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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 397 records · Page 22
All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

Advanced Sample Environments for in situ Neutron Diffraction Studies of Nuclear Materials

Summaries of this presentation are: (1) the author successfully developed and commissioned three sample environments and applied them to study scientific problems of nuclear materials; (2) sample changer - reliable, unattended operation, Reiche and Vogel, 2010; (3) creep furnace - 1000 C, 2.7 kN, texture, Reiche et al., 2012; (4) Zr-2.5Nb pressure tubes - deconvolute the contributions of heating, phase transformation, deformation at temperature in the {beta}-field, and phase transformation during cooling; (5) our data informs currently developed mechanical models predicting texture evolution during phase transformation and high temperature deformation (MST-8, LANL); (6) high-temperature furnace - >2200 C, texture, paper in progress; (7) UC - Bowman's NaCl-type structure correct for cubic UC{sub 2}, recent reactor safetly calculations by Chevalier and Fischer (2001) and independent work by Freyss (2010) incorrect, as fluorite structure is assumed; and (8) UC - order-disorder transition starting at 1800 C discovered which will improve current models, as these do not predict this transition (e.g. Basak, 2007), or confirm the prediction (Wen et al., 2012, T-1, LANL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

High pressure neutron diffraction on WAND 2 with a Paris-Edinburgh press

The Paris-Edinburgh press is a widely available, highly adaptable pressure cell commonly used while collecting neutron scattering data. Here, we detail the use of the VX3 and VX5 Paris-Edinburgh presses on the Wide-Angle Neutron Diffractometer (WAND 2 ) at the High Flux Isotope Reactor at Oak Ridge National Laboratory. We first give a detailed overview of the instrument setup and alignment capabilities used at WAND 2 . We then demonstrate the high pressure capabilities through three examples. In this work, the first example focuses on diffraction data obtained from a lithium-diamond mixture to 10 GPa with the use of single toroidal cubic boron nitride anvils. Other examples include the room temperature compressions of germanium (up to 16 GPa) and the mineral malachite with double toroidal sintered diamond anvils. This work thereby represents the first studies above 10 GPa at the High Flux Isotope Reactor and opens the door for future user experiments at these elevated pressures.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Determination of hydrogen site and occupancy in hydrous Mg 2 SiO 4 spinel by single-crystal neutron diffraction

Ringwoodite [(Mg,Fe 2+ ) 2 SiO 4 spinel] has been considered as one of the most important host minerals of water in the Earth's deep mantle. Its extensive hydration was observed in high-pressure synthesis experiments and also by its natural occurrence. Water can dissolve into ringwoodite as structurally bound hydrogen cations by substituting other cations, although the hydrogen site and its occupancy remain unclear. In this study, neutron time-of-flight single-crystal Laue diffraction analysis was carried out for synthetic hydrous ringwoodite. Hydrogen cations were found only in the sites in MgO 6 octahedra in the ringwoodite structure, which compensated the reduced occupancies of both magnesium and silicon cations. The refined cation occupancies suggest that the most plausible hydration mechanism is that three hydrogen cations simultaneously occupy an MgO 6 octahedron, whereas four such hydrogenated octahedra surround a vacant SiO 4 tetrahedron.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Time-of-Flight Neutron Diffraction (TOF-ND) Analyses of the Composition and Minting of Ancient Judaean “Biblical” Coins

TOF-ND elastic scattering of thermal neutrons offers some important advantages over X-ray diffraction (XRD), X-ray fluorescence (XRF), and metallography for the study of archaeological and numismatic problems. Traditional analytical methods are usually destructive and often probe only the surface. Neutrons deeply penetrate samples, simultaneously giving nondestructive bulk information about the crystal structure, composition, and texture (alignment of crystallites) from which thermomechanical manufacturing processes (e.g., cast, struck, or rolled) may be inferred. An analysis of the metal composition and minting processes used for making ancient Judaean bronze and leaded bronze coins from first century BCE and CE is used as a case study. One of the first ND analyses of the temperature used for striking bronze coins is also presented.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Rafting and elastoplastic deformation of superalloys studied by neutron diffraction

The rafting of monocrystalline Ni- and Co-based superalloys has been studied by neutron diffractometry. Lattice parameter misfit values and the difference in phase stiffnesses at room temperature, 650 °C, and 900 °C are presented. These microstructural parameters should assist in refining computer models that aim to predict precipitate evolution in superalloys and aid future alloy design. The nature of rafting is shown experimentally to be dependent upon the lattice parameter misfit. The 900 °C yield strength of the γ-phase of the Co-based superalloy with a rafted microstructure occurs at ~100 MPa, when loaded at a low strain rate.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Quantitative analysis of hydrogen sites and occupancy in deep mantle hydrous wadsleyite using single crystal neutron diffraction

Evidence from seismological and mineralogical studies increasingly indicates that water from the oceans has been transported to the deep earth to form water-bearing dense mantle minerals. Wadsleyite [(Mg, Fe2+)2SiO4] has been identified as one of the most important host minerals incorporating this type of water, which is capable of storing the entire mass of the oceans as a hidden reservoir. To understand the effects of such water on the physical properties and chemical evolution of Earth’s interior, it is essential to determine where in the crystal structure the hydration occurs and which chemical bonds are altered and weakened after hydration. Here, we conduct a neutron time-of-flight single-crystal Laue diffraction study on hydrous wadsleyite. Single crystals were grown under pressure to a size suitable for the experiment and with physical qualities representative of wet, deep mantle conditions. The results of this neutron single crystal diffraction study unambiguously demonstrate the method of hydrogen incorporation into the wadsleyite, which is qualitatively different from that of its denser polymorph, ringwoodite, in the wet mantle. The difference is a vital clue towards understanding why these dense mantle minerals show distinctly different softening behaviours after hydration.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2014

