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At least 1,513 records · Page 84
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Visualizing Light-Induced Microstrain and Phase Transition in Lead-Free Perovskites Using Time-Resolved X-Ray Diffraction

Metal halide perovskites have emerged as promising materials for optoelectronic applications in the last decade. A large amount of effort has been made to investigate the interplay between the crystalline lattice and photoexcited charge carriers as it is vital to their optoelectronic performance. Among them, ultrafast laser spectroscopy has been intensively utilized to explore the charge carrier dynamics of perovskites, from which the local structural information can only be extracted indirectly. Here, we have applied a time-resolved X-ray diffraction technique to investigate the structural dynamics of prototypical two-dimensional lead-free halide perovskite Cs 3 Bi 2 Br 9 nanoparticles across temporal scales from 80 ps to microseconds. We observed a quick recoverable (a few ns) photoinduced microstrain up to 0.15% and a long existing lattice expansion (~a few hundred nanoseconds) at mild laser fluence. Once the laser flux exceeds 1.4 mJ/cm 2 , the microstrain saturates and the crystalline phase partially transfers into a disordered phase. This photoinduced transient structural change can recover within the nanosecond time scale. Furthermore, these results indicate that photoexcitation of charge carriers couples with lattice distortion, which fundamentally affects the dielectric environment and charge carrier transport.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Redox-Induced Microstructure and Phase Dynamics in Nickel: Insights from In Situ Synchrotron X-ray Diffraction

Using in situ synchrotron X-ray diffraction, we interrogate the microstructural and phase evolution of polycrystalline nickel (Ni) during redox cycling in O 2 , H 2 , and H 2 O environments. Oxidation in O 2 promotes strong (111) texturing in both the NiO overlayer and the underlying Ni substrate. However, this crystallographic alignment is lost following reduction in H 2 and subsequent reoxidation, demonstrating irreversible microstructural changes. H 2 exposure leads to proton dissolution into the Ni lattice, triggering a localized phase transition from face-centered cubic (FCC) to hexagonal close-packed (HCP) Ni in hydrogen-saturated regions. In H 2 O-containing atmospheres, dissociative H 2 O adsorption produces protons that permeate the NiO layer, forming γ-NiOOH within the NiO lattice and HCP Ni beneath the NiO overlayer as protons accumulate. Kinetic analysis via the Johnson-Mehl-Avrami–Kolmogorov model uncovers distinct growth mechanisms: preoxidized Ni surfaces follow one-dimensional (1D) kinetics for NiO, γ-NiOOH, and HCP growth, whereas pristine Ni exhibits three-dimensional (3D) kinetics due to island-like nucleation and growth of NiO. Furthermore, these results highlight the critical interplay between H 2 O dissociation, hydrogen permeation, and redox-driven phase transformations, with practical implications in engineering nickel-based catalysts and hydrogen storage systems through controlled microstructural and phase evolution.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Fast and interpretable classification of small X-ray diffraction datasets using data augmentation and deep neural networks

X-ray diffraction (XRD) data acquisition and analysis is among the most time-consuming steps in the development cycle of novel thin-film materials. We propose a machine-learning-enabled approach to predict crystallographic dimensionality and space group from a limited number of thin-film XRD patterns. We overcome the scarce-data problem intrinsic to novel materials development by coupling a supervised machine learning approach with a model-agnostic, physics-informed data augmentation strategy using simulated data from the Inorganic Crystal Structure Database (ICSD) and experimental data. As a test case, 115 thin-film metal-halides spanning 3 dimensionalities and 7 space-groups are synthesized and classified. After testing various algorithms, we develop and implement an all convolutional neural network, with cross-validated accuracies for dimensionality and space-group classification of 93% and 89%, respectively. We propose average class activation maps, computed from a global average pooling layer, to allow high model interpretability by human experimentalists, elucidating the root-causes of misclassification. Finally, we systematically evaluate the maximum XRD pattern step size (data acquisition rate) before loss of predictive accuracy occurs, and determine it to be 0.16° 2θ, which enables an XRD pattern to be obtained and classified in 5.5 minutes or less.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Dehydration kinetics of nanoconfined water in beryl probed by high temperature single crystal synchrotron X-ray diffraction

