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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 559 records · Page 31
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

DEMAND, a Dimensional Extreme Magnetic Neutron Diffractometer at the High Flux Isotope Reactor

A two-dimensional (2D) Anger camera detector has been used at the HB-3A four-circle single-crystal neutron diffractometer at the High Flux Isotope Reactor (HFIR) since 2013. The 2D detector has enabled the capabilities of measuring sub-mm crystals and spin density maps, enhanced the efficiency of data collection and phase transition detection, and improved the signal-to-noise ratio. Recently, the HB-3A four-circle diffractometer has been undergoing a detector upgrade towards a much larger area, magnetic-field-insensitive, Anger camera detector. The instrument will become capable of doing single-crystal neutron diffraction under ultra-low temperatures (50 mK), magnetic fields (up to 8 T), electric fields (up to 11 kV/mm), and hydrostatic high pressures (up to 45 GPa). Furthermore, half-polarized neutron diffraction is also available to measure weak ferromagnetism and local site magnetic susceptibilities. With the new high-resolution 2D detector, the four-circle diffractometer has become more powerful for studying magnetic materials under extreme sample environment conditions; hence, it has been given a new name: DEMAND.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Isotropic parallel antiferromagnetism in the magnetic field induced charge-ordered state of $\mathrm{Sm Ru_4 P_{12}}$ caused by $p - f$ hybridization

Nature of the field-induced charge-ordered phase (phase II) of SmRu 4 P 12 has been investigated by resonant x-ray diffraction (RXD) and polarized neutron diffraction (PND), focusing on the relationship between the atomic displacements and the antiferromagnetic (AFM) moments of Sm. From the analysis of the interference between the nonresonant Thomson scattering and the resonant magnetic scattering, combined with the spectral function obtained from x-ray magnetic circular dichroism, it is shown that the AFM moment of Sm prefers to be parallel to the field (m AF ∥ H), giving rise to large and small moment sites around which the P 12 and Ru cage contract and expand, respectively. This is associated with the formation of the staggered ordering of the Γ 7 -like and Γ 8 -like crystal-field states, providing a strong piece of evidence for the charge order. PND was also performed to obtain complementary and unambiguous conclusion. In addition, isotropic and continuous nature of phase II is demonstrated by the field-direction invariance of the interference spectrum in RXD. Finally, crucial role of the p-f hybridization is shown by resonant soft x-ray diffraction at the P K edge (1s↔3p), where we detected a resonance due to the spin polarized 3p orbitals reflecting the AFM order of Sm.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Spin reorientation and magnetoelastic coupling in Tb 6 Fe 1-x Co x Bi 2 (x = 0, 0.125, 0.25, 0.375) alloy system

Tb 6 FeBi 2 adopts a noncentrosymmetric crystal structure and orders ferromagnetically at T C1 = 250 K with an additional magnetic transition at T C2 = 60 K. The low temperature magnetoelastic response in this material is strong, and is enhanced by cobalt substitution. In this paper, the temperature dependence of the atomic and magnetic structure of Tb 6 Fe 1-x Co x Bi 2 (x = 0, 0.125, 0.25, and 0.375) is reported from powder X-ray diffraction (XRD) and powder neutron diffraction (PND) measurements. Below the Néel temperature a ferrimagnetic ordering between the terbium and iron moments exists in all compounds studied. Related to the enhanced magnetostructural response, the Co-doped compounds undergo a crystallographic phase transition below about 60 K. This transition also involves a canting of the magnetic moments away from the c-axis. The structural transition is sluggish and not fully completed in the parent Tb 6 FeBi 2 compound, where a mixture of monoclinic and hexagonal phases is identified below 60 K. Lastly, the spin reorientation transition is discussed in terms of competing exchange interactions and magnetocrystalline anisotropies of the two Tb sites and Fe/Co sublattices.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Neutron scattering study of tantalum monohydride and monodeuteride

