. M.; Mauro, N. A.; Kelton, K. F.

2013-05-01

The short-range order in undercooled melts of the intermetallic Zr2Pd glass-forming alloy is investigated by combining electrostatic levitation (ESL) with high-energy X-ray diffraction and neutron diffraction. Experimentally determined structure factors are measured and analyzed with respect to various structures of short-range order. The comparative X-ray and neutron scattering experiments allow for investigations of topological and chemical short-range order. Based on these studies, no preference of a specific short-range order is found for the liquid Zr2Pd glass-forming alloy, even in the metastable state of the deeply undercooled melt. This is in agreement with an earlier report from X-ray diffraction and molecular-dynamics studies of a Zr75.5Pd24.5 liquid, which showed a broad distribution of cluster types. The results for the Zr2Pd liquid are discussed with respect to the glass-forming ability of this melt.

Magnetic and neutron diffraction study on quaternary oxides MTeMoO6 (M = Mn and Zn)

NASA Astrophysics Data System (ADS)

Doi, Yoshihiro; Suzuki, Ryo; Hinatsu, Yukio; Ohoyama, Kenji

2009-01-01

Crystal structures and magnetic properties of quaternary oxides MTeMoO6 (M = Mn and Zn) were investigated. From the Rietveld analyses for the powder x-ray and neutron diffraction measurements, their detailed structures have been determined. Both compounds have orthorhombic structure with space group P 21212 and a charge configuration of M2+Te4+Mo6+O6. ZnTeMoO6 shows diamagnetic behavior. In this structure, M ions are arranged in a square-planar manner. The temperature dependence of the magnetic susceptibility for MnTeMoO6 shows a broad peak at ~33 K, which is due to a two-dimensional characteristic of the magnetic interaction. In addition, this compound shows an antiferromagnetic transition at 20 K. The magnetic structure was determined by the powder neutron diffraction measurement at 3.3 K. The magnetic moments of Mn2+ ions (4.45 μB) order in a collinear antiferromagnetic arrangement along the b axis.

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

DOE PAGES

Garlea, Elena; Steiner, M. A.; Calhoun, C. A.; ...

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

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

NASA Astrophysics Data System (ADS)

Fiori, F.; Marcantoni, M.

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

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

Structural analysis of PrBaMn2O5+δ under SOFC anode conditions by in-situ neutron powder diffraction

NASA Astrophysics Data System (ADS)

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

2016-10-01

The crystal structure and oxygen stoichiometry of the proposed double perovskite solid oxide fuel cell (SOFC) anode material PrBaMn2O5+δ were determined under SOFC anode conditions via in-situ neutron diffraction. Measurements were performed in reducing atmospheres between 692 K and 984 K. The structure was fit to a tetragonal (space group P4/mmm) layered double perovskite structure with alternating Pr and Ba A-site cation layers. Under all conditions examined, the oxygen sites in the Ba and Mn layers were fully occupied, while the sites in the Pr layer were close to completely vacant. The results of the neutron diffraction experiments are compared to previous thermogravimetric analysis experiments to verify the accuracy of both experiments. PrBaMn2O5+δ was shown to be stable over a wide range of reducing atmospheres similar to anode operating conditions in solid oxide fuel cells without significant structural changes.

Hydrogenation properties of Li{sub x}Sr{sub 1−x}AlSi studied by quantum-chemical methods (0≤x≤1) and in-situ neutron powder diffraction (x=1)

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

Kunkel, Nathalie, E-mail: nathalie.kunkel@chimie-paristech.fr; FR 8.1 Universität des Saarlandes, Postach 151150, 66041 Saarbrücken; Reichert, Christian

2015-01-15

In-situ neutron powder diffraction studies of the Half-Heusler phase LiAlSi under high deuterium pressures and first principle calculations of solid solutions of Li{sub x}Sr{sub 1−x}AlSi and their hydrides Li{sub x}Sr{sub 1−x}AlSiH were carried out. In contrast to an earlier study, there is no experimental evidence for hydrogen (deuterium) uptake up to gas pressures of 15 MPa and temperatures of 550 °C. Instead a slow decomposition reaction according to LiAlSi+1/2H{sub 2}=LiH+Al+Si was found by in-situ neutron powder diffraction. Theoretical calculations by DFT methods on hypothetical solid solutions of Li{sub x}Sr{sub 1−x}AlSi show the LiAlSi type to be the energetically most stablemore » structure for 0.7« less

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.

Neutron diffraction study of the in situ oxidation of UO(2).

PubMed

Desgranges, Lionel; Baldinozzi, Gianguido; Rousseau, Gurvan; Nièpce, Jean-Claude; Calvarin, Gilbert

2009-08-17

This paper discusses uranium oxide crystal structure modifications that are observed during the low-temperature oxidation which transforms UO(2) into U(3)O(8). The symmetries and the structural parameters of UO(2), beta-U(4)O(9), beta-U(3)O(7), and U(3)O(8) were determined by refining neutron diffraction patterns on pure single-phase samples. Neutron diffraction patterns were also collected during the in situ oxidation of powder samples at 483 K. The lattice parameters and relative ratios of the four pure phases were measured during the progression of the isothermal oxidation. The transformation of UO(2) into U(3)O(8) involves a complex modification of the oxygen sublattice and the onset of complex superstructures for U(4)O(9) and U(3)O(7), associated with regular stacks of complex defects known as cuboctahedra, which consist of 13 oxygen atoms. The kinetics of the oxidation process are discussed on the basis of the results of the structural analysis.

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

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

Christien, F., E-mail: frederic.christien@univ-nantes.fr; Le Gall, R.; Telling, M. T. F.

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 rampingmore » 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.« less

Neutron Characterization of Encapsulated ATF-1/LANL-1 Mockup Fuel Capsules

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

Vogel, Sven C.; Borges, Nicholas Paul; Losko, Adrian Simon

Twenty pellets of mock-up accident tolerant fuels UN-U3Si5 were produced at LANL and loaded in two rodlet/capsule assemblies. Tomographic imaging and diffraction measurements were performed to characterize these samples at the Flight-Path 5 and HIPPO beam lines at LANSCE/LANL between November 2016 and January 2017 as well as in August 2017. The entire ~10 cm long, ~1 cm diameter fuel volume could be characterized, however due to time constraints only 2 mm slices in 4mm increments were characterized with neutron diffraction and a 28mm subset of the entire sample was characterized with energy-resolved neutron imaging. The double encapsulation of themore » fuel into two steel containers does not pose a problem for the neutron analysis and the methods could be applied to enriched as well irradiated fuels.« less

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

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

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

2017-01-31

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

Revealing the effect of edge contamination on vortex matter structure in a Nb single crystal with neutron diffraction techniques

NASA Astrophysics Data System (ADS)

Hanson, Helen; Wang, Xi; Luk, Michael; Shi, Jing; Ling, Xinsheng; Maranville, Brian; Majkrzak, Charles

2011-03-01

The vortex matter of type II superconductors provides a model system to study the effect of quenched random disorder on an elastic lattice, particularly in the framework of Bragg glass theory. Neutron scattering techniques are used to examine the structure of the vortex matter and to quantify the phase diagram. After measuring various thermal-magnetic histories, our data provided evidence for the edge contamination model in a Nb single crystal. Since surface oxidation is known to suppress the Bean-Livingston Surface barrier and the inhomogeneous distribution of surface impurities in Nb, we oxidize our sample surface and repeat our measurements. By comparing the data, we are able isolate the dynamic impact of the edge disorder from the static influence of bulk pinning. We discuss the various experimental obstacles in measuring the predicted Bragg glass state. We also report on Reverse Monte Carlo Refinement simulations modeling possible structures of our vortex matter. This research was supported by the U.S. DOE under grant DE- FG 02 - 07 ER46458.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review.

PubMed

Dwivedi, D; Lepkova, K; Becker, T

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

NASA Astrophysics Data System (ADS)

Dwivedi, D.; Lepkova, K.; Becker, T.

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

PubMed Central

Dwivedi, D.; Becker, T.

2017-01-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed. PMID:28413351

Structure and mechanical behavior of heavily drawn pearlite and martensite in a high carbon steel

NASA Astrophysics Data System (ADS)

Shiota, Y.; Tomota, Y.; Moriai, A.; Kamiyama, T.

2005-10-01

Neutron diffraction measurements have revealed that cementite peaks disappear in a pearlite steel with drawing and that the residual intergranular stresses are generated. The diffraction profiles in a heavily drawn specimen suggest the tetoragonality with a small c/a in the ferrite matrix. Although cementite was hardly observed in the heavily drawn specimen, its c/a value determined by neutron diffraction and mechanical behavior are quite different from those of as-quenched martensite. The changes in hardness and c/a with annealing or tempering were also different between heavily drawn pearlite and marteniste. Hence, most of carbon atoms do not exist inside the ferrite lattice in the drawn pearlite and multi-scaled heterogeneous plastic deformation in pearlite seems to affect the asymmetry in the diffraction profile. Fracture behavior and hardness change with tempering is different in the two microstructures.

Crystallization of a fungal lytic polysaccharide monooxygenase expressed from glycoengineered Pichia pastoris for X-ray and neutron diffraction

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

O'Dell, William B.; Swartz, Paul D.; Weiss, Kevin L.

Lytic polysaccharide monooxygenases (LPMOs) are carbohydrate-disrupting enzymes secreted by bacteria and fungi that break glycosidic bondsviaan oxidative mechanism. Fungal LPMOs typically act on cellulose and can enhance the efficiency of cellulose-hydrolyzing enzymes that release soluble sugars for bioethanol production or other industrial uses. The enzyme PMO-2 fromNeurospora crassa(NcPMO-2) was heterologously expressed inPichia pastoristo facilitate crystallographic studies of the fungal LPMO mechanism. Diffraction resolution and crystal morphology were improved by expressingNcPMO-2 from a glycoengineered strain ofP. pastorisand by the use of crystal seeding methods, respectively. These improvements resulted in high-resolution (1.20 Å) X-ray diffraction data collection at 100 K and themore » production of a largeNcPMO-2 crystal suitable for room-temperature neutron diffraction data collection to 2.12 Å resolution.« less

Three-dimensional welding residual stresses evaluation based on the eigenstrain methodology via X-ray measurements at the surface

NASA Astrophysics Data System (ADS)

Ogawa, Masaru

2014-12-01

In order to assure structural integrity for operating welded structures, it is necessary to evaluate crack growth rate and crack propagation direction for each observed crack non-destructively. Here, three dimensional (3D) welding residual stresses must be evaluated to predict crack propagation. Today, X-ray diffraction is used and the ultrasonic method has been proposed as non-destructive method to measure residual stresses. However, it is impossible to determine residual stress distributions in the thickness direction. Although residual stresses through a depth of several tens of millimeters can be evaluated non-destructively by neutron diffraction, it cannot be used as an on-site measurement technique. This is because neutron diffraction is only available in special irradiation facilities. Author pays attention to the bead flush method based on the eigenstrain methodology. In this method, 3D welding residual stresses are calculated by an elastic Finite Element Method (FEM) analysis from eigenstrains which are evaluated by an inverse analysis from released strains by strain gauges in the removal of the reinforcement of the weld. Here, the removal of the excess metal can be regarded as non-destructive treatment because toe of weld which may become crack starters can be eliminated. The effectiveness of the method has been proven for welded plates and pipes even with relatively lower bead height. In actual measurements, stress evaluation accuracy becomes poorer because measured values of strain gauges are affected by processing strains on the machined surface. In the previous studies, the author has developed the bead flush method that is free from the influence of the affecting strains by using residual strains on surface by X-ray diffraction. However, stress evaluation accuracy is not good enough because of relatively poor measurement accuracy of X-ray diffraction. In this study, a method to improve the estimation accuracy of residual stresses in this method is formulated, and it is shown numerically that inner welding residual stresses can be estimated accurately from the residual strains measured by X-ray diffraction.

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.

Study of the solid-state amorphization of (GaSb){sub 1-x}Ge{sub x} semiconductors by real-time neutron diffraction and electron microscopy

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

Fedotov, V. K., E-mail: fedotov@issp.ac.ru; Ponyatovsky, E. G.

2011-12-15

The spontaneous amorphization of high-pressure quenched phases of the GaSb-Ge system has been studied by neutron diffraction while slowly heating the phases at atmospheric pressure. The sequence of changes in the structural parameters of the initial crystalline phase and the final amorphous phase is established. The behavior of the phases and the correlation in the structural features of the phase transitions and anomalous thermal effects exhibit signs of the inhomogeneous model of solid-state amorphization.

On the atomic structure of liquid Ni-Si alloys: a neutron diffraction study

NASA Astrophysics Data System (ADS)

Gruner, S.; Marczinke, J.; Hennet, L.; Hoyer, W.; Cuello, G. J.

2009-09-01

The atomic structure of the liquid NiSi and NiSi2 alloys is investigated by means of neutron diffraction experiments with isotopic substitution. From experimental data-sets obtained using four Ni isotopes, partial structure factors and pair correlation functions are obtained by applying a reverse Monte Carlo modelling approach. Both alloys were found to exhibit a strong tendency to hetero-coordination within the first coordination shell. In particular, covalent Si-Si bonds with somewhat greater distances seem to influence the structure of the liquid NiSi alloy.

On the atomic structure of liquid Ni-Si alloys: a neutron diffraction study.

PubMed

Gruner, S; Marczinke, J; Hennet, L; Hoyer, W; Cuello, G J

2009-09-23

The atomic structure of the liquid NiSi and NiSi(2) alloys is investigated by means of neutron diffraction experiments with isotopic substitution. From experimental data-sets obtained using four Ni isotopes, partial structure factors and pair correlation functions are obtained by applying a reverse Monte Carlo modelling approach. Both alloys were found to exhibit a strong tendency to hetero-coordination within the first coordination shell. In particular, covalent Si-Si bonds with somewhat greater distances seem to influence the structure of the liquid NiSi alloy.

Twin-variant reorientation strain in Ni-Mn-Ga single crystal during quasi-static mechanical compression

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

Pramanick, Abhijit; An, Ke; Stoica, Alexandru Dan

2011-01-01

Twin variant reorientation in single crystal Ni-Mn-Ga during quasi-static mechanical compression was studied using in-situ neutron diffraction. The volume fraction of reoriented twin variants for different stress amplitudes were obtained from the changes in integrated intensities of high-order neutron diffraction peaks. It is shown that during compressive loading, ~85% of the twins were reoriented parallel to the loading direction resulting in a maximum macroscopic strain of ~5.5%, which is in agreement with measured macroscopic strain.

Deformation and Phase Transformation Processes in Polycrystalline NiTi and NiTiHf High Temperature Shape Memory Alloys

NASA Technical Reports Server (NTRS)

Benafan, Othmane

2012-01-01

The deformation and transformation mechanisms of polycrystalline Ni49.9Ti50.1 and Ni50.3Ti29.7Hf20 (in at.%) shape memory alloys were investigated by combined experimental and modeling efforts aided by an in situ neutron diffraction technique at stress and temperature. The thermomechanical response of the low temperature martensite, the high temperature austenite phases, and changes between these two states during thermomechanical cycling were probed and reported. In the cubic austenite phase, stress-induced martensite, deformation twinning and slip processes were observed which helped in constructing a deformation map that contained the limits over which each of the identified mechanisms was dominant. Deformation of the monoclinic martensitic phase was also investigated where the microstructural changes (texture, lattice strains, and phase fractions) during room-temperature deformation and subsequent thermal cycling were compared to the bulk macroscopic response. When cycling between these two phases, the evolution of inelastic strains, along with the shape setting procedures were examined and used for the optimization of the transformation properties as a function of deformation levels and temperatures. Finally, this work was extended to the development of multiaxial capabilities at elevated temperatures for the in situ neutron diffraction measurements of shape memory alloys on the VULCAN Diffractometer at Oak Ridge National Laboratory.

Chamber for mechanical testing in H2 with observation by neutron scattering

NASA Astrophysics Data System (ADS)

Connolly, Matthew; Bradley, Peter; Slifka, Andrew; Drexler, Elizabeth

2017-06-01

A gas-pressure chamber has been designed, constructed, and tested at a moderate pressure (3.4 MPa, 500 psi) and has the capability of mechanical loading of steel specimens for neutron scattering measurements. The chamber will allow a variety of in situ neutron scattering measurements: in particular, diffraction, quasielastic scattering, inelastic scattering, and imaging. The chamber is compatible with load frames available at the user facilities at the NIST Center for Neutron Research and Oak Ridge National Laboratory Spallation Neutron Source. A demonstration of neutron Bragg edge imaging using the chamber is presented.

Texture analysis at neutron diffractometer STRESS-SPEC

NASA Astrophysics Data System (ADS)

Brokmeier, H.-G.; Gan, W. M.; Randau, C.; Völler, M.; Rebelo-Kornmeier, J.; Hofmann, M.

2011-06-01

In response to the development of new materials and the application of materials and components in advanced technologies, non-destructive measurement methods of textures and residual stresses have gained worldwide significance in recent years. The materials science neutron diffractometer STRESS-SPEC at FRM II (Garching, Germany) is designed to be applied equally to texture and residual stress analyses by virtue of its very flexible configuration. Due to the high penetration capabilities of neutrons and the high neutron flux of STRESS-SPEC it allows a combined analysis of global texture, local texture, strain pole figure and FWHM pole figure in a wide variety of materials including metals, alloys, composites, ceramics and geological materials. Especially, the analysis of texture gradients in bulk materials using neutron diffraction has advantages over laboratory X-rays and EBSD for many scientific cases. Moreover, neutron diffraction is favourable for coarse-grained materials, where bulk information averaged over texture inhomogeneities is needed, and also stands out due to easy sample preparation. In future, the newly developed robot system for STRESS-SPEC will allow much more flexibility than an Eulerian cradle as on standard instruments. Five recent measurements are shown to demonstrate the wide range of possible texture applications at STRESS-SPEC diffractometer.

A brief History of Neutron Scattering at the Oak Ridge High Flux Isotope Reactor

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

Nagler, Stephen E; Mook Jr, Herbert A

2008-01-01

Neutron scattering at the Oak Ridge National Laboratory dates back to 1945 when Ernest Wollan installed a modified x-ray diffractometer on a beam port of the original graphite reactor. Subsequently, Wollan and Clifford Shull pioneered neutron diffraction and laid the foundation for an active neutron scattering effort that continued through the 1950s, using the Oak Ridge Research reactor after 1958, and, starting in 1966, the High Flux Isotope Reactor, or HFIR.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

PubMed

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

2018-05-01

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

Crystal structure studies with the Paris-Edinburgh cell: Neutron scattering aspects

NASA Astrophysics Data System (ADS)

Loveday, J. S.; Wilson, R. M.; Nelmes, R. J.; Besson, J. M.; Klotz, S.; Hamel, G.; Hull, S.

1994-07-01

The count rates achieved in neutron powder diffraction experiments create difficulties for high-pressure experiments because large sample volumes (˜100 mm3) must be used. Until recently it has been difficult to build suitable pressure cells with such large volumes and hence the maximum pressure for neutron diffraction has remained at the relatively low value of 3 GPa. We have now developed a pressure cell (the Paris-Edinburgh cell) which is capable of exceeding 10 GPa with a sample volume of ˜100 mm3 for use at the U.K. spallation source ISIS. Considerable effort has been devoted to the opimization of the cell, shielding, and detector geometry to enable the best possible data to be recorded. Finite-element calculations to correct for the systematic errors introduced by the attenuation of the pressure-cell materials have been developed and tested. As a result of this work we are now able to obtain accurate structural data to ˜12 GPa and recent studies of phase IV of ND3, the behaviour of the O-D bondlength in D2O ice VIII, and the structural pressure dependence of B4C illustrate the importance of the extension of neutron-diffraction studies to such pressures.

In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials

DOE PAGES

Liu, Y.; Wang, H.; Zhang, X.

2015-11-30

Though abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. We applied numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction in order to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. We briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. Moreover, in the amorphous CuZrAl, in situ nanoindentationmore » studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.« less

Structural and spectroscopic studies of a commercial glassy carbon

NASA Astrophysics Data System (ADS)

Parker, Stewart F.; Imberti, Silvia; Callear, Samantha K.; Albers, Peter W.

2013-12-01

Glassy carbon is a form of carbon made by heating a phenolic resin to high temperature in an inert atmosphere. It has been suggested that it is composed of fullerene-like structures. The aim of the present work was to characterize the material using both structural (neutron diffraction and transmission electron microscopy) and spectroscopic (inelastic neutron scattering, Raman and X-ray photoelectron spectroscopies) methods. We find no evidence to support the suggestion of fullerene-like material being present to a significant extent, rather the model that emerges from all of the techniques is that the material is very like amorphous carbon, consisting of regions of small graphite-like basic structural units of partly stacked but mismatched structure with the edges terminated by hydrogen or hydroxyls. We do find evidence for the presence of a small quantity of water trapped in the network and suggest that this may account for batch-to-batch variation in properties that may occur.

Neutron scattering study on cathode LiMn{sub 2}O{sub 4} and solid electrolyte 5(Li{sub 2}O)(P{sub 2}O{sub 5})

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

Kartini, E., E-mail: kartini@batan.go.id; Putra, Teguh P., E-mail: kartini@batan.go.id; Jahya, A. K., E-mail: kartini@batan.go.id

2014-09-30

Neutron scattering is very important technique in order to investigate the energy storage materials such as lithium-ion battery. The unique advantages, neutron can see the light atoms such as Hydrogen, Lithium, and Oxygen, where those elements are negligible by other corresponding X-ray method. On the other hand, the energy storage materials, such as lithium ion battery is very important for the application in the electric vehicles, electronic devices or home appliances. The battery contains electrodes (anode and cathode), and the electrolyte materials. There are many challenging to improve the existing lithium ion battery materials, in order to increase their lifemore » time, cyclic ability and also its stability. One of the most scientific challenging is to investigate the crystal structure of both electrode and electrolyte, such as cathodes LiCoO{sub 2}, LiMn{sub 2}O{sub 4} and LiFePO{sub 4}, and solid electrolyte Li{sub 3}PO{sub 4}. Since all those battery materials contain Lithium ions and Oxygen, the used of neutron scattering techniques to study their structure and related properties are very important and indispensable. This article will review some works of investigating electrodes and electrolytes, LiMn{sub 2}O{sub 4} and 5(Li{sub 2}O)(P{sub 2}O{sub 5}), by using a high resolution powder diffraction (HRPD) at the multipurpose research reactor, RSG-Sywabessy of the National Nuclear Energy Agency (BATAN), Indonesia.« less

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.

