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DOE OSTI2022

Harvesting Planck radiation for free-space optical communications in the long-wave infrared band

We demonstrate a free-space optical communication link with an optical transmitter that harvests naturally occurring Planck radiation from a warm body and modulates the emitted intensity. The transmitter exploits an electro-thermo-optic effect in a multilayer graphene device that electrically controls the surface emissivity of the device resulting in control of the intensity of the emitted Planck radiation. We design an amplitude-modulated optical communication scheme and provide a link budget for communications data rate and range based on our experimental electro-optic characterization of the transmitter. Finally, we present an experimental demonstration achieving error-free communications at 100 bits per second over laboratory scales.

Weinstein, Haley A.↗

DOE OSTI2023

Discrepant trends in global land-surface and air temperatures controlled by vegetation biophysical feedbacks

Satellite-based land surface temperature (Ts) with continuous global coverage is increasingly used as a complementary measure for air temperature (Ta), yet whether they observe similar temporal trends remains unknown. Here, we systematically analyzed the trend of the difference between satellite-based Ts and station-based Ta (Ts–Ta) over 2003–2022. We found the global land warming rate inffered from Ts was on average 42.6% slower than that from Ta (Ts–Ta trend: -0.011 °C yr -1 , p = 0.06) during daytime of summer. This slower Ts-based warming was attributed to recent Earth greening, which effectively cooled canopy surface through enhancing evapotranspiration and turbulent heat transfer. However, Ts showed faster warming than Ta during summer nighttime (0.015 °C yr -1 , p < 0.01), winter daytime (0.0069 °C yr -1 , p = 0.08) and winter nighttime (0.0042 °C yr -1 , p = 0.16), when vegetation activity is limited by temperature and solar radiation. Our results indicate potential biases in assessments of atmospheric warming and the vegetation-air temperature feedbacks using satellite-observed surface temperature proxies.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Surface-Tailoring and Morphology Control as Strategies for Sustainable Development in Transport Sector

Surface wetting plays an important role in the corrosion protection processes of aerospace applications. Here, we demonstrate the use of ultrafast femtosecond (fs) laser processing techniques to tailor the wetting properties of aluminum (Al) substrates by creating diverse surface morphologies. Specifically, two distinct laser scanning methods—dot-hatching and cross-hatching—were employed to fabricate microstructures on the substrates. By varying the incident laser parameters, we confirmed that the resulting surface morphologies exhibit different wetting behaviors, spanning from hydrophilicity to hydrophobicity. Furthermore, time-resolved spreading tests validate that dynamic wetting behaviors can also be modified. This fs laser processing approach provides a straightforward, one-step fabrication method for effectively modifying the wetting properties of Al alloys.

de Almeida Prado, Luis Antonio Sanchez↗

DOE OSTI2025

CO 2 Adsorption and Hydrogenation on Inverse InO x /Cu(111) Catalysts: Active Role of the Oxide–Metal Interface

The direct conversion of carbon dioxide (CO 2 ) into methanol via hydrogenation is essential for industrial applications. Recent studies on catalysts that contain an inverse oxide/metal configuration have shown very good catalytic performance for the CO 2 hydrogenation to methanol process. Here, in this study, we investigated the behavior of indium oxide-Cu(111) interfaces under pure CO 2 and CO 2 /H 2 mixtures using synchrotron-based ambient-pressure X-ray photoelectron spectroscopy (AP-XPS). Initially, a single layer of copper oxide (Cu x O) was grown on the Cu(111) surface by controlled oxidation. On this surface, indium was deposited at room temperature. Oxygen atoms transferred from Cu x O/Cu(111) to the indium metal upon deposition, forming In-O-Cu bonds and active interfaces. Although Cu(111) is not very active for the binding and activation of CO 2 , the formed InO x -Cu(111) interfaces had no problem adsorbing and dissociating the molecule at room temperature. Reaction of CO 2 with H 2 on InO x -Cu(111) yielded surface-bound H 3 CO, CO 2 δ− , CO 3 , and CH x species that are typical intermediates in the production of methanol and other oxygenates. The InO x -Cu(111) interface underwent dynamic chemical changes under reaction conditions, forming In-Cu alloys at low indium coverages (< 0.05 monolayer), while at higher indium coverages a mixture of an In-Cu and InO x was detected in XPS. These findings indicate that InO x /In-Cu interfaces can play a key role in processes aimed at the trapping and valorization of CO 2 .

