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At least 1,081 records · Page 60
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Recent Developments in Revealing the Impact of Complex Metal Oxide Reconstruction on Catalysis

Surface reconstruction of complex metal oxides refers to the alterations of the topmost catalyst surface, relative to the bulk structure, following exposure to pretreatment or reaction conditions during heterogeneous catalysis. (1) This structural and electronic transformation may involve (1) changes of the exposed crystallographic facets, (2) changes in chemical composition, such as the enrichment of specific elements, and, (3) morphological variations, including surface roughness and defects (Scheme 1). Beyond relaxation, surface reconstruction here also encompasses disruptions to the periodicity of the sublayers and changes to its stoichiometry. This change significantly influences the chemical properties of the catalyst surface, such as redox sites, (2) acid/base pairs, hydroxyl groups, (3) and surface defects. Surface reconstruction occurs due to the thermodynamic drive to lower the surface energy of the catalyst under the surrounding environment (e.g., temperature, chemical potential of species present). In addition to the treatment or reaction conditions, the extent of reconstruction also depends on the elements in the metal oxide structure. For instance, annealing ABO 3 perovskites (SrTiO 3 , BaTiO 3 , and BaZrO 3 ) at high temperatures (500 °C) in O 2 has a very different impact on the A/B ratio at the surface (ranging from 0.9 to 2.5), depending on the identity of A and B. (4) Metal oxide surface reconstruction under an electric field and exposure to acidic and alkaline media has recently gained increased attention in electrocatalysis, such as in the oxygen evolution reaction (OER); (5,6) however, in this Viewpoint we focus on the impact of surface reconstruction on thermal catalysis, a critical enduring research theme with ongoing challenges. Here, we start showcasing approaches to characterize surface reconstruction at the topmost surface layer, such as low-energy ion scattering (LEIS), discussing advantages and limitations. Next, we connect characterization of surface reconstruction to site-specific kinetic analysis, enabled via steady-state isotopic transient kinetic analysis (SSITKA), and we express our viewpoint on building structure–performance relationships by deeply understanding reconstructed surfaces. Later, we comment on the potential of tuning surface reconstruction to enhance catalytic performance. Finally, we explore the interplay between surface reconstruction and the “intelligent behavior”.

alcohol conversion↗
DOE OSTI2018

Sensitivity of Surface Resistance to Trapped Flux in High-Purity Large-Grain Niobium

Surface resistance arising from trapped flux is experimentally measured, by which the sensitivity to trapped flux is derived. Measurements are carried out with single-cell L-band SRF cavities made of high-purity large-grain niobium materials, immersed in a uniform externally applied magnetic field generated by a solenoid with its axis overlapping the cavity axis. The surface resistance is found by using the standard technique for Q0 measurement and the customary G/Q0 analysis. Q0 values at a fixed low surface field are used. The trapped flux is found by measuring flux densities at a selected location using a single-axis fluxgate magnetometer attached to the cavity outer surface: Ba*[1-(Bsc-Bnc)/(Bsc0-Bnc)], where Ba is the applied external field, Bnc and Bsc is the local flux density measured just above and below Tc, respectively, during a field-cooling of the cavity and afterwards its Q0 is measured, Bsc0 is measured in a separate zero-field-cooling while the cavity being kept in the same location after turning on the identical applied field Ba at a temperature well below Tc . Several magnetometers are placed at various locations. It is found that the sensitivity to trapped flux in high-purity large-grain niobium to be 1.9 n?/µT on average. This is to be compared to 3-9 n?/µT in high purity fine-grain niobium and 10-50 n?/µT in nitrogen-doped high-purity niobium reported by other groups. We will discuss the measurement results as well as the measurement techniques.

Geng, Rongli↗
DOE OSTI2017

Energy Production Demonstrator and Material Testing Station optimization for Megawatt proton beams

A simulation study of the Energy Production Demonstrator (EPD) concept – a solid heavy metal target irradiated by GeV-range intense proton beams and producing more energy than consuming – is carried out. Neutron production, fission, energy deposition, energy gain, testing volume and helium production are simulated using the MARS15 code for tungsten, thorium, and natural uranium targets in the proton energy range 0.5–120 GeV. This study shows that the proton energy range of 2–4 GeV is optimal for both a nat U EPD and the tungsten-based testing station for proton accelerator facilities. Simulation-based conservative estimates not including breeding and fission of plutonium suggest the proton beam current sufficient to produce 1 GW of thermal output power with the nat U EPD while supplying a relatively small fraction of that power to operate the accelerator. The thermal analysis has been performed and has shown that the EPD with a parallel proton beam feeding the core has a potential problem due to a possible core meltdown. In conclusion, a scheme has been proposed with a beam steering on the outer surface of the target; its thermal analysis indicates that slicing the target in shorter parts and maintaining a temperature of 25 °C on their surfaces would to avoid the target meltdown.

