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Results for “transmission x-ray microscopy”

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All sources NASA NTRS DOE OSTI

DOE OSTI2026

Soft X-ray reflection ptychography

Scanning transmission X-ray microscopy and ptychography have become mature tools for high-resolution, element-specific imaging of nanoscale structures. However, transmission geometries impose stringent constraints on sample thickness and preparation, thereby limiting investigations of extended or bulk specimens, especially in the soft X-ray region. Here, we demonstrate reflection-geometry soft X-ray ptychography as a robust imaging mode. Instrumental feasibility and spatial resolution are established using a lithographically defined Siemens star and barcode test pattern on a multilayer substrate. We empirically demonstrate a full-pitch spatial resolution of ca. 45 nm from Fourier ring correlation analysis of the reconstructed object. The results highlight the potential of the reflection geometry for nondestructive X-ray studies of materials without the need for transmissive samples.

Guenzing, Damian [Lawrence Berkeley National Labor↗

DOE OSTI2026

High Pressure Synthesis of Ultrasmall Nanodiamonds with Nitrogen Vacancy Centers

C–H terminated nanometer scale diamonds ( d = 1 to 15 nm) are synthesized from 1-fluoroadamantane at high pressure (6–8 GPa) and high temperature (500–1500 °C) in a multianvil press. High resolution transmission electron microscopy, X-ray diffraction, Raman, diffuse reflectance Fourier transform infrared, and X-ray absorption spectroscopies demonstrate the excellent crystallinity and atomically flat C–H terminated surfaces of nanodiamonds with (111) and (110) facets. The importance of hydrogen to the synthesis of nanodiamond and its faceting is discussed. Following vacancy generation, annealing and oxidation of the nanodiamonds, optically detected magnetic resonance and electron spin resonance coherence times ( T 2 = 0.9 and 2.1 μs) of nitrogen vacancy (NV) centers are measured. Finally, the obtained T 2 values are equivalent to the shallow NV centers (depth <10 nm) in bulk diamond crystals and larger nanocrystals prepared by mechanical milling.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Using X-ray spectrum imaging to quantify fission gas in high-burnup UO2 fuel

Analysis of fission gas bubbles (FGBs) in light-water reactor (LWR) fuel is needed to improve the understanding and predictive capability of fuel evolution under normal- and transient conditions. One of the most important parameters of a FGB is the pressure of the gas, primarily Xe, inside it. Bubble volume and location (inter- vs. intragranular) are important considerations as well. However, experimental analysis of such bubbles is challenging due to their small size and embedded nature, and usefulness of the data requires large numbers be analyzed. This paper proposes a method to measure the pressure of Xe bubbles using X-ray spectrum imaging (XSI) in scanning transmission electron microscopy (STEM). From X-ray generation and instrumental parameters, the number of Xe atoms yielding a given number of Xe L-series X-ray counts is estimated, and then from the estimated volume of the bubble the Xe density is estimated, which can then be converted to pressure via an equation-of-state. We apply the method to XSI datasets from high burnup (HBu) fuel from North Anna 1 reactor in as-irradiated and post-LOCA-test conditions and find Xe pressures in the FGBs clustered around 1 GPa.

Parish, Chad [ORNL] (ORCID:0000000312097439)↗

DOE OSTI2025

Effect of Preparation Conditions of Fe@SiO2 Catalyst on Its Structure Using High-Pressure Activity Studies in a 3D-Printed SS Microreactor

Fischer–Tropsch synthesis (FTS) in a 3D-printed stainless steel (SS) microchannel microreactor was investigated using Fe@SiO2 catalysts. The catalysts were prepared by two different techniques: one pot (OP) and autoclave (AC). The mesoporous structure of the two catalysts, Fe@SiO2 (OP) and Fe@SiO2 (AC), ensured a large contact area between the reactants and the catalyst. They were characterized by N2 physisorption, H2 temperature-programmed reduction (H2-TPR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron microscopy (XPS), and thermogravimetric analysis–differential scanning calorimetry (TGA-DSC) techniques. The AC catalyst had a clear core–shell structure and showed a much greater surface area than that prepared by the OP method. The activities of the catalysts in terms of FTS were studied in the 200–350 °C temperature range at 20-bar pressure with a H2/CO molar ratio of 2:1. The Fe@SiO2 (AC) catalyst showed higher selectivity and higher CO conversion to olefins than Fe@SiO2 (OP). Stability studies of both catalysts were carried out for 30 h at 320 °C at 20 bar with a feed gas molar ratio of 2:1. The Fe@SiO2 (AC) catalyst showed higher stability and yielded consistent CO conversion compared to the Fe@SiO2 (OP) catalyst.

