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At least 91 records · Page 5

Thermodynamic Control of Interface Directs MnO 2 Nucleation Chemistry for Dense and Conformal Electrodeposition

Manganese dioxide (MnO 2 ) is widely recognized as a promising material for high-energy-density energy storage systems due to its broad applicability and facile electrodeposition. However, achieving uniform, thin, and high-mass-loading MnO 2 coatings on high-surface-area electrodes remains a significant challenge. Conventional electrodeposition methods typically yield nonuniform, thick layers with poor conductivity and limited material utilization, restricting their practical use. Here, we uncover a thermodynamically engineered vanadyl/pervanadyl (VO 2+ /VO 2 + ) interface that fundamentally reshapes MnO 2 electrodeposition chemistry, enabling highly uniform and dense coatings. Here, combining in situ AFM measurement, Classical Nucleation Theory, and Johnson–Mehl–Avrami–Kolmogorov modeling, we show that this interface reduces early-stage detectable MnO 2 island size by 35-fold and shifts the MnO 2 growth from diffusion-limited to reaction-limited progressive nucleation. This thermodynamically controlled interface yields highly dense and conformal MnO 2 films with record-high mass loading of 241 mg cm –2 (1607 mg cm –3 ) on 3D-printed graphene aerogels, without compromising porosity or inducing thickness gradient. As a prototype demonstration, the resulting MnO 2 electrodes deliver record-setting volumetric performance in both capacitors (106 F cm –3 ) and Zn//MnO 2 pouch cells (162 mAh cm –3 ). Beyond energy storage, our findings demonstrate the significance of thermodynamic interface control in MnO 2 nucleation chemistry for achieving dense and uniform coatings on various substrates, with implications for electrocatalysis, semiconductor processing, and advanced materials manufacturing.

Batteries↗

Enhanced electrocatalytic activity of the Au-electrodeposited Pt nanoparticles-coated conducting oxide for the quantum dot-sensitized solar cells

Au was electrodeposited potentiostatically at 0.3 V for 5 min on nanoporous Pt nanoparticle-coated F-doped SnO{sub 2} (FTO/Pt) substrates. For comparison, Au-electrodeposited FTO (FTO/Au) and Au-uncoated FTO/Pt were prepared. FTO/Au showed large-sized Au clusters dispersed sparsely over FTO, which resulted in lower electrocatalytic activity than FTO/Pt. In contrast, FTO/Pt exhibited poor stability unlike FTO/Au due to poisoning by the adsorption of sulfur species. The Au-electrodeposited FTO/Pt (FTO/Pt/Au) consisted of small Au clusters deposited over the entire area of Pt due to the effective Au nucleation provided by nanoporous metallic Pt. FTO/Pt/Au exhibited enhanced electrocatalytic activity and excellent stability because the small Au particles well-dispersed over the nanoporous metallic Pt network provided numerous electrochemical reaction sites, and the Pt surface was not exposed to the electrolyte. When FTO/Pt/Au was used as the counter electrode (CE) of a quantum dot-sensitized solar cell, the significantly enhanced electrocatalytic activity of the FTO/Pt/Au CE facilitated the reduction reaction of S{sub n}{sup 2− }+ 2e{sup −} (CE) → S{sub n−1}{sup 2−} + S{sup 2−} at the CE/electrolyte interface, resulting in a significantly hindered recombination reaction, S{sub n}{sup 2− }+ 2e{sup −} (TiO{sub 2} in the photoanode) → S{sub n-1}{sup 2−} + S{sup 2−}, and significantly improved overall energy conversion efficiency.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Electrodeposition of Fe{sub 3}O{sub 4} layer from solution of Fe{sub 2}(SO{sub 4}){sub 3} with addition ethylene glycol

The electrodeposition of Fe{sub 3}O{sub 4} layer from the solution Fe{sub 2}(SO{sub 4}){sub 3} with the addition of ethylene glycol on Indium Tin Oxide (ITO) substrate has been performed. The electrodeposition was carried out using a voltage of 5 volts for 120 seconds, with and without the addition of 2% wt ethylene glycol. Significant effects of temperature on the resulting the samples is observed when they are heated at 400 °C. Structural characterization using X-ray diffraction (XRD) shows that all samples produce a layer of Fe{sub 3}O{sub 4} with particle size less than 50 nanometers. The addition of ethylene glycol and the heating of the sample causes a shrinkage in particle size. The scanning electron microscopy (SEM) characterization shows that Fe{sub 3}O{sub 4} layer resulting from the process of electrodeposition of Fe{sub 2}(SO{sub 4}){sub 3} without ethylene glycol, independent of whether the sample is heated or not, is uneven and buildup. Layer produced by the addition of ethylene glycol without heating produces spherical particles. On contrary, when the layer is heated the spherical particles transform to irregularly-shaped particles with smaller size.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Communication—Electrodeposition of Indium Directly on Silicon