Powder samples of TaH 0.89 and TaD0.96 are synthesized under a hydrogen (deuterium) pressure of 2.8 GPa and a temperature of 250 °C, then quenched to the liquid nitrogen temperature, recovered to ambient pressure and studied by neutron diffraction (ND) and inelastic neutron scattering (INS). The ND study shows that both hydrogen and deuterium atoms occupy tetrahedral interstitial sites in a distorted body centered cubic (bcc) crystal structure of metal atoms, while the ordering scenarios in TaH 0.89 and TaD 0.96 are different. Hydrogen and deuterium atoms are ordered in a layered fashion, forming long period superstructures with space groups P$\bar{4}$ and P222, respectively, so that the unit cells of the crystal structures of TaH 0.89 and TaD 0.96 are $\sqrt{2}$ × $\sqrt{2}$ × 7 and $\sqrt{2}$ × $\sqrt{2}$ × 8 supercells of the initial cubic unit cell. The INS study demonstrates a pronounced “soft” (trumpet-like) anharmonicity of the potential well for H and D atoms.

08 HYDROGEN↗
DOE OSTI2018

Phase transformations in oxides above 2000°C: experimental technique development

Here, the oxidation of boride and carbide-based ultra-high-temperature ceramics is the primary limiting factor for their use as aerodynamic surfaces. Understanding the behaviour of the oxides that can result from oxidation of metal borides and carbides at very high temperatures is essential to optimise and tailor the performance of these materials; yet experimental thermodynamic and structural data for refractory oxides above 2000°C are mostly absent. The following techniques that can be applied to fill this gap are discussed: (i) commercial ultra-high-temperature differential thermal analysis for investigation of phase transformations and melting in inert environments to 2500°C, (ii) a combination of laser heating with a splittable nozzle aerodynamic levitator for splat quenching and drop calorimetry from temperatures limited only by sample evaporation, (iii) synchrotron X-ray and neutron diffraction on laser-heated aerodynamically levitated oxide samples for in situ observation of phase transformations in variable atmospheres, refinement of high-temperature structures and thermal expansion. Recent experimental findings include anomalous thermal expansion of the defect fluorite phase of YSZ, thermodynamics of pyrochlore–fluorite transformation from high-temperature structure refinements, and measurement of thermal expansion to the melting temperatures and fusion enthalpies of Zr, Hf, La, Yb and Lu oxides. These methods provide temperatures, enthalpies and volume change for phase transformations above 2000°C, which are required for thermodynamic assessments and calculation of phase diagrams of multicomponent systems.

36 MATERIALS SCIENCE↗
DOE OSTI2018

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

In this paper, the physical properties of the spinel LiGaCr 4 S 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 LiGaCr 4 S 8 .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Complementary Measurements of Residual Stresses Before and After Base Plate Removal in an Intricate Additively-Manufactured Stainless-Steel Valve Housing

Residual stress measurements using neutron diffraction and the contour method were performed on a valve housing made from 316 L stainless steel powder with intricate three-dimensional internal features using laser powder-bed fusion additive manufacturing. The measurements captured the evolution of the residual stress fields from a state where the valve housing was attached to the base plate to a state where the housing was cut free from the base plate. Making use of this cut, thus making it a non-destructive measurement in this application, the contour method mapped the residual stress component normal to the cut plane (this stress field is completely relieved by cutting) over the whole cut plane, as well as the change in all stresses in the entire housing due to the cut. The non-destructive nature of the neutron diffraction measurements enabled measurements of residual stress at various points in the build prior to cutting and again after cutting. Good agreement was observed between the two measurement techniques, which showed large, tensile build-direction residual stresses in the outer regions of the housing. The contour results showed large changes in multiple stress components upon removal of the build from the base plate in two distinct regions: near the plane where the build was cut free from the base plate and near the internal features that act as stress concentrators. These observations should be useful in understanding the driving mechanisms for builds cracking near the base plate and to identify regions of concern for structural integrity. Neutron diffraction measurements were also used to show the shear stresses near the base plate were significantly lower than normal stresses, an important assumption for the contour method because of the asymmetric cut.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Single crystal magnetic structure and susceptibility of CoSe{sub 2}O{sub 5}