Neutron diffraction studies for realtime leaching of catalytic Ni

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

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Low temperature magnetic structure of CeRhIn 5 by neutron diffraction on absorption-optimized samples

Here, two aspects of the ambient pressure magnetic structure of heavy fermion material CeRhIn 5 have remained under some debate since its discovery: whether the structure is indeed an incommensurate helix or a spin density wave, and what is the precise magnitude of the ordered magnetic moment. By using a single crystal sample optimized for hot neutrons to minimize neutron absorption by Rh and In, here we report an ordered moment of $m=0.54(2)\,{{\mu}_{\text{B}}}$. In addition, by using spherical neutron polarimetry measurements on a similar single crystal sample, we have confirmed the helical nature of the magnetic structure, and identified a single chiral domain.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Atomic structure and grain shape evolution of nanodiamond during annealing in oxidizing atmosphere from neutron diffraction and MD simulations

In this work, real space pair-distribution function (PDF) analysis in conjunction with molecular dynamics (MD) simulations was applied to characterize crystal structure, shape and surface structure of diamond nanoparticles annealed in air up to 880 °C. MD simulated models of individual nanodiamond particles of various shapes and sizes were used to calculate theoretical radial distribution functions G(r) for powders with different grain size distributions. The calculated curves, showing distinct differences for the explored parameter space, were compared to the experimental G(r) functions obtained from neutron scattering for annealed detonated nanodiamond samples in a search for a model best describing the actual powders. It was found that as-synthesized nanodiamond grains are terminated by equally abundant (100), (110) and (111) crystallographic faces and their structure does not change upon annealing in air up to 280 °C. The shape and size of grains annealed above 480 °C changes due to surface etching. The etching rate differs between crystals faces and depends on temperature, resulting in the observed differences in grain shape. Below 680 °C the share of the (110) facets gradually increases and at 680 °C the grains become rhombic dodecahedra terminated solely by (110) surfaces. Further increase of the annealing temperature promotes formation of (111) surfaces and at 880 °C the preferred grain shape becomes an octahedron terminated by a variant of (111) surfaces possessing three dangling sp3 bonds per atom. At lower temperatures all grains become smaller and the size distribution moves towards the lower values. Furthermore, as the annealing temperature increases, the smallest grains disappear entirely and the average grain size grows back.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Direct observation of symmetrization of hydrogen bond in δ-AlOOH under mantle conditions using neutron diffraction

At ambient pressure, the hydrogen bond in materials such as ice, hydrates, and hydrous minerals that compose the Earth and icy planets generally takes an asymmetric O-H···O confguration. Pressure signifcantly afects this confguration, and it is predicted to become symmetric, such that the hydrogen is centered between the two oxygen atoms at high pressure. Changes of physical properties of minerals relevant to this symmetrization have been found; however, the atomic confguration around this symmetrization has remained elusive so far. Here we observed the pressure response of the hydrogen bonds in the aluminous hydrous minerals δ-AlOOH and δ-AlOOD by means of a neutron difraction experiment. We fnd that the transition from P21nm to Pnnm at 9.0GPa, accompanied by a change in the axial ratios of δ-AlOOH, corresponds to the disorder of hydrogen bond between two equivalent sites across the center of the O···O line. Symmetrization of the hydrogen bond is observed at 18.1GPa, which is considerably higher than the disorder pressure. Moreover, there is a signifcant isotope efect on hydrogen bond geometry and transition pressure. This study indicates that disorder of the hydrogen bond as a precursor of symmetrization may also play an important role in determining the physical properties of minerals such as bulk modulus and seismic wave velocities in the Earth’s mantle.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

Neutron diffraction reveals protonation states in pyridoxal‐5′‐phosphate‐free and glycine external aldimine‐bound serine hydroxymethyltransferase

Serine hydroxymethyltransferase (SHMT) is a critical enzyme in the one-carbon (1C) metabolism pathway catalyzing the reversible conversion of L-Ser into Gly and concurrent transfer of 1C unit to tetrahydrofolate (THF) to give 5,10-methylene-THF (5,10-MTHF), which is used in the downstream syntheses of biomolecules critical for cell proliferation. The cellular 1C metabolism is hijacked by many cancer types to support cancer cell proliferation, making SHMT a promising target for the design and development of novel small-molecule antimetabolite chemotherapies. To advance structure-assisted drug design, knowledge of SHMT catalysis is crucial, but can only be fully realized when the atomic details of each reaction step governed by the acid–base catalysis are elucidated by visualizing active site hydrogen atoms. Here, we used room-temperature neutron crystallography to directly determine protonation states in Thermus thermophilus SHMT (TthSHMT), capturing protomer A in the apo form lacking the coenzyme pyridoxal 5′-phosphate (PLP), and protomer B as a ternary complex with PLP–Gly-external aldimine and (6S)-5-methyltetrahydrofolate (5MTHF). We observed protonation of the Schiff base nitrogen in PLP–Gly and neutrality of the catalytic Lys226 side chain in the ternary complex, whereas Lys226 is protonated and positively charged in the apo-active site. Furthermore, we obtained an X-ray structure of TthSHMT in complex with the substrate THF, which binds identically as 5MTHF at the peripheral binding site. In conclusion, the unique structural and functional information provided by neutron crystallography, in combination with X-ray structures, can be employed in the rational design of SHMT inhibitors.

X-ray crystallography↗