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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 1,045 records · Page 58
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Surface Self-nanocrystallization in Copper Electroforming

The coarse columnar grain layer generated on top of electroforming deposits leads to low surface strength and poor global performance of deposits. Here, we introduce a particle abrasive-induced surface self-nanocrystallization process, which is a part of the electroforming process rather than involving complex poststeps using special equipment. It can generate a thickness-controllable surface nanocrystalline layer on top of copper deposits for performance enhancement. In this study, surface nanocrystalline layers of 10, 20, 50 and 120 μm were fabricated on top of 500-μm-thick copper deposits. The tensile strength of copper deposits increases from 234 to 246, 330, 383 and 421 MPa, with a corresponding decrease in elongation from 26 to 25, 24, 15 and 6%, respectively. The moderately thick surface nanocrystalline layer makes the copper deposits exhibit good comprehensive mechanical properties. In addition, the surface self-nanocrystallization also makes the copper deposits show a better corrosion resistance in a neutral aqueous 0.1 M NaCl solution. This study aims to promote a convenient, controllable and reliable surface self-nanocrystallization process in electroforming for improving the global performance of deposits.

36 MATERIALS SCIENCE↗
DOE OSTI2017

One-step construction of a molybdenum disulfide/multi-walled carbon nanotubes/polypyrrole nanocomposite biosensor for the ex-vivo detection of dopamine in mouse brain tissue

Highlights: • Ex vivo dopamine detection in mouse brain tissues of Parkinson's disease model. • Nanocomposite constructed by one-step electrochemical approach. • The synergetic performance enhancement of the sensor by nanocomposite. We developed a new strategy for construction of a biosensor for the neurotransmitter dopamine. The biosensor was constructed by one-step electrochemical deposition of a nanocomposite in aqueous solution at pH 7.0, consisting of molybdenum disulfide, multi-walled carbon nanotubes, and polypyrrole. A series of analytical methods was performed to investigate the surface characteristics and the improved electrocatalytic effect of the nanocomposite, including cyclic voltammetry, electrochemical impedance spectroscopy, field-emission scanning electron microscopy, atomic force microscopy, and Raman spectroscopy. The constructed biosensor showed high sensitivity (1.130 μAμM{sup −1}cm{sup −2}) with a dynamic linearity range of 25–1000 nM and a detection limit of 10 nM. Additionally, the designed sensor exhibited strong anti-interference ability and satisfactory reproducibility. The practical application of the sensor was manifested for the ex vivo determination of dopamine neurotransmitters using brain tissue samples of a mouse Parkinson's disease model.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2023

Emergent solvation phenomena in non-aqueous electrolytes with multiple anions

As the search for new battery chemistries with higher capacities and more stable supply chains expands, requiring increasingly complex electrolytes with multiple solvents and anions, it is becoming clear that understanding and controlling the working cation solvation structure is key to enabling improved stability and reversibility. In this work, we discover an emergent solvation behavior in multivalent electrolytes containing multiple anions, where bis(trifluoromethane sulfonyl) imide (TFSI⁻) anions that are fully dissociated in isolation form contact ion pairs with Zn 2+ when combined with more strongly coordinating halides. This coordination modifies the electrochemical response, activating additional redox species as the halide association strength weakens (i.e., Cl⁻ > Br⁻ > I⁻) and systematically lowering overpotentials for metal deposition. This work suggests a completely new framework for electrolyte design in which anion chemistry can be used to tune both the bulk speciation and the interfacial solvation structure, enabling profound changes to the electrochemical behavior of the system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Elucidating mechanisms of Li plating on Li anodes of lithium-based batteries

Lithium metal is known as a very promising anode material for lithium-based batteries possessing a quite high theoretical capacity. But it has been kept away from practical applications due to its extreme reactivity and potential safety hazards led by serious dendrite growth. The origins of dendrite formation may be associated with the mechanisms of Li plating and with the mode of charge transfer during Li reduction or oxidation at the anode-electrolyte interface. Here, density functional theory (DFT) calculations are conducted to analyze the electron transfer between Li (100) and Li cations located in the proximity of the surface in several simulation models. The study includes two common used solvents: ethylene carbonate and dimethoxyethane (EC and DME), and a LiPF 6 salt, that surround the Li cation over perfect, defect-containing, and Li 2 CO 3 -passivated Li (100) surfaces. Our calculations demonstrate that the Li cation is easily reduced when bonding to DME rather than EC and its preferred deposition site is the hollow site on both perfect and defective Li (100). Additionally, a compact Li 2 CO 3 layer inhibits the charge transfer from Li metal to Li cations, thus modifying Li plating. It is concluded that the extreme reactivity of the Li metal surface induces a strongly inhomogeneous electron distribution upon deposition of a cation on the surface. This strong charge inhomogeneity may promote uneven Li nucleation and growth, eventually resulting in dendritic behavior.