The structure of CoSe{sub 2}O{sub 5} consists of one-dimensional ribbons of edge-sharing CoO{sub 6} octahedra bound together by polyanionic subunits of Se{sub 2}O{sub 5}. Previous work on polycrystalline samples reported a canted antiferromagnetic arrangement of the magnetic moments below the ordering temperature of 8.5 K. Here, we report a single crystal investigation using variable temperature and field magnetic susceptibility and low-temperature neutron diffraction to more precisely characterize the nature of the magnetic ground state of CoSe{sub 2}O{sub 5}. Contrary to previous reports, we find that the single crystal magnetic structure shows no canting of the antiferromagnetic ground state, and in the process have identified several field-induced changes to the magnetization. We discuss these results in the context of the revised magnetic structure and highlight the importance of crystal growth for the accurate characterization of these properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Enhancing fatigue life by ductile-transformable multicomponent B2 precipitates in a high-entropy alloy

Catastrophic accidents caused by fatigue failures often occur in engineering structures. Thus, a fundamental understanding of cyclic-deformation and fatigue-failure mechanisms is critical for the development of fatigue-resistant structural materials. Here we report a high-entropy alloy with enhanced fatigue life by ductile-transformable multicomponent B2 precipitates. Its cyclic-deformation mechanisms are revealed by real-time in-situ neutron diffraction, transmission-electron microscopy, crystal-plasticity modeling, and Monte-Carlo simulations. Multiple cyclic-deformation mechanisms, including dislocation slips, precipitation strengthening, deformation twinning, and reversible martensitic phase transformation, are observed in the studied high-entropy alloy. Its improved fatigue performance at low strain amplitudes, i.e., the high fatigue-crack-initiation resistance, is attributed to the high elasticity, plastic deformability, and martensitic transformation of the B2-strengthening phase. This study shows that fatigue-resistant alloys can be developed by incorporating strengthening ductile-transformable multicomponent intermetallic phases.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Short- and medium-range order in Sb–Se glasses

Neutron diffraction measurements were performed to investigate the structure of Sb{sub x}Se{sub 100−x} bulk glasses with x=5, 10, 15, 20 and 25 at% Sb. The total pair distribution functions show two peaks at 2.36 Å and 2.64 Å, which are attributed to Se–Se and Sb–Se bonds, respectively. The coordination numbers calculated from these peaks indicate that Sb atoms are three-coordinated and Se atoms are two-coordinated for all the above compositions. However, the composition dependences of the first two peaks in the structure factors show an obvious change between 15 and 20 at% Sb, indicating that the medium-range structure is changed in this range of Sb content. In order to elucidate the medium-range structure, reverse Monte Carlo simulation was used with coordination number constraints. The structure models consisting of a mixture of the SbSe{sub 3/2} network and Se{sub n} chain clusters were in good agreement with neutron diffraction data for Se-rich glass (5, 10 and 15 at% Sb). On the other hand, a better fit was obtained for Sb{sub 25}Se{sub 75} glass with a model based on the network structure formed by connected SbSe{sub 3} units. - Graphical abstract: A 50 Å slice of the RMC configuration for Sb{sub 15}Se{sub 85} glass. - Highlights: • Sb atoms are three-coordinated and Se atoms are two-coordinated. • The medium-range structure changes between 15 and 20 at%. • The phase-separation tendency is observed in Se-rich glasses.