43 PARTICLE ACCELERATORS↗
DOE OSTI2019

Effect of X-ray beam on the molecular–topological structure of the surface of kynar® polyvinylidene fluoride resin

Thermomechanical analysis of poly(vinylidene fluoride) (PVDF) film shows that, unlike the completely amorphous structure of the native polymer, after irradiation with X-rays, the weight fraction of the crystalline modification in the polymer is 0.5. The initial PVDF film had a linear thermal expansion coefficient of α 1 = 11.33х10 5 K -1 and a glass transition temperature of T g =256 K. An efficient conversion of the amorphous structures of the polymer pseudo-network into crystalline networks occurs under X-ray irradiation. The irradiated polymer exhibits amorphous ( T g =239 K) and crystalline topological blocks ( T m =385 K). The presence of polyenyl and alkyl radicals is found in the electron paramagnetic resonance (EPR) spectra of the irradiated polymer. Lines with a splitting of 3.3 m T can be observed at the edges of the EPR spectra, consistent with radical centers like -CF 2 -C • H-CF 2 - . At high doses of radiolysis, polyenyl radicals are the main observed radicals. The macromolecular chains contain all three (α, β, γ) morphologies of the polymer. The Raman spectra show that X-ray irradiation can lead to carbonization and the formation of unsaturated bonds. Electronic structure calculations were used to aid in the analysis of the observed spectra.

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

A Constrained Data Assimilation Algorithm Based on GSI Hybrid 3D-EnVar and Its Application

Abstract Data assimilation (DA) at mesoscales is important for severe weather forecasts, yet the techniques of data assimilation at this scale remain a challenge. This study introduces dynamical constraints in the Gridpoint Statistical Interpolation (GSI) three-dimensional ensemble variational (3D-EnVar) data assimilation algorithm to enable the use of high-resolution surface observations of precipitation to improve atmospheric analysis at mesoscales. The constraints use the conservations of mass and moisture. Mass constraint suppresses the unphysical high-frequency oscillation, while moisture conservation constrains the atmospheric states to conform with the observed high-resolution precipitation. We show that the constrained data assimilation (CDA) algorithm significantly reduced the spurious residuals of the mass and moisture budgets compared to the original data assimilation (ODA). A case study is presented for a squall line over the Southern Great Plains on 20 May 2011 during Midlatitude Continental Convective Clouds Experiment (MC3E) of the Atmospheric Radiation Measurement (ARM) program by using ODA or CDA analysis as initial condition of forecasts. The state variables, and the location and intensity of the squall line are better simulated in the CDA experiment. Results show how surface observation of precipitation can be used to improve atmospheric analysis through data assimilation by using the dynamical constraints of mass and moisture conservations.

Wang, Jia↗
DOE OSTI2022

Understanding the structure and composition of recalcitrant oligosaccharides in hydrolysate using high-throughput biotin-based glycome profiling and mass spectrometry

Novel Immunological and Mass Spectrometry Methods for Comprehensive Analysis of Recalcitrant Oligosaccharides in AFEX Pretreated Corn Stover. Lignocellulosic biomass is a sustainable alternative to fossil fuel and is extensively used for developing bio-based technologies to produce products such as food, feed, fuel, and chemicals. The key to these technologies is to develop cost competitive processes to convert complex carbohydrates present in plant cell wall to simple sugars such as glucose, xylose, and arabinose. Since lignocellulosic biomass is highly recalcitrant, it must undergo a combination of thermochemical treatment such as Ammonia Fiber Expansion (AFEX), dilute acid (DA), Ionic Liquid (IL) and biological treatment such as enzyme hydrolysis and microbial fermentation to produce desired products. However, when using commercial fungal enzymes during hydrolysis, only 75–85% of the soluble sugars generated are monomeric sugars, while the remaining 15–25% are soluble recalcitrant oligosaccharides that cannot be easily utilized by microorganisms. Previously, we successfully separated and purified the soluble recalcitrant oligosaccharides using a combination of charcoal and celite-based separation followed by size exclusion chromatography and studies their inhibitory properties on enzymes. We discovered that the oligosaccharides with higher degree of polymerization (DP) containing methylated uronic acid substitutions were more recalcitrant towards commercial enzyme mixtures than lower DP and neutral oligosaccharides. Here, we report the use of several complementary techniques that include glycome profiling using plant biomass glycan specific monoclonal antibodies (mAbs) to characterize sugar linkages in plant cell walls and enzymatic hydrolysate, matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) using structurally-informative diagnostic peaks offered by negative ion post-secondary decay spectra, gas chromatography followed by mass spectrometry (GC–MS) to characterize oligosaccharide sugar linkages with and without derivatization. Since oligosaccharides (DP 4–20) are small, it is challenging to mobilize these molecules for mAbs binding and characterization. To overcome this problem, we have applied a new biotin-coupling based oligosaccharide immobilization method that successfully tagged most of the low DP soluble oligosaccharides on to a micro-plate surface followed by specific linkage analysis using mAbs in a high-throughput system. This new approach will help develop more advanced versions of future high throughput glycome profiling methods that can be used to separate and characterize oligosaccharides present in biomarkers for diagnostic applications.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2017

