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DOE OSTI2025

Crystal structure and thermal expansion of Ta 2 ⁢O 5 from neutron diffraction

Tantalum pentoxide (Ta 2 ⁢O 5 ) is a component of technologies ranging from photographic lenses to medical implants. Despite more than six decades of interest, however, there is no consensus on the crystal structure of Ta 2 ⁢O 5 . Here, we report the results of neutron diffraction experiments on Ta 2⁢ O 5 powders at temperatures up to 1000⁢°⁢C. Because neutron diffraction is sensitive to the positions of O atoms in the presence of heavy elements, our results provide strong evidence that the orthorhombic L SR structure can account for experimental observations better than any other proposal in the literature. Here, we also determine the anisotropic crystallographic thermal expansion parameters of Ta 2 ⁢O 5 , which are important for modeling the performance of Ta 2⁢ O 5 -bearing technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Crystal structure of 0.96(Na 0.5 Bi 0.5 TiO 3 )-0.04(BaTiO 3 ) from combined refinement of x-ray and neutron diffraction patterns

High-resolution x-ray and neutron diffraction of (0.96)Na 0.5 Bi 0.5 TiO 3 –(0.04)BaTiO 3 (NBT-4BT) reveal subtle structural distortions that evidence lower symmetry than allowed in the R3c space group. The combined refinement that best models the diffraction patterns is a two phase mixture of a monoclinic Cc phase and a minor fraction of a metrically cubic Pm 3¯ m phase (13 wt. %). The cubic phase is utilized to account for nanometer-scale regions whose local deviations from the long-range symmetry are not observed, such as polar nano-regions or tetragonal platelets. This suggests that the low symmetry found in the NBT-rich phases extends from 0 at. % to at least 4 at. % BT.

Usher, T -M↗

DOE OSTI2014

Processing of Neutron Diffraction Data for Strain Measurement in Geological Materials

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

Polsky, Yarom↗

DOE OSTI2025

High-resolution neutron diffraction determination of noncollinear antiferromagnetic order in the honeycomb magnetoelectric Fe 4 ⁢Nb 2⁢ O 9

Magnetoelectric systems offer potential for device applications exploiting coupled states between electric and magnetic properties. Among magnetoelectric materials, Fe 4 ⁢Nb 2 ⁢O 9 has attracted special attention because of its pronounced dielectric signal at high magnetic transition temperatures. However, the magnetic ground state, which is essential information for understanding its unusual magnetoelectricity, remains unclarified. Here, we report a noncollinear magnetic ground state of Fe 4 ⁢Nb 2 ⁢O 9 . To examine the magnetoelectric effect associated with sequential magnetic and structural transitions upon cooling, we conducted combined x-ray diffraction, magnetic susceptibility, magnetization, dielectric constant, and magnetodielectric experiments. Powder neutron diffraction experiments revealed a series of magnetic Bragg peaks and clear splitting of peaks via structural transition. Magnetic Rietveld refinements, combined with group theory analysis, determined a noncollinear antiferromagnetic structure including a significant 𝑐-axis moment component at 1.5 K. This article provides insights into the understanding of its magnetoelectric properties.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2012

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

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

36 MATERIALS SCIENCE↗

DOE OSTI2011

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

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.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Neutron diffraction probing hydrogen in monoclinic H 2 VOPO 4

Light hydrogen atoms are resolvable with neutrons; however, the massive incoherent background inhibits the diffraction quality. To improve the signal, isotope treatment by deuteration becomes a prerequisite for a successful crystallographic understanding of hydrogen-containing materials by neutron diffraction. Thanks to the low-background and high-resolution time-of-flight neutron diffractometer, this work demonstrates a direct and successful measurement of high-quality neutron diffraction patterns of H 2 VOPO 4 powders, a precursor of a high-capacity alkali-ion battery cathode. The Rietveld refinement identifies the hydrogen coordinates, occupancy, and thermal parameters in the H 2 VOPO 4 lattice. Finally, the result highlights the unique capability of neutron diffraction for the structure characterization of hydrogen-containing materials, potentially without requiring costly and possibly artifact-inducing deuteration for neutron diffraction.

