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At least 811 records · Page 45
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Control of deviatoric stress in the diamond anvil cell through thermal expansion mismatch stress in thin films

Elastic and plastic properties of materials and phase transitions at extreme conditions vary with both hydrostatic pressure and deviatoric stress. To generate and measure controlled deviatoric stress at pressures beyond those accessible with large volume differential and rotational presses and optical access for spectroscopy, experiments tested the combination of diamond anvil cell and thin film technology. Thin films of polycrystalline Cr-doped Al 2 O 3 ruby were prepared using pulsed laser deposition on single-crystal substrates of either Al 2 O 3 sapphire or yttria-stabilized cubic zirconia for contrasting initial film stress, and loaded in diamond anvil cells for confining stress. The piezospectroscopic response of the ruby films demonstrates consistently higher deviatoric stress in the film on zirconia relative to the film on the control sapphire, and an increase in deviatoric stress with applied load. Complementary synchrotron X-ray diffraction of the zirconia substrate confirmed that no pressure-induced phase transitions impacted the stress state of the ruby film, but differences in compressibility of film and substrate result in changes in film stress analogous to thermal expansion mismatch. Furthermore, this technique may be applied to evaluate elastic and plastic response of thin films of a variety of materials under extreme stress.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Dipole-lattice nanoparticle resonances in finite arrays

We investigate how the periodic lattices define the collective optical characteristics of the silicon and titanium nanoparticle arrays. We examine the effects of dipole lattice on the resonances of optical nanostructures, including those made of lossy materials, such as titanium. Our approach involves employing coupled-electric-magnetic-dipole calculations for finite-size arrays, as well as lattice sums for effectively infinite arrays. Our model shows that the convergence to the infinite-lattice limit is faster when the resonance is broad, requiring fewer array particles. Our approach differs from previous works by altering the lattice resonance through modifications in the array period. We observed that a higher number of nanoparticles is necessary to achieve convergence to the infinite-array limit. Additionally, we observe that the lattice resonances excited next to higher diffraction orders (such as second order) converge more quickly toward the ideal case of an infinite array than the lattice resonances related to the first diffraction order. This work reports on the significant advantages of using a periodic arrangement of lossy nanoparticles and the role of collective excitation in enhancing response from transition metals, such as titanium, nickel, tungsten, and so on. The periodic arrangement of nanoscatterers allows for the excitation of strong dipoles, boosting the performance of nanophotonic devices and sensors by improving the strength of localized resonances.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Combinatorial Cu-Ni Alloy Thin-Film Catalysts for Layer Number Control in Chemical Vapor-Deposited Graphene

We synthesized a combinatorial library of CuxNi1−x alloy thin films via co-sputtering from Cu and Ni targets to catalyze graphene chemical vapor deposition. The alloy morphology, composition, and microstructure were characterized via scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), and X-ray diffraction (XRD), respectively. Subsequently, the CuxNi1−x alloy thin films were used to grow graphene in a CH4-Ar-H2 ambient at atmospheric pressure. The underlying rationale is to adjust the CuxNi1−x composition to control the graphene. Energy dispersive x-ray spectroscopy (EDS) analysis revealed that a continuous gradient of CuxNi1−x (25 at. % < x < 83 at.%) was initially achieved across the 100 mm diameter substrate (~0.9%/mm composition gradient). The XRD spectra confirmed a solid solution was realized and the face-centered cubic lattice parameter varied from ~3.52 to 3.58 A˙, consistent with the measured composition gradient, assuming Vegard’s law. Optical microscopy and Raman analysis of the graphene layers suggest single layer growth occurs with x > 69 at.%, bilayer growth dominates from 48 at.% < x < 69 at.%, and multilayer (≥3) growth occurs for x < 48 at.%, where x is the Cu concentration. Finally, a large area of bi-layer graphene was grown via a CuxNi1−x catalyst with optimized catalyst composition and growth temperature.