Biochemistry & Molecular Biology↗

DOE OSTI2025

From Pollutant Removal to Renewable Energy: MoS2-Enhanced P25-Graphene Photocatalysts for Malathion Degradation and H2 Evolution

The widespread presence of pesticides—especially malathion—in aquatic environments presents a major obstacle to conventional remediation strategies, while the ongoing global energy crisis underscores the urgency of developing renewable energy sources such as hydrogen. In this context, photocatalytic water splitting emerges as a promising approach, though its practical application remains limited by poor charge carrier dynamics and insufficient visible-light utilization. Herein, we report the design and evaluation of a series of TiO2-based ternary nanocomposites comprising commercial P25 TiO2, reduced graphene oxide (rGO), and molybdenum disulfide (MoS2), with MoS2 loadings ranging from 1% to 10% by weight. The photocatalysts were fabricated via a two-step method: hydrothermal integration of rGO into P25 followed by solution-phase self-assembly of exfoliated MoS2 nanosheets. The composites were systematically characterized using X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectroscopy (DRS), and photoluminescence (PL) spectroscopy. Photocatalytic activity was assessed through two key applications: the degradation of malathion (20 mg/L) under simulated solar irradiation and hydrogen evolution from water in the presence of sacrificial agents. Quantification was performed using UV-Vis spectroscopy, gas chromatography–mass spectrometry (GC-MS), and thermal conductivity detection (GC-TCD). Results showed that the integration of rGO significantly enhanced surface area and charge mobility, while MoS2 served as an effective co-catalyst, promoting interfacial charge separation and acting as an active site for hydrogen evolution. Nearly complete malathion degradation (~100%) was achieved within two hours, and hydrogen production reached up to 6000 µmol g−1 h−1 under optimal MoS2 loading. Notably, photocatalytic performance declined with higher MoS2 content due to recombination effects. Overall, this work demonstrates the synergistic enhancement provided by rGO and MoS2 in a stable P25-based system and underscores the viability of such ternary nanocomposites for addressing both environmental remediation and sustainable energy conversion challenges.

Chemistry↗

DOE OSTI2026

Crystallographic registry in epitaxial V3O5 thin films

Crystallographic orientation plays a central role in determining transport properties in correlated oxides with low-hysteresis metal–insulator transitions. Here, V3O5 thin films were grown on Al2O3 (0001) and their crystallographic registry was evaluated using x-ray diffraction and cross-sectional transmission electron microscopy. θ–2θ measurements show a single out-of-plane orientation defined by the (202) reflection. Azimuthal φ-scans of the V3O5 (310) reflection exhibit twelve discrete maxima over 360°, indicating a finite set of in-plane orientations imposed by the substrate symmetry. High-resolution TEM and fast Fourier transform analysis confirm crystallographic coherence at the film–substrate interface. The electrical conductivity exhibits a metal–insulator transition at TMIT ≈ 423 K with no measurable thermal hysteresis and a total change of ~1.6 orders of magnitude between 300 and 480 K. These results establish crystallographic registry in epitaxial V3O5 thin films and provide a structurally well-defined system for future studies of orientation-dependent transport.\r\nT

36 MATERIALS SCIENCE↗

DOE OSTI2026

Directing Assembly of Mesoscale Multi‐Shell Morphologies of DNA Origami Crystals

Nature builds hierarchically ordered materials, such as seashells, wood, and bones, through spatially and temporally regulated growth. Mimicking such a level of control in synthetic systems remains challenging, particularly in achieving multiscale organizations with prescribed nanoscale arrangements and desired material morphologies. In this study, we introduce a DNA-based self-assembly strategy for constructing diverse multi-shell mesoscale morphologies from nanoscale lattices, enabling prescribed structural, and compositional 3D material patterns. Using DNA origami frames as modular monomers, we direct anisotropic epitaxial growth through addressable DNA frame binding motifs and encapsulate nanoparticles (NPs) in desired 3D patterns. Sequential monomer addition under thermodynamically favorable conditions enables shell growth through heterogeneous nucleation while minimizing unwanted homogeneous nucleation. Here, we demonstrate that DNA-encoded addressability enables epitaxial shell growth along specific lattice directions, yielding crystals with multilayered mesoscale organization, including tube-like (sushi roll) and plate-like (macaron) morphologies. Shell-specific NP configurations and compositions are achieved through addressable and differentiated placement of NPs within each shell, as validated by small-angle x-ray scattering and cross-sectional scanning transmission electron microscopy. We further demonstrate addressable NP release and reveal that shells modulate release kinetics. Together, these findings establish a platform for fabricating DNA origami crystals with programmable mesoscale morphologies, nanoscale structure, composition, and transport properties.