Analysis of Te and TeO 2 on CdZnTe Nuclear Detectors Treated with Hydrogen Bromide and Ammonium-Based Solutions

Surface defects caused during cutting and polishing in the fabrication of cadmium zinc telluride (CdZnTe) nuclear detectors limit their spectral performance. Chemical treatments are often used to remove surface damages and defects. In this paper, we present the analysis of Te and TeO 2 species on the surfaces of CdZnTe nuclear detectors treated with hydrogen bromide and ammonium-based solutions. The CdZnTe wafers were chemo-mechanically polished in a mixture of hydrogen bromide in hydrogen peroxide and ethylene glycol, followed by a chemical passivation in a mixture of ammonium fluoride and hydrogen peroxide solution. X-ray photoelectron spectroscopy showed significant conversion of Te to TeO 2 , thus producing a more chemically stable surface. The resistivity of the CdZnTe samples is in the order of 1010 ohms-cm. The current for a given applied voltage increased following the passivation and decreased after a 3-hour period. Results from spectral response measurements showed that the 59.5-keV gamma-peak of Am-241 was stable under the same channel for the surface treatment processes.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Disentangling nonradiative recombination processes in Ge micro-crystals on Si substrates

We address nonradiative recombination pathways by leveraging surface passivation and dislocation management in μm-scale arrays of Ge crystals grown on deeply patterned Si substrates. The time decay photoluminescence (PL) at cryogenic temperatures discloses carrier lifetimes approaching 45 ns in band-gap engineered Ge micro-crystals. This investigation provides compelling information about the competitive interplay between the radiative band-edge transitions and the trapping of carriers by dislocations and free surfaces. Furthermore, an in-depth analysis of the temperature dependence of the PL, combined with capacitance data and finite difference time domain modeling, demonstrates the effectiveness of GeO{sub 2} in passivating the surface of Ge and thus in enhancing the room temperature PL emission.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

The Role of Subsurface Flow on Evapotranspiration: A Global Sensitivity Analysis

Abstract Water resources are impacted by water‐energy balance fluxes at the land surface, most notably evapotranspiration ( ET ), the largest component of surface energy balance. While integrated hydrologic models show promise in quantifying the nonlinear dynamics at this interface, the model results are plagued by parametric uncertainties. Given the high computational demand of running multiple parameter spaces of these models, little is known about how these uncertainties propagate into land surface processes. In this work, we perform a global sensitivity analysis by computing Sobol and AMAE indices using a surrogate model constructed with a polynomial chaos expansion to assess the impacts of the subsurface physical properties on ET . We do so by modeling a semisynthetic test case. Our results show that the effects of vertical hydraulic conductivity, porosity, and the water retention curve parameter Van Genuchten α mainly control ET . However, we note that while evaporation ( E ) shows behavior similar to the ET with high sensitivity to the parameters controlling the flow in the unsaturated zone, transpiration ( T ) is very sensitive to the saturated zone parameters and groundwater flow, especially during periods without rain. Our results also show that heterogeneities in land cover impact the flow in the saturated zone. Furthermore, our work demonstrates that reduced‐order models can be developed to make integrated models more accessible for rigorous sensitivity analyses and calibration purposes.