36 MATERIALS SCIENCE↗

DOE OSTI2025

High-Temperature Neutron Diffraction Study of Vanadium and Vanadium–Niobium Null-Matrix Alloy for Spectrum Normalization

This study systematically evaluates a vanadium–niobium (V 94.1 Nb 5.9 ) null-matrix alloy as a reference material for neutron spectrum normalization and compares its performance with that of pure vanadium under identical experimental conditions. Neutron diffraction experiments are conducted on the VULCAN Engineering Materials Diffractometer at the Spallation Neutron Source, Oak Ridge National Laboratory, over a temperature range from room temperature to 1200 °C under vacuum. Pure vanadium exhibited distinct Bragg peaks across all temperatures, with its diffraction behavior influenced by both sample orientation and temperature. As the temperature increased, the diffraction peaks shifted to larger d-spacings and decreased in intensity, while spectral deviation near d ≈ 2.8 Å exceeded 10% at 1200 °C. In contrast, the V–Nb alloy produced a nearly featureless spectrum over the full d-spacing range, confirming near-complete cancellation of coherent scattering over the wide temperature range. Its spectra were insensitive to sample orientation, temperature, and microstructural evolution, with spectral deviation around d ≈ 2.8 Å exceeded 5% at 1200 °C. In conclusion, these results demonstrate that the V–Nb null-matrix alloy provides a thermally stable, efficient, and reliable normalization standard for time-of-flight diffractometers or other instrument where it is needed, enabling reduced data acquisition time and improved data quality in high-temperature neutron diffraction experiments.

Alloys↗

DOE OSTI2019

Magnetic ordering in rare earth metal dysprosium revealed by neutron diffraction studies in a large-volume diamond anvil cell

A high-pressure low-temperature neutron diffraction study has been carried out on rare earth metal Dysprosium (Dy) to 10.8 GPa and 8 K in a large-volume diamond anvil cell using a spallation neutron source. Dy crystallizes in an ambient pressure hexagonal close packed phase and forms an incommensurate helical antiferromagnetic phase, marked by the appearance of superlattice magnetic peaks below 176 K with a turn-angle between the hexagonal layers that increases both with increasing temperature and pressure. The ferromagnetic transition below 87 K is marked by an increase in intensity of nuclear peaks with disappearance of magnetic superlattice reflections. Dy transforms to an alpha-Samarium ( α-Sm ) phase at 7 GPa and only ferromagnetic ordering is observed for this high pressure phase. Here, the ferromagnetic transition is observed at 59 K in the α-Sm phase at 10.8 GPa in close agreement with the magnetic ordering temperature obtained from electrical transport measurements. In the entire pressure-temperature range of this study, Dy shows a negative thermal expansion coefficient of as much as -2.5 % in the magnetically ordered phases between 200 K and 8 K.

36 MATERIALS SCIENCE↗

DOE OSTI2018

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

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 2 O/D 2 O 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 as an instrument suitable for the study of aligned lipid multi-bilayers.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2019

Thermal desulfurization of pyrite: An in situ high-T neutron diffraction and DTA–TGA study

To study thermal desulfurization of pyrite (FeS 2 ), we conducted in situ neutron diffraction experiments in the temperature range 298–1073 K. Additionally, on heating, pyrite remained stable up to 773 K, at which it started to decompose into pyrrhotite (Fe 1-x S) and S 2 gas. Rietveld analysis of the neutron data from 298 to 773 K allowed determination of the thermal expansion coefficient of pyrite (space group Pa$\overline{3}$) to be α V = 3.7456 × 10 -5 K -1 , which largely results from the expansion of the Fe–S bond. With further increase in temperature to 1073 K, all the pyrite transformed to pyrrhotite (Fe 1-x S) at 873 K. Unit-cell parameters of Fe 1-x S (space group P6 3 /mmc) increase on heating and decrease on cooling. However, the rates in cell expansion are larger than those in contraction. This hysteresis behavior can be attributed to continuous desulfurization of pyrrhotite (i.e., x in Fe 1-x S decreases) with increasing temperature until the stoichiometric troilite (FeS) was formed at 1073 K. On cooling, troilite underwent a magnetic transition to an orthorhombic structure (space group Pnma) between 473 and 573 K. In addition, using differential thermal analysis (DTA) and thermogravimetric analysis (TGA) implemented with a differential scanning calorimeter, we performed kinetic measurements of pyrite decomposition. Finally, detailed peak profile and Arrhenius (k = A exp(-E a /RT)) analyses yielded an activation energy E a of 302.3 ± 28.6 kJ/mol (based on DTA data) or 302.5 ± 26.4 kJ/mol (based on TGA data) and a ln(A) of 35.3 ± 0.1.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Unraveling structural evolution of LiNi 0.5 Mn 1.5 O 4 by in situ neutron diffraction

