Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “in situ diffraction”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Unsupervised Segmentation and Clustering Workflow for Efficient Processing of 4D-STEM and 5D-STEM Data

Four-dimensional scanning transmission electron microscopy (4D-STEM) enables mapping of diffraction information with nanometer-scale spatial resolution, offering detailed insight into local structure, orientation, and strain. However, as data dimensionality and sampling density increase, particularly for in situ scanning diffraction experiments (5D-STEM), robust segmentation of structurally consistent behavior across sequential measurements becomes essential for efficient and physically meaningful analysis. Here, we introduce a clustering framework that identifies crystallographically distinct domains from 4D-STEM datasets. By using local diffraction-pattern similarity as a metric, the method extracts closed contours delineating spatially contiguous regions. This approach produces cluster-averaged diffraction patterns that improve signal quality while reducing data volume by orders of magnitude, enabling rapid and accurate orientation, phase, and strain mapping. We demonstrate the applicability of this approach to in situ liquid-cell 4D-STEM data of gold nanoparticle growth. Our method provides a scalable and generalizable route for spatially coherent segmentation, data compression, and quantitative structure–strain mapping across diverse 4D-STEM modalities. The full analysis code and example workflows are publicly available to support reproducibility and reuse.

4D-STEM↗
DOE OSTI2026

Coupled Chemical and Mechanical Control of Phase Stability in Lanthanide-Substituted BiVO 4

Doping is widely used to enhance the photoelectrochemical performance of BiVO 4 , yet solubility limits and polymorphic stability constrain compositional tuning. Here, in this study, the role of trivalent cation substitution (Ln = La, Nd, Dy, Ho, Y) on pressure-induced phase transformations in Bi 1–x Ln x VO 4 (x ≤ 0.5) is described. Powder X-ray and neutron diffraction reveal that increasing Ln content stabilizes the tetragonal zircon-type polymorph under ambient conditions, while applied pressures of up to ∼5 GPa promote conversion to the monoclinic fergusonite-type polymorph. In-situ neutron diffraction on Bi 0.8 La 0.2 VO 4 shows a reversible monoclinic to tetragonal transition near 2–3 GPa with a bulk modulus of 147 GPa. The extent of conversion depends strongly on dopant identity, concentration, and synthetic route, with mixed-phase solid-state samples converting more efficiently than phase-pure coprecipitated materials. These results demonstrate pressure as a viable pathway to access metastable, doped BiVO 4 compositions beyond conventional solubility limits.

Sypkes, Kathryn I. [University of Sydney, NSW (Aus↗
DOE OSTI2025

Evolution of dislocations during the rapid solidification in additive manufacturing

Materials processed by fusion-based additive manufacturing (AM) typically exhibit relatively high dislocation densities, along with cellular structures and elemental segregation. This representative structural feature significantly influences material performance; however, post-mortem microstructure characterizations of AM materials cannot capture the dynamic evolution of dislocations during the manufacturing process, thereby offering limited mechanism-based guidance for further advancing AM techniques and facilitating the qualification and certification of AM products. In this study, we conduct operando high-energy synchrotron X-ray diffraction experiments on wire-laser directed energy deposition of 316 L stainless steel. Through a unique configuration, our operando synchrotron experiments semi-quantitatively probe the dislocation density in solid phases and their dynamic changes during solidification and subsequent cooling. By integrating this advanced synchrotron technique with multi-physics simulation, in-situ neutron diffraction, and multi-scale electron microscopy characterization, our mechanistic study aims to elucidate the effects of rapid cooling and subsequent thermal cycling on the dislocation generation and evolution.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In Situ Cyclized Polyacrylonitrile Coating: Key to Stabilizing Porous High-Entropy Oxide Anodes for High-Performance Lithium-Ion Batteries