Maina, Fadji Zaouna↗
DOE OSTI2018

Molecule-Adsorbed Topological Insulator and Metal Surfaces: A Comparative First-Principles Study

We compare electronic structure characteristics of three different kinds of benzene-adsorbed (111) surfaces: that of Bi 2 Te 3 , a prototypical topological insulator, that of Au, a prototypical inert metal, and that of Pt, a prototypical catalytic metal. Using first-principles calculations based on dispersion-corrected density functional theory, we show that benzene is chemisorbed on Pt, but physisorbed on Au and Bi 2 Te 3 . Here, the adsorption on Bi 2 Te 3 is particularly weak, consistent with a minimal perturbation of the electronic structure at the surface of the topological insulator, revealed by a detailed analysis of the interaction of the molecular orbitals with the topological surface states.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Unraveling the Surface Termination and Evolution of Surface States for Electrocatalyst PtSn 4 in Alkaline HER

Semimetal PtSn 4 has been experimentally demonstrated as a promising topological electrocatalyst for the hydrogen evolution reaction (HER) under both acidic and alkaline conditions. While two possible mechanisms have been proposed to explain its activity, the role of its surface states in HER remains unclear. It is indeed in question how the surface states of this alloy evolve as HER proceeds. In this study, we investigate the surface termination that sustains conducting surface states on PtSn 4 , and we track their evolution during HER catalysis. We show that a reconstructed surface with a Sn-poor termination reproduces the scanning tunneling microscopy pattern observed in experiments and sustains a conducting surface. Through phase diagram and geometric structure analysis, we outline the HER profile following the Volmer–Heyrovsky mechanism. As hydrogen atoms adsorb onto the surface, the structure undergoes further reconstruction to an equilibrium phase with a coverage of two hydrides per unit cell. Meanwhile, the surface electronic bands evolve in response to interactions with the adsorbed hydrogen atoms. A hybridization diagram is further proposed for understanding the surface state evolution based on wave function and chemical bonding analyses. While the Pt atoms serve as conventional sites for hydrogen binding, the surface states of PtSn 4 are essential for stabilizing the hydrogen antibonding states via in-phase electronic interactions with the Sn components. This stabilization results in frontier surface bands that are responsible for driving the HER catalysis. Here, our findings provide a detailed description for the direct involvement of surface states on PtSn4 when employed as a catalyst for HER.

catalysts↗
DOE OSTI2016

Imprint control of BaTiO 3 thin films via chemically induced surface polarization pinning

Surface-adsorbed polar molecules can significantly alter the ferroelectric properties of oxide thin films. Thus, fundamental understanding and controlling the effect of surface adsorbates are crucial for the implementation of ferroelectric thin film devices, such as ferroelectric tunnel junctions. Herein, we report an imprint control of BaTiO 3 (BTO) thin films by chemically induced surface polarization pinning in the top few atomic layers of the water-exposed BTO films. Our studies based on synchrotron X-ray scattering and coherent Bragg rod analysis demonstrate that the chemically induced surface polarization is not switchable but reduces the polarization imprint and improves the bistability of ferroelectric phase in BTO tunnel junctions. Here, we conclude that the chemical treatment of ferroelectric thin films with polar molecules may serve as a simple yet powerful strategy to enhance functional properties of ferroelectric tunnel junctions for their practical applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Surface evolution of perfluoropolyether film at high speed quasi-contact conditions

Nanoscale analysis characterized by microscopy with atomic resolution demand that the targeted surface remains nearly static. Therefore, the interaction between two fast moving surfaces requires a unique methodology to capture its dynamics when contacts are of nominal area on the order of 100 μm{sup 2} but only a few angstroms in depth. We present a contact study of the head-disk interface in hard disk drives, which consists of a disk surface coated with a molecularly thin perfluoropolyether lubricant and a slider surface moving slightly separated from it with a relative velocity of 20 m/s and with 10 nm spacing. By investigating the slider dynamics and lubricant topography in-situ, we disclose that high-speed contact initiates when the slider shears the top surface of the lubricant. Such contact can pile up molecules a few angstroms high as “moguls” or annihilate existing ones through a 5–10 Å interference. The transitional spacing regime of mogul evolution is defined as “quasi-contact,” and it is the initial contact in the fast sliding interface.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2026

Reaction Optimization for Enzymatic Deconstruction of Industrially Relevant Nylon Composites