2D materials↗
DOE OSTI2024

Defect-Limited Mobility and Defect Thermochemistry in Mixed A-Cation Tin Perovskites: (CH3NH3)1-xCsxSnBr3

Hybrid organic-inorganic semiconductors crystallizing in the perovskite structure present a significant opportunity for realizing defect-tolerant semiconductors. In this work, we examine the solid solution, (CH3NH3)1-xCsxSnBr3, and identify the thermochemistry dictating the intrinsic carrier concentrations and how local structural distortions influences this electronic behavior. This family of compounds exhibits the expected systematic trend in decreasing optical gap with the cesium to methylammonium A-site mixing ratio, x, in the visible region. However, the carrier mobility, as determined from time-resolved microwave conductivity measurements, trends opposite to that expected from first-principles calculations combined with Boltzmann scattering theory calculations of the carrier mobility. We propose that this is a result of increasing carrier scattering with x in (CH3NH3)1-xCsxSnBr3 due to a significant increase in the carrier density with x. By examining the dependence of the carrier density as a function of x, we infer the compositional-dependence of the average enthalpy and nonconfigurational entropy per defect. While diffraction reveals a cubic aristotypic perovskite structure as a function of x at room temperature, the pair distribution functions obtained from synchrotron X-ray total scattering from these materials are better described by symmetry-adapted displacement modes of the Pm3m crystal structure, which we attribute to a large degree of anharmonic dynamics of the atom positions. This analysis shows that CH3NH3+-rich compositions retain mostly linear Sn-Br-Sn bonding environments through the displacements, while Cs+-rich compositions lead to more significantly bent Sn-Br-Sn environments. We propose that these bent bonding arrangements in Cs-rich compositions yield a higher propensity for defect formation. This also provides a rationale for carrier trapping that gives rise to anomalous microwave transients. Together, these results provide insight into the structure-dynamics-properties relationships in this highly anharmonic system with high amplitude atomic motions and low defect formation energies.

defect thermochemistry↗
DOE OSTI2026

Shock compression of diamond single crystals to 120 GPa: Refractive index and nonlinear photoelasticity

The optical response of transparent solids at extreme conditions is important for both fundamental science and many applications. Strong transparent solids are of particular interest for use as optical windows in dynamic compression experiments. Due to diamond’s exceptional strength and optical properties, laser-driven shock experiments and plate impact experiments were carried out to examine the diamond optical response for shock wave compression along two different crystal orientations. Using laser interferometry at 532 nm and 1550 nm wavelengths, optical transparency was observed and refractive indices were determined for [100] diamond at stresses up to 119 GPa and for [111] diamond at stresses up to 87 GPa. From these results, the nonlinear photoelastic response for [100] and [111] diamond was determined, revealing significant dependence on both crystal orientation and laser wavelength. To enable [100] diamond as an interferometry window in dynamic compression experiments, the requisite window corrections were determined for 532 nm and 1550 nm wavelengths. Because of diamond’s excellent x-ray transparency, the present findings will be particularly useful for incorporating [100] diamonds as windows in dynamic compression experiments involving x-ray diffraction or other x-ray diagnostics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Task Sharing of Proton Incorporation in Vertically Aligned Nanocomposite Triple Conductors: Growth, Structure, and Surface Exchange Kinetics

As protonic ceramic electrolysis cells emerge for efficient H 2 production, there is a need to develop air electrode materials enabling fast, durable steam splitting and proton incorporation. Single-phase triple conductors may fail to satisfy the myriad performance/stability requirements, and their critical charge-carriers (holes, oxygen vacancies, and protons) are in competition, limiting their concentrations. Instead, we propose task-sharing, vertically aligned nanocomposites (VANs), comprising a proton conductor (BaZr 0.9 Y 0.1 O 3-δ ) and a redox-active mixed ionic electronic conductor (Ce 0.9 Pr 0.1 O 2-δ ), that may enable rapid proton surface exchange at the solid–gas interface and transport along the solid–solid heterointerfaces. We grew VANs by pulsed laser deposition and investigated the interplay between their processing conditions, structure, and proton and oxygen surface exchange kinetics. We varied the substrate temperature, laser repetition rate, laser fluence, and processing oxygen pressure. The crystallinity and phases were characterized by grazing-incidence X-ray diffraction, and the strain and structural order as a function of depth were evaluated by angle-dependent synchrotron X-ray pair distribution function analysis. To evaluate the potential for interdiffusion, the formation energies of substitutional defects were simulated with density functional theory. Corresponding structural analysis and elemental mapping were performed by scanning/transmission electron microscopy, energy-dispersive X-ray spectroscopy, and electron energy-loss spectroscopy, indicating distinct nanoscale compositional regions with a hierarchical structure embedded in individual VANs columns and minimal interdiffusion across a bilayer film. Proton and oxygen surface exchange coefficients (k H , k O ) and polarization resistances were evaluated by electrical and optical relaxations and impedance spectroscopy of VAN-incorporated protonic ceramic electrochemical cells, respectively, at 400–500 °C, demonstrating values comparable to some of the best-known triple and mixed conductors.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Neutron Radiography and Computed Tomography of Biological Systems at the Oak Ridge National Laboratory's High Flux Isotope Reactor

