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At least 163 records · Page 9
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DOE OSTI2026

Irradiation Driven Restructuring of Nanocrystalline ThO 2 and Th 1–x U x O 2 Thin Films

Irradiation induced structural changes of actinide oxide materials is a key consideration in their development and use as nuclear fuels. This study reported on the synthesis of ThO 2 and Th 1–x U x O 2 (x = 0.15, 0.50) thin films, fabricated using electrospray-assisted solution combustion synthesis, and their responses to ion irradiation. Krypton ion irradiations, up to a fluence of 1 × 10 16 ions/cm 2 , were carried out to simulate radiation damage induced by fission products in a reactor environment. Structural and chemical changes induced by irradiation were analyzed using high-resolution scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDS), and electron energy-loss spectroscopy (EELS). It was determined that the extent and nature of irradiation-induced damage are strongly correlated with the uranium content. ThO 2 films were most susceptible to radiation-induced damage, with significant cavity formation and delamination from the substrate at high fluence. Of the compositions studied, Th 0.85 U 0.15 O 2 films showed the highest stability, characterized by moderate grain growth and the absence of voids or severe defect structures. In contrast, Th 0.5 U 0.5 O 2 films accumulated extensive damage, including the formation of a nanocrystalline central region. EELS analysis indicated that oxygen displacement is the primary driver of structural degradation in Th 0.5 U 0.5 O 2 films. α-particle spectroscopy confirmed minimal actinide loss across all compositions, underscoring the mechanical robustness of the films. These findings provide insight into the irradiation-induced damage mechanisms in Th O2 and Th 1–x U x O 2 systems, supporting their development as potential materials for nuclear fuels and irradiation-tolerant thin film targets in nuclear physics measurements.

Th1−xUxO2↗
DOE OSTI2026

Small Molecule Inhibitor-Modulated Al 2 O 3 Atomic Layer Deposition on Monolayer MoS 2 for Controlled Nucleation

The integration of ultrathin dielectrics on two-dimensional (2D) semiconductors is essential for advancing beyond-Si electronics. However, the intrinsic inertness of van der Waals 2D basal planes remains a primary bottleneck to achieving uniform dielectric nucleation and growth. Here, in this study, we introduce a small molecule inhibitor (SMI)-modulated thermal atomic layer deposition (ALD) strategy, exemplified by aluminum oxide (Al 2 O 3 ) ALD on monolayer molybdenum disulfide (1L MoS 2 ) with acetic acid (HAc) SMI. The ABC-type sequence comprises HAc inhibitor (A), trimethylaluminum (TMA) precursor (B), and deionized H 2 O coreactant (C). In situ quartz crystal microbalance (QCM) studies reveal robust HAc adsorption on Al 2 O 3 and suppression of subsequent oxide growth on HAc-passivated surfaces. When applied to 1L MoS 2 , this inhibitory pathway enables HAc to selectively passivate nascent Al 2 O 3 nuclei formed on the MoS 2 surface, limiting their three-dimensional (3D) island coarsening and redirecting precursor adsorption toward the uncovered basal plane. Consequently, nearly continuous ultrathin (∼1.5 nm) Al 2 O 3 films are achieved on 1L MoS 2 with markedly improved uniformity compared to standard Al 2 O 3 ALD using TMA and H 2 O, as validated by atomic force microscopy (AFM), cross-sectional scanning transmission electron microscopy (STEM), and energy-dispersive X-ray spectroscopy (EDS). Density functional theory (DFT) calculations further provide atomistic insight into HAc-modulated Al 2 O 3 nucleation, corroborating the energetic preference of HAc for Al 2 O 3 over MoS 2 and attenuated TMA adsorption on HAc-passivated surfaces. Spatially resolved Raman spectroscopy also confirms that the HAc-modulated process preserves the structural integrity of 1L MoS 2 , with only minimal strain and doping perturbations observed after dielectric deposition. This SMI-modulated approach offers a broadly applicable framework for controlling ALD nucleation across various inhibitors, ALD chemistries, and 2D materials, opening opportunities for reliable dielectric integration in next-generation nanoelectronics.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Laser-Assisted Synthesis of Monolayer 2D MoSe 2 Crystals with Tunable Vacancy Concentrations: Implications for Gas and Biosensing