High-entropy oxides (HEOs) composed of multiple metal elements have attracted great attention as anode materials for lithium-ion batteries (LIBs) due to the synergistic effects of various metal species. However, the practical applications of HEOs are still plagued by poor conductivity, unstable solid electrolyte interphase (SEI) and poor cycling stability. In this work, nanosized (FeCoNiCrMn) 3 O 4 HEO (NHEO) is prepared successfully by the NaCl-assisted mechanical ball-milling strategy. Novelly, polyacrylonitrile (PAN) is used as the binder and then in situ thermochemically cyclized to construct a cyclized PAN (cPAN) outer layer onto NHEO (NHEO-cPAN). The in situ formed cPAN coating not only improves the electrical conductivity, but also reinforces the structural and interfacial stability, and thereby, the resulted NHEO-cPAN electrode exhibits significantly enhanced rate and cyclic performance. Specifically, NHEO-PAN500 electrode delivers a high reversible capacity of 560 mAh g –1 at 5 A g –1 and a high-capacity retention of 83% over 800 cycles at 3 A g –1 . Furthermore, the structural evolution and electrochemical behavior of NHEO-PAN electrode during discharge/charge is systematically investigated by operando X-ray diffraction, in situ impedance spectroscopy and ex situ high-resolution transmission electron microscopy. Therefore, this work provides new insights into the engineering of electrode and interphase for high-performance HEO electrode materials, potentially enlightening the practical applications of HEO-based LIBs.

25 ENERGY STORAGE↗
DOE OSTI2025

Bridging Experiment and Theory to Reveal Compounds in K–Zn(Cd)–Bi Systems

This study investigates the facile hydride synthesis method guided by theoretical predictions to explore the K–T–Bi (T = Zn, Cd) phase spaces. Using an adaptive genetic algorithm (AGA) and density functional theory (DFT), candidate compositions are identified for experimental validation via a facile hydrides route, permitting experimental screening of K–Zn–Bi and “empty” K–Cd–Bi systems. The previously reported KZnBi and KZn 2 Bi 2 are synthesized alongside newly discovered KCdBi and KCd 2 Bi 2 . While the AGA and DFT predict the stability of these compounds, structural predictions align with the experiment only for KZnBi and KZn 2 Bi 2 . Single-crystal X-ray structure refinements confirm that KZnBi and KZn 2 Bi 2 adopt the hexagonal ZrBeSi- and tetragonal ThCr 2 Si 2 -structure types, respectively. KCdBi has tetragonal PbClF-structure type and KCd 2 Bi 2 belongs to the ThCr 2 Si 2 -structure type. A trend based on the ratio of the metal ionic radii allows to rationalize variation in the structure types within the ATBi family (A = Li–Cs), correctly identifying KCdBi as isostructural to NaZnBi. Thermal stability studied by high-temperature powder X-ray diffraction reveals that Zn-containing compounds melt at higher temperatures (821 K for KZn 2 Bi 2 ) than Cd-containing KCd 2 Bi 2 (635 K). This study highlights the efficacy of combining rapid synthesis techniques with predictive modeling, though structural predictions show some limitations in accuracy.

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

Influence of stacking fault energy and hydrogen on deformation mechanisms in high Mn austenitic steels during in-situ tensile testing

High Mn austenitic steels are considered an economical alloy system for hydrogen storage and transport applications. This study used stacking fault energy (SFE) as a design parameter to achieve hydrogen embrittlement (HE)-resistant high Mn austenitic alloys. The role of hydrogen on the deformation mechanisms of low (29 mJ/m 2 ) and high SFE (49 mJ/m 2 ) alloys was evaluated through in-situ neutron diffraction during tensile loading. Hydrogen-precharging increased yield strength, partly due to hydrogen-induced lattice distortion (i.e., solute strengthening). Hydrogen accelerated the increase in defect density, including dislocations and stacking faults. The formation of planar deformation structures (twins and stacking faults), relative to dislocations, plays a critical role in promoting hydrogen-assisted fracture. The stacking fault frequency parameter obtained from neutron diffraction quantifies planar deformation tendencies, correlated with HE sensitivity. The higher SFE alloy exhibited greater resistance to HE, associated with the reduced propensity to form stacking faults and twins upon deformation in the hydrogen-precharged condition.

