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At least 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Binding and stability of MgO monomers on anatase TiO 2 (101)

In catalysis, MgO is often used to modify the acid-base properties of support oxides and to stabilize supported metal atoms and particles on oxides. In this study, we show how the sublimation of MgO powder can be used to deposit MgO monomers, hither on anatase TiO 2 (101). A combination of X-ray electron spectroscopy, high-resolution scanning tunneling microscopy, and density functional theory is employed to gain insight into the MgO monomer binding, electronic and vibrational properties, and thermal stability. In the most stable configuration, the Mg and O of the MgO monomer bind to two surface oxygens and one undercoordinated surface titanium, respectively. The additional binding weakens the Mg-O monomer bond and makes the Mg more ionic. The monomers are thermally stable up to 650 K, where the onset of diffusion into the TiO 2 bulk is observed. Finally, the monomeric MgO species on TiO 2 (101) represent an ideal, atomically precise system with modified acid-base properties and will be employed in our future catalytic studies.

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

Electrical and structural properties of binary Ga–Sb phase change memory alloys

Material properties of Ga–Sb binary alloy thin films deposited under ultra-high vacuum conditions were studied for analog phase change memory (PCM) applications. Crystallization of this alloy was shown to occur in the temperature range of 180–264 °C, with activation energy >2.5 eV depending on the composition. X-ray diffraction (XRD) studies showed phase separation upon crystallization into two phases, Ga-doped A7 antimony and cubic zinc-blende GaSb. Synchrotron in situ XRD analysis revealed that crystallization into the A7 phase is accompanied by Ga out-diffusion from the grains. X-ray absorption fine structure studies of the local structure of these alloys demonstrated a bond length decrease with a stable coordination number of 4 upon amorphous-to-crystalline phase transformation. Mushroom cell structures built with Ga–Sb alloys on ø110 nm TiN heater show a phase change material resistance switching behavior with resistance ratio >100 under electrical pulse measurements. TEM and Energy Dispersive Spectroscopy (EDS) studies of the Ga–Sb cells after ∼100 switching cycles revealed that partial SET or intermediate resistance states are attained by the variation of the grain size of the material as well as the Ga content in the A7 phase. A mechanism for a reversible composition control is proposed for analog cell performance. These results indicate that Te-free Ga–Sb binary alloys are potential candidates for analog PCM applications.

Ume, Rubab (ORCID:0000000324766900)↗
DOE OSTI2026

Nanodomain Formation and Temperature-Dependent Diffusion in Deep Eutectic Solvents Revealed by Single-Molecule Tracking

Deep eutectic solvents (DESs) are typically regarded as homogeneous liquids; however, recent work shows that many exhibit nanoscale structural heterogeneity. Most studies attribute these nanoscale features to short-range chemical interactions. It is still unclear whether a long-range physical mechanism also plays a role. Here, in this study, we examined the nanoscale structure in two hydrophobic DESs, 1:3 tetrabutylammonium bromide: l-menthol (DES-butyl) and 1:3 tetraoctylammonium bromide: l-menthol (DES-octyl). The notation 1:3 represents the molar ratio of the hydrogen bond acceptors to hydrogen bond donors used in the synthesis of the DESs. Single-molecule tracking (SMT) coupled with maximum entropy method (MEM) analysis was used to measure the number of diffusion populations of a dilute concentration of an added fluorescent probe. The presence of more than one population of diffusion coefficients indicates the existence of multiple local environments for the fluorescent probe (i.e., nanoscale structures in the DES). DES-butyl showed a relatively narrow diffusion coefficient distribution centered at 0.55 μm 2 /s, whereas DES-octyl displayed two distinct diffusing populations at 20 °C, with diffusion coefficients of 0.12 μm 2 /s and 0.53 μm 2 /s for the slow and fast populations, respectively. As DES-octyl was heated, the slow-diffusing population steadily diminished and disappeared above ∼30 °C, indicating that the nanodomains present at lower temperatures collapse as the liquid becomes more thermodynamically mixed. This temperature-dependent homogenization is consistent with a physical mechanism of nanostructure formation, for example, liquid–liquid phase separation (LLPS), wherein the structure is not driven solely by specific chemical interactions. The SMT-MEM results suggest that a long-range physical mechanism is the most plausible origin of the measured nanoscale structure in DES-octyl.

