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At least 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Formate-Induced Dissolution and Reprecipitation of a Copper Electrocatalyst during Electrochemical CO 2 Reduction Reaction

Catalyst size, morphology, and crystal structure play crucial roles in determining the activity and selectivity of electrochemical CO 2 reduction reactions, which are known to change during the reaction process. A comprehensive understanding of how, when, and why these parameters evolve under operational conditions is essential for developing stable, efficient, and selective catalysts. In this study, we reveal that formate, one of the reaction products, contributes to the degradation of copper catalysts through a ligand-assisted dissolution mechanism. Utilizing in situ electrochemical atomic force microscopy and ex-situ scanning and transmission electron microscopies, we observed a significant reduction in the size of copper nanoparticles, which decreased from over 30 nm to less than 10 nm in diameter within 60 min of CO 2 RR. The temporal production of formate correlated with the particle size changes. Furthermore, analysis of the electrolyte using inductively coupled plasma optical emission spectroscopy confirmed the dissolution of copper nanoparticles. Control experiments involving various reaction products (H 2 , CO, and HCOO – ) demonstrated that formate significantly promotes copper dissolution, thereby highlighting its role in the ligand-assisted dissolution mechanism of copper electrocatalysts. In conclusion, our findings provide critical insights into copper catalyst behavior during electrochemical CO 2 reduction, facilitating the design of more resilient and effective electrocatalysts.

Catalysts↗
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 OSTI2021

Measurements of Neutron Scattering from a Copper Sample Using a Quasi-Differential Method in the Region from 2 keV to 20 MeV

Neutron scattering from a copper sample was measured at Rensselaer Polytechnic Institute utilizing the quasi-differential method. The measurement spanned the energy range from 0.5 to 20 MeV using the high-energy scattering system and from 2 keV to 0.5 MeV using the new mid-energy scattering system. Copper was selected as a material of interest to measure due to large discrepancies between experiments and simulations of the Zeus benchmark. The Zeus benchmark consists of a copper reflected highly enriched uranium system, and the angular distribution of copper scattering was thought to potentially be the cause of the discrepancy. The copper measurements found differences in the scattering response particularly in the incident energy region from 1 to 2 MeV for the high-energy measurement and from 2 to 4 keV in the mid-energy system. These differences are particularly noticeable at angles near 90 deg in the high-energy system and back angles in the mid-energy system. Additionally, for ENDF/B-VIII.0 there is a large discrepancy at the forward angle in the energy range around 0.5 MeV. For these reasons, a new evaluation of copper scattering utilizing these results is recommended and perhaps could help to improve the agreement with the Zeus benchmarks.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2022

A Finite Difference Analysis of the Effect of Graphene Additions on the Electrical Conductivity of Polycrystalline Copper

A finite-difference method was used to explore the effect of graphene on the bulk electrical conductivity of copper-graphene composites. In this capacity, grain orientation information from pure copper and copper-graphene composites were used to generate synthetic 3D microstructures. The electrical conductivity of these microstructures were calculated using the finite difference method assuming different average grain sizes. From these calculations, we demonstrate that when high-conductivity grain boundaries are present within the microstructure arising from the presence of graphene, an increase in the bulk electrical conductivity is observed. On the other hand, the difference in textures between copper and copper-graphene composites may not account for a significant difference in bulk electrical conductivity. In comparison, the copper grain size has a considerably larger effect on electrical conductivity as previously anticipated. This is one of the first demonstrations of a physical basis for enhanced conductivity composites and presents pathways for further investigations on the effects of composite microstructural features, material interfaces and graphene content on electrical performance.

Frazier, William E.↗
DOE OSTI2022

Enhanced electrical conductivity in graphene–copper multilayer composite

For many years, researchers have been trying to make a material more conductive than silver by incorporating carbon nanotubes or graphene into copper to form a composite material. However, after a decade-long effort, only a few groups reported successful results, raising concerns about the feasibility of this composite approach. Here, we report our effort to validate the multilayer graphene–copper composite approach for improving electrical conductivity. We demonstrate that, with an estimated 0.008 vol. % graphene addition, copper’s electrical conductivity was improved to 104.2% of International Annealed Copper Standard (IACS) at room temperature. If the copper substrate used to make the multilayer composite is discounted using the parallel resistance model, the conductivity is calculated to be 185% IACS. This result could be further improved if the thickness of the copper layers can be further reduced.

