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

Twinning-mediated work hardening and texture evolution in CrCoFeMnNi high entropy alloys at cryogenic temperature

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

Liu, T. K.; Wu, Z.; Stoica, A. D.

The cryogenic plastic deformation of CrCoFeMnNi high entropy alloy is characterized by three distinct stages based on the change of the work hardening rate. Microstructure and bulk texture at different strain levels were studied by electron backscatter diffraction (EBSD) and neutron diffraction. Our findings indicate that the deformation twins led to the constant work hardening rate at Stage II and resulted in the appearance of <115 >//TA texture component, while the dislocation slip was involved all though the entire plastic deformation. As a result, the twinning-mediated tensile plastic deformation at cryogenic temperature finally induced the strong {111}- < 112 >more » texture component and minor {001} < 110 > texture component accompanied with twinning-induced {115}< 552 > texture component.« less

Twinning-mediated work hardening and texture evolution in CrCoFeMnNi high entropy alloys at cryogenic temperature

DOE PAGES

Liu, T. K.; Wu, Z.; Stoica, A. D.; ...

2017-06-17

The cryogenic plastic deformation of CrCoFeMnNi high entropy alloy is characterized by three distinct stages based on the change of the work hardening rate. Microstructure and bulk texture at different strain levels were studied by electron backscatter diffraction (EBSD) and neutron diffraction. Our findings indicate that the deformation twins led to the constant work hardening rate at Stage II and resulted in the appearance of <115 >//TA texture component, while the dislocation slip was involved all though the entire plastic deformation. As a result, the twinning-mediated tensile plastic deformation at cryogenic temperature finally induced the strong {111}- < 112 >more » texture component and minor {001} < 110 > texture component accompanied with twinning-induced {115}< 552 > texture component.« less

In-situ neutron diffraction of a quasicrystal-containing Mg alloy interpreted using a new polycrystal plasticity model of hardening due to {10.2} tensile twinning

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

Agnew, S. R.; Singh, A.; Calhoun, C. A.

Due to the excellent balance of strength and ductility exhibited by some Mg-Zn-RE (Y subgroup rare earth element) alloys, which contain icosahedral quasicrystalline precipitates, it is of interest to examine their deformation mechanisms. Furthermore, the internal strain evolution Mg-3at%Zn-0.5 at%Y with 4 vol% i-phase was measured using in-situ neutron diffraction. The extruded samples exhibit an initially weak <10.0> || extrusion direction “rod texture,” distinct from the normally strong texture of extruded Mg alloys, but the grain size is unexceptional (16.7 ± 2.1 μm). The initially weak texture contributes to a nearly symmetric yielding response between tension and compression. The hardeningmore » responses are asymmetric, however, since {10.2} extension twinning is significantly more active during compressive straining, despite the initially weak texture. In-situ neutron diffraction tension and compression experiments parallel to the extrusion direction, together with elasto-plastic self-consistent (EPSC) crystal plasticity modeling, reveal the strength and hardening behavior of individual slip and twinning modes. A model that was previously published about twinning-detwinning (TDT) is implemented within the EPSC framework, and it is proven effective for describing the observed, mild tension-compression asymmetry. This is not possible with previous EPSC-based models of twinning. Finally, the description of hardening within the TDT model is modified, in order to accurately describe the evolution of internal strains within the twins.« less

In-situ neutron diffraction of a quasicrystal-containing Mg alloy interpreted using a new polycrystal plasticity model of hardening due to {10.2} tensile twinning

DOE PAGES

Agnew, S. R.; Singh, A.; Calhoun, C. A.; ...

2018-09-17

Due to the excellent balance of strength and ductility exhibited by some Mg-Zn-RE (Y subgroup rare earth element) alloys, which contain icosahedral quasicrystalline precipitates, it is of interest to examine their deformation mechanisms. Furthermore, the internal strain evolution Mg-3at%Zn-0.5 at%Y with 4 vol% i-phase was measured using in-situ neutron diffraction. The extruded samples exhibit an initially weak <10.0> || extrusion direction “rod texture,” distinct from the normally strong texture of extruded Mg alloys, but the grain size is unexceptional (16.7 ± 2.1 μm). The initially weak texture contributes to a nearly symmetric yielding response between tension and compression. The hardeningmore » responses are asymmetric, however, since {10.2} extension twinning is significantly more active during compressive straining, despite the initially weak texture. In-situ neutron diffraction tension and compression experiments parallel to the extrusion direction, together with elasto-plastic self-consistent (EPSC) crystal plasticity modeling, reveal the strength and hardening behavior of individual slip and twinning modes. A model that was previously published about twinning-detwinning (TDT) is implemented within the EPSC framework, and it is proven effective for describing the observed, mild tension-compression asymmetry. This is not possible with previous EPSC-based models of twinning. Finally, the description of hardening within the TDT model is modified, in order to accurately describe the evolution of internal strains within the twins.« less

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

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

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

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.

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

Crystallographic texture and microstructural changes in fusion welds of recrystallized Zry-4 rolled plates

NASA Astrophysics Data System (ADS)

Moya Riffo, A.; Vicente Alvarez, M. A.; Santisteban, J. R.; Vizcaino, P.; Limandri, S.; Daymond, M. R.; Kerr, D.; Okasinski, J.; Almer, J.; Vogel, S. C.

2017-05-01

This work presents a detailed characterization of the microstructural and crystallographic texture changes observed in the transition region in a weld between two Zircaloy-4 cold rolled and recrystallized plates. The microstructural study was performed by optical microscopy under polarized light and scanning electron microscopy (SEM). Texture changes were characterized at different lengthscales: in the micrometric size, orientation imaging maps (OIM) were constructed by electron backscatter diffraction (EBSD), in the millimetre scale, high energy XRD experiments were done at the Advanced Photon Source (USA) and compared to neutron diffraction texture determinations performed in the HIPPO instrument at Los Alamos National Laboratory. In the heat affected zone (HAZ) we observed the development of Widmanstätten microstructures, typical of the α(hcp) to β(bcc) phase transformation. Associated with these changes a rotation of the c-poles is found in the HAZ and fusion zone. While the base material shows the typical texture of a cold rolled plate, with their c-poles pointing 35° apart from the normal direction of the plate in the normal-transversal line, in the HAZ, c-poles align along the transversal direction of the plate and then re-orient along different directions, all of these changes occurring within a lengthscale in the order of mm. The evolution of texture in this narrow region was captured by both OIM and XRD, and is consistent with previous measurements done by Neutron Diffraction in the HIPPO diffractometer at Los Alamos National Laboratory, USA. The microstructural and texture changes along the HAZ were interpreted as arising due to the effect of differences in the cooling rate and β grain size on the progress of the different α variants during transformation. Fast cooling rates and large β grains are associated to weak variant selection during the β->α transformation, while slow cooling rates and fine β grains result in strong variant selection.

Crystallographic texture and microstructural changes in fusion welds of recrystallized Zry-4 rolled plates

DOE PAGES

Riffo, A. Moya; Vicente Alvarez, M. A.; Santisteban, J. R.; ...

2017-02-08

This study presents a detailed characterization of the microstructural and crystallographic texture changes observed in the transition region in a weld between two Zircaloy-4 cold rolled and recrystallized plates. The microstructural study was performed by optical microscopy under polarized light and scanning electron microscopy (SEM). Texture changes were characterized at different lengthscales: in the micrometric size, orientation imaging maps (OIM) were constructed by electron backscatter diffraction (EBSD), in the millimetre scale, high energy XRD experiments were done at the Advanced Photon Source (USA) and compared to neutron diffraction texture determinations performed in the HIPPO instrument at Los Alamos National Laboratory.more » In the heat affected zone (HAZ) we observed the development of Widmanstätten microstructures, typical of the α( hcp) to β( bcc) phase transformation. Associated with these changes a rotation of the c-poles is found in the HAZ and fusion zone. While the base material shows the typical texture of a cold rolled plate, with their c-poles pointing 35° apart from the normal direction of the plate in the normal-transversal line, in the HAZ, c-poles align along the transversal direction of the plate and then re-orient along different directions, all of these changes occurring within a lengthscale in the order of mm. The evolution of texture in this narrow region was captured by both OIM and XRD, and is consistent with previous measurements done by Neutron Diffraction in the HIPPO diffractometer at Los Alamos National Laboratory, USA. The microstructural and texture changes along the HAZ were interpreted as arising due to the effect of differences in the cooling rate and β grain size on the progress of the different α variants during transformation. Fast cooling rates and large β grains are associated to weak variant selection during the β–>α transformation, while slow cooling rates and fine β grains result in strong variant selection.« less

Crystallographic texture and microstructural changes in fusion welds of recrystallized Zry-4 rolled plates

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

Riffo, A. Moya; Vicente Alvarez, M. A.; Santisteban, J. R.

This study presents a detailed characterization of the microstructural and crystallographic texture changes observed in the transition region in a weld between two Zircaloy-4 cold rolled and recrystallized plates. The microstructural study was performed by optical microscopy under polarized light and scanning electron microscopy (SEM). Texture changes were characterized at different lengthscales: in the micrometric size, orientation imaging maps (OIM) were constructed by electron backscatter diffraction (EBSD), in the millimetre scale, high energy XRD experiments were done at the Advanced Photon Source (USA) and compared to neutron diffraction texture determinations performed in the HIPPO instrument at Los Alamos National Laboratory.more » In the heat affected zone (HAZ) we observed the development of Widmanstätten microstructures, typical of the α( hcp) to β( bcc) phase transformation. Associated with these changes a rotation of the c-poles is found in the HAZ and fusion zone. While the base material shows the typical texture of a cold rolled plate, with their c-poles pointing 35° apart from the normal direction of the plate in the normal-transversal line, in the HAZ, c-poles align along the transversal direction of the plate and then re-orient along different directions, all of these changes occurring within a lengthscale in the order of mm. The evolution of texture in this narrow region was captured by both OIM and XRD, and is consistent with previous measurements done by Neutron Diffraction in the HIPPO diffractometer at Los Alamos National Laboratory, USA. The microstructural and texture changes along the HAZ were interpreted as arising due to the effect of differences in the cooling rate and β grain size on the progress of the different α variants during transformation. Fast cooling rates and large β grains are associated to weak variant selection during the β–>α transformation, while slow cooling rates and fine β grains result in strong variant selection.« less

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

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

Application of neutron diffraction in characterization of texture evolution during high-temperature creep in magnesium alloys

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

Vogel, Sven C; Sediako, Dimitry; Shook, S

2010-01-01

A good combination of room-temperature and elevated temperature strength and ductility, good salt-spray corrosion resistance and exceUent diecastability are frequently among the main considerations in development of a new alloy. Unfortunately, there has been much lesser effort in development of wrought-stock alloys for high temperature applications. Extrudability and high temperature performance of wrought material becomes an important factor in an effort to develop new wrought alloys and processing technologies. This paper shows some results received in creep testing and studies of in-creep texture evolution for several wrought magnesium alloys developed for use in elevated-temperature applications. These studies were performed usingmore » E3 neutron spectrometer of the Canadian Neutron Beam Centre in Chalk River, ON, and HIPPO time-of-flight (TOF) spectrometer at Los Alamos Neutron Science Center, NM.« less

Quarzt Fabric Insights Across a Low P-High T Shear Zone

NASA Astrophysics Data System (ADS)

Gomez Barreiro, J.; Martinez-Catalan, J. R.; Benitez Perez, J.; Wenk, H.; Vogel, S. C.; Alcock, J. E.

2013-12-01

The evolution of mylonitic fabric in quartzites across a Low-P / High-T gradient within the Lugo Dome Extensional system (NW Spain) is analyzed. Quantitative texture measurements with TOF neutron diffraction, Shape preferred orientation (SPO) and Crystal Size Distribution (CSD) analyses were correlated with tectonothermal data to constraint the prevalence of ductile deformative fabrics exposed to cycles of dynamic and static recrystallization. Results suggest two stages in the evolution of mylonites in close correlation to thermal gradient, 1) a pervasive ductile deformation affecting most of the shear zone volume, with the development of symmetric cross girdle c-axes fabric suggesting slip on {c,r,m} and dynamically recrystallized microstructures which resulted into the refinement of the grain-size. 2) An heterogeneous deformation stage where strain partition led to the formation of relatively active and passive domains. During this late stage, at deeper levels, High T detachments show [c]{m} slip system and dynamic recrystallization activation, with monoclinic texture patterns, meanwhile, passive domains followed an static recrystallization with abnormal grain growth and minor variation of early orthogonal texture patterns Neutron diffraction data (cross) and Rietveld model obtained with MAUD (solid line) of a mylonitic quartzite. Some important planes are indicated for the major phases.

Investigation of rock samples by neutron diffraction and ultrasonic sounding

NASA Astrophysics Data System (ADS)

Burilichev, D. E.; Ivankina, T. I.; Klima, K.; Locajicek, T.; Nikitin, A. N.; Pros, Z.

2000-03-01

The interpretation of large-scale geophysical anisotropies largely depends upon the knowledge of rock anisotropies of any kind (compositions, foliations, grain shape, physical properties). Almost all physical rock properties (e.g. elastic, thermal, magnetic properties) are related to the textures of the rock constituents since they are anisotropic for the single crystal. Although anisotropy determinations are numerous, systematic investigations are scarce. Therefore, several rock samples with different microfabrics were selected for texture analysis and to determine its P-wave distributions at various confining pressures.

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

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.

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

POWTEX Neutron Diffractometer at FRM II - New Perspectives for In-Situ Rock Deformation Analysis

NASA Astrophysics Data System (ADS)

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

2012-04-01

In Geoscience quantitative texture analysis here defined as the quantitative analysis of the crystallographic preferred orientation (CPO), is a common tool for the investigation of fabric development in mono- and polyphase rocks, their deformation histories and kinematics. Bulk texture measurements also allow the quantitative characterisation of the anisotropic physical properties of rock materials. A routine tool to measure bulk sample volumes is neutron texture diffraction, as neutrons have large penetration capabilities of several cm in geological sample materials. The new POWTEX (POWder and TEXture) Diffractometer at the neutron research reactor FRM II in Garching, Germany is designed as a high-intensity diffractometer 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 time-resolved experiments and the measurement of larger sample series as necessary for the study of large scale geological structures. POWTEX is a dedicated beam line for geoscientific research. Effective texture measurements without sample tilting and rotation are possible firstly by utilizing a range of neutron wavelengths simultaneously (Time-of-Flight technique) and secondly by the high detector coverage (9.8 sr) and a high flux (~1 - 107 n/cm2s) at the sample. Furthermore the instrument and the angular detector resolution is designed also for strong recrystallisation textures as well as for weak textures of polyphase rocks. These instrument characteristics allow in-situ time-resolved texture measurements during deformation experiments on rocksalt, ice and other materials as large sample environments will be implemented at POWTEX. The in-situ deformation apparatus is operated by a uniaxial spindle drive with a maximum axial load of 250 kN, which will be redesigned to minimize shadowing effects inside the cylindrical detector. The HT deformatione 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 deformation apparatus is designed for continuous long-term deformation experiments and can be exchanged between in-situ and ex-situ placements during continuous operation inside and outside the neutron detector.

The neutron texture diffractometer at the China Advanced Research Reactor

NASA Astrophysics Data System (ADS)

Li, Mei-Juan; Liu, Xiao-Long; Liu, Yun-Tao; Tian, Geng-Fang; Gao, Jian-Bo; Yu, Zhou-Xiang; Li, Yu-Qing; Wu, Li-Qi; Yang, Lin-Feng; Sun, Kai; Wang, Hong-Li; Santisteban, J. r.; Chen, Dong-Feng

2016-03-01

The first neutron texture diffractometer in China has been built at the China Advanced Research Reactor, due to strong demand for texture measurement with neutrons from the domestic user community. This neutron texture diffractometer has high neutron intensity, moderate resolution and is mainly applied to study texture in commonly used industrial materials and engineering components. In this paper, the design and characteristics of this instrument are described. The results for calibration with neutrons and quantitative texture analysis of zirconium alloy plate are presented. The comparison of texture measurements with the results obtained in HIPPO at LANSCE and Kowari at ANSTO illustrates the reliability of the texture diffractometer. Supported by National Nature Science Foundation of China (11105231, 11205248, 51327902) and International Atomic Energy Agency-TC program (CPR0012)

Investigation of rail wheel steel crystallographic texture changes due to modification and thermomechanical treatment

NASA Astrophysics Data System (ADS)

Lychagina, T.; Nikolayev, D.; Sanin, A.; Tatarko, J.; Ullemeyer, K.

2015-04-01

In this work crystallographic texture for a set of rail wheel steel samples with different regimes of thermo-mechanical treatment and with and without modification by system Al-Mg-Si- Fe-C-Ca-Ti-Ce was measured by neutron diffraction. The texture measurements were carried out by using time-of-flight technique at SKAT diffractometer situated at IBR-2 reactor (Dubna, JINR, Russia). The three complete pole figures (110), (200), (211) of α-Fe phase in 5°×5°grid were extracted from a set of 1368 spectra measured for each sample. The samples were cut from rail wheel rim and from transitional zone (between rail wheel hub and wheel disk). It was concluded that the steel modification and some changes in the heat treatment modes of the rail wheels from the experimental (modified) and the conventional (non-modified) steel lead to reorientation of texture component.

Twinning-detwinning behavior during cyclic deformation of magnesium alloy

DOE PAGES

Lee, Soo Yeol; Wang, Huamiao; Gharghouri, Michael A.

2015-05-26

In situ neutron diffraction has been used to examine the deformation mechanisms of a precipitation-hardened and extruded Mg-8.5wt.%Al alloy subjected to (i) compression followed by reverse tension (texture T1) and (ii) tension followed by reverse compression (texture T2). Two starting textures are used: (1) as-extruded texture, T1, in which the basal pole of most grains is normal to the extrusion axis and a small portion of grains are oriented with the basal pole parallel to the extrusion axis; (2) a reoriented texture, T2, in which the basal pole of most grains is parallel to the extrusion axis. For texture T1,more » the onset of extension twinning corresponds well with the macroscopic elastic-plastic transition during the initial compression stage. The non-linear macroscopic stress/strain behavior during unloading after compression is more significant than during unloading after tension. For texture T2, little detwinning occurs after the initial tension stage, but almost all of the twinned volumes are detwinned during loading in reverse compression.« less

Effect of Extrusion Temperature on the Plastic Deformation of an Mg-Y-Zn Alloy Containing LPSO Phase Using In Situ Neutron Diffraction

NASA Astrophysics Data System (ADS)

Garces, G.; Perez, P.; Cabeza, S.; Kabra, S.; Gan, W.; Adeva, P.

2017-11-01

The evolution of the internal strains during in situ tension and compression tests has been measured in an MgY2Zn1 alloy containing long-period stacking ordered (LPSO) phase using neutron diffraction. The alloy was extruded at two different temperatures to study the influence of the microstructure and texture of the magnesium and the LPSO phases on the deformation mechanisms. The alloy extruded at 623 K (350 °C) exhibits a strong fiber texture with the basal plane parallel to the extrusion direction due to the presence of areas of coarse non-recrystallised grains. However, at 723 K (450 °C), the magnesium phase is fully recrystallised with grains randomly oriented. On the other hand, at the two extrusion temperatures, the LPSO phase orients their basal plane parallel to the extrusion direction. Yield stress is always slightly higher in compression than in tension. Independently on the stress sign and the extrusion temperature, the beginning of plasticity is controlled by the activation of the basal slip system in the dynamic recrystallized grains. Therefore, the elongated fiber-shaped LPSO phase which behaves as the reinforcement in a metal matrix composite is responsible for this tension-compression asymmetry.

Magnetic texturing due to the partial ordering of Fe+3 and Cu+2 in NdBaCuFeO5

NASA Astrophysics Data System (ADS)

Pissas, M.

2017-06-01

The crystal and magnetic structure of the oxygen deficient double perovskite NdBaCuFeO5 was studied, using neutron powder diffraction data. The structure was refined from neutron powder diffraction data using the space groups P 4 / mmm and P 4 mm . For 2K ⩽ T ⩽TN2 = 260K three families of magnetic Bragg peaks exist. These peaks can be indexed with commensurate propagation vectors k1 =[1/2 1/2 1/2], k2 =[1/2 1/2 0] and the incommensurate k3 =[1/2 1/2 0.4]. Above TN2 only magnetic Bragg peaks originated from k1 and k2 propagation, were observed. The incommensurate magnetic structure can be attributed to a circular inclined spiral ordering as in YBaCuFeO5 compound.

Crystallographic Characterization on Polycrystalline Ni-Mn-Ga Alloys with Strong Preferred Orientation.

PubMed

Li, Zongbin; Yang, Bo; Zou, Naifu; Zhang, Yudong; Esling, Claude; Gan, Weimin; Zhao, Xiang; Zuo, Liang

2017-04-27

Heusler type Ni-Mn-Ga ferromagnetic shape memory alloys can demonstrate excellent magnetic shape memory effect in single crystals. However, such effect in polycrystalline alloys is greatly weakened due to the random distribution of crystallographic orientation. Microstructure optimization and texture control are of great significance and challenge to improve the functional behaviors of polycrystalline alloys. In this paper, we summarize our recent progress on the microstructure control in polycrystalline Ni-Mn-Ga alloys in the form of bulk alloys, melt-spun ribbons and thin films, based on the detailed crystallographic characterizations through neutron diffraction, X-ray diffraction and electron backscatter diffraction. The presented results are expected to offer some guidelines for the microstructure modification and functional performance control of ferromagnetic shape memory alloys.

Process-structure-property relationships of micron thick gadolinium oxide films deposited by reactive electron beam-physical vapor deposition (EB-PVD)

NASA Astrophysics Data System (ADS)

Grave, Daniel A.

Gadolinium oxide (Gd2O3) is an attractive material for solid state neutron detection due to gadolinium's high thermal neutron capture cross section. Development of neutron detectors based on Gd2 O3 requires sufficiently thick films to ensure neutron absorption. In this dissertation work, the process-structure-property relationships of micron thick Gd2O3 films deposited by reactive electron-beam physical vapor deposition (EB-PVD) were studied. Through a systematic design of experiments, fundamental studies were conducted to determine the effects of processing conditions such as deposition temperature, oxygen flow rate, deposition rate, and substrate material on Gd2O3 film crystallographic phase, texture, morphology, grain size, density, and surface roughness. Films deposited at high rates (> 5 A/s) were examined via x-ray diffraction (XRD) and Raman spectroscopy. Quantitative phase volume calculations were performed via a Rietveld refinement technique. All films deposited at high rates were found to be fully monoclinic or mixed cubic/monoclinic phase. Generally, increased deposition temperature and increased oxygen flow resulted in increased cubic phase volume. As film thickness increased, monoclinic phase volume increased. Grazing incidence x-ray diffraction (GIXRD) depth profiling analysis showed that cubic phase was only present under large incidence angle (large penetration depth) measurements, and after a certain point, only monoclinic phase was grown. This was confirmed by transmission electron microscopy (TEM) analysis with selected area diffraction (SAD). Based on this information, a large compressive stress was hypothesized to cause the formation of the monoclinic phase and this hypothesis was confirmed by demonstrating the existence of a stress induced phase transition. An experiment was designed to introduce compressive stress into the Gd2O 3 films via ion beam assisted deposition (IBAD). This allowed for systematic increase in compressive stress while keeping a large adatom diffusion length on the film surface. Crystallographic texture evolution in the Gd2O3 films was investigated for different substrate types. At high rates, it was shown that films deposited on different substrates (quartz, silicon, sapphire, and GaN) all had similar theta-2theta diffraction patterns, suggesting that films grew similarly on different substrates due to the low adatom mobility. However, significant differences in texture were observed for films deposited at low rates (< 1 A/s) and high temperature (650°C) on different substrates. For evaluation of in-plane texture in the Gd2O 3 films, pole figure analysis was performed. Mixed phase films deposited at high rates and low temperature showed weak out-of-plane texture and random in-plane texture. Mixed phase films deposited at high temperatures possessed a fiber texture (strong out-of-plane texture), but lacked the necessary adatom mobility to develop in-plane texture. For single phase cubic films grown under low rates of deposition, out-of-plane texture was observed on quartz substrates. However, weak and strong in-plane textures were observed for sapphire and GaN substrates, respectively. The use of ion bombardment resulted in the formation of moderate biaxial texture for films grown on quartz. For films grown on sapphire, a very strong biaxial texture was achieved with ion bombardment which adds additional energy to the system. The effects of processing on the structure, composition, and interfacial chemistry of the Gd2O3 films were investigated. The results showed that films primarily adhered to the Structure-Zone models with a few exceptions. The deviation from the Structure-Zone model was explained by the combined effects of columnar growth, shadowing, and adatom mobility. At low deposition temperatures, decreasing oxygen flow resulted in increased film density due to higher adatom mobility. Films deposited at this temperature were characterized by small (10-15 nm) nanocrystalline grains with some porous disordered regions. The dielectric properties of Si(111)/Gd2O3/Ti/Au MOS capacitors were investigated. Moisture absorption in Gd2O 3 films was found to result in both increased dielectric loss (10x) and inflated dielectric constant values ( 40 %). Heat treatment of the films at 100 °C resulted in outgassing of moisture, reduction in dielectric constant, and excellent frequency dispersion of the dielectric constant over a range of 10 kHz-1 MHz. The effect of film processing on the dielectric constant was systematically investigated. Tuning of the dielectric constant from a value of 11 to a value of 24 was possible by manipulating the structure and crystallographic phase of the material via the processing conditions. Capacitance-voltage (C-V) and conductance-voltage (G-V) characteristics of GaN/AlGaN/Gd2O3/Ti/Au MOS capacitors were investigated. The effects of processing on fixed oxide charge, trapped oxide charge, and density of interface states were evaluated. Single phase cubic films deposited at low rates with near heteroepitaxial growth were shown to have the lowest density of trapped charge. (Abstract shortened by ProQuest.).

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

DOE PAGES

Yeager, John D.; Luscher, Darby J.; Vogel, Sven C.; ...

2016-02-02

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

Crystallographic Characterization on Polycrystalline Ni-Mn-Ga Alloys with Strong Preferred Orientation

PubMed Central

Li, Zongbin; Yang, Bo; Zou, Naifu; Zhang, Yudong; Esling, Claude; Gan, Weimin; Zhao, Xiang; Zuo, Liang

2017-01-01

Heusler type Ni-Mn-Ga ferromagnetic shape memory alloys can demonstrate excellent magnetic shape memory effect in single crystals. However, such effect in polycrystalline alloys is greatly weakened due to the random distribution of crystallographic orientation. Microstructure optimization and texture control are of great significance and challenge to improve the functional behaviors of polycrystalline alloys. In this paper, we summarize our recent progress on the microstructure control in polycrystalline Ni-Mn-Ga alloys in the form of bulk alloys, melt-spun ribbons and thin films, based on the detailed crystallographic characterizations through neutron diffraction, X-ray diffraction and electron backscatter diffraction. The presented results are expected to offer some guidelines for the microstructure modification and functional performance control of ferromagnetic shape memory alloys. PMID:28772826

Texture analysis of oxide dispersion strengthened (ODS) Fe alloys by X-ray and neutron diffraction

NASA Astrophysics Data System (ADS)

Béchade, J. L.; Mathon, M. H.; Branger, V.; Réglé, H.; Alamo, A.

2002-07-01

The ferritic ODS alloys studied were obtained by mechanical alloying. This strengthening method is very attractive, in particular for nuclear applications. In order to ensure the alloy a good compromise between mechanical resistance and ductility at high temperatures, it is necessary to control the microstructure and in particular the evolution during the recrystallization. First, a preliminary study, performed by X ray diffraction and optical microscopy, shows several grain growth mechanisms ; in particular, the “abnormal” grain growth mechanism which conducts to a large grain size [1], [2]. After annealing (3600s at 1470^{circ}C), the 30% cold-worked (swaging) alloys exhibit an heterogeneous microstructure with a large grains size ( 200 to 500 μm) in the heart and near the surface of the material when the intermediate zone is inhabited by small grains ( 1 μm). Fora higher cold-work level (60%), large size grains are only present in the periphery of the material. On account of the large grain size and strong heterogeneity of the microstructure, texture analysis using laboratory x-ray beam in not well adapted and so we have decided to use neutron beam. The neutron diffraction texture analysis has been performed at the Laboratoire Léon Brillouin on the 6T1 diffractometer on 2 different rods of the alloy (corresponding to the reduction ratios of 30% and 60%). Specific samples have been machined to characterise separately the zones with a different microstructure. After deformation, the alloys exhibit a typical α-fibre texture \\{ hkl \\} <1l0> whatever the area of the sample and the reduction ratio. After recrystallization, a very inhomogeneous texture is evidenced through the thickness of the sample, in particular for the rod deformed with a reduction ratio of 30% : in the heart and in the periphery of the rod, a “single-crystal” type texture is observed; the a fibre remains for the intermediate diameter of the rod. For the rod cold rolled with a reduction ratio of 60%, the α-fibre keeps on the heart of the material and as in the precedent case, a “single-crystal” type texture is observed near the surface of the sample. EBSD measurements have been performed to explicit at a local scale this behaviour and in order to furnish some input data for the simulation of static recrystallization. Les aciers ferritiques avec dispersion d'oxydes étudiés sont obtenus par métallurgie des poudres, ce qui leur confère une résistance mécanique accrue à haute température notamment pour des applications nucléaires. La difficulté pour l'utilisation de tels alliages réside dans la maîtrise de leur microstructure au cours de l'élaboration en particulier durant la recristallisation. Une première étude en diffraction des rayons-x et en métallographie optique a permis de révéler différents mécanismes de croissance du grain lors de la recristallisation, notamment une croissance “anormale” conduisant à une taille de grain très importante [t], [2]. Après recuit (3600s à 1470^{circ}C), précédé par un écrouissage de 30% sur des barres (par martelage) on voit apparaître une microstructure hétérogène à gros grains ( 200 à 500 μm) au coeur et en surface externe de la barre alors que la zone intermédiaire est peuplée de grains fins (sim 1 μm). Pour un écrouissage plus élevé (60%), après le même recuit, on ne voit apparaître des gros grains qu'en périphérie de la barre. Pour ce type de microstructure fortement hétérogène et à gros grains, la diffraction des rayons-x pour l'analyse de texture est mal adaptée, ce qui nous a conduit à utiliser la diffraction des neutrons sur le diffractomètre 6TI du Laboratoire Léon Brillouin. Les deux matériaux, écrouis de 30% et 60%, ont été analysés en réalisant des échantillons particuliers permettant d'étudier séparément le coeur et la périphérie. Après déformation, les deux échantillons présentent une texture de fibre α \\{ hkl \\} <1l0> en tout point de la barre. Après recristallisation, on retrouve une texture très hétérogène suivant le rayon de la barre, notamment après 30% : le coeur et la périphérie de la barre présentent une texture de type “mono-cristal”, la zone intermédiaire restant une fibre α. Après écrouissage de 60%, on garde la fibre α au coeur de la barre, la périphérie présentant, comme pour l'écrouissage précédent, une texture de type “mono-cristal”. Des analyses en EBSD ont également été réalisées pour foumir des éléments de compréhension sur les mécanismes locaux de recristallisation afin de simuler la recristallisation statique de ses alliages via une approche numérique.