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

Synthesis and Characterization of 5- and 6- Coordinated Alkali Pertechnetates

The local chemistry of technetium-99 ( 99 Tc) in oxide glasses is important for understanding the incorporation and long-term release of Tc from nuclear waste glasses, both those for legacy defense wastes and fuel reprocessing wastes. Tc preferably forms Tc(VII), Tc(IV), or Tc(0) in glass, depending on the level of reduction of the melt. Tc(VII) in oxide glasses is normally assumed to be isolated pertechnetate TcO 4 - anions surrounded by alkali, but can occasionally precipitate as alkali pertechnetate salts such as KTcO 4 and NaTcO 4 when Tc concentration is high. In these cases, Tc(VII) is 4-coordinated by oxygen. A reinvestigation of the chemistry of alkali-technetium-oxides formed under oxidizing conditions and at temperatures used to prepare nuclear waste glasses showed that higher coordinated alkali Tc(VII) oxide species had been reported, including those with the TcO 5 - and TcO 6 - anions. The chemistry of alkali Tc(VII) and other alkali-Tc-oxides is reviewed, along with relevant synthesis conditions. Additionally, we report attempts to make 5- and 6-coordinate pertechnetate compounds of K, Na, and Li, i.e. TcO 5 - and TcO 6 -. It was found that higher coordinated species are very sensitive to water, and easily decompose into their respective pertechnetates. It was difficult to obtain pure compounds, but mixtures of the pertechnetate and other phase(s) were frequently found, as evidenced by x-ray absorption spectroscopy (XAS), neutron diffraction (ND), and Raman spectroscopy. Low temperature electron paramagnetic resonance (EPR) measurements showed the possibility of Tc(IV) and Tc(VI) in Na 3 TcO 5 and Na 5 TcO 6 compounds. Here, it was hypothesized that the smaller counter cation would result in more stable pertechnetates. To confirm the synthesis method, LiReO 4 and Li 5 ReO 6 were prepared, and their Raman spectra match those in the literature. Subsequently, the Tc versions LiTcO 4 and Li 5 TcO 6 were synthesized and characterized by ND, Raman spectroscopy, XANES, and EXAFS. The Li 5 TcO 6 was a marginally stable compound that appears to have the same structure as that known for Li 5 ReO 6 . Implications of the experimental work on stability of alkali technetate compounds and possible role in the volatilization of Tc are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Magnetic structure of triangular lattice compound Tb2Ni0.90Si2.94

AlB 2 -type ternary intermetallic compound Tb 2 Ni 0.90 Si 2.94 (space group P 6=mmm, hP 3, No. 191) was reported to exhibit spin freezing behaviour of the ferromagnetic clusters present in the system below T f = 9:9 K, along with the presence of spatially limited antiferromagnetic phase. In this work, on the basis of variable temperature zero-field neutron diffraction measurements, we have shown that the antiferromagnetic phase transition occurs for the compound below T N ~13 K. Neutron diffraction study indicates ab-plane non-collinear sine-modulated antiferromagnetic ordering of the system with wave vectors of k 1 = [±1/6, ±1/6, 0] and k 2 = [±1/3, ±1/3, 0] down to 1.7 K. The weak and diffuse nature of the magnetic Bragg peaks along with limited coherence length further confirm the short-range nature of the antiferromagnetic phase in this compound.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Magnetic interactions in PdCrO 2 and their effects on its magnetic structure

We report a neutron scattering study of the metallic triangular lattice antiferromagnet PdCrO 2 . Powder neutron diffraction measurements confirm that the crystalline space group symmetry remains R$\bar{3}$m below T N . This implies that magnetic interactions consistent with the crystal symmetry do not stabilize the noncoplanar magnetic structure, which was one of two structures previously proposed on the basis of single crystal neutron diffraction measurements. Inelastic neutron scattering measurements find two gaps at low energies, which can be explained as arising from a dipolar-type exchange interaction. This symmetric anisotropic interaction also stabilizes a magnetic structure very similar to the coplanar magnetic structure, which was also suggested by the single crystal diffraction study. In conclusion, the higher-energy magnon dispersion can be modelled by linear spin-wave theory with exchange interactions up to sixth nearest neighbors, but discrepancies remain which hint at additional effects unexplained by the linear theory.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

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

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 planes 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.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Disorder-driven spin-reorientation in multiferroic h-YMn{sub 1−x}Fe{sub x}O{sub 3}