36 MATERIALS SCIENCE↗
NASA NTRS1991

Effects on LDEF exposed copper film and bulk

Two forms of copper were exposed to the Long Duration Exposure Facility (LDEF) Mission 1 environment: a copper film, initially 74.2 plus or minus 1.1 nm thick sputter coated on a fused silica flat and a bulk piece of oxygen-free, high conductivity (OFHC) copper. The optical density of the copper film changed from 1.33 to 0.70 where exposed, and the film thickness increased to 106.7 plus or minus 0.5 nm where exposed. The exposed area appears purple by reflection and green by transmission for the thin film and maroon color for the bulk copper piece. The exposed areas increased in thickness, but only increase in the thickness of the thin film sample could be readily measured. The increase in film thickness is consistent with the density changes occurring during conversion of copper to an oxide. However, we have not been able to confirm appreciable conversion to an oxide by x-ray diffraction studies. We have not yet subjected the sample to e-beams or more abusive investigations out of concern that the film might be modified.

Peters, Palmer N.↗
NASA NTRS1992

Effects on LDEF exposed copper film and bulk

Two forms of copper were exposed to the Long Duration Exposure Facility (LDEF) Mission 1 environment: a copper film initially 74.2 plus or minus 1.1 nm thick sputter coated on a fused silical flat and a bulk piece of oxygen free, high conductivity (OFHC) copper. The optical density of the copper film changed from 1.33 to 0.70 where exposed and the film thickness increased to 106.7 plus or minus 0.5 nm where exposed. The exposed area appears purple by reflection and green by transmission for the thin film and maroon color for the bulk copper piece. The exposed areas increased in thickness, but only increase in the thickness of thin film samples could be readily measured. The increase in film thickness is consistent with the density changes occurring during conversion of copper to an oxide. However, we have not been able to confirm appreciable conversion to an oxide by x ray diffraction studies. We have not yet subjected the sample to e-beams or more abusive conditions out of concern that the film might be modified.

Peters, Palmer N.↗
NASA NTRS1994

Excimer laser produced plasmas in copper wire targets and water droplets

Elastically scattered incident radiation (ESIR) from a copper wire target illuminated by a KrF laser pulse at lambda = 248 nm shows a dinstinct two-peak structure which is dependent on the incident energy. The time required to reach the critical electron density (n(sub c) approximately = 1.8 x 10(exp 22) electrons/cu cm) is estimated at 11 ns based on experimental results. Detailed ESIR characteristics for water have been reported previously by the authors. Initiation of the broadband emission for copper plasma begins at 6.5 +/- 1.45 ns after the arrival of the laser pulse. However, the broadband emission occurs at 11 +/- 0.36 ns for water. For a diatomic substance such as water, the electron energy rapidly dissipates due to dissociation of water molecules, which is absent in a monatomic species such as copper. When the energy falls below the excitation energy of the lowest electron state for water, it becomes a subexcitation electron. Lifetimes of the subexcited electrons to the vibrational states are estimated to be of the order of 10(exp -9) s. In addition, the ionization potential of copper (440-530 nm) is approximately 6 eV, which is about two times smaller than the 13 eV ionization potential reported for water. The higher ionization potential contributes to the longer observed delay time for plasma formation in water. After initiation, a longer time is required for copper plasma to reach its peak value. This time delay in reaching the maximum intensity is attributed to the energy loss during the interband transition in copper.