Neutrons have historically been used for a broad range of biological applications employing techniques such as small-angle neutron scattering, neutron spin echo, diffraction, and inelastic scattering. Unlike neutron scattering techniques that obtain information in reciprocal space, attenuation-based neutron imaging measures a signal in real space that is resolved on the order of tens of micrometers. The principle of neutron imaging follows the Beer-Lambert law and is based on the measurement of the bulk neutron attenuation through a sample. Greater attenuation is exhibited by some light elements (most notably, hydrogen), which are major components of biological samples. Contrast agents such as deuterium, gadolinium, or lithium compounds can be used to enhance contrast in a similar fashion as it is done in medical imaging, including techniques such as optical imaging, magnetic resonance imaging, X-ray, and positron emission tomography. For biological systems, neutron radiography and computed tomography have increasingly been used to investigate the complexity of the underground plant root network, its interaction with soils, and the dynamics of water flux in situ. Moreover, efforts to understand contrast details in animal samples, such as soft tissues and bones, have been explored. This manuscript focuses on the advances in neutron bioimaging such as sample preparation, instrumentation, data acquisition strategy, and data analysis using the High Flux Isotope Reactor CG-1D neutron imaging beamline. The aforementioned capabilities will be illustrated using a selection of examples in plant physiology (herbaceous plant/root/soil system) and biomedical applications (rat femur and mouse lung).

Bilheux, Hassina↗
DOE OSTI2023

Search for High-Pressure Silicon Phases: Reaching the Extreme Conditions with High-Intensity Laser Irradiation

Controlling electronic and optical properties of semiconducting materials could substantially expand their functionality and enable new pathways for the formation of ‘smart’ materials for emerging innovative applications. An emerging new path for the synthesis of exotic silicon (Si) polymorphs is irradiation of bulk diamond-cubic Si by ultrashort laser pulses at relativistic intensity above 1019 W/cm2. Exotic polymorphs are formed due to interaction with MeV-energy electrons generated in laser-produced high-temperature plasma state. The unusual Si structures are found in the form of 5–10 nm nanoparticles confined deep in the bulk of 500-μm-thick Si samples. Raman spectroscopy, electron microscopy and X-ray diffraction studies provide an unequivocal evidence of exotic Si phase formation. A key advantage of such relativistic irradiation lies thereby in the fact that large quantities of such exotic Si is synthesised embedded within the bulk diamond-cubic Si and that further the formed Si polymorphs are stable at ambient temperature and pressure. They are thus available for further studies for electronic applications in selective band gap engineering.