36 MATERIALS SCIENCE↗

DOE OSTI2021

Transformation of Highly Stable Pt Single Sites on Defect Engineered Ceria into Robust Pt Clusters for Vehicle Emission Control

Engineering surface defects on metal oxide supports could help promote the dispersion of active sites and catalytic performance of supported catalysts. Herein, a strategy of ZrO 2 doping was proposed to create rich surface defects on CeO 2 (CZO) and, with these defects, to improve Pt dispersion and enhance its affinity as single sites to the CZO support (Pt/CZO). The strongly anchored Pt single sites on CZO support were initially not efficient for catalytic oxidation of CO/C 3 H 6 . However, after a simple activation by H 2 reduction, the catalytic oxidation performance over Pt/CZO catalyst was significantly boosted and better than Pt/CeO 2 . Pt/CZO catalyst also exhibited much higher thermal stability. The structural evolution of Pt active sites by H 2 treatment was systematically investigated on aged Pt/CZO and Pt/CeO 2 catalysts. With H 2 reduction, ionic Pt single sites were transformed into active Pt clusters. Much smaller Pt clusters were created on CZO (ca. 1.2 nm) than on CeO 2 (ca. 1.8 nm) due to stronger Pt-CeO 2 interaction on aged Pt/CZO. Consequently, more exposed active Pt sites were obtained on the smaller clusters surrounded by more oxygen defects and Ce 3+ species, which directly translated to the higher catalytic oxidation performance of activated Pt/CZO catalyst in vehicle emission control applications.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Visual, Optical and Replica Inspections: Surface Preparation of 650 MHz NB Cavity for PIP-II Linac

Surface preparation of niobium superconducting RF cavities is a critical step for achieving good RF performance under the superconducting state. Surface defect, roughness, and contamination affect the accelerating gradient and quality factor of the cavities. We report surface inspection methods used to control the surface processing of 650 MHz cavities designated for the pre-production and prototype cryomodules for PIP-II linac. The cavity surface was routinely inspected visually, with an optical camera, and by microscopic scanning of surface replicas. This article covers details on the surface inspection methods and surface polishing process used to repair the surface.

43 PARTICLE ACCELERATORS↗

DOE OSTI2022

Toward controlling wetting hysteresis with nanostructured surfaces derived from block copolymer self-assembly

The synthesis of nanostructured surfaces via block copolymer (BCP) self-assembly enables a precise control of the surface feature shape within a range of dimensions of the order of tens of nanometers. Herein, this work studies how to exploit this ability to control the wetting hysteresis and liquid adhesion forces as the substrate undergoes chemical aging and changes in its intrinsic wettability. Via BCP self-assembly we fabricate nanostructured surfaces on silicon substrates with a hexagonal array of regular conical pillars having a fixed period (52 nm) and two different heights (60 and 200 nm), which results in substantially different lateral and top surface areas of the nanostructure. The wetting hysteresis of the fabricated surfaces is characterized using force–displacement measurements under quasistaic conditions and over sufficiently long periods of time for which the substrate chemistry and surface energy, characterized by the Young contact angle, varies significantly. The experimental results and theoretical analysis indicate that controlling the lateral and top area of the nanostructure not only controls the degree of wetting hysteresis but can also make the advancing and receding contact angles less susceptible to chemical aging. These results can help rationalize the design of nanostructured surfaces for different applications such as self-cleaning, enhanced heat transfer, and drag reduction in micro/nanofluidic devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2024

Goethite and Hematite Nucleation and Growth from Ferrihydrite: Effects of Oxyanion Surface Complexes