We report tuning the structural and electronic properties of atomically thin two-dimensional (2D) materials via defect and vacancy engineering is the key to enabling their potential use in various applications, including electronics, energy, and sensing devices. Vacancies are, for instance, becoming highly promising for the enhanced interaction of gases and biomolecules with 2D materials in energy and sensing applications. However, the deterministic generation of desirable vacancies with tunable concentrations remains a challenge in 2D materials due to the limitations in the current growth methods, such as the complex reaction chemistries and gas flow dynamics. Therefore, engineering defects and vacancies in 2D materials have been mainly limited to destructive top-down processes such as heating, ion bombardments, and laser postprocessing. Here, we introduce a single-step bottom-up synthesis approach for the growth of monolayer MoSe 2 crystals with tunable vacancy concentrations. This method utilizes the spatiotemporal properties and adjustable power densities of the lasers to control the vaporization dynamics of the stoichiometric MoSe 2 powders. Such a mechanism in the vaporization allows us to grow tunable stoichiometry monolayer MoSe 2–x crystals on the substrates. The localized and time-controlled (250 ms to 2 s) vaporization of the MoSe 2 powder by a CO 2 laser enables the formation of monolayer crystals with controlled vacancy concentrations ranging from ~1 to 20%. The effects of laser power, laser irradiation time, and background pressure on the tuning range and subsequent properties of the crystals are investigated and quantified using Raman and photoluminescence spectroscopy, scanning transmission electron microscopy (STEM), and time-correlated single-photon counting (TCSPC). This bottom-up synthesis is a promising approach that allows the deterministic vacancy tuning for future electronics and, in particular, gas and biosensing applications without the need for further postprocessing and potential structural disruption of the crystals.

2D materials↗
DOE OSTI2021

High-Resolution Imaging of Unstained Polymer Materials

Electron microscopy has played an important role in polymer characterization. Traditionally, electron diffraction is used to study crystalline polymers while transmission electron microscopy is used to study microphase separation in stained block copolymers and other multiphase systems. We describe developments that eliminate the barrier between these two approaches - it is now possible to image polymer crystals with atomic resolution. The focus of this Review is on high-resolution imaging (30 Å and smaller) of unstained polymers. Recent advances in hardware allow for capturing numerous (as many as 105) low-dose images from an unperturbed specimen; beam damage is a significant barrier to high-resolution electron microscopy of polymers. Machine-learning-based software is then used to sort and average the images to retrieve pristine structural information from a collection of noisy images. Acknowledging the heterogeneity in polymer samples prior to averaging is essential. Molecular conformations in a wide range of amphiphilic block copolymers, polymerized ionic liquids, and conjugated polymers can be gleaned from two-dimensional projections (2D), three-dimensional (3D) tomograms, and four-dimensional (4D) scanning transmission electron microscopy (STEM) data sets where 2D diffraction patterns are taken as a function of position. Some methods such as phase contrast STEM have been used to image closely related materials such as metal-organic frameworks but not polymers. With improvements in hardware and software, such methods may soon be applied to polymers. Our goal is to provide a comprehensive understanding of the strategies toward the high-resolution imaging of radiation sensitive polymer materials at different length scales.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Dehydrogenation of Propane and n -Butane Catalyzed by Isolated PtZn 4 Sites Supported on Self-Pillared Zeolite Pentasil Nanosheets