High Mn austenitic steel↗
DOE OSTI2025

Synthesis and post-heating treatment of inorganic NaF·Na 3 SbS 4 solid electrolytes

Sulfide-type sodium (Na) solid electrolytes (SEs) with halide doping have attracted serious interest due to their high ionic conductivity and great potential in solid-state Na batteries. While other halogens such as Cl, Br, I have been studied to enhance Na-ion transport in sulfide-type SEs, the introduction of fluorine (F) is rarely investigated. Moreover, synthetic parameters such as heating treatment temperatures strongly influence the structure and conductive properties of halide-doped sulfide SEs. Herein, we prepared xNaF·(1-x)Na 3 SbS 4 nanocomposites with varying concentration of F using a low-temperature (150 °C) heating method, and studied the effects of post-heating treatment on structure and conductivity. In-situ neutron diffraction was employed to investigate the structural evolution of X-doped Na 3 SbS 4 (X = F, Cl) during the post-heating treatment and cooling process. In addition, the post-heating treatment at 300 °C leads to increased ionic conductivity of xNaF·(1-x)Na 3 SbS 4 nanocomposites with various F contents. After 300 °C post-heating treatment, 0.2NaF·0.8Na 3 SbS 4 exhibited the highest conductivity of 0.48 mS cm –1 at room temperature. Moreover, improved electrochemical stability was also observed in Na-Sn symmetric cells, specially, with prolonged stable cycling for 300 h and much lower polarization voltage (<0.35 V). Furthermore, this work highlights the importance of post-heating treatment on the structural evolution and its role in exploring new halide-incorporated sulfide-type SEs, promoting the development of inorganic solid-state ionic conductors.

25 ENERGY STORAGE↗
DOE OSTI2026

High-temperature mechanical properties of a γ′-strengthened Co-based superalloy designed for additive manufacturing

GammaPrint®-700 is a recently developed high γ′ (∼70% volume fraction) CoNi-based superalloy designed to combine high-temperature mechanical performance with laser powder bed fusion processability. Room-temperature yield strength ranged from 610 to 658 MPa and increased to 661 MPa (longitudinal) and 730 MPa (transverse) at 760 °C. The creep behavior compared favorably to high-γ′ Ni-based superalloys manufactured via laser powder bed fusion such as Incoloy® 939 and Inconel® 738LC. In-situ neutron diffraction data measured during creep revealed that plastic deformation was largely localized to the γ phase at 760 °C, allowing the γ’ phase to elastically compensate and maintain creep strain resistance. Furthermore, at 900 °C, this load sharing behavior was weakened, contributing to accelerated creep rate and rupture.

Creep↗
DOE OSTI2025

Evaporation of a Reactive Nanofluid Sessile Drop: Capturing Rapid Emergence of Surface Crystals with In Situ Synchrotron X-ray Diffraction

Mechanisms for surface pattern formation from evaporation of a reactive nanofluid sessile drop are not well understood. In contrast to the coffee-ring effect from inert particles, rapid chemical and morphological transformation of reactive nanoparticles upon rapid evaporative drying are challenging to probe experimentally. Here, using grazing-incidence X-ray surface scattering, the nanostructure of nascent surface patterns has been probed as a ZnO nanofluid sessile drop rapidly dries. The high temporal resolution enabled by the high flux of synchrotron X-rays allows the observation of the emergence of Zn(OH) 2 surface crystals from the onset of evaporation and their rapid evolution into the final residual surface pattern, via transient layered complexes evident from the temporary appearance of X-ray diffraction peaks preceding Zn(OH) 2 formation. The results offer mechanistic insights of morphogenesis of surface patterns from evaporation-induced self-assembly and self-organization of reactive nanofluids, previously untenable using other experimental methods.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Low Melting Temperature Gallium–Indium Liquid Metal Anode for Solid-State Li-Ion Batteries