3D patterning↗

DOE OSTI2026

Complex-Concentrated Anion Doping Enables Ultra-Stable Lattice Oxygen and Structural Integrity in Lithium-Rich Layered Oxide Cathodes

Lithium- and manganese-rich layered oxides (LMR) stand out as next-generation lithium-ion cathode chemistries, which harness both transition-metal and lattice-oxygen redox processes to deliver exceptional capacity and energy density. However, their full potential is hindered by intrinsic oxygen instability and structural degradation, resulting in pronounced voltage fade and capacity decay. Here, we present a complex-concentrated anion-doping paradigm in which multiple anions, F, Br, and S, are incorporated into the oxygen sublattice to enhance oxygen-redox and structural stability. X-ray absorption spectroscopy and aberration-corrected scanning transmission electron microscopy confirm ultra-stable local oxygen coordination environments during long-term cycling, with detrimental phase transformations and oxygen-loss-induced cavitation dramatically inhibited. Notably, we show that the characteristic LiTM6 transition metal (TM) honeycomb ordering is preserved even after electrochemical cycling. Concurrently, this strategy yields an unprecedented volume change of only 0.63% upon charging to 4.8 V vs. Li+/Li, achieving the first zero-strain LMR cathode. The resulting LMR cathode delivers ultralow voltage fade (1 mV per cycle during the first 100 cycles and becomes negligible in subsequent cycles) and outstanding energy retention (93% after 200 cycles) in a pouch cell configuration. Our complex-concentrated anion-doping concept establishes a broadly applicable strategy for resolving chemo-mechanical failure mechanisms in ceramic intercalation electrodes for next-generation energy storage.

Li-ion batteries↗

DOE OSTI2026

Comprehensive structural characterization of charged polymers involved in moisture-driven direct air capture

This study provides a comprehensive structural characterization of commercially available alkaline anion-exchange polymers (Fumasep FAA-3 and IRA 900) used in moisture-driven direct air capture (DAC) of carbon dioxide. Using X-ray diffraction, SAXS/WAXS, atomic force microscopy, FIB-SEM, and transmission electron microscopy, the authors identify nanoscale clustering, porosity, swelling behavior, and humidity-dependent structural changes that influence CO₂ adsorption and release. These findings establish structure–function relationships critical for designing more durable and energy-efficient DAC polymer materials.

36 MATERIALS SCIENCE↗

NASA NTRS2026

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-Aluminosilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures for consideration as a thermal and environmental barrier coating (T/EBC) material. CYbS apatite powder was synthesized from the constituent oxides via a solid-state reaction method. Hot-pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high-angle annular dark-field imaging, selected area electron diffraction, and energy dispersive x-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1 to 50 h at 1200 °C as well as in those heat treated at 1300 °C for 1 h. Residual CMAS was depleted of Ca when cyclosilicate was present. Dendritic wollastonite (CaSiO3) was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

Narottam P Bansal↗

NASA NTRS2026

Thermal Inspection for the Assessment of Adhesively Bonded Metal Adherends

Certification of adhesively bonded structures is currently a challenge for aircraft manufacturers. The ability to certify bonds in primary structure can reduce dependence on fasteners and this will enable more efficient manufacturing. For example, drilling holes and installing fasteners in bonded joints can be a potentially significant bottleneck in airframe manufacturing. In addition, fasteners increase the airframe weight and can add stress concentration areas. Reducing fastener count can accelerate manufacturing and improve aircraft performance. NASA is currently investigating nondestructive evaluation (NDE) techniques to assess bond integrity. For example, bond thickness influences bond strength and therefore NDE techniques are being investigated to determine bond thickness. For bonded metal structures, there is a large difference in the thermal diffusivity between the 7075 aluminum alloy metal adherends and aircraft grade adhesive. Multi-layered thermal models show a large variation in the thermal response for bondline adhesive thicknesses that vary from 100 to 300 microns for adherend thicknesses of 0.163 cm. Experimental through-transmission thermal measurements reveal promise to quantitatively characterize the bondline thickness. Results were validated with X-ray computed tomography and optical microscopy measurements, and influence of porosity on the thermal model and measurements are investigated.