Opare-Addo, Jemima [Ames Laboratory (AMES), Ames, ↗
DOE OSTI2020

Manipulating the Geometric and Electronic Structures of Manganese Nitrides for Ammonia Synthesis

Abstract Manganese (Mn) nitrides are important nitrogen (N) carriers for small‐scale intermittent ammonia (NH 3 ) synthesis. However, only 3∼8 % of lattice N are converted into NH 3 . In this study, the geometric and electronic structures of well‐defined Mn 4 N and Mn 2 N lattices were altered using transition metal heteroatoms (Cr, Fe, Co, Ni, Mo) to understand the driving force behind lattice N diffusion and extraction. Density Functional Theory (DFT) revealed that the binding of early hydrogenation product (NH) follows a linear relationship with lattice N over a wide range of close‐packed surfaces. But, the binding of NH 2 and NH 3 are more sensitive to the geometric and electronic structures. Further, the chemical bonding can be quantitatively characterized with the covalency derived from Crystal Orbital Hamiltonian Population (COHP). In the Eley Rideal‐Mars van Krevelan pathway, the overall NH 3 formation free energy ( ) and lattice N diffusion barrier ( ) are the respective thermodynamic and kinetic determining factors. Aided by a rate‐determining step (RDS) model, Mn 4 N modified with Fe, Co, Ni single‐atom dopants all show enhanced rates for NH 3 formation.

Shan, Nannan↗
DOE OSTI2022

Correlation between Interface Microstructure and Bond Strength of Al6061/Al6061 HIP-Bonded Plates for Fuel Cladding Application

The effects of hot isostatic pressing (HIP) processing parameters on microstructure and bond strength of Al6061/Al6061 plate interfaces were systemically investigated at the micro- and nanoscale. The HIP bonding of the two aluminum plates was performed at four temperatures: 350°C, 400°C, 450°C, and 560°C. The results reveal the formation of micron scaled Mg 2 Si precipitate and uniform nano scaled Mg 2 Al 2 O 5 oxide at the interface. The formation of Mg 2 Al 2 O 5 is closely associated with the fast bulk diffusion of Mg from the Al matrix to the amorphous Al 2 O 3 /Al interface and subsequent reaction between Mg and Al 2 O 3 . Finally, the highest and lowest bond strengths were observed in samples HIP bonded at 450°C and 350°C, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Superior performance enabled by supramolecular interactions in metal-organic cathode: the power of weak bonds

Metal–organic-based electrode materials are increasingly appealing because both metal and organic linker are capable of undergoing redox processes, thus offering a high specific capacity. High porosity which can be achieved by the rational design of these materials is generally perceived as one of the major criteria for high rate performance. However, while Li-ion transport may be possible, oftentimes the counteranions (e.g., PF 6 - ) and solvent molecules are co-inserted into the porous host lattice, potentially hindering Li-ion diffusion pathways. Here, in this study, we propose the concept of close-packed metal–organic cathode stabilized by multiple supramolecular interactions as a viable solution for exceptional electrochemical performance. This is illustrated in a modularly designed redox-active [CuL(Py) 2 ] n (LH 4 = 1,4-dicyano-2,3,5,6-tetrahydroxybenzene, Py = pyridine). The mechanistic studies and DFT calculations confirm that the supramolecular interactions between its close-packed chains are the key to the flexible host lattice which only allows desolvated Li + to intercalate, while these weak bonds also stabilize the inserted Li in the preferred hopping sites, creating optimal diffusion paths. The performance observed in this work is found to be among the best ever reported for metal–organic cathodes with a capacity as high as 255 mA h g -1 at 65 mA g -1 (0.25C) and a reversible capacity of 59 mA h g -1 at ~26 A g -1 (100C) corresponding to 81% retention after 1000 cycles. These findings reveal a potential new strategy towards metal–organic-based electrodes with high performance and enhanced cycling stability.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Investigating intermolecular interactions among CO 2 , water and PEEK-ionene membrane using cryo ToF-SIMS and isotopic labeling