Direct electrodeposition of indium onto silicon paves the way for advances in microelectronics, photovoltaics, and optoelectronics. Indium is generally electrodeposited onto silicon utilizing a physically or thermally deposited metallic seed layer. Eliminating this layer poses benefits in microelectronics by reducing resistive interfaces and in vapor-liquid-solid conversion to III-V material by allowing direct contact to the single-crystal silicon substrate for epitaxial conversion. We investigated conditions to directly electrodeposit indium onto n-type Si(100). We illustrate that a two-step galvanostatic plating at low temperatures can consistently produce smooth, continuous films of indium over large areas, in bump morphologies, and conformally into inverted pyramids.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Robust Large-Scale Dynamic Windows using Reversible Metal Electrodeposition

This project funded the study and development of dynamic windows based on reversible metal electrodeposition (RME). Dynamic windows allow user control over light and heat flow into and out of buildings, which offer both advantages in building aesthetics (with worker productivity improvement of 2%) and energy efficiency (up to 20% savings) compared to static controls such as low emissivity coatings and blinds/shades. Despite these advantages, dynamic windows, which traditionally rely on electrochromic metal oxides or conductive organic molecules for light modulation have failed to significantly impact the market due to issues related to cost, color, and optical dynamic range. Dynamic windows based on reversible metal electrodeposition (RME) are an exciting alternative approach and have the potential to overcome the issues associated with traditional technologies. A RME dynamic window is an electrochemical cell that modulates light using the reversible electrodeposition of metal on and off a transparent conducting oxide (TCO), which serves as the working electrode. The electrolyte has nearly colorless metal salts dissolved, and application of a cathodic potential on the TCO reduces the metal cations across the TCO surface to their metallic form, making a thin film that is efficient at blocking out light. A reverse in polarity oxidizes the metal, where it dissolves into solution, returning the window back to transparent. The counter electrode typically employed is a metal mesh, which is used to balance the electrochemical reactions happening on the TCO working electrode. These RME dynamic windows have the largest dynamic range (capable of reaching <<0.1% transmission) with color neutral tinting of any existing technology using solution processed techniques, which positions the technology as a promising candidate to penetrate the residential market. We have successfully scaled up the windows from 25 cm2 to 929 cm 2 , and we have demonstrated significant improvements to both the cycle life (10,000 cycles in a 3-electrode half-cell) and shelf life (>1 month) of our windows. We have published our work in high impact journals (6 published and 2 manuscripts in prep), filed 5 patents, and have incorporated TYNT Technologies to commercialize the technology.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Pulse Electrodeposition for Carbonate-Rich Deposits from Seawater

Seawater electrodeposition is gaining renewed interest in the context of sustainable development, both to build climate-resilient coastal infrastructure and for ocean-based decarbonization applications. Most of the applications benefit from CaCO 3 -rich deposits, but constant-voltage electrodeposition results in a mixture of CaCO 3 and Mg(OH) 2 , especially at higher voltages where precipitation rates are more desirable. The use of pulse voltages can help control interfacial pH that dictates the precipitation reactions. Here, we explore the use of pulse electrodeposition as a function of pulse frequency and duty cycle to control deposit composition. The most CaCO 3 -rich deposits were obtained under 10 Hz frequency and 10% duty cycle conditions for the voltage window investigated (-0.8 V to -1.2 V vs. SCE). While pulsing the voltage increases the amount of CaCO 3 deposited, the energy required per gram of CaCO 3 is significantly higher (14.5×) when compared to the base case of applying a constant voltage of -0.8 V vs. SCE. Further optimization of pulse conditions, electrode materials, and system configuration could lead to finding parameters that result in exclusively carbonate deposits without compromising precipitation rates, which may prove to be more useful for corrosion protection, coastal infrastructure, and other applications in sustainable development.