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

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

Ekkebus, Allen E

Oak Ridge National Laboratory hosted two workshops in April 2007 relevant to nuclear engineering education. In the Neutron Stress, Texture, and Phase Transformation for Industry workshop [http://neutrons.ornl.gov/workshops/nst2/], several invited speakers gave examples of neutron stress mapping for nuclear engineering applications. These included John Root of National Research Council of Canada, Mike Fitzpatrick of the UK's Open University, and Yan Gao of GE Global Research on their experiences with industrial and academic uses of neutron diffraction. Xun-Li Wang and Camden Hubbard described the new instruments at ORNL that can be used for such studies. This was preceded by the Neutrons formore » Materials Science and Engineering educational symposium [http://neutrons.ornl.gov/workshops/edsym2007]. It was directed to the broad materials science and engineering community based in universities, industry and laboratories who wish to learn what the neutron sources in the US can provide for enhancing the understanding of materials behavior, processing and joining. Of particular interest was the presentation of Donald Brown of Los Alamos about using 'Neutron diffraction measurements of strain and texture to study mechanical behavior of structural materials.' At both workshops, the ORNL neutron scattering instruments relevant to nuclear engineering studies were described. The Neutron Residual Stress Mapping Facility (NRSF2) is currently in operation at the High Flux Isotope Reactor; the VULCAN Engineering Materials Diffractometer will begin commissioning in 2008 at the Spallation Neutron Source. For characteristics of these instruments, as well as details of other workshops, meetings, capabilities, and research proposal submissions, please visit http://neutrons.ornl.gov. To submit user proposals for time on NRSF2 contact Hubbard at hubbardcr@ornl.gov.« less

Neutron diffraction determination of the cell dimensions and thermal expansion of the fluoroperovskite KMgF3 from 293 to 3.6 K

NASA Astrophysics Data System (ADS)

Mitchell, Roger H.; Cranswick, Lachlan M. D.; Swainson, Ian

2006-11-01

The cell dimensions of the fluoroperovskite KMgF3 synthesized by solid state methods have been determined by powder neutron diffraction and Rietveld refinement over the temperature range 293 3.6 K using Pt metal as an internal standard for calibration of the neutron wavelength. These data demonstrate conclusively that cubic Pmoverline{3} m KMgF3 does not undergo any phase transitions to structures of lower symmetry with decreasing temperature. Cell dimensions range from 3.9924(2) Å at 293 K to 3.9800(2) Å at 3.6 K, and are essentially constant within experimental error from 50 to 3.6 K. The thermal expansion data are described using a fourth order polynomial function.

Magnetic order in the frustrated Ising-like chain compound Sr3NiIrO6

NASA Astrophysics Data System (ADS)

Lefrançois, E.; Chapon, L. C.; Simonet, V.; Lejay, P.; Khalyavin, D.; Rayaprol, S.; Sampathkumaran, E. V.; Ballou, R.; Adroja, D. T.

2014-07-01

We have studied the field and temperature dependencies of the magnetization of single crystals of Sr3NiIrO6. These measurements evidence the presence of an easy axis of anisotropy and two anomalies in the magnetic susceptibility. Neutron powder diffraction realized on a polycrystalline sample reveals the emergence of magnetic reflections below 75 K with magnetic propagation vector k ˜ (0, 0, 1), undetected in previous neutron studies [T. N. Nguyen and H.-C. zur Loye, J. Solid State Chem. 117, 300 (1995), 10.1006/jssc.1995.1277]. The nature of the magnetic ground state, and the presence of two anomalies common to this family of material, are discussed on the basis of the results obtained by neutron diffraction, magnetization measurements, and symmetry arguments.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography.

PubMed

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-05-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A-H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A-H bond lengths with those from neutron measurements for A-H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography

PubMed Central

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M.; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-01-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A–H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A–H bond lengths with those from neutron measurements for A–H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors. PMID:27386545

Difficult macromolecular structures determined using X-ray diffraction techniques.

PubMed

Hernández-Santoyo, Alejandra

2012-07-01

Macromolecular crystallography has been, for the last few decades, the main source of structural information of biological macromolecular systems and it is one of the most powerful techniques for the analysis of enzyme mechanisms and macromolecular interactions at the atomic level. In addition, it is also an extremely powerful tool for drug design. Recent technological and methodological developments in macromolecular X-ray crystallography have allowed solving structures that until recently were considered difficult or even impossible, such as structures at atomic or subatomic resolution or large macromolecular complexes and assemblies at low resolution. These developments have also helped to solve the 3D-structure of macromolecules from twin crystals. Recently, this technique complemented with cryo-electron microscopy and neutron crystallography has provided the structure of large macromolecular machines with great precision allowing understanding of the mechanisms of their function.

Neutron detectors for the ESS diffractometers

NASA Astrophysics Data System (ADS)

Stefanescu, I.; Christensen, M.; Fenske, J.; Hall-Wilton, R.; Henry, P. F.; Kirstein, O.; Müller, M.; Nowak, G.; Pooley, D.; Raspino, D.; Rhodes, N.; Šaroun, J.; Schefer, J.; Schooneveld, E.; Sykora, J.; Schweika, W.

2017-01-01

The ambitious instrument suite for the future European Spallation Source whose civil construction started recently in Lund, Sweden, demands a set of diverse and challenging requirements for the neutron detectors. For instance, the unprecedented high flux expected on the samples to be investigated in neutron diffraction or reflectometry experiments requires detectors that can handle high counting rates, while the investigation of sub-millimeter protein crystals will only be possible with large-area detectors that can achieve a position resolution as low as 200 μm. This has motivated an extensive research and development campaign to advance the state-of-the-art detector and to find new technologies that can reach maturity by the time the ESS will operate at full potential. This paper presents the key detector requirements for three of the Time-of-Flight (TOF) diffraction instrument concepts selected by the Scientific Advisory Committee to advance into the phase of preliminary engineering design. We discuss the detector technologies commonly employed at the existing similar instruments and their major challenges for ESS. The detector technologies selected by the instrument teams to collect the diffraction patterns are also presented. Analytical calculations, Monte-Carlo simulations, and real experimental data are used to develop a generic method to estimate the event rate in the diffraction detectors. We apply this method to make predictions for the future diffraction instruments, and thus provide additional information that can help the instrument teams with the optimisation of the detector designs.

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates.

PubMed

Silva, Chinthaka M; Rosseel, Thomas M; Kirkegaard, Marie C

2018-03-19

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18 , 4 × 10 19 , and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasing neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2 , with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. The cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.

Evidence for monoclinic distortion in the ground state phase of underdoped La 1.95Sr 0.05CuO 4: A single crystal neutron diffraction study

DOE PAGES

Singh, Anar; Schefer, Jurg; Sura, Ravi; ...

2016-03-24

The existing controversy about the symmetry of the crystal structure of the ground state of the critical doped La 1.95Sr 0.05CuO 4 has been resolved by analyzing the single crystal neutron diffraction data collected between 5 and 730 K. We observed small but significant intensities for "forbidden" reflections given by extinction rules of the orthorhombic Bmab space group at low temperatures. A careful investigation of neutron diffraction data reveals that the crystal structure of La 1.95Sr 0.05CuO 4 at 5 K is monoclinic with B2/m (2/m 1 1) space group. The monoclinic structure emerges from the orthorhombic structure in amore » continuous way; however, the structure is stable below similar to 120K which agrees with other observed phenomena. Lastly, our results on symmetry changes are crucial for the interpretation of physical properties also in other high temperature superconductors with similar structures.« less

Low temperature magnetic properties of Nd2Ru2O7

NASA Astrophysics Data System (ADS)

Ku, S. T.; Kumar, D.; Lees, M. R.; Lee, W.-T.; Aldus, R.; Studer, A.; Imperia, P.; Asai, S.; Masuda, T.; Chen, S. W.; Chen, J. M.; Chang, L. J.

2018-04-01

We present magnetic susceptibility, heat capacity, and neutron diffraction measurements of polycrystalline Nd2Ru2O7 down to 0.4 K. Three anomalies in the magnetic susceptibility measurements at 146, 21 and 1.8 K are associated with an antiferromagnetic ordering of the Ru4+ moments, a weak ferromagnetic signal attributed to a canting of the Ru4+ and Nd3+ moments, and a long-range-ordering of the Nd3+ moments, respectively. The long-range order of the Nd3+ moments was observed in all the measurements, indicating that the ground state of the compound is not a spin glass. The magnetic entropy of Rln2 accumulated up to 5 K, suggests the Nd3+ has a doublet ground state. Lattice distortions accompany the transitions, as revealed by neutron diffraction measurements, and in agreement with earlier synchrotron x-ray studies. The magnetic moment of the Nd3+ ion at 0.4 K is estimated to be 1.54(2)µ B and the magnetic structure is all-in all-out as determined by our neutron diffraction measurements.

Evidence for monoclinic distortion in the ground state phase of underdoped La{sub 1.95}Sr{sub 0.05}CuO{sub 4}: A single crystal neutron diffraction study

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

Singh, Anar, E-mail: singhanar@gmail.com; Schefer, Jürg; Frontzek, Matthias

2016-03-28

The existing controversy about the symmetry of the crystal structure of the ground state of the critical doped La{sub 1.95}Sr{sub 0.05}CuO{sub 4} has been resolved by analyzing the single crystal neutron diffraction data collected between 5 and 730 K. We observed small but significant intensities for “forbidden” reflections given by extinction rules of the orthorhombic Bmab space group at low temperatures. A careful investigation of neutron diffraction data reveals that the crystal structure of La{sub 1.95}Sr{sub 0.05}CuO{sub 4} at 5 K is monoclinic with B2/m (2/m 1 1) space group. The monoclinic structure emerges from the orthorhombic structure in a continuous way;more » however, the structure is stable below ∼120 K which agrees with other observed phenomena. Our results on symmetry changes are crucial for the interpretation of physical properties also in other high temperature superconductors with similar structures.« less

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

DOE PAGES

Keller, L.; White, J. S.; Babkevich, P.; ...

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) μ B at ambient pressure to 0.4(1) μ B close to themore » critical pressure P c ≈ 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

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

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

Keller, L.; White, J. S.; Babkevich, P.

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) μ B at ambient pressure to 0.4(1) μ B close to themore » critical pressure P c ≈ 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

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.

Exploring Jupiter's icy moons with old techniques and big facilities - new insights on sulfuric acid hydrates

NASA Astrophysics Data System (ADS)

Maynard-Casely, H. E.; Avdeev, M.; Brand, H.; Wallwork, K.

2013-12-01

Sulfuric acid hydrates have been proposed to be abundant on the surface of Europa [1], and hence would be important planetary forming materials for this moon and its companions Ganymede and Callisto. Understanding of the surface features and subsurface of these moons could be advanced by firmer knowledge of the icy materials that comprise them [2], insight into which can be drawn from firmer knowledge of physical properties and phase behaviour of the candidate materials. We wish to present results from a study that started with the question ';What form of sulfuric acid hydrate would form on the surface of Europa'. The intrinsic hydrogen-domination of planetary ices, makes studying these materials with laboratory powder diffraction very challenging. Insights into their crystalline phase behavior and the extraction of a number of thermal and mechanical properties is often only accessible with high-flux synchrotron x-ray diffraction and utilization of the large scattering cross section with neutron diffraction. We have used the Powder Diffraction beamline at Australian synchrotron [4] and the Echidna (High-resolution neutron powder diffraction) instrument of the Australian Nuclear Science and Technology Organization, [5] to obtain an number of new insights into the crystalline phases formed from sulfruic acid and water mixtures. These instruments have enabled the discovery a new water-rich sulfuric acid hydrate form [6], improved structural characterisation of existing forms [7] and a charting the phase diagram of this fundamental binary system [8]. This has revealed exciting potential for understanding more about the surface of Europa from space, perhaps even providing a window into its past. [1] Carlson, R.W., R.E. Johnson, and M.S. Anderson, Science, 1999. 286(5437): p. 97-99. [2] Fortes, A.D. and M. Choukroun. Space Sci Rev, 2010. 153(1-4): p. 185-218. [3] Blake, D., et al., Space Sci Rev,, 2012. 170(1-4): p. 341-399. [4] Wallwork, K.S., Kennedy B. J. and Wang, D., AIP Conf Proc, 2007. 879: p. 879-882. [5] Liss, K.D., et al., Phys B-Cond Mat, 2006. 385-86: p. 1010-1012. [6] Maynard-Casely, H.E., K.S. Wallwork, and M. Avdeev, (In review). [7] Maynard-Casely, H.E., H.E.A. Brand, and K.S. Wallwork, J.of App.Cryst, 2012. 45: p.1198-1207. [8] Maynard-Casely, H.E., K.S. Wallwork, and H.E.A. Brand, (In Preparation). Stages of the crystal structure determination of sulfruic acid octahydrate a) the oxygen and sulfur postions were determined from the synchrotron x-ray data b) Once neutron diffraction data was collected Fourier difference methods were used to locate hydrogen positions to determine c) the full structure of sulfuric acid octahydrate.

Frustrated magnetism in the double perovskite L a2LiOs O6 : A comparison with L a2LiRu O6

NASA Astrophysics Data System (ADS)

Thompson, C. M.; Marjerrison, C. A.; Sharma, A. Z.; Wiebe, C. R.; Maharaj, D. D.; Sala, G.; Flacau, R.; Hallas, A. M.; Cai, Y.; Gaulin, B. D.; Luke, G. M.; Greedan, J. E.

2016-01-01

The frustrated double perovskite L a2LiOs O6 , based on O s5 +(5 d3,t23 ) is studied using magnetization, elastic neutron scattering, heat capacity, and muon spin relaxation (μSR) techniques and compared with isostructural (P 21/n ) L a2LiRu O6 ,R u5 +(4 d3,t23 ) . While previous studies of L a2LiOs O6 showed a broad susceptibility maximum (χmax) near 40 K, heat capacity data indicate a sharp peak at 30 K, similar to L a2LiRu O6 with χmax˜30 K and a heat capacity peak at 24 K. Significant differences between the two materials are seen in powder neutron diffraction where the magnetic structure is described by k =(1 /2 1 /2 0 ) for L a2LiOs O6 , while L a2LiRu O6 has been reported with k =(000 ) , structure for face centered lattices. For the k =(1 /2 1 /2 0 ) structure, one has antiferromagnetic layers stacked antiferromagnetically, while for k =(0 0 0 ) structure, ferromagnetic layers are stacked antiferromagnetically. In spite of these differences, both can be considered as type I fcc antiferromagnetic structures. For L a2LiOs O6 , the magnetic structure is best described in terms of linear combinations of basis vectors belonging to irreducible representations Γ2 and Γ4. The combinations Γ2- Γ4 and Γ2+Γ4 could not be distinguished from refinement of the data. In all cases, the O s5 + moments lie in the y z plane with the largest component along y . The total moment is 1.81(4) μB. For L a2LiRu O6 , the R u5 + moments are reported to lie in the x z plane. In addition, while neutron diffraction, μSR and NMR data indicate a unique TN=24 K for L a2LiRu O6 , the situation for L a2LiOs O6 is more complex, with heat capacity, neutron diffraction, and μSR indicating two ordering events at 30 and 37 K, similar to the cases of cubic B a2YRu O6 and monoclinic S r2YRu O6 .

In-situ High-energy X-ray Diffraction Study of the Local Structure of Supercooled Liquid Si

NASA Technical Reports Server (NTRS)

Lee, G. W.; Kim, T. H.; Sieve, B.; Gangopadhyay, A. K.; Hyers, R. W.; Rathz, T. J.; Rogers, J. R.; Robinson, D. S.; Kelton, K. F.; Goldman, A. I.

2005-01-01

While changes in the coordination number for liquid silicon upon supercooling, signaling an underlying liquid-liquid phase transition, have been predicted, x-ray and neutron measurements have produced conflicting reports. In particular some studies have found an increase in the first shell coordination as temperature decreases in the supercooled regime, while others have reported increases in the coordination number with decreasing temperature. Employing the technique of electrostatic levitation coupled with high energy x-ray diffraction (125 keV), and rapid data acquisition (100ms collection times) using an area detector, we have obtained high quality structural data more deeply into the supercooled regime than has been possible before. No change in coordination number is observed in this temperature region, calling into question previous experimental claims of structural evidence for the existence of a liquid-liquid phase transition.

An Overview of Hardware for Protein Crystallization in a Magnetic Field.

PubMed

Yan, Er-Kai; Zhang, Chen-Yan; He, Jin; Yin, Da-Chuan

2016-11-16

Protein crystallization under a magnetic field is an interesting research topic because a magnetic field may provide a special environment to acquire improved quality protein crystals. Because high-quality protein crystals are very useful in high-resolution structure determination using diffraction techniques (X-ray, neutron, and electron diffraction), research using magnetic fields in protein crystallization has attracted substantial interest; some studies have been performed in the past two decades. In this research field, the hardware is especially essential for successful studies because the environment is special and the design and utilization of the research apparatus in such an environment requires special considerations related to the magnetic field. This paper reviews the hardware for protein crystallization (including the magnet systems and the apparatus designed for use in a magnetic field) and progress in this area. Future prospects in this field will also be discussed.

An Overview of Hardware for Protein Crystallization in a Magnetic Field

PubMed Central

Yan, Er-Kai; Zhang, Chen-Yan; He, Jin; Yin, Da-Chuan

2016-01-01

Protein crystallization under a magnetic field is an interesting research topic because a magnetic field may provide a special environment to acquire improved quality protein crystals. Because high-quality protein crystals are very useful in high-resolution structure determination using diffraction techniques (X-ray, neutron, and electron diffraction), research using magnetic fields in protein crystallization has attracted substantial interest; some studies have been performed in the past two decades. In this research field, the hardware is especially essential for successful studies because the environment is special and the design and utilization of the research apparatus in such an environment requires special considerations related to the magnetic field. This paper reviews the hardware for protein crystallization (including the magnet systems and the apparatus designed for use in a magnetic field) and progress in this area. Future prospects in this field will also be discussed. PMID:27854318

Reintroducing electrostatics into macromolecular crystallographic refinement: application to neutron crystallography and DNA hydration.

PubMed

Fenn, Timothy D; Schnieders, Michael J; Mustyakimov, Marat; Wu, Chuanjie; Langan, Paul; Pande, Vijay S; Brunger, Axel T

2011-04-13

Most current crystallographic structure refinements augment the diffraction data with a priori information consisting of bond, angle, dihedral, planarity restraints, and atomic repulsion based on the Pauli exclusion principle. Yet, electrostatics and van der Waals attraction are physical forces that provide additional a priori information. Here, we assess the inclusion of electrostatics for the force field used for all-atom (including hydrogen) joint neutron/X-ray refinement. Two DNA and a protein crystal structure were refined against joint neutron/X-ray diffraction data sets using force fields without electrostatics or with electrostatics. Hydrogen-bond orientation/geometry favors the inclusion of electrostatics. Refinement of Z-DNA with electrostatics leads to a hypothesis for the entropic stabilization of Z-DNA that may partly explain the thermodynamics of converting the B form of DNA to its Z form. Thus, inclusion of electrostatics assists joint neutron/X-ray refinements, especially for placing and orienting hydrogen atoms. Copyright © 2011 Elsevier Ltd. All rights reserved.

Reintroducing Electrostatics into Macromolecular Crystallographic Refinement: Application to Neutron Crystallography and DNA Hydration

PubMed Central

Fenn, Timothy D.; Schnieders, Michael J.; Mustyakimov, Marat; Wu, Chuanjie; Langan, Paul; Pande, Vijay S.; Brunger, Axel T.

2011-01-01

Summary Most current crystallographic structure refinements augment the diffraction data with a priori information consisting of bond, angle, dihedral, planarity restraints and atomic repulsion based on the Pauli exclusion principle. Yet, electrostatics and van der Waals attraction are physical forces that provide additional a priori information. Here we assess the inclusion of electrostatics for the force field used for all-atom (including hydrogen) joint neutron/X-ray refinement. Two DNA and a protein crystal structure were refined against joint neutron/X-ray diffraction data sets using force fields without electrostatics or with electrostatics. Hydrogen bond orientation/geometry favors the inclusion of electrostatics. Refinement of Z-DNA with electrostatics leads to a hypothesis for the entropic stabilization of Z-DNA that may partly explain the thermodynamics of converting the B form of DNA to its Z form. Thus, inclusion of electrostatics assists joint neutron/X-ray refinements, especially for placing and orienting hydrogen atoms. PMID:21481775

A furnace with rotating load frame for in situ high temperature deformation and creep experiments in a neutron diffraction beam line

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

Reiche, H. M.; New Mexico State University, Las Cruces, New Mexico 88003; Vogel, S. C.

2012-05-15

A resistive furnace combined with a load frame was built that allows for in situ neutron diffraction studies of high temperature deformation, in particular, creep. A maximum force of 2700 N can be applied at temperatures up to 1000 deg. C. A load control mode permits studies of, e.g., creep or phase transformations under applied uni-axial stress. In position control, a range of high temperature deformation experiments can be achieved. The examined specimen can be rotated up to 80 deg. around the vertical compression axis allowing texture measurements in the neutron time-of-flight diffractometer HIPPO (High Pressure - Preferred Orientation). Wemore » present results from the successful commissioning, deforming a Zr-2.5 wt.% Nb cylinder at 975 deg. C. The device is now available for the user program of the HIPPO diffractometer at the LANSCE (Los Alamos Neutron Science Center) user facility.« less

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

DOE PAGES

Liao, Jian -Hong; Dhayal, Rajendra Singh; Wang, Xiaoping; ...

2014-10-07

The structure of a nanospheric polyhydrido copper cluster, [Cu 20(H) 11{S 2P(O iPr) 2} 9], was determined by single-crystal neutron diffraction. Cu 20 cluster consists of an elongated triangular orthobicupola constructed from 18 Cu atoms that encapsulate a [Cu 2H 5} 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 μ 3-hydrides in pyramidal geometry, two μ 4-hydrides in tetrahedral cavity, and three μ 4-hydrides in an unprecedented near square-planar geometry. The neutron data set was collected on a small crystal ofmore » 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.« less

Hyperfine Fields of 181Ta in UFe4Al8

NASA Astrophysics Data System (ADS)

Marques, J. G.; Barradas, N. P.; Alves, E.; Ramos, A. R.; Gonçalves, A. P.; da Silva, M. F.; Soares, J. C.