Cryogenic time-of-flight secondary ion mass spectrometry (cryo ToF-SIMS) has emerged as a powerful tool for investigating molecular interactions, speciation, and dynamics in materials for CO 2 capture. In this study, we apply cryo ToF-SIMS to probe interactions between CO 2 , water, and PEEK-ionene membranes—a promising material for direct CO 2 capture due to its selectivity, durability, and efficiency. Despite this potential, the mechanisms governing CO 2 diffusion and the influence of water vapor on CO 2 behavior remain unclear. To address this, we loaded PEEK-ionene membranes with 13 CO 2 and D 2 O and employed cryo ToF-SIMS to visualize the 3D distribution of CO 2 and water within the membrane. While prior studies suggest that 13 CO 2 is absorbed under ambient conditions, our cryo ToF-SIMS analysis revealed no enhancement of the 13 C/ 12 C ratio, suggesting weak CO 2 -membrane interactions. As a result, CO 2 vaporizes even at low temperatures (−140°C) under vacuum conditions. In contrast, D 2 O displayed a relatively homogeneous distribution in the membrane, suggesting stronger water-membrane interactions via hydrogen bonding (18–20 kJ/mol). Interestingly, CO 2 was not detected in D 2 O-loaded membranes, indicating minimal interference from water vapor on CO 2 diffusion. As a comparison, the cryo ToF-SIMS data show that 13 CO 2 can readily react with a basic Na 2 CO 3 aqueous solution to form NaH 13 CO 3 . These findings demonstrate cryo ToF-SIMS as a critical technique for understanding gas-water-membrane interactions, offering insights for membrane functionalization to improve CO 2 capture efficiency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Mechanism of Metal Intercalation under Graphene through Small Vacancy Defects

Metal intercalation under graphene has attracted extensive experimental and theoretical research because of its capability to manipulate the electronic structure and properties of graphene. However, the pathways and mechanisms of intercalation are still not well understood. Here, we systematically investigate the intercalation process of metal atoms through graphene vacancies using first-principles calculations. We show that the energy barrier for metal atom penetration through the vacancies in graphene is small as long as the size of the vacancy is larger than a mono-vacancy. However, metal atoms are strongly bonded to the vacancy so that the detachment energy of a metal atom from the vacancy is extremely high. This inhibits the diffusion of the metal atom into the gallery beneath the surface to complete the intercalation process. On the other hand, our calculation results show that the detachment energy of a metal atom from a metal dimer at small vacancy defects is significantly reduced, making intercalation much easier. Therefore, the key step limiting the intercalation process is the detachment of the metal atoms from vacancy defects. This finding from our study provides useful insight into the defect-assisted intercalation mechanism.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

The role of water vapor during the synthesis of hydrogen doped In 2 O 3

Hydrogen-doped In 2 O 3 synthesized using magnetron sputtering or atomic layer deposition in the presence of water vapor has high transparency in the near infra-red region and mobility values that are almost three to four times of those in commercially used In 2 O 3 :Sn at a much lower carrier concentration. However, simple questions like what happens when water molecules enter In 2 O 3 or why the dominant charge carrier changes from an oxygen vacancy in In 2 O 3 :Sn to H + in In 2 O 3 are not clear. Using hybrid functional based density functional theory calculations, in this study we show that water molecules spontaneously split into H + and OH – . The H + interstitial bonds with an oxygen in In 2 O 3 , and the OH – interstitial occupies a vacant lattice site or is trapped by an oxygen vacancy. Thus, in agreement with experimental findings, our results suggest that the concentration of oxygen vacancies decreases as the partial pressure of water increases. The charge transition level, ϵ ( – / + ) , of a hydrogen interstitial and the Fermi level at which the formation energies of OH – and H + are equal lie above the conduction band minimum, suggesting that the H + interstitial has a lower formation energy. In addition, water molecules do not exhibit any propensity to form clusters, meaning that H + ions can diffuse and remain spatially separated from each other.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Conditional diffusion machine-learning framework for mapping valence electron distribution from convergent beam electron diffraction