The presence of oxyanions, such as nitrate (NO 3 – ) and phosphate (PO 4 3– ), regulates the nucleation and growth of goethite (Gt) and hematite (Hm) during the transformation of ferrihydrite (Fh). Our previous studies showed that oxyanion surface complexes control the rate and pathway of Fh transformation to Gt and Hm. However, how oxyanion surface complexes control the mechanism of Gt and Hm nucleation and growth during the Fh transformation is still unclear. Here, we used synchrotron scattering methods and cryogenic transmission electron microscopy to investigate the effects of NO 3 – outer-sphere complexes and PO 4 3– inner-sphere complexes on the mechanism of Gt and Hm formation from Fh. Our TEM results indicated that Gt particles form through a two-step model in which Fh particles first transform to Gt nanoparticles and then crystallographically align and grow to larger particles by oriented attachment (OA). In contrast, for the formation of Hm, imaging shows that Fh particles first aggregate and then transform to Hm through interface nucleation. This is consistent with our X-ray scattering results, which demonstrate that NO 3 – outer-sphere and PO 4 3– inner-sphere complexes promote the formation of Gt and Hm, respectively. These results have implications for understanding the coupled interactions of oxyanions and iron oxy-hydroxides in Earth-surface environments.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Energy Surplus and an Atmosphere‐Land‐Surface “Tug of War” Control Future Evapotranspiration

Abstract The 21st century evapotranspiration (ET) trends over the continental U.S. are assessed using innovative, energy‐based principles. Annual ET is projected to increase with high confidence at the rate of 20 mm for every 1℃ of rise in near‐surface air temperature, or 0.45 or 0.98 mm/year/year, depending on the emission scenario. The ET trajectory is dominated (58%) by the increase of land‐surface net radiative energy. An enhancement of the fraction of energy taken up by ET becomes a more important controller (53%) in late 21st century, under the high emission scenario. This increase is explained by the “tug of war” between atmospheric vapor demand and land‐surface ability to supply water. An assessment of future water availability (precipitation minus ET) shows no significant changes at the continental scale. This outcome nevertheless hides strong spatial variability, emphasizing the role of ET in shaping the distribution of water availability among human populations.

Xu, Donghui↗

DOE OSTI2021

System and method for monitoring atomic absorption during a surface modification process

A processing system monitors and/or controls a surface modification process occurring on a substrate within a processing chamber. An optical processing module having a light emission submodule to output a generated light signal and an optical detection submodule to detect a resultant light signal, is connected via fiber optic cables to light illuminating and light receiving components located within the chamber. A processor determines an amount of atomic absorption by an atomic element encountered by a probing beam passing between the illuminating and receiving components, based on the intensity of the generated light signal, the intensity of the received light signal and optionally the spontaneous emission of the atomic element in the absence of illumination by a probing beam. Based on the determined amount, the system derives a plurality of parameters of the modified substrate, their spatial and temporal uniformity, and information about process conditions in the processing chamber.

Atanasoff, George↗

DOE OSTI2020

Control of single-ligand chemistry on thiolated Au 25 nanoclusters

Diverse methods have been developed to tailor the number of metal atoms in metal nanoclusters, but control of surface ligand number at a given cluster size is rare. Here we demonstrate that reversible addition and elimination of a single surface thiolate ligand (-SR) on gold nanoclusters can be realized, opening the door to precision ligand engineering on atomically precise nanoclusters. We find that oxidative etching of [Au 25 SR 18 ] – nanoclusters adds an excess thiolate ligand and generates a new species, [Au 25 SR 19 ] 0 . The addition reaction can be reversed by CO reduction of [Au 25 SR 19 ] 0 , leading back to [Au 25 SR 18 ] – and eliminating precisely one surface ligand. Intriguingly, we show that the ligand shell of Au 25 nanoclusters becomes more fragile and rigid after ligand addition. This reversible addition/elimination reaction of a single surface ligand on gold nanoclusters shows potential to precisely control the number of surface ligands and to explore new ligand space at each nuclearity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Pretreatment Effects on the Surface Chemistry of Small Oxygenates on Molybdenum Trioxide

Understanding surface reactions of biomass-derived oxygenates on metal oxides is important for designing catalysts for valorization of biomass. As such, This work elucidated the effect of different pretreatments on molybdenum trioxide (MoO 3 ) to understand how surface reactivity is controlled by the surface oxidation state. The catalyst was pretreated in oxidative, inert, and reducing environments. The inert and reducing pretreatments created oxygen vacancies on the catalyst surface that acted as active sites for the adsorption of oxygenated molecules, with the reducing pretreatment yielding a higher density of these active sites. Exposing the catalyst to an alcoholic solvent such as methanol also led to a partial reduction similar to the inert pretreatment. After pretreatment, the catalyst was exposed to ethanol, acetaldehyde, and crotonaldehyde with subsequent characterization by diffuse reflectance infrared spectroscopy (DRIFTS), temperature-programmed desorption (TPD), X-ray absorption near edge spectroscopy (XANES), and X-ray photoelectron spectroscopy (XPS). Density functional theory (DFT) was also used to determine adsorption configurations and energies of ethanol, acetaldehyde, and crotonaldehyde. Reduced surfaces were shown to have a stronger affinity for carbonyls, leading to a higher activity for the aldol condensation of acetaldehyde and ethanol to C 4 molecules. Catalysts pretreated in an oxidative environment were completely inactive toward chemisorption and reaction of acetaldehyde.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Switchable wetting of oxygen-evolving oxide catalysts