Rapp, Ludovic↗
DOE OSTI2020

Structure and Negative Thermal Expansion in Zr 0.3 Sc 1.7 Mo 2.7 V 0.3 O 12

A 2 M 3 O 12 -based materials have received considerable attention owing to their wide range of negative thermal expansion (NTE) and chemical flexibility toward novel materials design. However, the structure and NTE mechanism remain challenging. In this paper, Zr 4+ and V 5+ are used as a unit to compensatorily replace Sc 3+ and Mo 6+ in Sc 2 Mo 3 O 12 to tune its thermal expansion. Its crystal structure, phase transition, NTE property, and corresponding mechanisms are studied by high-resolution synchrotron X-ray diffraction, powder X-ray diffraction, ultralow-frequency Raman spectroscopy, and density functional theory calculations. The results show that Zr 0.3 Sc 1.7 Mo 2.7 V 0.3 O 12 adopts an orthorhombic (Pbcn) structure at room temperature, with V atoms occupying the position of Mo1 atoms and Zr atoms occupying the position of Sc atoms, and transforms to monoclinic (P2 1 /a) structure at similar to ~133 K (45 K lower than that of Sc 2 Mo 3 O 12 ). It exhibits excellent NTE in a broader range. Most of the phonon modes below 350 cm -1 have negative Grüneisen parameters, of which the lowest and next-lowest frequency (38.5 and 45.8 cm -1 ) optical phonon modes arising from the translational vibrations of the Sc/Zr and Mo/V atoms in the plane of the nonlinear linkage Sc/Zr-O-Mo/V have the largest and next-largest negative Grüneisen parameters and positive total anharmonicity, and contribute most to the NTE.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

X-ray nanodiffraction imaging reveals distinct nanoscopic dynamics of an ultrafast phase transition

Significance Phase transitions, the changes between states of matter with distinct electronic, magnetic, or structural properties, are at the center of condensed matter physics and underlie valuable technologies. First-order phase transitions are intrinsically heterogeneous. When driven by ultrashort excitation, nanoscale phase regions evolve rapidly, which has posed a significant experimental challenge to characterize. The newly developed laser-pumped X-ray nanodiffraction imaging technique reported here has simultaneous 100-ps temporal and 25-nm spatial resolutions. This approach reveals pathways of the nanoscale structural rearrangement upon ultrafast optical excitation, different from those transitions under slowly varying parameters. The spatiotemporally resolved structural characterization provides crucial nanoscopic insights into ultrafast phase transitions and opens opportunities for controlling nanoscale phases on ultrafast time scales.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Boride-based Ceramic Super-high Temperature Thermocouples in Harsh Environments (Final Scientific/Technical Report)

An electromotive force (emf) can be generated along a temperature gradient between the cold end and hot end of a thermoelectric material, termed the Seebeck effect. Based on the Seebeck effect, metallic alloys have been extensively employed to detect temperatures for centuries, named thermocouples. However, commercially available thermocouple alloys suffer from limitations, such as oxidation, chemical degradation, and poor long-term stability under high-temperature harsh environments. This DOE-funded project aimed to develop high-temperature, chemically tolerant thermocouples suitable for operation in extreme environments relevant to semiconducting thermoelectric materials. The research focused on boride-based semiconducting thermoelectric compounds as candidates for next-generation thermocouples with enhanced oxidation resistance, chemical stability, and thermal robustness under conditions representative of charcoal-fired electricity facilities. During the funded years, boride materials were synthesized using an arc-plasma technique under ambient air and argon atmospheres, enabling scalable and cost-effective production compared with conventional boride fabrication methods. The synthesized borides were processed into nanostructured powders, followed by consolidation into dense bulk materials using a spark plasma sintering (SPS) bottom-up approach. Comprehensive characterization was performed, including microstructural analysis, electrical transport measurements, and optical and thermal property evaluation. Both p-type and n-type boride electric legs were fabricated and integrated into boride-based thermocouples. The thermal and irradiation stabilities of the boride nanomaterials and bulk thermoelectric materials were systematically evaluated to assess suitability for long-term operation in harsh environments. Additionally, 12 students were broadly hands-on trained spanning the full research workflow, including word processing and technical editing (e.g., LATEX for manuscript and poster preparation), data collection and analysis (using Python and related libraries and hardware interfaces), sample preparation (including arc-plasma synthesis and spark plasma sintering), and advanced characterization techniques (such as X-ray diffraction, UV–vis spectroscopy, electron microscopy, differential thermal analysis (DTA), and Seebeck coefficient measurements, etc). Overall, this project demonstrated the feasibility of boride-based thermoelectric materials as durable high-temperature thermocouples, providing a promising pathway toward robust temperature sensing technologies aligned with DOE energy infrastructure and extreme-environment monitoring needs.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2022