Quantitative convergent beam electron diffraction (CBED) enables determination of aspherical valence electron distributions through refinement of low-order structure factors, which are highly sensitive to chemical bonding and charge density variations. However, conventional quantitative CBED (QCBED) requires solving a highly nonlinear inverse problem with many coupled parameters, and computationally intensive dynamical diffraction calculations, making it time-consuming and difficult to apply to complex systems. More broadly, reconstructing charge density and orbital electron distribution from diffraction data has long been a central challenge in both x-ray and electron crystallography. Here, in this study, we introduce an artificial-intelligence (AI)-based framework that replaces traditional refinement with a data-driven inverse solver. Using a large synthetic CBED dataset generated by Bloch-wave simulations, we train a conditional diffusion model to directly infer crystal structural parameters and multipole density formalism parameters, and hence valence electron distributions, from CBED patterns alone. By learning from forward simulations across realistic parameter space, the model effectively solves the inverse problem. Compared with direct regression approaches, the diffusion-based framework provides posterior parameter distributions for rigorous uncertainty quantification while preserving quantitative fidelity and reducing analysis time by orders of magnitude. By eliminating the need for external single-crystal x-ray diffraction data and complex nonlinear refinement, this approach enables practical, high-throughput, and in situ quantitative CBED, enabling real-time mapping of valence electron distributions and their correlation with functional responses in quantum and energy materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Discerning structure sensitivity of Ni-core Pd-shell nanoparticles for enhanced nitrite reduction

Denitrification using Pd-based catalysts converts N-oxyanions into harmless products. However, the metal cost and scarcity are barriers to application. In this work, we synthesize water-suspended, structure-controlled Ni-core/Pd-shell nanoparticles (Ni@Pd NPs) that show Pd-catalyzed nitrite (NO 2 − ) reduction catalysis promoted by Ni. The NPs immobilized on Al 2 O 3 (0.47 wt % Pd and 0.74 wt % Ni) have higher NH 4 + selectivity and higher catalytic activity than wet-impregnated Pd/Al 2 O 3 (1.0 wt % Pd), i.e., 315.4 vs. 132.1 Lg surface Pd −1 min −1 . X-ray photoelectron spectroscopy (XPS) and CO-diffuse reflectance infrared Fourier transform spectroscopy (CO-DRIFTS) analyses show that Ni increases Pd electron density, which is proposed to lower the bond dissociation energy barrier for nitric oxide surface intermediate. Low-coordinated Pd atoms correlate to high activity and low NH 4 + selectivity. Using CatCost software, we estimate Ni@Pd/Al 2 O 3 to have a ∼40% lower manufacturing cost compared to wet-impregnated Pd/Al 2 O 3 . This rationally designed catalyst illustrates how nickel promotes Pd catalysis and how Pd usage can be lowered for denitrification and other hydrogenation reactions.