Propene and 1,3-butadiene are important building-block chemicals that can be produced by dehydrogenation of propane and butane over Pt catalysts. The challenge is to develop highly active and selective catalysts that are resistant to deactivation by Pt sintering and coke formation. We have recently shown that these objectives can be met for propane dehydrogenation using atomically dispersed Pt atoms anchored to neighboring ≡SiOZn-OH groups bonded to the framework dealuminated zeolite BEA. In the present study, we demonstrate that significantly superior performance can be achieved by using self-pillared pentasil (SPP) zeolite nanosheets. Following catalyst reduction in H 2 , atomic-resolution, scanning transmission electron microscopy (STEM) and X-ray absorption spectroscopy (XAS) indicate that Pt is stabilized in structures well approximated as (≡Si-O-Zn) 4-5 Pt. These species are highly active, selective, and stable for propane dehydrogenation (PDH) to give propene and for n-butane dehydrogenation (BDH) to give 1,3-butadiene. No catalyst deactivation was observed after 12 days of time on stream, and the selectivity remained at nearly 100% for PDH conducted at 823 K and a weight hourly space velocity (WHSV) of 1,350 h -1 . The apparent rate coefficient for PDH over this catalyst is significantly higher than that reported previously for Pt-containing catalysts. For BDH at 823 K and a WHSV of 3560 h -1 , the selectivity to butene isomers and 1,3-butadiene is 98.9%, and the selectivity to 1,3-butadiene is 45%. Here, we propose that the high catalyst stability observed during PDH and BDH is a consequence of a large fraction of the Pt-containing centers being located on the external surface of the zeolite nanosheets, where nascent coke precursors can desorb before condensing to form coke.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Cascade Reaction of Ethanol to Butadiene over Ag-Promoted, Silica- or Zeolite-Supported Ta, Y, Pr, or La Oxide Catalysts

Ethanol converts to 1,3-butadiene in the presence of suitable multifunctional catalysts. In this work, Lewis acid cations Ta, Y, Pr, and La were dispersed on amorphous silica or beta zeolite, and after physically mixing with silica-supported Ag nanoparticles, were tested in the cascade reaction of ethanol to butadiene at 573 K. The Lewis acid catalysts were characterized by X-ray fluorescence, N 2 physisorption, scanning transmission electron microscopy (STEM), X-ray diffraction, diffuse reflectance (DR) UV-Vis and X-ray photoelectron spectroscopy. High-resolution STEM images confirmed the small oxide cluster size on the silica support. Results from DR UV-Vis spectroscopy showed zeolite-supported Ta and Pr catalysts had a smaller metal oxide cluster size, relative to their SiO 2 counterparts. X-ray photoelectron spectroscopy confirmed the oxidation state of the cations supported on the zeolite remained the same as that of their SiO 2 -supported analogues. The selectivity of the C 4 coupling products toward butadiene relative to butanol correlated with acid strength of the Lewis acid cations, as evaluated by the 2-propanol decomposition reaction to propene and acetone, with Ta being the most selective. In conclusion, the rate of C-C coupling over the zeolite-supported cations was enhanced by an order of magnitude compared to those cations supported on amorphous SiO 2 .

C-C bond formation↗
DOE OSTI2021

Structural and Valence State Modification of Cobalt in CoPt Nanocatalysts in Redox Conditions

Platinum is the primary catalyst for many chemical reactions in the field of heterogeneous catalysis. However, platinum is both expensive and rare. Therefore, it is advantageous to combine Pt with another metal to reduce cost while also enhancing stability. To that end, Pt is often combined with Co to form Co-Pt nanocrystals. However, dynamical restructuring effects that occur during reaction in Co-Pt ensembles can impact catalytic properties. In this study, model Co 2 Pt 3 nanoparticles supported on carbon were characterized during a redox cycle with two in situ approaches, namely X-ray absorption spectroscopy (XAS) and scanning transmission electron microscopy (STEM) using a multimodal microreactor. The sample was exposed to temperatures up to 500 °C under H 2 , and then to O 2 at 300 °C. Irreversible segregation of Co in the Co-Pt particles was seen during redox cycling and substantial changes of the oxidation state of Co were observed. After the H 2 treatment, a fraction of Co could not be fully reduced and incorporated into a mixed Co-Pt phase. Re-oxidation of the sample increased Co segregation, and the segregated material had a different valence state than in the fresh, oxidized sample. Furthermore, this in situ study describes dynamical restructuring effects in CoPt nano-catalysts at the atomic scale that are crucial to understand to improve the design of catalysts used in major chemical processes.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Role of the Mineral in the Self-Healing of Cracks in Human Enamel