The surface wettability of catalysts is typically controlled via surface treatments that promote catalytic performance. Here we report on potential-regulated hydrophobicity/hydrophilicity at cobalt-based oxide interfaces with an alkaline solution. The switchable wetting of single particles, directly related to their activity and stability towards the oxygen evolution reaction, was revealed by electrochemical liquid-phase transmission electron microscopy. Analysis of the movement of the liquid in real time revealed distinctive wettability behaviour associated with specific potential ranges. At low potentials, an overall reduction of the hydrophobicity of the oxides was probed. Upon reversible reconstruction towards the surface oxyhydroxide phase, electrowetting was found to cause a change in the interfacial capacitance. At high potentials, the evolution of molecular oxygen, confirmed by operando electron energy-loss spectroscopy, was accompanied by a globally thinner liquid layer. This work directly links the physical wetting with the chemical oxygen evolution reaction of single particles, providing fundamental insights into solid–liquid interfacial interactions of oxygen-evolving oxides.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Toward High Efficiency Water Processed Organic Photovoltaics: Controlling the Nanoparticle Morphology with Surface Energies

Here efficient organic photovoltaic devices fabricated from water-based colloidal dispersions with donor:acceptor composite nanoparticles achieving up to 9.98% power conversion efficiency (PCE) are reported. This high efficiency for water processed organic solar cells is attributed to morphology control by surface energy matching between the donor and the acceptor materials. Indeed, due to a low interfacial energy between donor and the acceptor, no large phase separation occurs during the nanoparticle formation process as well as upon thermal annealing. Indeed, synchrotron-based scanning transmission X-ray microscopy reveals that the internal morphology of composite nanoparticles is intermixed as well as the active layer morphology after thermal treatment. The PCE of this system reaches 85% that of devices prepared from chlorinated solvent. The gap between water-based inks and organic solvent-based inks gets narrower, which is promising for the development of eco-friendly processing and fabrication of organic photovoltaics.

14 SOLAR ENERGY↗

DOE OSTI2020

Femtosecond photoemission electron microscopy of surface plasmon polariton beam steering via nanohole arrays

Directional control over surface plasmon polariton (SPP) waves is a prerequisite for the development of miniaturized optical circuitry. Here, the efficacy of single and dual component SPP steering elements is explored through photoemission electron microscopy. Our imaging scheme relies on two-color photoemission and counter-propagating SPP generation, which collectively allow SPPs to be visualized in real space. Wave-vector difference mixing between two-dimensional arrays of nanoholes and photon momenta enables SPP steering with directionality governed by the array lattice constant. The magnitude of grating momentum required to achieve counter-propagation guarantees efficient steering over the full range of the negative half-space. In our dual component configuration, separate SPP generation and Bragg diffraction based steering optics are employed. We find that array Bragg planes principally influence the SPP angles through the array band structure, which allows us to visualize both positive and negative refractory waves.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2020

Surface SiO 2 Thickness Controls Uniform-to-Localized Transition in Lithiation of Silicon Anodes for Lithium-Ion Batteries