CO-DRIFTS↗
DOE OSTI2024

Ternary Complexes of BiI 3 /CuI and SbI 3 /CuI with Tetrahydrothiophene

Reactions of BiI 3 /CuI mixtures with tetrahydrothiophene (THT) in toluene produce 2-D sheet networks BiCu 3 I 6 (THT) n (n = 2, 3, or 4), depending on reaction conditions. All three structures are based on BiI 6 octahedra, which share pairs of (μ 2 -I) 2 with Cu 3 (THT) n units. BiCu 3 I 6 (THT) 2 features Cu 2 (μ 2 -I) 2 rhombs with close Cu···Cu interactions and is accompanied by formation of the very complex HBi 3 Cu 12 I 22 (THT) 8 . Reactions of SbI 3 /CuI with THT in toluene produced a SbCu 3 I 6 (THT) 2 network shows Cu 3 (μ 2 -THT) 2 units, like its Bi congener, but Cu 6 (μ 2 -I) 6 barrels rather than rhombs. Isolated SbI 3 units are stacked above the Cu 6 I 6 barrels. A molecular compound, Sb 3 Cu 3 I 12 (THT) 6 consists of a face-sharing Sb 3 I 12 stack, in which the Cu-THT units are bonded in asymmetric fashion about the central SbI 6 . Metal-halide bonds were investigated via QTAIM and NLMO analyses, demonstrating that these bonds are largely ionic and occur between the Bi/Sb and I p orbitals. Hirshfeld analysis shows significant H···H and H···I interactions. Diffuse reflectance spectroscopy (DRS) reveals band edges for the Bi species of 1.71–1.82 eV, while those for the neutral Sb complexes are in the range of 1.94–2.06 eV. Mapping of the electronic structure via density of state calculations indicates population of antibonding Bi/Sb–I orbitals in the excited state.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

IDENTIFICATION OF ADSORBA TION OF ADSORBATE FT-IR BANDS USING IN-SI -IR BANDS USING IN-SITU TECHNIQUES: Pd SPECIATION AND ADSORPTION CHEMISTRY OF Pd-ZEOLITES FOR PASSIVE NOx ADSORPTION

To meet increasingly stringent automotive emissions standards, further improvements in catalytic converter design are necessary. Current automotive catalyst systems are effective at eliminating emission of nitrogen oxides (NOx) once the catalyst reaches operational temperature (~200 °C). NOx emitted at lower catalyst temperatures now comprises most of the NOx released during a typical test cycle. Referred to as “the cold start problem” this issue has come to the forefront of automotive catalyst development, as mitigating these emissions is necessary to further reduce automotive emissions. Passive NOx adsorbers present an appealing solution to the cold start problem, these being a class of materials that chemisorb exhaust components such as NOx, carbon monoxide (CO) and hydrocarbons at near-ambient temperatures, and then desorb these compounds once the downstream catalyst has reached operational temperature. An effective passive NOx adsorber must have several properties: high NOx adsorption at near-ambient temperatures, near-complete NOx desorption at temperatures within the operational range, high thermal stability, and resistance to automotive exhaust components at high temperatures. The potential environmental impact of such a system is substantial, as NOx emissions currently result in the formation of millions of tons of smog and acid rain each year. Pd-exchanged zeolites have shown promise for deployment as Passive NOx adsorbers, though much remains to be understood about their adsorption chemistry and deactivation. In-situ Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) provides a convenient probe of adsorbed species, most automotive exhaust components possessing IR-active chemical bonds. By examining the evolution of IR bands under various pretreatments and adsorbates, the overall Pd-speciation and adsorptive zeolite sites of each material can be characterized, and the identities of IR bands can be deduced. In this work, microreactor-MS analysis of the adsorption and desorption behavior of these materials was also examined, these results being coupled with in-situ DRIFTS temperature programmed desorption (TPD) to correlate desorption events with specific adsorbed species. A pair of zeolite frameworks of similar Si/Al ratio but differing pore size were examined, Beta zeolite (BEA) and Chabazite (CHA) representing a medium- and small-pore framework, respectively. The effect of Pd-loading on BEA was examined, as well as the various deactivation pathways and active sites of each material.

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

Microstructural Characteristics, Mechanical Properties, and Corrosion Behavior of Field-Assisted Diffusion Welded Alloy 617

This study investigated the microstructural characteristics, mechanical response, and corrosion resistance of Alloy 617 diffusion welded by electric field-assisted sintering (EFAS). The microstructure exhibited good grain boundary (GB) migration across the interface and flat interface in the samples bonded at different conditions. Graded grain size was observed, with grain coarsening being more significant near sample surface due to EFAS-induced temperature gradient. Tensile testing revealed that the specimens fractured in the matrix away from the interface. The peak strength of 807 MPa was obtained in the samples welded at 1000°C. The materials obtained at 1100°C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed the flat interfaces were less ductile compared to the matrix. The hardness reduced near sample surfaces due to enlarged grains induced by temperature gradient. The interfaces with GB migration exhibited improved corrosion resistance in molten salt compared to the flat interfaces.

