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DOE OSTI2020

Consolidating Lithiothermic-Ready Transition Metals for Li2S-Based Cathodes

Li 2 S holds a promising role as a high-capacity Li-containing cathode, circumventing use of metallic lithium in constructing next-generation batteries to replace current Li-ion batteries. However, progress of Li 2 S cathode has been plagued by its intrinsic drawbacks, including high activation potentials, poor rate performance, and rapid capacity fading during long cycling. In this work, a series of Li 2 S/transition metal (TM) nanocomposites are synthesized via a lithiothermic reduction reaction, and it is realized that the presence of TMs in Li 2 S matrix can transform electrochemical behaviors of Li 2 S. On the one hand, the incorporation of W, Mo, or Ti greatly increases electronic and ionic conductivity of Li 2 S composites and inhibits the polysulfide dissolution via the TM—S bond, effectively addressing the drawbacks of Li 2 S cathodes. In particular, Li 2 S/W and Li 2 S/Mo exhibit the highest ionic conductivity of solid-phase Li-ion conductors ever-reported: 5.44 × 10 –2 and 3.62 × 10 –2 S m –1 , respectively. On the other hand, integrating Co, Mn, and Zn turns Li 2 S into a prelithiation agent, forming metal sulfides rather than S 8 after the full charge. These interesting findings may shed light on the design of Li 2 S-based cathode materials.

25 ENERGY STORAGE↗

DOE OSTI2025

Capture of volatile RuO 4 from oxidized simulated used nuclear fuel solutions

Ruthenium is a challenging fission product in used nuclear fuel (UNF) reprocessing due to its complex redox chemistry, variable speciation in nitric acid, partial extractability, and volatility. This work presents a strategy for Ru removal based on the volatilization of RuO 4 using the strong oxidant sodium bismuthate, followed by RuO 2 deposition onto various substrates. Among the materials tested, polymer-based substrates such as polyolefin wax film (Parafilm®), exhibited superior performance, achieving up to near-quantitative Ru removal from solution. After dissolution of the substrate, 99.6% of the Ru was recovered as RuO 2 . The deposition mechanism onto the polyolefin wax film involves both physisorption and chemical reaction through oxidative cleavage of olefinic bonds within the polymer. In contrast, on inorganic substrates such as Al foil, RuO 4 undergoes incomplete surface adsorption and reduction, as confirmed by FTIR and XPS analyses. This approach remains effective under conditions of simulated oxidation of UNF solutions, selectively removing Ru while leaving other fission products in solution. As a result, capture of RuO 4 offers a practical and efficient strategy for ruthenium decontamination and recovery, offering a route for integration into existing UNF reprocessing flowsheets to enhance overall process safety and performance.

Ruthenium↗

DOE OSTI2024

Advancing Insights into Electrochemical Pre‐Treatments of Supported Nanoparticle Electrocatalysts by Combining a Design of Experiments Strategy with In Situ Characterization

Activation, break-in, and/or pre-treatment protocols are generally applied to energy conversion devices before regular operation to reach stable performance. There remains much to understand about the relationships among physical properties, performance, and electrochemical pre-treatments. Here, a design-of-experiments (DoE) strategy is employed to address this gap by demonstrating the influence of five pre-treatment parameters for carbon-supported Pt-nanoparticle catalysts on the electrocatalytic oxygen reduction reaction (ORR). A subset of pre-treatments, developed using a central composite design, are tested in a flow cell combined with an inductively-coupled plasma mass spectrometer (on-line ICP-MS). The DoE-based approach facilitates comprehensive insights from two orders of magnitude fewer experiments than a conventional grid search. The coupled on-line ICP-MS setup enables effective catalysis and real-time catalyst dissolution data. Leveraging insights from DoE for on-line ICP-MS and additional characterization, a model is built between the degradation of a multi-dimensional supported Pt surface, its performance, and applied electrochemical parameters. These investigations identify surface modifications, such as oxidation, and subsequent restructuring of Pt during pre-treatment as a primary cause of performance deterioration during ORR. By combining DoE with advanced characterization techniques, a powerful approach is demonstrated to gain a mechanistic understanding of pre-treatment protocols that can be broadly adapted to various reaction chemistries.