Silicon is a promising anode material for lithium-ion batteries because of its high capacity, but its widespread adoption has been hampered by a low cycle life arising from mechanical failure and the absence of a stable solid–electrolyte interphase (SEI). Understanding SEI formation and its impact on cycle life is made more complex by the oxidation of silicon materials in air or during synthesis, which leads to SiO x coatings of varying thicknesses that form the true surface of the electrode. Here, the lithiation of SiO 2 -coated Si is studied in a controlled manner using SiO 2 coatings of different thicknesses grown on Si wafers via thermal oxidation. SiO 2 thickness has a profound effect on lithiation: below 2 nm, SEI formation followed by uniform lithiation occurs at positive voltages versus Li/Li + . Si lithiation is reversible, and SiO 2 lithiation is largely irreversible. Above 2 nm SiO 2 , voltammetric currents decrease exponentially with SiO 2 thickness. For 2–3 nm SiO 2 , SEI formation above 0.1 V is suppressed, but a hold at low or negative voltages can initiate charge transfer whereupon SEI formation and uniform lithiation occur. Cycling of Si anodes with an SiO 2 coating thinner than 3 nm occurs at high Coulombic efficiency (CE). If an SiO 2 coating is thicker than 3–4 nm, the behavior is totally different: lithiation at positive voltages is strongly inhibited, and lithiation occurs at poor CE and is highly localized at pinholes which grow over time. As they grow, lithiation becomes more facile and the CE increases. Pinhole growth is proposed to occur via rapid transport of Li along the SiO 2 /Si interface radially outward from an existing pinhole, followed by the lithiation of SiO 2 from the interface outward.

25 ENERGY STORAGE↗

DOE OSTI2024

Porosity in Sr 1-x Ca x FeO 3-δ oxygen carriers: The role of surface area and pretreatment on storage activity

Perovskite oxides have generated interest as robust, low-temperature oxygen carrier materials for a variety of clean energy applications, including chemical looping gasification and air separations. Methods to improve O 2 desorption kinetics are vital to allow these carriers to compete economically with traditional metal oxide carriers or cryogenic separations. In this report we investigated the cumulative roles that surface area, pretreatment, and elemental composition have on the oxygen storage properties of a state-of-the-art carrier system, Sr 1-x Ca x FeO 3-δ (x = 0.20, 0.25, 0.30) synthesized using multiple methods. Porous materials synthesized by the Pechini, or citrate, method had their surface area controlled using the synthesis temperature. The high surface area of the Sr 0.7 Ca 0.3 FeO 3-δ materials is most beneficial at low operating temperatures, such as 350 and 400 °C, as their reduction rates are twice as fast as those obtained with their bulk counterparts. These effects are observed at higher operating temperatures and within a single composition, but temperature tunability using variable Ca 2+ substitution in the Sr 1-x Ca x FeO 3-δ overshadows the improvements gained from higher surface areas. Additionally, we establish that pretreatment in N2 at an elevated temperature is necessary to enhance kinetics further. For maximum efficiency, pretreatment at the synthesis temperature is suggested for the Pechini method-synthesized systems, whereas 800 °C is adequate for bulk materials.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Frustrated Coulombic and Cation Size Effects on Nanoscale Boehmite Aggregation: A Tumbler Small- and Ultra-Small-Angle Neutron Scattering Study

To better understand the effects of solution chemistry on particle aggregation in the complex legacy tank wastes at the Hanford (WA) and Savannah River (SC) sites, we have performed a series of tumbler small- and ultra-small-angle neutron scattering experiments on 20 wt % solid slurries of nanoparticulate aluminum oxyhydroxide (boehmite) with M 1+ nitrates of various concentrations and radii. In this study, the solutes consisted of H, Li, Na, K, and Rb nitrates at 10 –5 , 10 –3 , 10 –1 , 2, and 4 molal (m) concentrations, as well as in pure H 2 O. Synthetic boehmite nanoparticles were used with a size range from ~20 to 30 nm. Tumbler cells were used to keep the solids from settling. Although particles initially form individual rhombohedral platelets, once placed in solution, they quickly form well-bonded stacks, primary aggregates, up to ~1500 Å long, and a second level of aggregates whose concentration and structure vary as a function of cation type and concentration. Aggregation generally increases with increased solute concentration and with cation radius up to a concentration somewhat above 10 –1 m, at which point the trend reverses. Primary aggregates become more rodlike and larger. The Kirkwood-like reversal probably reflects a change from Derjaguin–Landau–Verwey–Overbeek (DLVO)/Debye behavior controlled by surface chemistry to a frustrated Coulombic system controlled by the solution structure. These data suggest that an understanding of the effects of salt concentration and chemistry on nanoparticle aggregate structures provides useful physical insights into the microscopic origin of slurry rheology in the Hanford and Savannah River legacy wastes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