Human enamel is an incredibly resilient biological material, withstanding repeated daily stresses for decades. The mechanisms behind this resilience remain an open question, with recent studies demonstrating a crack-deflection mechanism contributing to enamel toughness and other studies detailing the roles of the organic matrix and remineralization. Here, we focus on the mineral and hypothesize that self-healing of cracks in enamel nanocrystals may be an additional mechanism acting to prevent catastrophic failure. To test this hypothesis, we used a molecular dynamics (MD) approach to compare the fracture behavior of hydroxyapatite (HAP) and calcite, the main minerals in human enamel and sea urchin teeth, respectively. In this work, we find that cracks heal under pressures typical of mastication by fusion of crystals in HAP but not in calcite, which is consistent with the resilience of HAP enamel that calcite teeth lack. Scanning transmission electron microscopy (STEM) images of structurally intact ("sound") human enamel show dashed-line nanocracks that resemble and therefore might be the cracks healed by fusion of crystals produced in silico . The fast, self-healing mechanism shown here is common in soft materials and ceramics but has not been observed in single crystalline materials at room temperature. The crack self-healing in sound enamel nanocrystals, therefore, is unique in the human body and unique in materials science, with potential applications in designing bioinspired materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Probing Oxidation-Driven Amorphized Surfaces in a Ta(110) Film for Superconducting Qubit

Recent advances in superconducting qubit technology have led to significant progress in quantum computing, but the challenge of achieving a long coherence time remains. Despite the excellent lifetime performance that tantalum (Ta) based qubits have demonstrated to date, the majority of superconducting qubit systems, including Ta-based qubits, are generally believed to have uncontrolled surface oxidation as the primary source of the two-level system loss in two-dimensional transmon qubits. Therefore, atomic-scale insight into the surface oxidation process is needed to make progress toward a practical quantum processor. Here, in this study, the surface oxidation mechanism of native Ta films and its potential impact on the lifetime of superconducting qubits were investigated using advanced scanning transmission electron microscopy (STEM) techniques combined with density functional theory calculations. The results suggest an atomistic model of the oxidized Ta(110) surface, showing that oxygen atoms tend to penetrate the Ta surface and accumulate between the two outermost Ta atomic planes; oxygen accumulation at the level exceeding a 1:1 O/Ta ratio drives disordering and, eventually, the formation of an amorphous Ta 2 O 5 phase. In addition, we discuss how the formation of a noninsulating ordered TaO 1–δ (δ < 0.1) suboxide layer could further contribute to the losses of superconducting qubits. Subsurface oxidation leads to charge redistribution and electric polarization, potentially causing quasiparticle loss and decreased current-carrying capacity, thus affecting superconducting qubit coherence. The findings enhance the comprehension of the realistic factors that might influence the performance of superconducting qubits, thus providing valuable guidance for the development of future quantum computing hardware.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Significance of a Solid Electrolyte Interphase on Separation of Anode and Cathode Materials from Spent Li-Ion Batteries by Froth Flotation

The separation of electrode active materials from spent Li-ion batteries (LIBs) by froth flotation is challenging due to the changes in surface properties of electrode active materials from cycling as well as the presence of organic binders. In this work, the froth flotation separation of aged anode and cathode composite materials from spent LIBs was systematically investigated after the materials were heat treated. The results show that aged anode and cathode materials from spent LIBs can be well separated from each other after a heating process in air at 400 degrees C and at which some of the PVDF binder remains intact. The underlying mechanism was investigated by X-ray photoelectron spectroscopy (XPS), contact angle measurements, and scanning transmission electron microscopy (STEM) coupled with energy-dispersive X-ray spectroscopy (EDX). The results from the XPS and contact angle measurements show that there is a hydrophilic and oxygen-rich layer on the surface of aged anode materials. This hydrophilic surface, associated with the solid electrolyte interface (SEI) layer, impacts the froth flotation process significantly. The results also show that both the SEI layers and PVDF binder residues on the surface are removed at 400 degrees C for an hour, restoring the hydrophobicity of the anode materials, which, in turn, benefits the separation of anode and cathode materials. The STEM/EDX elemental analysis data confirms that there are 20 nm-thick oxygen-rich SEI layers on the surfaces, which can be removed after a heating process. The present result illustrates the significance of the SEI layers in flotation separation of electrode materials and sheds new lights into the future development of the recycling processes for the separation of anode and cathode composite materials from spent Li-ion batteries.

