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DOE OSTI2025

In Situ/Operando Probing of Dynamic Phase Structures of Alumina‐Supported Ultrasmall Copper‐Gold Alloy Nanoparticles Under Reaction Conditions

Abstract The ability to control phase structures and surface sites of ultrasmall alloy nanoparticles under reaction conditions is essential for preparing catalysts by design. This is, however, challenging due to limited understanding of the atomic‐scale phases and their correlation with the ensemble‐averaged structures and activities of catalysts during catalytic reactions. We reveal here a dynamic structural stability of alumina‐supported ultrasmall and equiatomic copper‐gold alloy nanoparticles under reaction conditions as a model system in the in situ/operando study. In situ atomic‐scale morphological tracking under oxygen reveals temperature‐dependent dynamic crystalline‐amorphous dual‐phase structures, showing dynamic stability over an elevated temperature range. This atomic‐scale dynamic phase stability coincides with a “conversion plateau” observed for carbon monoxide oxidation on the catalyst. It is substantiated by the stable lattice ordering/disordering structures and surface sites with oscillatory characteristics shown by operando ensemble‐average structural tracking of the catalyst during the oxidation reaction. The understanding of the atomic‐scale dynamic phase structures in correlation with the ensemble‐average dynamic ordering/disordering phase structures and surface sites provides fresh insights into the unique synergy of the supported alloy nanoparticles. This understanding has implications for the design and structural tuning of active and stable ultrasmall alloy catalysts under elevated temperatures.

Chemistry↗

DOE OSTI2025

Chemical and Chemical-Mechanical Polishing of Surface Roughness on L-PBF/GRCop-42 Cu-Cr-Nb Additive Manufactured 10-GHz RF Structures

Laser-based powder bed fusion (L-PBF) allows additive manufacture (AM) of lower hybrid current drive (LHCD) radio-frequency (RF) launchers from Glenn Research Copper, a Cr 2 Nb precipitation-hardened alloy (GRCop-42) in configurations unachievable with conventional machining. Rough surfaces in AM components increase RF losses and lead to arcing in high-power vacuum RF applications. Chemical polishing, chemical-mechanical polishing, or a combination of both were utilized to planarize the internal surfaces of RF structures, resulting in surface roughness as low as R a = 0.2 µm. Refinement in polishing techniques now enables GRCop-42 alloys (4 at. % Cr, 2 at. % Nb) to achieve similar surface roughness to GRCop-84 (8 at. % Cr, 4 at. % Nb) and equivalent cavity losses to extruded oxygen-free copper waveguides at 10 GHz.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1991

Analysis of surfaces from the LDEF A0114, phase 4

Progress made from 1 Mar. to 31 Aug. 1991 is presented. The work concentrated on profilometry measurements of eroded and corroded sample surfaces, optical transmission measurements, analysis of the pinhole camera, and x-ray photoelectron spectroscopic (XPS) analysis of some samples. The following papers are presented: (1) observation of Be-7 on the surface of the Long Duration Exposure Facility (LDEF) Spacecraft; (2) measurement of the passive attitude control performance of a recovered spacecraft; (3) effects on LDEF exposed copper flim and bulk; (4) measurements of erosion characteristics for metal and polymer surfaces using profilometry; (5) the interactions of atmospheric cosmogenic radionuclides with spacecraft surfaces; (6) pinhole cameras as sensors for atomic oxygen in orbit; and (7) interaction of atomic oxygen with solid surfaces in low earth orbit- results from LDEF experiment A0114.