Song, Kyo-Dong↗
NASA NTRS2002

Characteristics of Pool Boiling on Graphite-Copper Composite Surfaces

Nucleate pool boiling performance of different liquids on graphite-copper composite (Gr-Cu) surfaces has been experimentally studied and modeled. Both highly wetting fluids, such as freon-113 and pentane, and a moderately wetting fluid (water) were tested on the Gr-Cu surfaces with different graphite-fiber volume fractions to reveal the enhancement effects of the composite surfaces on the nucleate pool boiling. Results of the experiments show that the graphite-fiber volume fraction has an optimum value. The Gr-Cu composite surface with 25 percent graphite-fiber volume (f=0.25) has a maximum enhancement effect on the nucleate boiling heat transfer comparing to the pure copper surface. For the highly wetting fluid, the nucleate boiling heat transfer is generally enhanced on the Gr- Cu composite surfaces by 3 to 6 times shown. In the low heat flux region, the enhancement is over 6 times, but in the high heat flux region, the enhancement is reduced to about 40%. For the moderately wetting fluid (water), stronger enhancement of nucleate boiling heat transfer is achieved on the composite surface. It shown the experimental results in which one observes the nucleate boiling heat transfer enhancement of 5 to 10 times in the low heat flux region and an enhancement of 3 to 5 times in the high heat flux region. Photographs of bubble departure during the initial stage of nucleate boiling indicate that the bubbles detached from the composite surface are much smaller in diameter than those detached from the pure copper surface. Typical photographs are presented.It shows that the bubbles departed from the composite surface have diameters of only O(0.1) mm, while those departed from the pure copper surface have diameters of O(1) mm. It is also found that the bubbles depart from the composite surface at a much higher frequency, thus forming vapor columns. These two phenomena combined with high thermal conductivity of the graphite fiber are considered the mechanisms for such a significant augmentation in nucleate boiling heat transfer on the composite surfaces. A physical model is developed to describe the phenomenon of bubble departure from the composite surface: The preferred site of bubble nucleation is the fiber tip because of higher tip temperature than the surrounding copper base and poor wettability of the graphite tip compared with that of the base material (copper). The high evaporation rate near the contact line produces the vapor cutback due to the vapor recoil pushing the three-phase line outwards from the fiber tip, and so a neck of the bubble is formed near the bubble bottom. Evaporation and surface tension accelerate the necking process and finally result in the bubble departure while a new small bubble is formed at the tip when the surface tension pushes the three-phase line back to the tip. The process is schematically shown. The proposed model is based on and confirmed by experimental results.

Zhang, Nengli↗
NASA NTRS2008

Long-Term Effects of Soldering By-Products on Nickel-Coated Copper Wire

An analysis of thirty-year-old, down graded flight cables was conducted to determine the makeup of a green material on the surface of the shielded wire near soldered areas and to ascertain if the green material had corroded the nickel-coated copper wire. Two likely candidates were possible due to the handling and environments to which these cables were exposed. The flux used to solder the cables is known to contain abietic acid, a carboxylic acid found in many pine rosins used for the soldering process. The resulting material copper abietate is green in color and is formed during the application of heat during soldering operations. Copper (II) chloride, which is also green in color is known to contaminate flight parts and is corrosive. Data is presented that shows the material is copper abietate, not copper (II) chloride, and more importantly that the abietate does not aggressively attack nickel-plated copper wire.

Rolin, T. D.↗
DOE OSTI2020

Method and composition for reducing nitrates, nitrites, and/or hydroxylamine in water using a homogeneous reduced copper tetra-substituted fluorinated pinacolate ligand catalyst complex

A method for reducing nitrates, nitrites, and/or hydroxylamine in water using a homogeneous reduced copper tetra-substituted fluorinated pinacolate ligand catalyst complex. The method includes dissolving a copper(II) tetra-substituted fluorinated pinacolate ligand pre-catalyst complex in water having an excess amount of nitrates, nitrites, and/or hydroxylamine therein. The dissolved copper(II) tetra-substituted fluorinated pinacolate ligand pre-catalyst complex in the water is subjected to electrochemical reduction to form a homogeneous reduced copper tetra-substituted fluorinated pinacolate ligand catalyst complex. The homogeneous reduced copper tetra-substituted fluorinated pinacolate ligand catalyst complex reduces the nitrates, nitrites, and/or hydroxylamine in the water to compounds with nitrogen in a lower oxidation state with the homogeneous reduced copper tetra-substituted fluorinated pinacolate ligand catalyst complex.

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

Copper nanoparticle structures for reduction of carbon dioxide to multicarbon products

This disclosure provides systems, methods, and apparatus related to copper nanoparticle structures for reduction of carbon dioxide to multicarbon products. In one aspect, a method includes providing a plurality of copper nanoparticles. The plurality of copper nanoparticles are deposited on a support. The plurality of copper nanoparticles are transformed to a plurality of copper structures during an operation in which carbon dioxide is reduced. The plurality of copper nanoparticles on the support are used as a working electrode in an electrochemical cell during the operation.

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

Crystalline phase transitions and water-soluble complexes of copper(Ⅰ) 2-hydroxyethanethiolate