In Situ Neutron Diffraction Study of the Influence of Microstructure on the Mechanical Response of Additively Manufactured 304L Stainless Steel

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

Brown, D. W.; Adams, D. P.; Balogh, L.

In situ neutron diffraction measurements were completed for this study during tensile and compressive deformation of stainless steel 304L additively manufactured (AM) using a high power directed energy deposition process. Traditionally produced wrought 304L material was also studied for comparison. The AM material exhibited roughly 200 MPa higher flow stress relative to the wrought material. Crystallite size, crystallographic texture, dislocation density, and lattice strains were all characterized to understand the differences in the macroscopic mechanical behavior. The AM material’s initial dislocation density was about 10 times that of the wrought material, and the flow strength of both materials obeyed themore » Taylor equation, indicating that the AM material’s increased yield strength was primarily due to greater dislocation density. Finally, a ~50 MPa flow strength tension/compression asymmetry was observed in the AM material, and several potential causes were examined.« less

In Situ Neutron Diffraction Study of the Influence of Microstructure on the Mechanical Response of Additively Manufactured 304L Stainless Steel

DOE PAGES

Brown, D. W.; Adams, D. P.; Balogh, L.; ...

2017-10-10

In situ neutron diffraction measurements were completed for this study during tensile and compressive deformation of stainless steel 304L additively manufactured (AM) using a high power directed energy deposition process. Traditionally produced wrought 304L material was also studied for comparison. The AM material exhibited roughly 200 MPa higher flow stress relative to the wrought material. Crystallite size, crystallographic texture, dislocation density, and lattice strains were all characterized to understand the differences in the macroscopic mechanical behavior. The AM material’s initial dislocation density was about 10 times that of the wrought material, and the flow strength of both materials obeyed themore » Taylor equation, indicating that the AM material’s increased yield strength was primarily due to greater dislocation density. Finally, a ~50 MPa flow strength tension/compression asymmetry was observed in the AM material, and several potential causes were examined.« less

Texture and anisotropy in ferroelectric lead metaniobate

NASA Astrophysics Data System (ADS)

Iverson, Benjamin John

Ferroelectric lead metaniobate, PbNb2O6, is a piezoelectric ceramic typically used because of its elevated Curie temperature and anisotropic properties. However, the piezoelectric constant, d33, is relatively low in randomly oriented ceramics when compared to other ferroelectrics. Crystallographic texturing is often employed to increase the piezoelectric constant because the spontaneous polarization axes of grains are better aligned. In this research, crystallographic textures induced through tape casting are distinguished from textures induced through electrical poling. Texture is described using multiple quantitative approaches utilizing X-ray and neutron time-of-flight diffraction. Tape casting lead metaniobate with an inclusion of acicular template particles induces an orthotropic texture distribution. Templated grain growth from seed particles oriented during casting results in anisotropic grain structures. The degree of preferred orientation is directly linked to the shear behavior of the tape cast slurry. Increases in template concentration, slurry viscosity, and casting velocity lead to larger textures by inducing more particle orientation in the tape casting plane. The maximum 010 texture distributions were two and a half multiples of a random distribution. Ferroelectric texture was induced by electrical poling. Electric poling increases the volume of material oriented with the spontaneous polarization direction in the material. Samples with an initial paraelectric texture exhibit a greater change in the domain volume fraction during electrical poling than randomly oriented ceramics. In tape cast samples, the resulting piezoelectric response is proportional to the 010 texture present prior to poling. This results in property anisotropy dependent on initial texture. Piezoelectric properties measured on the most textured ceramics were similar to those obtained with a commercial standard.

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

NASA Astrophysics Data System (ADS)

Reiche, Helmut Matthias

Generation IV nuclear reactor concepts, such as the supercritical-water-cooled nuclear reactor (SCWR), are actively researched internationally. Operating conditions above the critical point of water (374°C, 22.1 MPa) and fuel core temperature that potentially exceed 1850°C put a high demand on the surrounding materials. For their safe application, it is essential to characterize and understand the material properties on an atomic scale such as crystal structure and grain orientation (texture) changes as a function of temperature and stress. This permits the refinement of models predicting the macroscopic behavior of the material. Neutron diffraction is a powerful tool in characterizing such crystallographic properties due to their deep penetration depth into condensed matter. This leads to the ability to study bulk material properties, as opposed to surface effects, and allows for complex sample environments to study e.g. the individual contributions of thermo-mechanical processing steps during manufacturing, operating or accident scenarios. I present three sample environments for in situ neutron diffraction studies that provide such crystallographic information and have been successfully commissioned and integrated into the user program of the High Pressure -- Preferred Orientation (HIPPO) diffractometer at the Los Alamos Neutron Science Center (LANSCE) user facility. I adapted a sample changer for reliable and fast automated texture measurements of multiple specimens. I built a creep furnace combining a 2700 N load frame with a resistive vanadium furnace, capable of temperatures up to 1000°C, and manipulated by a pair of synchronized rotation stages. This combination allows following deformation and temperature dependent texture and strain evolutions in situ. Utilizing the presented sample changer and creep furnace we studied pressure tubes made of Zr-2.5wt%Nb currently employed in CANDURTM nuclear reactors and proposed for future SCWRs, acting as the primary containment vessel of high temperature heavy water (D2O) inside the reactor core. The measured sample texture shows that upon traversing the phase transition, which proceeded according to the Burger orientation relationship, variant selection occurred during heating and cooling of the zirconium alloy. Experimental results of lattice strains depending on the crystallographic orientation can be used to calculate strain pole figures which grant insight into the three-dimensional mechanical response of a polycrystalline aggregate and represent an extremely powerful material model validation tool. Lastly, I developed a resistive graphite high-temperature furnace with sample motion for in situ crystal structure and texture measurements of nuclear materials at steady-state temperatures up to at least 2200°C. This permits in situ observation of e.g. phase transitions and coefficients of thermal expansion, as well as phase formation and texture development during solidification. Utilizing this apparatus, I investigated the carbothermic reduction of UO2 nanopowder forming uranium carbide, a promising Generation IV reactor fuel. The onset of the UO2 + 2C → UC + CO2 reaction was observed at 1440°C with the bulk portion being complete at 1500°C. I describe the novel synthesis for this nanoparticle UO2 powder, which closely imitates observed nano grains in partially burnt reactor fuels. Of the three opposing structure models reported for the non-quenchable cubic UC2 phase, stable between 1769°C and 2560°C, the NaCl-type structure according to Bowman is found to be correct. This is deemed major progress as the CaF2-type structure was used for recent thermal modeling of safety critical factors in nuclear reactors. A temperature dependent increase in density due to carbon diffusion has been observed and quantified. I provide first experimental data of an unspecified, reversible order-disorder transition in this delta-phase with its onset at ˜1800°C which is likely due to rotating C2 molecules in the sublattice.

Plastic Deformation of Magnesium Alloy Subjected to Compression-First Cyclic Loading

NASA Astrophysics Data System (ADS)

Lee, Soo Yeol; Gharghouri, Michael A.; Root, John H.

In-situ neutron diffraction has been employed to study the deformation mechanisms in a precipitation-hardened and extruded Mg-8.5wt.% Al alloy subjected to compression followed by reverse tension. The starting texture is such that the basal poles of most grains are oriented normal to the extrusion axis and a small portion of grains are oriented with the basal pole parallel to the extrusion axis. Diffraction peak intensities for several grain orientations monitored in-situ during deformation show that deformation twinning plays an important role in the elastic-plastic transition and subsequent plastic deformation behavior. Significant non-linear behavior is observed during unloading after compression and appears to be due to detwinning. This effect is much stronger after compressive loading than after tensile loading.

Analysis and interpretation of diffraction data from complex, anisotropic materials

NASA Astrophysics Data System (ADS)

Tutuncu, Goknur

Most materials are elastically anisotropic and exhibit additional anisotropy beyond elastic deformation. For instance, in ferroelectric materials the main inelastic deformation mode is via domains, which are highly anisotropic crystallographic features. To quantify this anisotropy of ferroelectrics, advanced X-ray and neutron diffraction methods were employed. Extensive sets of data were collected from tetragonal BaTiO3, PZT and other ferroelectric ceramics. Data analysis was challenging due to the complex constitutive behavior of these materials. To quantify the elastic strain and texture evolution in ferroelectrics under loading, a number of data analysis techniques such as the single peak and Rietveld methods were used and their advantages and disadvantages compared. It was observed that the single peak analysis fails at low peak intensities especially after domain switching while the Rietveld method does not account for lattice strain anisotropy although it overcomes the low intensity problem via whole pattern analysis. To better account for strain anisotropy the constant stress (Reuss) approximation was employed within the Rietveld method and new formulations to estimate lattice strain were proposed. Along the way, new approaches for handling highly anisotropic lattice strain data were also developed and applied. All of the ceramics studied exhibited significant changes in their crystallographic texture after loading indicating non-180° domain switching. For a full interpretation of domain switching the spherical harmonics method was employed in Rietveld. A procedure for simultaneous refinement of multiple data sets was established for a complete texture analysis. To further interpret diffraction data, a solid mechanics model based on the self-consistent approach was used in calculating lattice strain and texture evolution during the loading of a polycrystalline ferroelectric. The model estimates both the macroscopic average response of a specimen and its hkl-dependent lattice strains for different reflections. It also tracks the number of grains (or domains) contributing to each reflection and allows for domain switching. The agreement between the model and experimental data was found to be satisfactory.

Texture and elastic anisotropy of a mylonitic anorthosite from the Morin Shear Zone (Quebec, Canada)

NASA Astrophysics Data System (ADS)

Gómez Barreiro, Juan; Wenk, Hans-Rudolf; Vogel, Sven

2015-02-01

A sample of anorthosite from the granulite facies Morin Shear Zone (Quebec, Canada) was investigated for crystal preferred orientation and elastic anisotropy. Time-of-flight neutron diffraction data obtained with the HIPPO diffractometer at LANSCE were analyzed with the Rietveld method to obtain orientation distribution functions of the principal phases (plagioclase, clinopyroxene and orthopyroxene). Texture and microstructures are compatible with the plastic deformation of the aggregate under high-T conditions. All mineral phases depict a significant preferred orientation that could be related to the general top-to-the north shearing history of the Morin Shear Zone. Texture patterns suggest that (010)[001] in plagioclase and (110)[001] in clinopyroxene are likely dominant slip systems. Using preferred orientation data P- and S-waves velocities and elastic anisotropy were calculated and compared with previous studies to explore elastic properties of rocks with different pyroxene-plagioclase mixtures. P-wave velocity, S-wave splitting and anisotropy increase with clinopyroxene content. Seismic anisotropy is linked to the texture symmetry which can lead to large deviations between actual anisotropy and that measured along Cartesian XYZ sample directions (lineation/foliation reference frame). This is significant for the prediction and interpretation of seismic data, particularly for monoclinic or triclinic texture symmetries.

Quantitative fabric analysis of eclogite facies mylonites: texture and microtomography

NASA Astrophysics Data System (ADS)

Gomez Barreiro, J.; Voltolini, M.; Martinez-Catalan, J. R.; Benitez-Perez, J. M.; Diez-fernandez, R.; Wenk, H. R.; Vogel, S. C.; Mancini, L.

2014-12-01

Understanding the flow of rock deformed under eclogite facies conditions is crucial to constraint the dynamics of a subducting slab. Prograde metamorphism during burial in a subduction zone proceeds across several lithologies, resulting in heterogeneous eclogitization and potentially different processes. In order to explore the expression of such a variety in terms of a deformative fabric, we have analyzed texture and shape fabric of eclogites and eclogitic orthogneisses from the Malpica-Tui unit (NW Spain). We explore the same rock volumes with TOF-neutron diffraction (HIPPO @ LANSCE) and synchrotron microtomography (SYRMEP @Elettra). Orientation distribution functions were extracted after Rietveld refinement in MAUD and morphometric data (size, aspect ratio, orientation) were obtained after image processing with FIJI, Blob3D and MATLAB. Shape fabric reflects the macroscopic foliation and lineation and correlates with texture. Garnet fabric is particularly important because of the rheological implications of its mechanical behavior. Garnet shows little elongation in both samples, and texture is significant, what probably points to a relatively dry deformative environment, with diffusion-assisted dislocation. This eclogites could represent a rigidification stage in the subduction channel preserved during the exhumation at high-P and high-T documented in the Malpica-Tui unit during the Variscan orogeny.

Effect of annealing conditions on the microstructure and magnetic properties of sintered Nd-Fe-B magnets as seen by magnetic small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Périgo, Élio A.; Titov, Ivan; Weber, Raoul; Mettus, Denis; Peral, Inma; Vallcorba, Oriol; Honecker, Dirk; Feoktystov, Artem; Michels, Andreas

2018-03-01

We have investigated the effect of the annealing conditions (heating rate and temperature) on the magnetic microstructure of sintered Nd-Fe-B magnets by means of magnetometry, scanning electron microscopy, high-energy synchrotron x-ray diffraction, and small-angle neutron scattering (SANS). While the temperature treatment has a strong effect on the coercivity (reduction by about 50% on annealing), the associated changes in the microstructure do surprisingly not show up (or at best only very weakly) in the neutron-scattering signal, which probes a mesoscopic real-space length scale ranging between about 1–300 nm. On the other hand, the x-ray data reveal microstructural changes in the Nd-rich phases, presumably due to modifications in grain-boundary regions. Moreover, we observe an unusual diamond-shaped angular anisotropy in the SANS cross section, which strongly points towards the existence of texture in the nuclear microstructure.

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.

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

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)

Intergrannular strain evolution in a zircaloy-4 alloy with Widmanstatten microstructure

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

Clausen, Bjorn; Vogel, Sven C; Garlea, Eena

2009-01-01

A Zircaloy-4 alloy with Widmanstatten-Basketweave microstructure and random texture has been used to study the deformation systems responsible for the polycrystalline plasticity at the grain level. The evolution of internal strain and bulk texture is investigated using neutron diffraction and an elasto-plastic self-consistent (EPSC) modeling scheme. The macroscopic stress-strain behavior and intergranular (hkil-specific) strain development, parallel and perpendicular to the loading direction, were measured in-situ during uniaxial tensile loading. Then, the EPSC model was employed to simulate the experimental results. This modeling scheme accounts for the thermal anisotropy; elastic-plastic properties of the constituent grains; and activation, reorientation, and stress relaxationmore » associated with twinning. The agreement between the experiment and the model will be discussed as well as the critical resolved shear stresses (CRSS) and the hardening coefficients obtained from the model.« less

In situ observation of self-propagating high temperature syntheses of Ta5Si3, Ti5Si3 and TiB2 by proton and X-ray radiography

NASA Astrophysics Data System (ADS)

Bernert, T.; Winkler, B.; Haussühl, E.; Trouw, F.; Vogel, S. C.; Hurd, A. J.; Smilowitz, L.; Henson, B. F.; Merrill, F. E.; Morris, C. L.; Mariam, F. G.; Saunders, A.; Juarez-Arellano, E. A.

2013-08-01

Self-propagating high temperature reactions of tantalum and titanium with silicon and titanium with boron were studied using proton and X-ray radiography, small-angle neutron scattering, neutron time-of-flight, X-ray and neutron diffraction, dilatometry and video recording. We show that radiography allows the observation of the propagation of the flame front in all investigated systems and the determination of the widths of the burning zones. X-ray and neutron diffraction showed that the reaction products consisted of ≈90 wt% of the main phase and one or two secondary phases. For the reaction 5Ti + 3Si → Ti5Si3 flame front velocities of 7.1(3)-34.2(4) mm/s were determined depending on the concentration of a retardant added to the starting material, the geometry and the green density of the samples. The flame front width was determined to be 1.17(4)-1.82(8) mm and depends exponentially on the flame front velocity. Similarly, for the reaction Ti + 2B → TiB2 flame front velocities of 15(2)-26.6(4) mm/s were determined, while for a 5Ta + 3Si → Ta5Si3 reaction the flame front velocity was 7.05(4) mm/s. The micro structure of the product phase Ta5Si3 shows no texture. From SANS measurements the dependence of the specific surface of the product phase on the particle sizes of the starting materials was studied.

Preliminary 3D In-situ measurements of the texture evolution of strained H2O ice during annealing using neutron Laue diffractometry

NASA Astrophysics Data System (ADS)

Journaux, Baptiste; Montagnat, Maurine; Chauve, Thomas; Ouladdiaf, Bachir; Allibon, John

2015-04-01

Dynamic recrystallization (DRX) strongly affects the evolution of microstructure (grain size and shape) and texture (crystal preferred orientation) in materials during deformation at high temperature. Since texturing leads to anisotropic physical properties, predicting the effect of DRX is essential for industrial applications, for interpreting geophysical data and modeling geodynamic flows, and predicting ice sheet flow and climate evolution. A large amount of literature is available related to metallurgy, geology or glaciology, but there remains overall fundamental questions about the relationship between nucleation, grain boundary migration and texture development at the microscopic scale. Previous measurements of DRX in ice were either conducted using 2D ex-situ techniques such as AITA [1,2] or Electron Backscattering Diffraction (EBSD) [3], or using 3D statistical ex-situ [4] or in-situ [5] techniques. Nevertheless, all these techniques failed to observe at the scale of nucleation processes during DRX in full 3D. Here we present a new approach using neutron Laue diffraction, which enable to perform 3D measurements of in-situ texture evolution of strained polycrystalline H2O ice (>2% at 266 K) during annealing at the microscopic scale. Thanks the CYCLOPS instrument [6] (Institut Laue Langevin Grenoble, France) and the intrinsic low background of this setup, preliminary observations enabled us to follow, in H2O ice, the evolution of serrated grain boundaries, and kink-band during annealing. Our observations show a significant evolution of the texture and internal misorientation over the course of few hours at an annealing temperature of 268.5 K. In the contrary, ice kink-band structures seem to be very stable over time at near melting temperatures. The same samples have been analyzed ex-situ using EBSD for comparison. These results represent a first step toward in-situ microscopic measurements of dynamic recrystallization processes in ice during strain. This experiment has been conducted in the frame of the ANR-funded DREAM project that focuses on the recrystallization processes in anisotropic materials. References [1] D. S. Russell-Head and C.J.L. Wilson., 2001, Journal of Glaciology, 24, 117-130. [2] Wilson, C.J.L., Peternell, M., Piazolo, S., Luzin, V., 2014, Journal of Structural Geology, Microdynamics of Ice, 61, 50-77. [3] M. Montagnat, T. Chauve, F. Barou, A. Tommasi, B. Beausir, C. Fressengeas., in prep. [4] T. H. Jacka and J. Li., 2000, In T. Hondoh, editor, Physics of Ice Core Records, pages 83-102. Hokkaido University Press, Sapporo. [5] S. Piazolo, C. J. L. Wilson, V. Luzin, C. Brouzet, and M. Peternell., 2013, Geochemistry, Geophysics, Geosystems, 14, 4185-4194. [6] B. Ouladdiaf et al., 2011, Journal of Applied Crystallography, 44, 392-397.

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

Neutron Time-of-Flight Diffractometer HIPPO at LANSCE

NASA Astrophysics Data System (ADS)

Vogel, Sven; Williams, Darrick; Zhao, Yusheng; Bennett, Kristin; von Dreele, Bob; Wenk, Hans-Rudolf

2004-03-01

The High-Pressure Preferred Orientation (HIPPO) neutron diffractometer is the first third-generation neutron time-of-flight powder diffractometer to be constructed in the United States. It produces extremely high intensity by virtue of a short (9 m) initial flight path on a high intensity water moderator and 1380 3He detector tubes covering 4.5 m2 of detector area from 10' to 150' in scattering angles. HIPPO was designed and manufactured as a joint effort between LANSCE and University of California with the goals of attaining world-class science and making neutron powder diffractometry an accessible and available tool to the national user community. Over two decades of momentum transfer are available (0.1-30 A-1) to support studies of amorphous solids; magnetic diffraction; small crystalline samples; and samples subjected to extreme environments such as temperature, pressure, or magnetic fields. The exceptionally high data rates of HIPPO also make it useful for time-resolved studies. In addition to the standard ancillary equipment (100-position sample/texture changer, closed-cycle He refrigerator, furnace), HIPPO has unique high-pressure cells capable of achieving pressures of 30 GPA at ambient and high (2000 K) temperature with samples up to 100 mm3 in volume.

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

Applied Crystallography - Proceedings of the XVth Conference

NASA Astrophysics Data System (ADS)

Morawiec, H.; Ströż, D.

1993-06-01

The Table of Contents for the full book PDF is as follows: * Foreword * The International Centre for Diffraction Data and Its Future Developments * The Rietveld Method - A Historical Perspective * Real Structure in Quantitative Powder Diffraction Phase Analysis * Neutron Focusing Optics in Applied Crystallography * The Crystal Structures of Oxygen Deficient Rare Earth Oxides * Short-Range Order in Layer-Structured Ba1-xSrxBi2Nb2O9 Ferroelectrics * Radial Distribution Function as a Tool of Structural Studies on Noncrystalline Materials * Determination of Radial Distribution Function (RDF) of Electrodeposited Cu-Cd Alloys After Annealing * Spheres Packing as a Factor Describing the Local Environment and Structure Stability * X-Ray Stress Measurement of Samples Combined with Diffraction Line Analysis * Phase Stability and Martensitic Transformation in Cu-Zn and Cu-Zn-Al Single Crystals * Order, Defects, Precipitates and the Martensitic Transformation in β Cu-Zn-Al * Effect of γ Precipitates on the Martensitic Transformation in Cu-Zn-Al Alloys * Phase Transitions and Shape Memory Effect in a Thermomechanically Treated NiTi Alloy * Structure of Martensite and Bainite in CuAlMn Alloys * Glass-Ceramics * Mechanism of Texture Formation at the Rolling of Low Stacking Fault Energy Metals and Alloys * Shear Texture of Zinc and the Conditions of Its Occuring * The Development of Texture of ZnAlMg Sheets Depending on Deformation Geometry * Texture Stability of the D.S. NiAlMoCrTi Alloy After Heat Treatment * X-Ray Diffraction Method for Controlling of Texture Evolution in Layers * Texture and Lattice Imperfections Study of Some Low Alloyed Copper Alloys * Selected Examples of the Calculation of the Orientation Distribution Function for Low Crystal and Sample Symmetries * Automatical X-Ray Quantitative Phase Analysis * Application of a PC Computer for Crystallographic Calculations * Electron Diffraction Analysis using a Personal Computer * CA.R.INE Crystallography Version 2.1-1992 * PC-MINREF: The Computer Program Package for Neutron Refinement of Incommensurate Multiphase Crystal and Magnetic Structures on IBM PC Computers * Possibilities of Deflections from Stoichiometry Investigation for Phases of b1-b37 Structure by X-Ray Method * A Computer Program: “Measurement of Elastic Constants of Phases in Nontextured Polycrystalline Materials by X-Ray Method” * Crystallite Sizes and Lattice Strains of Hydrogenatid Tungsten Carbid Powder * The Bragg-Case Images of Dislocations at Different Absorption * Extended X-Ray Bremsstrahlung Isochromat of Molybdenum * Size Distribution Determination of Heterogeneity Regions in Electrodeposited Metals by Saxs Method * The Possibility of the Application of the CH2I2 - Paraffin Oil Mixture as a Masking Liquid for Metal/Carrier Systems in Saxs Investigations * Investigation on Mechanical Alloying and Amorphisation Processes by the Rietveld Method * Growth of β' Phase Single Crystals of Sn-Sb Alloy * Effect of Oxygen Agglomeration on Structure of Annealed Cz-Si Single Crystal * X-Ray Investigation of Non-Uniform Stress Fields * Problem of Polytype Structures Series for Martensitic Phases of Metals and Alloys * Structure of Strain-Induced Martensite in β-CuZnAl Alloy * The Effect of Heat Treatment on the Phase Transitions in NiTiCo Shape Memory Alloy * 9R → 18R Phase Transformation in Cu-13Zn-8Al Alloy * Effect of Austenite Thermal Instability on Characteristics of Martensitic Transformation in Fe-Ni Alloys * Vacuum Annealing Study of Thin Ti Layers on High Carbon Steel Substrates * Vacuum Annealing Study of Thin Ta Layers on High Carbon Steel Substrates * Investigation of Speed of Ionic Sputtering of NiTi Alloys in Sea 02 Auger Spectrometer * Effect of Precipitation Hardening on Thermal Stability of Austenite in Fe-Ni Alloys * Structure of 18Cr-25Ni-Nb L Steel After Two Years Operation in Catalytic Tubes * Influence of Magnetic Field on Mechanical Barkhausen Effect Stress Dependence in Steel * Precipitation Structure in High Strength Aluminium Alloys * Morphology of Laser Treated Al-Zn and Al-Fe Alloys * Structure of Rapidly Solidified AlFe and AlFeNi Ribbons After Continuous Heating * X-Ray Diffractometric Investigations of Anatase—Rutile Titanium Dioxide Forms Transformation in the Presence of Some Additives * Investigations on Phase Transformation of Coprecipitated Iron-Magnesium Hydroxides * Determination of the Crystallinity of Polymer Blends by X-Ray Diffraction Method * XPD Study of the Selected Magnesium Compounds with the Expected Pharmacological Activity * Supermolecular Structure of the Nylon 6.10 Crystallized from the Melt and Its Changes During Heating * The Analysis of Substructural Parameters of PZT-Type Ferroelectric Ceramics

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.

EPICS Controlled Collimator for Controlling Beam Sizes in HIPPO

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

Napolitano, Arthur Soriano; Vogel, Sven C.

2017-08-03

Controlling the beam spot size and shape in a diffraction experiment determines the probed sample volume. The HIPPO - High-Pressure-Preferred Orientation– neutron time-offlight diffractometer is located at the Lujan Neutron Scattering Center in Los Alamos National Laboratories. HIPPO characterizes microstructural parameters, such as phase composition, strains, grain size, or texture, of bulk (cm-sized) samples. In the current setup, the beam spot has a 10 mm diameter. Using a collimator, consisting of two pairs of neutron absorbing boron-nitride slabs, horizontal and vertical dimensions of a rectangular beam spot can be defined. Using the HIPPO robotic sample changer for sample motion, themore » collimator would enable scanning of e.g. cylindrical samples along the cylinder axis by probing slices of such samples. The project presented here describes implementation of such a collimator, in particular the motion control software. We utilized the EPICS (Experimental Physics Interface and Control System) software interface to integrate the collimator control into the HIPPO instrument control system. Using EPICS, commands are sent to commercial stepper motors that move the beam windows.« less

Novel diamond cells for neutron diffraction using multi-carat CVD anvils.

PubMed

Boehler, R; Molaison, J J; Haberl, B

2017-08-01

Traditionally, neutron diffraction at high pressure has been severely limited in pressure because low neutron flux required large sample volumes and therefore large volume presses. At the high-flux Spallation Neutron Source at the Oak Ridge National Laboratory, we have developed new, large-volume diamond anvil cells for neutron diffraction. The main features of these cells are multi-carat, single crystal chemical vapor deposition diamonds, very large diffraction apertures, and gas membranes to accommodate pressure stability, especially upon cooling. A new cell has been tested for diffraction up to 40 GPa with an unprecedented sample volume of ∼0.15 mm 3 . High quality spectra were obtained in 1 h for crystalline Ni and in ∼8 h for disordered glassy carbon. These new techniques will open the way for routine megabar neutron diffraction experiments.

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

Novel diamond cells for neutron diffraction using multi-carat CVD anvils

DOE PAGES

Boehler, R.; Molaison, J. J.; Haberl, B.

2017-08-17

Traditionally, neutron diffraction at high pressure has been severely limited in pressure because low neutron flux required large sample volumes and therefore large volume presses. At the high-flux Spallation Neutron Source at the Oak Ridge National Laboratory, we have developed in this paper new, large-volume diamond anvil cells for neutron diffraction. The main features of these cells are multi-carat, single crystal chemical vapor deposition diamonds, very large diffraction apertures, and gas membranes to accommodate pressure stability, especially upon cooling. A new cell has been tested for diffraction up to 40 GPa with an unprecedented sample volume of ~0.15 mm 3.more » High quality spectra were obtained in 1 h for crystalline Ni and in ~8 h for disordered glassy carbon. Finally, these new techniques will open the way for routine megabar neutron diffraction experiments.« less

Revisiting elastic anisotropy of biotite gneiss from the Outokumpu scientific drill hole based on new texture measurements and texture-based velocity calculations

NASA Astrophysics Data System (ADS)

Wenk, H.-R.; Vasin, R. N.; Kern, H.; Matthies, S.; Vogel, S. C.; Ivankina, T. I.

2012-10-01

A sample of biotite gneiss from the Outokumpu deep drilling project in Finland was investigated by Kern et al. (2008) for crystal preferred orientation and elastic anisotropy. Considerable differences between measured acoustic velocities and velocities calculated on the basis of texture patterns were observed. Measured P-wave anisotropy was 15.1% versus a Voigt average yielding 7.9%. Here we investigate the same sample with different methods and using different averaging techniques. Analyzing time-of-flight neutron diffraction data from Dubna-SKAT and LANSCE-HIPPO diffractometers with the Rietveld technique, much stronger preferred orientation for biotite is determined, compared to conventional pole-figure analysis reported previously. The comparison reveals important differences: HIPPO has much better counting statistics but pole figure coverage is poor. SKAT has better angular resolution. Using the new preferred orientation data and applying a self-consistent averaging method that takes grain shapes into account, close agreement of calculated and measured P-wave velocities is observed (12.6%). This is further improved by adding 0.1 vol.% flat micropores parallel to the biotite platelets in the simulation (14.9%).

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.

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

PubMed

Benafan, O; Padula, S A; Skorpenske, H D; An, K; Vaidyanathan, R

2014-10-01

A gripping capability 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. The proposed capability allowed for the acquisition of neutron spectra during tension, compression, torsion, and/or complex loading paths at elevated temperatures. The design consisted of age-hardened, Inconel(®) 718 grips with direct attachment to the existing MTS load frame having axial and torsional capacities of 100 kN and 400 N·m, respectively. Internal cooling passages were incorporated into the gripping system for fast cooling rates during high temperature experiments up to ∼1000 K. The specimen mounting couplers combined a threaded and hexed end-connection for ease of sample installation/removal without introducing any unwanted loads. Instrumentation of this capability is documented in this work along with various performance parameters. The gripping system was utilized to investigate deformation in NiTi shape memory alloys under various loading/control modes (e.g., isothermal, isobaric, and cyclic), and preliminary results are presented. The measurements facilitated the quantification of the texture, internal strain, and phase fraction evolution in NiTi shape memory alloys under various loading/control modes.