Gregory, John C.↗

NASA NTRS2004

Enhanced Boiling on Micro-Configured Composite Surfaces Under Microgravity Conditions

Two experimental setups: High Heat Flux Pool Boiling Setup and Optical system of Measuring Contact Angle and Spreading Parameters were established and a series of experiments was conducted. The experimental work on the nucleate boiling performance of both Freon-113 and water on the composite surfaces has been finished and the results show that the composite surface with 25% volume fraction of graphite fibers in the copper matrix has the best enhancing performance. Stronger enhancement was obtained for water compared to Freon-113. The wall superheat initiating boiling was reduced 40% and 35% and the heat flux of the nucleate boiling was augmented up to ten times and 6.7 times, respectively. A bubble departure model has been presented to explain the enhancement mechanism of the boiling heat transfer on the composite surfaces. A powerful optical method to measure contact angle and spreading parameters of liquids on solid surfaces, including both transparent and non-transparent substrates, has been developed and successfully used in the measurements for various liquid-solid systems. The experimental work on identification of profiles near three-phase line by laser shadowgraphy method has been finished and the characteristics of the three-phase line for different liquid-solid systems were unveiled, which is very important to understand the mechanism of boiling under microgravity conditions. The four basic patterns of sessile profile were discovered through caustics and caustic-diffraction analysis by applying wave theory in shadowgraphy technology, which contributes to clearly explain the different characteristics of wetting and spreading of various liquids on a solid surface, and therefore to further understand the bubble departure mechanisms. A new working pattern of heat pipes using working fluids with positive surface-tension gradient against temperature was discovered and analyzed, and then the new heat pipe systems using this kind of working fluids have been presented. Two patent devices, i.e. Shadowgraphic Method to Measure Properties of Sessile Drops and Heat Pipe Systems Using New Working Fluids, have been developed; the former has been approved by The United States Patent & Trademark Office and the latter is being examined.

Source record↗

DOE OSTI2021

Flexible Fabric-Based IDC Sensors for Conformal Curved Surface Applications

Interdigital capacitor (IDC) sensors are attractive in-situ sensors that can be used to measure permittivity variations in materials. Such sensors could be powerful enablers for cable insulation aging detection. Since insulation aging is correlated with a change in its material permittivity an IDC can measure that change via its measured capacitance. A new thin, flexible fabric-based IDC sensor is introduced for application on conformal curved surfaces such as an electrical cable surface. A multielectrode IDC and its backplane were fabricated using conductive copper polyester taffeta fabrics that were adhesively bonded to nonconductive polyester fabric. The sensor because of its soft flexible structure eliminates the problem of sensor conductor damage which is common for printed circuit board (PCB) type sensors when conformed to the surface of a cable. It also significantly reduces the airgap between the electrodes and the surface that they must contact in order to measure the capacitance. Airgap reduction and consistency are important in order to accurately predict permittivity variations in cable insulation material due to aging. Both PCB-based sensors and the new fabric-based sensors were built and tested on unaged cables and cables that underwent accelerated aging. Results demonstrate the proposed advantages of the novel fabric-based IDC sensor.

interdigital capacitor sensor, IDC, NDE, PCB senso↗

NASA NTRS1999

Flow Trajectories in Friction Stir Welding

In the Friction Stir Welding (FSW) process, a rotating, shouldered tool with a threaded pin is inserted under pressure along the seam of two pieces of metal which are tightly clamped together, and secured against a rigid anvil underneath. The rotating pin travels along the seam and through a combination of pressure and friction heating produces a zone of plastic deformation around the pin within the workpiece on either side of the seam. As the pin is moved in the direction of welding, the plasticised material moves around the tool and bonds together behind it. The elements of the material flow behavior are a combination of three elements. There is a rotational transport of material being carried around the tool, extrusion of material being forced around the pin on both sides into the cavity created behind it, and a lifting and dropping of material as it is stirred and mixed by the rotating action of the pin. It was assumed that rotational motion of the plastic zone is the primary mechanism for transport of material around the welding tool. A kinematic mathematical model was used to compute trajectories of material movement for various distributions of rotational slip within the plastic zone. These trajectories were then compared with the results of an experiment that produced radiographs of markers embedded in a workpiece that was welded with the FSW process. It was assumed that the copper wire markers retained their original length as the aluminum material flowed around them. The kinematic model included a constraint so that the displacements were such that the total length of the wire markers did not increase after deformation. There was good agreement between the calculated trajectories for the case of localized slip at the outer surface of the plastic deformation zone and the radiographs of the copper wire markers. The trajectories differed markedly from the radiograph traces when a distributed slip zone was assumed. It was concluded that the flow field could be described generally by a rotating plug model with slip occurring on the surface at the outer boundary of the plastic zone.