25 ENERGY STORAGE↗
DOE OSTI2024

Electrolytic recovery of metals from lithium battery cathodes in moisture-tolerant molten hydroxide salt

Lithium-ion battery recycling offers an opportunity to develop innovative technologies to close the loop on the battery materials cycle and increase the resilience of the battery supply chain. Here, in this study, we demonstrate a two-step pyroelectrochemical method for producing mixed-metals from lithium-ion cathodes in a molten hydroxide salt. Mixed metal oxides in the form of insoluble lithium-ion cathode materials of LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) and spent lithium-ion battery materials (black mass) were electrochemically reduced to a soluble form and dissolved into a molten hydroxide salt bath. Electrochemical characterization of the process salt indicated accumulation of dissolved transition metals in the salt. A separate cathode was used to produce alloys of Ni, Mn, and Co electrochemically from the dissolved lithium-ion cathode materials. Characterization by scanning electron microscopy fitted with an energy dispersive X-ray spectrometer showed transition metals present in the cathode materials were recovered at the separate cathode. This approach represents a scalable, low temperature pyroelectrochemical process that can potentially reduce the cost and close the loop of battery cathode recycling.

25 ENERGY STORAGE↗
DOE OSTI2021

Electrochemically active surface area controls HER activity for Fe x Ni 100–x films in alkaline electrolyte

We report the synthesis and electrocatalytic activity of Fe x Ni 100-x electrochemically deposited films were investigated. Films were evaluated for the hydrogen evolution reaction (HER) in alkaline media with respect to composition and electrochemically active surface area (ECSA). Results demonstrate that films of higher or equal Fe content had an ECSA tenfold greater than films with higher Ni. When normalized by geometric surface area, Fe 50 Ni 50 films required the lowest overpotential of -390 mV to reach a current density of -10 mA cm -2 . However, when normalized by the ECSA, intrinsic HER activity increases as Ni content increases. Tafel slope, ECSA, microscopy, and impedance spectroscopy analyses allow a decoupled analysis of surface area versus activity effects on overall measured HER activity. Furthermore, these analyses collectively demonstrate that the increase in electrocatalytic activity is attributed to the increase in ECSA and not to an enhancement in the intrinsic activity by Fe and Ni component interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Elucidating mechanisms of oxide growth and surface passivation on zinc thin film electrodes in alkaline solutions using the electrochemical quartz crystal microbalance

For this study, we utilized electrochemical quartz crystal microbalance to understand electrochemical passivation of the zinc electrode in alkaline media and subsequent oxide growth and stripping. The formation of native zinc oxide on a near pristine Zn surface upon contact with 1 M KOH electrolyte was observed. The surface was seen to roughen with time. During Zn dissolution, the measured mass-charge ratio corresponded to the removal of ZnO and not merely Zn. The mechanism of passivation was determined to be caused by electrochemical etching to form pores. The etching leads to a build-up of solid ZnO and Zn(OH) 2 due to electrochemical reactions on the surfaces of the pores. These reactions functionally close the pores off from the bulk. The cycle of Zn deposition and dissolution develops a porous network, which may be the origin of mossy Zn deposits that plague reversible Zn metal batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Fabrication and temperature-dependent magnetic properties of one-dimensional multilayer Au–Ni–Au–Ni–Au nanowires

Multilayer Au–Ni–Au–Ni–Au nanowires with a controlled diameter of ∼100 nm were synthesized by electrochemical deposition in porous alumina templates. The length of each Ni-segment was controlled up to ∼230 nm, while the length of the Au segment sandwiched between two Ni segments was ∼180 nm. X-ray diffraction patterns and energy-dispersive X-ray spectra confirmed the formation of purely crystalline nanowires. The magnetic properties of the multilayer Au–Ni–Au–Ni–Au nanowires were investigated in the temperature range 2–300 K. Room-temperature magnetic hysteresis confirmed the ferromagnetic nature of the nanowires. The plot of coercivity as a function of temperature (from 2 to 300 K) followed law applicable for ferromagnetic nanostructures. The magnetization tended to increase as the temperature decreased, following the modified Bloch's law similar to ferromagnetic nanoparticles. - Graphical abstract: (a) SEM image of Au–Ni–Au–Ni–Au nanowire with 230 nm Ni segment length and 180 nm Au sandwiched between Ni segments (b) Kneller's law (c) Bloch's law Display Omitted - Highlights: • Electrochemical fabrication of Au–Ni–Au–Ni–Au nanowires in alumina templates. • Formation of beadlike structure of Ni segments. • Coercivity versus T follows Kneller's law for ferromagnetic materials. • Magnetization as a function of temperature follows the modified Bloch's law.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Interrupted in situ EBSD study of texture evolution and mechanism of surface grains in electroformed Ni after annealing with an initially duplex <100> + <111> fiber texture during uniaxial tensile deformation