54 ENVIRONMENTAL SCIENCES↗

Kinetic Investigation by Batch Processing of Film Growth during the Electrodeposition of Titanium from Ethaline

Titanium electrodeposition as a technological advance has been out of reach due to the poor film quality obtained when using previously developed methods. This study shows that the electrodeposition of Ti is possible and feasible from the deep eutectic solvent ethaline. Moreover, this study shows through batch analysis that this deposition has temperature-dependent aspects that alter the film deposition kinetics upon modest heating. This ultraviolet–visible spectroscopic study is highlighting the more facile reduction of Ti 4+ to Ti 3+ and then to Ti 2+ at elevated temperatures. Understanding the underlying kinetics of electrodeposition opens up new venues for the application of this important metal.

36 MATERIALS SCIENCE↗

Electrodeposition and Properties of Composites Consisting of Carbon Nanotubes and Copper

Copper–matrix–carbon nanotubes (Cu–CNTs) composite films were prepared in a Cu plating solution with multiwall carbon nanotubes (MWCNTs) using electrodeposition. The MWCNTs surface treatment method, electroplating solution system, electroplating conditions, heat treatment process and other parameters of this process are discussed. The results showed that MWCNTs purified by HCl treatment and dispersed by stearyltrimethylammonium bromide are more suitable as add-on materials for the preparation of the copper matrix composite films by electrodeposition. An appropriate heat treatment process was able to improve the structures and properties of the composite films. The final products showed that the MWCNTs were evenly distributed in the composite films and joined with the copper grains to form a mutually entangled mesh structure with excellent corrosion resistance (3.19 × 10{sup −8} Ω M) and a hardness of 53.5 HV. All this was possible through extensive optimization of the electrodeposition and post-treatment parameters.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

A dynamically bare metal interface enables reversible magnesium electrodeposition at 50 mAh cm −2

Understanding and facilitating pure magnesium nucleation/growth electrodeposition behavior with ultrahigh Coulombic efficiency is complicated by the phenomenon of solid electrolyte interphase (SEI) formation in state-of-the-art, halogen-free magnesium electrolytes. Defining the electrolyte properties necessary to achieve ideal electrodeposition/stripping (E/S) thus remains elusive. Here, in this work, we reveal for the first time, rapid magnesium electrodeposition behavior that forms densely aligned, micron-sized thin platelets by establishing a dynamic bare magnesium/electrolyte interface during high-rate net plating. This effectively “SEI-free” interface allows facile magnesium diffusion and migration in stripping with near-unity E/S efficiency under demanding conditions over long-term cycling. The intrinsic electrolyte stability of the salt/solvent at the molecular level is the key to forming such an interface. The efficacy of the dynamic bare interface and an electrodeposited, free-standing magnesium anode is demonstrated in a high-areal-capacity full cell. These findings provide new design principles and fundamental understanding of interfacial chemistry in multivalent metal batteries.

Mg full cell↗

Factors that Determine the Length Scale for Uniform Tinting in Dynamic Windows Based on Reversible Metal Electrodeposition

Dynamic windows based on reversible metal electrodeposition are attractive compared to conventional electrochromics because they can have neutral color, high contrast, and potentially lower cost, yet they are not nearly as developed and the design rules for making them function at large scale are not presented in the literature. We model the voltage drops that occur in the transparent electrodes to get insight on how to obtain uniform electrodeposition of metals over large-area. By optimizing the surface and density of the Pt nanoparticles used to nucleate metal growth, we lower the nucleation barrier for electrodeposition by 70 mV. We show that the growth rate of the metal films is determined by diffusion rather than reaction kinetics, which makes it possible to achieve uniform film deposition over a range of potentials from -300 mV to -700 mV. As a result, we demonstrate 100 cm 2 dynamic windows that are color-neutral and tint uniformly from a clear state (> 60%) to a dark state (< 5%) in less than one minute.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Selective cobalt and nickel electrodeposition for lithium-ion battery recycling through integrated electrolyte and interface control

Abstract Molecularly-selective metal separations are key to sustainable recycling of Li-ion battery electrodes. However, metals with close reduction potentials present a fundamental challenge for selective electrodeposition, especially for critical elements such as cobalt and nickel. Here, we demonstrate the synergistic combination of electrolyte control and interfacial design to achieve molecular selectivity for cobalt and nickel during potential-dependent electrodeposition. Concentrated chloride allows for the speciation control via distinct formation of anionic cobalt chloride complex (CoCl 4 2- ), while maintaining nickel in the cationic form ([Ni(H 2 O) 5 Cl] + ). Furthermore, functionalizing electrodes with a positively charged polyelectrolyte (i.e., poly(diallyldimethylammonium) chloride) changes the mobility of CoCl 4 2- by electrostatic stabilization, which tunes cobalt selectivity depending on the polyelectrolyte loading. This strategy is applied for the multicomponent metal recovery from commercially-sourced lithium nickel manganese cobalt oxide electrodes. We report a final purity of 96.4 ± 3.1% and 94.1 ± 2.3% for cobalt and nickel, respectively. Based on a technoeconomic analysis, we identify the limiting costs arising from the background electrolyte, and provide a promising outlook of selective electrodeposition as an efficient separation approach for battery recycling.