Plastics such as polyamides (PAs) possess unique physicochemical properties that make them indispensable in modern society. However, their energy‐intensive production and challenging end‐of‐life management highlight the urgent need for efficient recycling or remanufacturing solutions. Enzymatic depolymerization offers a promising route toward circular recycling, yet remains constrained by limited enzyme characterization, lack of validation under industrially relevant conditions and substrates, and overall performance. Here, we optimized the reaction conditions for three recently discovered nylon‐degrading enzymes. One of them, Nyl12, achieved product titers with PA6 and PA66 that exceed previously reported values, without enzyme engineering or substrate pretreatment. We further demonstrated the scalability of the process and its application to complex PA‐based materials used in microelectronic components. Analysis of substrate features, including surface area and particle size, revealed key parameters governing enzymatic activity and provided a framework for future pretreatment and process optimization efforts. In combination, these efforts provide a new benchmark for enzymatic nylon recycling.

nylon↗
DOE OSTI2020

Nitrate Radical Facilitates Indirect Benzyl Alcohol Oxidation on Bismuth(III) Vanadate Photoelectrodes

Bismuth(III) vanadate (BiVO 4 ) films show activity for direct benzyl alcohol (PhCH 2 OH) oxidation to benzaldehyde (PhCHO) in acetonitrile solvent. Introducing tetrabutylammonium nitrate (Bu 4 NNO 3 ) drastically reduces the overpotential required to generate the PhCHO product while maintaining a high faradaic efficiency (FE) >90%. BiVO 4 corrosion accompanies PhCH 2 OH oxidation. However, the presence of nitrate ions (NO 3 - ) results in significantly less bismuth- and vanadium-ion leaching (determined by ICP-MS analysis), as well as reduced surface roughening (determined by SEM imaging). In this reaction, it is proposed that rate-determining NO 3 - oxidation generates a highly reactive nitrate radical (NO 3 ∙) that reacts with PhCH 2 OH by hydrogen-atom abstraction (HAT). NO 3 - is stoichiometrically consumed by the irreversible formation of electrochemically inert HNO 3 , characterized by an EC i mechanism, rather than a catalytic EC' mechanism. In the presence of PhCH 2 OH, NO 3 - oxidation on BiVO 4 becomes more facile; every order of magnitude increase in PhCH 2 OH concentration shifts the NO 3 - / NO 3 ∙ equilibrium potential negatively by 200 mV. The shift results from the introduction of a consumption pathway for the nitrate radical intermediate via a coupled chemical step with benzyl alcohol. This report is the first example of photoelectrochemical NO 3 ∙ generation to initiate indirect PhCH 2 OH oxidation.

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

Degradation Diagnostics from the Subsurface of Lithium-Ion Battery Electrodes

Despite the long-established rocking-chair theory of lithium-ion batteries (LIBs), developing novel characterization methodology with higher spatiotemporal resolution facilitates a better understanding of the solid electrolyte interphase studies to shape the reaction mechanisms. In this work, we develop a Xenon ion plasma focused ion beam (Xe + PFIB)-based characterization technique to probe the cross-sectional interface of both ternary cathode and graphite anode electrodes, with the focus on revealing the chemical composition and distribution underneath the electrode surface by in-depth analysis of secondary ions. Particularly, the lithium fluoride is detected in the pristine cathode prior to contact with the electrolyte, reflecting that the electrode degradation is in the form of the loss of lithium inventory during electrode preparation. This degradation is related to the hydrolysis of the cathode material and the decomposition of the PVDF binder. Here, through the quantitative analysis of the transition-metal degradation products, manganese is found to be the dominant element in the newly formed inactive fluoride deposition on the cathode, while no transition metal signal can be found inside the anode electrode. These insights at high resolution implemented via a PFIB-based characterization technique not only enrich the understanding of the degradation mechanism in the LIBs but also identify and enable a high-sensitivity methodology to obtain the chemical survey at the subsurface, which will help remove the capacity-fade observed in most LIBs.

25 ENERGY STORAGE↗
DOE OSTI2017

Effect of Oxide Additives on Phase Evolution and Tribological Behavior of Zirconia-Toughened Alumina Composite

Four different zirconia-toughened alumina added with different pairs of oxides (CeO{sub 2}, TiO{sub 2}, CuO, ZnO and SnO{sub 2}) were prepared through the co-precipitation technique. Conventional sintering resulted in relative densities ≥96%. Phase analyses of these composites were performed by x-ray diffraction. Vicker’s hardness and tribological behavior of all ZTA composites were studied. Microstructure analysis of polished and worn surfaces was carried out to understand and correlate the mechanical/tribological behavior with the microstructure. A different wear mechanism is observed in ZTA containing CeO{sub 2} and TiO{sub 2} which resulted in considerable improvement in tribological behavior with a minimum specific wear rate of 9 × 10{sup −7} mm{sup 3}/Nm.

36 MATERIALS SCIENCE↗