Solid-state Li-ion batteries are attracting attention for their enhanced safety features, higher energy density, and broader operational temperature range compared to systems based on liquid electrolytes. However, current solid-state Li-ion batteries face performance challenges, such as suboptimal cycling and poor rate capabilities, often due to inadequate interfacial contact between the solid electrolyte and electrodes. To address this issue, we incorporated a gallium–indium (Ga–In) liquid metal as the anode in a solid-state Li-ion battery setup, employing Li 6 PS 5 Cl as the solid electrolyte. Operating at room temperature, this configuration achieved an initial capacity of 389 mAh g –1 and maintained 88% of this capacity after 30 cycles at a 0.05 C rate. It also demonstrated a capacity retention of 66% after 500 cycles at a 0.5 C rate. In comparison to solid anode materials, such as tin, the Ga–In liquid metal exhibited superior cycling stability and rate capacity, which is due to the self-healing and fluid properties of the alloy that ensure stable interfacial contact with solid electrolytes. In situ X-ray diffraction (XRD) and ex situ scanning electron microscope (SEM) analyses revealed that indium does not directly participate in the lithiation/delithiation process. Instead, it helps maintain the alloy’s low melting point, facilitating its return to a liquid state after delithiation. In a comparative analysis of stack pressure during cycling in cells utilizing Ga–In liquid metal and tin, the Ga–In liquid metal cell demonstrated an ability to buffer pressure increases associated with deformation. In conclusion, these findings suggest a promising approach for enhancing solid-state batteries by integrating liquid metal anodes, which improve interfacial contact and stability.

Alloys↗
DOE OSTI2025

Gas-mediated defect engineering in earth-abundant Mn-rich layered oxides for non-aqueous sodium-based batteries

Gases are often by-products of battery materials during cell formation and degradation, affecting the cycle life and safety of rechargeable batteries. However, understanding gas-mediated (electro)-chemical reactions and nanoscale structural transformations during the synthesis of battery electrode materials remains challenging because of the lack of suitable characterization routes and the complexity of the interplay between thermodynamics and kinetics. Here, in this study, we use operando synchrotron X-ray diffraction, in situ transmission X-ray microscopy and multiscale modelling to elucidate the reaction pathways and microstructural defect development of earth-abundant Mn-rich layered oxides as positive electrode materials for sodium-based batteries. In particular, we demonstrate the dominant role of CO 2 over O 2 and H 2 O (g) in modulating the competition between entropy and enthalpy during solid-state synthesis. Using Ni 0.25 Mn 0.75 CO 3 as a model precursor, we reveal that CO 2 generation favours the formation of entropy-driven metastable intermediates, suppresses closed pore/nanovoids formation and decreases chemical heterogeneity and residual lattice strain of Mn-rich layered oxides during the synthesis. This result motivates a fast-sintering strategy to promote CO 2 release, which ultimately leads to improved chemo-mechanical and electrochemical stability of the Mn-rich positive electrodes when tested in non-aqueous Na metal coin cells.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Dual-precipitates enhance fatigue resistance in an additively manufactured high-entropy alloy