36 - MATERIALS SCIENCE↗
DOE OSTI2025

Enhanced Interfacial Bonding of Graft Copolymers

To understand how thermoplastic welding strength can be tuned through chemical modifications and macromolecular topology, we combined coarse-grained molecular dynamics (MD) simulations with experimental validation. Our simulations examined the diffusion dynamics of both linear and graft polymers across representative interfaces, revealing that diffusion-controlled interdigitation follows a power law, with the exponent decreasing from 0.34 to 0.11 as grafting density increases from 7.5 to 196% (with side chains grafted to both sides of a monomer unit). The addition of side chains enhances welding efficiency, as dense bottlebrush polymers with high grafting density reach maximum rupture strength faster than linear polymers. However, their saturated rupture strength is lower. This observation is subsequently corroborated by experimental lap-shear tests comparing linear polyethylene with octene grafted polyethylene elastomers. Our MD simulations show that unlike linear polymers, where backbone entanglements dominate, the grafted side chains introduce mechanisms in addition to entanglement dilution. The rapid interdigitation of side chains creates a dense mesh of entropic van der Waals contacts, which can also enhance the film welding. Furthermore, our MD simulations reveal a brittle rupture behavior in linear and comb-like (mildly grafted) polymers, while bottlebrush (densely grafted) polymers display elastomeric behavior with a pronounced stress plateau prior to fracture. Our simulations deconvolute the influence of polymer topology on deformation behavior. The rate of polymer deformation becomes lower than the applied strain rate prior to rupture, and the onset of this deviation is progressively delayed from linear to bottlebrush polymers. This trend highlights the critical role of molecular architecture in governing the mechanical response. In conclusion, these results provide deeper insight into the underlying welding mechanisms of topological polymers and present a potential approach for mitigating the interface anisotropy that is inherent in advanced manufacturing techniques such as fused filament fabrication.

graft copolymers↗
DOE OSTI2020

Competition between Hückel’s Rule and Jahn–Teller Distortion in Small Carbon Rings: A Quantum Monte Carlo Study

Structural properties and energetics of carbon rings are studied with the diffusion Monte Carlo (DMC) method. Our DMC-based geometry optimization reveals that both polyynic C 4n and cumulenic C 4n+2 rings exhibit bond length alternations for n >= 3, which is understood to be due to Jahn-Teller distortions. The bond length alternation even in a cumulenic (4n + 2) carbon ring was experimentally observed in a recently synthesized C 18 molecule. From a comparison of the DMC cohesive energies of C 4n with those of C 4n + 2 , we present a comprehensive picture of the competition between Huckel's rule and Jahn-Teller distortion in small carbon rings; the former is more dominant than the latter for n < 5 where C 4n + 2 rings are more stable than C 4n , while C 4n rings are as stable as C 4n + 2 for n < 5 where dimerization effects due to Jahn-Teller distortion are more important.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Fast Proton Transfer and Hydrogen Evolution Reactivity Mediated by [Co 13 C 2 (CO) 24 ] 4–

A common approach to speeding up proton transfer (PT) by molecular catalysts is manipulation of the secondary coordina-tion sphere with proton relays and these enhance overall reaction rates by orders of magnitude. In contrast, heterogenous electrocatalysts have band structures that promote facile PT concerted with electron transfer (ET), known as the Volmer mechanism. Here in this paper, we show that [Co 13 C 2 (CO) 24 ] 4– , containing multiple Co-Co bonds to statistically enhance observed rates of PT, promotes PT on the order of 2.3 × 10 9 M -1 s -1 which suggests a diffusion-limited rate. The fast ET and PT chemistry is at-tributed to the delocalized electronic structure of [Co 13 C 2 (CO) 24 ] 4– . Electrochemical characterization of [Co 13 C 2 (CO) 24 ] 4– in the presence and absence of protons reveals ET kinetics and diffusion behavior similar to other small clusters such as nano-materials and fullerenes.

08 HYDROGEN↗