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

NASA Astrophysics Data System (ADS)

Benafan, O.; Padula, S. A.; Skorpenske, H. D.; An, K.; Vaidyanathan, R.

2014-10-01

A gripping capability 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. The proposed capability allowed for the acquisition of neutron spectra during tension, compression, torsion, and/or complex loading paths at elevated temperatures. The design consisted of age-hardened, Inconel® 718 grips with direct attachment to the existing MTS load frame having axial and torsional capacities of 100 kN and 400 N.m, respectively. Internal cooling passages were incorporated into the gripping system for fast cooling rates during high temperature experiments up to ˜1000 K. The specimen mounting couplers combined a threaded and hexed end-connection for ease of sample installation/removal without introducing any unwanted loads. Instrumentation of this capability is documented in this work along with various performance parameters. The gripping system was utilized to investigate deformation in NiTi shape memory alloys under various loading/control modes (e.g., isothermal, isobaric, and cyclic), and preliminary results are presented. The measurements facilitated the quantification of the texture, internal strain, and phase fraction evolution in NiTi shape memory alloys under various loading/control modes.

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

Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

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

McGonegle, David, E-mail: d.mcgonegle1@physics.ox.ac.uk; Wark, Justin S.; Higginbotham, Andrew

2015-08-14

A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

DOE PAGES

McGonegle, David; Milathianaki, Despina; Remington, Bruce A.; ...

2015-08-11

A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. In conclusion, the simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

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.

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.

Direct evidence for the spin cycloid in strained nanoscale bismuth ferrite thin films

PubMed Central

Bertinshaw, Joel; Maran, Ronald; Callori, Sara J.; Ramesh, Vidya; Cheung, Jeffery; Danilkin, Sergey A.; Lee, Wai Tung; Hu, Songbai; Seidel, Jan; Valanoor, Nagarajan; Ulrich, Clemens

2016-01-01

Magnonic devices that utilize electric control of spin waves mediated by complex spin textures are an emerging direction in spintronics research. Room-temperature multiferroic materials, such as bismuth ferrite (BiFeO3), would be ideal candidates for this purpose. To realize magnonic devices, a robust long-range spin cycloid with well-known direction is desired, since it is a prerequisite for the magnetoelectric coupling. Despite extensive investigation, the stabilization of a large-scale uniform spin cycloid in nanoscale (100 nm) thin BiFeO3 films has not been accomplished. Here, we demonstrate cycloidal spin order in 100 nm BiFeO3 thin films through the careful choice of crystallographic orientation, and control of the electrostatic and strain boundary conditions. Neutron diffraction, in conjunction with X-ray diffraction, reveals an incommensurate spin cycloid with a unique [11] propagation direction. While this direction is different from bulk BiFeO3, the cycloid length and Néel temperature remain equivalent to bulk at room temperature. PMID:27585637

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.

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

NASA Astrophysics Data System (ADS)

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

2013-05-01

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

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

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

DOE PAGES

Aydogan, E.; El-Atwani, O.; Takajo, S.; ...

2018-02-09

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

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

Aydogan, E.; El-Atwani, O.; Takajo, S.

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

In situ neutron diffraction in quantifying deformation behaviors of nano-sized carbide strengthened UFG ferritic steel

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

Liang, J. W.; Shen, Y. F.; Zhang, C. S.

Here, the microstructures and mechanical properties of a low-alloy medium-carbon steel with a duplex microstructure composed of nanoscale spheroidized carbides in ultrafine-grained (UFG) ferritic steel are examined. The average grain size of the studied steel is ~ 430 nm, and these grains coexist with numerous carbides. Neutron diffraction reveals that the intensity of (011) and (022) peaks for the UFG sample is significantly enhanced, suggesting that the (011)//RD texture is a result of the warm rolling process. The lattice parameter of UFG steel is smaller than that of a martensitic steel (M steel) counterpart, indicating a lower carbon concentration inmore » the lattice. The estimated dislocation densities for M steel and UFG steel are 2.59 × 10 14 cm –2 and 1.76 × 10 12 cm –2, respectively. The UFG steel reveals a nearly isotropic lattice strain response under initial tension from 0 to 450 MPa, where the lattice strains of the (110), (002), and (112) planes are identical. The increase of lattice strain of the (110) plane becomes smaller than that of the (002) and (112) planes as the stress exceeds 450 MPa, suggesting that the nanosized carbides contribute to the hardening ability by promoting the accumulation of geometrically necessary dislocations around the particles, and the (110) lattice becomes harder compared to the other two planes.« less

In situ neutron diffraction in quantifying deformation behaviors of nano-sized carbide strengthened UFG ferritic steel

DOE PAGES

Liang, J. W.; Shen, Y. F.; Zhang, C. S.; ...

2018-04-25

Here, the microstructures and mechanical properties of a low-alloy medium-carbon steel with a duplex microstructure composed of nanoscale spheroidized carbides in ultrafine-grained (UFG) ferritic steel are examined. The average grain size of the studied steel is ~ 430 nm, and these grains coexist with numerous carbides. Neutron diffraction reveals that the intensity of (011) and (022) peaks for the UFG sample is significantly enhanced, suggesting that the (011)//RD texture is a result of the warm rolling process. The lattice parameter of UFG steel is smaller than that of a martensitic steel (M steel) counterpart, indicating a lower carbon concentration inmore » the lattice. The estimated dislocation densities for M steel and UFG steel are 2.59 × 10 14 cm –2 and 1.76 × 10 12 cm –2, respectively. The UFG steel reveals a nearly isotropic lattice strain response under initial tension from 0 to 450 MPa, where the lattice strains of the (110), (002), and (112) planes are identical. The increase of lattice strain of the (110) plane becomes smaller than that of the (002) and (112) planes as the stress exceeds 450 MPa, suggesting that the nanosized carbides contribute to the hardening ability by promoting the accumulation of geometrically necessary dislocations around the particles, and the (110) lattice becomes harder compared to the other two planes.« less

Characterization of beryllium deformation using in-situ x-ray diffraction

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

Magnuson, Eric Alan; Brown, Donald William; Clausen, Bjorn

2015-08-24

Beryllium’s unique mechanical properties are extremely important in a number of high performance applications. Consequently, accurate models for the mechanical behavior of beryllium are required. However, current models are not sufficiently microstructure aware to accurately predict the performance of beryllium under a range of processing and loading conditions. Previous experiments conducted using the SMARTS and HIPPO instruments at the Lujan Center(LANL), have studied the relationship between strain rate and texture development, but due to the limitations of neutron diffraction studies, it was not possible to measure the response of the material in real-time. In-situ diffraction experiments conducted at the Advancedmore » Photon Source have allowed the real time measurement of the mechanical response of compressed beryllium. Samples of pre-strained beryllium were reloaded orthogonal to their original load path to show the reorientation of already twinned grains. Additionally, the in-situ experiments allowed the real time tracking of twin evolution in beryllium strained at high rates. The data gathered during these experiments will be used in the development and validation of a new, microstructure aware model of the constitutive behavior of beryllium.« less

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.

Texture and structure contribution to low-temperature plasticity enhancement of Mg-Al-Zn-Mn Alloy MA2-1hp after ECAP and annealing

NASA Astrophysics Data System (ADS)

Serebryany, V. N.; D'yakonov, G. S.; Kopylov, V. I.; Salishchev, G. A.; Dobatkin, S. V.

2013-05-01

Equal channel angular pressing (ECAP) in magnesium alloys due to severe plastic shear deformations provides both grain refinement and the slope of the initial basal texture at 40°-50° to the pressing direction. These changes in microstructure and texture contribute to the improvement of low-temperature plasticity of the alloys. Quantitative texture X-ray diffraction analysis and diffraction of backscattered electrons are used to study the main textural and structural factors responsible for enhanced low-temperature plasticity based on the example of magnesium alloy MA2-1hp of the Mg-Al-Zn-Mn system. The possible mechanisms of deformation that lead to this positive effect are discussed.

Role of B19' martensite deformation in stabilizing two-way shape memory behavior in NiTi

DOE PAGES

Benafan, O.; Padula, S. A.; Noebe, R. D.; ...

2012-11-01

Deformation of a B19' martensitic, polycrystallineNi49.9Ti50.1 (at. %) shape memoryalloy and its influence on the magnitude and stability of the ensuing two-way shape memory effect (TWSME) was investigated by combined ex situ mechanical experimentation and in situneutron diffraction measurements at stress and temperature. The microstructural changes (texture, lattice strains, and phase fractions) during room-temperature deformation and subsequent thermal cycling were captured and compared to the bulk macroscopic response of the alloy. With increasing uniaxial strain, it was observed that B19' martensite deformed by reorientation and detwinning with preferred selection of the (1¯50) M and (010) M variants, (201¯) B19' deformationmore » twinning, and dislocation activity. These mechanisms were indicated by changes in bulk texture from the neutron diffraction measurements. Partial reversibility of the reoriented variants and deformation twins was also captured upon load removal and thermal cycling, which after isothermal deformation to strains between 6% and 22% resulted in a strong TWSME. Consequently, TWSME functional parameters including TWSME strain, strain reduction, and transformation temperatures were characterized and it was found that prior martensite deformation to 14% strain provided the optimum condition for the TWSME, resulting in a stable two-way shape memory strain of 2.2%. Thus, isothermal deformation of martensite was found to be a quick and efficient method for creating a strong and stable TWSME in Ni₄₉.₉Ti₅₀.₁.« less

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

In situ x-ray diffraction observation of multiple texture turnovers in sputtered Cr films

NASA Astrophysics Data System (ADS)

Zhao, Z. B.; Rek, Z. U.; Yalisove, S. M.; Bilello, J. C.

2004-11-01

A series of Cr films were deposited onto native oxides of (100) Si substrates via a confocal deposition geometry in a magnetron sputter chamber. The film growth chamber was incorporated with an in situ x-ray diffraction system, which allowed the collection of x-ray diffraction data on the growing film in a quasi real time fashion without interruption of film deposition. The in situ x-ray diffraction, coupled with other ex situ characterization techniques, was used to study structural evolutions of the Cr films deposited at various Ar pressures. It was observed that the evolution of the crystallographic structures of Cr films was very sensitive to both deposition conditions and film thickness. With the confocal deposition geometry, the Cr films developed various types of out-of-plane textures. In addition to the (110) and (100) types of textures commonly reported for vapor deposited Cr films, the (111) and (112) types of textures were also observed. The film deposited at low Ar pressure (2 mTorr) developed strong (111) type texture. With the increase in either Ar pressure or film thickness, the Cr films tended to develop (112) and (100) types of texture. At high Ar pressures (>10 mTorr), several changes in texture type with increasing film thickness were observed. The sequence can be described as (110)-->(112)-->(100). The strong tendency for these films to ultimately assume the (100) type of texture could be related to significant rises in substrate temperatures during the late stages of film growth with high Ar pressures. The observation of the multiple texture type changes suggests that the evolution of Cr films is controlled by complex growth kinetics. The competitive growth of grains with different orientations can be altered not only by controllable deposition parameters such as Ar pressure, but also by the variations of in situ film attributes (e.g., residual stress and substrate temperature) occurring concurrently with film growth.

Energy-dispersive neutron imaging and diffraction of magnetically driven twins in a Ni2MnGa single crystal magnetic shape memory alloy

NASA Astrophysics Data System (ADS)

Kabra, Saurabh; Kelleher, Joe; Kockelmann, Winfried; Gutmann, Matthias; Tremsin, Anton

2016-09-01

Single crystals of a partially twinned magnetic shape memory alloy, Ni2MnGa, were imaged using neutron diffraction and energy-resolved imaging techniques at the ISIS spallation neutron source. Single crystal neutron diffraction showed that the crystal produces two twin variants with a specific crystallographic relationship. Transmission images were captured using a time of flight MCP/Timepix neutron counting detector. The twinned and untwinned regions were clearly distinguishable in images corresponding to narrow-energy transmission images. Further, the spatially-resolved transmission spectra were used to elucidate the orientations of the crystallites in the different volumes of the crystal.

Texture and phase analysis of deformed SUS304 by using HIPPO

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

Takajo, Shigehiro; Vogel, Sven C.

2016-11-15

These slides represent the author's research activity at Los Alamos National Laboratory (LANL), which is about texture and phase analysis of deformed SUS304 by using HIPPO. The following topics are covered: diffraction histogram at each sample position, diffraction histogram (all bank data averaged), possiblity of ε-phase, MAUD analysis with including ε-phase.

Phase Transformation Temperatures and Solute Redistribution in a Quaternary Zirconium Alloy

NASA Astrophysics Data System (ADS)

Cochrane, C.; Daymond, M. R.

2018-05-01

This study investigates the phase stability and redistribution of solute during heating and cooling of a quaternary zirconium alloy, Excel (Zr-3.2Sn-0.8Mo-0.8Nb). Time-of-flight neutron diffraction data are analyzed using a novel Vegard's law-based approach to determine the phase fractions and location of substitutional solute atoms in situ during heating from room temperature up to 1050 °C. It is seen that this alloy exhibits direct nucleation of the β Zr phase from martensite during tempering, and stable retention of the β Zr phase to high temperatures, unlike other two-phase zirconium alloys. The transformation strains resulting from the α \\leftrightarrow β transformation are shown to have a direct impact on the development of microstructure and crystallographic texture.

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.

Fiber vs Rolling Texture: Stress State Dependence for Cold-Drawn Wire

NASA Astrophysics Data System (ADS)

Zorina, M. A.; Karabanalov, M. S.; Stepanov, S. I.; Demakov, S. L.; Loginov, Yu. N.; Lobanov, M. L.

2018-02-01

The texture of the cold-drawn copper wire was investigated along the radius using electron backscatter diffraction. The complex fiber texture of the central region of the wire was considered as the rolling texture consisting of a set of preferred orientations. The texture of the periphery region was revealed to be similar to the shear texture. The orientation-dependent properties of the wire were proven to be determined by the texture of the near-surface layers.

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.

Neutron Reflectivity and Grazing Angle Diffraction

PubMed Central

Ankner, J. F.; Majkrzak, C. F.; Satija, S. K.

1993-01-01

Over the last 10 years, neutron reflectivity has emerged as a powerful technique for the investigation of surface and interfacial phenomena in many different fields. In this paper, a short review of some of the work on neutron reflectivity and grazing-angle diffraction as well as a description of the current and planned neutron rcflectometers at NIST is presented. Specific examples of the characterization of magnetic, superconducting, and polymeric surfaces and interfaces are included. PMID:28053457

X-ray diffraction analysis of residual stresses in textured ZnO thin films

NASA Astrophysics Data System (ADS)

Dobročka, E.; Novák, P.; Búc, D.; Harmatha, L.; Murín, J.

2017-02-01

Residual stresses are commonly generated in thin films during the deposition process and can influence the film properties. Among a number of techniques developed for stress analysis, X-ray diffraction methods, especially the grazing incidence set-up, are of special importance due to their capability to analyze the stresses in very thin layers as well as to investigate the depth variation of the stresses. In this contribution a method combining multiple {hkl} and multiple χ modes of X-ray diffraction stress analysis in grazing incidence set-up is used for the measurement of residual stress in strongly textured ZnO thin films. The method improves the precision of the stress evaluation in textured samples. Because the measurements are performed at very low incidence angles, the effect of refraction of X-rays on the measured stress is analyzed in details for the general case of non-coplanar geometry. It is shown that this effect cannot be neglected if the angle of incidence approaches the critical angle. The X-ray stress factors are calculated for hexagonal fiber-textured ZnO for the Reuss model of grain-interaction and the effect of texture on the stress factors is analyzed. The texture in the layer is modelled by Gaussian distribution function. Numerical results indicate that in the process of stress evaluation the Reuss model can be replaced by much simpler crystallite group method if the standard deviation of Gaussian describing the texture is less than 6°. The results can be adapted for fiber-textured films of various hexagonal materials.

Grain Orientation Dependence of the Residual Lattice Strain in a Cold Rolled Interstitial-Free Steel

DOE PAGES

Xie, Qingge; Gorti, Sarma B.; Sidor, Jurij; ...

2018-01-10

The experimentally measured grain-orientation-dependent residual lattice strains, evolved in an interstitia-free steel after 70% cold rolling reduction, are studied by means of crystal elastic visco-plastic finite element simulations, which provides a very satisfactory prediction of deformation texture. The calculated residual lattice strain pole figure matches well with the experimentally measured counterpart within the highest density regions of major texture components observed. Both experimental evidence and results of modeling clearly indicate that the residual lattice strain is orientation dependent, based on comprehensive information on the evolution of residual lattice strain in various crystallographic orientations during plastic deformation. It appears that inmore » a cold rolled material, there is a general correlation between the stresses developed just prior to unloading and the residual lattice strains in particular directions. Here, it is also shown that the cumulative plastic shear does not reveal a clear correlation with the components of residual lattice strain while presented in the normal correlation plot, however, this relationship can be better understood by means of the orientation distribution function of residual lattice strain, which can be derived from the neutron or X-ray diffraction experiments.« less

Grain Orientation Dependence of the Residual Lattice Strain in a Cold Rolled Interstitial-Free Steel

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

Xie, Qingge; Gorti, Sarma B.; Sidor, Jurij

The experimentally measured grain-orientation-dependent residual lattice strains, evolved in an interstitia-free steel after 70% cold rolling reduction, are studied by means of crystal elastic visco-plastic finite element simulations, which provides a very satisfactory prediction of deformation texture. The calculated residual lattice strain pole figure matches well with the experimentally measured counterpart within the highest density regions of major texture components observed. Both experimental evidence and results of modeling clearly indicate that the residual lattice strain is orientation dependent, based on comprehensive information on the evolution of residual lattice strain in various crystallographic orientations during plastic deformation. It appears that inmore » a cold rolled material, there is a general correlation between the stresses developed just prior to unloading and the residual lattice strains in particular directions. Here, it is also shown that the cumulative plastic shear does not reveal a clear correlation with the components of residual lattice strain while presented in the normal correlation plot, however, this relationship can be better understood by means of the orientation distribution function of residual lattice strain, which can be derived from the neutron or X-ray diffraction experiments.« less

Diffraction in neutron imaging-A review

NASA Astrophysics Data System (ADS)

Woracek, Robin; Santisteban, Javier; Fedrigo, Anna; Strobl, Markus

2018-01-01

Neutron imaging is a highly successful experimental technique ever since adequate neutron sources were available. In general, neutron imaging is performed with a wide wavelength spectrum for best flux conditions in transmission geometry. Neutrons provide outstanding features in the penetration of many structural materials, which often makes them more suited for bulk sample studies than other forms of radiation, often in particular as they are also highly sensitive to some light elements, especially Hydrogen. In contrast to neutron scattering applications, imaging resolves macroscopic structures, nowadays down to, in the best case, below 10 micrometre, directly in real space. However, since more than a decade there is a growing number of techniques and applications in neutron imaging that - supported by powerful neutron sources - are taking advantage of wavelength resolved measurements. In this review we summarize and discuss this outstanding development and how wavelength resolved transmission neutron imaging is successfully exploiting diffraction mechanisms to access crystal structure information in the Angstrom regime, which conventionally is probed in reciprocal space by diffraction techniques. In particular the combination of information gained in real space and on crystallographic length scales makes this neutron imaging technique a valuable tool for a wide range of new applications, while it also qualifies neutron imaging to fully profit from the new generation of powerful pulsed neutron sources.

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.

Improved sample manipulation at the STRESS-SPEC neutron diffractometer using an industrial 6-axis robot for texture and strain analyses

NASA Astrophysics Data System (ADS)

Randau, C.; Brokmeier, H. G.; Gan, W. M.; Hofmann, M.; Voeller, M.; Tekouo, W.; Al-hamdany, N.; Seidl, G.; Schreyer, A.

2015-09-01

The materials science neutron diffractometer STRESS-SPEC located at FRM II is a dedicated instrument for strain and pole figure measurements. Both methods make complementary demands on sample handling. On one hand pole figure measurements need a high degree of freedom to orient small samples and on the other hand in strain investigations it is often necessary to handle large and heavy components. Therefore a robot based sample positioning system was developed, which has the capability to provide both possibilities. Based on this new robot system further developments like a full automated sample changer system for texture measurements were accomplished. Moreover this system opens the door for combined strain and texture analysis at STRESS-SPEC.

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.

High resolution neutron Larmor diffraction using superconducting magnetic Wollaston prisms

DOE PAGES

Li, Fankang; Feng, Hao; Thaler, Alexander N.; ...

2017-04-13

The neutron Larmor diffraction technique has been implemented using superconducting magnetic Wollaston prisms in both single-arm and double-arm configurations. Successful measurements of the coefficient of thermal expansion of a single-crystal copper sample demonstrates that the method works as expected. Our experiment involves a new method of tuning by varying the magnetic field configurations in the device and the tuning results agree well with previous measurements. The difference between single-arm and double-arm configurations has been investigated experimentally. Here, we conclude that this measurement benchmarks the applications of magnetic Wollaston prisms in Larmor diffraction and shows in principle that the setup canmore » be used for inelastic phonon line-width measurements. The achievable resolution for Larmor diffraction is comparable to that using Neutron Resonance Spin Echo (NRSE) coils. Furthermore, the use of superconducting materials in the prisms allows high neutron polarization and transmission efficiency to be achieved.« less

Effect of electrical and mechanical poling history on domain orientation and piezoelectric properties of soft and hard PZT ceramics

NASA Astrophysics Data System (ADS)

Marsilius, Mie; Granzow, Torsten; Jones, Jacob L.

2011-02-01

The superior piezoelectric properties of all polycrystalline ferroelectrics are based on the extent of non-180° domain wall motion under electrical and mechanical poling loads. To distinguish between 180° and non-180° domain wall motion in a soft-doped and a hard-doped lead zirconate titanate (PZT) ceramic, domain texture measurements were performed using x-ray and neutron diffraction after different loading procedures. Comparing the results to measurements of the remanent strain and piezoelectric coefficient allowed the differentiation between different microstructural contributions to the macroscopic parameters. Both types of ceramic showed similar behavior under electric field, but the hard-doped material was more susceptible to mechanical load. A considerable fraction of the piezoelectric coefficient originated from poling by the preferred orientation of 180° domains.

Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

NASA Technical Reports Server (NTRS)

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

2002-01-01

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

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

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

Chandran, Ravi

In this research, phase transitions in the bulk electrodes for Li-ion batteries were investigated using neutron diffraction (ND) as well as neutron imaging techniques. The objectives of this research is to design of a novel in situ electrochemical cell to obtain Rietveld refinable neutron diffraction experiments using small volume electrodes of various laboratory/research-scale electrodes intended for Li-ion batteries. This cell is also to be used to investigate the complexity of phase transitions in Li(Mg) alloy electrodes, either by diffraction or by neutron imaging, which occur under electrochemical lithiation and delithiation, and to determine aspects of phase transition that enable/limit energymore » storage capacity. Additional objective is to investigate the phase transitions in electrodes made of etched micro-columns of silicon and investigate the effect of particle/column size on phase transitions and nonequilibrium structures. An in situ electrochemical cell was designed successfully and was used to study the phase transitions under in-situ neutron diffraction in both the electrodes (anode/cathode) simultaneously in graphite/LiCoO 2 and in graphite/LiMn 2O 4 cells each with two cells. The diffraction patterns fully validated the working of the in situ cell. Additional experimental were performed using the Si micro-columnar electrodes. The results revealed new lithiation phenomena, as evidenced by mosaicity formation in silicon electrode. These experiments were performed in Vulcan diffractometer at SNS, Oak Ridge National Laboratory. In parallel, the spatial distribution of Li during lithiation and delithiation processes in Li-battery electrodes were investigated. For this purpose, neutron tomographic imaging technique has been used for 3D mapping of Li distribution in bulk Li(Mg) alloy electrodes. It was possible to observe the phase boundary of Li(Mg) alloy indicating phase transition from Li-rich BCC β-phase to Li-lean α-phase. These experiments have been performed at CG-1D Neutron Imaging Prototype Station at SNS.« less

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

Investigation of dissimilar metal welds by energy-resolved neutron imaging.

PubMed

Tremsin, Anton S; Ganguly, Supriyo; Meco, Sonia M; Pardal, Goncalo R; Shinohara, Takenao; Feller, W Bruce

2016-08-01

A nondestructive study of the internal structure and compositional gradient of dissimilar metal-alloy welds through energy-resolved neutron imaging is described in this paper. The ability of neutrons to penetrate thick metal objects (up to several cm) provides a unique possibility to examine samples which are opaque to other conventional techniques. The presence of Bragg edges in the measured neutron transmission spectra can be used to characterize the internal residual strain within the samples and some microstructural features, e.g. texture within the grains, while neutron resonance absorption provides the possibility to map the degree of uniformity in mixing of the participating alloys and intermetallic formation within the welds. In addition, voids and other defects can be revealed by the variation of neutron attenuation across the samples. This paper demonstrates the potential of neutron energy-resolved imaging to measure all these characteristics simultaneously in a single experiment with sub-mm spatial resolution. Two dissimilar alloy welds are used in this study: Al autogenously laser welded to steel, and Ti gas metal arc welded (GMAW) to stainless steel using Cu as a filler alloy. The cold metal transfer variant of the GMAW process was used in joining the Ti to the stainless steel in order to minimize the heat input. The distributions of the lattice parameter and texture variation in these welds as well as the presence of voids and defects in the melt region are mapped across the welds. The depth of the thermal front in the Al-steel weld is clearly resolved and could be used to optimize the welding process. A highly textured structure is revealed in the Ti to stainless steel joint where copper was used as a filler wire. The limited diffusion of Ti into the weld region is also verified by the resonance absorption.

Influence of warm rolling temperature on ferrite recrystallization in low C and IF steels

NASA Astrophysics Data System (ADS)

Barnett, Matthew Robert

Experiments involving single pass laboratory rolling and isothermal salt bath annealing were carried out; three steels were studied: a titanium stabilized interstitial free grade and two low carbon grades, one of which contained a particularly low level of manganese (˜0.009wt.%). The two low carbon grades were produced such that any complication from AlN precipitation was avoided. X-ray, neutron diffraction, optical metallography and mechanical testing measurements were carried out on the samples before and after annealing. The main aim of this work was to further the understanding of the metallurgy of recrystallization after ferrite rolling at temperatures between room temperature and 700sp°C. Deformation textures, recrystallization kinetics, final grain sizes and recrystallization textures were quantified for all the samples and experimental conditions. A major conclusion based on these data is that the influence of rolling temperature is far greater in the low carbon samples than in the IF grade. Indeed, the IF results alter only marginally with increasing temperature. In the low carbon grades, however, the rolling texture sharpens, recrystallization slows, the final grain size coarsens, and the recrystallization texture changes when the rolling temperature is increased. This distinct difference between the two steel types is explained in terms of their contrasting deformation behaviors. Solute carbon and nitrogen in the low carbon grades interact with dislocations causing high stored energy levels after low temperature rolling (due to dynamic strain aging) and high strain rate sensitivities during high temperature rolling (due to the solute drag of dislocations in the transition region between DSA and DRC). Nucleation during subsequent recrystallization is strongly influenced by both the stored energy and the strain rate sensitivity. The latter affects the occurrence of the flow localisations that enhance nucleation.

Structures having enhanced biaxial texture

DOEpatents

Goyal, Amit; Budai, John D.; Kroeger, Donald M.; Norton, David P.; Specht, Eliot D.; Christen, David K.

1999-01-01

A biaxially textured alloy article includes a rolled and annealed biaxially textured base metal substrate characterized by an x-ray diffraction phi scan peak of no more than 20.degree. FWHM; and a biaxially textured layer of an alloy or another material on a surface thereof. The article further includes at least one of an electromagnetic device or an electro-optical device epitaxially joined to the alloy.

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.

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.

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.

New Process for the Goss Texture Formation and Magnetic Property in Silicon Steel Sheet by Hot Asymmetric Rolling and Annealing

NASA Astrophysics Data System (ADS)

Nam, Su Kwon; Kim, Gwang-Hee; Lee, Dong Nyung; Kim, Insoo

2018-03-01

The shear deformation texture of bcc metals is characterized by the Goss orientation, or {110}<001>, which is a highly useful orientation for grain-oriented silicon steels because it gives rise to high magnetic permeability along the <100> direction. To obtain the Goss texture, or {110}<001>, in silicon steel sheets, a silicon steel sheet was subjected to an 89 pct reduction in thickness via asymmetric rolling at 750 °C. This step resulted in the well-developed Goss texture. When multiple asymmetrically rolled steel sheets were subsequently annealed, one at 900 °C for 1 hour and the other at 1200 °C for a short period of 5 minutes in a box furnace with air atmosphere, a strong Goss texture was developed in the silicon steel sheets. The texture was measured via X-ray diffraction and electron backscatter diffraction. The magnetization curve of each specimen was measured by the vibrating sample magnetometer and the measured magnetization curve showed the typical soft magnetic characteristics.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

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).

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.

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.

Microstructure and Crystallographic Texture Evolution During the Friction-Stir Processing of a Precipitation-Hardenable Aluminum Alloy

NASA Astrophysics Data System (ADS)

Nadammal, Naresh; Kailas, Satish V.; Szpunar, Jerzy; Suwas, Satyam

2015-05-01

Friction-stir processing (FSP) has been proven as a successful method for the grain refinement of high-strength aluminum alloys. The most important attributes of this process are the fine-grain microstructure and characteristic texture, which impart suitable properties in the as-processed material. In the current work, FSP of the precipitation-hardenable aluminum alloy 2219 has been carried out and the consequent evolution of microstructure and texture has been studied. The as-processed materials were characterized using electron back-scattered diffraction, x-ray diffraction, and electron probe microanalysis. Onion-ring formation was observed in the nugget zone, which has been found to be related to the precipitation response and crystallographic texture of the alloy. Texture development in the alloy has been attributed to the combined effect of shear deformation and dynamic recrystallization. The texture was found heterogeneous even within the nugget zone. A microtexture analysis revealed the dominance of shear texture components, with C component at the top of nugget zone and the B and A2* components in the middle and bottom. The bulk texture measurement in the nugget zone revealed a dominant C component. The development of a weaker texture along with the presence of some large particles in the nugget zone indicates particle-stimulated nucleation as the dominant nucleation mechanism during FSP. Grain growth follows the Burke and Turnbull mechanism and geometrical coalescence.

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

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.