X-ray computed tomography↗

NASA NTRS2026

Thermal Inspection for the Assessment of Adhesively Bonded Metal Adherents

bondline thickness↗

DOE OSTI2026

Defect-Limited Carrier Lifetime in Epitaxially Strained Germanium-On-Silicon Heterostructures

Epitaxially strained germanium-on-silicon (Ge-on-Si) heterostructures are central to next-generation photonic and electronic devices, yet their performance remains strongly constrained by defect-limited carrier lifetimes. In this work, we investigate the impact of defects on the carrier lifetime in relaxed Ge-on-Si and strained Ge-on-Si heterostructures. High-resolution X-ray diffraction quantifies the strain-state in Ge and reveals signatures of strain relaxation due to lattice mismatch. Cross-sectional and plan-view transmission electron microscopy analyses enable direct visualization of interfacial defects and quantification of threading dislocation densities (TDDs) within the Ge layer. However, the presence of a dense misfit dislocation network obscures the threading dislocation signatures, preventing reliable TDD determination by plan-view transmission electron microscopy in strained-Ge (..epsilon..-Ge). To assess the defect density in this case, etch-pit density measurements were performed, providing an alternative means of quantifying the TDDs in the ..epsilon..-Ge layer. Carrier lifetime measurements by microwave-reflection photoconductive decay reveal a clear relationship with TDDs ranging from 5 x 103 cm-2 to 2 x 1010 cm-2, confirming Shockley-Read-Hall recombination as the limiting mechanism at lower defect densities, with TDD-dominated recombination at higher defect densities. The Ge-on-Si relaxed heterostructure exhibited lifetimes much lower (~12 ns) than the lattice-matched Ge on gallium arsenide (GaAs) (~158 ns) heterostructure. Introducing controlled tensile strain reduces defect formation, suppresses strain-relaxation pathways, and leads to measurable improvements in minority carrier lifetime from 12 ns to 171 ns. These results establish a direct relation between defect suppression and carrier recombination dynamics in both relaxed Ge-on-Si grown directly on Si and strained Ge-on-Si heterostructures incorporating compound-semiconductor buffer layers, offering a materials-driven pathway for engineering Ge with improved carrier lifetime for photonic applications.

36 MATERIALS SCIENCE↗

DOE OSTI2026

In-Situ TEM Molten Salt Corrosion

Molten salt reactors (MSRs) offer a compelling pathway for next-generation nuclear energy, with advantages in thermal efficiency, inherent safety, and flexible fuel management. Yet, halide-based molten salts introduce significant materials challenges, particularly alloy corrosion. Alloy performance in these environments ultimately depends on understanding how corrosion initiates and progresses at the nanoscale, however most existing models rely on post-exposure characterization, leaving degradation mechanisms largely inferred rather than directly observed. NiCr alloys have garnered interest in MSRs applications as the Ni-based matrix provides strength and creep resistance, while Cr content offers oxidation resistance in air. However, NiCr corrosion resistance in chloride salts has proven poor due to preferential chromium dissolution, the formation of Cr-depleted pathways, and grain-boundary attack. This work aims to directly visualize corrosion of Ni-20Cr exposed to LiCl-KCl using in-situ Transmission Electron Microscopy (TEM) to capture real-time microstructural evolution during corrosion. Experiments will be performed at ~800 °C under controlled pressure conditions while utilizing Energy-Dispersive X-ray Spectroscopy (EDS) to analyze elemental redistribution. Observation of chromium depletion fronts, associated surface restructuring, and localized chloride enrichment are expected. Ultimately, this study is expected to provide a link between microscale processes and the macroscopic degradation behaviors relevant to MSR operation in advanced reactor environments. Simultaneously, this approach enables future in-situ investigations regarding alloy composition, salt chemistry, and their influence on corrosion pathways and long-term stability.?