36 MATERIALS SCIENCE↗

Regulating electrodeposition morphology of lithium: towards commercially relevant secondary Li metal batteries

Lithium, the lightest and most electronegative metallic element, has long been considered the ultimate choice as a battery anode for mobile, as well as in some stationary applications. The high electronegativity of Li is, however, a double-edged sword—it facilitates a large operating voltage when paired with essentially any cathode, promising a high cell-level energy density. It is also synonymous with a high chemical reactivity and low reduction potential. The interfaces a Li metal anode forms with any other material (liquid or solid) in an electrochemical cell are therefore always mediated by one or more products of its chemical or electrochemical reactions with that material. The physical, crystallographic, mechanical, electrochemical, and transport properties of the resultant new material phases (interphases) regulate all interfacial processes at a Li metal anode, including electrodeposition during battery recharge. This Review takes recent efforts aimed at manipulating the structure, composition, and physical properties of the solid electrolyte interphase (SEI) formed on an Li anode as a point of departure to discuss the structural, electrokinetic, and electrochemical requirements for achieving high anode reversibility. An important conclusion is that while recent reports showing significant advances in the achievement of highly reversible Li anodes, e.g. as measured by the coulombic efficiency (CE), raise prospects for as significant progress towards commercially relevant Li metal batteries, the plateauing of achievable CE values to around 99 ± 0.5% apparent from a comprehensive analysis of the literature is problematic because CE values of at least 99.7%, and preferably >99.9% are required for Li metal cells to live up to the potential for higher energy density batteries offered by the Li metal anode. On this basis, we discuss promising approaches for creating purpose-built interphases on Li, as well as for fabricating advanced Li electrode architectures for regulating Li electrodeposition morphology and crystallinity. Considering the large number of physical and chemical factors involved in achieving fine control of Li electrodeposition, we believe that achievement of the remaining ~0.5% in anode reversibility will require fresh approaches, perhaps borrowed from other fields. We offer perspectives on both current and new strategies for achieving such Li anodes with the specific aim of engaging established contributors and newcomers to the field in the search for scalable solutions.

25 ENERGY STORAGE↗

Surface diffusion manifestation in electrodeposition of metal anodes

Metal anode-based battery systems have been deemed indispensable towards energy storage renaissance engendering extensive research into strategies countering dendritic growth of metal electrodeposition. Fundamentally, the morphological evolution of a material is uniquely characterized by the heights of its self-diffusion barrier across multiple pathways. Herein, based on a coarse-grained kinetic Monte Carlo method, we derive insights into the nucleation and growth of metallic electrodeposits in liquid electrolytes, governed by surface self-diffusion characteristics cognizant of the diverse diffusion routes including terrace, away from step and interlayer pathways. We deconvolve the roles played by each of these surface diffusion mechanisms in conjunction with the electrochemical reaction rate on the deposition morphology regime (film vs. mossy vs. fractal). We identify interlayer diffusion as the predominant morphology-determining mechanism; dendrite-free deposition even at moderate current rates constrains this diffusion barrier to an upper limit. Additionally, we highlight subtle features amidst the realm of the morphological growth assortment that connect to the cell's electrochemical performance. Finally, we delineate morphological features of Li, Na, Mg and Al based on their respective surface diffusion barriers and applied overpotentials, and provide a baseline for the interpretation of experimental observations. This fundamental study sheds light on the mesoscale underpinnings of morphological variances in mono-valent and multi-valent metal electrodeposition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Stability of Electrodeposition at Solid-Solid Interfaces and Implications for Metal Anodes

We generalize the conditions for stable electrodeposition at isotropic solid-solid interfaces using a kinetic model which incorporates the effects of stresses and surface tension at the interface. We develop a stability diagram that shows two regimes of stability: a previously known pressure-driven mechanism and a new density-driven stability mechanism that is governed by the relative density of metal in the two phases. We show that inorganic solids and solid polymers generally do not lead to stable electrodeposition, and provide design guidelines for achieving stable electrodeposition.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