25 ENERGY STORAGE↗
DOE OSTI2020

Epitaxial and Strong Support Interactions between Pt and LaFeO 3 Films Stabilize Pt Dispersion

The ability to stabilize very small Pt crystallites in supported-metal catalysts following harsh treatments is an important industrial problem. Herein, we demonstrate that Pt particles can be maintained in the 1- to 2-nm range following multiple oxidation and reduction cycles at 1073 K when the particles are supported on 0.5-nm LaFeO 3 films that have been deposited onto MgAl 2 O 4 using atomic layer deposition (ALD). Characterization by Scanning Transmission Electron Microscopy (STEM) suggest that, when the catalyst is oxidized at 1073 K, the Pt crystallites are oriented with respect to the underlying LaFeO 3 . X-Ray Absorption Spectroscopy (XAS) also shows evidence for changes in the Pt environment. CO-oxidation rates for the reduced catalyst remain unchanged after five redox cycles at 1073 K. Epitaxial growth of Pt clusters and the consequent strong metal-support interaction between Pt and LaFeO 3 are indicated to be prime reasons for the enhanced catalytic performances.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Stabilization of NbTe 3 , VTe 3 , and TiTe 3 via Nanotube Encapsulation

The structure of MX 3 transition metal trichalcogenides (TMTs, with M a transition metal and X a chalcogen) is typified by one-dimensional (1D) chains weakly bound together via van der Waals interactions. This structural motif is common across a range of M and X atoms (e.g. NbSe 3 , HfTe 3 , TaS 3 ), but not all M and X combinations are stable. We report here that three new members of the MX 3 family which are not stable in bulk, specifically NbTe 3 , VTe 3 , and TiTe 3 , can be synthesized in the few- to single-chain limit via nano-confined growth within the stabilizing cavity of multi-walled carbon nanotubes. Transmission electron microscopy (TEM) and atomic-resolution scanning transmission electron microscopy (STEM) reveal the chain-like nature and the detailed atomic structure. The synthesized materials exhibit behavior unique to few-chain quasi-1D structures, such as multi-chain spiraling and a trigonal anti-prismatic rocking distortion in the single-chain limit. Density functional theory (DFT) calculations provide insight into the crystal structure and stability of the materials, as well as their electronic structure.

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

Measuring and directing charge transfer in heterogenous catalysts

Abstract Precise control of charge transfer between catalyst nanoparticles and supports presents a unique opportunity to enhance the stability, activity, and selectivity of heterogeneous catalysts. While charge transfer is tunable using the atomic structure and chemistry of the catalyst-support interface, direct experimental evidence is missing for three-dimensional catalyst nanoparticles, primarily due to the lack of a high-resolution method that can probe and correlate both the charge distribution and atomic structure of catalyst/support interfaces in these structures. We demonstrate a robust scanning transmission electron microscopy (STEM) method that simultaneously visualizes the atomic-scale structure and sub-nanometer-scale charge distribution in heterogeneous catalysts using a model Au-catalyst/SrTiO 3 -support system. Using this method, we further reveal the atomic-scale mechanisms responsible for the highly active perimeter sites and demonstrate that the charge transfer behavior can be readily controlled using post-synthesis treatments. This methodology provides a blueprint for better understanding the role of charge transfer in catalyst stability and performance and facilitates the future development of highly active advanced catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Mending cracks atom-by-atom in rutile TiO2 with electron beam radiolysis

Abstract Rich electron-matter interactions fundamentally enable electron probe studies of materials such as scanning transmission electron microscopy (STEM). Inelastic interactions often result in structural modifications of the material, ultimately limiting the quality of electron probe measurements. However, atomistic mechanisms of inelastic-scattering-driven transformations are difficult to characterize. Here, we report direct visualization of radiolysis-driven restructuring of rutile TiO 2 under electron beam irradiation. Using annular dark field imaging and electron energy-loss spectroscopy signals, STEM probes revealed the progressive filling of atomically sharp nanometer-wide cracks with striking atomic resolution detail. STEM probes of varying beam energy and precisely controlled electron dose were found to constructively restructure rutile TiO 2 according to a quantified radiolytic mechanism. Based on direct experimental observation, a “two-step rolling” model of mobile octahedral building blocks enabling radiolysis-driven atomic migration is introduced. Such controlled electron beam-induced radiolytic restructuring can be used to engineer novel nanostructures atom-by-atom.