Bernstein, Edward L.↗

NASA NTRS1991

High temperature superconductor analog electronics for millimeter-wavelength communications

The performance of high temperature superconductor (HTS) passive microwave circuits up to X-band was encouraging when compared to their metallic counterparts. The extremely low surface resistance of HTS films up to about 10 GHz enables a reduction in loss by as much as 100 times compared to copper when both materials are kept at about 77 K. However, a superconductor's surface resistance varies in proportion to the frequency squared. Consequently, the potential benefit of HTS materials to millimeter-wave communications requires careful analysis. A simple ring resonator was used to evaluate microstrip losses at Ka-band. Additional promising components were investigated such as antennas and phase shifters. Prospects for HTS to favorable impact millimeter-wave communications systems are discussed.

Romanofsky, R. R.↗

NASA NTRS1991

High temperature superconductor analog electronics for millimeter-wavelength communications

Romanofsky, R. R.↗

NASA NTRS1976

The use of ERTS/LANDSAT imagery in relation to airborne remote sensing for terrain analysis in western Queensland, Australia

The author has identified the following significant results. Distinctive spectral signatures were found associated with areas of near surface bedrock with covered ground east of Dugald River and along the Thorntonia River valley west of Lady Annie. Linears identified in the Dugald River area on LANDSAT 2 imagery taken in March and July 1975 over the Cloncurry-Dobbyn area, displayed preferred orientation. A linear group with NE-SW orientation was identified in the Lady Annie area. In this area, the copper mineralization in the Mt. Kelly area occurs along a well marked linear with NNW/SSE direction apparent on images for March, September, and November 1975. Geobotanical anomalies provided surface expression of the copper deposits in Mt. Kelley.

Cole, M. M.↗

DOE OSTI2024

Nanocomposite Materials for Radionuclide Sequestration from Groundwater Environments

The half-lives of radionuclides range from fractions of a second to billions of years. Since no practical method of altering radioactive decay exists, and since exposure to either the energy emitted from radioactive decay or chemical properties of radionuclides poses dire health risks, radioactive materials must be segregated and controlled. The capture, treatment, and disposition of radioactive materials remain an extraordinary challenge. In here, we focus our attention on the synthesis and characterization of a unique class of nanocomposite materials that have potential for removal of radionuclide contamination. Specifically, we report a simple approach to decorate the surface of iron-based (Fe/FexOy) material with various nano-catalysts. Specifically, copper (Cu), tin (Sn), and silver (Ag) nanoparticles were prepared through two different reduction approaches, namely, citrate and cetyltrimethylammonium bromide (CTAB) methods, on the iron-based material surface. All samples were characterized by a variety of analytical tools, which included scanning electron microscopy (SEM), electron-dispersive X-ray microanalysis (EDS), and EDS mapping to elucidate materials’ morphology as well as nano-catalysts’ loading and location on the iron-based structures.

Hunyadi Murph, Simona E.↗

NASA NTRS2022

Un-Numbered Operational Areas PRL 229 Railroad Tie Disposal Area Pond Confirmation Sampling Report