Measuring and Modeling the Effects of Mechanical Twinning on the Behavior of Magnesium Alloys

NASA Astrophysics Data System (ADS)

Agnew, Sean; Wu, Peidong; Inal, Kaan; El Kadiri, Haitham; Wang, Jian; Tome, Carlos

Our community has learned a great deal about twinning in Mg alloys over the past decade. Some of these things were known qualitatively in prior decades, but we have now developed a proficiency in characterization and computational modeling which permits a quantitative description of these twinning-induced effects over a wide range of strain rates, temperatures, loading conditions, and in a variety of alloy families. These capabilities could only be dreamed of by prior generations. This lecture will review the effects of the main twinning mode, {10.2} extension twinning (e.g., tension-compression yield asymmetry, yield plateau, anisotropy, rapid strain hardening, detwinning, etc.); characterization, primarily by diffraction-based techniques (electron, X-ray, and neutron); and modeling by crystal plasticity-based methods. Strategies to control these effects through microstructure, texture, and alloy design will be proposed. Finally, outstanding questions which merit further research will be highlighted.

Gradual pressure-induced change in the magnetic structure of the noncollinear antiferromagnet Mn3Ge

NASA Astrophysics Data System (ADS)

Sukhanov, A. S.; Singh, Sanjay; Caron, L.; Hansen, Th.; Hoser, A.; Kumar, V.; Borrmann, H.; Fitch, A.; Devi, P.; Manna, K.; Felser, C.; Inosov, D. S.

2018-06-01

By means of powder neutron diffraction we investigate changes in the magnetic structure of the coplanar noncollinear antiferromagnet Mn3Ge caused by an application of hydrostatic pressure up to 5 GPa. At ambient conditions the kagomé layers of Mn atoms in Mn3Ge order in a triangular 120∘ spin structure. Under high pressure the spins acquire a uniform out-of-plane canting, gradually transforming the magnetic texture to a noncoplanar configuration. With increasing pressure the canted structure fully transforms into the collinear ferromagnetic one. We observed that magnetic order is accompanied by a noticeable magnetoelastic effect, namely, spontaneous magnetostriction. The latter induces an in-plane magnetostrain of the hexagonal unit cell at ambient pressure and flips to an out-of-plane strain at high pressures in accordance with the change of the magnetic structure.

Carrier density control of magnetism and Berry phases in doped EuTiO3

NASA Astrophysics Data System (ADS)

Ahadi, Kaveh; Gui, Zhigang; Porter, Zach; Lynn, Jeffrey W.; Xu, Zhijun; Wilson, Stephen D.; Janotti, Anderson; Stemmer, Susanne

2018-05-01

In materials with broken time-reversal symmetry, the Berry curvature acts as a reciprocal space magnetic field on the conduction electrons and is a significant contribution to the magnetotransport properties, including the intrinsic anomalous Hall effect. Here, we report neutron diffraction, transport, and magnetization measurements of thin films of doped EuTiO3, an itinerant magnetic material, as a function of carrier density and magnetic field. These films are itinerant antiferromagnets at all doping concentrations. At low carrier densities, the magnetoresistance indicates a metamagnetic transition, which is absent at high carrier densities (>6 × 1020 cm-3). Strikingly, the crossover coincides with a sign change in the spontaneous Hall effects, indicating a sign change in the Berry curvature. We discuss the results in the context of the band structure topology and its coupling to the magnetic texture.

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.

Characterization of Tubing from Advanced ODS alloy (FCRD-NFA1)

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

Maloy, Stuart Andrew; Aydogan, Eda; Anderoglu, Osman

2016-09-20

Fabrication methods are being developed and tested for producing fuel clad tubing of the advanced ODS 14YWT and FCRD-NFA1 ferritic alloys. Three fabrication methods were based on plastically deforming a machined thick-wall tube sample of the ODS alloys by pilgering, hydrostatic extrusion or drawing to decrease the outer diameter and wall thickness and increase the length of the final tube. The fourth fabrication method consisted of the additive manufacturing approach involving solid-state spray deposition (SSSD) of ball milled and annealed powder of 14YWT for producing thin-wall tubes. Of the four fabrication methods, two methods were successful at producing tubing formore » further characterization: production of tubing by high-velocity oxy-fuel spray forming and production of tubing using high-temperature hydrostatic extrusion. The characterization described shows through neutron diffraction the texture produced during extrusion while maintaining the beneficial oxide dispersion. In this research, the parameters for innovative thermal spray deposition and hot extrusion processing methods have been developed to produce the final nanostructured ferritic alloy (NFA) tubes having approximately 0.5 mm wall thickness. Effect of different processing routes on texture and grain boundary characteristics has been investigated. It was found that hydrostatic extrusion results in combination of plane strain and shear deformations which generate rolling textures of α- and γ-fibers on {001}<110> and {111}<110> together with a shear texture of ζ-fiber on {011}<211> and {011}<011>. On the other hand, multi-step plane strain deformation in cross directions leads to a strong rolling textures of θ- and ε-fiber on {001}<110> together with weak γ-fiber on {111}<112>. Even though the amount of the equivalent strain is similar, shear deformation leads to much lower texture indexes compared to the plane strain deformations. Moreover, while 50% of hot rolling brings about a large number of high-angle grain boundaries (HAB), 44% of shear deformation results in large amount of low-angle boundaries (LAB) showing the incomplete recrystallization.« less

Bone structure studies with holographic interferometric nondestructive testing and x-ray methods

NASA Astrophysics Data System (ADS)

Silvennoinen, Raimo; Nygren, Kaarlo; Rouvinen, Juha; Petrova, Valentina V.

1994-02-01

Changes in the biomechanics and in the molecular texture and structure of isolated radioulnar bones of subadult European moose (Alces alces L.) collected in various environmentally polluted areas of Finland were investigated by means of holographic interferometric non- destructive testing (HNDT), radiological, morphometrical, and x-ray diffraction methods. By means of small caudal-cranial bending forces, the surface movements of the lower end (distal epiphysis) of the radial bone were recorded with the HNDT method. To study bone molecular texture and structure changes under external compressing forces, the samples for x-ray diffraction analysis were taken from the upper end of the ulnar bone (olecranon tip). Results showed that the bones obtained from the Harjavalta area and those of North Karelian moose showing malnutrition and healing femoral fractures produced different HNDT pictures compared with the four normally developed North Karelian moose. In the x-ray diffraction, the Harjavalta samples showed changes in molecular texture and structure compared with the samples from the apparently normal North Karelian animals.

Microstructure, microtexture and precipitation in the ultrafine-grained surface layer of an Al-Zn-Mg-Cu alloy processed by sliding friction treatment

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

Chen, Yanxia

2017-01-15

Precipitate redistribution and texture evolution are usually two concurrent aspects accompanying grain refinement induced by various surface treatment. However, the detailed precipitate redistribution characteristics and process, as well as crystallographic texture in the surface refined grain layer, are still far from full understanding. In this study, we focused on the microstructural and crystallographic features of the sliding friction treatment (SFT) induced surface deformation layer in a 7050 aluminum alloy. With the combination of transmission electron microscopy (TEM) and high angle angular dark field scanning TEM (HAADF-STEM) observations, a surface ultrafine grain (UFG) layer composed of both equiaxed and lamellar ultrafinemore » grains and decorated by high density of coarse grain boundary precipitates (GBPs) were revealed. Further precession electron diffraction (PED) assisted orientation mapping unraveled that high angle grain boundaries rather than low angle grain boundaries are the most favorable nucleation sites for GBPs. The prominent precipitate redistribution can be divided into three successive and interrelated stages, i.e. the mechanically induced precipitate dissolution, solute diffusion and reprecipitation. The quantitative prediction based on pipe diffusion along dislocations and grain boundary diffusion proved the distribution feasibility of GBPs around UFGs. Based on PED and electron backscatter diffraction (EBSD) analyses, the crystallographic texture of the surface UFG layer was identified as a shear texture composed of major rotated cube texture (001) 〈110〉 and minor (111) 〈112〉, while that of the adjoining lamellar coarse grained matrix was pure brass. The SFT induced surface severe shear deformation is responsible for texture evolution. - Highlights: •The surface ultrafine grain layer in a 7050 aluminum alloy was focused. •Precipitate redistribution and texture evolution were discussed. •The quantitative prediction proved the distribution feasibility of GBPs. •Precession electron diffraction orientation mapping showed a shear texture.« less

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.

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.

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.

Texture measurement of shaped material by impulse acoustic microscopy

PubMed

Eyraud; Nadal; Gondard

2000-03-01

All the microstructural parameters involved in metallurgical processes are difficult to determine directly on a shaped material. The aim of this paper is to use an impulse line-focus acoustic microscope (LFAM) as a non-destructive alternative to X-ray diffraction for measuring texture of slightly anisotropic materials. We apply it to characterize the rolling and annealing texture for tantalum sheets.

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.

Efficient optical analysis of surface texture combinations for silicon solar cells

NASA Astrophysics Data System (ADS)

Tucher, Nico; Eisenlohr, Johannes; Kiefel, Peter; Gebrewold, Habtamu; Höhn, Oliver; Hauser, Hubert; Müller, Claas; Goldschmidt, Jan Christoph; Bläsi, Benedikt

2016-04-01

Surface textures can significantly improve anti-reflective and light trapping properties of silicon solar cells. Combining standard pyramidal front side textures with scattering or diffractive rear side textures has the potential to further increase the light path length inside the silicon and thereby increase the solar cell efficiency. In this work we introduce the OPTOS (Optical Properties of Textured Optical Sheets) simulation formalism and apply it to the modelling of silicon solar cells with different surface textures at front and rear side. OPTOS is a matrix-based method that allows for the computationally-efficient calculation of non-coherent light propagation within textured solar cells, featuring multiple textures that may operate in different optical regimes. After calculating redistribution matrices for each individual surface texture with the most appropriate technique, optical properties like angle dependent reflectance, transmittance or absorptance can be determined via matrix multiplications. Using OPTOS, we demonstrate for example that the integration of a diffractive grating at the rear side of solar cells with random pyramids at the front results in an absorptance gain that corresponds to a photocurrent density enhancement of 0.73 mA/cm2 for a 250 μm thick cell. The re-usability of matrices enables the investigation of different solar cell thicknesses within minutes. For thicknesses down to 50 μm the simulated gain increases up to 1.22 mA/cm2. The OPTOS formalism is furthermore not restricted with respect to the number of textured interfaces. By combining two or more textured sheets to effective interfaces, it is possible to optically model a complete photovoltaic module including EVA and potentially textured glass layers with one calculation tool.

Effect of wheel speed and annealing temperature on microstructure and texture evolution of Ni{sub 45}Mn{sub 36.6}In{sub 13.4}Co{sub 5} ribbon

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

Feng, Yan, E-mail: yanfeng@nwpu.edu.cn

Ni{sub 45}Mn{sub 36.6}In{sub 13.4}Co{sub 5} magnetic shape memory alloy was successfully produced as preferentially textured ribbon by melting spinning with different wheel speed. X-ray diffraction (XRD) and electron back scatter diffraction (EBSD) were used to study structure and texture evolution of these melt-spun ribbons. The thickness of melt-spun ribbon is 42 μm, 65 μm and 30 μm depending on wheel speed of 1 0 m/s, 15 m/s and 20 m/s, respectively. Density of α fiber texture (〈100〉//ND) vary with wheel speed changes, and is most intensive in the ribbon with wheel speed of 15 m/s. Grains of the ribbons growmore » after being annealed at 873 K, 973 K, 1073 K and 1173 K, recrystallization was not observed in ribbons after being annealed at 873 K but occurred in ribbons after being annealed at higher temperatures. The α fiber texture becomes weaker to some extent after annealing at different temperatures, due to new recrystallization texture formed at the process of annealing. - Highlights: •Sectional part of shape memory ribbon is firstly investigated by EBSD method. •Thickness and texture of ribbons vary with wheel speed. •Annealing temperature affect texture and microstructure evolution greatly. •Recrystallization textures were observed in ribbons after being annealed.« less

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.

Investigation of dissimilar metal welds by energy-resolved neutron imaging

DOE PAGES

Tremsin, Anton S.; Ganguly, Supriyo; Meco, Sonia M.; ...

2016-06-09

A nondestructive study of the internal structure and compositional gradient of dissimilar metal-alloy welds through energy-resolved neutron imaging is described in this paper. The ability of neutrons to penetrate thick metal objects (up to several cm) provides a unique possibility to examine samples which are opaque to other conventional techniques. The presence of Bragg edges in the measured neutron transmission spectra can be used to characterize the internal residual strain within the samples and some microstructural features, e.g. texture within the grains, while neutron resonance absorption provides the possibility to map the degree of uniformity in mixing of the participatingmore » alloys and intermetallic formation within the welds. In addition, voids and other defects can be revealed by the variation of neutron attenuation across the samples. This paper demonstrates the potential of neutron energy-resolved imaging to measure all these characteristics simultaneously in a single experiment with sub-mm spatial resolution. Two dissimilar alloy welds are used in this study: Al autogenously laser welded to steel, and Ti gas metal arc welded (GMAW) to stainless steel using Cu as a filler alloy. The cold metal transfer variant of the GMAW process was used in joining the Ti to the stainless steel in order to minimize the heat input. The distributions of the lattice parameter and texture variation in these welds as well as the presence of voids and defects in the melt region are mapped across the welds. The depth of the thermal front in the Al–steel weld is clearly resolved and could be used to optimize the welding process. As a result, a highly textured structure is revealed in the Ti to stainless steel joint where copper was used as a filler wire. The limited diffusion of Ti into the weld region is also verified by the resonance absorption.« less

Investigation of dissimilar metal welds by energy-resolved neutron imaging

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

Tremsin, Anton S.; Ganguly, Supriyo; Meco, Sonia M.

A nondestructive study of the internal structure and compositional gradient of dissimilar metal-alloy welds through energy-resolved neutron imaging is described in this paper. The ability of neutrons to penetrate thick metal objects (up to several cm) provides a unique possibility to examine samples which are opaque to other conventional techniques. The presence of Bragg edges in the measured neutron transmission spectra can be used to characterize the internal residual strain within the samples and some microstructural features, e.g. texture within the grains, while neutron resonance absorption provides the possibility to map the degree of uniformity in mixing of the participatingmore » alloys and intermetallic formation within the welds. In addition, voids and other defects can be revealed by the variation of neutron attenuation across the samples. This paper demonstrates the potential of neutron energy-resolved imaging to measure all these characteristics simultaneously in a single experiment with sub-mm spatial resolution. Two dissimilar alloy welds are used in this study: Al autogenously laser welded to steel, and Ti gas metal arc welded (GMAW) to stainless steel using Cu as a filler alloy. The cold metal transfer variant of the GMAW process was used in joining the Ti to the stainless steel in order to minimize the heat input. The distributions of the lattice parameter and texture variation in these welds as well as the presence of voids and defects in the melt region are mapped across the welds. The depth of the thermal front in the Al–steel weld is clearly resolved and could be used to optimize the welding process. As a result, a highly textured structure is revealed in the Ti to stainless steel joint where copper was used as a filler wire. The limited diffusion of Ti into the weld region is also verified by the resonance absorption.« less

Investigation of dissimilar metal welds by energy-resolved neutron imaging

PubMed Central

Tremsin, Anton S.; Ganguly, Supriyo; Meco, Sonia M.; Pardal, Goncalo R.; Shinohara, Takenao; Feller, W. Bruce

2016-01-01

A nondestructive study of the internal structure and compositional gradient of dissimilar metal-alloy welds through energy-resolved neutron imaging is described in this paper. The ability of neutrons to penetrate thick metal objects (up to several cm) provides a unique possibility to examine samples which are opaque to other conventional techniques. The presence of Bragg edges in the measured neutron transmission spectra can be used to characterize the internal residual strain within the samples and some microstructural features, e.g. texture within the grains, while neutron resonance absorption provides the possibility to map the degree of uniformity in mixing of the participating alloys and intermetallic formation within the welds. In addition, voids and other defects can be revealed by the variation of neutron attenuation across the samples. This paper demonstrates the potential of neutron energy-resolved imaging to measure all these characteristics simultaneously in a single experiment with sub-mm spatial resolution. Two dissimilar alloy welds are used in this study: Al autogenously laser welded to steel, and Ti gas metal arc welded (GMAW) to stainless steel using Cu as a filler alloy. The cold metal transfer variant of the GMAW process was used in joining the Ti to the stainless steel in order to minimize the heat input. The distributions of the lattice parameter and texture variation in these welds as well as the presence of voids and defects in the melt region are mapped across the welds. The depth of the thermal front in the Al–steel weld is clearly resolved and could be used to optimize the welding process. A highly textured structure is revealed in the Ti to stainless steel joint where copper was used as a filler wire. The limited diffusion of Ti into the weld region is also verified by the resonance absorption. PMID:27504075

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

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

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

Christien, F., E-mail: frederic.christien@univ-nantes.fr; Telling, M.T.F.; Department of Materials, University of Oxford, Parks Road, Oxford

2013-08-15

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

Dislocation structure in textured zirconium tensile-deformed along rolling and transverse directions determined by X-ray diffraction line profile analysis

NASA Astrophysics Data System (ADS)

Fan, Zhijian; Jóni, Bertalan; Xie, Lei; Ribárik, Gábor; Ungár, Tamás

2018-04-01

Specimens of cold-rolled zirconium were tensile-deformed along the rolling (RD) and the transverse (TD) directions. The stress-strain curves revealed a strong texture dependence. High resolution X-ray line profile analysis was used to determine the prevailing active slip-systems in the specimens with different textures. The reflections in the X-ray diffraction patterns were separated into two groups. One group corresponds to the major and the other group to the random texture component, respectively. The dislocation densities, the subgrain size and the prevailing active slip-systems were evaluated by using the convolutional multiple whole profile (CMWP) procedure. These microstructure parameters were evaluated separately in the two groups of reflections corresponding to the two different texture components. Significant differences were found in both, the evolution of dislocation densities and the development of the fractions of and type slip systems in the RD and TD specimens during tensile deformation. The differences between the RD and TD stress-strain curves are discussed in terms of the differences of the microstructure evolution.

Crystallographic texture and earing behavior analysis for different second cold reductions of double-reduction tinplate

NASA Astrophysics Data System (ADS)

Liao, Lu-hai; Zheng, Xiao-fei; Kang, Yong-lin; Liu, Wei; Yan, Yan; Mo, Zhi-ying

2018-06-01

Since the production of tinplate with non-earing properties is difficult, especially when it is produced via the double-reduction process, the optimal degree of second cold reduction is particularly important for achieving desirable drawing properties. The evolution of texture and the earing propensity of double-reduction tinplate with different extents of second reduction were investigated in this study. Optical microscopy and scanning electron microscopy were used to observe the changes in the microstructure at various extents of reduction. Two common testing methods, X-ray diffraction (XRD) and electron backscatter diffraction, were used to investigate the texture of the specimens, which revealed the effects of deformation percentage on the final texture development and the change in the grain boundary. The earing rate was determined via earing tests involving measurement of the height of any ear. The results obtained from both XRD analyses and earing tests revealed the same ideal value for the second cold reduction on the basis of the relationship between crystallographic texture and the degree of earing.

Relationships Between the Phase Transformation Kinetics, Texture Evolution, and Microstructure Development in a 304L Stainless Steel Under Biaxial Loading Conditions: Synchrotron X-ray and Electron Backscatter Diffraction Studies

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

Cakmak, Ercan; Choo, Hahn; Kang, Jun-Yun

2015-02-11

The relationships between the martensitic phase transformation kinetics, texture evolution, and the microstructure development in the parent austenite phase were studied for a 304L stainless steel that exhibits the transformation-induced plasticity effect under biaxial loading conditions at ambient temperature. The applied loading paths included: pure torsion, simultaneous biaxial torsion/tension, simultaneous biaxial torsion/compression, and stepwise loading of tension followed by torsion (i.e., first loading by uniaxial tension and then by pure torsion in sequence). Synchrotron X-ray and electron backscatter diffraction techniques were used to measure the evolution of the phase fractions, textures, and microstructures as a function of the applied strains.more » The influence of loading character and path on the changes in martensitic phase transformation kinetics is discussed in the context of (1) texture-transformation relationship and the preferred transformation of grains belonging to certain texture components over the others, (2) effects of axial strains on shear band evolutions, and (3) volume changes associated with martensitic transformation.« less

Deformation Behavior and TExture Evolution of Steel Alloys under Axial-Torsional Loading

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

Siriruk, A.; Kant, M.; Penumadu, D.

2011-06-01

Using hollow cylinder samples with suitable geometry obtained from round bar stock, the deformation behavior of bcc Fe based 12L14 steel alloy is evaluated under multi-axial conditions. A stacked strain gage rosette and extensometer mounted on the cylindrical surface at the mid height of the specimen provided strain tensor as a function of applied stress for pure tensile and torsion tests prior to yielding. This study examines elastic and yield behavior and effects of these with respect to texture evolution. Hollow cylinder specimen geometry (tubes) with small wall thickness and relatively (to its thickness) large inner diameter is used. Themore » variation of observed yield surface in deviatoric plane and the effect on mode of deformation (tension versus torsion versus its combination) on stress-strain behavior is discussed. Bulk texture was studied using neutron time-of-flight diffractometer at High-Pressure-Preferred Orientation (HIPPO) - Los Alamos Neutron Science Center (LANSCE) instrument and the evolution of texture and related anisotropy for pure tension versus torsion are also included.« 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 .

Calculation of Debye-Scherrer diffraction patterns from highly stressed polycrystalline materials

DOE PAGES

MacDonald, M. J.; Vorberger, J.; Gamboa, E. J.; ...

2016-06-07

Calculations of Debye-Scherrer diffraction patterns from polycrystalline materials have typically been done in the limit of small deviatoric stresses. Although these methods are well suited for experiments conducted near hydrostatic conditions, more robust models are required to diagnose the large strain anisotropies present in dynamic compression experiments. A method to predict Debye-Scherrer diffraction patterns for arbitrary strains has been presented in the Voigt (iso-strain) limit. Here, we present a method to calculate Debye-Scherrer diffraction patterns from highly stressed polycrystalline samples in the Reuss (iso-stress) limit. This analysis uses elastic constants to calculate lattice strains for all initial crystallite orientations, enablingmore » elastic anisotropy and sample texture effects to be modeled directly. Furthermore, the effects of probing geometry, deviatoric stresses, and sample texture are demonstrated and compared to Voigt limit predictions. An example of shock-compressed polycrystalline diamond is presented to illustrate how this model can be applied and demonstrates the importance of including material strength when interpreting diffraction in dynamic compression experiments.« less

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

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.

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.

Low temperature texture development in Nd2Fe14B/α-Fe nanocomposite magnets via equal channel angular pressing

NASA Astrophysics Data System (ADS)

Besley, L.; Garitaonandia, J. S.; Molotnikov, A.; Kishimoto, H.; Kato, A.; Davies, C.; Suzuki, K.

2018-05-01

While suitable texture has been developed in Nd2Fe14B/α-Fe nanocomposites via thermomechanical processing methods such as die upsetting by incorporating low melting point eutectic Nd-Cu additives, significant grain coarsening occurs during this process due to the high temperature and long timescales involved, resulting in a loss of exchange coupling. Equal channel angular pressing (ECAP) is a severe plastic deformation technique which has been successfully used to produce a suitable texture in single-phase Nd2Fe14B at temperatures on the order of 500°C while preserving grain sizes on the order of 20-30nm. We investigate the development of texture in a commercial Nd2Fe14B/α-Fe nanocomposite alloy with added Nd90Cu10 produced via ECAP and then characterise it using texture x-ray diffraction and magnetic measurements. It is found that initial texture can be developed in this nanocomposite system at T = 520°C via ECAP. The average grain size of Nd2Fe14B as measured via X-ray diffraction after ECAP remains below 50nm with a developed texture. The effect of varying the amount of Nd90Cu10 additive is also investigated. It is found that with decreasing Nd90Cu10, the degree of texture is reduced while the volume fraction of α-Fe increases. This work demonstrates the development of texture in nanocomposite Nd2Fe14B/α-Fe with Nd-Cu additives whilst maintaining a grain size of approximately 50nm.

Cube texture formation during the early stages of recrystallization of Al-1%wt.Mn and AA1050 aluminium alloys

NASA Astrophysics Data System (ADS)

Miszczyk, M. M.; Paul, H.

2015-08-01

The cube texture formation during primary recrystallization was analysed in plane strain deformed samples of a commercial AA1050 alloy and an Al-1%wt.Mn model alloy single crystal of the Goss{110}<001> orientation. The textures were measured with the use of X-ray diffraction and scanning electron microscopy equipped with an electron backscattered diffraction facility. After recrystallization of the Al-1%wt.Mn single crystal, the texture of the recrystallized grains was dominated by four variants of the S{123}<634> orientation. The cube grains were only sporadically detected by the SEM/EBSD system. Nevertheless, an increased density of <111> poles corresponding to the cube orientation was observed. The latter was connected with the superposition of four variants of the S{123}<634> orientation. This indicates that the cube texture after the recrystallization was a ‘compromise texture’. In the case of the recrystallized AA1050 alloy, the strong cube texture results from both the increased density of the particular <111> poles of the four variants of the S orientation and the ∼40°(∼< 111>)-type rotation. The first mechanism transforms the Sdef-oriented areas into Srex ones, whereas the second the near S-oriented, as-deformed areas into near cube-oriented grains.

Effects of high temperature and film thicknesses on the texture evolution in Ag thin films

NASA Astrophysics Data System (ADS)

Eshaghi, F.; Zolanvari, A.

2017-04-01

In situ high-temperature X-ray diffraction techniques were used to study the effect of high temperatures (up to 600°C) on the texture evolution in silver thin films. Ag thin films with different thicknesses of 40, 80, 120 and 160nm were sputtered on the Si(100) substrates at room temperature. Then, microstructure of thin films was determined using X-ray diffraction. To investigate the influence of temperature on the texture development in the Ag thin films with different thicknesses, (111), (200) and (220) pole figures were evaluated and orientation distribution functions were calculated. Minimizing the total energy of the system which is affected by competition between surface and elastic strain energy was a key factor in the as-deposited and post annealed thin films. Since sputtering depositions was performed at room temperature and at the same thermodynamic conditions, the competition growth caused the formation of the {122} < uvw \\rangle weak fiber texture in as-deposited Ag thin films. It was significantly observed that the post annealed Ag thin films showed {111} < uvw \\rangle orientations as their preferred orientations, but their preferred fiber texture varied with the thickness of thin films. Increasing thin film thickness from 40nm to 160nm led to decreasing the intensity of the {111} < uvw \\rangle fiber texture.

Elasticity study of textured barium strontium titanate thin films by X-ray diffraction and laser acoustic waves

NASA Astrophysics Data System (ADS)

Chaabani, Anouar; Njeh, Anouar; Donner, Wolfgang; Klein, Andreas; Hédi Ben Ghozlen, Mohamed

2017-05-01

Ba0.65Sr0.35TiO3 (BST) thin films of 300 nm were deposited on Pt(111)/TiO2/SiO2/Si(001) substrates by radio frequency magnetron sputtering. Two thin films with different (111) and (001) fiber textures were prepared. X-ray diffraction was applied to measure texture. The raw pole figure data were further processed using the MTEX quantitative texture analysis software for plotting pole figures and calculating elastic constants and Young’s modulus from the orientation distribution function (ODF) for each type of textured fiber. The calculated elastic constants were used in the theoretical studies of surface acoustics waves (SAW) propagating in two types of multilayered BST systems. Theoretical dispersion curves were plotted by the application of the ordinary differential equation (ODE) and the stiffness matrix methods (SMM). A laser acoustic waves (LAW) technique was applied to generate surface acoustic waves (SAW) propagating in the BST films, and from a recursive process, the effective Young’s modulus are determined for the two samples. These methods are used to extract and compare elastic properties of two types of BST films, and quantify the influence of texture on the direction-dependent Young’s modulus.

Microstructure and Texture Development during Cold Rolling in UNS S32205 and UNS S32760 Duplex Stainless Steels

NASA Astrophysics Data System (ADS)

Kumar, Amit; Khatirkar, Rajesh Kisni; Chalapathi, Darshan; Kumar, Gulshan; Suwas, Satyam

2017-05-01

In the present study, microstructure and texture evolution during cold rolling in UNS S32205 and UNS S32760 duplex stainless steel was investigated. Both steels were unidirectionally cold rolled up to 80 pct thickness reduction. Scanning electron microscopy and electron backscattered diffraction (EBSD) were used for microstructural characterization, while X-ray diffraction (XRD) was used for the measurement of bulk texture. Strain-induced martensite (SIM) was identified and quantified with the help of magnetic measurements (B-H curve and magnetization saturation). With the increase in plastic strain, the grains became morphologically elongated along the rolling direction with the reduction in average band thickness and band spacing. SIM increased with the increase in deformation and was found to be a function of strain and the SFE of austenite. The increase in SIM was much more pronounced in UNS S32205 steel as compared to UNS S32760 steel. After cold rolling, strong α-fiber (RD//<110>) texture was developed in ferrite, while brass texture was dominant in austenite for both steels. The strength of texture components and fibers was stronger in UNS S32760 steel. Another significant feature was the development of weak γ-fiber (ND//<111>) in UNS S32760 steel at intermediate deformation.

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.

Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis, electron backscatter and neutron diffraction techniques.

PubMed

Hunter, N J R; Wilson, C J L; Luzin, V

2017-02-01

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross-polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal-plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three-dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

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.

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.

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

Coexistence of colossal stress and texture gradients in sputter deposited nanocrystalline ultra-thin metal films

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

Kuru, Yener; Welzel, Udo; Mittemeijer, Eric J.

2014-12-01

This paper demonstrates experimentally that ultra-thin, nanocrystalline films can exhibit coexisting colossal stress and texture depth gradients. Their quantitative determination is possible by X-ray diffraction experiments. Whereas a uniform texture by itself is known to generally cause curvature in so-called sin{sup 2}ψ plots, it is shown that the combined action of texture and stress gradients provides a separate source of curvature in sin{sup 2}ψ plots (i.e., even in cases where a uniform texture does not induce such curvature). On this basis, the texture and stress depth profiles of a nanocrystalline, ultra-thin (50 nm) tungsten film could be determined.

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.

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

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.

Relationships Between the Phase Transformation Kinetics, Texture Evolution, and Microstructure Development in a 304L Stainless Steel Under Biaxial Loading Conditions: Synchrotron X-ray and Electron Backscatter Diffraction Studies

DOE PAGES

Cakmak, Ercan; Choo, Hahn; Kang, Jun-Yun; ...

2015-02-11

Here we report that the relationships between the martensitic phase transformation kinetics, texture evolution, and the microstructure development in the parent austenite phase were studied for a 304L stainless steel that exhibits the transformation-induced plasticity effect under biaxial loading conditions at ambient temperature. The applied loading paths included: pure torsion, simultaneous biaxial torsion/tension, simultaneous biaxial torsion/compression, and stepwise loading of tension followed by torsion (i.e., first loading by uniaxial tension and then by pure torsion in sequence). Synchrotron X-ray and electron backscatter diffraction techniques were used to measure the evolution of the phase fractions, textures, and microstructures as a functionmore » of the applied strains. The influence of loading character and path on the changes in martensitic phase transformation kinetics is discussed in the context of (1) texture-transformation relationship and the preferred transformation of grains belonging to certain texture components over the others, (2) effects of axial strains on shear band evolutions, and (3) volume changes associated with martensitic transformation.« less

Quantitative texture analysis of talc in mantle hydrated mylonites

NASA Astrophysics Data System (ADS)

Benitez-Perez, J. M.; Gomez Barreiro, J.; Wenk, H. R.; Vogel, S. C.; Soda, Y.; Voltolini, M.; Martinez-Catalan, J. R.