Unexpected features in the optical vibrational spectra of δ-UO 3

Uranium trioxide displays a complex chemical phase space, with at least six structurally distinct polymorphs accessible via different synthetic routes. Remarkably, despite its technological importance, full structural and electronic characterization of these polymorphs remains an open area of study. δ-UO 3 in particular has attracted significant theoretical attention due to its high point group and space group symmetries, having U (VI) in octahedral coordination with polyhedra interconnected through corner-sharing to build a 3-D cubic lattice with space group symmetry Pm-3m and Z = 1. Critical experimental information, such as its optical vibrational spectra, are not known. Here, we study the Raman and infrared (IR) spectra of δ-UO 3 together with the support of density functional theory (DFT) calculations for spectral interpretation. A symmetry analysis of the DFT-predicted phonon eigenmodes indicates that δ-UO 3 should have two IR active modes and no Raman active modes. Experimental results, however, indicate significant Raman scattering from δ-UO 3 . We therefore propose four potential explanations for this apparent contradiction: a possible tetragonal distortion to the cubic cell, the existence of a surface impurity layer, vacancy scattering, and structural activation of Raman signal. We use powder X-ray diffraction and confocal Raman spectroscopy with depth profiling to investigate these possibilities and suggest future experiments to explore this phenomenon in more detail. Understanding the lattice dynamics of δ-UO 3 is important for identification of technogenic U phases via Raman and infrared spectroscopy and our results indicate that the simple understanding of δ-UO 3 as a high-symmetry cubic structure should be reconsidered.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2025

Laser-driven ultrafast transmission electron microscopy

Recent advances in lasers and electron optics technology have allowed transmission electron microscopes to achieve high spatial and temporal resolution, making them capable of tracking atoms, charges and spin motions down to the attosecond and nanometre scales. This Primer discusses the most common and practical experimental implementation of time-resolved transmission electron microscopy and the stroboscopic mode for evaluating ultrafast reversible dynamics. An in-depth discussion of photo-induced near-field electron microscopy, a technique unique to laser-assisted electron microscopy, is also provided, covering its prospective applications in the study of coherent phenomena in quantum materials. The experimental strategies and limitations in investigating the structural dynamics of materials and nanostructures by imaging, diffraction and spectroscopy are also described in detail, with a direct comparison with more conventional and established techniques. Here, we provide key information for new researchers who intend to use ultrafast transmission electron microscopy to address new challenges in specific materials science, condensed matter and nanophotonics.

Transmission electron microscopy↗
DOE OSTI2020

Equation of State of TiN at High Pressures and Temperatures: A Possible Host for Nitrogen in Planetary Mantles

Nitrogen, the most abundant element in Earth's atmosphere, is also a primary component of solid nitride minerals found in meteorites and on Earth's surface. If they remain stable to high pressures and temperatures, these nitrides may also be important reservoirs of nitrogen in planetary interiors. We used synchrotron X-ray diffraction to measure the thermal equation of state and phase stability of titanium nitride (TiN) in a laser-heated diamond anvil cell at pressures up to ~70 GPa and temperatures up to ~2500 K. TiN maintains the cubic B1 (NaCl-type) crystal structure over the entire pressure and temperature range explored. It has K 0 = 274(4) GPa, K 0 ' = 3.9(2), and γ 0 = 1.39(4) for a fixed V 0 = 76.516(30) Å 3 (based on experimental measurements), q = 1, and θ 0 = 579 K. Additionally, we collected Raman spectra of TiN up to ~60 GPa, where we find that the transverse acoustic (TA), longitudinal acoustic (LA), and transverse optical (TO) phonon modes exhibit mode Grüneisen parameters of 1.66(17), 0.54(15), and 0.93(4), respectively. Based on our equation of state, TiN has a density of ~5.6–6.4 g/cm 3 at Earth's lower mantle conditions, significantly more dense than both the mantle of the Earth and the estimated densities of the mantles of other terrestrial planets, but less dense than planetary cores. Furthermore, we find that TiN remains stable against physical decomposition at the pressures and temperatures found within Earth's mantle, making it a plausible reservoir for deep planetary nitrogen if chemical conditions allow its formation.