2001-11-01

The γ γ Perturbed Angular Correlation technique was used to study the hyperfine interaction of 181Ta at the Hf site(s) in UFe4Al8 at room temperature and 12 K. The data at room temperature are well described by two electric field gradients, while at low temperature two combined hyperfine interactions have to be considered, one with the magnetic hyperfine field collinear with the c-axis and another with the magnetic hyperfine field in the basal plane. The results are compared with previous Mössbauer and neutron diffraction experiments and the lattice site of Hf is discussed.

Idealized powder diffraction patterns for cellulose polymorphs

USDA-ARS?s Scientific Manuscript database

Cellulose samples are routinely analyzed by X-ray diffraction to determine their crystal type (polymorph) and crystallinity. However, the connection is seldom made between those efforts and the crystal structures of cellulose that have been determined with synchrotron X-radiation and neutron diffrac...

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.

Neutron diffraction, specific heat and magnetization studies on Nd{sub 2}CuTiO{sub 6}

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

Rayaprol, S., E-mail: sudhindra@csr.res.in; Kaushik, S. D.; Kumar, Naresh

2016-05-23

Structural and physical properties of a double-perovskite compound, Nd{sub 2}CuTiO{sub 6} have been studied using neutron diffraction, magnetization and specific heat measurements. The compound crystallizes in an orthorhombic structure in space group Pnma. The interesting observation we make here is that, though no long range magnetic order is observed between 2 and 300 K, the low temperature specific heat and magnetic susceptibility behavior exhibits non-Fermi liquid like behavior in this insulating compound. The magnetization and specific heat data are presented and discussed in light of these observations.

Neutron diffraction and μ SR studies of two polymorphs of nickel niobate NiNb 2 O 6

DOE PAGES

Munsie, T. J. S.; Wilson, M. N.; Millington, A.; ...

2017-10-13

Neutron diffraction and muon spin relaxation (μSR) studies are presented in this paper for the newly characterized polymorph of NiNb 2O 6 (β-NiNb 2O 6) with space group P4 2/n and μSR data only for the previously known columbite structure polymorph with space group Pbcn. The magnetic structure of the P4 2/n form was determined from neutron diffraction using both powder and single-crystal data. Powder neutron diffraction determined an ordering wave vector →k=( 1/ 2, 1/ 2, 1/ 2). Single-crystal data confirmed the same →k vector and showed that the correct magnetic structure consists of antiferromagnetically coupled chains running alongmore » the a or b axis in adjacent Ni 2+ layers perpendicular to the c axis, which is consistent with the expected exchange interaction hierarchy in this system. The refined magnetic structure is compared with the known magnetic structures of the closely related trirutile phases, NiSb 2O 6 and NiTa 2O 6. μSR data finds a transition temperature of T N~15K for this system, while the columbite polymorph exhibits a lower T N=5.7(3) K. Our μSR measurements also allowed us to estimate the critical exponent of the order parameter β for each polymorph. We found β =0.25(3) and 0.16(2) for the β and columbite polymorphs, respectively. The single-crystal neutron scattering data give a value for the critical exponent β =0.28(3) for β-NiNb 2O 6, in agreement with the μSR value. While both systems have β values less than 0.3, which is indicative of reduced dimensionality, this effect appears to be much stronger for the columbite system. Finally, in other words, although both systems appear to be well described by S=1 spin chains, the interchain interactions in the β polymorph are likely much larger.« less

Neutron diffraction and μ SR studies of two polymorphs of nickel niobate NiNb2O6

NASA Astrophysics Data System (ADS)

Munsie, T. J. S.; Wilson, M. N.; Millington, A.; Thompson, C. M.; Flacau, R.; Ding, C.; Guo, S.; Gong, Z.; Aczel, A. A.; Cao, H. B.; Williams, T. J.; Dabkowska, H. A.; Ning, F.; Greedan, J. E.; Luke, G. M.

2017-10-01

Neutron diffraction and muon spin relaxation (μ SR ) studies are presented for the newly characterized polymorph of NiNb2O6 (β -NiNb2O6) with space group P4 2/n and μ SR data only for the previously known columbite structure polymorph with space group P b c n . The magnetic structure of the P4 2/n form was determined from neutron diffraction using both powder and single-crystal data. Powder neutron diffraction determined an ordering wave vector k ⃗=(1/2 ,1/2 ,1/2 ) . Single-crystal data confirmed the same k ⃗ vector and showed that the correct magnetic structure consists of antiferromagnetically coupled chains running along the a or b axis in adjacent Ni2 + layers perpendicular to the c axis, which is consistent with the expected exchange interaction hierarchy in this system. The refined magnetic structure is compared with the known magnetic structures of the closely related trirutile phases, NiSb2O6 and NiTa2O6 . μ SR data finds a transition temperature of TN˜15 K for this system, while the columbite polymorph exhibits a lower TN=5.7 (3 ) K. Our μ SR measurements also allowed us to estimate the critical exponent of the order parameter β for each polymorph. We found β =0.25 (3 ) and 0.16(2) for the β and columbite polymorphs, respectively. The single-crystal neutron scattering data give a value for the critical exponent β =0.28 (3 ) for β -NiNb2O6 , in agreement with the μ SR value. While both systems have β values less than 0.3, which is indicative of reduced dimensionality, this effect appears to be much stronger for the columbite system. In other words, although both systems appear to be well described by S =1 spin chains, the interchain interactions in the β polymorph are likely much larger.

Neutron diffraction and μ SR studies of two polymorphs of nickel niobate NiNb 2 O 6

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

Munsie, T. J. S.; Wilson, M. N.; Millington, A.

Neutron diffraction and muon spin relaxation (μSR) studies are presented in this paper for the newly characterized polymorph of NiNb 2O 6 (β-NiNb 2O 6) with space group P4 2/n and μSR data only for the previously known columbite structure polymorph with space group Pbcn. The magnetic structure of the P4 2/n form was determined from neutron diffraction using both powder and single-crystal data. Powder neutron diffraction determined an ordering wave vector →k=( 1/ 2, 1/ 2, 1/ 2). Single-crystal data confirmed the same →k vector and showed that the correct magnetic structure consists of antiferromagnetically coupled chains running alongmore » the a or b axis in adjacent Ni 2+ layers perpendicular to the c axis, which is consistent with the expected exchange interaction hierarchy in this system. The refined magnetic structure is compared with the known magnetic structures of the closely related trirutile phases, NiSb 2O 6 and NiTa 2O 6. μSR data finds a transition temperature of T N~15K for this system, while the columbite polymorph exhibits a lower T N=5.7(3) K. Our μSR measurements also allowed us to estimate the critical exponent of the order parameter β for each polymorph. We found β =0.25(3) and 0.16(2) for the β and columbite polymorphs, respectively. The single-crystal neutron scattering data give a value for the critical exponent β =0.28(3) for β-NiNb 2O 6, in agreement with the μSR value. While both systems have β values less than 0.3, which is indicative of reduced dimensionality, this effect appears to be much stronger for the columbite system. Finally, in other words, although both systems appear to be well described by S=1 spin chains, the interchain interactions in the β polymorph are likely much larger.« less

Neutron resonance spin-echo upgrade at the three-axis spectrometer FLEXX

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

Groitl, F., E-mail: felix.groitl@psi.ch; Quintero-Castro, D. L.; Habicht, K.

2015-02-15

We describe the upgrade of the neutron resonance spin-echo setup at the cold neutron triple-axis spectrometer FLEXX at the BER II neutron source at the Helmholtz-Zentrum Berlin. The parameters of redesigned key components are discussed, including the radio frequency (RF) spin-flip coils, the magnetic shield, and the zero field coupling coils. The RF-flippers with larger beam windows allow for an improved neutron flux transfer from the source to the sample and further to the analyzer. The larger beam cross sections permit higher coil inclination angles and enable measurements on dispersive excitations with a larger slope of the dispersion. Due tomore » the compact design of the spin-echo units in combination with the increased coil tilt angles, the accessible momentum-range in the Larmor diffraction mode is substantially enlarged. In combination with the redesigned components of the FLEXX spectrometer, including the guide, the S-bender polarizer, the double focusing monochromator, and a Heusler crystal analyzer, the count rate increased by a factor of 15.5, and the neutron beam polarization is enhanced. The improved performance extends the range of feasible experiments, both for inelastic scattering on excitation lifetimes in single crystals, and for high-resolution Larmor diffraction. The experimental characterization of the instrument components demonstrates the reliable performance of the new neutron resonance spin-echo option, now available for the scientific community at FLEXX.« less

Energy-selective Neutron Imaging for Three-dimensional Non-destructive Probing of Crystalline Structures

NASA Astrophysics Data System (ADS)

Peetermans, S.; Bopp, M.; Vontobel, P.; Lehmann, E. H.

Common neutron imaging uses the full polychromatic neutron beam spectrum to reveal the material distribution in a non-destructive way. Performing it with a reduced energy band, i.e. energy-selective neutron imaging, allows access to local variation in sample crystallographic properties. Two sample categories can be discerned with different energy responses. Polycrystalline materials have an energy-dependent cross-section featuring Bragg edges. Energy-selective neutron imaging can be used to distinguish be- tween crystallographic phases, increase material sensitivity or penetration, improve quantification etc. An example of the latter is shown by the examination of copper discs prior to machining them into linear accelerator cavity structures. The cross-section of single crystals features distinct Bragg peaks. Based on their pattern, one can determine the orientation of the crystal, as in a Laue pattern, but with the tremendous advantage that the operation can be performed for each pixel, yielding crystal orientation maps at high spatial resolution. A wholly different method to investigate such samples is also introduced: neutron diffraction imaging. It is based on projections formed by neutrons diffracted from the crystal lattice out of the direct beam. The position of these projections on the detector gives information on the crystal orientation. The projection itself can be used to reconstruct the crystal shape. A three-dimensional mapping of local Bragg reflectivity or a grain orientation mapping can thus be obtained.

Structure of Se-Te glasses studied using neutron, X-ray diffraction and reverse Monte Carlo modelling

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

Itoh, Keiji, E-mail: itoh@okayama-u.ac.jp; Research Reactor Institute, Kyoto University, Kumatori, Osaka 590-0494

Pulsed neutron diffraction and synchrotron X-ray diffraction measurements were performed on Se{sub 100-x}Te{sub x} bulk glasses with x=10, 20, 30 and 40. The coordination numbers obtained from the diffraction results demonstrate that Se and Te atoms are twofold coordinated and the glass structure is formed by the chain network. The three-dimensional structure model for Se{sub 60}Te{sub 40} glass obtained by using reverse Monte Carlo modelling shows that the alternating arrangements of Se and Te atoms compose the major part of the chain clusters but several other fragments such as Se{sub n} chains and Te-Te dimers are also present in largemore » numbers. The chain clusters have geometrically disordered forms and the interchain atomic order is different from those in the crystal structures of trigonal Se and trigonal Te. - Graphical abstract: Coordination environment in Se{sub 60}Te{sub 40} glass.« less

Residual stress determination in an overlay dissimilar welded pipe by neutron diffraction

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

Woo, Wan Chuck; Em, Vyacheslav; Hubbard, Camden R

2011-01-01

Residual stresses were determined through the thickness of a dissimilar weld overlay pipe using neutron diffraction. The specimen has a complex joining structure consisting of a ferritic steel (SA508), austenitic steel (F316L), Ni-based consumable (Alloy 182), and overlay of Ni-base superalloy (Alloy 52M). It simulates pressurized nozzle components, which have been a critical issue under the severe crack condition of nuclear power reactors. Two neutron diffractometers with different spatial resolutions have been utilized on the identical specimen for comparison. The macroscopic 'stress-free' lattice spacing (d{sub o}) was also obtained from both using a 2-mm width comb-like coupon. The results showmore » significant changes in residual stresses from tension (300-400 MPa) to compression (-600 MPa) through the thickness of the dissimilar weld overlay pipe specimen.« less

Characterization of the intermediate-range order in new superionic conducting AgI-Ag2S-AgPO3 glasses by neutron diffraction

NASA Astrophysics Data System (ADS)

Kartini, E.; Kennedy, S. J.; Itoh, K.; Fukunaga, T.; Suminta, S.; Kamiyama, T.

Superionic conducting glasses are of considerable technological interest because of their use in batteries, sensors, and displays. We have investigated the new ternary systems AgI-Ag2S-AgPO3 where the ratio AgI:Ag2S is 1:1. The system (AgI)x(Ag2S)x(AgPO3)1-2x, for a AgI+Ag2S fraction less than 82mol%, yields glasses. We have used a neutron-diffraction technique to obtain the total scattering structure factor S(Q) of this system at room temperature by using the HIT spectrometer at the High Energy Accelerator (KEK), Tsukuba, Japan. As for AgI-AgPO3 glasses, S(Q) shows a peak at anomalously low Q in the range from 0.6 to 0.9 Å-1. This peak is not observed in the corresponding glass Ag2S-AgPO3 or pure AgPO3. The peak depends strongly on the dopant salt. Its intensity increases as the amount of (AgI+Ag2S) increases and its position shifts to lower Q, while the number density of the glasses decreases with x. This peak can be associated with an intermediate structure of particles lying inside a continuous host with the characteristic length between 5 and 10 Å [1].

Structure of the intermediate Zr/sub 2/Br/sub 2/H by neutron diffraction and its structural and bonding relationships to other phases

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

Wijeyesekera, S.D.; Corbett, J.D.

1986-12-17

The structures of the isomorphous Zr/sub 2/Br/sub 2/D and Zr/sub 2/Br/sub 2/H have been solved and refined by using Rietveld techniques on pulsed neutron diffraction data obtained from the powdered samples at 14 K (C2/m, a = 19.437 (3) A, b = 3.5253 (4) A, c = 5.9036 (6) A, ..beta.. = 100.98 (1)/sup 0/, R(profile)/R(expected) = 2.44 for the deuteride). The structure consists of layers sequenced Br-Zr-H-H-Zr-Br and arranged such that hydride lies in zigzag chains of distorted metal tetrahedra (or butterflies) (d(Zr-D) = 2.03-2.20 A; d(D-D) = 2.93 A). The structure is intermediate between ZrBr (ccp) and ZrBrHmore » (hcp heavy atoms, double H in trigonal-antiprismatic interstices) and can be generated by concerted intraslab slippage from either. The hemihydride effectively retains most of the strong Zr-Zr bonding of the ZrBr parent while tetrahedral bonding of hydrogen to metal is gained that is absent in ZrBrH. The energetics associated with the contrasting structures of YClH/sub x/ (ZrBr type) and ZrBrH are considered in terms of the results of extended-Hueckel band calculations. 25 references, 7 figures, 3 tables.« less

Characterization of the new neutron imaging and materials science facility IMAT

NASA Astrophysics Data System (ADS)

Minniti, Triestino; Watanabe, Kenichi; Burca, Genoveva; Pooley, Daniel E.; Kockelmann, Winfried

2018-04-01

IMAT is a new cold neutron imaging and diffraction instrument located at the second target station of the pulsed neutron spallation source ISIS, UK. A broad range of materials science and materials testing areas will be covered by IMAT. We present the characterization of the imaging part, including the energy-selective and energy-dispersive imaging options, and provide the basic parameters of the radiography and tomography instrument. In particular, detailed studies on mono and bi-dimensional neutron beam flux profiles, neutron flux as a function of the neutron wavelength, spatial and energy dependent neutron beam uniformities, guide artifacts, divergence and spatial resolution, and neutron pulse widths are provided. An accurate characterization of the neutron beam at the sample position, located 56 m from the source, is required to optimize collection of radiographic and tomographic data sets and for performing energy-dispersive neutron imaging via time-of-flight methods in particular.

A high performance neutron powder diffractometer at 3 MW Triga Mark-II research reactor in Bangladesh

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

Kamal, I., E-mail: imtiaz-kamal26@yahoo.com; Yunus, S. M., E-mail: yunussm11@yahoo.com; Datta, T. K., E-mail: tk-datta4@yahoo.com

2016-07-12

A high performance neutron diffractometer called Savar Neutron Diffractometer (SAND) was built and installed at radial beam port-2 of TRIGA Mark II research reactor at AERE, Savar, Dhaka, Bangladesh. Structural studies of materials are being done by this technique to characterize materials crystallograpohically and magnetically. The micro-structural information obtainable by neutron scattering method is very essential for determining its technological applications. This technique is unique for understanding the magnetic behavior in magnetic materials. Ceramic, steel, electronic and electric industries can be benefited from this facility for improving their products and fabrication process. This instrument consists of a Popovicimonochromator with amore » large linear position sensitive detector array. The monochromator consists of nine blades of perfect single crystal of silicon with 6 mm thickness each. The monochromator design was optimized to provide maximum flux on 3 mm diameter cylindrical sample with a relatively flat angular dependence of resolution. Five different wave lengths can be selected by orienting the crystal at various angles. A sapphire filter was used before the primary collimator to minimize the first neutron. The detector assembly is composed of 15 linear position sensitive proportional counters placed at either 1.1 m or 1.6 m from the sample position and enclosed in a air pad supported high density polythene shield. Position sensing is obtained by charge division using 1-wide NIM position encoding modules (PEM). The PEMs communicate with the host computer via USB. The detector when placed at 1.1 m, subtends 30° (2θ) at each step and covers 120° in 4 steps. When the detector is placed at 1.6 m it subtends 20° at each step and covers 120° in 6 steps. The instrument supports both low and high temperature sample environment. The instrument supports both low and high temperature sample environment. The diffractometer is a state-of-the art technology for diffraction study in our country.« less

A high performance neutron powder diffractometer at 3 MW Triga Mark-II research reactor in Bangladesh

NASA Astrophysics Data System (ADS)

Kamal, I.; Yunus, S. M.; Datta, T. K.; Zakaria, A. K. M.; Das, A. K.; Aktar, S.; Hossain, S.; Berliner, R.; Yelon, W. B.

2016-07-01

A high performance neutron diffractometer called Savar Neutron Diffractometer (SAND) was built and installed at radial beam port-2 of TRIGA Mark II research reactor at AERE, Savar, Dhaka, Bangladesh. Structural studies of materials are being done by this technique to characterize materials crystallograpohically and magnetically. The micro-structural information obtainable by neutron scattering method is very essential for determining its technological applications. This technique is unique for understanding the magnetic behavior in magnetic materials. Ceramic, steel, electronic and electric industries can be benefited from this facility for improving their products and fabrication process. This instrument consists of a Popovicimonochromator with a large linear position sensitive detector array. The monochromator consists of nine blades of perfect single crystal of silicon with 6mm thickness each. The monochromator design was optimized to provide maximum flux on 3mm diameter cylindrical sample with a relatively flat angular dependence of resolution. Five different wave lengths can be selected by orienting the crystal at various angles. A sapphire filter was used before the primary collimator to minimize the first neutron. The detector assembly is composed of 15 linear position sensitive proportional counters placed at either 1.1 m or 1.6 m from the sample position and enclosed in a air pad supported high density polythene shield. Position sensing is obtained by charge division using 1-wide NIM position encoding modules (PEM). The PEMs communicate with the host computer via USB. The detector when placed at 1.1 m, subtends 30˚ (2θ) at each step and covers 120˚ in 4 steps. When the detector is placed at 1.6 m it subtends 20˚ at each step and covers 120˚ in 6 steps. The instrument supports both low and high temperature sample environment. The instrument supports both low and high temperature sample environment. The diffractometer is a state-of-the art technology for diffraction study in our country.

NEUTRON DIFFRACTION INVESTIGATIONS OF FERROMAGNETIC PALLADIUM AND IRON GROUP ALLOYS

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

Cable, J.W.; Wollan, E.O.; Koehler, W.C.

1962-03-01

In order to account for the magnetic properties of alloys It becomes important to determine the individual magnetic moments of the constituent atoms. This determination can be accomplished by means of neutron diffraction and magnetic induction measurements. Such measurements are made on the ferromagnetic alloys Pd/sub 3/Fe, PdFe, Pd/sub 3/Co, PdCo, Ni/sub 3/Co, and NiCo. The average moment values are obtained from magnetic induction measurements while the differences in the atomic moments are determined from either the ferromagnetic diffuse scattering by the disordered alloys or the superlattice reflections by the ordered alloys. (auth)

Change in the magnetic structure of (Bi,Sm)FeO3 thin films at the morphotropic phase boundary probed by neutron diffraction

NASA Astrophysics Data System (ADS)

Maruyama, Shingo; Anbusathaiah, Varatharajan; Fennell, Amy; Enderle, Mechthild; Takeuchi, Ichiro; Ratcliff, William D.

2014-11-01

We report on the evolution of the magnetic structure of BiFeO3 thin films grown on SrTiO3 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.

Neutron powder diffraction study on the iron-based nitride superconductor ThFeAsN

NASA Astrophysics Data System (ADS)

Mao, Huican; Wang, Cao; Maynard-Casely, Helen E.; Huang, Qingzhen; Wang, Zhicheng; Cao, Guanghan; Li, Shiliang; Luo, Huiqian

2017-03-01

We report neutron diffraction and transport results on the newly discovered superconducting nitride ThFeAsN with T_c= 30 \\text{K} . No magnetic transition, but a weak structural distortion around 160 K, is observed by cooling from 300 K to 6 K. Analysis on the resistivity, Hall transport and crystal structure suggests that this material behaves as an electron optimally doped pnictide superconductor due to extra electrons from nitrogen deficiency or oxygen occupancy at the nitrogen site, which, together with the low arsenic height, may enhance the electron itinerancy and reduce the electron correlations, thus suppressing the static magnetic order.

Magnetic structure of Ho0.5Y0.5Mn6Sn6 compound studied by powder neutron diffraction

NASA Astrophysics Data System (ADS)

Li, X.-Y.; Peng, L.-C.; He, L.-H.; Zhang, S.-Y.; Yao, J.-L.; Zhang, Y.; Wang, F.-W.

2018-05-01

The crystallographic and magnetic structures of the HfFe6Ge6-type compound Ho0.5Y0.5Mn6Sn6 have been studied by powder neutron diffraction and in-situ Lorentz transmission electron microscopy. Besides the nonlinear thermal expansion of lattice parameters, an incommensurate conical spiral magnetic structure was determined in the temperature interval of 2-340 K. A spin reorientation transition has been observed from 50 to 300 K, where the alignment of the c-axis component of magnetic moments of the Ho sublattice and the Mn sublattice transfers from ferrimagnetic to ferromagnetic.

In situ neutron diffraction study of micromechanical interactions and phase transformation in Ni-Mn-Ga alloy under uniaxial and hydrostatic stress.