Here, we report that the electrochemical properties of the spinel LiNi 0.5 Mn 1.5 O 4 cathode material are influenced by the synthesis processes, which determines the impurity phase and the distribution of Ni and Mn in the spinel structure. Taking advantage of neutron's high sensitivity to Ni and Mn, in situ neutron diffraction has been employed to quantify the phase formation/structural evolution process under continuous heating/cooling and isothermal annealing conditions. The results show that the subtle Ni and Mn ordering process occurs slowly at 700 °C and the degree of ordering can be controlled by the annealing time. At temperatures above 750 °C, the LiNi 0.5 Mn 1.5 O 4 spinel phase starts to decompose into the rock-salt impurity phase accompanied by the release of O 2 . The rock-salt phase reverts back to the spinel phase upon cooling along with the oxygen uptake. In conclusion, the dynamic process of structural evolution of LiNi 0.5 Mn 1.5 O 4 that was unraveled by in situ neutron diffraction is valuable for guiding the synthesis of cathode materials with desirable properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Flux Growth of Cerium Nickel Gallides Studied by In Situ Neutron Diffraction

In this work, reactions of cerium and nickel in excess molten gallium were monitored by neutron diffraction during heating and cooling. The formation of binary intermediates CeGa 2 and Ni 2 Ga 3 was observed during heating. During cooling of the molten mixture from 900 °C, precipitation of BaAl 4 -type CeNi 0.74 Ga 3.26 occurred at 850 °C. Upon cooling to 650 °C, this compound reacted in the flux to form Ce 2 NiGa 10 and then Ce 2 NiGa 12 , the latter of which persisted to room temperature. Making use of this information, subsequent reactions were quenched at 750 °C to isolate crystals of CeNi 0.74 Ga 3.26 for further study. Similar reactions replacing Ce with La and quenching above 750 °C yielded LaNi 0.35 Ga 3.65 crystals. Magnetic susceptibility studies on CeNi 0.74 Ga 3.26 indicate that the cerium is trivalent; the Ce 3+ moments undergo a strongly anisotropic ferromagnetic ordering with moment perpendicular to the c axis below 7 K. Heat capacity data show little evidence of heavy fermion behavior. Resistivity measurements show that both LaNi0.35Ga3.65 and CeNi 0.74 Ga 3.26 exhibit metallic behavior. Density of states calculations support this and indicate that Ni/Ga mixing in the compound stabilizes the structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

A furnace with rotating load frame for in situ high temperature deformation and creep experiments in a neutron diffraction beam line

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). We 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.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Solving the P–O/P–OH riddle: direct synthesis and neutron diffraction characterization of dianionic dithiophosphonates

Here, we report the first definitive neutron diffraction study aimed at resolving the P–OH/P$=$O structural ambiguity in metal dithiophosphonates. The small NH 4 counterion forces a rare syn-configuration via an extended hydrogen-bonding network. Neutron analysis definitively confirmed the fully deprotonated P$=$O moiety, thus confirming the formation of a dianionic dithiophosphonate, a versatile synthon in homoleptic and heteroleptic coordination environments.

Pillay, Michael N. [National Dong Hwa Univ. (Taiwa↗

DOE OSTI2018

Synchrotron X-Ray and Neutron Diffraction, Total Scattering, and Small-Angle Scattering Techniques for Rechargeable Battery Research

Synchrotron X-ray and neutron scientific facilities are the most advanced resources with a large variety of state of the art instrumentations and powerful tools for materials research. X-rays and neutrons interact with matter in different ways and offer complementary views of materials at various levels. In this article, we will focus on the techniques and applications of synchrotron X-ray and neutron diffraction, total scattering and small-angle scattering for rechargeable battery research. They all belong to the elastic scattering category and provide structure information at different length scales. Here, the diffraction method is generally used to determine the phase and precise atomistic information of crystalline materials, while the total scattering coupled with pair-distribution function analysis can probe local atomic structure of materials no matter they are well crystallized or in amorphous/liquid phases. The small-angle scattering techniques provide us with material size and shape information at nanometer scales. Advantages of synchrotron high-energy X-rays will also be presented, which is particularly suited for the pair-distribution-function studies. We will pay much attention to the technical perspectives and some experimental specifications for the best uses of these methods for battery materials research.