Understanding changes in material properties through external stimuli plays a key role in validating the expected performance of materials and engineering material properties in a controlled manner. Here, we introduce a fundamental protocol to deduce dehydration reactions kinetics of water confined in nanopore channels, with the cyclosilicate beryl as the scaffold of interest, using time-resolved synchrotron X-ray diffraction (SXRD), in the temperature interval of 298–1038 K. The temperature-dependent intensity (I) of the strongest reflection (112) was used as the crystallite variable. An estimation of an isobaric thermal crystallite coefficient, k, analogous with the isobaric thermal expansion coefficient, established the rate of relative crystallization as a function of temperature, $\frac{∂I}{∂T}$. A plot of lnk and $\frac{1}{T}$ gives rise to two kinetic steps, indicating a slow dehydration stage up to ~ 700 K and a fast dehydration stage up to the investigated temperature 1038 K. The crystal structure of beryl determined up to 1038 K, in temperature increment as small as 10 K, indicates the presence of channel ions Na and Fe and a gradual decrease of water upon heating.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

X-ray diffraction of metastable structures from supercooled liquid hydrogen

We report time resolved observations of the crystallization from liquid hydrogen, supercooled to temperatures below the melting point, using 11.2 keV X-ray diffraction from the Linac Coherent Light Source (LCLS). Changes to the metastable solid and liquid structure factors have been dynamically measured. This allows for a direct determination of the lowest energy crystal polymorphs, the stacking probabilities, as well as the liquid and solid densities and temperatures. Such measurements provide experimental evidence of an Arrhenius-like growth kinetics along the stacking direction during supercooling.

36 MATERIALS SCIENCE↗
DOE OSTI2022

In situ analysis of the nucleation of O- and Zn-polar ZnO nanowires using synchrotron-based X-ray diffraction

The selection of the polarity of ZnO nanowires grown by chemical bath deposition offers a great advantage for their integration into a wide variety of engineering devices. However, the nucleation process of ZnO nanowires and its dependence on their polarity is still unknown despite its importance for optimizing their morphology and properties and thus to enhance the related device performances. To tackle this major issue, we combine an in situ analysis of the nucleation process of O- and Zn-polar ZnO nanowires on O- and Zn-polar ZnO single crystals, respectively, using synchrotron radiation-based grazing incidence X-ray diffraction with ex situ transmission and scanning electron microscopy. We show that the formation of ZnO nanowires obeys three successive phases from the induction, through nucleation to growth phases. Additionally, the characteristics of each phase, including the nucleation temperature, the shape and dimension of nuclei, as well as their radial and axial development are found to depend on the polarity of ZnO nanowires. A comprehensive description reporting the dominant physicochemical processes in each phase and their dependence on the polarity of ZnO nanowires is presented, revisiting their formation process step-by-step. These findings provide a deeper understanding of the phenomena at work during the growth of ZnO nanowires by chemical bath deposition and open the perspective to develop a more accurate control of their properties at each step of the formation process.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

Photo-induced structural dynamics of o -nitrophenol by ultrafast electron diffraction

The photo-induced dynamics of o-nitrophenol, particularly its photolysis, has garnered significant scientific interest as a potential source of nitrous acid in the atmosphere. Although the photolysis products and preceding photo-induced electronic structure dynamics have been investigated extensively, the nuclear dynamics accompanying the non-radiative relaxation of o-nitrophenol on the ultrafast timescale, which include an intramolecular proton transfer step, have not been experimentally resolved. Herein, we present a direct observation of the ultrafast nuclear motions mediating photo-relaxation using ultrafast electron diffraction. Here, this work spatiotemporally resolves the loss of planarity which enables access to a conical intersection between the first excited state and the ground state after the proton transfer step, on the femtosecond timescale and with sub-Angstrom resolution. Our observations, supported by ab initio multiple spawning simulations, provide new insights into the proton transfer mediated relaxation mechanism in o-nitrophenol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

In-situ energy dispersive x-ray diffraction study of the growth of CuO nanowires by annealing method

The in-situ growth of CuO nanowires was studied by Energy Dispersive X-ray Diffraction (EDXRD) to observe the mechanism of growth. The study was carried out for comparison at two temperatures—at 500 °C, the optimum temperature of the nanowires growth, and at 300 °C just below the temperature range of the growth. The in situ observation revealed the successive oxidation of Cu foil to Cu{sub 2}O layer and finally to CuO layer. Further analysis showed the presence of a compressive stress in CuO layer due to interface at CuO and Cu{sub 2}O layers. The compressive stress was found to increase with the growth of the nanowires at 500 °C while it relaxed with the growth of CuO layer at 300 °C. The present results do not support the existing model of stress relaxation induced growth of nanowires. Based on the detailed Transmission Electron Microscope, Scanning Electron Microscope, and EDXRD results, a microstructure based growth model has been suggested.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Determination of transient atomic structure of laser-excited materials from time-resolved diffraction data