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

Complexions at the iron-magnetite interface

Synthesizing distinct phases and controlling crystalline defects are key concepts in materials design. These approaches are often decoupled, with the former grounded in equilibrium thermodynamics and the latter in nonequilibrium kinetics. By unifying them through defect phase diagrams, we can apply phase equilibrium models to thermodynamically evaluate defects—including dislocations, grain boundaries, and phase boundaries—establishing a theoretical framework linking material imperfections to properties. Using scanning transmission electron microscopy (STEM) with differential phase contrast (DPC) imaging, we achieve the simultaneous imaging of heavy Fe and light O atoms, precisely mapping the atomic structure and chemical composition at the iron-magnetite (Fe/Fe 3 O 4 ) interface. We identify a well-ordered two-layer interface-stabilized phase state (referred to as complexion) at the Fe[001]/Fe 3 O 4 [001] interface. Using density-functional theory (DFT), we explain the observed complexion and map out various interface-stabilized phases as a function of the O chemical potential. The formation of complexions increases interface adhesion by 20% and alters charge transfer between adjacent materials, impacting transport properties. Our findings highlight the potential of tunable defect-stabilized phase states as a degree of freedom in materials design, enabling optimized corrosion protection, catalysis, and redox-driven phase transitions, with applications in materials sustainability, efficient energy conversion, and green steel production.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Vacancy-induced suppression of charge density wave order and its impact on magnetic order in kagome antiferromagnet FeGe

Two-dimensional (2D) kagome lattice metals are interesting because their corner sharing triangle structure enables a wide array of electronic and magnetic phenomena. Recently, post-growth annealing is shown to both suppress charge density wave (CDW) order and establish long-range CDW with the ability to cycle between states repeatedly in the kagome antiferromagnet FeGe. Here we perform transport, neutron scattering, scanning transmission electron microscopy (STEM), and muon spin rotation (μSR) experiments to unveil the microscopic mechanism of the annealing process and its impact on magneto-transport, CDW, and magnetism in FeGe. Annealing at 560 °C creates uniformly distributed Ge vacancies, preventing the formation of Ge-Ge dimers and thus CDW, while 320 °C annealing concentrates vacancies into stoichiometric FeGe regions with long-range CDW. The presence of CDW order greatly affects the anomalous Hall effect, incommensurate magnetic order, and spin-lattice coupling in FeGe, placing FeGe as the only kagome lattice material with tunable CDW and magnetic order.

critical phenomena↗
DOE OSTI2021

Probing atomic-scale symmetry breaking by rotationally invariant machine learning of multidimensional electron scattering

Abstract The 4D scanning transmission electron microscopy (STEM) method maps the structure and functionality of solids on the atomic scale, yielding information-rich data sets describing the interatomic electric and magnetic fields, structural and electronic order parameters, and other symmetry breaking distortions. A critical bottleneck is the dearth of analytical tools that can reduce complex 4D-STEM data to physically relevant descriptors. We propose an approach for the systematic exploration of 4D-STEM data using rotationally invariant variational autoencoders (rrVAE), which disentangle the general rotation of the object from other latent representations. The implementation of purely rotational rrVAE is discussed as are applications to simulated data for graphene and zincblende structures. The rrVAE analysis of experimental 4D-STEM data of defects in graphene is illustrated and compared to the classical center-of-mass analysis. This approach is universal for probing symmetry-breaking phenomena in complex systems and can be implemented for a broad range of diffraction methods.

36 MATERIALS SCIENCE↗