25 ENERGY STORAGE↗

DOE OSTI2015

Crystal structure of α- and β-Na{sub 2}U{sub 2}O{sub 7}: From Rietveld refinement using powder neutron diffraction data

The crystal structures of α- and β-Na{sub 2}U{sub 2}O{sub 7} have been determined from neutron powder diffraction. At 293 K, the compound α-Na{sub 2}U{sub 2}O{sub 7} has a monoclinic unit cell, space group P2{sub 1}/a, with a=12.7617(14) Å, b=7.8384(10) Å, c=6.8962(9) Å, β=111.285(9)°, and Z=4. At 773 K, β-Na{sub 2}U{sub 2}O{sub 7} is also monoclinic, space group C2/m, with a=12.933(1) Å, b=7.887(1) Å, c=6.9086(8) Å, β=110.816(10)°, and Z=4. The structures can be described by layers U{sub 2}O{sub 7}{sup 2−} built from corner linked deformed UO{sub 6} octahedra with pentagonal UO{sub 7} bipyramids in between linked with common edges to each other and to the octahedra. The Na atoms occupy the interlayer space. The Na{sub 2}U{sub 2}O{sub 7} layers are similar as in K{sub 2}U{sub 2}O{sub 7}, but with a different stacking sequence of the layers. The layers in β-Na{sub 2}U{sub 2}O{sub 7} are more symmetric. The relationship with the compounds A{sub 2}U{sub 2}O{sub 7} (A=K, Rb, and Cs) is discussed. - Graphical abstract: The U{sub 2}O{sub 7} layer of α-Na{sub 2}U{sub 2}O{sub 7} (left) at 293 K and of β-Na{sub 2}U{sub 2}O{sub 7} (right) at 773 K determined by neutron diffraction. Some Na atoms between the layers are visible. - Highlights: • Na{sub 2}U{sub 2}O{sub 7} has been prepared by means of a solid state reaction. • The structure has been determined using neutron diffraction. • At 293 K, the compound adopts a monoclinic structure with space group P2{sub 1}/a. • The structure at 773 K is closely related, and is described in the space group C2/m.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2013

Preparation and neutron diffraction study of Dion-Jacobson type oxynitrides LiLaTa{sub 2}O{sub 7−3x}N{sub 2x} (x = 0.09, 0.29)

Highlights: ► Dion-Jacobson oxynitrides LiLaTa{sub 2}O{sub 7−3x}N{sub 2x}□{sub x} (x < 0.3) by ammonolysis of LiLaTa{sub 2}O{sub 7}. ► Enhanced thermal stability and band gap narrowing by the oxynitride modification. ► Locations of N and □ within LiLaTa{sub 2}O{sub 7−3x}N{sub 2x} by neutron diffraction and {sup 7}Li MAS NMR. -- Abstract: Ammonolytic heating of Dion-Jacobson type layered perovskite LiLaTa{sub 2}O{sub 7} produced oxynitride derivatives LiLaTa{sub 2}O{sub 7−3x}N{sub 2x}□{sub x}via the substitution, 3O{sup 2−} → 2N{sup 3−} + □. The nitridation level increased with raising the temperature and/or increasing the time of reaction, reaching the limit at x ≈ 0.3 by the ammonolysis at 650 °C for 48 h. Upon the nitridation, tetragonal pristine lattice underwent a axis expansion together with c axis contraction. Neutron Rietveld refinement of LiLaTa{sub 2}O{sub 7} and LiLaTa{sub 2}O{sub 7−3x}N{sub 2x} (x = 0.09, 0.29) revealed that the Li-centered tetrahedra are gradually compressed along the 2-fold rotation axis, with the increase of x. Solid state {sup 7}Li nuclear magnetic resonance spectroscopy suggested that the anion vacancy resides mostly on the interlayer surface of perovskite block. As measured from the diffuse-reflectance spectroscopy, the nitridation induced marked reduction in the band gap magnitude, from 4.11 eV (x = 0) to 3.35 eV (x = 0.09) to 2.76 eV (x = 0.29).

36 MATERIALS SCIENCE↗