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

Peng, R. L.; Wang, Y. D.; Nie, Z. H.

2008-01-01

This paper deals with the experimental study of stress-induced phase transformation in a polycrystalline Ni-Mn-Ga alloy under uniaxial compression and its powder under hydrostatic compression. In situ neutron diffraction experiments were employed to follow changes in the structure and lattice strains caused by the applied stresses. Large lattice strains that are dependent on the lattice planes or grain orientations were observed in the parent Heusler phase for both the bulk material and the powder sample. The development of such anisotropic strains and the influence of external load conditions are discussed in the paper.

Residual stress characterization of steel TIG welds by neutron diffraction and by residual magnetic stray field mappings

NASA Astrophysics Data System (ADS)

Stegemann, Robert; Cabeza, Sandra; Lyamkin, Viktor; Bruno, Giovanni; Pittner, Andreas; Wimpory, Robert; Boin, Mirko; Kreutzbruck, Marc

2017-03-01

The residual stress distribution of tungsten inert gas welded S235JRC+C plates was determined by means of neutron diffraction (ND). Large longitudinal residual stresses with maxima around 600 MPa were found. With these results as reference, the evaluation of residual stress with high spatial resolution GMR (giant magneto resistance) sensors was discussed. The experiments performed indicate a correlation between changes in residual stresses (ND) and the normal component of local residual magnetic stray fields (GMR). Spatial variations in the magnetic field strength perpendicular to the welds are in the order of the magnetic field of the earth.

POWTEX - A new High-Intensity Powder and Texture Diffractometer at FRM II, Garching Germany

NASA Astrophysics Data System (ADS)

Walter, J. M.; Brückel, T.; Dronskowski, R.; Hansen, B. T.; Houben, A.; Klein, H.; Leiss, B.; Vollbrecht, A.; Sowa, H.

2009-05-01

In recent years, neutron diffraction has become a routine tool in Geoscience for experimental high-field (HP/HT/HH) powder diffraction and for the quantitative analysis of the crystallographic preferred orientation (CPO). Quantitative texture analysis is e.g. involved in the research fields of fabric development in mono- and polyphase rocks, deformation histories and kinematics during mountain building processes and the characterization of flow kinematics in lava flows. Secondly the quantitative characterization of anisotropic physical properties of both rock and analogue materials is conducted by bulk texture measurements of sometimes larger sample volumes. This is easily achievable by neutron diffraction due to the high penetration capabilities of the neutrons. The resulting geoscientific need for increased measuring time at neutron diffraction facilities with the corresponding technical characteristics and equipment will in future be satisfied by this high-intensity diffractometer at the neutron research reactor FRM II in Garching, Germany. It will be built by a consortium of groups from the RWTH Aachen, Forschungszentrum Jülich and the University of Göttingen, who will also operate the instrument. The diffractometer will be optimized to high intensities (flux) with an equivalent sufficient resolution for polyphase rocks. Furthermore a broad range of d-values (0.5 to 15 Å) will be measurable. The uniqueness of this instrument is the geoscientific focus on different sample environments for in situ-static and deformation experiments (stress, strain and annealing/recrystallisation) and (U)HP/(U)HT experiments. A LP/LT or atmospheric-P deformation rig for in situ-deformation experiments on ice, halite or rock analogue materials is planned, to allow in situ-measurements of the texture development during deformation and annealing. Additionally a uniaxial HT/MP deformation apparatus for salt deformation experiments and an adapted Griggs- type deformation rig are also designated. Furthermore an uniaxial stress frame for in situ stress investigations is planned to conduct simultaneous measurements of stress, elastic or plastic deformation and texture. Other sample environments for geoscientific application will be HP/HT furnaces and pressure cells for powder diffraction investigations. Furthermore the diffractometer will be built in combination with a high-pressure multi anvil up to 25 GPa and 2500 K built by the University of Bayreuth at the same beam line. The detector concept allows single shot texture measurements and therefore the measurement of larger geological sample series as necessary for the investigations of complete geological structures. This concept is complementary to the geoscience neutron texture diffractometer in Dubna, Russia and the stress diffractometer STRESS-SPEC located also at the Garching research reactor. For powder diffraction the diffractometer will be complementary to the existing high-resolution powder diffractometer SPODI at the FRM-II. It will offer the possibility of short, high-intensity parametric powder diffraction measurements in dependency of temperature, electrical, magnetic and stress fields due to the higher flux at the sample. The optimization to high-intensities and therefore short measuring times will also allow time-resolved measurements of kinetic reactions even of small sample volumes.

In-situ neutron diffraction of LaCoO3 perovskite under uniaxial compression. I. Crystal structure analysis and texture development

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

Aman, Amjad; Chen, Yan; Lugovy, Mykola

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 hysteresismore » 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.« less

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.

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

PubMed Central

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

2014-01-01

The rigidity temperature of a solidifying alloy is the temperature at which the solid plus liquid phases are sufficiently coalesced to transmit long range tensile strains and stresses. It determines the point at which thermally induced deformations start to generate internal stresses in a casting. As such, it is a key parameter in numerical modelling of solidification processes and in studying casting defects such as solidification cracking. This temperature has been determined in Al-Cu alloys using in situ neutron diffraction during casting in a dog bone shaped mould. In such a setup, the thermal contraction of the solidifying material is constrained and stresses develop at a hot spot that is irradiated by neutrons. Diffraction peaks are recorded every 11 s using a large detector, and their evolution allows for the determination of the rigidity temperatures. We measured rigidity temperatures equal to 557 °C and 548 °C, depending on cooling rate, for a grain refined Al-13 wt% Cu alloy. At high cooling rate, rigidity is reached during the formation of the eutectic phase and the solid phase is not sufficiently coalesced, i.e., strong enough, to avoid hot tear formation. PMID:28788507

Minimization of spurious strains by using a Si bent-perfect-crystal monochromator: neutron surface strain scanning of a shot-peened sample

NASA Astrophysics Data System (ADS)

Rebelo Kornmeier, Joana; Gibmeier, Jens; Hofmann, Michael

2011-06-01

Neutron strain measurements are critical at the surface. When scanning close to a sample surface, aberration peak shifts arise due to geometrical and divergence effects. These aberration peak shifts can be of the same order as the peak shifts related to residual strains. In this study it will be demonstrated that by optimizing the horizontal bending radius of a Si (4 0 0) monochromator, the aberration peak shifts from surface effects can be strongly reduced. A stress-free sample of fine-grained construction steel, S690QL, was used to find the optimal instrumental conditions to minimize aberration peak shifts. The optimized Si (4 0 0) monochromator and instrument settings were then applied to measure the residual stress depth gradient of a shot-peened SAE 4140 steel sample to validate the effectiveness of the approach. The residual stress depth profile is in good agreement with results obtained by x-ray diffraction measurements from an international round robin test (BRITE-EURAM-project ENSPED). The results open very promising possibilities to bridge the gap between x-ray diffraction and conventional neutron diffraction for non-destructive residual stress analysis close to surfaces.

Neutron diffraction and electrical transport studies on magnetic ordering in terbium at high pressures and low temperatures

DOE PAGES

Thomas, Sarah A.; Montgomery, Jeffrey M.; Tsoi, Georgiy 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

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

PubMed

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

2014-02-12

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

Extracting grain-orientation-dependent data from in situ time-of-flight neutron diffraction. I. Inverse pole figures

DOE PAGES

Stoica, Grigoreta M.; Stoica, Alexandru Dan; An, Ke; ...

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

SMA texture and reorientation: simulations and neutron diffraction studies

NASA Astrophysics Data System (ADS)

Gao, Xiujie; Brown, Donald W.; Brinson, L. Catherine

2005-05-01

With increased usage of shape memory alloys (SMA) for applications in various fields, it is important to understand how the material behavior is affected by factors such as texture, stress state and loading history, especially for complex multiaxial loading states. Using the in-situ neutron diffraction loading facility (SMARTS diffractometer) and ex situ inverse pole figure measurement facility (HIPPO diffractometer) at the Los Alamos Neutron Science Center (LANCE), the macroscopic mechanical behavior and texture evolution of Nickel-Titanium (Nitinol) SMAs under sequential compression in alternating directions were studied. The simplified multivariant model developed at Northwestern University was then used to simulate the macroscopic behavior and the microstructural change of Nitinol under this sequential loading. Pole figures were obtained via post-processing of the multivariant results for volume fraction evolution and compared quantitatively well to the experimental results. The experimental results can also be used to test or verify other SMA constitutive models.

Recent Advances in the Understanding of the Influence of Electric and Magnetic Fields on Protein Crystal Growth

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

Pareja-Rivera, Carina; Cuéllar-Cruz, Mayra; Esturau-Escofet, Nuria

Here, in this contribution we use nonconventional methods that help to increase the success rate of a protein crystal growth, and consequently of structural projects using X-ray diffraction techniques. In order to achieve this purpose, this contribution presents new approaches involving more sophisticated techniques of protein crystallization, not just for growing protein crystals of different sizes by using electric fields, but also for controlling crystal size and orientation. Also, this latter was possible through the use of magnetic fields that allow to obtain protein crystals suitable for both high-resolution X-ray and neutron diffraction crystallography where big crystals are required. Thismore » contribution discusses some pros, cons and realities of the role of electromagnetic fields in protein crystallization research, and their effect on protein crystal contacts. Additionally, we discuss the importance of room and low temperatures during data collection. Finally, we also discuss the effect of applying a rather strong magnetic field of 16.5 T, for shorts and long periods of time, on protein crystal growth, and on the 3D structure of two model proteins.« less

Recent Advances in the Understanding of the Influence of Electric and Magnetic Fields on Protein Crystal Growth

DOE PAGES

Pareja-Rivera, Carina; Cuéllar-Cruz, Mayra; Esturau-Escofet, Nuria; ...

2016-12-05

Here, in this contribution we use nonconventional methods that help to increase the success rate of a protein crystal growth, and consequently of structural projects using X-ray diffraction techniques. In order to achieve this purpose, this contribution presents new approaches involving more sophisticated techniques of protein crystallization, not just for growing protein crystals of different sizes by using electric fields, but also for controlling crystal size and orientation. Also, this latter was possible through the use of magnetic fields that allow to obtain protein crystals suitable for both high-resolution X-ray and neutron diffraction crystallography where big crystals are required. Thismore » contribution discusses some pros, cons and realities of the role of electromagnetic fields in protein crystallization research, and their effect on protein crystal contacts. Additionally, we discuss the importance of room and low temperatures during data collection. Finally, we also discuss the effect of applying a rather strong magnetic field of 16.5 T, for shorts and long periods of time, on protein crystal growth, and on the 3D structure of two model proteins.« less

Thermal neutron detector based on COTS CMOS imagers and a conversion layer containing Gadolinium

NASA Astrophysics Data System (ADS)

Pérez, Martín; Blostein, Juan Jerónimo; Bessia, Fabricio Alcalde; Tartaglione, Aureliano; Sidelnik, Iván; Haro, Miguel Sofo; Suárez, Sergio; Gimenez, Melisa Lucía; Berisso, Mariano Gómez; Lipovetzky, Jose

2018-06-01

In this work we will introduce a novel low cost position sensitive thermal neutron detection technique, based on a Commercial Off The Shelf CMOS image sensor covered with a Gadolinium containing conversion layer. The feasibility of the neutron detection technique implemented in this work has been experimentally demonstrated. A thermal neutron detection efficiency of 11.3% has been experimentally obtained with a conversion layer of 11.6 μm. It was experimentally verified that the thermal neutron detection efficiency of this technique is independent on the intensity of the incident thermal neutron flux, which was confirmed for conversion layers of different thicknesses. Based on the experimental results, a spatial resolution better than 25 μm is expected. This spatial resolution makes the proposed technique specially useful for neutron beam characterization, neutron beam dosimetry, high resolution neutron imaging, and several neutron scattering techniques.

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

DOE PAGES

Mauro, N. A.; Vogt, A. J.; Derendorf, K. S.; ...

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 Zr 64Ni 36 measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample ( 100 mg).« less

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

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

Mauro, N. A., E-mail: namauro@noctrl.edu; Vogt, A. J.; Derendorf, K. S.

2016-01-15

Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. However, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality 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%. To demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr{sub 64}Ni{sub 36} measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample (∼100 mg)« less

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates

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

Silva, Chinthaka M.; Rosseel, Thomas M.; Kirkegaard, Marie C.

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18, 4 × 10 19, and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasingmore » neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2, with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. In conclusion, the cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.« less

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates

DOE PAGES

Silva, Chinthaka M.; Rosseel, Thomas M.; Kirkegaard, Marie C.

2018-03-07

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18, 4 × 10 19, and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasingmore » neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2, with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. In conclusion, the cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.« less

Experimental determination of spin-dependent electron density by joint refinement of X-ray and polarized neutron diffraction data.

PubMed

Deutsch, Maxime; Claiser, Nicolas; Pillet, Sébastien; Chumakov, Yurii; Becker, Pierre; Gillet, Jean Michel; Gillon, Béatrice; Lecomte, Claude; Souhassou, Mohamed

2012-11-01

New crystallographic tools were developed to access a more precise description of the spin-dependent electron density of magnetic crystals. The method combines experimental information coming from high-resolution X-ray diffraction (XRD) and polarized neutron diffraction (PND) in a unified model. A new algorithm that allows for a simultaneous refinement of the charge- and spin-density parameters against XRD and PND data is described. The resulting software MOLLYNX is based on the well known Hansen-Coppens multipolar model, and makes it possible to differentiate the electron spins. This algorithm is validated and demonstrated with a molecular crystal formed by a bimetallic chain, MnCu(pba)(H(2)O)(3)·2H(2)O, for which XRD and PND data are available. The joint refinement provides a more detailed description of the spin density than the refinement from PND data alone.

The new HMI beamline MAGS: an instrument for hard X-ray diffraction at BESSY.

PubMed

Dudzik, Esther; Feyerherm, Ralf; Diete, Wolfgang; Signorato, Riccardo; Zilkens, Christopher

2006-11-01

The Hahn-Meitner-Institute Berlin is operating the new hard X-ray diffraction beamline MAGS at the Berlin synchrotron radiation source BESSY. The beamline is intended to complement the existing neutron instrumentation at the Berlin Neutron Scattering Centre. The new beamline uses a 7 T multipole wiggler to produce photon fluxes in the 10(11)-10(12) photons s(-1) (100 mA)(-1) (0.1% bandwidth)(-1) range at energies from 4 to 30 keV at the experiment. It has active bendable optics to provide flexible horizontal and vertical focusing and to compensate the large heat load from the wiggler source. The experimental end-station consists of a six-circle Huber diffractometer which can be used with an additional (polarization) analyser and different sample environments. The beamline is intended for single-crystal diffraction and resonant magnetic scattering experiments for the study of ordering phenomena, phase transitions and materials science.

Probing magnetic order in CuFeO2 through nuclear forward scattering in high magnetic fields

NASA Astrophysics Data System (ADS)

Strohm, C.; Lummen, T. T. A.; Handayani, I. P.; Roth, T.; Detlefs, C.; van der Linden, P. J. E. M.; van Loosdrecht, P. H. M.

2013-08-01

Determining the magnetic order of solids in high magnetic fields is technologically challenging. Here we probe the cascade of magnetic phase transitions in frustrated multiferroic CuFeO2 using nuclear forward scattering (NFS) in pulsed magnetic fields up to 30 T. Our results are in excellent agreement with detailed neutron diffraction experiments, currently limited to 15 T, while providing experimental confirmation of the proposed higher field phases for both H∥c and H⊥c. We thus establish NFS as a valuable tool for spin structure studies in very high fields, both complementing and expanding on the applicability of existing techniques.

Structure Evolution and Thermoelectric Properties of Carbonized Polydopamine Thin Films.

PubMed

Li, Haoqi; Aulin, Yaroslav V; Frazer, Laszlo; Borguet, Eric; Kakodkar, Rohit; Feser, Joseph; Chen, Yan; An, Ke; Dikin, Dmitriy A; Ren, Fei

2017-03-01

Carbonization of nature-inspired polydopamine can yield thin films with high electrical conductivity. Understanding of the structure of carbonized PDA (cPDA) is therefore highly desired. In this study, neutron diffraction, Raman spectroscopy, and other techniques indicate that cPDA samples are mainly amorphous with some short-range ordering and graphite-like structure that emerges with increasing heat treatment temperature. The electrical conductivity and the Seebeck coefficient show different trends with heat treatment temperature, while the thermal conductivity remains insensitive. The largest room-temperature ZT of 2 × 10 -4 was obtained on samples heat-treated at 800 °C, which is higher than that of reduced graphene oxide.

Charge Fluctuations in the NdO1-xFxBiS2 Superconductors

NASA Astrophysics Data System (ADS)

Athauda, Anushika; Mizuguchi, Yoshikazu; Nagao, Masanori; Neuefeind, Joerg; Louca, Despina

2017-12-01

The local atomic structure of superconducting NdO1-xFxBiS2 (x = 0.2 and 0.4) is investigated using neutron diffraction and the pair density function analysis technique. In the non-superconducting x = 0.2 composition, ferrodistortive displacements of the pyramidal sulfur ions break the tetragonal symmetry and a superlattice structure emerges with peaks appearing at h + k odd reflections superimposed on the even reflections of the P4/nmm symmetry. In the superconducting x = 0.4 composition, similar ferrodistortive displacements are observed but with different magnitudes coupled with in-plane Bi distortions which are indicative of charge fluctuations.

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

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

Bennett, Brad C.; Meilleur, Flora; Myles, Dean A A

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 statesmore » 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.« less

Structure and Dynamics of Quasi-Ordered Systems

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

Eckert, J.; Redondo, A.; Henson, N.J.

1999-07-09

The functionality of many materials of both fundamental and technological interest is often critically dependent on the nature and extent of any disorder that may be present. In addition, it is often difficult to understand the nature of disorder in quite well ordered systems. There is therefore an urgent need to develop better tools, both experimental and computational, for the study of such quasi-ordered systems. To this end, the authors have used neutron diffraction studies in an attempt to locate small metal clusters or molecules randomly distributed inside microporous catalytic materials. Specifically, they have used pair distribution function (PDF) analysis,more » as well as inelastic neutron scattering (INS) spectroscopy, to study interactions between adsorbate molecules and a microporous matrix. They have interfaced these experimental studies with computations of PDF analysis as well as modeling of the dynamics of adsorbates. These techniques will be invaluable in elucidating the local structure and function of many of these classes of materials.« less

Daniel Shechtman and Quasicrystals

Science.gov Websites

toolbox that included transmission electron microscopy, X-ray diffraction and neutron diffraction. The searchQuery x Find DOE R&D Acccomplishments Navigation dropdown arrow The Basics dropdown arrow Home About Letters, Vol. 53, Issue 20: 1951-1953; November 12, 1984 Nuclear γ-ray resonance observations in an

Radiation attenuation by single-crystal diamond windows

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

Guthrie, M.; Pruteanu, C. G.; Donnelly, M. -E.

As artificial diamond becomes more cost effective it is likely to see increasing use as a window for sample environment equipment used in diffraction experiments. Such windows are particularly useful as they exhibit exceptional mechanical properties in addition to being highly transparent to both X-ray and neutron radiation. A key application is in high-pressure studies, where diamond anvil cells (DACs) are used to access extreme sample conditions. However, despite their utility, an important consideration when using single-crystal diamond windows is their interaction with the incident beam. In particular, the Bragg condition will be satisfied for specific angles and wavelengths, leadingmore » to the appearance of diamond Bragg spots on the diffraction detectors but also, unavoidably, to loss of transmitted intensity of the beam that interacts with the sample. This effect can be particularly significant for energy-dispersive measurements, for example, in time-of-flight neutron diffraction work using DACs. This article presents a semi-empirical approach that can be used to correct for this effect, which is a prerequisite for the accurate determination of diffraction intensities.« less

Radiation attenuation by single-crystal diamond windows

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

Guthrie, Malcolm; Pruteanu, Ciprian G.; Donnelly, Mary -Ellen

As artificial diamond becomes more cost effective it is likely to see increasing use as a window for sample environment equipment used in diffraction experiments. Such windows are particularly useful as they exhibit exceptional mechanical properties in addition to being highly transparent to both X-ray and neutron radiation. A key application is in high-pressure studies, where diamond anvil cells (DACs) are used to access extreme sample conditions. However, despite their utility, an important consideration when using single-crystal diamond windows is their interaction with the incident beam. In particular, the Bragg condition will be satisfied for specific angles and wavelengths, leadingmore » to the appearance of diamond Bragg spots on the diffraction detectors but also, unavoidably, to loss of transmitted intensity of the beam that interacts with the sample. This effect can be particularly significant for energy-dispersive measurements, for example, in time-of-flight neutron diffraction work using DACs. Furthermore, this article presents a semi-empirical approach that can be used to correct for this effect, which is a prerequisite for the accurate determination of diffraction intensities.« less

Radiation attenuation by single-crystal diamond windows

DOE PAGES

Guthrie, Malcolm; Pruteanu, Ciprian G.; Donnelly, Mary -Ellen; ...

2017-02-01

As artificial diamond becomes more cost effective it is likely to see increasing use as a window for sample environment equipment used in diffraction experiments. Such windows are particularly useful as they exhibit exceptional mechanical properties in addition to being highly transparent to both X-ray and neutron radiation. A key application is in high-pressure studies, where diamond anvil cells (DACs) are used to access extreme sample conditions. However, despite their utility, an important consideration when using single-crystal diamond windows is their interaction with the incident beam. In particular, the Bragg condition will be satisfied for specific angles and wavelengths, leadingmore » to the appearance of diamond Bragg spots on the diffraction detectors but also, unavoidably, to loss of transmitted intensity of the beam that interacts with the sample. This effect can be particularly significant for energy-dispersive measurements, for example, in time-of-flight neutron diffraction work using DACs. Furthermore, this article presents a semi-empirical approach that can be used to correct for this effect, which is a prerequisite for the accurate determination of diffraction intensities.« less

Suppression of magnetic order in CaCo1.86As2 with Fe substitution: Magnetization, neutron diffraction, and x-ray diffraction studies of Ca (Co1-xFex) yAs2

NASA Astrophysics Data System (ADS)

Jayasekara, W. T.; Pandey, Abhishek; Kreyssig, A.; Sangeetha, N. S.; Sapkota, A.; Kothapalli, K.; Anand, V. K.; Tian, W.; Vaknin, D.; Johnston, D. C.; McQueeney, R. J.; Goldman, A. I.; Ueland, B. G.