58 GEOSCIENCES↗
DOE OSTI2025

Long-lived photoinduced polar states in metal halide perovskites

Ferroic polarization in hybrid perovskites is crucial for enhancing photovoltaic performance and developing potential electronic applications. Controlling ferroic polarization with an optical field enables probing of ferroic polarization without the unwanted interface ionic effects caused by electronic contacts. This study employs ultrafast near-infrared photoexcitation to control dynamic structural transitions in soft single crystalline hybrid Cu (II) halide perovskites, achieving a long-lived polar state (beyond 104 s) at room temperature. We probe reversible long-lived polar domains under near-infrared photoexcitation using in-situ second harmonic generation microscopy. Theoretical calculation informs the polar lattice microstrain likely induced by anisotropic structure deformation in octahedral copper halide under near-infrared photoexcitation. The reversible slow structure deformation is further confirmed by in-situ photo-induced X-ray diffraction measurement. This work provides a material platform for understanding, controlling, and probing polarization under photoexcitation. Our methodology enables the identification of previously undiscovered polar phases in ferroelectric halide perovskites.

Dou, Yixuan↗
DOE OSTI2025

Chirality in the Kagome Metal CsV 3 ⁢Sb 5

Using x-ray photoelectron diffraction (XPD) and angle-resolved photoemission spectroscopy, we study photoemission intensity changes related to changes in the geometric and electronic structure in the kagome metal CsV 3 ⁢Sb 5 upon transition to an unconventional charge density wave (CDW) state. The XPD patterns reveal the presence of a chiral atomic structure in the CDW phase. Furthermore, using circularly polarized x-rays, we have found a pronounced nontrivial circular dichroism in the angular distribution of the valence band photoemission in the CDW phase, indicating a chirality of the electronic structure. This observation is consistent with the proposed orbital loop current order. In view of a negligible spontaneous Kerr signal in recent magneto-optical studies, the results suggest an antiferromagnetic coupling of the orbital magnetic moments along the 𝑐 axis. Here, while the inherent structural chirality may also induce circular dichroism, the observed asymmetry values seem to be too large in the case of the weak structural distortions caused by the CDW.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2021

Local Structural Disorder in Metavanadates MV 2 O 6 (M = Zn and Cu) Synthesized by the Deep Eutectic Solvent Route: Photoactive Oxides with Oxygen Vacancies

Metavanadates MV 2 O 6–δ (M = Zn and Cu) are synthesized by using a deep eutectic solvent (DES), a mixture of hydrogen bond donor and acceptor, as a reaction medium. Dissolution of stable binary metal oxides in a DES followed by a heat treatment yields phase-pure vanadates. According to in situ powder X-ray diffraction, ternary phases (α-Zn 2 V 2 O 7 and β-Cu 2–x V 2 O 7 , x ~ 0.27) are intermediates in the reaction pathway taken. Identifying a polymorphic phase transformation temperature for CuV 2 O 6 as well as the narrow temperature range between formation and decomposition for both metavanadates allows for tackling the challenge of the synthesis of these materials. The oxygen vacancy introduced by the DES route is accompanied by the formation of reduced V 4+ and Cu + in the oxide matrix, based on X-ray photoelectron spectroscopy. These oxygen vacancies modify the vibrational modes in the corresponding Raman spectra and are also responsible for broad optical absorptions in the 1.8–1.1 eV range. The optical band gaps of the materials are found at 1.8 eV (CuV 2 O 6 ) and 2.2 eV (ZnV 2 O 6 ), approximately 0.1–0.3 eV below the values reported in the literature. The reduced band gaps and sub-band gap photon absorption are key features of the oxygen-deficient metavanadates. Surface photovoltage spectroscopy reveals that all the synthesized vanadates are n-type materials with electrons as the majority charge carriers, and photoelectrochemical measurements confirm photoanodic currents for methanol oxidation. Furthermore, these results provide insight into the synthesis and structure–property relationship of the metavanadates for their potential use as photoanodes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