The time evolution of the Bragg peaks of photo-excited gold nanofilms is measured using transmission ultrafast electron diffraction (UED) with 3.0 MeV electron pulses and the corresponding structure evolution is calculated using two-temperature molecular dynamics (2T-MD). The good agreement obtained between the measured and calculated Bragg peaks, over the full experimental timescale, enables the lattice temperature effects and the structural changes to be disentangled for the first time. The agreement demonstrates that 2T-MD is a reliable method for solving the inverse problem of structure determination of laser irradiated metals in UED measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2013

In-situ x-ray diffraction study of the growth of highly strained epitaxial BaTiO{sub 3} thin films

In-situ synchrotron x-ray diffraction was performed during the growth of BaTiO{sub 3} thin films on SrTiO{sub 3} substrates using both off-axis RF magnetron sputtering and pulsed laser deposition techniques. It was found that the films were ferroelectric during the growth process, and the presence or absence of a bottom SrRuO{sub 3} electrode played an important role in the growth of the films. Pulsed laser deposited films on SrRuO{sub 3} displayed an anomalously high tetragonality and unit volume, which may be connected to the previously predicted negative pressure phase of BaTiO{sub 3}.

36 MATERIALS SCIENCE↗
DOE OSTI2013

In-situ stress analysis with X-Ray diffraction for yield locus characterization of sheet metals

A main problem in the field of sheet metal characterization is the inhomogeneous plastic deformation in the gauge regions of specimens which causes the analytically calculated stresses to differ from the sought state of stress acting in the middle of the gauge region. To overcome this problem, application of X-Ray diffraction is analyzed. For that purpose a mobile X-ray diffractometer and an optical strain measurement system are mounted on a universal tensile testing machine. This enables the recording of the whole strain and stress history of a material point. The method is applied to uniaxial tension tests, plane strain tension tests and shear tests to characterize the interstitial free steel alloy DC06. The applicability of the concepts of stress factors is verified by uniaxial tension tests. The experimentally obtained values are compared with the theoretical values calculated with crystal elasticity models utilizing the orientation distribution functions (ODF). The relaxation problem is addressed which shows itself as drops in the stress values with the strain kept at a constant level. This drop is analyzed with elasto-viscoplastic material models to correct the measured stresses. Results show that the XRD is applicable to measure the stresses in sheet metals with preferred orientation. The obtained yield locus is expressed with the Yld2000–2D material model and an industry oriented workpiece is analyzed numerically. The comparison of the strain distribution on the workpiece verifies the identified material parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Neutron diffraction study of MnNiGa{sub 2}—Structural and magnetic behaviour

MnNiGa{sub 2} crystallizes in the L21 (Heusler) structure and has a ferromagnetic ordering temperature T{sub C} ∼ 192 K. Rietveld refinement of the neutron diffraction patterns indicates that the Ga atoms occupy the equivalent 8c position, while Mn and Ni share the 4a (0, 0, 0) and 4b (0.5, 0.5, 0.5) sites with a mixed occupancy of Mn and Ni atoms. It is found that that ∼83% of Mn and ∼17% Ni are located at the 4a site while ∼83% of Ni and ∼17% Mn occupy the 4b site. There is no evidence of a magneto-volume effect around T{sub C}. In agreement with this finding, our detailed critical exponent analyses of isothermal magnetization curves and the related Arrott plots confirm that the magnetic phase transition at T{sub C} is second order.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Thermoelastic study of nanolayered structures using time-resolved X-ray diffraction at high repetition rate

We investigate the thermoelastic response of a nanolayered sample composed of a metallic SrRuO{sub 3} electrode sandwiched between a ferroelectric Pb(Zr{sub 0.2}Ti{sub 0.8})O{sub 3} film with negative thermal expansion and a SrTiO{sub 3} substrate. SrRuO{sub 3} is rapidly heated by fs-laser pulses with 208 kHz repetition rate. Diffraction of X-ray pulses derived from a synchrotron measures the transient out-of-plane lattice constant c of all three materials simultaneously from 120 ps to 5 μs with a relative accuracy up to Δc/c = 10{sup −6}. The in-plane propagation of sound is essential for understanding the delayed out-of-plane compression of Pb(Zr{sub 0.2}Ti{sub 0.8})O{sub 3}.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Study of microstress state of P91 steel using complementary mechanical Barkhausen, magnetoacoustic emission, and X-ray diffraction techniques