2017-02-01

Magnetization, neutron diffraction, and high-energy x-ray diffraction results for Sn-flux grown single-crystal samples of Ca (Co1-xFex) yAs2 , 0 ≤x ≤1 , 1.86 ≤y ≤2 , are presented and reveal that A-type antiferromagnetic order, with ordered moments lying along the c axis, persists for x ≲0.12 (1 ) . The antiferromagnetic order is smoothly suppressed with increasing x , with both the ordered moment and Néel temperature linearly decreasing. Stripe-type antiferromagnetic order does not occur for x ≤0.25 , nor does ferromagnetic order for x up to at least x =0.104 , and a smooth crossover from the collapsed-tetragonal (cT) phase of CaCo1.86As2 to the tetragonal (T) phase of CaFe2As2 occurs. These results suggest that hole doping CaCo1.86As2 has a less dramatic effect on the magnetism and structure than steric effects due to substituting Sr for Ca.

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

PubMed

Murshed, M Mangir; Kuhs, Werner F

2009-04-16

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

AND/R: Advanced neutron diffractometer/reflectometer for investigation of thin films and multilayers for the life sciences

PubMed Central

Dura, Joseph A.; Pierce, Donald J.; Majkrzak, Charles F.; Maliszewskyj, Nicholas C.; McGillivray, Duncan J.; Lösche, Mathias; O'Donovan, Kevin V.; Mihailescu, Mihaela; Perez-Salas, Ursula; Worcester, David L.; White, Stephen H.

2011-01-01

An elastic neutron scattering instrument, the advanced neutron diffractometer/reflectometer (AND/R), has recently been commissioned at the National Institute of Standards and Technology Center for Neutron Research. The AND/R is the centerpiece of the Cold Neutrons for Biology and Technology partnership, which is dedicated to the structural characterization of thin films and multilayers of biological interest. The instrument is capable of measuring both specular and nonspecular reflectivity, as well as crystalline or semicrystalline diffraction at wave-vector transfers up to approximately 2.20 Å−1. A detailed description of this flexible instrument and its performance characteristics in various operating modes are given. PMID:21892232

Real time neutron diffraction and NMR of the Empress II glass-ceramic system.

PubMed

O'Donnell, M D; Hill, R G; Karpukhina, N; Law, R V

2011-10-01

This study reports real time neutron diffraction on the Empress II glass-ceramic system. The commercial glass-ceramics was characterized by real time neutron diffraction, ³¹P and ²⁹Si solid-state MAS-NMR, DSC and XRD. On heating, the as-received glass ceramic contained lithium disilicate (Li₂Si₂O₅), which melted with increasing temperature. This was revealed by neutron diffraction which showed the Bragg peaks for this phase had disappeared by 958°C in agreement with thermal analysis. On cooling lithium metasilicate (Li₂SiO₃) started to form at around 916°C and a minor phase of cristobalite at around 852°C. The unit cell volume of both Li-silicate phases increased linearly with temperature at a rate of +17×10⁻³ ų.°C⁻¹. Room temperature powder X-ray diffraction (XRD) of the material after cooling confirms presence of the lithium metasilicate and cristobalite as the main phases and shows, in addition, small amount of lithium disilicate and orthophosphate. ³¹P MAS-NMR reveals presence of the lithiorthophosphate (Li₃PO₄) before and after heat treatment. The melting of lithium disilicate on heating and crystallisation of lithium metasilicate on cooling agree with endothermic and exotermic features respectively observed by DSC. ²⁹Si MAS-NMR shows presence of lithium disilicate phase in the as-received glass-ceramic, though not in the major proportion, and lithium metasilicate in the material after heat treatment. Both phases have significantly long T₁ relaxation time, especially the lithium metasilicate, therefore, a quantitative analysis of the ²⁹Si MAS-NMR spectra was not attempted. Significance. The findings of the present work demonstrate importance of the commercially designed processing parameters in order to preserve desired characteristics of the material. Processing the Empress II at a rate slower than recommended 60°C min⁻¹ or long isothermal hold at the maximal processing temperature 920°C can cause crystallization of lithium metasilicate and cristobalite instead of lithium disilicate as major phase. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Crystal Structure of Hydrazinium Iodide by Neutron Diffraction

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

Campbell, Eric V.; Wang, Xiaoping; Miller, Joel S.

The structure of hydrazinium iodide, [H 5N 2] +·I -, at 100 K has monoclinic (P2 1/n) symmetry from single crystal neutron diffraction with a = 7.4599(7) Å, b = 5.3185(6) Å, c = 10.1628(11) Å, β = 103.150(10)°, V = 392.64(7) Å 3, Z = 4. The refinement converged to R = 0.0575, wR 2 = 0.1602, S = 1.022. Data for the crystal structure was collected on the SNS TOPAZ single-crystal time-of-flight Laue diffractometer. The compound has a one-dimensional structure which displays N–H···N hydrogen bonding. Finally, accurate intra- and intermolecular N–H distances have been determined.

Crystal Structure of Hydrazinium Iodide by Neutron Diffraction

DOE PAGES

Campbell, Eric V.; Wang, Xiaoping; Miller, Joel S.

2017-10-31

The structure of hydrazinium iodide, [H 5N 2] +·I -, at 100 K has monoclinic (P2 1/n) symmetry from single crystal neutron diffraction with a = 7.4599(7) Å, b = 5.3185(6) Å, c = 10.1628(11) Å, β = 103.150(10)°, V = 392.64(7) Å 3, Z = 4. The refinement converged to R = 0.0575, wR 2 = 0.1602, S = 1.022. Data for the crystal structure was collected on the SNS TOPAZ single-crystal time-of-flight Laue diffractometer. The compound has a one-dimensional structure which displays N–H···N hydrogen bonding. Finally, accurate intra- and intermolecular N–H distances have been determined.

When combined X-ray and polarized neutron diffraction data challenge high-level calculations: spin-resolved electron density of an organic radical.

PubMed

Voufack, Ariste Bolivard; Claiser, Nicolas; Lecomte, Claude; Pillet, Sébastien; Pontillon, Yves; Gillon, Béatrice; Yan, Zeyin; Gillet, Jean Michel; Marazzi, Marco; Genoni, Alessandro; Souhassou, Mohamed

2017-08-01

Joint refinement of X-ray and polarized neutron diffraction data has been carried out in order to determine charge and spin density distributions simultaneously in the nitronyl nitroxide (NN) free radical Nit(SMe)Ph. For comparison purposes, density functional theory (DFT) and complete active-space self-consistent field (CASSCF) theoretical calculations were also performed. Experimentally derived charge and spin densities show significant differences between the two NO groups of the NN function that are not observed from DFT theoretical calculations. On the contrary, CASSCF calculations exhibit the same fine details as observed in spin-resolved joint refinement and a clear asymmetry between the two NO groups.

Low-dimensional ordering and fluctuations in methanol-{beta}-hydroquinone clathrate studied by x-ray and neutron diffraction

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

Rheinstaedter, Maikel C.; Enderle, Mechthild; Kloepperpieper, Axel

2005-01-01

Methanol-{beta}-hydroquinone clathrate has been established as a model system for dielectric ordering and fluctuations and is conceptually close to magnetic spin systems. In x-ray and neutron diffraction experiments, we investigated the ordered structure, the one-dimensional (1D) and the three-dimensional critical scattering in the paraelectric phase, and the temperature dependence of the lattice constants. Our results can be explained by microscopic models of the methanol pseudospin in the hydroquinone cage network, in consistency with previous dielectric investigations. A coupling of the 1D fluctuations to local strains leads to an anomalous temperature dependence of the 1D lattice parameter in the paraelectric regime.

In-situ neutron diffraction study of martensitic variant redistribution in polycrystalline Ni-Mn-Ga alloy under cyclic thermo-mechanical treatment

NASA Astrophysics Data System (ADS)

Li, Zongbin; Zhang, Yudong; Esling, Claude; Gan, Weimin; Zou, Naifu; Zhao, Xiang; Zuo, Liang

2014-07-01

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⟩7M preferential orientation along the loading axis. As a result, the saturation of magnetization became easier to be reached.

In-situ neutron diffraction study of martensitic variant redistribution in polycrystalline Ni-Mn-Ga alloy under cyclic thermo-mechanical treatment

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

Li, Zongbin; Zou, Naifu; Zhao, Xiang

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.

Neutron Diffraction Study On Gamma To Alpha Phase Transition In Ce0.9th0.1 Alloy

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

Lashley, Jason C1; Heffner, Robert H; Llobet, A

2008-01-01

Comprehensive neutron diffraction measurements were performed to study the isostructural {gamma} {leftrightarrow} {alpha} phase transition in Ce{sub 0.9}Th{sub 0.1} alloy. Using Rietveld refinements, we obtained lattice and thermal parameters as a function of temperature. From the temperature slope of the thermal parameters, we determined Debye temperatures {Theta}{sup {gamma}}{sub D} = 133(1) K and {Theta}{sup {alpha}}{sub D} = 140(1) K for the {gamma} phase and the {alpha} phase, respectively. This result implies that the vibrational entropy change is not significant at the {gamma} {leftrightarrow} {alpha} transition, contrary to that from elemental Cerium [Phys. Rev. Lett. 92, 105702, 2004].

Electron Diffraction Using Transmission Electron Microscopy

PubMed Central

Bendersky, Leonid A.; Gayle, Frank W.

2001-01-01

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

Development of pair distribution function analysis

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

Vondreele, R.; Billinge, S.; Kwei, G.

1996-09-01

This is the final report of a 3-year LDRD project at LANL. It has become more and more evident that structural coherence in the CuO{sub 2} planes of high-{Tc} superconducting materials over some intermediate length scale (nm range) is important to superconductivity. In recent years, the pair distribution function (PDF) analysis of powder diffraction data has been developed for extracting structural information on these length scales. This project sought to expand and develop this technique, use it to analyze neutron powder diffraction data, and apply it to problems. In particular, interest is in the area of high-{Tc} superconductors, although wemore » planned to extend the study to the closely related perovskite ferroelectric materials andother materials where the local structure affects the properties where detailed knowledge of the local and intermediate range structure is important. In addition, we planned to carry out single crystal experiments to look for diffuse scattering. This information augments the information from the PDF.« less

Thermal stress effects in intermetallic matrix composites

NASA Technical Reports Server (NTRS)

Wright, P. K.; Sensmeier, M. D.; Kupperman, D. S.; Wadley, H. N. G.

1993-01-01

Intermetallic matrix composites develop residual stresses from the large thermal expansion mismatch (delta-alpha) between the fibers and matrix. This work was undertaken to: establish improved techniques to measure these thermal stresses in IMC's; determine residual stresses in a variety of IMC systems by experiments and modeling; and, determine the effect of residual stresses on selected mechanical properties of an IMC. X ray diffraction (XRD), neutron diffraction (ND), synchrotron XRD (SXRD), and ultrasonics (US) techniques for measuring thermal stresses in IMC were examined and ND was selected as the most promising technique. ND was demonstrated on a variety of IMC systems encompassing Ti- and Ni-base matrices, SiC, W, and Al2O3 fibers, and different fiber fractions (Vf). Experimental results on these systems agreed with predictions of a concentric cylinder model. In SiC/Ti-base systems, little yielding was found and stresses were controlled primarily by delta-alpha and Vf. In Ni-base matrix systems, yield strength of the matrix and Vf controlled stress levels. The longitudinal residual stresses in SCS-6/Ti-24Al-llNb composite were modified by thermomechanical processing. Increasing residual stress decreased ultimate tensile strength in agreement with model predictions. Fiber pushout strength showed an unexpected inverse correlation with residual stress. In-plane shear yield strength showed no dependence on residual stress. Higher levels of residual tension led to higher fatigue crack growth rates, as suggested by matrix mean stress effects.

Multidataset Refinement Resonant Diffraction, and Magnetic Structures

PubMed Central

Attfield, J. Paul

2004-01-01

The scope of Rietveld and other powder diffraction refinements continues to expand, driven by improvements in instrumentation, methodology and software. This will be illustrated by examples from our research in recent years. Multidataset refinement is now commonplace; the datasets may be from different detectors, e.g., in a time-of-flight experiment, or from separate experiments, such as at several x-ray energies giving resonant information. The complementary use of x rays and neutrons is exemplified by a recent combined refinement of the monoclinic superstructure of magnetite, Fe3O4, below the 122 K Verwey transition, which reveals evidence for Fe2+/Fe3+ charge ordering. Powder neutron diffraction data continue to be used for the solution and Rietveld refinement of magnetic structures. Time-of-flight instruments on cold neutron sources can produce data that have a high intensity and good resolution at high d-spacings. Such profiles have been used to study incommensurate magnetic structures such as FeAsO4 and β–CrPO4. A multiphase, multidataset refinement of the phase-separated perovskite (Pr0.35Y0.07Th0.04Ca0.04Sr0.5)MnO3 has been used to fit three components with different crystal and magnetic structures at low temperatures. PMID:27366599

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

DOE PAGES

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

Structure, magnetic properties, polarized neutron diffraction, and theoretical study of a copper(II) cubane.

PubMed

Aronica, Christophe; Chumakov, Yurii; Jeanneau, Erwann; Luneau, Dominique; Neugebauer, Petr; Barra, Anne-Laure; Gillon, Béatrice; Goujon, Antoine; Cousson, Alain; Tercero, Javier; Ruiz, Eliseo

2008-01-01

The paper reports the synthesis, X-ray and neutron diffraction crystal structures, magnetic properties, high field-high frequency EPR (HF-EPR), spin density and theoretical description of the tetranuclear CuII complex [Cu4L4] with cubane-like structure (LH2=1,1,1-trifluoro-7-hydroxy-4-methyl-5-aza-hept-3-en-2-one). The simulation of the magnetic behavior gives a predominant ferromagnetic interaction J1 (+30.5 cm(-1)) and a weak antiferromagnetic interaction J2 (-5.5 cm(-1)), which correspond to short and long Cu-Cu distances, respectively, as evidence from the crystal structure [see formulate in text]. It is in agreement with DFT calculations and with the saturation magnetization value of an S=2 ground spin state. HF-EPR measurements at low temperatures (5 to 30 K) provide evidence for a negative axial zero-field splitting parameter D (-0.25+/-0.01 cm(-1)) plus a small rhombic term E (0.025+/-0.001 cm(-1), E/D = 0.1). The experimental spin distribution from polarized neutron diffraction is mainly located in the basal plane of the CuII ion with a distortion of yz-type for one CuII ion. Delocalization on the ligand (L) is observed but to a smaller extent than expected from DFT calculations.

On the temperature dependence of H-U{sub iso} in the riding hydrogen model

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

Lübben, Jens; Volkmann, Christian; Grabowsky, Simon

The temperature dependence of hydrogen U{sub iso} and parent U{sub eq} in the riding hydrogen model is investigated by neutron diffraction, aspherical-atom refinements and QM/MM and MO/MO cluster calculations. Fixed values of 1.2 or 1.5 appear to be underestimated, especially at temperatures below 100 K. The temperature dependence of H-U{sub iso} in N-acetyl-l-4-hydroxyproline monohydrate is investigated. Imposing a constant temperature-independent multiplier of 1.2 or 1.5 for the riding hydrogen model is found to be inaccurate, and severely underestimates H-U{sub iso} below 100 K. Neutron diffraction data at temperatures of 9, 150, 200 and 250 K provide benchmark results for thismore » study. X-ray diffraction data to high resolution, collected at temperatures of 9, 30, 50, 75, 100, 150, 200 and 250 K (synchrotron and home source), reproduce neutron results only when evaluated by aspherical-atom refinement models, since these take into account bonding and lone-pair electron density; both invariom and Hirshfeld-atom refinement models enable a more precise determination of the magnitude of H-atom displacements than independent-atom model refinements. Experimental efforts are complemented by computing displacement parameters following the TLS+ONIOM approach. A satisfactory agreement between all approaches is found.« less

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

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

Jacobs, Philipp; Houben, Andreas; Senyshyn, Anatoliy

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 parallelmore » 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.« less

Thermomechanical behavior and microstructural evolution of a Ni(Pd)-rich Ni 24.3Ti 49.7Pd 26 high temperature shape memory alloy

DOE PAGES

Benafan, O.; Garg, A.; Noebe, R. D.; ...

2015-04-20

We investigated the effect of thermomechanical cycling on a slightly Ni(Pd)-rich Ni 24.3Ti 49.7Pd 26 (near stochiometric Ni–Ti basis with Pd replacing Ni) high temperature shape memory alloy. Furthermore, aged tensile specimens (400 °C/24 h/furnace cooled) were subjected to constant-stress thermal cycling in conjunction with microstructural assessment via in situ neutron diffraction and transmission electron microscopy (TEM), before and after testing. It was shown that in spite of the slightly Ni(Pd)-rich composition and heat treatment used to precipitation harden the alloy, the material exhibited dimensional instabilities with residual strain accumulation reaching 1.5% over 10 thermomechanical cycles. This was attributed tomore » insufficient strengthening of the material (insufficient volume fraction of precipitate phase) to prevent plasticity from occurring concomitant with the martensitic transformation. In situ neutron diffraction revealed the presence of retained martensite while cycling under 300 MPa stress, which was also confirmed by transmission electron microscopy of post-cycled samples. Neutron diffraction analysis of the post-thermally-cycled samples under no-load revealed residual lattice strains in the martensite and austenite phases, remnant texture in the martensite phase, and peak broadening of the austenite phase. The texture we developed in the martensite phase was composed mainly of those martensitic tensile variants observed during thermomechanical cycling. Presence of a high density of dislocations, deformation twins, and retained martensite was revealed in the austenite state via in-situ TEM in the post-cycled material, providing an explanation for the observed peak broadening in the neutron diffraction spectra. Despite the dimensional instabilities, this alloy exhibited a biased transformation strain on the order of 3% and a two-way shape memory effect (TWSME) strain of ~2%, at relatively high actuation temperatures.« less

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB6 Single Crystals

PubMed Central

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; Tutmaher, J. A.; Leiner, J. C.; Lumsden, M. D.; Lavelle, C. M.; Wang, X. P.; Hoffmann, C.; Siegler, M. A.; Haldolaarachchige, N.; Young, D. P.; McQueen, T. M.

2016-01-01

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-ray computed tomography experiments we observe that natural isotope containing (SmB6) and doubly isotope enriched (154Sm11B6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB6. These results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported. PMID:26892648

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB 6 Single Crystals

DOE PAGES

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; ...

2016-02-19

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB 6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB 6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB 6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-raymore » computed tomography experiments we observe that natural isotope containing (SmB 6) and doubly isotope enriched ( 154Sm 11B 6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB 6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB 6. Finally, these results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB 6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported.« less

Current trends in protein crystallization.

PubMed

Gavira, José A

2016-07-15

Proteins belong to the most complex colloidal system in terms of their physicochemical properties, size and conformational-flexibility. This complexity contributes to their great sensitivity to any external change and dictate the uncertainty of crystallization. The need of 3D models to understand their functionality and interaction mechanisms with other neighbouring (macro)molecules has driven the tremendous effort put into the field of crystallography that has also permeated other fields trying to shed some light into reluctant-to-crystallize proteins. This review is aimed at revising protein crystallization from a regular-laboratory point of view. It is also devoted to highlight the latest developments and achievements to produce, identify and deliver high-quality protein crystals for XFEL, Micro-ED or neutron diffraction. The low likelihood of protein crystallization is rationalized by considering the intrinsic polypeptide nature (folded state, surface charge, etc) followed by a description of the standard crystallization methods (batch, vapour diffusion and counter-diffusion), including high throughput advances. Other methodologies aimed at determining protein features in solution (NMR, SAS, DLS) or to gather structural information from single particles such as Cryo-EM are also discussed. Finally, current approaches showing the convergence of different structural biology techniques and the cross-methodologies adaptation to tackle the most difficult problems, are presented. Current advances in biomacromolecules crystallization, from nano crystals for XFEL and Micro-ED to large crystals for neutron diffraction, are covered with special emphasis in methodologies applicable at laboratory scale. Copyright © 2015 Elsevier Inc. All rights reserved.

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

Ritscher, A.; Helmholtz-Zentrum Berlin für Materialien und Energie, Hahn-Meitner-Platz 1, 14109 Berlin; Hoelzel, M.

In this work a series of stoichiometric Cu{sub 2}ZnSnS{sub 4} (CZTS) samples annealed at different temperatures in the range of 473–623 K were investigated. The temperature dependence of the Cu/Zn-order-disorder behavior was analyzed by neutron powder diffraction measurements. Cu fully occupies the 2a and Sn the 2b position within the whole temperature range. For Zn and the remaining Cu on sites 2d and 2c, a clear change from ordered to disordered kesterite structure is found. The critical temperature T{sub c} for this Landau-type second order transition was determined as 552±2 K. It was found that in Cu{sub 2}ZnSnS{sub 4} verymore » long annealing times are necessary to reach equilibrium at low temperatures. - Graphical abstract: The order-disorder transition in Cu{sub 2}ZnSnS{sub 4} was investigated using neutron diffraction techniques on samples annealed in the temperature range of 473–623 K. The critical temperature T{sub c} for this Landau-type second order transition was determined as 552±2 K. Display Omitted - Highlights: • The order-disorder transformation of Cu{sub 2}ZnSnS{sub 4} follows a Landau‐type behavior for a second order transition. • The critical exponent β is 0.57±0.06. • The critical temperature was determined as 552±2 K. • A fully ordered (within the standard deviation) Cu{sub 2}ZnSnS{sub 4} sample was synthesized.« less

Refinement of the crystal structure of the high-temperature phase G0 in (NH4)2WO2F4 (powder, x-ray, and neutron scattering)

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

Novak, D. M.; Smirnov, Lev S; Kolesnikov, Alexander I

2013-01-01

The (NH4)2WO2F4 compound undergoes a series of phase transitions: G0 -> 201 K -> G1 -> 160 K -> G2, with a significant change in entropy ( S1 ~ Rln10 at the G0 -> G1 transition), which indicates significant orientational disordering in the G0 phase and the order disorder type of the phase transition. X-ray diffraction is used to identify the crystal structure of the G0 phase as rhombohedral (sp. gr. Cmcm, Z = 4), determine the lattice parameters and the positions of all atoms (except hydrogen), and show that [WO2F4]2 ions can form a superposition of dynamic and staticmore » orientational disorders in the anionic sublattice. A determination of the orientational position of [NH4]+ ions calls for the combined method of elastic and inelastic neutron scattering. Inelastic neutron scattering is used to determine the state of hindered rotation for ammonium ions in the G0 phase. Powder neutron diffraction shows that the orientational disorder of NH4 ions can adequately be described within the free rotation approximation.« less

Small-angle neutron scattering study of the short-range organization of dispersed CsNi[Cr(CN){sub 6}] nanoparticles

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

Ridier, Karl; Gillon, Béatrice; André, Gilles

2015-09-21

Prussian blue analogues magnetic nanoparticles (of radius R{sub 0} = 2.4–8.6 nm) embedded in PVP (polyvinylpyrrolidone) or CTA{sup +} (cetyltrimethylammonium) matrices have been studied using neutron diffraction and small angle neutron scattering (SANS) at several concentrations. For the most diluted particles in neutral PVP, the SANS signal is fully accounted for by a “single-particle” spherical form factor with no structural correlations between the nanoparticles and with radii comparable to those inferred from neutron diffraction. For higher concentration in PVP, structural correlations modify the SANS signal with the appearance of a structure factor peak, which is described using an effective “mean-field” model. A newmore » length scale R{sup * }≈ 3R{sub 0}, corresponding to an effective repulsive interaction radius, is evidenced in PVP samples. In CTA{sup +}, electrostatic interactions play a crucial role and lead to a dense layer of CTA{sup +} around the nanoparticles, which considerably alter the SANS patterns as compared to PVP. The SANS data of nanoparticles in CTA{sup +} are best described by a core-shell model without visible inter-particle structure factor.« less

Residual stresses in a stainless steel - titanium alloy joint made with the explosive technique

NASA Astrophysics Data System (ADS)

Taran, Yu V.; Balagurov, A. M.; Sabirov, B. M.; Evans, A.; Davydov, V.; Venter, A. M.