Platinum↗

DOE OSTI2020

The Evaluation of Chemical Decontamination for Contaminated Carbon Steel Scrap by Multiphase Treatment Process - 20249

There is a significant growth in the field of decommissioning of nuclear facilities due the fact that for a lot of them their end of life is nearing. In Taiwan, the government plans to steadily reduce the dependence on nuclear power and moves gradually towards a nuclear-free homeland. Therefore, the development of decommissioning technology becomes the significant issue for the next coming years. The decommissioning of a nuclear power plant is a long process and practical work including radiological surveys, decontamination, dismantling, and the subsequent waste management. Chemical decontamination is an important task in the decommissioning of nuclear power plants and is usually performed by circulating the chemical solution in selected systems or full systems in order to reduce dose levels. However, the decontamination of segmented metal parts is also considered to reduce the contamination to such levels that they may be disposed of at a lower classification or be unconditionally released, and it helps to achieve the goal of waste minimization and provide a more economical cost for disposal management. Chemical decontamination technology is used to remove the contaminated oxides deposited on the surface of metals by dissolving them with chemical mechanisms, such as chelation, acidic or alkaline dissolution, redox reaction and so on. Carbon steel is the major material used in systems and pipelines in the nuclear power plant, thus it is also commonly selected as the target to be decontaminated in the decommissioning process. In this study, the effectiveness of chemical decontamination is evaluated by using multiphase treatment process including the reduction and the oxidation steps. In the step of redox reaction, the oxidation state of the substance is very important. Especially metals of some oxidation states show solubility in water, which has a decisive influence on the chemical decontamination. The experiment of decontamination of metal scraps is carried out by the immersion method within a chemical solution. The relative operation parameters such as temperature, pH, and concentration of the chemical solution are recorded to demonstrate the effect of the decontamination process. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Liquid–Solid Boundaries Dominate Activity of CO 2 Reduction on Gas-Diffusion Electrodes

Electrochemical CO 2 electrolysis to produce hydrocarbon fuels or material feedstocks offers a renewable alternative to fossilized carbon sources. Gas-diffusion electrodes (GDEs), composed of solid electrocatalysts on porous supports positioned near the interface of a conducting electrolyte and CO 2 gas, have been able to demonstrate the substantial current densities needed for future commercialization. These higher reaction rates have often been ascribed to the presence of a three-phase interface, where solid, liquid, and gas provide electrons, water, and CO 2 , respectively. Conversely, mechanistic work on electrochemical reactions implicates a fully two-phase reaction interface, where gas molecules reach the electrocatalyst’s surface by dissolution and diffusion through the electrolyte. Because the discrepancy between an atomistic three-phase versus two-phase reaction has substantial implications for the design of catalysts, gas-diffusion layers, and cell architectures, the nuances of nomenclatures and governing phenomena surrounding the three-phase-region require clarification. In this paper we outline the macro, micro, and atomistic phenomena occurring within a gas-diffusion electrode to provide a focused discussion on the architecture of the often-discussed three-phase region for CO 2 electrolysis. From this information, we comment on the outlook for the broader CO 2 electroreduction GDE cell architecture.

CO2 reduction↗

DOE OSTI2023

Room Temperature Electrorefining of Rare Earth Metals from End-of-use Nd-Fe-B Magnets

Recovering rare earth elements (REE) from used permanent magnets, which contains about 30 wt.% of rare earth elements, has been persistent technological challenge. Current recycling methods relies on pyrometallurgical or hydrometallurgical processes which are energy- and chemical- intensive and not economically and environmentally viable for rare earth containing magnets. Enabling efficient and simplistic recovery and refining of REEs contained in End-of-Use (EoU) products, such as Neodymium-Iron-Boron (Nd-Fe-B) based magnets will play an important and complementary role in the total supply of REEs in the future. We designed a new electrochemical method and demonstrated a room temperature one-pot process that concurrently separates and electroplates REE from commercial Nd-Fe-B magnets. By establishing selective oxidation and reductive potential as electrochemical control parameter along with electrochemically compatible non-aqueous electrolyte system, we demonstrated selective electroleaching of lanthanides (Nd and Preseodymium (Pr)) from anode and concurrent plating as alloy at Pt cathode. The morphological and chemical evolution of the Nd-Fe-B magnets during electroleaching reveals the electrochemical stimuli and rate of dissolution depends on microstructural complexities of the Nd-Fe-B magnet. The concomitant electroplating process leads to Nd-Pr based alloy which can be used as raw metallic alloy for manufacturing new permanent magnet and other devices. Our study demonstrates a scalable separation and refining methodology, based on widely available organic electrolyte system and without any consumptive chemical use, for selective lanthanide recovery from waste magnets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Continuous Encodable Reshaping of Gold Nanocrystals through Facet Modulation