Highlights: • The texture evolution of the electroformed Ni was investigated by using an interrupted in situ electron backscattered diffraction. • The initial <100> fiber component evolved into the metastable cube component with a weaker copper component. • Only a few grains of the initial <111> fiber component evolved into the copper orientation. - Abstract: The texture evolution process and mechanism of surface grains in electroformed Ni after annealing with an initially duplex <100> + <111> fiber texture during uniaxial tensile deformation were investigated by using interrupted in situ electron backscattered diffraction. The results showed that the initially duplex <100> + <111> fiber texture evolved into the metastable Cube orientation with a weak Cu orientation during the uniaxial tensile deformation. The volume fractions of <100> and <111> fiber texture decreased from 54.0% to 29.3% and 16.6% to 6.6%, respectively. The volume of the Cube orientation remained almost stable at 12%, whereas that of the Cu orientation increased from 1% to 2.9%. A simulation of the final preferred orientation based on the Taylor model was a cubic texture, which qualitatively agreed well with the experimental result. The simulated results indicated that the formed Cube and Cu textures evolved from the initial <100> and <111> fiber textures, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2013

One-step electrochemical synthesis of a graphene–ZnO hybrid for improved photocatalytic activity

Graphical abstract: - Highlights: • Graphene–ZnO hybrid was synthesized by one-step electrochemical deposition. • Graphene–ZnO hybrid presents a special structure and wide UV–vis absorption spectra. • Graphene–ZnO hybrid exhibits an exceptionally higher photocatalytic activity for the degradation of dye methylene blue. - Abstract: A graphene–ZnO (G-ZnO) hybrid was synthesized by one-step electrochemical deposition. During the formation of ZnO nanostructure by cathodic electrochemical deposition, the graphene oxide was electrochemically reduced to graphene simultaneously. Scanning electron microscope images, X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectra, and UV–vis absorption spectra indicate the resulting G-ZnO hybrid presents a special structure and wide UV–vis absorption spectra. More importantly, it exhibits an exceptionally higher photocatalytic activity for the degradation of dye methylene blue than that of pure ZnO nanostructure under both ultraviolet and sunlight irradiation.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Fabrication of uniformly dispersed Ag nanoparticles loaded TiO{sub 2} nanotube arrays for enhancing photoelectrochemical and photocatalytic performances under visible light irradiation

Graphical abstract: Uniformly dispersed Ag nanoparticles (NPs) were successfully loaded on both the outer and inner surface of the TiO{sub 2} nanotube arrays (NTs) through a simple polyol method, which exhibited the enhanced photoelectrochemical and photocatalytic performances under visible-light irradiation due to the more effective separation of photo-generated electron–hole pairs and faster interfacial charge transfer. - Highlights: • Highly dispersed Ag nanoparticles (NPs) are successfully prepared by polyol method. • Ag NPs are uniformly loaded on the surface of the TiO{sub 2} nanotube arrays (NTs). • Ag/TiO{sub 2}-NTs exhibit the enhanced photocatalytic activity under visible-light. • The enhanced photocurrent is explained by electrochemical impedance spectroscopy. - Abstract: Uniformly dispersed Ag nanoparticles (NPs) were successfully loaded on both the outer and inner surface of the TiO{sub 2} nanotube arrays (NTs) through a simple polyol method. The as-prepared Ag/TiO{sub 2}-NTs were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and UV–vis diffusion reflectance spectroscopy. Photoelectrochemical behaviors were investigated via photocurrent response and electrochemical impedance spectroscopy (EIS). Photocatalytic activity of Ag/TiO{sub 2}-NTs was evaluated by degradation of acid orange II under visible light irradiation. The results showed that photocatalytic efficiency of Ag/TiO{sub 2}-NTs is more than 5 times higher than that of pure TiO{sub 2} NTs. Comparing with the electrochemical deposition method, the photocatalytic activity of Ag/TiO{sub 2}-NTs prepared by polyol method has been obviously increased.