2014-12-01

A quantitative texture analysis of talc-serpentinite mylonites developed in highly deformed ultramafic rocks from different orogenic contexts have been done with neutorn diffraction at HIPPO (Los Álamos National Laboratory). Mineral assemblage, metamorphic evolution and deformative fabric of these samples could be correlated with those verified along the shallow levels (<100km; <5GPa) of a subduction zone. The hydration of mantle (ultramafic) rocks at those levels it is likely to occur dynamically, with important implications on seismogenesis. Given the high anisotropy of the major phases in the samples (i.e. talc and antigorite) it is expected to influence seismic anisotropy of the whole system, in the presence of texture. However to date there was no data on the crystallographic preferred orientation of talc and examples of antigorite textures are very limited. We explore the contribution of talc texture to the seismic anisotropy of mantle hydrated mylonites. Acknowledgements: This work has been funded by research project CGL2011-22728 of Spanish Ministry of Economy and Competitiveness. JGB and JMBP are grateful to the Ramón y Cajal and FPI funding programs. Access to HIPPO (LANSCE) to conduct diffraction experiments is kindly acknowledged.

Local texture and strongly linked conduction in spray-pyrolyzed TlBa2Ca2Cu3O(8+x) deposits

NASA Astrophysics Data System (ADS)

Kroeger, D. M.; Goyal, A.; Specht, E. D.; Wang, Z. L.; Tkaczyk, J. E.; Sutliff, J. A.; Deluca, J. A.

Local texture in polycrystalline TlBa2Ca2 Cu3O(8+x) deposits has been determined from transmission electron microscopy, electron backscatter diffraction patterns and x-ray diffraction. The small-grained deposits had excellent c-axis alignment and contained colonies of grains with similar but not identical a-axis orientations. Most grain boundaries within a colony have small misorientation angles and should not be weak links. It is proposed that long range conduction utilizes a percolative network of small angle grain boundaries at colony intersections.

Deciphering the Possible Role of Strain Path on the Evolution of Microstructure, Texture, and Magnetic Properties in a Fe-Cr-Ni Alloy

NASA Astrophysics Data System (ADS)

Kumar, Amit; Khatirkar, Rajesh Kisni; Gupta, Aman; Shekhawat, Satish K.; Suwas, Satyam

2018-06-01

In the present work, the influence of strain path on the evolution of microstructure, crystallographic texture, and magnetic properties of a two-phase Fe-Cr-Ni alloy was investigated. The Fe-Cr-Ni alloy had nearly equal proportion of austenite and ferrite and was cold rolled up to a true strain of 1.6 (thickness reduction) using two different strain paths—unidirectional rolling and multi-step cross rolling. The microstructures were characterized by scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD), while crystallographic textures were determined using X-ray diffraction. For magnetic characterization, B-H loops and M-H curves were measured and magnetic force microscopy was performed. After unidirectional rolling, ferrite showed the presence of strong α-fiber (rolling direction, RD//<110>) and austenite showed strong brass type texture (consisting of Brass (Bs) ({110}<112>), Goss ({110}<001>), and S ({123}<634>)). After multi-step cross rolling, strong rotated cube ({100}<110>) was developed in ferrite, while austenite showed ND (normal direction) rotated brass ( 10 deg) texture. The strain-induced martensite (SIM) was found to be higher in unidirectionally rolled samples than multi-step cross-rolled samples. The coherently diffracting domain size, micro-strain, coercivity, and core loss also showed a strong correlation with strain and strain path. More strain was partitioned into austenite than ferrite during deformation (unidirectional as well as cross rolling). Further, the strain partitioning (in both austenite and ferrite) was found to be higher in unidirectionally rolled samples.

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

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise.

PubMed

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; Ramebäck, Henrik; Marie, Olivier; Ravat, Brice; Delaunay, François; Young, Emma; Blagojevic, Ned; Hester, James R; Thorogood, Gordon; Nelwamondo, Aubrey N; Ntsoane, Tshepo P; Roberts, Sarah K; Holliday, Kiel S

2018-01-01

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2 , U 3 O 8 and an intermediate species U 3 O 7 in the third material.

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.

Texture and anisotropy in the bismuth sodium titanate system

NASA Astrophysics Data System (ADS)

Fancher, Christoher M.

Bi0.5Na0.5TiO3 has received interest as a potential replacement for lead containing ferroelectrics. However, the piezoelectric response of pure Bi0.5Na0.5TiO 3 does not compare to the strong piezoelectric response of lead based piezoelectrics. To increase the piezoelectric response, Bi0.5Na 0.5TiO3 has been alloyed with BaTiO3 and K 0.5Na0.5NbO3. Another route to enhance the response is to take advantage of the anisotropic properties by inducing a preferred crystallographic orientation. Both routes were used to investigate the effect a crystallographic texture has on the strain response of Bi0.5Na 0.5TiO3-based ceramics. A crystallographic texture was induced by templated grain growth of pure phase Bi0.5Na0.5TiO3 templates using the tape casting method to orient template particles relative to the tape cast normal. Sintered Bi0.5Na0.5TiO3-based materials developed a strong (00l)pc fiber texture relative to the tape cast normal, with no preferential alignment relative to the tape cast plane. Textured Bi0.5Na0.5TiO3-(5)BaTiO3 showed a piezoelectric response of 245 pC/N, a better than 50% enhancement from the 150 pC/N response of randomly oriented samples. The Bi0.5Na0.5TiO3-(5)BaTiO3-(2)K 0.5Na0.5NbO3 (x,y) system has been shown to undergo electric-field-induced phase transformation from a pseudocubic to polar phase. For (7,2) a strong 8.7 multiples of a random distribution (MRD) crystallographic texture increased the macroscopic strain response by 50%. Applying the electric field perpendicular to the fiber texture axis reduces the macroscopic strain response of textured (7,2) by 17%. The affect field direction has on the electric-field-induced phase transformations of textured (7,2) was investigated using in situ electric field dependent diffraction. In situ diffraction data showed the high strain response of textured (7,2) can be attributed to a reversible pseudocubic to tetragonal transformation. The field-induced tetragonal phase nucleates preferentially with a strong c-axis alignment in the electric field direction, ferroelastic domain texture. In situ diffraction data suggests the origin of the reduction in strain associated with a field applied perpendicular to the fiber texture axis is the result of a shorter induced lattice spacing and lower domain texture.

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

Calculation of Debye-Scherrer diffraction patterns from highly stressed polycrystalline materials

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

MacDonald, M. J., E-mail: macdonm@umich.edu; SLAC National Accelerator Laboratory, Menlo Park, California 94025; Vorberger, J.

2016-06-07

Calculations of Debye-Scherrer diffraction patterns from polycrystalline materials have typically been done in the limit of small deviatoric stresses. Although these methods are well suited for experiments conducted near hydrostatic conditions, more robust models are required to diagnose the large strain anisotropies present in dynamic compression experiments. A method to predict Debye-Scherrer diffraction patterns for arbitrary strains has been presented in the Voigt (iso-strain) limit [Higginbotham, J. Appl. Phys. 115, 174906 (2014)]. Here, we present a method to calculate Debye-Scherrer diffraction patterns from highly stressed polycrystalline samples in the Reuss (iso-stress) limit. This analysis uses elastic constants to calculate latticemore » strains for all initial crystallite orientations, enabling elastic anisotropy and sample texture effects to be modeled directly. The effects of probing geometry, deviatoric stresses, and sample texture are demonstrated and compared to Voigt limit predictions. An example of shock-compressed polycrystalline diamond is presented to illustrate how this model can be applied and demonstrates the importance of including material strength when interpreting diffraction in dynamic compression experiments.« less

Microstructure, texture evolution and magnetic properties of strip-casting non-oriented 6.5 wt.% Si electrical steel doped with cerium

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

Li, Hao-Ze, E-mail: lhzqq83@163.com; Liu, Hai-Tao; Liu, Zhen-Yu, E-mail: zyliu@mail.neu.edu.cn

A 0.3 mm thick non-oriented 6.5 wt.% Si electrical steel sheet doped with cerium is produced by twin-roll strip casting, hot rolling, warm rolling and annealing. A detailed study of the cerium precipitates in the as-cast strip, microstructure and texture evolution at different processing stages is carried out by electron probe micro-analysis, optical microscopy, X-ray diffraction and electron backscattered diffraction analysis. Grain interior distributing precipitates identified as Ce-oxides, Ce-oxysulfides and Ce-phosphides, and boundary distributing Ce-oxides and Ce-phosphides are observed in the as-cast strip. The initial as-cast strip is characterized by a much finer solidification microstructure and dominated by obvious //ND texture through the strip thickness. After hot and warm rolling, inhomogeneous microstructure containing large amounts of in-grain shear bands is characterized by mixed < 110 >//RD and < 111 >//ND textures. The texture of the annealed sheet with a relatively large average grain size is far more optimized by the domination of the beneficial cube, rotated cube, (001)< 120 > to (001)< 130 > and Goss texture components, and the elimination of the detrimental γ-fiber texture, leading to a superior magnetic induction and improved iron loss. - Highlights: • An Fe–6.5 wt.% Si as-cast strip doped with cerium was produced. • A thin warm rolled sheet with limited edge cracks was obtained. • Microstructure and texture evolution at each stage were investigated. • Strong λ-fiber and Goss recrystallization textures were formed. • The magnetic properties of the annealed sheet were significantly improved.« less

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

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.

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

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.

Absence of dynamic strain aging in an additively manufactured nickel-base superalloy.

PubMed

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

2018-05-25

Dynamic strain aging (DSA), observed macroscopically as serrated plastic flow, has long been seen in nickel-base superalloys when plastically deformed at elevated temperatures. Here we report the absence of DSA in Inconel 625 made by additive manufacturing (AM) at temperatures and strain rates where DSA is present in its conventionally processed counterpart. This absence is attributed to the unique AM microstructure of finely dispersed secondary phases (carbides, N-rich phases, and Laves phase) and textured grains. Based on experimental observations, we propose a dislocation-arrest model to elucidate the criterion for DSA to occur or to be absent as a competition between dislocation pipe diffusion and carbide-carbon reactions. With in situ neutron diffraction studies of lattice strain evolution, our findings provide a new perspective for mesoscale understanding of dislocation-solute interactions and their impact on work-hardening behaviors in high-temperature alloys, and have important implications for tailoring thermomechanical properties by microstructure control via AM.

Deformation behavior of additively manufactured GP1 stainless steel

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

Clausen, B.; Brown, D. W.; Carpenter, J. S.

In-situ neutron diffraction measurements were performed in this paper during heat-treating and uniaxial loading of additively manufactured (AM) GP1 material. Although the measured chemical composition of the GP1 powder falls within the composition specifications of 17-4 PH steel, a fully martensitic alloy in the wrought condition, the crystal structure of the as-built GP1 material is fully austenitic. Chemical analysis of the as-built material shows high oxygen and nitrogen content, which then significantly decreased after heat-treating in a vacuum furnace at 650 °C for one hour. Significant austenite-to-martensite phase transformation is observed during compressive and tensile loading of the as-built andmore » heat-treated material with accompanied strengthening as martensite volume fraction increases. During loading, the initial average phase stress state in the martensite is hydrostatic compression independent of the loading direction. Finally, preferred orientation transformation in austenite and applied load accommodation by variant selection in martensite are observed via measurements of the texture development.« less

Magneto-orbital helices: a novel coupling mechanism between magnetism and ferroelectricity in multiferroic CaMn7O12

NASA Astrophysics Data System (ADS)

Radaelli, Paolo G.; Perks, Natasha; Johnson, Roger D.; Martin, Christine; Chapon, Laurent

2013-03-01

The trigonal quadruple perovskite CaMn7O12 displays one of the largest magnetically induced ferroelectric polarisations measured to date (2870 μC m-2). Ferroelectricity appears below 90 K, together with an incommensurate helical magnetic modulation, and cannot be explained within the framework developed for cycloidal magnets. We report an unprecedented magneto-orbital texture in multiferroic CaMn7O12, which is directly connected to ferroelectricity. X-ray and neutron diffraction characterisation of the structural and magnetic modulations in these ``magneto-orbital helices'', and analysis of magnetic exchange shows that orbital order is crucial in stabilising a chiral magnetic structure. Additionally, the presence of a global structural rotation enables the magnetic helicity to couple with the lattice, giving rise to electric polarisation. These novel principles open up the possibility of discovering new multiferroics with even larger polarization and higher transition temperatures. Work at Oxford was funded by EPSRC grant EP/J003557/1.

Anisotropy of diamagnetic susceptibility in Thassos marble: A comparison between measured and modeled data

NASA Astrophysics Data System (ADS)

de Wall, Helga; Bestmann, Michel; Ullemeyer, Klaus

2000-11-01

A study of shear zones within the calcite marble complex of the island of Thassos (Greece) shows that the low field anisotropy of magnetic susceptibility (AMS)-technique can be successfully applied to diamagnetic rocks for characterizing rock fabrics. The strain path involves both an early pure shear stage and a simple shear overprint that is documented by a transition from triaxial (neutral) to uniaxial (prolate) shapes of AMS ellipsoids. The maximum susceptibility is oriented perpendicular to the rock foliation, reflecting the preferred orientation of calcite c-axes in the protolith as well as in the mylonites. For three samples that represent different types of calcite fabrics, the AMS was recalculated from neutron and electron backscatter diffraction textural data. A comparison of the measured and modeled data shows a good coincidence for the orientation of the principal AMS axes and for the recalculated anisotropy data. Both measured and modeled data sets reflect the change from neutral to distinct prolate ellipsoids during progressive deformation.

Deformation behavior of additively manufactured GP1 stainless steel

DOE PAGES

Clausen, B.; Brown, D. W.; Carpenter, J. S.; ...

2017-04-22

In-situ neutron diffraction measurements were performed in this paper during heat-treating and uniaxial loading of additively manufactured (AM) GP1 material. Although the measured chemical composition of the GP1 powder falls within the composition specifications of 17-4 PH steel, a fully martensitic alloy in the wrought condition, the crystal structure of the as-built GP1 material is fully austenitic. Chemical analysis of the as-built material shows high oxygen and nitrogen content, which then significantly decreased after heat-treating in a vacuum furnace at 650 °C for one hour. Significant austenite-to-martensite phase transformation is observed during compressive and tensile loading of the as-built andmore » heat-treated material with accompanied strengthening as martensite volume fraction increases. During loading, the initial average phase stress state in the martensite is hydrostatic compression independent of the loading direction. Finally, preferred orientation transformation in austenite and applied load accommodation by variant selection in martensite are observed via measurements of the texture development.« less

Profiling pleural effusion cells by a diffraction imaging method

NASA Astrophysics Data System (ADS)

Al-Qaysi, Safaa; Hong, Heng; Wen, Yuhua; Lu, Jun Q.; Feng, Yuanming; Hu, Xin-Hua

2018-02-01

Assay of cells in pleural effusion (PE) is an important means of disease diagnosis. Conventional cytology of effusion samples, however, has low sensitivity and depends heavily on the expertise of cytopathologists. We applied a polarization diffraction imaging flow cytometry method on effusion cells to investigate their features. Diffraction imaging of the PE cell samples has been performed on 6000 to 12000 cells for each effusion cell sample of three patients. After prescreening to remove images by cellular debris and aggregated non-cellular particles, the image textures were extracted with a gray level co-occurrence matrix (GLCM) algorithm. The distribution of the imaged cells in the GLCM parameters space was analyzed by a Gaussian Mixture Model (GMM) to determine the number of clusters among the effusion cells. These results yield insight on textural features of diffraction images and related cellular morphology in effusion samples and can be used toward the development of a label-free method for effusion cells assay.

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.

Optimization of PbTiO3 Seed Layers for PZT MEMS Actuators

DTIC Science & Technology

2008-12-01

14. ABSTRACT The material properties of sol-gel lead zirconate titanate ( PZT ) are inherently linked with its crystallinity and texture . The use...will lead to a greater degree of texturing within the PZT thin film. Figure 6. X-ray diffraction data for PT seed solution. (001) oriented...previous studies PZT 45/55 has shown a higher piezoelectric coefficient compared to PZT 52/48 due to the random crystalline texture of the existing

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.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

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

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

DOE PAGES

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; ...

2018-01-24

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

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.

Post Deformation Annealing Behaviour of Mg-Al-Sn Alloys

NASA Astrophysics Data System (ADS)

Kabir, Abu Syed Humaun; Su, Jing; Sanjari, Mehdi; Jung, In-Ho; Yue, Stephen

In this study, effects of dynamically formed precipitates on the microstructure and texture evolutions were investigated after the post deformation annealing for various times. Two ternary alloys of Mg, Al and Sn were designed, produced and deformed at 300°C at a strain rate of 0.01s-1 to form different amounts of strain induced precipitates during deformation. Subsequent annealing at deformation temperature was performed for up to 4 hours. Microstructures and precipitation were investigated by optical and scanning electron microscopes and macro and micro-texture were measured by X-ray diffraction (XRD) and Electron Back-Scattered Diffraction (EBSD) techniques, respectively. It was found that certain amount of strain induced precipitates was necessary to prevent grain growth for a certain time during annealing by grain boundary pinning effect. Also, texture randomization was possible with the presence of precipitates after certain time of annealing.

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

Illuminating the Past: The Neutron as a Tool in Archaeology

ERIC Educational Resources Information Center

Kockelmann, W.; Kirfel, A.; Siano, S.; Frost, C. D.

2004-01-01

Neutrons can be produced in nuclear reactions and used as very versatile probes for condensed matter research. Since their introduction in the 1950s neutron scattering techniques have evolved to be very powerful tools for investigating the properties of condensed matter. Here we present the concept of neutron diffraction and how this technique can…

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 .

Textural Evolution During Micro Direct Metal Deposition of NiTi Alloy

NASA Astrophysics Data System (ADS)

Khademzadeh, Saeed; Bariani, Paolo F.; Bruschi, Stefania

2018-03-01

In this research, a micro direct metal deposition process, newly developed as a potential method for micro additive manufacturing was used to fabricate NiTi builds. The effect of scanning strategy on grain growth and textural evolution was investigated using scanning electron microscope equipped with electron backscattered diffraction detector. Investigations showed that, the angle between the successive single tracks has an important role in grain size distribution and textural evolution of NiTi phase. Unidirectional laser beam scanning pattern developed a fiber texture; conversely, a backward and forward scanning pattern developed a strong < {100} > ‖‖ RD texture on the surface of NiTi cubic samples produced by micro direct metal deposition.

Textural Evolution During Micro Direct Metal Deposition of NiTi Alloy

NASA Astrophysics Data System (ADS)

Khademzadeh, Saeed; Bariani, Paolo F.; Bruschi, Stefania

2018-07-01

In this research, a micro direct metal deposition process, newly developed as a potential method for micro additive manufacturing was used to fabricate NiTi builds. The effect of scanning strategy on grain growth and textural evolution was investigated using scanning electron microscope equipped with electron backscattered diffraction detector. Investigations showed that, the angle between the successive single tracks has an important role in grain size distribution and textural evolution of NiTi phase. Unidirectional laser beam scanning pattern developed a fiber texture; conversely, a backward and forward scanning pattern developed a strong < {100} > ‖‖ RD texture on the surface of NiTi cubic samples produced by micro direct metal deposition.

Non-invasive characterisation of SIX Japanese hand-guards (tsuba)

NASA Astrophysics Data System (ADS)

Barzagli, Elisa; Grazzi, Francesco; Civita, Francesco; Scherillo, Antonella; Pietropaolo, Antonino; Festa, Giulia; Zoppi, Marco

2013-12-01

In this work we present a systematic study of Japanese sword hand-guards ( tsuba) carried out by means of non-invasive techniques using neutrons. Several tsuba from different periods, belonging to the Japanese Section of the Stibbert Museum, were analysed using an innovative approach to characterise the bulk of the samples, coupling two neutron techniques, namely Time of Flight Neutron Diffraction (ToF-ND) and Nuclear Resonance Capture Analysis (NRCA). The measurements were carried out on the same instrument: the INES beam-line at the ISIS spallation pulsed neutron source (UK). NRCA analysis allows identifying the elements present in the sample gauge volume, while neutron diffraction is exploited to quantify the phase distribution and other micro-structural parameters of the metal specimen. The results show that all samples are made of high-quality metal, either steel or copper alloy, with noticeable changes in composition and working techniques, depending on the place and time of manufacturing.

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

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.

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

Effect of cold deformation on the recrystallization behavior of FePd alloy at the ordering temperature using electron backscatter diffraction

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

Lin, Hung-Pin; Chen, Yen-Chun; Chen, Delphic

2014-08-15

In this study, the evolution of the recrystallization texture and microstructure was investigated after annealing of 50% and 90% cold-rolled FePd alloy at 530 °C. The FePd alloy was produced by vacuum arc melting in an atmosphere of 97% Ar and 3% H{sub 2}. The specimens were cold rolled to achieve 50% and 90% reduction in thickness. Electron backscatter diffraction measurements were performed on the rolling direction–normal direction section. With increased deformation from 50% to 90%, recrystallized texture transition occurs. For the 50% cold-rolled alloy, the preferred orientation is (0 1 0) [11 0 1], which is close to themore » cubic orientation after 400 h of annealing. For the 90% cold-rolled alloy, the orientation changes to (0 5 4) [22–4 5] after 16 h of annealing. - Highlights: • Texture and microstructure in cold-rolled FePd alloy was investigated during annealing using EBSD. • The recrystallized texture of 50% cold-rolled FePd is (0 1 0) [11 0 1] at 530 °C for 400 hours. • The recrystallized texture of 90% cold-rolled FePd is changed to (0 5 4) [22–4 5] at 530 °C after 16 hours.« less

Characterization of crystallographic properties of thin films using X-ray diffraction

NASA Astrophysics Data System (ADS)

Zoo, Yeongseok

2007-12-01

Silver (Ag) has been recognized as one of promising candidates in Ultra-Large Scale Integrated (ULSI) applications in that it has the lowest bulk electrical resistivity of all pure metals and higher electromigration resistance than other interconnect materials. However, low thermal stability on Silicon Dioxide (Si02) at high temperatures (e.g., agglomeration) is considered a drawback for the Ag metallization scheme. Moreover, if a thin film is attached on a substrate, its properties may differ significantly from that of the bulk, since the properties of thin films can be significantly affected by the substrate. In this study, the Coefficient of Thermal Expansion (CTE) and texture evolution of Ag thin films on different substrates were characterized using various analytical techniques. The experimental results showed that the CTE of the Ag thin film was significantly affected by underlying substrate and the surface roughness of substrate. To investigate the alloying effect for Ag meatallization, small amounts of Copper (Cu) were added and characterized using theta-2theta X-ray Diffraction (XRD) scan and pole figure analysis. These XRD techniques are useful for investigating the primary texture of a metal film, (111) in this study, which (111) is the notation of a specific plane in the orthogonal coordinate system. They revealed that the (111) textures of Ag and Ag(Cu) thin films were enhanced with increasing temperature. Comparison of texture profiles between Ag and Ag(Cu) thin films showed that Cu additions enhanced (111) texture in Ag thin films. Accordingly, the texture enhancement in Ag thin films by Cu addition was discussed. Strained Silicon-On-Insulator (SSOI) is being considered as a potential substrate for Complementary Metal-Oxide-Semiconductor (CMOS) technology since the induced strain results in a significant improvement in device performance. High resolution X-ray diffraction (XRD) techniques were used to characterize the perpendicular and parallel strains in SSOI layers. XRD diffraction profiles generated from the crystalline SSOI layer provided a direct measurement of the layer's strain components. In addition, it has demonstrated that the rotational misalignment between the layer and the substrate can be incorporated within the biaxial strain equations for epitaxial layers. Based on these results, the strain behavior of the SSOI layer and the relation between strained Si and SiO2 layers are discussed for annealed samples.

Influence of Nd and Y on texture of as-extruded Mg-5Li-3Al-2Zn alloy

NASA Astrophysics Data System (ADS)

Wu, Liqun; Zhang, Tianlong; Cui, Chongliang; Wu, Ruizhi; Zhang, Milin; Hou, Legan

2016-07-01

Mg-5Li-3Al-2Zn alloys with the additions of Y and Nd were prepared using induction melting furnace under the atmosphere of pure argon; then they were extruded. The textures of the as-extruded alloys were analyzed by pole figures and electron backscatter diffraction. Results show that the addition of a small amount of Nd can weaken the basal texture. The further increase of Nd content has no corresponding further influence on texture. When a small amount of Y is used to replace Nd, the basal texture can be further weakened and the prismatic slip system can be further activated. In the alloy of Mg-5Li-3Al-2Zn-1.2Y-0.8Nd, the basal textures almost vanish.

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

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.

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.

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

Texture and Elastic Anisotropy of Mantle Olivine

NASA Astrophysics Data System (ADS)

Nikitin, A. N.; Ivankina, T. I.; Bourilitchev, D. E.; Klima, K.; Locajicek, T.; Pros, Z.

Eight olivine rock samples from different European regions were collected for neu- tron texture analyses and for P-wave velocity measurements by means of ultrasonic sounding at various confining pressures. The orientation distribution functions (ODFs) of olivine were determined and pole figures of the main crystallographic planes were calculated. The spatial P-wave velocity distributions were determined at confining pressures from 0.1 to 400 MPa and modelled from the olivine textures. In dependence upon the type of rock (xenolith or dunite) different behavior of both the P-wave veloc- ity distributions and the anisotropy coefficients with various confining pressures was observed. In order to explain the interdependence of elastic anisotropy and hydrostatic pressure, a model for polycrystalline olivine rocks was suggested, which considers the influence of the crystallographic and the mechanical textures on the elastic behaviour of the polycrystal. Since the olivine texture depends upon the active slip systems and the deformation temperature, neutron texture analyses enable us to estimate depth and thermodynamical conditions during texture formation.

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

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

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.

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.

In-situ Indentation and Correlated Precession Electron Diffraction Analysis of a Polycrystalline Cu Thin Film

NASA Astrophysics Data System (ADS)

Guo, Qianying; Thompson, Gregory B.

2018-04-01

In-situ TEM nanoindentation of a polycrystalline Cu film was cross-correlated with precession electron diffraction (PED) to quantify the microstructural evolution. The use of PED is shown to clearly reveal features, such as grain size, that are easily masked by diffraction contrast created by the deformation. Using PED, the accompanying grain refinement and change in texture as well as the preservation of specific grain boundary structures, including a ∑3 boundary, under the indent impression were quantified. The nucleation of dislocations, evident in low-angle grain boundary formations, was also observed under the indent. PED quantification of texture gradients created by the indentation process linked well to bend contours observed in the bright-field images. Finally, PED enabled generating a local orientation spread map that gave an approximate estimation of the spatial distribution of strain created by the indentation impression.

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

Evolution of microstructure in stainless martensitic steel for seamless tubing

NASA Astrophysics Data System (ADS)

Pyshmintsev, I. Yu.; Bityukov, S. M.; Pastukhov, V. I.; Danilov, S. V.; Vedernikova, L. O.; Lobanov, M. L.

2017-12-01

Scanning electron microscopy with orientation analysis by the electron backscatter diffraction (EBSD) method is used to study microstructures and textures formed in the 0.08C-13Cr-3Ni-Mo-V-Nb steel through seamless tube production route: after hot deformation by extrusion; after quenching from various temperatures and subsequent high tempering. It is shown that the martensitic microstructure formed both after hot deformation and after quenching is characterized by the presence of deformation crystallographic texture, which is predetermined by the texture of austenite. The effect of heat treatment on texture, packet refinement, lath width, precipitation of carbides and Charpy impact energy is analyzed.

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

Optical-diffraction method for determining crystal orientation

DOEpatents

Sopori, B.L.

1982-05-07

Disclosed is an optical diffraction technique for characterizing the three-dimensional orientation of a crystal sample. An arbitrary surface of the crystal sample is texture etched so as to generate a pseudo-periodic diffraction grating on the surface. A laser light beam is then directed onto the etched surface, and the reflected light forms a farfield diffraction pattern in reflection. Parameters of the diffraction pattern, such as the geometry and angular dispersion of the diffracted beam are then related to grating shape of the etched surface which is in turn related to crystal orientation. This technique may be used for examining polycrystalline silicon for use in solar cells.

3-D study of texture and elastic anisotropy on rocks from NW Italy Ivrea zone

NASA Astrophysics Data System (ADS)

Pros, Z.; Lokajicek, T.; Prikryl, R.; Klima, K.; Nikitin, A. N.; Ivankina, T. I.; Martinkova, M.

2003-04-01

The direct measurement of physical properties of lower crustal and upper mantle rocks, which can be found on the Earth's surface, could be used for the improving of our knowledge of deep rocks. These results could be used mainly for the correction of geological and geophysical models based on the indirect data. Elastic properties of rocks are one of the most important parameters studied and could be applied in many fields of Earth sciences. In this study several quite different methods were applied to determine elastic properties. P-wave ultrasonic sounding of mafic and ultrabasic rock samples in 132 independent directions at several levels of confining pressure enable to determine elastic anisotropy of P-wave velocity. The samples were collected in nearby of Balmuccia ultra basic massif (Ivrea zone, southern Alps, NW Italy). This method revealed large directional variance of maximum P-wave velocity and different symmetric (orthorhombic vs. transversal isotropic) of elastic waves 3-D distribution, that has not been found on these rocks before. Identical samples were studied by means of neutron diffraction. Neutron diffraction provide data on CPO orientation in identical spherical samples, on which was measured P-wave velocity. Laboratory 3-D measurement of P-wave velocity thus present powerful method for detection of magmatic fabric features not visible by naked eye. One dunite sample exhibits P-wave velocity approaching to that of olivine crystal 9.8 km/s due to the strong CPO of olivine in this sample. Such observation was not done before on the natural olivine-rich rocks. It follows from the comparison of measured and calculated P-wave velocities, that these values are more reliable than data obtained from measurement in few directions only. This project was supported by Grant Agency of the Czech Republic No.: 205/01/1430.

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.