Magnetic structure evolution of multiferroic hexagonal YMn{sub 1−x}Fe{sub x}O{sub 3} (x = 0, 0.05, and 0.1) has been studied by carrying out detailed temperature-dependent neutron diffraction at zero and 5 T fields. Thermodynamic data confirm antiferromagnetic ordering at T{sub N} in all the compositions. Our sub-T{sub N} neutron diffraction results assign the magnetic structure of pure YMnO{sub 3} to Γ{sub 1} irreducible representation. Over the perturbative-doping range, magnetic structure changes via Γ{sub 1} + Γ{sub 2} for YMn{sub 0.95}Fe{sub 0.05}O{sub 3} on to Γ{sub 2} for YMn{sub 0.9}Fe{sub 0.1}O{sub 3}, as the maiden compositional analogue of spin-reorientation; its occurrence in temperature-domain already reported for several manganites. Moreover, while the large thermal isostructural changes observed above T{sub N} are subdued in the ordered state, small alterations by the applied 5 T-field are relatively uniform across, confirming strong magneto-elastic nature of the system. Decrease of the ordered magnetic moment (μ{sub ord}) and planar magnetic frustration noted with Fe-doping is enhanced by the applied field, apparently through canting.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Presence of Induced Weak Ferromagnetism in Fe-Substituted YFe x Cr 1–x O 3 Crystalline Compounds

Fe-substituted YFe x Cr 1–x O 3 crystalline compounds show promising magnetic and multiferroic properties. Here we report the synthesis and characterization of several compositions from this series. Using the autocombustion route, various compositions (x = 0.25, 0.50, 0.6, 0.75, 0.9, and 1) were synthesized as high-quality crystalline powders. In order to obtain microscopic and atomic information about their structure and magnetism, characterization was performed using room temperature X-ray diffraction and energy dispersion analysis as well as temperature-dependent neutron diffraction, magnetometry, and 57 Fe Mössbauer spectrometry. Rietveld analysis of the diffraction data revealed a crystallite size of 84 (8) nm for YFeO 3 , while energy dispersion analysis indicated compositions close to the nominal compositions. The magnetic results suggested an enhancement of the weak ferromagnetism for the YFeO 3 phase due to two contributions. First, a high magnetocrystalline anisotropy was associated with the crystalline character that favored a unique high canting angle of the antiferromagnetic phase (13°), as indicated by the neutron diffraction analysis. This was also evidenced by the high magnetic hysteresis curves up to 90 kOe by a remarkable high critical coercivity value of 46.7 kOe at room temperature. Second, the Dzyaloshinskii–Moriya interactions between homogenous and heterogeneous magnetic pairs resulted from the inhomogeneous distribution of Fe 3+ and Cr 3+ ions, as indicated by 57 Fe Mössbauer studies. Together, these results point to new methods of controlling the magnetic properties of these materials.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Investigating the non-classical M-H 2 bonding in OsClH 3 (PPh 3 ) 3

Dihydrogen ligation to metal centers results in a wide range of metal-hydrogen interactions. Compounds containing non-classical dihydrogen ligands in which the H-H contacts are significantly longer than the 0.74 A distance found in solid H 2 are classified as Kubas-like compounds, stretched dihydrogen ligands, or compressed dihydrides, depending on the H-H contact length. Compounds containing stretched dihydrogen and compressed dihydride ligands are somewhat rare. Developing a more complete understanding of the metal-hydrogen and hydrogen-hydrogen interactions in these species may provide insights into the mechanisms for the oxidative addition reaction and hydrogen storage. Here, we use diffraction and inelastic neutron scattering (INS) measurements, paired with both molecular and solid-state density functional theory (DFT), to fully characterize the nature of the metal-hydrogen and hydrogen-hydrogen interactions in a previously reported compound, OsClH 3 (PPh 3 ) 3 . In that report, the H-H distance was measured as 1.48(2) A by single-crystal neutron diffraction and was described as a "stretched" dihydrogen. The INS-generated phonon density of states is well described by the DFT calculations, including those normal modes dominated by the vibrational motions of the three Os-ligated hydrogen atoms. Additionally, the resulting calculated electron charge density landscape indicates that there is no remnant bonding character between the Os-ligated hydrogen atoms in the compound. Based on these findings, we update the understanding of the metal-hydrogen bonding in this complex and reclassify it as a compressed dihydride. As such, OsClH 3 (PPh 3 ) 3 represents a rare example of a non-classical compressed dihydride species.

08 HYDROGEN↗