2012-02-01

Joining of pipes from stainless steel (SS) and titanium (Ti) alloy still experience serious technical problems. Recently, reliable and hermetic joining of SS and Ti pipes has been achieved with the explosive bonding technique in the Russian Federal Nuclear Center. Such adapters are earmarked for use at the future International Linear Collider. The manufactured SS-Ti adapters have excellent mechanical behavior at room and liquid nitrogen temperatures, during high-pressure tests and thermal cycling. We here report the first neutron diffraction investigation of the residual stresses in a SS-Ti adapter on the POLDI instrument at the SINQ spallation source. The strain scanning across the adapter walls into the SS-SS and SS-Ti pipes sections encompassed measurement of the axial, radial and hoop strain components, which were transformed into residual stresses. The full stress information was successfully determined for the three steel pipes involved in the joint. The residual stresses do not exceed 300 MPa in magnitude. All stress components have tensile values close to the adapter internal surface, whilst they are compressive close to the outer surface. The strong incoherent and weak coherent neutron scattering cross-sections of Ti did not allow for the reliable determination of stresses inside the titanic pipe.

Neutron assay in mixed radiation fields with a 6Li-loaded plastic scintillator

NASA Astrophysics Data System (ADS)

Balmer, M. J. I.; Gamage, K. A. A.; Taylor, G. C.

2015-08-01

A novel technique for assay of thermal and fast neutrons in a 6Li-loaded plastic scintillator is presented. Existing capture-gated thermal neutron detection techniques were evaluated with the 6Li-loaded plastic scintillator studied in this work. Using simulations and experimental work, shortcomings in its performance were highlighted. As a result, it was proposed that by separating the combined fast and thermal neutron events from gamma events, using established pulse shape discrimination techniques, the thermal neutron events could then be assayed. Experiments were conducted at the National Physical Laboratory, Teddington, performing neutron assays with seven different neutron fields using the proposed technique. For each field, thermal and fast neutron content was estimated and were shown to corroborate with the seven synthesised fields.

Debye temperatures and magnetic structures of UFe xAl 12- x (3.6⩽ x⩽5) intermetallic alloys

NASA Astrophysics Data System (ADS)

Rećko, K.; Dobrzyński, L.; Szymański, K.; Hoser, A.

2000-03-01

Uranium ternary compounds UFe xAl 12- x crystallize in a body-centred tetragonal structure ThMn 12 (I 4/mmm No.139). The neutron powder diffraction, magnetization measurements as well as Mössbauer investigations clearly indicate the magnetic ordering within the iron sites. The rearrangement of iron magnetic moments from uncompensated antiferromagnetic system in UFe xAl 12- x with x<4, through coexistence of antiferro- and ferromagnetic iron components (4⩽ x<5) to pure ferromagnetic ordering for alloy with x=5 is observed. The neutron diffraction studies of magnetic structures of the aforementioned powder samples show a very rich world of possible uranium-iron magnetic interactions. For all these alloys the magnetic neutron scattering is generally weak in comparison to the nuclear one. Because of identical chemical and magnetic unit cells there are no pure magnetic reflections. Therefore, in order to extract magnetic part of the scattering one should be particularly careful in taking proper account of the thermal vibration effects.

Zigzag spin structure in layered honeycomb L i3N i2Sb O6 : A combined diffraction and antiferromagnetic resonance study

NASA Astrophysics Data System (ADS)

Kurbakov, A. I.; Korshunov, A. N.; Podchezertsev, S. Yu.; Malyshev, A. L.; Evstigneeva, M. A.; Damay, F.; Park, J.; Koo, C.; Klingeler, R.; Zvereva, E. A.; Nalbandyan, V. B.

2017-07-01

The magnetic structure of L i3N i2Sb O6 has been determined by low-temperature neutron diffraction, and the crystal structure has been refined by a combination of synchrotron and neutron powder diffraction. The monoclinic (C 2 /m ) symmetry, assigned previously to this pseudohexagonal layered structure, has been unambiguously proven by peak splitting in the synchrotron diffraction pattern. The structure is based on essentially hexagonal honeycomb-ordered N i2Sb O6 layers alternating with L i3 layers, all cations and anions being in an octahedral environment. The compound orders antiferromagnetically below TN=15 K , with the magnetic supercell being a 2 a ×2 b multiple of the crystal cell. The magnetic structure within the honeycomb layer consists of zigzag ferromagnetic spin chains coupled antiferromagnetically. The ordered magnetic moment amounts to 1.62 (2 ) μB/Ni , which is slightly lower than the full theoretical value. Upon cooling below TN, the spins tilt from the c axis, with a maximum tilting angle of 15 .6∘ at T =1.5 K . Our data imply non-negligible ferromagnetic interactions between the honeycomb layers. The observed antiferromagnetic resonance modes are in agreement with the two-sublattice model derived from the neutron data. Orthorhombic anisotropy shows up in zero-field splitting of Δ =198 ±4 and 218 ±4 GHz . Above TN, the electron spin resonance data imply short-range antiferromagnetic order up to about 80 K.

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.

Neutron Scattering Studies of Vortex Matter in Type-II Superconductors

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

Xinsheng Ling

2012-02-02

The proposed program is an experimental study of the fundamental properties of Abrikosov vortex matter in type-II superconductors. Most superconducting materials used in applications such as MRI are type II and their transport properties are determined by the interplay between random pinning, interaction and thermal fluctuation effects in the vortex state. Given the technological importance of these materials, a fundamental understanding of the vortex matter is necessary. The vortex lines in type-II superconductors also form a useful model system for fundamental studies of a number of important issues in condensed matter physics, such as the presence of a symmetry-breaking phasemore » transition in the presence of random pinning. Recent advances in neutron scattering facilities such as the major upgrade of the NIST cold source and the Spallation Neutron Source are providing unprecedented opportunities in addressing some of the longstanding issues in vortex physics. The core component of the proposed program is to use small angle neutron scattering and Bitter decoration experiments to provide the most stringent test of the Bragg glass theory by measuring the structure factor in both the real and reciprocal spaces. The proposed experiments include a neutron reflectometry experiment to measure the precise Q-dependence of the structure factor of the vortex lattice in the Bragg glass state. A second set of SANS experiments will be on a shear-strained Nb single crystal for testing a recently proposed theory of the stability of Bragg glass. The objective is to artificially create a set of parallel grain boundaries into a Nb single crystal and use SANS to measure the vortex matter diffraction pattern as a function of the changing angle between the applied magnetic field to the grain boundaries. The intrinsic merits of the proposed work are a new fundamental understanding of type-II superconductors on which superconducting technology is based, and a firm understanding of phases and phase transitions in condensed matter systems with random pinning. The broader impact of the program includes the training of future generation of neutron scientists, and further development of neutron scattering and complementary techniques for studies of superconducting materials. The graduate and undergraduate students participating in this project will learn the state-of-the-art neutron scattering techniques, acquire a wide range of materials research experiences, and participate in the frontier research of superconductivity. This should best prepare the students for future careers in academia, industry, or government.« less

Technical Report: Understanding Functional Lyotropic Liquid Crystal Network Phase Self-Assembly and the Properties of Nanoconfined Water

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

Mahanthappa, Mahesh K; Yethiraj, Arun

Through the synergistic interplay of molecular dynamics (MD) simulations, chemical synthesis, and materials characterization by X-ray and neutron scattering techniques, this project investigated the phase behaviors of new classes of aqueous lyotropic liquid crystals (LLCs) and the properties of water nanoconfined within their pores. A portion of our studies focused on the synthesis of new classes of alkylsulfonic acid and alkylphosphonate amphiphiles, which were shown to undergo water-induced self-assembly to form a wide variety of nanostructured morphologies with unusually high degrees of long-range translational order observed by small- angle X-ray scattering (SAXS). Sample LLC morphologies that were observed include themore » lamellar (L!), tricontinuous double gyroid (G), hexagonally-packed cylinders (H), and low symmetry discontinuous micellar (I) Frank-Kasper phases. Since the G and H phases are the most promising for the development of selective ion transporting membranes for energy applications, we sought the characterize the structure and dynamics of water confined within the sub-3 nm pores of these LLCs using wide-angle neutron diffraction (WAND) and quasielastic neutron scattering (QENS) experiments performed at the Spallation Neutron Source at Oak Ridge National Laboratory. Using molecular dynamics (MD) simulations, we validated models for analyzing this QENS data to obtain water self-diffusion coefficients in LLC G and H phases of carboxylate and sulfonate surfactant LLCs as a function of the identities of their charge compensating counterions.« less

Structure evolution and thermoelectric properties of carbonized polydopamine thin films

DOE PAGES

Li, Haoqi; Aulin, Yaroslav V.; Frazer, Laszlo; ...

2017-02-13

Carbonization of nature-inspired polydopamine can yield thin films with high electrical conductivity. Understanding of the structure of carbonized PDA (cPDA) is therefore highly desired. In this study, neutron diffraction, Raman spectroscopy, and other techniques indicate that cPDA samples are mainly amorphous with some short-range ordering and graphite-like structure that emerges with increasing heat treatment temperature. The electrical conductivity and the Seebeck coefficient show different trends with heat treatment temperature, while the thermal conductivity remains insensitive. Finally, the largest room-temperature ZT of 2 × 10 –4 was obtained on samples heat-treated at 800 °C, which is higher than that of reducedmore » graphene oxide.« less

Floating zone growth of α-Na 0.90MnO 2 single crystals

DOE PAGES

Dally, Rebecca; Clement, Raphaele J.; Chisnell, Robin; ...

2016-12-03

Here, single crystal growth of α-Na xMnO 2 (x=0.90) is reported via the floating zone technique. The conditions required for stable growth and intergrowth-free crystals are described along with the results of trials under alternate growth atmospheres. Chemical and structural characterizations of the resulting α-Na 0.90MnO 2 crystals are performed using ICP-AES NMR, XANES, XPS, and neutron diffraction measurements. As a layered transition metal oxide with large ionic mobility and strong correlation effects, α-Na xMnO 2 is of interest to many communities, and the implications of large volume, high purity, single crystal growth are discussed.

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

Kalsi, Deepti; Rayaprol, S.; Siruguri, V.

We report the crystallographic properties of RE{sub 2}NiGe{sub 3} (RE=La, Ce) synthesized by arc melting. Rietveld refinement on the powder neutron diffraction (ND) data suggest both compounds are isostructural and crystallize in the non-centrosymmetric Er{sub 2}RhSi{sub 3} type structure having hexagonal space group P6{sup ¯}2c. In the crystal structure of RE{sub 2}NiGe{sub 3}, two dimensional arrangements of nickel and germanium atoms lead to the formation of hexagonal layers with rare earth atoms sandwiched between them. Magnetic susceptibility measurements performed in low fields exhibit antiferromagnetic ordering in cerium compound around (T{sub o}=) 3.2 K. Neutron diffraction measurements at 2.8 K (i.e.,more » at T« less

Neutron scattering investigation of a macroscopic single crystal of a lyotropic Lα phase

NASA Astrophysics Data System (ADS)

Goecking, K. D.; Monkenbusch, M.

1998-07-01

Water-rich lamellar samples of the quaternary microemulsion SDS-pentanol-water-dodecane have been prepared in form of 1 mm×10 mm×20 mm macroscopic mono domains. The shape is given by the quartz cuvette containing the sample, the layer planes are parallel to the cuvette walls. Diffraction patterns and "rocking curves" have been obtained by neutron diffraction using a triple-axis spectrometer. Three "pseudo-Bragg peaks" have been observed, their (relative) intensities yield a new experimental access to estimate the product of the elastic constants η-2 propto Bκ resulting in a lower value than obtained from synchrotron investigation using peak shape fitting (Roux D. et al., Micelles, Membranes, Microemulsions and Monolayers (Springer, New York, Berlin) 1994).

Preliminary neutron diffraction analysis of challenging human manganese superoxide dismutase crystals

DOE PAGES

Azadmanesh, Jahaun; Trickel, Scott R.; Weiss, Kevin L.; ...

2017-03-29

Superoxide dismutases (SODs) are enzymes that protect against oxidative stress by dismutation of superoxide into oxygen and hydrogen peroxide through cyclic reduction and oxidation of the active-site metal. The complete enzymatic mechanisms of SODs are unknown since data on the positions of hydrogen are limited. Here, we present, methods for large crystal growth and neutron data collection of human manganese SOD (MnSOD) using perdeuteration and the MaNDi beamline at Oak Ridge National Laboratory. Furthermore, The crystal from which the human MnSOD data set was obtained is the crystal with the largest unit-cell edge (240 Å) from which data have beenmore » collectedvianeutron diffraction to sufficient resolution (2.30 Å) where hydrogen positions can be observed.« less

Preliminary neutron diffraction analysis of challenging human manganese superoxide dismutase crystals

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

Azadmanesh, Jahaun; Trickel, Scott R.; Weiss, Kevin L.

Superoxide dismutases (SODs) are enzymes that protect against oxidative stress by dismutation of superoxide into oxygen and hydrogen peroxide through cyclic reduction and oxidation of the active-site metal. The complete enzymatic mechanisms of SODs are unknown since data on the positions of hydrogen are limited. Here, we present, methods for large crystal growth and neutron data collection of human manganese SOD (MnSOD) using perdeuteration and the MaNDi beamline at Oak Ridge National Laboratory. Furthermore, The crystal from which the human MnSOD data set was obtained is the crystal with the largest unit-cell edge (240 Å) from which data have beenmore » collectedvianeutron diffraction to sufficient resolution (2.30 Å) where hydrogen positions can be observed.« less

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.

Neutron diffraction study of a non-strichiometric Ni-Mn-Ga MSM alloy

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

Ari-Gur, Pnina; Garlea, Vasile O

2013-01-01

The structure and chemical order of a Heusler alloy of non-stoichiometric composition Ni-Mn-Ga were studied using constant-wavelength (1.538 ) neutron diffraction at 363K and the diffraction pattern was refined using the FullProf software. At this temperature the structure is austenite (cubic) with Fm-3m space group and lattice constant of a = 5.83913(4) [ ]. The chemical order is of critical importance in these alloys, as Mn becomes antiferromagnetic when the atoms are closer than the radius of the 3d shell. In the studied alloy the refinement of the site occupancy showed that the 4b (Ga site) contained as much asmore » 22% Mn; that significantly alters the distances between the Mn atoms in the crystal and, as a result, also the exchange energy between some of the Mn atoms. Based on the refinement, the composition was determined to be Ni1.91Mn1.29Ga0.8« less

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

Ari-Gur, Pnina; Garlea, Vasile O.; Cao, Huibo

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 Ni 1.91Mn 1.29Ga 0.8 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 spacemore » group P 1 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

Measurement of D-7Li Neutron Production in Neutron Generators Using the Threshold Activation Foil Technique

NASA Astrophysics Data System (ADS)

Coventry, M. D.; Krites, A. M.

Measurements to determine the absolute D-D and D-7Li neutron production rates with a neutron generator running at 100-200 kV acceleration potential were performed using the threshold activation foil technique. This technique provides a clear measure of fast neutron flux and with a suitable model, the neutron output. This approach requires little specialized equipment and is used to calibrate real-time neutron detectors and to verify neutron output. We discuss the activation foil measurement technique and describe its use in determining the relative contributions of D-D and D-7Li reactions to the total neutron yield and real-time detector response and compare to model predictions. The D-7Li reaction produces neutrons with a continuum of energies and a sharp peak around 13.5 MeV for measurement techniques outside of what D-D generators can perform. The ability to perform measurements with D-D neutrons alone, then add D-7Li neutrons for inelastic gamma production presents additional measurement modalities with the same neutron source without the use of tritium. Typically, D-T generators are employed for inelastic scattering applications but have a high regulatory burden from a radiological aspect (tritium inventory, liability concerns) and are export-controlled. D-D and D-7Li generators avoid these issues completely.

Design and Characterisation of Metallic Glassy Alloys of High Neutron Shielding Capability

NASA Astrophysics Data System (ADS)

Khong, J. C.; Daisenberger, D.; Burca, G.; Kockelmann, W.; Tremsin, A. S.; Mi, J.

2016-11-01

This paper reports the design, making and characterisation of a series of Fe-based bulk metallic glass alloys with the aim of achieving the combined properties of high neutron absorption capability and sufficient glass forming ability. Synchrotron X-ray diffraction and pair distribution function methods were used to characterise the crystalline or amorphous states of the samples. Neutron transmission and macroscopic attenuation coefficients of the designed alloys were measured using energy resolved neutron imaging method and the very recently developed microchannel plate detector. The study found that the newly designed alloy (Fe48Cr15Mo14C15B6Gd2 with a glass forming ability of Ø5.8 mm) has the highest neutron absorption capability among all Fe-based bulk metallic glasses so far reported. It is a promising material for neutron shielding applications.

Design and Characterisation of Metallic Glassy Alloys of High Neutron Shielding Capability.

PubMed

Khong, J C; Daisenberger, D; Burca, G; Kockelmann, W; Tremsin, A S; Mi, J

2016-11-16

This paper reports the design, making and characterisation of a series of Fe-based bulk metallic glass alloys with the aim of achieving the combined properties of high neutron absorption capability and sufficient glass forming ability. Synchrotron X-ray diffraction and pair distribution function methods were used to characterise the crystalline or amorphous states of the samples. Neutron transmission and macroscopic attenuation coefficients of the designed alloys were measured using energy resolved neutron imaging method and the very recently developed microchannel plate detector. The study found that the newly designed alloy (Fe 48 Cr 15 Mo 14 C 15 B 6 Gd 2 with a glass forming ability of Ø5.8 mm) has the highest neutron absorption capability among all Fe-based bulk metallic glasses so far reported. It is a promising material for neutron shielding applications.

Suppression of magnetic order in CaCo 1.86 As 2 with Fe substitution: Magnetization, neutron diffraction, and x-ray diffraction studies of Ca ( Co 1 – x Fe x ) y As 2

DOE PAGES

Jayasekara, W. T.; Pandey, Abhishek; Kreyssig, A.; ...

2017-02-23

Magnetization, neutron diffraction, and high-energy x-ray diffraction results for Sn-flux grown single-crystal samples of Ca(Co 1–xFe x) yAs 2, 0 ≤ x ≤ 1, 1.86 ≤ y ≤ 2, are presented and reveal that A-type antiferromagnetic order, with ordered moments lying along the c axis, persists for x ≲ 0.12(1). The antiferromagnetic order is smoothly suppressed with increasing x, with both the ordered moment and Néel temperature linearly decreasing. Stripe-type antiferromagnetic order does not occur for x ≤ 0.25, nor does ferromagnetic order for x up to at least x = 0.104, and a smooth crossover from the collapsed-tetragonal (cT)more » phase of CaCo 1.86As 2 to the tetragonal (T) phase of CaFe 2As 2 occurs. Furthermore, these results suggest that hole doping CaCo 1.86As 2 has a less dramatic effect on the magnetism and structure than steric effects due to substituting Sr for Ca.« less

Suppression of magnetic order in CaCo 1.86 As 2 with Fe substitution: Magnetization, neutron diffraction, and x-ray diffraction studies of Ca ( Co 1 – x Fe x ) y As 2

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

Jayasekara, W. T.; Pandey, Abhishek; Kreyssig, A.

Magnetization, neutron diffraction, and high-energy x-ray diffraction results for Sn-flux grown single-crystal samples of Ca(Co 1–xFe x) yAs 2, 0 ≤ x ≤ 1, 1.86 ≤ y ≤ 2, are presented and reveal that A-type antiferromagnetic order, with ordered moments lying along the c axis, persists for x ≲ 0.12(1). The antiferromagnetic order is smoothly suppressed with increasing x, with both the ordered moment and Néel temperature linearly decreasing. Stripe-type antiferromagnetic order does not occur for x ≤ 0.25, nor does ferromagnetic order for x up to at least x = 0.104, and a smooth crossover from the collapsed-tetragonal (cT)more » phase of CaCo 1.86As 2 to the tetragonal (T) phase of CaFe 2As 2 occurs. Furthermore, these results suggest that hole doping CaCo 1.86As 2 has a less dramatic effect on the magnetism and structure than steric effects due to substituting Sr for Ca.« less

Boroxol rings from diffraction data on vitreous boron trioxide.