Electron backscatter diffraction study of deformation and recrystallization textures of individual phases in a cross-rolled duplex steel

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

Zaid, Md; Bhattacharjee, P.P., E-mail: pinakib@iith.ac.in

2014-10-15

The evolution of microstructure and texture during cross-rolling and annealing was investigated by electron backscatter diffraction in a ferritic–austenitic duplex stainless steel. For this purpose an alloy with nearly equal volume fraction of the two phases was deformed by multi-pass cross-rolling process up to 90% reduction in thickness. The rolling and transverse directions were mutually interchanged in each pass by rotating the sample by 90° around the normal direction. In order to avoid deformation induced phase transformation and dynamic strain aging, the rolling was carried out at an optimized temperature of 898 K (625 °C) at the warm-deformation range. Themore » microstructure after cross warm-rolling revealed a lamellar structure with alternate arrangement of the bands of two phases. Strong brass and rotated brass components were observed in austenite in the steel after processing by cross warm-rolling. The ferrite in the cross warm-rolling processed steel showed remarkably strong RD-fiber (RD//< 011 >) component (001)< 011 >. The development of texture in the two phases after processing by cross warm-rolling could be explained by the stability of the texture components. During isothermal annealing of the 90% cross warm-rolling processed material the lamellar morphology was retained before collapse of the lamellar structure to the mutual interpenetration of the phase bands. Ferrite showed recovery resulting in annealing texture similar to the deformation texture. In contrast, the austenite showed primary recrystallization without preferential orientation selection leading to the retention of deformation texture. The evolution of deformation and annealing texture in the two phases of the steel was independent of one another. - Highlights: • Effect of cross warm-rolling on texture formation is studied in duplex steel. • Brass texture in austenite and (001)<110 > in ferrite are developed. • Ferrite shows recovery during annealing retaining the (001)<110 > component. • Austenite shows recrystallization during annealing retaining the deformation texture. • The deformation of recrystallization of two phases is independent of one other.« less

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 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.

Texture evolution in Oxide Dispersion Strengthened (ODS) steel tubes during pilgering process

NASA Astrophysics Data System (ADS)

Vakhitova, E.; Sornin, D.; Barcelo, F.; François, M.

2017-10-01

Oxide Dispersion Strengthened (ODS) steels are foreseen as fuel cladding material in the coming generation of Sodium Fast Reactors (SFR). Cladding tubes are manufactured by hot extrusion and subsequent cold forming steps. In this study, a 9 wt% Cr ODS steel exhibiting α-γ phase transformation at high temperature is cold formed under industrial conditions with a large section reduction in two pilgering steps. The influence of pilgering process parameters and intermediate heat treatment on the microstructure evolution is studied experimentally using Electron Backscattering Diffraction (EBSD) and X-ray Diffraction (XRD) methods. Pilgered samples show elongated grains and a high texture formation with a preferential orientation along the rolling direction. During the heat treatment, grain morphology is recovered from elongated grains to almost equiaxed ones, while the well-known α-fiber texture presents an unexpected increase in intensity. The remarkable temperature stability of this fiber is attributed to a crystallographic structure memory effect during phase transformations.

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.

Shock Melting of Iron Silicide as Determined by In Situ X-ray Diffraction.

NASA Astrophysics Data System (ADS)

Newman, M.; Kraus, R. G.; Wicks, J. K.; Smith, R.; Duffy, T. S.

2016-12-01

The equation of state of core alloys at pressures and temperatures near the solid-liquid coexistence curve is important for understanding the dynamics at the inner core boundary of the Earth and super-Earths. Here, we present a series of laser driven shock experiments on textured polycrystalline Fe-15Si. These experiments were conducted at the Omega and Omega EP laser facilities. Particle velocities in the Fe-15Si samples were measured using a line VISAR and were used to infer the thermodynamic state of the shocked samples. In situ x-ray diffraction measurements were used to probe the melting transition and investigate the potential decomposition of Fe-15Si in to hcp and B2 structures. This work examines the kinetic effects of decomposition due to the short time scale of dynamic compression experiments. In addition, the thermodynamic data collected in these experiments adds to a limited body of information regarding the equation of state of Fe-15Si, which is a candidate for the composition in Earth's outer core. Our experimental results show a highly textured solid phase upon shock compression to pressures ranging from 170 to 300 GPa. Below 320 GPa, we observe diffraction peaks consistent with decomposition of the D03 starting material in to an hcp and a cubic (potentially B2) structure. Upon shock compression above 320 GPa, the intense and textured solid diffraction peaks give way to diffuse scattering and loss of texture, consistent with melting along the Hugoniot. When comparing these results to that of pure iron, we can ascertain that addition of 15 wt% silicon increases the equilibrium melting temperature significantly, or that the addition of silicon significantly increases the metastability of the solid phase, relative to the liquid. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

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.

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.

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

Lattice-Preferred Orientation in Deformed Novaculite - Comparison of in-situ Results Using BEARTEX and Post-Mortem EBSD Analyses

NASA Astrophysics Data System (ADS)

Willenweber, A.; Thomas, S.; Burnley, P. C.

2012-12-01

The Berkeley Texture Package BEARTEX is a Windows-based computer software that combines various algorithms to analyze lattice-preferred orientation in polycrystalline materials. BEARTEX was initially designed to interpret diffraction intensity data from pole figure goniometers. Recently it has been successfully used to process synthetic forsterite powder diffraction data from in-situ synchrotron X-ray diffraction taken during deformation (Bollinger et al. 2012). Our study aims to test the practicability of using BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz (novaculite) during deformation. In-situ X-ray diffraction data was collected during the deformation of novaculite at 2.5 GPa and up to 1000 °C in a D-DIA apparatus using the ten-element energy-dispersive detector at the NSLS beamline X17B2. Diffraction intensities are a function of crystal orientation, expressed in azimuth angle η and pole distance ψ. The latter is the angle between the normal of a given diffraction plane and the vertical direction of the D-DIA apparatus - our principal stress direction during compression. Orientation-dependent diffraction intensities were corrected for different responses of the single detectors and x-ray absorption effects of the anvils. Orientation distributions (ODs) and inverse pole figures were calculated using BEARTEX. In addition, electron backscatter diffraction (EBSD) analyses were carried out on the deformed novaculite samples. Generated pole figures were compared with those derived from BEARTEX. Textural properties of our novaculite starting material complicated the BEARTEX analyses. The relatively strong variation of grain sizes in our natural specimens caused non-random diffraction intensity distributions. Those lead to non-random distributions of crystal orientations when analyzed with BEARTEX, although pole figures from EBSD data clearly show random crystal orientations. In an attempt to solve this problem, we employed a scanning routine when recording in-situ synchrotron X-ray diffraction and so collected diffraction from multiple sample volumes rather than from one single spot. Here, we will present a comparison of pole figures derived from independent BEARTEX and EBSD analyses for a series of novaculite experiments and discuss the practicability of BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz. REFERENCES C. BOLLINGER, S. MERKEL AND P. RATERRON (2012): In situ quantitative analysis of stress and texture development in forsterite aggregates deformed at 6 GPa and 1373 K. J. Appl. Cryst., 45, 263-271.

Early history of neutron scattering at oak ridge

NASA Astrophysics Data System (ADS)

Wilkinson, M. K.

1986-03-01

Most of the early development of neutron scattering techniques utilizing reactor neutrons occurred at the Oak Ridge National Laboratory during the years immediately following World War II. C.G. Shull, E.O. Wollan, and their associates systematically established neutron diffraction as a quantitative research tool and then applied this technique to important problems in nuclear physics, chemical crystallography, and magnetism. This article briefly summarizes the very important research at ORNL during this period, which laid the foundation for the establishment of neutron scattering programs throughout the world.

Pulsed Neutron Powder Diffraction for Materials Science

NASA Astrophysics Data System (ADS)

Kamiyama, T.

2008-03-01

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

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.

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.

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

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.

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

Acceleration of color computer-generated hologram from three-dimensional scenes with texture and depth information

NASA Astrophysics Data System (ADS)

Shimobaba, Tomoyoshi; Kakue, Takashi; Ito, Tomoyoshi

2014-06-01

We propose acceleration of color computer-generated holograms (CGHs) from three-dimensional (3D) scenes that are expressed as texture (RGB) and depth (D) images. These images are obtained by 3D graphics libraries and RGB-D cameras: for example, OpenGL and Kinect, respectively. We can regard them as two-dimensional (2D) cross-sectional images along the depth direction. The generation of CGHs from the 2D cross-sectional images requires multiple diffraction calculations. If we use convolution-based diffraction such as the angular spectrum method, the diffraction calculation takes a long time and requires large memory usage because the convolution diffraction calculation requires the expansion of the 2D cross-sectional images to avoid the wraparound noise. In this paper, we first describe the acceleration of the diffraction calculation using "Band-limited double-step Fresnel diffraction," which does not require the expansion. Next, we describe color CGH acceleration using color space conversion. In general, color CGHs are generated on RGB color space; however, we need to repeat the same calculation for each color component, so that the computational burden of the color CGH generation increases three-fold, compared with monochrome CGH generation. We can reduce the computational burden by using YCbCr color space because the 2D cross-sectional images on YCbCr color space can be down-sampled without the impairing of the image quality.

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 .

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

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.

Fabrication and Enhancement of Critical Currents of Silver Sheathed

NASA Astrophysics Data System (ADS)

Hu, Qingyu

X-ray diffraction was used to characterise the phase composition and to investigate the formation mechanism of the (Bi,Pb)_2Sr_2Ca_2Cu _3O_{10} phase from the precursor with (Bi,Pb)_2Sr_2CaCu _2O_8 as the main phase. The reaction is found to be a two-dimensional nucleation (random)-growth type, (-(ln(1-F)) ^{1/2} = kt, where F is the conversional fraction of (Bi,Pb) _2Sr_2CaCu_2O_8 phase and t is the sintering time. The two dimensional behaviour of the critical current in (Bi,Pb)_2Sr2Ca_2Cu _3O_{10}/Ag tapes was observed and analysed by introducing an effective grain misalignment angle, varphi_{eff}. This angle was found to be identical to the average crystallographic grain misalignment angle in the superconducting core. Furthermore, after fast neutron irradiation, which is isotropical, the J_{c}'s of the tapes were modified by the introduction of artificial defects, but the varphi_{eff}'s remained the same. The transport critical current of (Bi,Pb) _2Sr_2Ca_2Cu_3O_ {10}/Ag tapes was measured in magnetic fields up to 15 T and at temperatures from of 4.2 to 84 K. At high temperatures, the J_ {c} is strongly anisotropic and the anisotropy increases rapidly with magnetic field, whereas at low temperatures the critical current is less anisotropic and the anisotropy is almost field independent above 1 T. The transport J_{c }'s in (Bi,Pb)_2Sr_2Ca _2Cu_3O_{10}/Ag tapes at 77 K and higher magnetic fields after neutron irradiation are significantly enhanced. This enhancement is attributed to an improvement in the flux pinning capability of this material by the neutron-induced defects. The angular dependence of J_{c} is still consistent with two-dimensionality, i.e. flux pinning of pancake and/or Josephson vortices is directly confirmed by this transport measurement. Short multifilamentary (Bi,Pb)_2Sr_2Ca_2Cu_2O_{10 }/Ag tapes were fabricated. The sintering parameters were optimised to be 832^circ C and 180 h. The multifilamentary tape consists mainly of pure (Bi,Pb)_2Sr_2Ca _2Cu_3O_{10} with a (00l) preferred orientation, like the single filamentary tape. The mass densities of the (Bi,Pb)_2Sr_2Ca_2Cu_3O_{10 }/Ag wire and tape vary during the mechanical deformation process, as one of the steps of the oxide-powder -in-tube technique used to fabricate the composite superconductor. Results show that the rolling has a more significant effect on densifying the tape core, whereas the drawing process can only densify the core to about 75% of the theoretical density. Since the textured (Bi,Pb)_2Sr_2Ca _2Cu_3O_{10} phase forms by epitaxial growth on the textured (Bi,Pb) _2Sr_2CaCu_2O_8 seed crystals, the deformation induced texture is critical. The formation of the amorphous phase is harmful to the texturing of the (Bi,Pb)_2Sr_2Ca_2Cu _2O_{10} phase, which finally leads to a degradation of critical currents. (Abstract shortened by UMI.).

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 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.

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

Backscattered Diffraction | Materials Science | NREL

Science.gov Websites

crystalline orientation (left) and grain distribution (right). EBSD images showing properties of crystalline investigate misorientation between grain boundaries, texture, grain distribution, deformation, strain, and

A diffraction based study of the deformation mechanisms in anomalously ductile B2 intermetallics

NASA Astrophysics Data System (ADS)

Mulay, Rupalee Prashant

For many decades, the brittle nature of most intermetallic compounds (e.g. NiAl) has been the limiting factor in their practical application. Many B2 (CsCl prototypical structure) intermetallics are known to exhibit slip on the <001>{110} slip mode, which provides only 3 independent slip systems and, hence, is unable to satisfy the von Mises (a.k.a. Taylor) criterion for polycrystalline ductility. As a result, inherent polycrystalline ductility is unexpected. Recent discovery of a number of ductile B2 intermetallics has raised questions about possible violation of the von Mises criterion by these alloys. These ductile intermetallic compounds are MR (metal (M) combined with a rare earth metal or group IV refractory metal (R)) alloys and are stoichiometric, ordered compounds. Single crystal slip trace analyses have only identified the presence of <100>{011} or <100>{010} slip systems. More than 100 other B2 MR compounds are known to exist and many of them have already been shown to be ductile (e.g., CuY, AgY, CuDy, CoZr, CoTi, etc.). Furthermore, these alloys exhibit a large Bauschinger effect. The present work uses several diffraction based techniques including electron back scattered diffraction (EBSD), X-ray diffraction (XRD) and in-situ neutron diffraction; in conjunction with scanning electron microscopy (SEM), transmission electron microscopy (TEM), mechanical testing, and crystal plasticity modeling, to elucidate the reason for ductility in select B2 alloys, explore the spread of this ductility over the B2 family, and understand the Bauschinger effect in these alloys. Several possible explanations (e.g., slip of <111> dislocations, strong texture, phase transformations and twinning) for the anomalous ductility were explored. An X-ray diffraction based analysis ruled out texture, phase purity and departure from order as explanations for the anomalous ductility in MR alloys. In-situ neutron diffraction and post deformation SEM, EBSD, and TEM were unable to detect any evidence for phase transformations in CoTi and CoZr. Also, post deformation characterization did not reveal any evidence of twinning. However, TEM based g·b analysis and EBSD based in-grain misorientation axis (IGMA) analysis showed that beyond a transition in the strain hardening behavior in CoTi, slip modes involving dislocations with <110> and <111> Burgers vectors are activated. The slip of such dislocations can reduce stress concentrations that could otherwise lead to premature fracture, thus providing a satisfying explanation for the anomalous ductility of CoTi and related compounds, like CoZr. Dislocation self-energy calculations accounting for elastic anisotropy suggest that the choice of slip direction in these alloys is mobility-, rather than source-, limited. The reach of this "ductilizing effect" over B2 alloys was explored by producing, characterizing, and testing a number of simple metal-rare earth metal compounds, namely MgY, MgNd and MgCe. MgR intermetallics with the B2 structure were found to be brittle and exhibit a cleavage type fracture indicating that the ductilizing effect is not as widespread as was initially thought. MgY and MgNd were found to primarily cleave along the {100} planes, while MgCe was found to cleave on the {111} planes. A large Bauschinger effect was observed in several of the anomalously ductile B2 compounds, such that the material actually begins to yield in the reverse direction on unloading. When only the primary slip mode <100>{011} is active in CoZr (prior to a transition in strain hardening), the buildup of intergranular stresses is large and is chiefly responsible for the observed Bauschinger effect. However, past the aforementioned transition in strain hardening, the effect of intergranular stresses diminishes. The results demonstrate that the activation of hard, secondary slip modes causes the internal strains to develop more uniformly among the grains, thus reducing the intergranular stresses which cause the Bauschinger effect. Crystal plasticity modeling, which accounts for the initial paucity of independent slip modes and allows for the activation of complementary hard slip modes, reproduces these trends in the Bauschinger effect and provides additional evidence that the experimental observations have correctly identified the cause of the anomalous ductility.

Texture evolution during isothermal, isostrain, and isobaric loading of polycrystalline shape memory NiTi

NASA Astrophysics Data System (ADS)

Nicholson, D. E.; Padula, S. A.; Benafan, O.; Vaidyanathan, R.

2017-06-01

In situ neutron diffraction was used to provide insights into martensite variant microstructures during isothermal, isobaric, and isostrain loading in shape memory NiTi. The results show that variant microstructures were equivalent for the corresponding strain, and more importantly, the reversibility and equivalency were immediately evident in variant microstructures that were first formed isobarically but then reoriented to near random self-accommodated microstructures following isothermal deformation. Variant microstructures formed isothermally were not significantly affected by a subsequent thermal cycle under constant strain. In all loading cases considered, the resulting variant microstructure correlated with strain and did not correlate with stress. Based on the ability to select a variant microstructure for a given strain despite thermomechanical loading history, the results demonstrated here can be obtained by following any sequence of thermomechanical loading paths over multiple cycles. Thus, for training shape memory alloys (repeating thermomechanical cycling to obtain the desired variant microstructure), optimal paths can be selected so as to minimize the number of training cycles required, thereby increasing the overall stability and fatigue life of these alloys in actuator or medical applications.

Nano-chemo-mechanical signature of conventional oil-well cement systems: Effects of elevated temperature and curing time

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

Krakowiak, Konrad J., E-mail: kjkrak@mit.edu; Thomas, Jeffrey J., E-mail: JThomas39@slb.com; Musso, Simone, E-mail: SMusso@slb.com

2015-01-15

With ever more challenging (T,p) environments for cementing applications in oil and gas wells, there is a need to identify the fundamental mechanisms of fracture resistant oil well cements. We report results from a multi-technique investigation of behavior and properties of API class G cement and silica-enriched cement systems subjected to hydrothermal curing from 30 °C to 200 °C; including electron probe microanalysis, X-ray diffraction, thermogravimetry analysis, electron microscopy, neutron scattering (SANS), and fracture scratch testing. The results provide a new insight into the link between system chemistry, micro-texture and micro-fracture toughness. We suggest that the strong correlation found betweenmore » chemically modulated specific surface and fracture resistance can explain the drop in fracture properties of neat oil-well cements at elevated temperatures; the fracture property enhancement in silica-rich cement systems, between 110° and 175 °C; and the drop in fracture properties of such systems through prolonged curing over 1 year at 200 °C.« less

Deformation fields near a steady fatigue crack with anisotropic plasticity

DOE PAGES

Gao, Yanfei

2015-11-30

In this work, from finite element simulations based on an irreversible, hysteretic cohesive interface model, a steady fatigue crack can be realized if the crack extension exceeds about twice the plastic zone size, and both the crack increment per loading cycle and the crack bridging zone size are smaller than the plastic zone size. The corresponding deformation fields develop a plastic wake behind the crack tip and a compressive residual stress field ahead of the crack tip. In addition, the Hill’s plasticity model is used to study the role of plastic anisotropy on the retardation of fatigue crack growth andmore » the elastic strain fields. It is found that for Mode-I cyclic loading, an enhanced yield stress in directions that are inclined from the crack plane will lead to slower crack growth rate, but this retardation is insignificant for typical degrees of plastic anisotropy. Furthermore, these results provide key inputs for future comparisons to neutron and synchrotron diffraction measurements that provide full-field lattice strain mapping near fracture and fatigue crack tips, especially in textured materials such as wrought or rolled Mg alloys.« less

Deformation fields near a steady fatigue crack with anisotropic plasticity

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

Gao, Yanfei

In this work, from finite element simulations based on an irreversible, hysteretic cohesive interface model, a steady fatigue crack can be realized if the crack extension exceeds about twice the plastic zone size, and both the crack increment per loading cycle and the crack bridging zone size are smaller than the plastic zone size. The corresponding deformation fields develop a plastic wake behind the crack tip and a compressive residual stress field ahead of the crack tip. In addition, the Hill’s plasticity model is used to study the role of plastic anisotropy on the retardation of fatigue crack growth andmore » the elastic strain fields. It is found that for Mode-I cyclic loading, an enhanced yield stress in directions that are inclined from the crack plane will lead to slower crack growth rate, but this retardation is insignificant for typical degrees of plastic anisotropy. Furthermore, these results provide key inputs for future comparisons to neutron and synchrotron diffraction measurements that provide full-field lattice strain mapping near fracture and fatigue crack tips, especially in textured materials such as wrought or rolled Mg alloys.« less

Uncovering three-dimensional gradients in fibrillar orientation in an impact-resistant biological armour.

PubMed

Zhang, Y; Paris, O; Terrill, N J; Gupta, H S

2016-05-23

The complex hierarchical structure in biological and synthetic fibrous nanocomposites entails considerable difficulties in the interpretation of the crystallographic texture from diffraction data. Here, we present a novel reconstruction method to obtain the 3D distribution of fibres in such systems. An analytical expression is derived for the diffraction intensity from fibres, explaining the azimuthal intensity distribution in terms of the angles of the three dimensional fibre orientation distributions. The telson of stomatopod (mantis shrimp) serves as an example of natural biological armour whose high impact resistance property is believed to arise from the hierarchical organization of alpha chitin nanofibrils into fibres and twisted plywood (Bouligand) structures at the sub-micron and micron scale. Synchrotron microfocus scanning X-ray diffraction data on stomatopod telson were used as a test case to map the 3D fibre orientation across the entire tissue section. The method is applicable to a range of biological and biomimetic structures with graded 3D fibre texture at the sub-micron and micron length scales.

Uncovering three-dimensional gradients in fibrillar orientation in an impact-resistant biological armour

NASA Astrophysics Data System (ADS)

Zhang, Y.; Paris, O.; Terrill, N. J.; Gupta, H. S.

2016-05-01

The complex hierarchical structure in biological and synthetic fibrous nanocomposites entails considerable difficulties in the interpretation of the crystallographic texture from diffraction data. Here, we present a novel reconstruction method to obtain the 3D distribution of fibres in such systems. An analytical expression is derived for the diffraction intensity from fibres, explaining the azimuthal intensity distribution in terms of the angles of the three dimensional fibre orientation distributions. The telson of stomatopod (mantis shrimp) serves as an example of natural biological armour whose high impact resistance property is believed to arise from the hierarchical organization of alpha chitin nanofibrils into fibres and twisted plywood (Bouligand) structures at the sub-micron and micron scale. Synchrotron microfocus scanning X-ray diffraction data on stomatopod telson were used as a test case to map the 3D fibre orientation across the entire tissue section. The method is applicable to a range of biological and biomimetic structures with graded 3D fibre texture at the sub-micron and micron length scales.

Uncovering three-dimensional gradients in fibrillar orientation in an impact-resistant biological armour

PubMed Central

Zhang, Y.; Paris, O.; Terrill, N. J.; Gupta, H. S.

2016-01-01

The complex hierarchical structure in biological and synthetic fibrous nanocomposites entails considerable difficulties in the interpretation of the crystallographic texture from diffraction data. Here, we present a novel reconstruction method to obtain the 3D distribution of fibres in such systems. An analytical expression is derived for the diffraction intensity from fibres, explaining the azimuthal intensity distribution in terms of the angles of the three dimensional fibre orientation distributions. The telson of stomatopod (mantis shrimp) serves as an example of natural biological armour whose high impact resistance property is believed to arise from the hierarchical organization of alpha chitin nanofibrils into fibres and twisted plywood (Bouligand) structures at the sub-micron and micron scale. Synchrotron microfocus scanning X-ray diffraction data on stomatopod telson were used as a test case to map the 3D fibre orientation across the entire tissue section. The method is applicable to a range of biological and biomimetic structures with graded 3D fibre texture at the sub-micron and micron length scales. PMID:27211574

Multiscale measurements on temperature-dependent deformation of a textured magnesium alloy with synchrotron x-ray imaging and diffraction

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

Lu, L.; Bie, B. X.; Li, Q. H.

2017-06-01

In situ synchrotron x-ray imaging and diffraction are used to investigate deformation of a rolled magnesium alloy under uniaxial compression at room and elevated temperatures along two different directions. The loading axis (LA) is either perpendicular or parallel to the normal direction, and these two cases are referred to as LA⊥ and LAk loading, respectively. Multiscale measurements including stressestrain curves (macroscale), strain fields (mesoscale), and diffraction patterns (microscale) are obtained simultaneously. Due to initial texture, f1012g extension twinning is predominant in the LA⊥ loading, while dislocation motion prevails in the LAk loading. With increasing temperature, fewer f1012g extension twins aremore » activated in the LA⊥ samples, giving rise to reduced strain homogenization, while pyramidal slip becomes readily activated, leading to more homogeneous deformation for the LAk loading. The difference in the strain hardening rates is attributed to that in strain field homogenization for these two loading directions« less

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.

Single crystal to polycrystal neutron transmission simulation

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

Dessieux, Luc Lucius; Stoica, Alexandru Dan; Bingham, Philip R.

A collection of routines for calculation of the total cross section that determines the attenuation of neutrons by crystalline solids is presented. The total cross section is calculated semi-empirically as a function of crystal structure, neutron energy, temperature, and crystal orientation. The semi-empirical formula includes the contribution of parasitic Bragg scattering to the total cross section using both the crystal’s mosaic spread value and its orientation with respect to the neutron beam direction as parameters. These routines allow users to enter a distribution of crystal orientations for calculation of total cross sections of user defined powder or pseudo powder distributions,more » which enables simulation of non-uniformities such as texture and strain. In conclusion, the spectra for neutron transmission simulations in the neutron thermal energy range (2 meV–100 meV) are presented for single crystal and polycrystal samples and compared to measurements.« less

Single crystal to polycrystal neutron transmission simulation

DOE PAGES

Dessieux, Luc Lucius; Stoica, Alexandru Dan; Bingham, Philip R.

2018-02-02

A collection of routines for calculation of the total cross section that determines the attenuation of neutrons by crystalline solids is presented. The total cross section is calculated semi-empirically as a function of crystal structure, neutron energy, temperature, and crystal orientation. The semi-empirical formula includes the contribution of parasitic Bragg scattering to the total cross section using both the crystal’s mosaic spread value and its orientation with respect to the neutron beam direction as parameters. These routines allow users to enter a distribution of crystal orientations for calculation of total cross sections of user defined powder or pseudo powder distributions,more » which enables simulation of non-uniformities such as texture and strain. In conclusion, the spectra for neutron transmission simulations in the neutron thermal energy range (2 meV–100 meV) are presented for single crystal and polycrystal samples and compared to measurements.« less

Annealing effect and photovoltaic properties of nano-ZnS/textured p-Si heterojunction.

PubMed

Ji, Liang-Wen; Hsiao, Yu-Jen; Tang, I-Tseng; Meen, Teen-Hang; Liu, Chien-Hung; Tsai, Jenn-Kai; Wu, Tien-Chuan; Wu, Yue-Sian

2013-11-09

The preparation and characterization of heterojunction solar cell with ZnS nanocrystals synthesized by chemical bath deposition method were studied in this work. The ZnS nanocrystals were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Lower reflectance spectra were found as the annealing temperature of ZnS film increased on the textured p-Si substrate. It was found that the power conversion efficiency (PCE) of the AZO/ZnS/textured p-Si heterojunction solar cell with an annealing temperature of 250°C was η = 3.66%.

Annealing effect and photovoltaic properties of nano-ZnS/textured p-Si heterojunction

PubMed Central

2013-01-01

The preparation and characterization of heterojunction solar cell with ZnS nanocrystals synthesized by chemical bath deposition method were studied in this work. The ZnS nanocrystals were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Lower reflectance spectra were found as the annealing temperature of ZnS film increased on the textured p-Si substrate. It was found that the power conversion efficiency (PCE) of the AZO/ZnS/textured p-Si heterojunction solar cell with an annealing temperature of 250°C was η = 3.66%. PMID:24206942

Annealing effect and photovoltaic properties of nano-ZnS/textured p-Si heterojunction

NASA Astrophysics Data System (ADS)

Ji, Liang-Wen; Hsiao, Yu-Jen; Tang, I.-Tseng; Meen, Teen-Hang; Liu, Chien-Hung; Tsai, Jenn-Kai; Wu, Tien-Chuan; Wu, Yue-Sian

2013-11-01

The preparation and characterization of heterojunction solar cell with ZnS nanocrystals synthesized by chemical bath deposition method were studied in this work. The ZnS nanocrystals were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Lower reflectance spectra were found as the annealing temperature of ZnS film increased on the textured p-Si substrate. It was found that the power conversion efficiency (PCE) of the AZO/ZnS/textured p-Si heterojunction solar cell with an annealing temperature of 250°C was η = 3.66%.

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.

Light Management in Transparent Conducting Oxides by Direct Fabrication of Periodic Surface Arrays

NASA Astrophysics Data System (ADS)

Eckhardt, S.; Sachse, C.; Lasagni, A. F.

Line- and hexagonal-like periodic textures were fabricated on aluminium zinc oxide (AZO) using direct laser interference patterning method. It was found that hexagonally patterned surfaces show a higher performance in both transparency and diffraction properties compared to line-like textured and non-patterned substrates. Furthermore, the electrical resistance of the processed AZO coated substrates remained below the tolerance values for transparent conducting electrodes.

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.

Influence of different kinds of rolling on the crystallographic texture and magnetic induction of a NOG 3 wt% Si steel

NASA Astrophysics Data System (ADS)

Silva, J. M.; Baêta Júnior, E. S.; Moraes, N. R. D. C.; Botelho, R. A.; Felix, R. A. C.; Brandao, L.

2017-01-01

The purpose of this work was to study the influence of different kinds of rolling on the magnetic properties of NOG steel, an electric steel widely used in electrical motors. These properties are highly correlated with the crystallographic texture of the material, which can be changed by rolling. Three kinds of rolling were examined: conventional rolling, cross-rolling and asymmetrical rolling. The crystallographic texture was determined by X-ray diffraction and the magnetic properties were calculated from a theoretical model that related the magnetic induction to crystallographic texture through the anisotropy energy. The results show that cross-rolling yields higher values of magnetic induction than the other processes.

Crystallographic texture in pulsed laser deposited hydroxyapatite bioceramic coatings

PubMed Central

Kim, Hyunbin; Camata, Renato P.; Lee, Sukbin; Rohrer, Gregory S.; Rollett, Anthony D.; Vohra, Yogesh K.