36 MATERIALS SCIENCE↗
DOE OSTI2015

One step electrochemical synthesis of bimetallic PdAu supported on nafion–graphene ribbon film for ethanol electrooxidation

Highlights: • Electrochemical deposition of bimetallic PdAu NPs. • Highly loaded PdAu NPs are obtained. • Nafion–graphene supported PdAu NPs shows good activity for ethanol electrooxidation. - Abstract: A nafion–graphene ribbon (Nf–GR) supported bimetallic PdAu nanoparticles (PdAu/Nf–GR) catalyst was prepared by electrochemical codeposition of Pd and Au at constant potential. The prepared catalyst was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), transmission electron microscopy (TEM) and X-ray diffraction analysis (XRD). The average particle size of PdAu nanoparticles (NPs) determined from XRD was 3.5 nm. The electrocatalytic activity of the PdAu/Nf–GR catalyst was examined by cyclic voltametry. It was observed that the as prepared catalyst showed efficient activity and good stability for ethanol electrooxidation in alkaline medium.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Al-doped ZnO seed layer-dependent crystallographic control of ZnO nanorods by using electrochemical deposition

Highlights: • Polar and semipolar ZnO NRs were successfully achieved by hydrothermal synthesis. • Semipolar and polar ZnO NRs were grown on ZnO and AZO/m-sapphire, respectively. • Al % of AZO/m-sapphire enhanced the lateral growth rate of polar ZnO NRs. - Abstract: We investigated the effect of an Al-doped ZnO film on the crystallographic direction of ZnO nanorods (NRs) using electrochemical deposition. From high-solution X-ray diffraction measurements, the crystallographic plane of ZnO NRs grown on (1 0 0) ZnO/m-plane sapphire was (1 0 1). The surface grain size of the (100) Al-doped ZnO (AZO) film decreased with increasing Al content in the ZnO seed layer, implying that the Al dopant accelerated the three-dimensional (3D) growth of the AZO film. In addition, it was found that with increasing Al doping concentration of the AZO seed layer, the crystal orientation of the ZnO NRs grown on the AZO seed layer changed from [1 0 1] to [0 0 1]. With increasing Al content of the nonpolar (1 0 0) AZO seed layer, the small surface grains with a few crystallographic planes of the AZO film changed from semipolar (1 0 1) ZnO NRs to polar (0 0 1) ZnO NRs due to the increase of the vertical [0 0 1] growth rate of the ZnO NRs owing to excellent electrical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Enhanced conduction in CdSe nanowires on 200 keV phosphorous negative ion implantation

Highlights: • CdSe nanowires were prepared by template assisted electro-deposition. • CdSe nanowires were implanted with 200 keV P{sup −} ions at different fluence. • Structure of CdSe NWs remained intact on ion implantation. • Optical band gap of CdSe NWs decreased after implantation. • The electrical conduction improved due to dominance of ionization effects. - Abstract: For II–VI compound semiconductor nanostructures, ion implantation is considered to be an area of significant interest due to its potential use in the fabrication of the extensive variety of novel optoelectric devices. CdSe nanowires with diameter 80 nm have been grown via the template-assisted electro-deposition method and were subsequently implanted with 200 keV negative phosphorous ions at fluence ranging from 10{sup 11} ions/cm{sup 2} to 10{sup 13} ions/cm{sup 2}. SRIM-TRIM simulation studies are done to understand the course and nature of events occurring during implantation. Pre- and post-implanted samples were characterized by Scanning electron microscope (SEM), X-Ray diffraction (XRD), UV–vis spectroscopy and Probe station with a Keithley source meter. Structural studies reveal no modification in crystal structure upon implantation. An increase of phosphorous content led to an apparent red shift in the optical band gap and an improvement in conductivity. These modifications are attributed to the ionization and the creation of damage on implantation.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

Electrophoretic deposition for improved trace element homogeneity in silica reference materials

Spatially-resolved analysis requires homogeneous reference materials (RMs) to make reliable quantitative measurements. Here we previously developed an electrophoretic deposition (EPD) method for fabrication of glassy microanalytical RMs with superior platinum-group element homogeneity **[1], and now include further dopants. For 39 trace elements, we analyzed dopant homogeneity in sintered silica (SiO 2 ) samples consolidated either mechanically by die-pressing (DP) or by EPD. A set of EPD and DP samples was made from each of two nanoparticle feedstocks produced by variations of the Stöber process **[2]. Spatially-resolved dopant distribution was characterized in all samples by laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS). In both sample sets, homogeneity of most trace elements was substantially improved by EPD relative to their DP counterpart.

36 MATERIALS SCIENCE↗