PubMed

Soper, Alan K

2011-09-14

There has been a considerable debate about the nature of the short range atomic order in vitreous B(2)O(3). Some authorities state that it is not possible to build a model of glassy boron oxide of the correct density containing a large number of six-membered rings which also fits experimental diffraction data, but recent computer simulations appear to overrule that view. To discover which view is correct I use empirical potential structure refinement (EPSR) on existing neutron and x-ray diffraction data to build two models of vitreous B(2)O(3). One of these consists only of single boron and oxygen atoms arranged in a network to reproduce the diffraction data as closely as possible. This model has less than 10% of boron atoms in boroxol rings. The second model is made up of an equimolar mixture of B(3)O(3) hexagonal ring 'molecules' and BO(3) triangular molecules, with no free boron or oxygen atoms. This second model therefore has 75% of the boron atoms in boroxol rings. It is found that both models give closely similar diffraction patterns, suggesting that the diffraction data in this case are not sensitive to the number of boroxol rings present in the structure. This reinforces recent Raman, ab initio, and NMR claims that the percentage of boroxol rings in this material may be as high as 75%. The findings of this study probably explain why some interpretations based on different simulation techniques only find a small fraction of boroxol rings. The results also highlight the power of EPSR for the extraction of accurate atomistic representations of amorphous structures, provided adequate additional, non-scattering data (such as Raman and NMR in this case) are available.

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

Trahan, Alexis Chanel

The objectives of this presentation are to introduce the basic physics of neutron production, interactions and detection; identify the processes that generate neutrons; explain the most common neutron mechanism, spontaneous and induced fission and (a,n) reactions; describe the properties of neutron from different sources; recognize advantages of neutron measurements techniques; recognize common neutrons interactions; explain neutron cross section measurements; describe the fundamental of 3He detector function and designs; and differentiate between passive and active assay techniques.

Neutron diffraction study of the inverse spinels Co2TiO4 and Co2SnO4

NASA Astrophysics Data System (ADS)

Thota, S.; Reehuis, M.; Maljuk, A.; Hoser, A.; Hoffmann, J.-U.; Weise, B.; Waske, A.; Krautz, M.; Joshi, D. C.; Nayak, S.; Ghosh, S.; Suresh, P.; Dasari, K.; Wurmehl, S.; Prokhnenko, O.; Büchner, B.

2017-10-01

We report a detailed single-crystal and powder neutron diffraction study of Co2TiO4 and Co2SnO4 between the temperature 1.6 and 80 K to probe the spin structure in the ground state. For both compounds the strongest magnetic intensity was observed for the (111)M reflection due to ferrimagnetic ordering, which sets in below TN=48.6 and 41 K for Co2TiO4 and Co2SnO4 , respectively. An additional low intensity magnetic reflection (200)M was noticed in Co2TiO4 due to the presence of an additional weak antiferromagnetic component. Interestingly, from both the powder and single-crystal neutron data of Co2TiO4 , we noticed a significant broadening of the magnetic (111)M reflection, which possibly results from the disordered character of the Ti and Co atoms on the B site. Practically, the same peak broadening was found for the neutron powder data of Co2SnO4 . On the other hand, from our single-crystal neutron diffraction data of Co2TiO4 , we found a spontaneous increase of particular nuclear Bragg reflections below the magnetic ordering temperature. Our data analysis showed that this unusual effect can be ascribed to the presence of anisotropic extinction, which is associated to a change of the mosaicity of the crystal. In this case, it can be expected that competing Jahn-Teller effects acting along different crystallographic axes can induce anisotropic local strain. In fact, for both ions Ti3 + and Co3 +, the 2 tg levels split into a lower dx y level yielding a higher twofold degenerate dx z/dy z level. As a consequence, one can expect a tetragonal distortion in Co2TiO4 with c /a <1 , which we could not significantly detect in the present work.

TRACE ELEMENT DISTRIBUTION IN SEDIMENTS OF THE MID-ATLANTIC RIDGE.

DTIC Science & Technology

MARINE GEOLOGY, ATLANTIC OCEAN), (*OCEAN BOTTOM, MINERALS), SEDIMENTATION, IRON, COBALT, MANGANESE, STRONTIUM, CHLORITES, NEUTRON ACTIVATION, GEOCHEMISTRY, CALCITE , CARBONATES, X RAY DIFFRACTION, CLAY MINERALS, THESES

Using Neutron Diffraction to Determine the Low-Temperature Behavior of Pb2+ in Lead Feldspar

NASA Astrophysics Data System (ADS)

Kolbus, L. M.; Anovitz, L. M.; Chakoumackos, B. C.; Wesolowski, D. J.

2014-12-01

Feldspar minerals comprise 60% of the Earth's crust, so it imperative that the properties of feldspar be well understood for seismic modeling. The structure of feldspar consists of a three-dimensional framework of strongly-bonded TO4 tetrahedra formed by the sharing of oxygen atoms between tetrahedra. The main solid solution series found in natural feldspars are alkali NaAlSi3O8 -KAlSi3O8 and plagioclase CaAl2Si2O8-NaAlSi3O8. Recently, efforts have been made to systematically quantify feldspars structural change at non-ambient temperatures by considering only the relative tilts of the tetrahedral framework [1]. This serves as a tool to predict various behaviors of the structure such as the relative anisotropy of unit cell parameters and volume evolution with composition and temperature. Monoclinic feldspars are well predicted by the model [1], but discrepancies still remain between the model predictions and real structures with respect to absolute values of the unit cell parameters. To improve the existing model, a modification must be made to account for the M-cation interaction with its surrounding oxygen atoms. We have, therefore, chosen to study the structure of Pb-feldspar (PbAl2Si2O8), which provides the opportunity to characterize a monoclinic Al2Si2 feldspar containing a large M-site divalent cation using neutron diffraction. Neutron diffraction allows for the characterization of the M-site cation interaction between the oxygen atoms in the polyhedral cage by providing information to accurately determine the atomic displacement parameters.. Lead feldspar was synthesized for this study using the method described in [2], and confirmed to have a monoclinic C2/m space group. In this talk we will present structural determinations and atomic displacement parameters of Pb-feldspar from 10 - 300K generated from Neutron diffraction at the POWGEN beamline at the Spallation Neutron Source at Oak Ridge National lab, and compare our results to those predicted by the tetrahedral tilting model. [1] Angel, R.J. Ross, N.L, Zhao, J, Sochalski-Kolbus, L., Kruger, H., Schmidt, B.C. (2013) European Journal of Mineralogy, 25: 597-614. [2] Benna, P., Tribaudino, M., Bruno, E. (1996) American Mineralogist, 81: 1337-1343.

Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

NASA Astrophysics Data System (ADS)

Lunt, A. J. G.; Xie, M. Y.; Baimpas, N.; Zhang, S. Y.; Kabra, S.; Kelleher, J.; Neo, T. K.; Korsunsky, A. M.

2014-08-01

Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

Direct comparison of elastic incoherent neutron scattering experiments with molecular dynamics simulations of DMPC phase transitions.

PubMed

Aoun, Bachir; Pellegrini, Eric; Trapp, Marcus; Natali, Francesca; Cantù, Laura; Brocca, Paola; Gerelli, Yuri; Demé, Bruno; Marek Koza, Michael; Johnson, Mark; Peters, Judith

2016-04-01

Neutron scattering techniques have been employed to investigate 1,2-dimyristoyl-sn -glycero-3-phosphocholine (DMPC) membranes in the form of multilamellar vesicles (MLVs) and deposited, stacked multilamellar-bilayers (MLBs), covering transitions from the gel to the liquid phase. Neutron diffraction was used to characterise the samples in terms of transition temperatures, whereas elastic incoherent neutron scattering (EINS) demonstrates that the dynamics on the sub-macromolecular length-scale and pico- to nano-second time-scale are correlated with the structural transitions through a discontinuity in the observed elastic intensities and the derived mean square displacements. Molecular dynamics simulations have been performed in parallel focussing on the length-, time- and temperature-scales of the neutron experiments. They correctly reproduce the structural features of the main gel-liquid phase transition. Particular emphasis is placed on the dynamical amplitudes derived from experiment and simulations. Two methods are used to analyse the experimental data and mean square displacements. They agree within a factor of 2 irrespective of the probed time-scale, i.e. the instrument utilized. Mean square displacements computed from simulations show a comparable level of agreement with the experimental values, albeit, the best match with the two methods varies for the two instruments. Consequently, experiments and simulations together give a consistent picture of the structural and dynamical aspects of the main lipid transition and provide a basis for future, theoretical modelling of dynamics and phase behaviour in membranes. The need for more detailed analytical models is pointed out by the remaining variation of the dynamical amplitudes derived in two different ways from experiments on the one hand and simulations on the other.

High-pressure/low-temperature neutron scattering of gas inclusion compounds: Progress and prospects

PubMed Central

Zhao, Yusheng; Xu, Hongwu; Daemen, Luke L.; Lokshin, Konstantin; Tait, Kimberly T.; Mao, Wendy L.; Luo, Junhua; Currier, Robert P.; Hickmott, Donald D.

2007-01-01

Alternative energy resources such as hydrogen and methane gases are becoming increasingly important for the future economy. A major challenge for using hydrogen is to develop suitable materials to store it under a variety of conditions, which requires systematic studies of the structures, stability, and kinetics of various hydrogen-storing compounds. Neutron scattering is particularly useful for these studies. We have developed high-pressure/low-temperature gas/fluid cells in conjunction with neutron diffraction and inelastic neutron scattering instruments allowing in situ and real-time examination of gas uptake/release processes. We studied the formation of methane and hydrogen clathrates, a group of inclusion compounds consisting of frameworks of hydrogen-bonded H2O molecules with gas molecules trapped inside the cages. Our results reveal that clathrate can store up to four hydrogen molecules in each of its large cages with an intermolecular H2–H2 distance of only 2.93 Å. This distance is much shorter than that in the solid/metallic hydrogen (3.78 Å), suggesting a strong densification effect of the clathrate framework on the enclosed hydrogen molecules. The framework-pressurizing effect is striking and may exist in other inclusion compounds such as metal-organic frameworks (MOFs). Owing to the enormous variety and flexibility of their frameworks, inclusion compounds may offer superior properties for storage of hydrogen and/or hydrogen-rich molecules, relative to other types of compounds. We have investigated the hydrogen storage properties of two MOFs, Cu3[Co(CN)6]2 and Cu3(BTC)2 (BTC = benzenetricarboxylate), and our preliminary results demonstrate that the developed neutron-scattering techniques are equally well suited for studying MOFs and other inclusion compounds. PMID:17389387

The construction of a high resolution crystal backscattering spectrometer HERMES I

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

Larese, J.Z.

There is a need in the United States for a state-of-the-art, cold-neutron, crystal backscattering spectrometer (CBS) designed to investigate the structure and dynamics of condensed matter systems by the simultaneous utilization of long wavelength elastic diffraction and high-energy-resolution inelastic scattering. Cold neutron spectroscopy with CBS-type instruments has already made many important contributions to the study of atomic and molecular diffusion in biomaterials, polymers, semiconductors, liquid crystals, superionic conductors and the like. Such instruments have also been invaluable for ultra high resolution investigations of the low-lying quantum tunneling processes that provide direct insight into the dynamical response of solids at themore » lowest energies. Until relatively recently, however, all such instruments were located at steady-state reactors. This proposal describes HERMES I (High Energy Resolution Machines I) a CBS intended for installation at the LANSCE pulsed neutron facility of Los Alamos National Laboratory. As explained in detail in the main text, the authors propose to construct an updated, high-performance CBS which incorporates neutron techniques developed during the decade since IRIS was built, i.e., improved supermirror technology, a larger area crystal analyzer and high efficiency wire gas detectors. The instrument is designed in such a way as to be readily adaptable to future upgrades. HERMES I, they believe, will substantially expand the range and flexibility of neutron investigations in the United States and open new and potentially fruitful directions for condensed matter exploration. This document describes a implementation plan with a direct cost range between $4.5 to 5.6 M and scheduled duration of 39--45 months for identified alternatives.« less

Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite

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

Hua, Zilong; Guillen, Donna Post; Harris, William

2016-09-01

A thermal neutron absorbing material, comprised of 28.4 vol% HfAl3 in an Al matrix, was developed to serve as a conductively cooled thermal neutron filter to enable fast flux materials and fuels testing in a pressurized water reactor. In order to observe the microstructural change of the HfAl3-Al composite due to neutron irradiation, an EBSD-FIB characterization approach is developed and presented in this paper. Using the focused ion beam (FIB), the sample was fabricated to 25µm × 25µm × 20 µm and mounted on the grid. A series of operations were carried out repetitively on the sample top surface tomore » prepare it for scanning electron microscopy (SEM). First, a ~100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. Last, the surface was scanned by Electron Backscattering Diffraction (EBSD) to obtain the two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three-dimensional models were obtained from samples of the original and post-irradiation HfAl3-Al composite respectively, from which the most significant microstructural change caused by neutron irradiation apparently is the size reduction of both HfAl3 and Al grains. The possible reason is the thermal expansion and related thermal strain from the thermal neutron absorption. This technique can be applied to three-dimensional microstructure characterization of irradiated materials.« less

Aerodynamic laser-heated contactless furnace for neutron scattering experiments at elevated temperatures

NASA Astrophysics Data System (ADS)

Landron, Claude; Hennet, Louis; Coutures, Jean-Pierre; Jenkins, Tudor; Alétru, Chantal; Greaves, Neville; Soper, Alan; Derbyshire, Gareth

2000-04-01

Conventional radiative furnaces require sample containment that encourages contamination at elevated temperatures and generally need windows which restrict the entrance and exit solid angles required for diffraction and scattering measurements. We describe a contactless windowless furnace based on aerodynamic levitation and laser heating which has been designed for high temperature neutron scattering experiments. Data from initial experiments are reported for crystalline and amorphous oxides at temperatures up to 1900 °C, using the spallation neutron source ISIS together with our laser-heated aerodynamic levitator. Accurate reproduction of thermal expansion coefficients and radial distribution functions have been obtained, demonstrating the utility of aerodynamic levitation methods for neutron scattering methods.

On the crystal structure of Cr2N precipitates in high-nitrogen austenitic stainless steel. III. Neutron diffraction study on the ordered Cr2N superstructure.

PubMed

Lee, Tae-Ho; Kim, Sung-Joon; Shin, Eunjoo; Takaki, Setsuo

2006-12-01

The ordered structure of Cr(2)N precipitates in high-nitrogen austenitic steel was investigated utilizing high-resolution neutron powder diffractometry (HRPD). On the basis of the Rietveld refinement of neutron diffraction patterns, the ordered Cr2N superstructure was confirmed to be trigonal (space group P31m), with lattice parameters a=4.800 (4) and c=4.472 (5) A, as suggested in previous transmission electron microscopy studies [Lee, Oh, Han, Lee, Kim & Takaki (2005). Acta Cryst. B61, 137-144; Lee, Kim & Takaki (2006). Acta Cryst. B62, 190-196]. The occupancies of the N atoms in four crystallographic sites [1(a), 1(b), 2(d) and 2(c) Wyckoff sites] were determined to be 1.00 (5), 0.0, 0.74 (9) and 0.12 (3), respectively, reflecting a partial disordering of N atoms along the c axis. The position of the metal atom was specified to be x=0.346 (8) and z=0.244 (6), corresponding to a deviation from the ideal position (x=0.333 and z=0.250). This deviation caused the ((1/3 1/3)(0))-type superlattice reflection to appear. A comparison between the ideal and measured crystal structures of Cr2N was performed using a computer simulation of selected-area diffraction patterns.

Phase diagram of multiferroic KCu3As2O7(OD ) 3

NASA Astrophysics Data System (ADS)

Nilsen, Gøran J.; Simonet, Virginie; Colin, Claire V.; Okuma, Ryutaro; Okamoto, Yoshihiko; Tokunaga, Masashi; Hansen, Thomas C.; Khalyavin, Dmitry D.; Hiroi, Zenji

2017-06-01

The layered compound KCu3As2O7(OD ) 3 , comprising distorted kagome planes of S =1 /2 Cu2 + ions, is a recent addition to the family of type-II multiferroics. Previous zero-field neutron diffraction work has found two helically ordered regimes in KCu3As2O7(OD ) 3 , each showing a distinct coupling between the magnetic and ferroelectric order parameters. Here, we extend this work to magnetic fields up to 20 T using neutron powder diffraction, capacitance, polarization, and high-field magnetization measurements, hence determining the H -T phase diagram. We find metamagnetic transitions in both low-temperature phases around μ0Hc˜3.7 T, which neutron powder diffraction reveals to correspond to rotations of the helix plane away from the easy plane, as well as a small change in the propagation vector. Furthermore, we show that the sign of the ferroelectric polarization is reversible in a magnetic field, although no change is observed (or expected on the basis of the magnetic structure) due to the transition at 3.7 T. We finally justify the temperature dependence of the polarization in both zero-field ordered phases by a symmetry analysis of the free energy expansion, and attempt to account for the metamagnetic transition by adding anisotropic exchange interactions to our existing model for KCu3As2O7(OD ) 3 .

Neutron diffraction study and theoretical analysis of the antiferromagnetic order and the diffuse scattering in the layered kagome system CaBaCo2Fe2O7

NASA Astrophysics Data System (ADS)

Reim, J. D.; Rosén, E.; Zaharko, O.; Mostovoy, M.; Robert, J.; Valldor, M.; Schweika, W.

2018-04-01

The hexagonal swedenborgite, CaBaCo2Fe2O7 , is a chiral frustrated antiferromagnet, in which magnetic ions form alternating kagome and triangular layers. We observe a long-range √{3 }×√{3 } antiferromagnetic order setting in below TN=160 K by neutron diffraction on single crystals of CaBaCo2Fe2O7 . Both magnetization and polarized neutron single crystal diffraction measurements show that close to TN spins lie predominantly in the a b plane, while upon cooling the spin structure becomes increasingly canted due to Dzyaloshinskii-Moriya interactions. The ordered structure can be described and refined within the magnetic space group P 31 m' . Diffuse scattering between the magnetic peaks reveals that the spin order is partial. Monte Carlo simulations based on a Heisenberg model with two nearest-neighbor exchange interactions show a similar diffuse scattering and coexistence of the √{3 }×√{3 } order with disorder. The coexistence can be explained by the freedom to vary spins without affecting the long-range order, which gives rise to ground-state degeneracy. Polarization analysis of the magnetic peaks indicates the presence of long-period cycloidal spin correlations resulting from the broken inversion symmetry of the lattice, in agreement with our symmetry analysis.

Mott localization in a pure stripe antiferromagnet Rb 1 - δ Fe 1.5 - σ S 2

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

Wang, Meng; Yi, Ming; Cao, Huibo

A combination of neutron diffraction and angle-resolved photoemission spectroscopy measurements on a pure antiferromagnetic stripe Rb 1-δFe 1.5-σS 2 is reported. A neutron diffraction experiment on a powder sample shows that a 98% volume fraction of the sample is in the antiferromagnetic stripe phase with rhombic iron vacancy order and a refined composition of Rb 0.66Fe 1.36S 2, and that only 2% of the sample is in the block antiferromagnetic phase with √5×√5 iron vacancy order. Furthermore, a neutron diffraction experiment on a single crystal shows that there is only a single phase with the stripe antiferromagnetic order with themore » refined composition of Rb 0.78Fe 1.35S 2, while the phase with block antiferromagnetic order is absent. Angle-resolved photoemission spectroscopy measurements on the same crystal with the pure stripe phase reveal that the electronic structure is gapped at the Fermi level with a gap larger than 0.325 eV. The data collectively demonstrate that the extra 10% iron vacancies in addition to the rhombic iron vacancy order effectively impede the formation of the block antiferromagnetic phase; the data also suggest that the stripe antiferromagnetic phase with rhombic iron vacancy order is a Mott insulator.« less

A neutron diffraction study of the magnetic phases of CsCuCl3 for in-plane fields up to 17 T

NASA Astrophysics Data System (ADS)

Stüßer, N.; Schotte, U.; Hoser, A.; Meschke, M.; Meißner, M.; Wosnitza, J.

2002-05-01

Neutron diffraction investigations have been performed to study the magnetization process of CsCuCl3 with the magnetic field aligned within the ab-plane. In zero field the stacked, triangular-lattice antiferromagnet (TLA) CsCuCl3 has a helical structure incommensurate in the chain direction normal to the ab-plane. The magnetic phase diagram was investigated from 2 K up to TN in fields up to 17 T. The phase line for the expected incommensurate-commensurate (IC-C) phase transition could be determined throughout the whole phase diagram. At low temperature the IC-C transition is roughly at half the saturation field HS. The neutron diffraction patterns were found to be well described by a sinusoidally modulated spiral in fields up to HS/3. The initial increase of the scattering intensity in rising field indicates a continuous reduction of the spin frustration on the triangular lattice. Between HS/3 and HS/2 a new phase occurs where the spiral vector has a plateau in its field dependence. Close to the IC-C transition a growing asymmetry of magnetic satellite-peak intensities indicates domain effects which are related to the lifting of the chiral degeneracy in the ab-plane in rising field. The phase diagram obtained has some similarities with those calculated for stacked TLAs by considering the effects of quantum and thermal fluctuations.

Phase Equilibria and Crystallography of Ceramic Oxides

PubMed Central

Wong-Ng, W.; Roth, R. S.; Vanderah, T. A.; McMurdie, H. F.

2001-01-01

Research in phase equilibria and crystallography has been a tradition in the Ceramics Division at National Bureau of Standards/National Institute of Standatrds and Technology (NBS/NIST) since the early thirties. In the early years, effort was concentrated in areas of Portland cement, ceramic glazes and glasses, instrument bearings, and battery materials. In the past 40 years, a large portion of the work was related to electronic materials, including ferroelectrics, piezoelectrics, ionic conductors, dielectrics, microwave dielectrics, and high-temperature superconductors. As a result of the phase equilibria studies, many new compounds have been discovered. Some of these discoveries have had a significant impact on US industry. Structure determinations of these new phases have often been carried out as a joint effort among NBS/NIST colleagues and also with outside collaborators using both single crystal and neutron and x-ray powder diffraction techniques. All phase equilibria diagrams were included in Phase Diagrams for Ceramists, which are collaborative publications between The American Ceramic Society (ACerS) and NBS/NIST. All x-ray powder diffraction patterns have been included in the Powder Diffraction File (PDF). This article gives a brief account of the history of the development of the phase equilibria and crystallographic research on ceramic oxides in the Ceramics Division. Represented systems, particularly electronic materials, are highlighted. PMID:27500068

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

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

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

DOE PAGES

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.; ...

2016-11-11

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

The impact of chemical doping on the magnetic state of the Sr{sub 2}YRuO{sub 6} double perovskite

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

Kayser, Paula; Ranjbar, Ben; Kennedy, Brendan J.