2008-01-01

The orientation texture of pulsed laser deposited hydroxyapatite coatings was studied by X-ray diffraction techniques. Increasing the laser energy density of the KrF excimer laser used in the deposition process from 5 to 7 J/cm2 increases the tendency for the c-axes of the hydroxyapatite grains to be aligned perpendicular to the substrate. This preferred orientation is most pronounced when the incidence direction of the plume is normal to the substrate. Orientation texture of the hydroxyapatite grains in the coatings is associated with the highly directional and energetic nature of the ablation plume. Anisotropic stresses, transport of hydroxyl groups and dehydroxylation effects during deposition all seem to play important roles in the texture development. PMID:18563207

Unraveling skyrmion spin texture using resonant soft x-ray scattering

NASA Astrophysics Data System (ADS)

Roy, Sujoy

2015-03-01

The recent discovery of skyrmions, that were originally predicted in context of high energy physics, in magnetic materials has sparked tremendous interest in the research community due to its rich physics and potential in spintronics applications. Skyrmions have an unusual spin texture that manifests as magnetic knot and can be easily moved around. Understanding the fundamental physics and mechanisms for controlling their dynamical properties presents important scientific challenges. So far experimental verifications of the skyrmions in magnetic systems have come from neutron scattering and Lorentz transmission electron microscopy (TEM) measurements. In this talk we report the first observation of the skyrmions using resonant soft x-ray scattering. We have used soft x-rays tuned to the Cu L3 edge to diffract off the skyrmion lattice in a multiferroic Cu2OSeO3 compound. We show that in Cu2OSeO3 there exist two skyrmion lattices arising due to the two inequivalent Cu-O sublattices that have two different magnetically active d-orbitals. The two skyrmion sublattices are mutually rotated with respect to each other. The angle of rotation could be changed by an external magnetic field, thereby indicating possible existence of a new phase. We have also studied skyrmion spin texture in an ultra-thin Fe/Gd multilayer that shows perpendicular anisotropy. The Fe/Gd sample exhibits a near perfect aligned stripe phase. Within a small range of temperature and magnetic field we observe a hexagonal scattering pattern due to skyrmion bubbles. Analysis of the scattering pattern suggests that the skyrmion lattice unit cell contains two skyrmions. The biskyrmion state is also revealed by Lorentz TEM images. The near room temperature discovery of skyrmion in a technology relevant material is a significant step towards using skyrmions in magnetic devices. Work at LBNL was supported by the Office of Basic Energy Sciences of the U.S. Department of Energy (Contract No. DE-AC02-05CH11231).

Extrapolation of bulk rock elastic moduli of different rock types to high pressure conditions and comparison with texture-derived elastic moduli

NASA Astrophysics Data System (ADS)

Ullemeyer, Klaus; Lokajíček, Tomás; Vasin, Roman N.; Keppler, Ruth; Behrmann, Jan H.

2018-02-01

In this study elastic moduli of three different rock types of simple (calcite marble) and more complex (amphibolite, micaschist) mineralogical compositions were determined by modeling of elastic moduli using texture (crystallographic preferred orientation; CPO) data, experimental investigation and extrapolation. 3D models were calculated using single crystal elastic moduli, and CPO measured using time-of-flight neutron diffraction at the SKAT diffractometer in Dubna (Russia) and subsequently analyzed using Rietveld Texture Analysis. To define extrinsic factors influencing elastic behaviour, P-wave and S-wave velocity anisotropies were experimentally determined at 200, 400 and 600 MPa confining pressure. Functions describing variations of the elastic moduli with confining pressure were then used to predict elastic properties at 1000 MPa, revealing anisotropies in a supposedly crack-free medium. In the calcite marble elastic anisotropy is dominated by the CPO. Velocities continuously increase, while anisotropies decrease from measured, over extrapolated to CPO derived data. Differences in velocity patterns with sample orientation suggest that the foliation forms an important mechanical anisotropy. The amphibolite sample shows similar magnitudes of extrapolated and CPO derived velocities, however the pattern of CPO derived velocity is closer to that measured at 200 MPa. Anisotropy decreases from the extrapolated to the CPO derived data. In the micaschist, velocities are higher and anisotropies are lower in the extrapolated data, in comparison to the data from measurements at lower pressures. Generally our results show that predictions for the elastic behavior of rocks at great depths are possible based on experimental data and those computed from CPO. The elastic properties of the lower crust can, thus, be characterized with an improved degree of confidence using extrapolations. Anisotropically distributed spherical micro-pores are likely to be preserved, affecting seismic velocity distributions. Compositional variations in the polyphase rock samples do not significantly change the velocity patterns, allowing the use of RTA-derived volume percentages for the modeling of elastic moduli.

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

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

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.

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).

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.

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

Shear-Coupled Grain Growth and Texture Development in a Nanocrystalline Ni-Fe Alloy during Cold Rolling

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

Li, Li; Ungár, Tamás; Toth, Laszlo S.

The evolution of texture, grain size, grain shape, dislocation and twin density has been determined by synchrotron X-ray diffraction and line profile analysis in a nanocrystalline Ni- Fe alloy after cold rolling along different directions related to the initial fiber and the long axis of grains. The texture evolution has been simulated by the Taylor-type relaxed constraints viscoplastic polycrystal model. The simulations were based on the activity of partial dislocations in correlation with the experimental results of dislocation density determination. The concept of stress-induced shear-coupling is supported and strengthened by both the texture simulations and the experimentally determined evolution ofmore » the microstructure parameters. Grain-growth and texture evolution are shown to proceed by the shear-coupling mechanism supported by dislocation activity as long as the grain size is not smaller than about 20 nm.« less

Strength and texture of Pt compressed to 63 GPa

NASA Astrophysics Data System (ADS)

Dorfman, Susannah M.; Shieh, Sean R.; Duffy, Thomas S.

2015-02-01

Angle- and energy-dispersive X-ray diffraction experiments in a radial geometry were performed in the diamond anvil cell on polycrystalline platinum samples at pressures up to 63 GPa. Observed yield strength and texture depend on grain size. For samples with 70-300-nm particle size, the yield strength is 5-6 GPa at ˜60 GPa. Coarse-grained (˜2-μm particles) Pt has a much lower yield strength of 1-1.5 GPa at ˜60 GPa. Face-centered cubic metals Pt and Au have lower strength to shear modulus ratio than body-centered cubic or hexagonal close-packed metals. While a 300-nm particle sample exhibits the <110> texture expected of face-centered-cubic metals under compression, smaller and larger particles show a weak mixed <110> and <100> texture under compression. Differences in texture development may also occur due to deviations from uniaxial stress under compression in the diamond anvil cell.

Catalogue of X-Ray Texture Data for Al-Cu-Li Alloy 1460, 2090, 2096 and 2195 Near-Net-Shape Extrusions, Sheet and Plate

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Hafley, Robert A.; Alexa, Joel A.

1998-01-01

The effect of crystallographic texture on the mechanical properties of near-net-shape extrusions is of major interest ff these products are to find application in launch vehicle or aircraft structures. The objective of this research was to produce a catalogue containing quantitative texture information for extruded product, sheet and plate. The material characterized was extracted from wide, integrally stiffened panels fabricated from the Al-Cu-Li alloys 1460, 2090, 2096 and 2195. The textural characteristics of sheet and plate products of the same alloys were determined for comparison purposes. The approach involved using X-ray diffraction to generate pole figures in combination with orientation distribution function analysis. The data were compiled as a function of location in the extruded cross-sections and the variation in the major deformation- and recrystallization-related texture components was identified.

Texture-Induced Anisotropy in an Inconel 718 Alloy Deposited Using Electron Beam Freeform Fabrication

NASA Technical Reports Server (NTRS)

Tayon, W.; Shenoy, R.; Bird, R.; Hafley, R.; Redding, M.

2014-01-01

A test block of Inconel (IN) 718 was fabricated using electron beam freeform fabrication (EBF(sup 3)) to examine how the EBF(sup 3) deposition process affects the microstructure, crystallographic texture, and mechanical properties of IN 718. Tests revealed significant anisotropy in the elastic modulus for the as-deposited IN 718. Subsequent tests were conducted on specimens subjected to a heat treatment designed to decrease the level of anisotropy. Electron backscatter diffraction (EBSD) was used to characterize crystallographic texture in the as-deposited and heat treated conditions. The anisotropy in the as-deposited condition was strongly affected by texture as evidenced by its dependence on orientation relative to the deposition direction. Heat treatment resulted in a significant improvement in modulus of the EBF(sup 3) product to a level nearly equivalent to that for wrought IN 718 with reduced anisotropy; reduction in texture through recrystallization; and production of a more homogeneous microstructure.

Texture evolution during nitinol martensite detwinning and phase transformation

NASA Astrophysics Data System (ADS)

Cai, S.; Schaffer, J. E.; Ren, Y.; Yu, C.

2013-12-01

Nitinol has been widely used to make medical devices for years due to its unique shape memory and superelastic properties. However, the texture of the nitinol wires has been largely ignored due to inherent complexity. In this study, in situ synchrotron X-ray diffraction has been carried out during uniaxial tensile testing to investigate the texture evolution of the nitinol wires during martensite detwinning, variant reorientation, and phase transformation. It was found that the thermal martensitic nitinol wire comprised primarily an axial (1¯20), (120), and (102)-fiber texture. Detwinning initially converted the (120) and (102) fibers to the (1¯20) fiber and progressed to a (1¯30)-fiber texture by rigid body rotation. At strains above 10%, the (1¯30)-fiber was shifted to the (110) fiber by (21¯0) deformation twinning. The austenitic wire exhibited an axial (334)-fiber, which transformed to the near-(1¯30) martensite texture after the stress-induced phase transformation.

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

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

In Situ Assessment of Lattice in an Al-Li Alloy

NASA Technical Reports Server (NTRS)

Beaudoin, A. J.; Obstalecki, M.; Tayon, W.; Hernquist, M.; Mudrock, R.; Kenesei, P.; Lienert, U.

2013-01-01

The lattice strains of individual grains are measured in an Al-Li alloy, AA 2195, using high-energy X-ray diffraction at a synchrotron source. The diffraction of individual grains in this highly textured production alloy was isolated through use of a depth-defining aperture. It is shown that hydrostatic stress, and in turn the stress triaxiality, can vary significantly from grain to grain.

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...

A quasi-in-situ EBSD observation of the transformation from rolling texture to recrystallization texture in V-4Cr-4Ti alloy

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

Peng, Lixia

Recrystallization texture evolution of rolled V-4Cr-4Ti alloy has been investigated by quasi-in-situ EBSD (electron back-scattering diffraction) method. Concurrently, the precipitates were characterized by SEM (Scanning Electron Microscopy). It was found that both the initial rolling textures and the distribution of the precipitates affected the formation of the recrystallization texture. It was revealed that the texture transformations of (558) 〈110〉 + (665) 〈110〉 to (334) 〈483〉 + (665) 〈1 1 2.4〉 were possibly attributed to the selective drag induced by the sparsely dispersed Ti-rich precipitates. While the densely distributed Ti-rich precipitates were responsible for the randomized recrystallization texture. Finally, when themore » precipitates were absent, the orientation changes from (112) 〈110〉 and (558) 〈110〉 to (111) 〈112〉 and (001) <110> to (001) <520> were observed. - Highlights: • Micro recrystallization texture evolution in V-4Cr-4Ti alloys is reported for the first time. • The volume fraction of Ti-rich precipitates has significant effect on the recrystallization texture evolution. • The dissolution of the Ti-rich precipitates above 1100 °C induces the strengthening of (111) <112> texture.« less

Incident flux angle induced crystal texture transformation in nanostructured molybdenum films

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

Chen, L.; Lu, T.-M.; Wang, G.-C.

2012-07-15

Molybdenum films were observed to undergo a dramatic change in crystal texture orientation when the incident flux angle was varied in an oblique angle sputter deposition on amorphous substrates. Reflection high-energy electron diffraction pole figure and scanning electron microscopy were used to analyze in detail the texture orientation of the films. The normal incident deposition resulted in a fiber texture film with the minimum energy (110) crystal plane parallel to the substrate surface. A (110)[110] biaxial texture was observed for the samples grown with low incident angles of less than 45 Degree-Sign , with respect to the surface normal. Onmore » the other hand, for an oblique angle deposition of larger than 60 Degree-Sign , a (111)[112] biaxial texture was observed and appeared to be consistent with a zone T structure where the geometrically fastest growth [001] direction of a crystal plays a dominant role in defining the texture. We argue that a structural transition had occurred when the incident flux was varied from near normal incidence to a large angle.« less

Microstructural and Textural Differences Induced by Water and Furnace Cooling in Commercially Pure Zr Annealed in the α + β Region

NASA Astrophysics Data System (ADS)

Chai, Linjiang; Wang, Tingting; Ren, Yi; Song, Bo; Guo, Ning; Chen, Liangyu

2018-07-01

In this work, a commercially pure Zr sheet with a typical bimodal basal texture was annealed in an α + β region and then subjected to different coolings (in water and furnace). Microstructures and textures of both the as-received and the heat-treated specimens were investigated by electron channeling contrast imaging and electron backscatter diffraction techniques. Results show that a duplex microstructure consisting of untransformed bulk α grains and twinned martensitic plates is produced in the water-cooled specimen, which possesses a weakened texture compared to the initial one. For the specimen cooled in furnace, however, a uniform microstructure fully comprised of coarser equiaxed grains with a strengthened texture is obtained. Analyses reveal that the rapid cooling in water could suppress variant selection behaviors during β → α transformation and allow α plates with scattered orientations to be nucleated inside β phases, contributing to the weakened texture. In contrast, during slow cooling in furnace, β boundaries would act as preferred nucleation sites of α embryos, resulting in a strong variant selection that accounts for the intensified texture.

Microstructural and Textural Differences Induced by Water and Furnace Cooling in Commercially Pure Zr Annealed in the α + β Region

NASA Astrophysics Data System (ADS)

Chai, Linjiang; Wang, Tingting; Ren, Yi; Song, Bo; Guo, Ning; Chen, Liangyu

2018-03-01

In this work, a commercially pure Zr sheet with a typical bimodal basal texture was annealed in an α + β region and then subjected to different coolings (in water and furnace). Microstructures and textures of both the as-received and the heat-treated specimens were investigated by electron channeling contrast imaging and electron backscatter diffraction techniques. Results show that a duplex microstructure consisting of untransformed bulk α grains and twinned martensitic plates is produced in the water-cooled specimen, which possesses a weakened texture compared to the initial one. For the specimen cooled in furnace, however, a uniform microstructure fully comprised of coarser equiaxed grains with a strengthened texture is obtained. Analyses reveal that the rapid cooling in water could suppress variant selection behaviors during β → α transformation and allow α plates with scattered orientations to be nucleated inside β phases, contributing to the weakened texture. In contrast, during slow cooling in furnace, β boundaries would act as preferred nucleation sites of α embryos, resulting in a strong variant selection that accounts for the intensified texture.

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.

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.

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

The effect of texture in (Bi3.5Nd0.5)(Ti2.97Nb0.03)O12 ceramics

NASA Astrophysics Data System (ADS)

Cao, Ziping; Ding, Aili; Zheng, Xinsen; Qiu, Pingsun; Cheng, Wenxiu

2004-11-01

(Bi3.5Nd0.5) (Ti2.97Nb0.03)O12 ferroelectric ceramics was successfully prepared by a hot-pressing method. XRD diffraction confirms that the samples hold different texture in the sliced planes parallel and perpendicular to the hot-pressing axis, respectively. The anisotropy of ferroelectric, dielectric and piezoelectric properties were all observed in the textured ceramics. Due to the great improvement of ferroelectric and piezoelectric properties, the sample which was sliced along the direction parallel to the hot-pressing axis can be considered as a good candidate of high temperature piezoelectric materials.

Relation between textured surface and diffuse reflectance of Cu films

NASA Astrophysics Data System (ADS)

Shukla, Gaurav; Angappane, S.

2018-04-01

Cu nanostructures namely chevron, slanted and vertical posts deposited on Si substrate by glancing angle deposition (GLAD) technique using DC magnetron sputtering are studied to understand the optical reflectance properties of various textures. The X-ray diffraction analysis confirmed the crystalline nature of the different structures of deposited Cu films. The FESEM images confirmed the formation of chevron, slanted and vertical posts. From the optical reflectance spectra, we found that the reflectance is more for chevron than vertical and slanted posts which have almost the same reflectance over the entire wavelength. The films with chevron texture would find various applications, like, light detector, light trapping, sensors etc.

Hybrid processing and anisotropic sintering shrinkage in textured ZnO ceramics

PubMed Central

Keskinbora, Kahraman; Suzuki, Tohru S; Ozgur Ozer, I; Sakka, Yoshio; Suvaci, Ender

2010-01-01

We have studied the combined effects of the templated grain growth and magnetic alignment processes on sintering, anisotropic sintering shrinkage, microstructure development and texture in ZnO ceramics. Suspensions of 0–10 vol % ZnO template particles were slip cast in a 12 T rotating magnetic field. Sintering and texture characteristics were investigated via thermomechanical analysis and electron backscatter diffraction, respectively. Sintering as well as texture characteristics depend on template concentration. For the studied ZnO system, there is a critical template concentration (2 vol % in this study) above which densification is limited by the templates owing to constrained sintering. Below this limit, the densification is enhanced and the anisotropic shrinkage is reduced, which is attributed to densifying characteristics of the templates. PMID:27877373

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.

Enhancement of Stereo Imagery by Artificial Texture Projection Generated Using a LIDAR

NASA Astrophysics Data System (ADS)

Veitch-Michaelis, Joshua; Muller, Jan-Peter; Walton, David; Storey, Jonathan; Foster, Michael; Crutchley, Benjamin

2016-06-01

Passive stereo imaging is capable of producing dense 3D data, but image matching algorithms generally perform poorly on images with large regions of homogenous texture due to ambiguous match costs. Stereo systems can be augmented with an additional light source that can project some form of unique texture onto surfaces in the scene. Methods include structured light, laser projection through diffractive optical elements, data projectors and laser speckle. Pattern projection using lasers has the advantage of producing images with a high signal to noise ratio. We have investigated the use of a scanning visible-beam LIDAR to simultaneously provide enhanced texture within the scene and to provide additional opportunities for data fusion in unmatched regions. The use of a LIDAR rather than a laser alone allows us to generate highly accurate ground truth data sets by scanning the scene at high resolution. This is necessary for evaluating different pattern projection schemes. Results from LIDAR generated random dots are presented and compared to other texture projection techniques. Finally, we investigate the use of image texture analysis to intelligently project texture where it is required while exploiting the texture available in the ambient light image.

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

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

Textures of water-rich mud sediments from the continental margin offshore Costa Rica (IODP expeditions 334 and 344)

NASA Astrophysics Data System (ADS)

Kuehn, Rebecca; Stipp, Michael; Leiss, Bernd

2017-04-01

During sedimentation and burial at continental margins, clay-rich sediments develop crystallographic preferred orientations (textures) depending on the ongoing compaction as well as size distribution and shape fabrics of the grains. Such textures can control the deformational properties of these sediments and hence the strain distribution in active continental margins and also the frictional behavior along and around the plate boundary. Strain-hardening and discontinuous deformation may lead to earthquake nucleation at or below the updip limit of the seismogenic zone. We want to investigate the active continental margin offshore Costa Rica where the oceanic Cocos plate is subducted below the Caribbean plate at a rate of approximately 9 cm per year. The Costa Rica trench is well-known for shallow seismogenesis and tsunami generation. As it is an erosive continental margin, both the incoming sediments from the Nazca plate as well as the slope sediments of the continental margin can be important for earthquake nucleation and faulting causing sea-floor breakage. To investigate texture and composition of the sediments and hence their deformational properties we collected samples from varying depth of 7 different drilling locations across the trench retrieved during IODP expeditions 334 and 344 as part of the Costa Rica Seismogenesis Project (CRISP). Texture analysis was carried out by means of synchrotron diffraction, as only this method is suitable for water-bearing samples. As knowledge on the sediment composition is required as input parameter for the texture data analysis, additional X-ray powder diffraction analysis on the sample material has been carried out. Samples for texture measurements were prepared from the original drill cores using an internally developed cutter which allows to produce cylindrical samples with a diameter of about 1.5 cm. The samples are oriented with respect to the drill core axis. Synchrotron texture measurements were conducted at the ESRF (European Synchrotron Radiation Facility) in Grenoble and the DESY (German Electron Synchrotron) in Hamburg. Samples were measured in transmission mode perpendicular to their cylinder axis with a beam diameter of 500 µm. Measurements were taken from 0 to 175° in 5° steps resulting in 36 images from a 2D image plate detector. Measurement time was in a range from 1 to 3 seconds. Due to the different, low symmetric mineral phases a large number of mostly overlapping reflections results. Such data can only be analyzed by the Rietveld method, in our case implemented in the software package MAUD (Materials Analysis Using Diffraction). Preliminary results show distinct textures depending on the composition and the origin of the samples, i.e. on drilling location and depth, which may be critical for strain localization and faulting of these samples. The results are also important for the analysis of experimentally deformed samples from the same drill cores which showed structurally weak and structurally strong deformation behavior during triaxial compression.

Local texture and grain boundary misorientations in high H(C) oxide superconductors

NASA Astrophysics Data System (ADS)

Kroeger, D. M.; Goyal, A.; Specht, E. D.; Tkaczyk, J. E.; Sutliff, J.; Deluca, J. A.; Wang, Z. L.; Riley, G. N., Jr.

The orientations of hundreds of contiguous grains in high J(C) TlBa2Ca2Cu3O(x) deposits and (Bi, Pb)2 Sr2Ca2Cu3O(y) powder-in-tube tapes have been determined from electron back scatter diffraction patterns (EBSP). The misorientation angles and axes of rotation (angle/axis pairs) for grain boundaries connecting these grains were calculated. For both materials the population of low angle boundaries was found to be much larger than expected from calculations based on the macroscopic texture. The TlBa2Ca2Cu3O(x) deposits exhibit pronounced local texture which has been defined by EBSP and x-ray diffraction. Locally grains show significant in-plane (a-axis) alignment even though macroscopically a-axes are random, indicating the presence of colonies of grains with similar a-axis orientations. In (Bi, Pb)2 Sr2Ca2Cu3O(x) tapes no local texture was observed. In both materials the existence of connected networks of small angle grain boundaries can be inferred. Coincident site lattice (CSL) grain boundaries are also present in higher than expected numbers. Grain boundary energy thus appears to play a significant role in enhancing the population of potentially strongly-linked boundaries. We propose that long range strongly-linked conduction occurs through a percolative network small angle (and perhaps CSL) grain boundaries.

Measuring twinning and slip in shock-compressed Ta from in-situ x-ray diffraction

NASA Astrophysics Data System (ADS)

Wehrenberg, Christopher; McGonegle, David; Sliwa, Marcin; Suggit, Matt; Wark, Justin; Lee, Hae Ja; Nagler, Bob; Tavella, Franz; Remington, Bruce; Rudd, Rob; Lazicki, Amy; Park, Hye-Sook; Swift, Damian; Zepeda-Ruiz, Louis; Higginbotham, Andrew; Bolme, Cindy

2017-06-01

A fundamental understanding of high-pressure and high-strain-rate deformation rests on grasping the underlying microstructural processes, such as twinning and dislocation generation and transport (slip), yet simulations and ex-post-facto recovery experiments provide conflicting answers to these basic issues. Here, we report direct, in-situ observation of twinning and slip in shock compressed Ta using in-situ x-ray diffraction. A series of shock experiments were performed on the Matter in Extreme Conditions end station at LCLS. Direct laser ablation was used to drive a shock, ranging in pressure from 10-300 GPa, into a Ta sample with an initial (110) fiber texture. The subsequent changes in texture were observed in-situ by examining the azimuthal distribution of the diffraction intensity and found to match twinning and lattice rotation. Measurements of the twin fraction and lattice rotation were used to calculate the equivalent plastic strain from twinning and slip. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

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.

Neutron Scattering Studies on Large Length Scale Sample Structures

NASA Astrophysics Data System (ADS)

Feng, Hao

Neutron scattering can be used to study structures of matter. Depending on the interested sample properties, different scattering techniques can be chosen. Neutron reflectivity is more often used to detect in-depth profile of layered structures and the interfacial roughness while transmission is more sensitive to sample bulk properties. Neutron Reflectometry (NR) technique, one technique in neutron reflectivity, is first discussed in this thesis. Both specular reflectivity and the first order Bragg intensity were measured in the NR experiment with a diffraction grating in order to study the in-depth and the lateral structure of a sample (polymer) deposited on the grating. However, the first order Bragg intensity solely is sometimes inadequate to determine the lateral structure and high order Bragg intensities are difficult to measure using traditional neutron scattering techniques due to the low brightness of the current neutron sources. Spin Echo Small Angle Neutron Scattering (SESANS) technique overcomes this resolution problem by measuring the Fourier transforms of all the Bragg intensities, resulting in measuring the real-space density correlations of samples and allowing the accessible length scale from few-tens of nanometers to several microns. SESANS can be implemented by using two pairs of magnetic Wollaston prims (WP) and the accessible length scale is proportional to the magnetic field intensity in WPs. To increase the magnetic field and thus increase the accessible length scale, an apparatus named Superconducting Wollaston Prisms (SWP) which has a series of strong, well-defined shaped magnetic fields created by superconducting coils was developed in Indiana University in 2016. Since then, various kinds of optimization have been implemented, which are addressed in this thesis. Finally, applications of SWPs in other neutron scattering techniques like Neutron Larmor Diffraction (NLD) are discussed.

Crystallography of refractory metal nuggets in carbonaceous chondrites: A transmission Kikuchi diffraction approach

NASA Astrophysics Data System (ADS)

Daly, Luke; Bland, Phil A.; Dyl, Kathryn A.; Forman, Lucy V.; Saxey, David W.; Reddy, Steven M.; Fougerouse, Denis; Rickard, William D. A.; Trimby, Patrick W.; Moody, Steve; Yang, Limei; Liu, Hongwei; Ringer, Simon P.; Saunders, Martin; Piazolo, Sandra

2017-11-01

Transmission Kikuchi diffraction (TKD) is a relatively new technique that is currently being developed for geological sample analysis. This technique utilises the transmission capabilities of a scanning electron microscope (SEM) to rapidly and accurately map the crystallographic and geochemical features of an electron transparent sample. TKD uses a similar methodology to traditional electron backscatter diffraction (EBSD), but is capable of achieving a much higher spatial resolution (5-10 nm) (Trimby, 2012; Trimby et al., 2014). Here we apply TKD to refractory metal nuggets (RMNs) which are micrometre to sub-micrometre metal alloys composed of highly siderophile elements (HSEs) found in primitive carbonaceous chondrite meteorites. TKD allows us to analyse RMNs in situ, enabling the characterisation of nanometre-scale variations in chemistry and crystallography, whilst preserving their spatial and crystallographic context. This provides a complete representation of each RMN, permitting detailed interpretation of their formation history. We present TKD analysis of five transmission electron microscopy (TEM) lamellae containing RMNs coupled with EBSD and TEM analyses. These analyses revealed textures and relationships not previously observed in RMNs. These textures indicate some RMNs experienced annealing, forming twins. Some RMNs also acted as nucleation centres, and formed immiscible metal-silicate fluids. In fact, each RMN analysed in this study had different crystallographic textures. These RMNs also had heterogeneous compositions, even between RMNs contained within the same inclusion, host phase and even separated by only a few nanometres. Some RMNs are also affected by secondary processes at low temperature causing exsolution of molybdenite. However, most RMNs had crystallographic textures indicating that the RMN formed prior to their host inclusion. TKD analyses reveal most RMNs have been affected by processing in the protoplanetary disk. Despite this alteration, RMNs still preserve primary crystallographic textures and heterogeneous chemical signatures. This heterogeneity in crystallographic relationships, which mostly suggest that RMNs pre-date their host, is consistent with the idea that there is not a dominant RMN forming process. Each RMN has experienced a complex history, supporting the suggestion of Daly et al. (2017), that RMNs may preserve a diverse pre-solar chemical signature inherited from the Giant Molecular Cloud.

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.

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.

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.

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.

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.

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.

Modeling the microstructural changes during hot tandem rolling of AA5 XXX aluminum alloys: Part II. Textural evolution

NASA Astrophysics Data System (ADS)

Wells, M. A.; Samarasekera, I. V.; Brimacombe, J. K.; Hawbolt, E. B.; Lloyd, D. J.

1998-06-01

In Part II of this article, the experimental work undertaken to measure the effect of deformation parameters (temperature, strain, and strain rate) on the texture formation during hot deformation and the evolution during subsequent recrystallization is described. In addition, the isothermal kinetics of development of individual texture components were also determined. A neutron diffractometer was used to measure the texture in the as-hot-deformed aluminum samples, and the samples were then heat treated in a 400 °C salt bath for various lengths of time, with the texture being remeasured at various stages in the recrystallization process. Using data from the experimental program, the texture evolution during recrystallization was modeled by applying a modified form of the Avrami equation. Results indicated that, of the deformation parameters studied, textural development was most sensitive to the deformation temperature for both alloys. In addition, modeling results revealed that the Cu component ({112} <111>) was the first to recrystallize, typically followed by the S ({123} <634>) and Bs ({110} <112>) components. This is in agreement with earlier work which indicated that the Bs component was the hardest to recrystallize, possibly because it is able to deform on very few slip systems and, hence, the dislocation interaction may be low.

{bold {ital In situ}} measurements of texture and phase development in (Bi,Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub 10}{endash}Ag tapes

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

Thurston, T.R.; Haldar, P.; Wang, Y.L.

Hard x-rays from a synchrotron source were utilized in diffraction experiments performed at elevated temperatures (up to {approximately}870{degree}C) on (Bi,Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub 10} (Bi-2223) tapes {ital completely} encased in silver. The general behavior of the phase and texture development under typical processing conditions was determined, and the effects that several variations in processing conditions had on the phase and texture development were examined. These results and their implications for improving processing conditions are discussed. {copyright} {ital 1997 Materials Research Society.}

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

Comprehensive Deformation Analysis of a Newly Designed Ni-Free Duplex Stainless Steel with Enhanced Plasticity by Optimizing Austenite Stability

NASA Astrophysics Data System (ADS)

Moallemi, Mohammad; Zarei-Hanzaki, Abbas; Eskandari, Mostafa; Burrows, Andrew; Alimadadi, Hossein

2017-08-01

A new metastable Ni-free duplex stainless steel has been designed with superior plasticity by optimizing austenite stability using thermodynamic calculations of stacking fault energy and with reference to literature findings. Several characterization methods comprising optical microscopy, magnetic phase measurements, X-ray diffraction (XRD) and electron backscattered diffraction were employed to study the plastic deformation behavior and to identify the operating plasticity mechanisms. The results obtained show that the newly designed duplex alloy exhibits some extraordinary mechanical properties, including an ultimate tensile strength of 900 MPa and elongation to fracture of 94 pct due to the synergistic effects of transformation-induced plasticity and twinning-induced plasticity. The deformation mechanism of austenite is complex and includes deformation banding, strain-induced martensite formation, and deformation-induced twinning, while the ferrite phase mainly deforms by dislocation slip. Texture analysis indicates that the Copper and Rotated Brass textures in austenite (FCC phase) and {001}<110> texture in ferrite and martensite (BCC phases) are the main active components during tensile deformation. The predominance of these components is logically related to the strain-induced martensite and/or twin formation.

FAST TRACK COMMUNICATION: Directional annealing-induced texture in melt-spun (Sm12Co88)99Nb1 alloy

NASA Astrophysics Data System (ADS)

Jayaraman, T. V.; Rogge, P.; Shield, J. E.