This Confirmatory Sampling (CS) Report (CSR) was prepared for the National Aeronautics and Space Administration (NASA), Kennedy Space Center (KSC), Florida in accordance with the CS Work Plan (CSWP) (HGL, 2022a). The CSR summarizes investigation activities performed on the Railroad Tie Disposal Area (RTDA) of the Un-Numbered Operational Areas (UNOA), Potential Release Location (PRL) 229 located at KSC. HydroGeoLogic, Inc. (HGL) prepared this report under Contract Number 80KSC019D0012. The purpose of the CSR is to provide information to evaluate the level of potential contamination in surface water and sediment samples collected from the RTDA PRL 229 Pond and determine if contaminants pose unacceptable risks to ecological receptors. The CSR provides analytical data of 10 sets of surface water and sediment samples collected in 2021. Surface water samples were analyzed for volatile organic compounds (VOCs), semi-volatile organic compounds (SVOCs), polynuclear aromatic hydrocarbon (PAHs), metals, hardness, and salinity, while sediment samples were analyzed for metals, total organic carbon (TOC), SVOCs, PAHs, and total petroleum hydrocarbons (TPH). The CSR includes a Screening Level Ecological Risk Assessment (SLERA) conducted under KSC’s Resource Conservation and Recovery Act (RCRA) Corrective Action Program to determine if unacceptable risks to ecological receptors exist at PRL 229 Pond. Metals and PAHs were detected in surface water samples, including detections of antimony, arsenic, barium, calcium, copper, lead, magnesium, thallium, zinc, anthracene, benzo(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, benzo(g,h,i)perylene, benzo(k)fluoranthene, chrysene, dibenzo(a,h)anthracene, fluoranthene, indeno(1,2,3-c,d)pyrene and pyrene. Based on measured salinity (1.03 to 1.21 parts per thousand), the pond was identified as freshwater. Sediment analytical results also contained detections of metals and PAHs, including antimony, arsenic, barium, beryllium, cadmium, chromium, copper, lead, mercury, nickel, selenium, thallium, zinc, anthracene benzo(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, benzo(g,h,i)perylene, benzo(k)fluoranthene, chrysene, dibenzo(a,h)anthracene, fluoranthene, indeno(1,2,3-c,d)pyrene and pyrene. Potential risks to ecological receptors were evaluated in accordance with the SLERA Work Plan and the Decision Process Document for the Resource Conservation and Recovery Act (RCRA) Corrective Action Program at KSC (DPD) (Geosyntec, 2019), and using the 2021 sediment and surface water analytical results. Potential ecological receptors evaluated in the SLERA include the aquatic community, benthic invertebrates, aquatic birds, and aquatic mammals. The SLERA included Steps 2a through 2c of the Ecological Risk Assessment (ERA) process in accordance with the DPD. Using multiple lines of evidence, the SLERA concluded that many of the detected analytes are present at concentrations similar to those in background or reference locations at KSC, and/or at concentrations that would not pose a significant risk to ecological communities. There are no screening values available for the avian community, and PAHs are bioaccumulative compounds. For this reason, food web modeling was completed as a supplement to Step 2c to provide a quantitative evaluation of this exposure pathway. Food web modeling indicates that PAHs are unlikely to pose a risk to birds exposed to site sediment and surface water. Based on the results of the SLERA, the contaminants in sediment and surface water pose no to minimal risk to the ecological communities that could live or forage at the site. Based on the results of the SLERA, no further study is recommended for the RTDA Pond at PRL 229.

Confirmation Sampling↗

NASA NTRS1973

Texturing in metals as a result of sliding

Sliding friction experiments were conducted with copper, nickel, iron, and cobalt sliding on themselves in air and argon. The resulting wear surfaces were examined with X-ray analysis to determine if surface texturing had occurred as a result of sliding. Results of the investigation indicate that, for the face-centered-cubic metals copper and nickel, a (111) texture develops with the (111) planes tilted 10 deg in the direction of sliding. The body-centered-cubic metal iron exhibited a (110) texture with the (100) direction oriented in the direction of sliding. It also exhibited a 10 deg tilt in the direction of sliding. The environment influenced the results in that the degree of texture observed in argon was less than that seen in air for iron. No texturing was observed for the close-packed-hexagonal metal cobalt. Recrystallization was observed with copper as a result of sliding.

Wheeler, D. R.↗

NASA NTRS1975

Texturing in metals as a result of sliding

Sliding friction experiments were conducted with copper, nickel, iron and cobalt sliding on themselves in air and argon. The resulting wear surfaces were examined by X-ray analysis to determine if surface texturing had occurred as a result of sliding. Results of the investigation indicate that, for the face-centered-cubic metals copper and nickel, a (111) texture develops with the (111) planes tilted 10 deg in the direction of sliding. The body-centered-cubic metal iron exhibited a (110) texture with the (111) direction oriented in the direction of sliding. It also exhibited a 10 deg tilt in the direction of sliding. The environment influenced the results in that the degree of texture observed in argon was less than that seen in air for iron. No texturing was observed for the close-packed-hexagonal metal cobalt. Recrystallization was observed with copper as a result of sliding.