To accomplish the intense desire of high-strength materials for enhanced energy-efficiency, recent research applies a combined strategy of additive-manufacturing and precipitation-strengthening in high entropy alloys. In a context, Al 0.2 Co 1.5 CrFeNi 1.5 Ti 0.3 nanoprecipitation-strengthened system was developed, demonstrating very convincing strength and toughness. Moreover, additive-manufacturing facilitated additional strength by well-decorated cell-boundaries with blocky L2 1 precipitates and homogeneously distributed L1 2 precipitates. However, fatigue research of this alloy remained unexplored despite being the main precursor for structural applications. In this study low-cycle fatigue behavior of this alloy in both as-built and precipitation-strengthened (aged) conditions has been explored, combined with in-situ neutron diffraction investigation. Findings revealed a substantial cyclic-stress profile and a notable fatigue-life below ±0.50% strain-amplitude, exceeding 10 5 cycles at ±0.30% strain-amplitude. These demonstrate the potential to carry higher payloads with marked engineering-reliability. Residual-stress estimation revealed strain-compatibility between the matrix and L1 2 precipitate, indicating a crack-initiation immune interface. A comparative examination of dislocation character revealed shifting towards pure edge-character in aged alloy indicates precipitates promoted planar-slip during deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2025

X-ray diffraction strains in laser-ablated aluminum, nickel, sodium, and invar: Pressures to 475 GPa

Dynamically compressed materials in longitudinal waves are described by two physical models: hydrostatic pressure, with equal, normal, principal stresses or material uniaxially strained in the wave propagation direction. These models are disparate, so experimental comparisons and evaluations are important. Polycrystalline material in a state of hydrostatic pressure will have no eccentricity of x-ray-diffracted Debye–Scherrer rings. A general three-dimensional solution of Bragg diffracted x rays based on principal crystallographic strains in the compression wave was found. The distortion of x-ray diffraction beams has been used for strain measurements; the analysis developed incorporates a strained reciprocal lattice and the incident x-ray beam. Strain-distorted Polanyi surfaces form an annulus of compression with an ellipsoid of revolution in reciprocal space, which is intersected by Ewald's sphere for Bragg diffraction. The in situ measurements for strain describe nanosecond diffraction evaluated using two planes, (hkl) and (h′k′l′), both in the same crystallographic phase. Diffraction from Al, Ni, Na, and Invar quantifies the compression axial strains in these materials: The compression axial ratios are 0.65, 1.05, 0.88, and 1.58 at pressures of 291, 402, 409, and 367 GPa for the respective materials. Crystal structure transformations with homogeneous pressurized stresses, mandating equal normal strains, should not be anticipated to agree with heterogeneous, uniaxially strained, and sheared crystalline phases. Measurements support in-plane strains increasing with pressure, p , in fcc and hcp aluminum as ε 22 = −0.21 p /TPa.

Alloys↗
DOE OSTI2025

Creep Property of Intermetallic Dispersive Steels for Nuclear Applications

To meet the materials performance demands of next-generation nuclear and high-temperature energy systems, a new class of intermetallic-dispersive steels (IDS) has been designed through integrated computational thermodynamics and alloy design strategies. The IDS alloys incorporate coherent L1₂ (γ′-Ni₃Al) nanoprecipitates within an Fe–Ni–Cr austenitic matrix, engineered to achieve both high temperature strength and thermodynamic stability while suppressing the formation of detrimental δ-Ni₃Nb and η-Ni₃Ti phases. Initial creep testing of Ti-IDS and TiTa-IDS alloys demonstrates rupture lives comparable to or exceeding those of Inconel 718 and ODS steels, despite being fabricated through conventional ingot metallurgy. Step-load creep tests identified a stress threshold near 300–350 MPa for the onset of tertiary creep, and in-situ neutron diffraction experiments on Ti-IDS revealed clear load partitioning between the matrix and γ′ precipitates: elastic strain is shared by both phases, while plastic strain localizes in the matrix. These results confirm that stable γ′–matrix interfaces play a dominant role in retarding dislocation motion and enhancing creep resistance. In FY26, the program will conduct repeat creep rupture testing of TiTa-IDS at 650 °C/400 MPa, initiate long-term rupture testing of TiNb-IDS, and perform TEM-based microstructural characterization to elucidate dislocation–precipitate interactions and microstructural stability. Collectively, these efforts will establish the mechanistic foundation for next-generation high-temperature structural materials based on the IDS concept.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