High density of genuine growth twins in electrodeposited aluminum

We demonstrate electrodeposition as a synthesis method for fabrication of Al coatings, up to 10 μm thick, containing a high density of genuine growth twins. This has not been expected since the twin boundary energy of pure Al is very high. TEM methods were used to analyze deposited Al and its nanoscaled twins. DFT methods confirmed that the influence of the substrate is limited to the layers close to the interface. Our findings are different from those achieved by sputtering of Al coatings restricted to a thickness less than 100 nm with twins dominated by epitaxial effects. We propose that in the case of electrodeposition, a high density of twins arises because of fast nucleation and is additionally promoted by a monolayer of adsorbed hydrogen originating from water impurities. Therefore, electrodeposition is a viable approach for tailoring the structure and properties of thicker, deposited Al coatings reinforced by twins.

Science & Technology - Other Topics↗

Study of Am electrodeposition from AmCl 3 -LiCl-KCl Molten Salt

In this work, the electrodeposition reaction of Am in AmCl 3 -LiCl-KCl molten salt was studied using voltammetry and chronoamperometry. Electrodeposition of Am was shown to proceed via a two – step reaction scheme, involving the one-electron transfer reduction of Am 3+ to Am 2+ , followed by the two-electron transfer reduction of intermediate Am 2+ to Am 0 . A low Coulombic efficiency of Am deposition was measured despite the Am deposition occurring within the thermodynamic stability window of the supporting LiCl-KCl electrolyte. We hypothesize that the low efficiency is due to out-diffusion of the intermediate Am 2+ species away from the electrode surface. Experimental observations provide evidence of a kinetically – limited electrodeposition reaction, which allows for the loss of intermediate Am 2+ via diffusion leading to Am deposition inefficiency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Platinum and CeO 2-x Occlusion Electrodeposition at Unsupported Vulcan XC-72R for Methanol and Ethanol Oxidation Reactions in Alkaline Media

Abstract Platinum was electrodeposited in a slurry solution of CeO2 and Vulcan XC-72R to produce Pt/CeO2-x/Vulcan XC-72R catalysts by using the Rotating Disk Slurry Electrodeposition (RoDSE) Technique. The activity of the catalysts was measured towards methanol and ethanol oxidation reactions in alkaline conditions by cyclic voltammetry and chronoamperometry. The electrochemical results were compared to those obtained on commercial catalysts. Pt/CeO2-x/Vulcan XC-72R (with ~ 26 wt.% Pt) catalyst was the most active for both alcohol oxidation reactions when compared to commercial 40 wt.% and 20% /Vulcan XC-72R (ETEK) catalysts. The mass activity increases 2.0x and 2.4x for methanol and ethanol oxidation reactions when compare with 40 and 20 Pt wt. % commercial catalysts, respectively. The Pt/CeO2-x/Vulcan XC-72R catalysts contained Pt nanoparticles growth within the cerium oxide through an occlusion electrodeposition method. These effects were systematically investigated using X-ray Diffraction (XRD), High Resolution Transmission Electron Microscopy (HR-TEM), and X-ray Photoelectron Spectroscopy (XPS).

Suleiman Mahmoud, Amal↗

Electrodeposition of metals and metal/cermet composites in low gravity

Electrodeposition experiments were carried out on the bench and a KC-135 aircraft at 0.01 g in anticipation of microgravity flights on NASA's Space Transportation System Shuttle. Experimental results obtained by interferometry compare concentration gradients as a function of time in the vicinity of a reducing electrode (cathode) for Cu(+2) and Co(+2) electrodeposition cells. No difference was found between bench and 0.01 g produced gradients for a .1M CuSO4 cell, but a significant difference was noted between the gradients in a 1M CoSO4 cell even though the bench cells were operated in a nonconvecting shielded (cathode over anode) mode. The gradient for Co(+2) depletion produced at 0.01 g was greater and the entire layer was thicker than found on the bench. Neutral buoyancy/matched density codeposition experiments were performed on the bench in an attempt to physically duplicate the results of metal/cermet codepositions in microgravity. Polystyrene spheres with average diameter 11.8 microns and density approximately matching that of 1M CoSO4 were utilized to emulate nonsedimenting cermets in microgravity. The cells were operated in a shielded convectionless mode. Comparison with literature data on codeposition with stirred cells indicate significant improvement in volume percent neutral occluded in the depositing metal matrix. A multicell electrodeposition flight apparatus that has been designed, constructed and is undergoing testing is discussed.

Riley, Clyde↗