36 - MATERIALS SCIENCE↗

DOE OSTI2026

Formation of Bimetallic Nanoparticles via Exsolution Using a Reducible Metal Oxide Capping Layer

Bimetallic nanoparticles are promising catalysts that can improve performance in heterogeneous catalysis and solid-state electrochemistry. Exsolution is a useful method for forming such nanoparticles; however, it is limited by the elements present within the host oxide lattice. Here, in this work, we develop and demonstrate a strategy to form bimetallic particles from La 0.5 Sr 0.5 Ti 0.94 Ni 0.06 O 3 (LSTN) exsolution and using a reducible SnO 2 capping layer, expanding the range of elements available for bimetallic nanoparticle formation. Using this capping layer strategy, we formed nickel–tin (Ni 0 –Sn 0 ) bimetallic nanoparticles via exsolution. We used in situ near-ambient pressure X-ray photoelectron spectroscopy to monitor surface chemical changes during exsolution, showing that first, SnO 2 volatilized. This SnO 2 loss exposed the perovskite surface of LSTN to reducing conditions, which induced Ni exsolution, and compounded with SnO 2 reduction led to the formation of bimetallic Ni 0 –Sn 0 particles. To evaluate the associated microstructural evolution, we measured grazing incidence small-angle X-ray scattering (GISAXS), which confirmed the loss of the SnO 2 capping layer, and scattering simulations suggested the formation of bimetallic particles. We confirmed the bimetallic nanoparticle composition and morphology by Auger spectroscopy and scanning transmission electron microscopy. The resulting bimetallic nanoparticles were smaller and more thermally stable than the monometallic Ni counterparts on LSTN. This capping layer and exsolution approach allow synthesizing multimetallic nanoparticles and can be applied to other reducible metal oxides and perovskite hosts, broadening the compositional space for advanced catalytic materials.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Epitaxial registry and transport properties in V4O7 thin films

We report the growth of V4O7 thin films deposited simultaneously on amorphous SiO2 and crystalline c-cut Al2O3 substrates. x-ray diffraction shows that films grown on SiO2 are polycrystalline with no preferred orientation, while films grown on Al2O3 exhibit a well-defined out-of-plane orientation and an in-plane registry consistent with epitaxial growth. Transmission electron microscopy confirms the crystallographic relationship between the V4O7 film and the Al2O3 substrate. Atomic force microscopy indicates substantially lower surface roughness for films grown on Al2O3 (~6 nm) compared to those grown on SiO2 (~22 nm), and Raman spectroscopy confirms stabilization of the same V4O7 phase on both substrates. Electrical transport measurements reveal a metal–insulator transition near 244 K for both substrates, with thermal hysteresis not exceeding ~1 K. Although the transition temperature remains essentially unchanged, films grown on Al2O3 exhibit higher conductivity over the entire temperature range, exceeding that of films grown on SiO2 by approximately two orders of magnitude at 100 K and by a factor of five at 300 K. These results indicate that the conductivity differences are consistent with variations in microstructural connectivity associated with crystallographic order.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Superconducting Material Growth for Radio-Frequency (RF) Cavities

Superconducting radio-frequency (SRF) cavities, usually manufactured from Niobium (Nb), are vital components of modern particle accelerators because of their ability to achieve high acceleration gradients with little power dissipation. Naturally forming Nb surface oxides significantly alter cavity performance by changing surface resistance. A nondestructive characterization of oxide thickness is helpful for relating surface processing treatments to cavity performance. This work develops a protocol to measure Nb oxide thickness using Angle-Resolved X-ray Photoelectron Spectroscopy (ARXPS) while correcting instrumental errors. Using uniform bulk standard samples (Silver, Aluminum oxide, and Germanium), we determined a baseline correction factor to account for analyzer-related intensity evolution as the measurement angle increases. The correction factor was then applied to Nb 3d ARXPS data. Applying the Strohmeier equation to the corrected data yielded a Nb2O5 thickness of 6.04 nm, closely matching the 5.5 (±.05) nm value obtained from cross-sectional transmission electron microscopy. Our approach will bring a method to incorporate inherent errors in the thickness measurements using ARXPS and can be broadly applied to improve the accuracy of thickness measurements in a wide range of heterostructures.

Lambert, Nathan [Fermilab]↗

DOE OSTI2026

Superconducting Material Growth for Radio-Frequency (RF) Cavities

Lambert, Nathan [Fermilab]↗