The impact of chemical doping of the type Sr{sub 2−x}A{sub x}YRuO{sub 6} (A=Ca, Ba) on the low temperature magnetic properties of Sr{sub 2}YRuO{sub 6}, probed using variable temperature magnetic susceptibility, neutron diffraction and heat capacity measurements, are described. Specific-heat measurements of un-doped Sr{sub 2}YRuO{sub 6} reveal two features at ∼26 and ∼30 K. Neutron scattering measurements at these temperatures are consistent with a change from a 2D ordered state to the 3D type 1 AFM state. Magnetic and structural studies of a number of doped oxides are described that highlight the unique low temperature behavior of Sr{sub 2}YRuO{sub 6} andmore » demonstrate that doping destabilizes the intermediate 2D ordered state. - Graphical abstract: Neutron diffraction measurements of the ordered double perovskite Sr{sub 2}YRuO{sub 6}reveal a with a change from a 2D ordered state to the 3D type 1 AFM state upon cooling. The impact of chemical doping Sr{sub 2−x}A{sub x}YRuO{sub 6} (A=Ca, Ba) on the low temperature magnetic properties have also been investigated and these highlight the unique low temperature behavior of Sr{sub 2}YRuO{sub 6} with doping destabilizing the intermediate 2D ordered state. - Highlights: • Crystal and Magnetic Structure of Sr{sub 2}YRuO{sub 3} was studied using Neutron Diffraction. • Effect of doping on the magnetic ground state established. • Origin of two low temperature transitions discussed.« less

Design and Characterisation of Metallic Glassy Alloys of High Neutron Shielding Capability

PubMed Central

Khong, J. C.; Daisenberger, D.; Burca, G.; Kockelmann, W.; Tremsin, A. S.; Mi, J.

2016-01-01

This paper reports the design, making and characterisation of a series of Fe-based bulk metallic glass alloys with the aim of achieving the combined properties of high neutron absorption capability and sufficient glass forming ability. Synchrotron X-ray diffraction and pair distribution function methods were used to characterise the crystalline or amorphous states of the samples. Neutron transmission and macroscopic attenuation coefficients of the designed alloys were measured using energy resolved neutron imaging method and the very recently developed microchannel plate detector. The study found that the newly designed alloy (Fe48Cr15Mo14C15B6Gd2 with a glass forming ability of Ø5.8 mm) has the highest neutron absorption capability among all Fe-based bulk metallic glasses so far reported. It is a promising material for neutron shielding applications. PMID:27848991

A technique for determining the deuterium/hydrogen contrast map in neutron macromolecular crystallography.

PubMed

Chatake, Toshiyuki; Fujiwara, Satoru

2016-01-01

A difference in the neutron scattering length between hydrogen and deuterium leads to a high density contrast in neutron Fourier maps. In this study, a technique for determining the deuterium/hydrogen (D/H) contrast map in neutron macromolecular crystallography is developed and evaluated using ribonuclease A. The contrast map between the D2O-solvent and H2O-solvent crystals is calculated in real space, rather than in reciprocal space as performed in previous neutron D/H contrast crystallography. The present technique can thus utilize all of the amplitudes of the neutron structure factors for both D2O-solvent and H2O-solvent crystals. The neutron D/H contrast maps clearly demonstrate the powerful detectability of H/D exchange in proteins. In fact, alternative protonation states and alternative conformations of hydroxyl groups are observed at medium resolution (1.8 Å). Moreover, water molecules can be categorized into three types according to their tendency towards rotational disorder. These results directly indicate improvement in the neutron crystal structure analysis. This technique is suitable for incorporation into the standard structure-determination process used in neutron protein crystallography; consequently, more precise and efficient determination of the D-atom positions is possible using a combination of this D/H contrast technique and standard neutron structure-determination protocols.

Teaming with Brookhaven National Laboratory

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

Yang, G.

BNL has started growing CdZnTeSe crystals for room-temperature radiation detector applications. The addition of Se to CdTe reduces the concentration of secondary phases and sub-grain boundary networks. The addition of Zn increases the energy band gap. Material characterization to understand the limiting factors of radiation detection material and to improve the properties continues to be a core element of an extensive R&D program at the LBNL’s ALS and BNL’s NSLS-II synchrotron facilities. ALS’s Beamline 3.3.2 is available for 60% of its beamtime and allows us to perform both White Beam X-ray Diffraction Topography and Micron Scale X-ray Detector Mapping. Themore » latter technique is extremely useful when measuring scintillators because it allows us to subtract contributions from the variability in the counting statistics, and also the fluctuations due to delta electrons, and non-proportionality. BNL has recently developed a new type of thermal neutron detector using pad technology in combination with 3He gas operated in ionization mode. The new detector is used for coded aperture thermal neutron imaging.« less

Internal Stress Distribution Measurement of TIG Welded SUS304 Samples Using Neutron Diffraction Technique

NASA Astrophysics Data System (ADS)

Muslih, M. Refai; Sumirat, I.; Sairun; Purwanta

2008-03-01

The distribution of residual stress of SUS304 samples that were undergone TIG welding process with four different electric currents has been measured. The welding has been done in the middle part of the samples that was previously grooved by milling machine. Before they were welded the samples were annealed at 650 degree Celsius for one hour. The annealing process was done to eliminate residual stress generated by grooving process so that the residual stress within the samples was merely produced from welding process. The calculation of distribution of residual stress was carried out by measuring the strains within crystal planes of Fe(220) SUS304. Strain, Young modulus, and Poisson ratio of Fe(220) SUS304 were measured using DN1-M neutron diffractometer. Young modulus and Poisson ratio of Fe(220) SUS304 sample were measured in-situ. The result of calculations showed that distribution of residual stress of SUS304 in the vicinity of welded area is influenced both by treatments given at the samples-making process and by the electric current used during welding process.

Neutron spectrum determination in a sub-critical assembly using the multi-disc neutron activation technique

NASA Astrophysics Data System (ADS)

Koseoglou, P.; Vagena, E.; Stoulos, S.; Manolopoulou, M.

2016-09-01

Neutron spectrum of the sub-critical nuclear assembly-reactor of Aristotle University of Thessaloniki was measured at three radial distances from the reactor core. The neutron activation technique was applied irradiating 15 thick foils - disc of various elements at each position. The data of 38 (n, γ), (n, p) and (n, α) reactions were analyzed for specific activity determination. Discs instead of foils were used due to the relevant low neutron flux, so the gamma self-absorption as well as the neutron self-shielding factors has been calculated using GEANT simulations in order to determine the activity induced. The specific activities calculated for all isotopes studied were the input to the SANDII code, which was built specifically for the neutron spectrum de-convolution when the neutron activation technique is used. For the optimization of the results a technique was applied in order to minimize the influence of the initial-"guessed" spectrum shape SANDII uses. The neutron spectrum estimated presents a peak in the regions of (i) thermal neutrons ranged between 0.001 and 1 eV peaking at neutron energy ∼0.1 eV and (ii) fast neutrons ranged between 0.1 and 20 MeV peaking at neutron energy ∼1.2 MeV. The reduction of thermal neutrons is higher than the fast one as the distance from the reactor core increases since thermal neutrons capture by natural U-fuel has higher cross section than the fast neutrons.

An in situ neutron diffraction study of plastic deformation in a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite

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

Wang, D. M.; Chen, Yan; Mu, Juan

Micro-mechanical behaviors of a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite in the plastic regime were investigated by continuous in situ neutron diffraction during compression. Three stages of the plastic deformation were observed according to the work-hardening rate. Here, the underlying natures of the work hardening, correlating with the lattice/microscopic strain evolution, are revealed for the three stages: (1) the initiation of shear bands, (2) the phase load transferring from the amorphous phase to the B2 phase and (3) the accelerated martensitic transformation and the work hardening of the polycrystalline phases promoted by the rapid propagation of the shearmore » bands.« less

Unravelling the low thermal expansion coefficient of cation-substituted YBaCo 4O 7+δ

DOE PAGES

Manthiram, Arumugam; Huq, Ashfia; Kan, Wang Hay; ...

2016-01-12

With an aim to understand the origin of the low thermal expansion coefficients (TECs), cation substituted YBaCo 4O 7-type oxides have been investigated by in-situ neutron diffraction, bond valence sum (BVS), thermogravimetric analysis, and dilatometry. The compositions YBaCo 4O 7+δ, Y 0.9ln 0.1BaCo 3ZnO 7+δ, and Y 0.9ln 0.1BaCo 3Zn 0.6Fe 0.4O 7+δ) were synthesized by solid-state reaction at 1200 °C. Here, Rietveld refinement of the joint synchrotron X-ray and neutron diffraction data shows that the Zn and Fe dopants have different preferences to substitute the Co ions in the 6c and 2a sites.

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.

Type I and type II residual stress in iron meteorites determined by neutron diffraction measurements

NASA Astrophysics Data System (ADS)

Caporali, Stefano; Pratesi, Giovanni; Kabra, Saurabh; Grazzi, Francesco

2018-04-01

In this work we present a preliminary investigation by means of neutron diffraction experiment to determine the residual stress state in three different iron meteorites (Chinga, Sikhote Alin and Nantan). Because of the very peculiar microstructural characteristic of this class of samples, all the systematic effects related to the measuring procedure - such as crystallite size and composition - were taken into account and a clear differentiation in the statistical distribution of residual stress in coarse and fine grained meteorites were highlighted. Moreover, the residual stress state was statistically analysed in three orthogonal directions finding evidence of the existence of both type I and type II residual stress components. Finally, the application of von Mises approach allowed to determine the distribution of type II stress.

An in situ neutron diffraction study of plastic deformation in a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite

DOE PAGES

Wang, D. M.; Chen, Yan; Mu, Juan; ...

2018-05-21

Micro-mechanical behaviors of a Cu 46.5Zr 46.5Al 7 bulk metallic glass composite in the plastic regime were investigated by continuous in situ neutron diffraction during compression. Three stages of the plastic deformation were observed according to the work-hardening rate. Here, the underlying natures of the work hardening, correlating with the lattice/microscopic strain evolution, are revealed for the three stages: (1) the initiation of shear bands, (2) the phase load transferring from the amorphous phase to the B2 phase and (3) the accelerated martensitic transformation and the work hardening of the polycrystalline phases promoted by the rapid propagation of the shearmore » bands.« less

Low Temperature Magnetic Ordering of the Magnetic Ionic Plastic Crystal, Choline[FeCl4

NASA Astrophysics Data System (ADS)

de Pedro, I.; García-Saiz, A.; Andreica, D.; Fernández Barquín, L.; Fernández-Díaz, M. T.; Blanco, J. A.; Amato, A.; Rodríguez Fernández, J.

2015-11-01

We report on the nature of the low temperature magnetic ordering of a magnetic ionic plastic crystal, Choline[FeCl4]. This investigation was carried out using heat capacity measurements, neutron diffraction experiments and muon spin relaxation (μSR) spectroscopy. The calorimetric measurements show the onset of an unusual magnetic ordering below 4 K with a possible second magnetic phase transition below 2 K. Low temperature neutron diffraction data reveal a three dimensional antiferromagnetic ordering at 2 K compatible with the previous magnetometry results. The analysis of μSR spectra indicates a magnetic phase transition below 2.2 K. At 1.6 K, the analysis of the shape of the μSR spectra suggests the existence of an additional magnetic phase with features of a possible incommensurate magnetic structure.

Revealing the membrane-bound structure of neurokinin A using neutron diffraction

NASA Astrophysics Data System (ADS)

Darkes, Malcolm J. M.; Hauss, Thomas; Dante, Silvia; Bradshaw, Jeremy P.

2000-03-01

Neurokinin A (or substance K) belongs to the tachykinin family, a group of small amphipathic peptides that bind to specific membrane-embedded, G-protein coupled receptors. The agonist/receptor complex is quaternary in nature because the receptor binding sites are thought to be located within the lipid bilayer and because the role of water cannot be ignored. The cell membrane acts as a solvent to accumulate peptide and an inducer of peptide secondary structure. The three-dimensional shape that the peptide assumes when associated to the cell membrane will be an important parameter with regards to the receptor selectivity and affinity. Neutron diffraction measurements were carried out in order to define the location of the N-terminus of the peptide in synthetic phospholipid multi-bilayer stacks.

X-ray and neutron diffraction anomalies preceding martensitic phase transformation in AuCuZn2 alloys

NASA Astrophysics Data System (ADS)

Nagasawa, A.; Makita, T.; Nakanishi, N.; Iizumi, M.; Morii, Y.

1988-04-01

The present paper gives the results obtained by the X-ray and neutron diffraction studies on the single crystals of the beta-1 AuCuZn2 alloys. As precursor phenomena, the dispersion relation of the [110] TA1 phonon exhibits significant dip near 2/3 [110] q max position and anomalous peaks appear around 1/3 and 2/3 [110] q max positions. Characteristics of the interplanar force constants, obtained by the analysis of the dispersion relation, and the positions of the anomalous peaks predict the martensite structures to be formed in the beta phase alloys. In the present case, both the 6R and 18R martensites will be formed by cooling and/or under the stress field.

Neutron powder diffraction study on the structures of LaNi 5- xAl xD y compounds

NASA Astrophysics Data System (ADS)

Du, Honglin; Zhang, Wenyong; Wang, Changsheng; Han, Jingzhi; Yang, Yingchang; Chen, Bo; Xie, Chaomei; Sun, Kai; Zhang, Baisheng

2003-10-01

The structures of LaNi 5- xAl xD y ( x=0.75, 0.25, y=1.01, 1.10, 1.91 and 3.1) were systematically investigated by neutron and X-ray diffraction. D atoms are found to enter the 6m site of the α-phase but not the reported 12n site, while the 6m and 12n sites of the β-phase. In the case of LaNi 4.75Al 0.25D y with lower Al content and symmetry, D atoms do not enter the α-phase but occupy the 4h site besides the 6m and 12n sites of the β-phase. The relationship between structures and properties is also discussed.

Structural studies of the rhombohedral and orthorhombic monouranates: CaUO{sub 4}, α-SrUO{sub 4}, β-SrUO{sub 4} and BaUO{sub 4}

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

Murphy, Gabriel; Kennedy, Brendan J., E-mail: kennedyb@chem.usyd.edu.au; Johannessen, Bernt

The structures of some AUO{sub 4} (A=Ca, Sr, or Ba) oxides have been determined using a combination of neutron and synchrotron X-ray diffraction, supported by X-ray absorption spectroscopic measurements at the U L{sub 3}-edge. The smaller Ca cation favours a rhombohedral AUO{sub 4} structure with 8-coordinate UO{sub 8} moieties whilst an orthorhombic structure based on UO{sub 6} groups is found for BaUO{sub 4}. Both the rhombohedral and orthorhombic structures can be stabilised for SrUO{sub 4}. The structural studies suggest that the bonding requirements of the A site cation play a significant role in determining which structure is favoured. In themore » rhombohedral structure, Bond Valence Sums demonstrate the A site is invariably overbonded, which, in the case of rhombohedral α-SrUO{sub 4}, is compensated for by the formation of vacancies in the oxygen sub-lattice. The uranium cation, with its flexible oxidation state, is able to accommodate this by inducing vacancies along its equatorial coordination site as demonstrated by neutron powder diffraction. - Graphical abstract: Diffraction studies of AUO{sub 4} (A = Ca, Sr, or Ba) oxides reveal the importance of the bonding requirements of the A site cation in determining whether the structure is rhombohedral or orthorhombic. - Highlights: • Structures of AUO{sub 4} ( A = Ca Sr, Ba) refined against X-ray and Neutron diffraction. • The alkali cations size has a dramatic effect on the crystal structure. • Smaller cations favouring a rhombohedral structure. • Oxygen vacancies to stabilise the rhombohedral structure in SrUO{sub 4}.« less

Evidence for existence of functional monoclinic phase in sodium niobate based solid solution by powder neutron diffraction

NASA Astrophysics Data System (ADS)

Mishra, S. K.; Jauhari, Mrinal; Mittal, R.; Krishna, P. S. R.; Reddy, V. R.; Chaplot, S. L.

2018-04-01

We have carried out systematic temperature-dependent neutron diffraction measurements in conjunction with dielectric spectroscopy from 6 to 300 K for sodium niobate based compounds (1-x) NaNbO3-xBaTiO3 (NNBTx). The dielectric constant is measured as a function of both temperature and frequency. It shows an anomaly at different temperatures in cooling and heating cycles and exhibits a large thermal hysteresis of ˜150 K for the composition x = 0.03. The dielectric constant is found to be dispersive in nature and suggests a relaxor ferroelectric behavior. In order to explore structural changes as a function of temperature, we analyzed the powder neutron diffraction data for the compositions x = 0.03 and 0.05. Drastic changes are observed in the powder profiles near 2θ ˜ 30.6°, 32.1°, and 34.6° in the diffraction pattern below 200 K during cooling and above 190 K in heating cycles, respectively. The disappearance of superlattice reflection and splitting in main perovskite peaks provide a signature for structural phase transition. We observed stabilization of a monoclinic phase (Cc) at low temperature. This monoclinic phase is believed to provide a flexible polarization rotation and considered to be directly linked to the high performance piezoelectricity in materials. The thermal hysteresis for composition x = 0.03 is larger than that for x = 0.05. This suggests that the addition of BaTiO3 to NaNbO3 suppresses the thermal hysteresis. It is also observed that the structural phase transition temperature decreases upon increasing the dopant concentration.

Spallation radiation effects in materials

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

Mansur, L.K.; Farrell, K.; Wechsler, M.S.

1996-06-01

Spallation refers to the process whereby particles (chiefly neutrons) are ejected from nuclei upon bombardment by high-energy protons. Spallation neutron sources (SNS`s) use these neutrons for neutron scattering and diffraction research, and SNS`s are proposed as the basis for systems for tritium production and transmutation of nuclear waste. Materials in SNS`s are exposed to the incident proton beam (energies typically about 1000 MeV) and to the spallation neutrons (spectrum of energies extending up to about 1000 MeV). By contrast the fission neutrons in nuclear reactors have an average energy of only about 2 MeV, and the neutrons in fusion reactorsmore » would have energies below about 14 MeV. Furthermore, the protons and neutrons in SNS`s for scattering and diffraction research are pulsed at frequencies of about 10 to 60 Hz, from which significant changes in the kinetics of point and extended defects may be expected. In addition, much higher transmutation rates occur in SNS-irradiated materials, On the whole, then, significant differences in microstructural development and macroscopic properties may result upon exposure in SNS systems, as compared with fission and fusion irradiations. In a more general sense, subjecting materials to new radiation environments has almost routinely led to new discoveries. To the extent that data are avaiable, however, the spallation environment appears to increase the degree of damage without introducing totally new effects. The first part of this presentation is an overview of radiation effects in materials, outlining essential concepts and property changes and their physical bases. This background is followed by a description of SNS irradiation environments and the effects on materials of exposure to these environments. A special discussion is given of the selection of target (e.g., liquid mercury), container (e.g., austenitic stainless steel or ferritic/martensitic steel), and structural materials in SNS systems.« less

Microstructural evolution of neutron irradiated 3C-SiC

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

Sprouster, David J.; Koyanagi, Takaaki; Dooryhee, Eric

The microstructural response of neutron irradiated 3C-SiC have been investigated over a wide irradiation temperature and fluence range via qualitative and quantitative synchrotron-based X-ray diffraction characterization. Here, we identify several neutron fluence- and irradiation temperature-dependent changes in the microstructure, and directly highlight the specific defects introduced through the course of irradiation. By quantifying the microstructure, we aim to develop a more detailed understanding of the radiation response of SiC. Such studies are important to build mechanistic models of material performance and to understand the susceptibility of various microstructures to radiation damage for advanced energy applications.

Microstructural evolution of neutron irradiated 3C-SiC

DOE PAGES

Sprouster, David J.; Koyanagi, Takaaki; Dooryhee, Eric; ...

2017-03-18

The microstructural response of neutron irradiated 3C-SiC have been investigated over a wide irradiation temperature and fluence range via qualitative and quantitative synchrotron-based X-ray diffraction characterization. Here, we identify several neutron fluence- and irradiation temperature-dependent changes in the microstructure, and directly highlight the specific defects introduced through the course of irradiation. By quantifying the microstructure, we aim to develop a more detailed understanding of the radiation response of SiC. Such studies are important to build mechanistic models of material performance and to understand the susceptibility of various microstructures to radiation damage for advanced energy applications.

Inelastic neutron scattering experiments with the monochromatic imaging mode of the RITA-II spectrometer

NASA Astrophysics Data System (ADS)

Bahl, C. R. H.; Lefmann, K.; Abrahamsen, A. B.; Rønnow, H. M.; Saxild, F.; Jensen, T. B. S.; Udby, L.; Andersen, N. H.; Christensen, N. B.; Jakobsen, H. S.; Larsen, T.; Häfliger, P. S.; Streule, S.; Niedermayer, Ch.

2006-05-01

Recently a monochromatic multiple data taking mode has been demonstrated for diffraction experiments using a RITA type cold neutron spectrometer with a multi-bladed analyser and a position-sensitive detector. Here, we show how this mode can be used in combination with a flexible radial collimator to perform real inelastic neutron scattering experiments. We present the results from inelastic powder, single crystal dispersion and single crystal constant energy mapping experiments. The advantages and complications of performing these experiments are discussed along with a comparison between the imaging mode and the traditional monochromatic focussing mode.

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

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

Ye, Feng; Chi, Songxue; Chakoumakos, Bryan C

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 Kmore » 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.« less

No evidence for orbital loop currents in charge-ordered YBa2Cu3O6 +x from polarized neutron diffraction

NASA Astrophysics Data System (ADS)

Croft, T. P.; Blackburn, E.; Kulda, J.; Liang, Ruixing; Bonn, D. A.; Hardy, W. N.; Hayden, S. M.

2017-12-01

It has been proposed that the pseudogap state of underdoped cuprate superconductors may be due to a transition to a phase which has circulating currents within each unit cell. Here, we use polarized neutron diffraction to search for the corresponding orbital moments in two samples of underdoped YBa2Cu3O6 +x with doping levels p =0.104 and 0.123. In contrast to some other reports using polarized neutrons, but in agreement with nuclear magnetic resonance and muon spin rotation measurements, we find no evidence for the appearance of magnetic order below 300 K. Thus, our experiment suggests that such order is not an intrinsic property of high-quality cuprate superconductor single crystals. Our results provide an upper bound for a possible orbital loop moment which depends on the pattern of currents within the unit cell. For example, for the CC-θI I pattern proposed by Varma, we find that the ordered moment per current loop is less than 0.013 μB for p =0.104 .