The paper deals with assessment of microstress state of martensite P91 steel using three complementary techniques: mechanical Barkhausen emission, magnetoacoustic emission (MAE), and X-ray diffraction (XRD) profile analysis. Magnetic coercivity Hc and microstructure were investigated with inductive magnetometry and magnetic force microscopy (MFM), respectively. Internal stress level of P91 steel was modified by heat treatment. Steel samples were austenitized, quenched, and then tempered at three temperatures (720 °C, 750 °C, and 780 °C) during increasing time (from 15 min up to 240 min). The microstrain level ε{sub i} was evaluated using Williamson–Hall method. It was revealed that during tempering microstrain systematically decreases from ε{sub i} = 2.5 × 10{sup −3} for as quenched state down to ε{sub i} = 0.3 × 10{sup −3} for well tempered samples. Both mechanical hardness (Vicker's HV) and magnetic hardness (coercivity) decrease almost linearly with decreasing microstrain while the MAE and MBE intensities strongly increase. Tempering leads to evident shift of the MeBN intensity maximum recorded for the first load towards lower applied strain values and to increase of MAE intensity. This indicates that the microstress state deduced by magnetic techniques is correlated with microstrains evaluated with XRD technique.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Strength and equation of state of NaCl from radial x-ray diffraction

The strength and equation of state of NaCl were determined under nonhydrostatic compression up to 27 GPa using an energy-dispersive radial x-ray diffraction technique in a diamond-anvil cell using the lattice strain theory. Together with estimation of the high-pressure shear modulus, it is suggested that NaCl could support a maximum differential stress of 0.980 GPa at 22.6 GPa under uniaxial compression. The differential stress rapidly drops at 27.2 GPa due to the phase transition from B1 phase to B2 phase for NaCl. The hydrostatic compression data of B1 phase yield a bulk modulus K{sub 0} = 25.6(8) GPa and its pressure derivative K{sub 0}′ = 5.16(20) using Pt pressure scale. In addition, a comparative study of the observed pressures from Pt scale and ruby-fluorescence scale shows that the ruby-fluorescence pressures may reflect the lower stress state under nonhydrostatic compression compared with hydrostatic compression.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Photometric study of single-shot energy-dispersive x-ray diffraction at a laser plasma facility

The low repetition rates and possible shot-to-shot variations in laser-plasma studies place a high value on single-shot diagnostics. For example, white-beam scattering methods based on broadband backlighter x-ray sources are used to determine changes in the structure of laser-shocked crystalline materials by the evolution of coincidences of reciprocal lattice vectors and kinematically allowed momentum transfers. Here, we demonstrate that white-beam techniques can be extended to strongly disordered dense plasma and warm dense matter systems where reciprocal space is only weakly structured and spectroscopic detection is consequently needed to determine the static structure factor and thus, the ion-ion radial distribution function. Specifically, we report a photometric study of energy-dispersive x-ray diffraction (ED-XRD) for structural measurement of high energy density systems at large-scale laser facilities such as OMEGA and the National Ignition Facility. We find that structural information can be obtained in single-shot ED-XRD experiments using established backlighter and spectrometer technologies.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2014

High-pressure x-ray diffraction study of YBO{sub 3}/Eu{sup 3+}, GdBO{sub 3}, and EuBO{sub 3}: Pressure-induced amorphization in GdBO{sub 3}

Angle-dispersive synchrotron X-ray diffraction measurements were performed on vaterite-type YBO{sub 3}/Eu{sup 3+}, GdBO{sub 3}, and EuBO{sub 3}, respectively, up to 41 GPa at room temperature using a diamond-anvil cell. Pressure-induced amorphization was observed in hexagonal GdBO{sub 3} with a significant compression along the c-axis. Compared to the ions of the distorted GdBO{sub 3} phase, its anions may lose their long-range order prior to the cations at high pressures. Based on the experimental pressure-volume data, the obtained bulk moduli of YBO{sub 3}/Eu{sup 3+} and GdBO{sub 3} are 329 and 321 GPa, respectively, which are more than 90% larger than that of EuBO{sub 3} (167 GPa) and are presumably attributed to Gd{sup 3+} and Y{sup 3+} with a high density of d valence electrons.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Neutron diffraction study of the magnetic-field-induced transition in Mn{sub 3}GaC

The antiperovskite Mn{sub 3}GaC undergoes an isostructural cubic–cubic first order transition from a low-temperature, large-cell-volume antiferromagnetic state to a high-temperature, small-cell-volume ferromagnetic state at around 160 K. The transition can also be induced by applying a magnetic field. We study here the isothermal magnetic-field-evolution of the transition as ferromagnetism is stabilized at the expense of antiferromagnetism. We make use of the presence of the two distinct cell volumes of the two magnetic states as a probe to observe by neutron diffraction the evolution of the transition, as the external magnetic field carries the system from the antiferromagnetic to the ferromagnetic state. We show that the large-volume antiferromagnetic and the small-volume ferromagnetic states coexist in the temperature range of the transition. The ferromagnetic state is progressively stabilized as the field increases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