2010-07-01

Developing texture in nanocrystalline permanent magnet alloys is of significant importance. Directional annealing is shown to produce texture in the permanent magnet alloy (Sm12Co88)99Nb1. Melt spinning produced isotropic grain structures of the hard magnetic metastable SmCo7 phase, with grain sizes of ~300 nm. Conventional annealing of melt-spun (Sm12Co88)99Nb1 alloy produced Sm2Co17 phase with random crystallographic orientation. Directional annealing of melt-spun (Sm12Co88)99Nb1 alloy, with appropriate combinations of annealing temperature and translational velocity, produced Sm2Co17 phase with (0 0 0 6) in-plane texture, as determined by x-ray diffraction analysis and magnetic measurements. The magnetization results show out-of-plane remanence higher than the in-plane remanence resulting in the degree of 'magnetic' texture in the order of 25-40%. Coercivity values above 2 kOe were maintained. The texture development via directional annealing while minimizing exposure to elevated temperatures provides a new route to anisotropic high-energy permanent magnets.

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

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

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.

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.

Texture Evolution During Laser Direct Metal Deposition of Ti-6Al-4V

DOE PAGES

Sridharan, Niyanth; Chaudhary, Anil; Nandwana, Peeyush; ...

2016-01-20

Titanium alloys are used in a wide variety of high performance applications and hence the processing of the titanium and the resulting microstructures after additive manufacturing has received significant attention. During additive manufacturing the processing route involves the transition from a liquid to solid state. The addition of successive layers results in a complex microstructure due to solid-state transformations. The current study focuses on understanding the phase transformations and relate it to the transformation texture in Ti-6Al-4V to identify conditions leading to a strong alpha transformation texture. The as deposited builds were characterized using optical microscopy and electron backscattered diffraction.more » The results showed columnar prior β grains with a martensitic structure after the deposition of a single layer. On subsequent depositions the martensitic microstructure decomposes to a colony and basketweave microstructure with a stronger transformation texture. The alpha texture with a colony and basketweave microstructure shows a stronger transformation texture as a result of variant selection. Thus by controlling the cooling rate of the build from the β transus it is possible to control the alpha transformation texture.« less

Texture Evolution During Laser Direct Metal Deposition of Ti-6Al-4V

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

Sridharan, Niyanth; Chaudhary, Anil; Nandwana, Peeyush

Titanium alloys are used in a wide variety of high performance applications and hence the processing of the titanium and the resulting microstructures after additive manufacturing has received significant attention. During additive manufacturing the processing route involves the transition from a liquid to solid state. The addition of successive layers results in a complex microstructure due to solid-state transformations. The current study focuses on understanding the phase transformations and relate it to the transformation texture in Ti-6Al-4V to identify conditions leading to a strong alpha transformation texture. The as deposited builds were characterized using optical microscopy and electron backscattered diffraction.more » The results showed columnar prior β grains with a martensitic structure after the deposition of a single layer. On subsequent depositions the martensitic microstructure decomposes to a colony and basketweave microstructure with a stronger transformation texture. The alpha texture with a colony and basketweave microstructure shows a stronger transformation texture as a result of variant selection. Thus by controlling the cooling rate of the build from the β transus it is possible to control the alpha transformation texture.« less

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

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.

Texture and microstructure evolution in single-phase Ti{sub x}Ta{sub 1-x}N alloys of rocksalt structure

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

Koutsokeras, L. E.; Department of Materials Science and Engineering, University of Ioannina, GR-45100 Ioannina; Abadias, G.

2011-08-15

The mechanisms controlling the structural and morphological features (texture and microstructure) of ternary transition metal nitride thin films of the Ti{sub x}Ta{sub 1-x}N system, grown by various physical vapor deposition techniques, are reported. Films deposited by pulsed laser deposition, dual cathode magnetron sputtering, and dual ion beam sputtering have been investigated by means of x-ray diffraction in various geometries and scanning electron microscopy. We studied the effects of composition, energetic, and kinetics in the evolution of the microstructure and texture of the films. We obtain films with single and mixed texture as well as films with columnar ''zone-T'' and globularmore » type morphology. The results have shown that the texture evolution of ternary transition metal nitrides as well as the microstructural features of such films can be well understood in the framework of the kinetic mechanisms proposed for their binary counterparts, thus giving these mechanisms a global application.« 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

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.

Rotatable multifunctional load frames for neutron diffractometers at FRM II—design, specifications and applications

NASA Astrophysics Data System (ADS)

Hoelzel, M.; Gan, W. M.; Hofmann, M.; Randau, C.; Seidl, G.; Jüttner, Ph.; Schmahl, W. W.

2013-05-01

Novel tensile rigs have been designed and manufactured at the research reactor Heinz Maier-Leibnitz (FRM II, Garching near Munich). Besides tensile and compressive stress, also torsion can be applied. The unique Eulerian cradle type design (ω, χ, and φ axis) allows orienting the stress axis with respect to the scattering vector. Applications of these tensile rigs at our neutron diffractometers enable various investigations of structural changes under mechanical load, e.g. crystallographic texture evolution, stress-induced phase transformations or lattice expansion, and the anisotropy of mechanical response.

The bowing potential of granitic rocks: rock fabrics, thermal properties and residual strain

NASA Astrophysics Data System (ADS)

Siegesmund, S.; Mosch, S.; Scheffzük, Ch.; Nikolayev, D. I.

2008-10-01

The bowing of natural stone panels is especially known for marble slabs. The bowing of granite is mainly known from tombstones in subtropical humid climate. Field inspections in combination with laboratory investigations with respect to the thermal expansion and the bowing potential was performed on two different granitoids (Cezlak granodiorite and Flossenbürg granite) which differ in the composition and rock fabrics. In addition, to describe and explain the effect of bowing of granitoid facade panels, neutron time-of-flight diffraction was applied to determine residual macro- and microstrain. The measurements were combined with investigations of the crystallographic preferred orientation of quartz and biotite. Both samples show a significant bowing as a function of panel thickness and destination temperature. In comparison to marbles the effect of bowing is more pronounced in granitoids at temperatures of 120°C. The bowing as well as the thermal expansion of the Cezlak sample is also anisotropic with respect to the rock fabrics. A quantitative estimate was performed based on the observed textures. The effect of the locked-in stresses may also have a control on the bowing together with the thermal stresses related to the different volume expansion of the rock-forming minerals.

On a Fast and Accurate In Situ Measuring Strategy for Recrystallization Kinetics and Its Application to an Al-Fe-Si Alloy

NASA Astrophysics Data System (ADS)

Kühbach, Markus; Brüggemann, Thiemo; Molodov, Konstantin D.; Gottstein, Günter

2015-03-01

In the current study, we detail a novel in situ X-ray diffraction-based bulk measurement technique, which allows for the continuous tracking of primary recrystallization kinetics. The approach is based on measuring the diffracted intensity that is correlated with the evolution of the volume fraction of particular texture components during annealing of a sample within a texture goniometer. The method is applied in an experimental study on a cold-rolled industrial Al-Fe-Si alloy. For comparison purposes, the macrotexture and the hardness evolution were monitored ex situ along isothermal and nonisothermal annealing. These measurements were then contrasted to the in situ obtained growth kinetics of recrystallizing grains in beta-fiber deformation and cube orientation. The results showed clearly that this method can be reliably utilized for the characterization of recrystallization kinetics in an industrial context.

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.

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

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.

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.

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.

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.

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.

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.

High Strength and Ductility of Additively Manufactured 316L Stainless Steel Explained

NASA Astrophysics Data System (ADS)

Shamsujjoha, Md.; Agnew, Sean R.; Fitz-Gerald, James M.; Moore, William R.; Newman, Tabitha A.

2018-04-01

Structure-property relationships of an additively manufactured 316L stainless steel were explored. A scanning electron microscope and electron backscattered diffraction (EBSD) analysis revealed a fine cellular-dendritic (0.5 to 2 μm) substructure inside large irregularly shaped grains ( 100 μm). The cellular structure grows along the <100> crystallographic directions. However, texture analysis revealed that the main <100> texture component is inclined by 15 deg from the building direction. X-ray diffraction line profile analysis indicated a high dislocation density of 1 × 1015 m-2 in the as-built material, which correlates well with the observed EBSD microstructure and high-yield strength, via the traditional Taylor hardening equation. Significant variations in strain hardening behavior and ductility were observed for the horizontal (HB) and vertical (VB) built samples. Ductility of HB and VB samples measured 49 and 77 pct, respectively. The initial growth texture and subsequent texture evolution during tensile deformation are held responsible for the observed anisotropy. Notably, EBSD analysis of deformed samples showed deformation twins, which predominately form in the grains with <111> aligned parallel to the loading direction. The VB samples showed higher twinning activity, higher strain hardening rates at high strain, and therefore, higher ductility. Analysis of annealed samples revealed that the observed microstructures and properties are thermally stable, with only a moderate decrease in strength and very similar levels of ductility and anisotropy, compared with the as-built condition.

High Strength and Ductility of Additively Manufactured 316L Stainless Steel Explained

NASA Astrophysics Data System (ADS)

Shamsujjoha, Md.; Agnew, Sean R.; Fitz-Gerald, James M.; Moore, William R.; Newman, Tabitha A.

2018-07-01

Structure-property relationships of an additively manufactured 316L stainless steel were explored. A scanning electron microscope and electron backscattered diffraction (EBSD) analysis revealed a fine cellular-dendritic (0.5 to 2 μm) substructure inside large irregularly shaped grains ( 100 μm). The cellular structure grows along the <100> crystallographic directions. However, texture analysis revealed that the main <100> texture component is inclined by 15 deg from the building direction. X-ray diffraction line profile analysis indicated a high dislocation density of 1 × 1015 m-2 in the as-built material, which correlates well with the observed EBSD microstructure and high-yield strength, via the traditional Taylor hardening equation. Significant variations in strain hardening behavior and ductility were observed for the horizontal (HB) and vertical (VB) built samples. Ductility of HB and VB samples measured 49 and 77 pct, respectively. The initial growth texture and subsequent texture evolution during tensile deformation are held responsible for the observed anisotropy. Notably, EBSD analysis of deformed samples showed deformation twins, which predominately form in the grains with <111> aligned parallel to the loading direction. The VB samples showed higher twinning activity, higher strain hardening rates at high strain, and therefore, higher ductility. Analysis of annealed samples revealed that the observed microstructures and properties are thermally stable, with only a moderate decrease in strength and very similar levels of ductility and anisotropy, compared with the as-built condition.

The 2003 phreatomagmatic eruptions of Anatahan volcano - Textural and petrologic features of deposits at an emergent island volcano

USGS Publications Warehouse

Pallister, J.S.; Trusdell, F.A.; Brownfield, I.K.; Siems, D.F.; Budahn, J.R.; Sutley, S.F.

2005-01-01

Stratigraphic and field data are used in conjunction with textural and chemical evidence (including data from scanning electron microscope, electron microprobe, X-ray fluorescence, X-ray diffraction, and instrumental neutron activation analysis) to establish that the 2003 eruption of Anatahan volcano was mainly phreatomagmatic, dominated by explosive interaction of homogeneous composition low-viscosity crystal-poor andesite magma with water. The hydromagmatic mode of eruption contributed to the significant height of initial eruptive columns and to the excavation and eruption of altered rock debris from the sub-volcanic hydrothermal system. Volatile contents of glass inclusions in equilibrium phenocrysts less abundances of these constituents in matrix glass times the estimated mass of juvenile magma indicate minimum emissions of 19 kt SO2 and 13 kt Cl. This petrologic estimate of SO2 emission is an order-of-magnitude less than an estimate from TOMS. Similarly, inferred magma volumes from the petrologic data are an order of magnitude greater than those modeled from deformation data. Both discrepancies indicate additional sources of volatiles, likely derived from a separate fluid phase in the magma. The paucity of near-source volcanic-tectonic earthquakes preceding the eruption, and the dominance of sustained long-period tremor are attributed to the ease of ascent of the hot low-viscosity andesite, followed by a shallow phreatomagmatic mode of eruption. Phreatomagmatic eruptions are probably more common at emergent tropical island volcanoes, where shallow fresh-water lenses occur at near-sea-level vents. These relations suggest that phreatomagmatic explosions contributed to the formation of many of the near-sea-level craters and possibly even to the small calderas at the other Mariana islands.

Microstructure, crystallographic texture and mechanical properties of friction stir welded AA2017A

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

Ahmed, M.M.Z., E-mail: mohamed_ahmed4@s-petrol.suez.edu.eg; Department of Metallurgical and Materials Engineering, Suez Canal University, Suez 43721; Wynne, B.P.

2012-02-15

In this study a thick section (20 mm) friction stir welded AA2017A-T451 has been characterized in terms of microstructure, crystallographic texture and mechanical properties. For microstructural analysis both optical and scanning electron microscopes have been used. A detailed crystallographic texture analysis has been carried out using the electron back scattering diffraction technique. Crystallographic texture has been examined in both shoulder and probe affected regions of the weld NG. An entirely weak texture is observed at the shoulder affected region which is mainly explained by the effect of the sequential multi pass deformation experienced by both tool probe and tool shoulder.more » The texture in the probe dominated region at the AS side of the weld is relatively weak but still assembles the simple shear texture of FCC metals with B/B{sup Macron} and C components existing across the whole map. However, the texture is stronger at the RS than at the AS of the weld, mainly dominated byB/B{sup Macron} components and with C component almost absent across the map. An alternating bands between (B) components and (B{sup Macron }) component are observed only at the AS side of the weld. - Highlights: Black-Right-Pointing-Pointer Detailed investigation of microstructure and crystallographic texture. Black-Right-Pointing-Pointer The grain size is varied from the top to the bottom of the NG. Black-Right-Pointing-Pointer An entirely weak texture is observed at the shoulder affected region. Black-Right-Pointing-Pointer The texture in the probe affected region is dominated by simple shear texture.« less

Sputtered Modified Barium Titanate for Thin-Film Capacitor Applications.

PubMed

Reynolds, Glyn J; Kratzer, Martin; Dubs, Martin; Felzer, Heinz; Mamazza, Robert

2012-04-10

New apparatus and a new process for the sputter deposition of modified barium titanate thin-films were developed. Films were deposited at temperatures up to 900 °C from a Ba₀ .96 Ca 0. 04 Ti 0. 82 Zr 0. 18 O₃ (BCZTO) target directly onto Si, Ni and Pt surfaces and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Film texture and crystallinity were found to depend on both deposition temperature and substrate: above 600 °C, the as-deposited films consisted of well-facetted crystallites with the cubic perovskite structure. A strongly textured Pt (111) underlayer enhanced the (001) orientation of BCZTO films deposited at 900 °C, 10 mtorr pressure and 10% oxygen in argon. Similar films deposited onto a Pt (111) textured film at 700 °C and directly onto (100) Si wafers showed relatively larger (011) and diminished intensity (00ℓ) diffraction peaks. Sputter ambients containing oxygen caused the Ni underlayers to oxidize even at 700 °C: Raising the process temperature produced more diffraction peaks of NiO with increased intensities. Thin-film capacitors were fabricated using ~500 nm thick BCZTO dielectrics and both Pt and Ni top and bottom electrodes. Small signal capacitance measurements were carried out to determine capacitance and parallel resistance at low frequencies and from these data, the relative permittivity (e r ) and resistivity (r) of the dielectric films were calculated; values ranged from ~50 to >2,000, and from ~10⁴ to ~10 10 Ω∙cm, respectively.

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

Channeling effect in polycrystalline deuterium-saturated CVD diamond target bombarded by deuterium ion beam

NASA Astrophysics Data System (ADS)

Bagulya, A. V.; Dalkarov, O. D.; Negodaev, M. A.; Rusetskii, A. S.; Chubenko, A. P.; Ralchenko, V. G.; Bolshakov, A. P.

2015-07-01

At the ion accelerator HELIS at LPI, the neutron yield is investigated in DD reactions within a strongly textured polycrystalline deuterium-saturated CVD diamond under irradiation by a deuterium ion beam with the energy of less than 30 keV. The measurements of the neutron flux in the beam direction are performed using a multichannel detector based on 3He counters, in dependence on the target angle, β, with respect to the beam axis. A significant anisotropy in the neutron yield is observed. At β = 0° the yield is higher by a factor of 3 as compared to that at β = ±45°. The possible reasons for the anisotropy, including ion channeling, are discussed.

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.

Electron backscatter and X-ray diffraction studies on the deformation and annealing textures of austenitic stainless steel 310S

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

Nezakat, Majid, E-mail: majid.nezakat@usask.ca

We studied the texture evolution of thermo-mechanically processed austenitic stainless steel 310S. This alloy was cold rolled up to 90% reduction in thickness and subsequently annealed at 1050 °C. At the early stages of deformation, strain-induced martensite was formed from deformed austenite. By increasing the deformation level, slip mechanism was found to be insufficient to accommodate higher deformation strains. Our results demonstrated that twinning is the dominant deformation mechanism at higher deformation levels. Results also showed that cold rolling in unidirectional and cross rolling modes results in Goss/Brass and Brass dominant textures in deformed samples, respectively. Similar texture components aremore » observed after annealing. Thus, the annealing texture was greatly affected by texture of the deformed parent phase and martensite did not contribute as it showed an athermal reversion during annealing. Results also showed that when the fraction of martensite exceeds a critical point, its grain boundaries impeded the movement of austenite grain boundaries during annealing. As a result, recrystallization incubation time would increase. This caused an incomplete recrystallization of highly deformed samples, which led to a rational drop in the intensity of the texture components. - Highlights: •Thermo-mechanical processing through different cold rolling modes can induce different textures. •Martensite reversion is athermal during annealing. •Higher fraction of deformation-induced martensite can increase the annealing time required for complete recrystallization. •Annealing texture is mainly influenced by the deformation texture of austenite.« less

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

Annealing texture of nanostructured IF steel

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

Jamaati, Roohollah, E-mail: jamaati@nit.ac.ir

In the present work, the evolution of annealing texture in nanostructured interstitial free steel fabricated via accumulative roll bonding (ARB) process was investigated. Textural evolution after post-annealing of ARB-processed samples was evaluated using X-ray diffraction. There were several texture transitions in the γ-fiber and ζ-fiber during ARB and post-annealing treatment. It was found that with increasing the number of ARB cycles, the volume fraction of the low angle grain boundary decreased and the high angle grain boundary fraction increased. Also, the shear texture was dominant after the first cycle, while for other samples, the rolling texture was dominant. The one-cyclemore » sample clearly indicated a weak α-fiber and γ-fiber and a relatively strong ζ-fiber. In addition, during the recrystallization and before the grain growth, the intensity of α-fiber and γ-fiber decreased, the intensity of ζ-fiber increased, and the intensity of (011)〈100〉 orientation in the ε-fiber and η-fiber increased. Moreover, it was concluded that the transition from the rolling texture to the shear one was a sign of occurrence of the recrystallization (before the grain growth). Finally, with increasing the number of ARB cycles, the intensity of rolling and shear textures saturated and a stable texture formed. - Highlights: • There were texture transitions in the γ-fiber and ζ-fiber. • When the number of cycles increased, the low angle grain boundaries decreased. • The shear texture was dominant after the first cycle. • Transition from rolling texture to shear one was a sign of recrystallization. • With increasing the number of ARB cycles, a stable texture formed.« less

Scatterometry—fast and robust measurements of nano-textured surfaces

NASA Astrophysics Data System (ADS)

Hannibal Madsen, Morten; Hansen, Poul-Erik

2016-06-01

Scatterometry is a fast, precise and low cost way to determine the mean pitch and dimensional parameters of periodic structures with lateral resolution of a few nanometer. It is robust enough for in-line process control and precise and accurate enough for metrology measurements. Furthermore, scatterometry is a non-destructive technique capable of measuring buried structures, for example a grating covered by a thick oxide layer. As scatterometry is a non-imaging technique, mathematical modeling is needed to retrieve structural parameters that describe a surface. In this review, the three main steps of scatterometry are discussed: the data acquisition, the simulation of diffraction efficiencies and the comparison of data and simulations. First, the intensity of the diffracted light is measured with a scatterometer as a function of incoming angle, diffraction angle and/or wavelength. We discuss the evolution of the scatterometers from the earliest angular scatterometers to the new imaging scatterometers. The basic principle of measuring diffraction efficiencies in scatterometry has remained the same since the beginning, but the instrumental improvements have made scatterometry a state-of-the-art solution for fast and accurate measurements of nano-textured surfaces. The improvements include extending the wavelength range from the visible to the extreme ultra-violet range, development of Fourier optics to measure all diffraction orders simultaneously, and an imaging scatterometer to measure area of interests smaller than the spot size. Secondly, computer simulations of the diffraction efficiencies are discussed with emphasis on the rigorous coupled-wave analysis (RCWA) method. RCWA has, since the mid-1990s, been the preferred method for grating simulations due to the speed of the algorithms. In the beginning the RCWA method suffered from a very slow convergence rate, and we discuss the historical improvements to overcome this challenge, e.g. by the introduction of Li’s factorization rules and the introduction of the normal vector method. The third step is the comparison, where the simulated diffraction efficiencies are compared to the experimental data using an inverse modeling approach. We discuss both a direct optimization scheme using a differential evolution algorithm and a library search strategy where diffraction efficiences of expected structures are collected in a database. For metrology measurements two methods are described for estimating the uncertainty of the fitting parameters. The first method is based on estimating the confidence limits using constant chi square boundaries, which can easily be computed when using the library search strategy. The other method is based on calculating the covariances of all the free parameters using a least square optimization. Scatterometry is already utilized in the semiconductor industry for in-line characterization. However, it also has a large potential for other industrial sectors, including sectors making use of injection molding or roll-2-roll fabrication. Using the library search strategy, the comparison can be performed in ms, making in-line characterization possible and we demonstrate that scatterometry can be used for quality control of injection molded nano-textured plastic samples. With the emerging methods of highly parallel manufacturing of nano-textured devices, scatterometry has great potential to deliver a characterization method for in-line quality control and metrology measurements, which is not possible with conventional characterization techniques. However, there are some open challenges for the scatterometry techniques. These include corrections for measuring on non-ideal samples with a large surface roughness or line-edge roughness and the path towards performing traceable scatterometry measurements.

Unraveling Recrystallization Mechanisms Governing Texture Development from Rare Earth Element Additions to Magnesium

NASA Astrophysics Data System (ADS)

Imandoust, Aidin

The origin of texture components associated with rare-earth (RE) element additions in wrought magnesium (Mg) alloys is a long-standing problem in magnesium technology. The objective of this research is to identify the mechanisms accountable for rare-earth texture during dynamic recrystallization (DRX). Towards this end, we designed binary Mg-Cerium and Mg-Gadolinium alloys along with complex alloy compositions containing zinc, yttrium and Mischmetal. Binary alloys along with pure Mg were designed to individually investigate their effects on texture evolutions, while complex compositions are designed to develop randomized texture, and be used in automotive and aerospace applications. We selected indirect extrusion to thermo-mechanically process our materials. Different extrusion ratios and speeds were designed to produce partially and fully recrystallized microstructures, allowing us to analyze DRX from its early stages to completion. X-ray diffraction, electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) were used to conduct microstructure and texture analyses. Our analyses revealed that rare-earth elements in zinc-containing magnesium alloys promote discontinuous dynamic recrystallization at the grain boundaries. During nucleation, the effect of rare earth elements on orientation selection was explained by the concomitant actions of multiple Taylor axes in the same grain. Isotropic grain growth was observed due to rare earth elements segregating to grain boundaries, which lead to texture randomization. The nucleation in binary Mg-RE alloys took place by continuous formation of necklace structures. Stochastic relaxation of basal and non-basal dislocations into low-angle grain boundaries produced chains of embryos with nearly random orientations. Schmid factor analysis showed a lower net activation of dislocations in RE textured grains compared to ones on the other side of the stereographic triangle. Lower dislocation densities within RE grains favored their growth by setting the boundary migration direction toward grains with higher dislocation density, thereby decreasing the system energy. We investigated the influence of RE elements on extension twinning induced hardening. RE addition enhanced tensile twinning induced hardening significantly. EBSD analysis illustrated that tensile twins cross low angle grain boundaries in Mg-RE alloys, which produced large twins and facilitated transmutation of basal to prismatic dislocations. Higher activity of pyramidal II dislocations in Mg-RE alloys resulted in higher twinning induced hardening.

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.

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

NASA Astrophysics Data System (ADS)

Krishnan, Vinu B.

Shape memory alloys are incorporated as actuator elements due to their inherent ability to sense a change in temperature and actuate against external loads by undergoing a shape change as a result of a temperature-induced phase transformation. The cubic so-called austenite to the trigonal so-called R-phase transformation in NiTiFe shape memory alloys offers a practical temperature range for actuator operation at low temperatures, as it exhibits a narrow temperature-hysteresis with a desirable fatigue response. Overall, this work is an investigation of selected science and engineering aspects of low temperature NiTiFe shape memory alloys. The scientific study was performed using in situ neutron diffraction measurements at the newly developed low temperature loading capability on the Spectrometer for Materials Research at Temperature and Stress (SMARTS) at Los Alamos National Laboratory and encompasses three aspects of the behavior of Ni46.8Ti50Fe3.2 at 92 K (the lowest steady state temperature attainable with the capability). First, in order to study deformation mechanisms in the R-phase in NiTiFe, measurements were performed at a constant temperature of 92 K under external loading. Second, with the objective of examining NiTiFe in one-time, high-stroke, actuator applications (such as in safety valves), a NiTiFe sample was strained to approximately 5% (the R-phase was transformed to B19' phase in the process) at 92 K and subsequently heated to full strain recovery under a load. Third, with the objective of examining NiTiFe in cyclic, low-stroke, actuator applications (such as in cryogenic thermal switches), a NiTiFe sample was strained to 1% at 92 K and subsequently heated to full strain recovery under load. Neutron diffraction spectra were recorded at selected time and stress intervals during these experiments. The spectra were subsequently used to obtain quantitative information related to the phase-specific strain, texture and phase fraction evolution using the Rietveld technique. The mechanical characterization of NiTiFe alloys using the cryogenic capability at SMARTS provided considerable insight into the mechanisms of phase transformation and twinning at cryogenic temperatures. Both mechanisms contribute to shape memory and pseudoelasticity phenomena. Three phases (R, B19' and B33 phases) were found to coexist at 92 K in the unloaded condition (nominal holding stress of 8 MPa). For the first time the elastic modulus of R-phase was reported from neutron diffraction experiments. Furthermore, for the first time a base-centered orthorhombic (B33) martensitic phase was identified experimentally in a NiTi-based shape memory alloy. The orthorhombic B33 phase has been theoretically predicted in NiTi from density function theory (DFT) calculations but hitherto has never been observed experimentally. The orthorhombic B33 phase was observed while observing shifting of a peak (identified to be {021}B33) between the {111}R and {100}B19' peaks in the diffraction spectra collected during loading. Given the existing ambiguity in the published literature as to whether the trigonal R-phase belongs to the P3 or P3¯ space groups, Rietveld analyses were separately carried out incorporating the symmetries associated with both space groups and the impact of this choice evaluated. The constrained recovery of the B19' phase to the R-phase recorded approximately 4% strain recovery between 150 K and 170 K, with half of that recovery occurring between 160 K and 162 K. Additionally, the aforementioned research methodology developed for Ni46.8Ti50Fe3.2 shape memory alloys was applied to experiments performed on a new high temperature Ni 29.5Ti50.5Pd20 shape memory alloys. The engineering aspect focused on the development of (i) a NiTiFe based thermal conduction switch that minimized the heat gradient across the shape memory actuator element, (ii) a NiTiFe based thermal conduction switch that incorporated the actuator element in the form of helical springs, and (iii) a NiTi based release mechanism. Patents are being filed for all the three shape memory actuators developed as a part of this work. This work was supported by grants from SRI, NASA (NAG3-2751) and NSF (CAREER DMR-0239512) to UCF. Additionally, this work benefited from the use of the Lujan Center at the Los Alamos Neutron Science Center, funded by the United States Department of Energy, Office of Basic Energy Sciences, under Contract No. W-7405-ENG-36.

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.

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

Effect of Ar9+ irradiation on Zr-1Nb-1Sn-0.1Fe alloy characterized by Grazing Incidence X-ray diffraction technique

NASA Astrophysics Data System (ADS)

Dutta, Argha; Das, Kalipada; Gayathri, N.; Menon, Ranjini; Nabhiraj, P. Y.; Mukherjee, Paramita

2018-03-01

The microstructural parameters such as domain size and microstrain have been estimated from Grazing Incidence X-ray Diffraction (GIXRD) data for Ar9+ irradiated Zr-1Nb-1Sn-0.1Fe sample as a function of dpa (dose). Detail studies using X-ray Diffraction Line Profile Analysis (XRDLPA) from GIXRD data has been carried out to characterize the microstructural parameters like domain size and microstrain. The reorientation of the grains due to effect of irradiation at high dpa (dose) has been qualitatively assessed by the texture parameter P(hkl).

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

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

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.

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.

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

In-situ laser ultrasonic measurement of the hcp to bcc transformation in commercially pure titanium

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

Shinbine, A., E-mail: alyssa.shinbine@gmail.com; Garcin, T.; Sinclair, C.

2016-07-15

Using a novel in-situ laser ultrasonic technique, the evolution of longitudinal velocity was used to measure the α − β transformation during cyclic heating and cooling in commercially pure titanium. In order to quantify the transformation kinetics, it is shown that changes in texture can not be ignored. This is particularly important in the case of titanium where significant grain growth occurs in the β-phase leading to the ultrasonic wave sampling a decreasing number of grains on each thermal treatment cycle. Electron backscatter diffraction measurements made postmortem in the region where the ultrasonic pulse traveled were used to obtain anmore » estimate of such local texture and grain size changes. An analysis technique for including the anisotropy of wave velocity depending on local texture is presented and shown to give self consistent results for the transformation kinetics. - Highlights: • Laser ultrasound and EBSD interpret the hcp/bcc phase transformation in cp-Ti. • Grain growth and texture produced variation in velocity during similar treatments. • Texture was deconvoluted from phase addition to obtain transformation kinetics.« less

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.

The new materials science diffractometer STRESS-SPEC at FRM-II

NASA Astrophysics Data System (ADS)

Hofmann, M.; Schneider, R.; Seidl, G. A.; Rebelo-Kornmeier, J.; Wimpory, R. C.; Garbe, U.; Brokmeier, H.-G.

2006-11-01

In response to the development of new materials and the application of materials and components in new technologies the direct measurement, calculation and evaluation of textures and residual stresses has gained worldwide significance in recent years. In order to cater for the development of these analytical techniques the Materials Science Diffractometer STRESS-SPEC at FRM-II is designed to be equally applied to texture or residual stress analysis by virtue of its flexible configuration and the high neutron flux at the sample position. The instrument is now available for routine operation and here we present details of first experiments and instrument performance.

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).

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.

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