We report the coordination polymer copper(I) 2-hydroxyethanethiolate, (CuSCH 2 CH 2 OH) n , though insoluble in all common solvents, dissolved readily in basic aqueous solutions of the thiolate anion (HOCH 2 CH 2 S – ) of 2-mercaptoethanol to form a single species: the tetranuclear cluster [Cu 4 (μ-SCH 2 CH 2 OH) 6 ] 2– . From this solution were grown X-ray quality single crystals of copper(I) 2-hydroxyethanethiolate. This compound underwent a hitherto unknown crystal phase transition at ca. 6 °C, from point group P2 1 2 1 2 1 to Pna2 1 , with noticeable changes in the geometry of the Cu-S layer and in the orientation of the alkylthiolate side chains. When the bulky base tetrabutylammonium hydroxide was employed in the aqueous thiolate solution used to dissolve (CuSCH 2 CH 2 OH) n , the water-soluble polynuclear copper(I) complex bis(tetrabutylammonium) hexakis(μ-2-hydroxyethanethiolato) tetracuprate(I), [(C 4 H 9 ) 4 N] 2 [Cu 4 (μ-SCH 2 CH 2 OH) 6 ], could be isolated as X-ray quality crystals. Structural characterization of this complex revealed a tetrahedral arrangement of copper(I) centers with thiolates bridging the edges of the tetrahedra. On standing, this complex degraded to a larger polynuclear Cu(I) sulfide cluster.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Significantly Promoting the Thermal Conductivity and Machinability of Negative Thermal Expansion Alloy via In Situ Precipitation of Copper Networks

Rapid advancements in electronic devices yield an urgent demand for high-performance electronic packaging materials with high thermal conductivity, low thermal expansion, and great mechanical properties. However, it is a great challenge for current design philosophies to fulfill all the requirements simultaneously. Here, an effective strategy is proposed for significantly promoting the thermal conductivity and machinability of negative thermal expansion alloy (Zr,Nb)Fe 2 through eutectic precipitation of copper networks. The eutectic dual-phase alloy exhibits an isotropic chips-matched thermal expansion coefficient and a thermal conductivity enhancement exceeding 200% compared with (Zr,Nb)Fe 2 , along with an ultimate compressive strength of 550 MPa. The addition of copper reorganizes the composition of (Zr,Nb)Fe 2 , which smooths the magnetic transition and shifts it toward higher temperature, resulting in linear low thermal expansion in a wide temperature range. The highly fine eutectic copper lamellae construct high thermal conductivity networks within (Zr,Nb)Fe 2 , serving as highways for heat transfer electrons and phonons. The in situ forming of eutectic copper lamellae also facilitates the mechanical properties by enhancing interfacial bonding and bearing additional stress after yielding of (Zr,Nb)Fe 2 . This work provides a novel strategy for promoting thermal conductivity and mechanical properties of negative thermal expansion alloys via eutectic precipitation of copper networks.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Dynamic Strength of Copper at High Pressures Using Pressure Shear Plate Experiments

Measurement of strength at high pressures is critical to understanding the behavior of materials subjected to extreme loading conditions. Recent developments have extended the pressure shear plate impact (PSPI) technique to the high-pressure regime. Such experiments provide a unique opportunity to extract the complete stress-strain behavior of materials at relatively high pressures. The modified technique includes a new fiber-optic heterodyne transverse velocity interferometer system and new analysis methods to account for the inelastic response of the anvil plates. In this study, PSPI experiments are conducted on oxygen-free high conductivity (OFHC) copper at pressures ranging from 10 to 43 GPa and at strain rates of ~10 5 s -1 . Complete stress-strain curves of copper are obtained using a hybrid methodology that relies on numerical simulations and particle velocity records gathered in these experiments. Experiments are conducted at similar pressures and strain rates using two types of anvils that undergo different levels of plastic strains: tool steel and tungsten carbide, to check the robustness of the hybrid method. The behavior of copper at these high pressures and strain rates is compared with previous literature data, and the effect of pressure and strain rate on the strength behavior of copper are discussed. Here, it was observed that the rate of change in yield strength change in pressure was 2.5 times the rate of change of shear modulus with pressure. The strength models that predict the response of copper at these extreme conditions are also examined and validated.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Physical structure of constitutional isomers influences antiproliferation activity of thiosemicarbazone-alkylthiocarbamate copper complexes