Wheeler, D. R.↗

DOE OSTI2025

Investigating the Effects of Copper Impurity Deposition on the Structure and Electrochemical Behavior of Hydrogen Evolution Electrocatalyst Materials

Electrolysis of impure water (such as seawater) has recently garnered research interest as it may enable hydrogen production at reduced costs. However, the tendency of impurity ions and other species to degrade electrocatalysts and membranes within an electrolyzer is a serious challenge. Here, we investigate the effects of copper impurities of varying concentrations on the hydrogen evolution reaction (HER) using platinum electrocatalysts. A decrease of current density is observed with an increasing copper concentration. By comparing the effect of ionic impurities on current density at different concentrations, we gain insight into how impurities can interfere with the HER at different potentials. Surface characterization of the electrodes reveals differences in the morphology and extent of copper deposition on HER-active platinum vs inactive gold electrodes. This enables an improved understanding of how copper nucleates and grows on the two types of electrodes under different electrochemical conditions while also confirming deposition in low-concentration cases, as present in seawater. The results indicate that copper electrodeposition competes with the HER, and the nature of copper electrodeposition varies depending on the electrocatalytic activity of the electrode. This study provides insight toward catalyst design that can withstand the effects of impurity-induced degradation over extended use.

08 HYDROGEN↗

DOE OSTI2024

Pseudocapacitance Facilitates the Electrocatalytic Reduction of Carbon Dioxide

Electroreduction of CO 2 to value-added products is a promising strategy for CO 2 reuse, where copper has a unique ability to produce oxygenates and C 2+ products. Unfortunately, the electronic factors making copper so unique are unknown, which limits the ability to design improved catalysts. By combining in situ surface-sensitive X-ray resonant photoelectron spectroscopy with density functional theory calculations, the complex electronic structure of copper is uncovered during the electrocatalytic reduction of CO 2 . It is found that the pseudocapacitive charging of copper, produced by the incorporation of protons and electrons into the subsurface, facilitates the activation of CO 2 , while simultaneously increasing the barrier for H-H coupling. The net result is that cathodic pseudocapacitive charge suppresses the hydrogen evolution reaction and promotes the production of hydrocarbons and oxygenated products on copper. These results represent a new paradigm in the understanding of CO 2 reduction, highlighting the key role of pseudocapacitive charge in the reaction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1978

Secondary electron emission properties of conducting surfaces for use in multistage depressed collectors

An Auger spectrometer in ultrahigh vacuum was used to measure the secondary emission properties of a number of candidate collector-materials including beryllium, carbon, (soot and pyrolytic graphite), copper, titanium carbide and tantalum. The advantage of the technique used is that the surface chemical constituents could be determined just before the secondary emission characteristics of the surface were measured. Pyrolytic graphite roughened by sputter etching showed the most favorable results for depressed collector use.

Forman, R.↗

NASA NTRS1978

Braze alloy spreading on steel

Scanning electron microscopy (SEM) and Auger electron microscopy (AEM) were employed to observe elemental surface decomposition resulting from the brazing of a copper-treated steel. Two types of steel were used for the study, stainless steel (treated with a eutectic silver-copper alloy), and low-carbon steel (treated with pure copper). Attention is given to oxygen partial pressure during the processes; a low enough pressure (8 x 10 to the -5th torr) was found to totally inhibit the spreading of the filler material at a fixed heating cycle. With both types of steel, copper treatment enhanced even spreading at a decreased temperature.

Siewert, T. A.↗

NASA NTRS1996

Activated-Carbon Sorbent With Integral Heat-Transfer Device

Prototype adsorption device used, for example, in adsorption heat pump, to store natural gas to power automobile, or to separate components of fluid mixtures. Device includes activated carbon held together by binder and molded into finned heat-transfer device providing rapid heating or cooling to enable rapid adsorption or desorption of fluids. Concepts of design and fabrication of device equally valid for such other highly thermally conductive devices as copper-finned tubes, and for such other high-surface-area sorbents as zeolites or silicates.

Jones, Jack A.↗