A series of hybrid thiosemicarbazone-alkylthiocarbamate copper complexes with similar electronic environments but distinct physical structures have been prepared, characterized, and evaluated for antiproliferation activity. The complexes include the constitutional isomers (1-phenylpropane-1-imine-(O-ethylthiocarbamato)-2-one-(N-methylthiosemicarbazonato))copper(II) (CuL 1 ) and (1-phenylpropane-1-one-(N-methylthiosemicarbazonato)-2-imine-(O-ethylthiocarbamato))copper(II) (CuL 2 ) along with (1-propane-1-imine-(O-ethylthiocarbamato)-2-one-(N-methylthiosemicarbazonato))copper(II) (CuL 3 ). Complexes CuL 1 and CuL 2 differ in the positions of the pendent thiosemicarbazone (TSC) and alkylthiocarbamate (ATC) moieties on the 1-phenylpropane backbone. Complex CuL 3 employs a propane backbone with the TSC in the 2-position as in CuL 1 . The isomer pair CuL 1 and CuL 2 have equivalent electronic environments with indistinguishable Cu II/I potentials (E 1/2 = -0.86 V vs. ferrocenium/ferrocene) and electron paramagnetic resonance (EPR) spectra (g ∥ = 2.26, g ⊥ = 2.08). The electronic structure of CuL 3 has a similar E 1/2 of -0.84 V and identical EPR parameters to CuL 1, 2 . Single crystal X-ray diffraction studies confirm a consistent donor environment with no substantial variation in the Cusingle bondN or Cusingle bondS bond distances and angles between the complexes. The antiproliferation activities of the CuL 1–3 were evaluated against the lung adenocarcinoma cell line (A549) and nonmalignant lung fibroblast cell line (IMR-90) using the MTT assay. CuL 1 had the highest A549 activity ( A549 EC 50 = 0.065 μM) and selectivity ( IMR-90 EC 50 / A549 EC 50 = 20). The constitutional isomer CuL 2 displayed decreased A549 activity (0.18 μM) and selectivity (10.6). The complex CuL 3 displayed activity (0.009 μM) similar to CuL 1 but with a lack of selectivity (1.0). Cellular copper loading determined by ICP-MS was consistent with the activity and selectivity trends. The complexes CuL 1–3 did not induce reactive oxygen species (ROS) generation.

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

A preliminary investigation into the electrodeposition and synthesis of radiopure Copper–Chromium alloys for rare-event physics detector systems

Current investigations into neutrinoless double beta decay and the direct detection of dark matter require increasingly sensitive detector systems that demand ultra-low background materials. These requirements have previously been attained using ultra-radiopure electroformed (EF) copper. However, pure copper possesses high ductility and relatively low strength, which necessitates the need for large amounts of material and extra care during fabrication to help minimize galling and mechanical failure. Furthermore, we investigate an alloying alternative to pure EF copper by examining low wt% copper chrome (Cu–Cr) solid solution alloys, with inquiries into alloy hardness, strength, and radiopurity. Alloyed Cu–Cr layered samples are shown to exhibit significantly increased hardness compared to EF copper, for example showing a 50% increase in exhibited hardness using less than 1% Cr by weight, with limited negative impact to the material’s radiopurity.

Background↗
DOE OSTI2023

ATCUN-like Copper Site in βB2-Crystallin Plays a Protective Role in Cataract-Associated Aggregation

Cataract is the leading cause of blindness worldwide, and it is caused by crystallin damage and aggregation. Senile cataractous lenses have relatively high levels of metals, while some metal ions can directly induce the aggregation of human γ-crystallins. Here, for this work, we evaluated the impact of divalent metal ions in the aggregation of human βB2-crystallin, one of the most abundant crystallins in the lens. Turbidity assays showed that Pb 2+ , Hg 2+ , Cu 2+ , and Zn 2+ ions induce the aggregation of βB2-crystallin. Metal-induced aggregation is partially reverted by a chelating agent, indicating the formation of metal-bridged species. Our study focused on the mechanism of copper-induced aggregation of βB2-crystallin, finding that it involves metal-bridging, disulfide-bridging, and loss of protein stability. Circular dichroism and electron paramagnetic resonance (EPR) revealed the presence of at least three Cu 2+ binding sites in βB2-crystallin, one of them with spectroscopic features typical for Cu 2+ bound to an amino-terminal copper and nickel (ATCUN) binding motif, which is found in Cu transport proteins. The ATCUN-like Cu binding site is located at the unstructured N-terminus of βB2-crystallin, and it could be modeled by a peptide with the first six residues in the protein sequence (NH 2 -ASDHQF-). Isothermal titration calorimetry indicates a nanomolar Cu 2+ binding affinity for the ATCUN-like site. An N-truncated form of βB2-crystallin is more susceptible to Cu-induced aggregation and is less thermally stable, indicating a protective role for the ATCUN-like site. EPR and X-ray absorption spectroscopy studies reveal the presence of a copper redox active site in βB2-crystallin that is associated with metal-induced aggregation and formation of disulfide-bridged oligomers. Our study demonstrates metal-induced aggregation of βB2-crystallin and the presence of putative copper binding sites in the protein. Whether the copper-transport ATCUN-like site in βB2-crystallin plays a functional/protective role or constitutes a vestige from its evolution as a lens structural protein remains to be elucidated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