Shape control of nanocrystals (NCs) is crucial for tuning their assembly behavior and functional properties, yet the precise manipulation of facet composition remains challenging. Here, we present a nanocrystal reshaping strategy to control and modulate the facets of gold (Au) NCs. Our one-pot approach, conducted at room temperature, requires only initial Au NCs, Au 3+ ions, and surfactants, distinguishing it from conventional reduction-mediated “etching-and-regrowth” methods. Detailed structural studies using electron microscopy, small-angle X-ray scattering (SAXS), and UV−vis spectroscopy reveal the surfactant-encoded pathway for NC transformation from shaped particles to spheres and then into various polyhedral shapes while preserving the individual particles' volume. The proposed reshaping mechanism involves the dissolution of surface Au atoms into Au + complexes in the presence of Au 3+ and surfactant, followed by surfactant-guided redeposition and formation of facets with different atomic planes. Using the ethanol oxidation reaction (EOR) as a probe, we observe a quasi-linear decrease in onset potential and an increase in activity with increasing {100} facet exposure. This work broadens synthetic strategies by offering precise NC reshaping and facet control.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Uncovering phase transformation, morphological evolution, and nanoscale color heterogeneity in tungsten oxide electrochromic materials

Controlling the electrochemical interfacial processes that govern the durability of electrochromic devices represents a key challenge in developing sustainable and cost-effective smart windows. Here, we revisit the classical tungsten trioxide (WO 3 ) materials as a platform to uncover the previously unknown interrelationship between phase transformation, morphological evolution, and nanoscale color heterogeneity in these materials. Through synchrotron/electron spectroscopic and imaging analyses, we report that the WO 3 –electrolyte interface is influenced by the tungsten dissolution and redeposition during the electrochemical cycling. The tungsten redeposition provokes the in situ crystal growth, which ultimately leads to the phase transformation from the semicrystalline WO 3 to a nanoflake-shaped, proton-trapped tungsten trioxide dihydrate (H x WO 3 · 2 H 2 O). The multidimensional quantification of the electronic structure reveals that the tungsten reduction caused by the proton trapping is heterogeneous at the nanometric scale and is responsible for the nanoscale color heterogeneity. The interplay between phase transformation, morphological evolution, and nanoscale color heterogeneity results in degraded optical modulation, switching kinetics, coulombic efficiency, and bleached-state transparency. Our results highlight that the high interfacial reactivity near the electrode surface may be the underlying mechanism for undesired bulk structural changes of electrochromic materials, and calls for fundamental studies in probing and controlling the electrode–electrolyte interfacial processes in electrochromic devices.

36 MATERIALS SCIENCE↗

NASA NTRS2013

Wireless Chalcogenide Nanoionic-Based Radio-Frequency Switch

A new nonvolatile nanoionic switch is powered and controlled through wireless radio-frequency (RF) transmission. A thin layer of chalcogenide glass doped with a metal ion, such as silver, comprises the operational portion of the switch. For the switch to function, an oxidizable electrode is made positive (anode) with respect to an opposing electrode (cathode) when sufficient bias, typically on the order of a few tenths of a volt or more, is applied. This action causes the metal ions to flow toward the cathode through a coordinated hopping mechanism. At the cathode, a reduction reaction occurs to form a metal deposit. This metal deposit creates a conductive path that bridges the gap between electrodes to turn the switch on. Once this conductive path is formed, no further power is required to maintain it. To reverse this process, the metal deposit is made positive with respect to the original oxidizable electrode, causing the dissolution of the metal bridge thereby turning the switch off. Once the metal deposit has been completely dissolved, the process self-terminates. This switching process features the following attributes. It requires very little to change states (i.e., on and off). Furthermore, no power is required to maintain the states; hence, the state of the switch is nonvolatile. Because of these attributes the integration of a rectenna to provide the necessary power and control is unique to this embodiment. A rectenna, or rectifying antenna, generates DC power from an incident RF signal. The low voltages and power required for the nanoionic switch control are easily generated from this system and provide the switch with a novel capability to be operated and powered from an external wireless device. In one realization, an RF signal of a specific frequency can be used to set the switch into an off state, while another frequency can be used to set the switch to an on state. The wireless, miniaturized, and nomoving- part features of this switch make it suitable for applications such as integration into garments, RFID (radio-frequency identification) tags, and conformal structures (e.g., aircraft wings, sounding rockets contours, etc). In the case of RFID tags the innovation will provide countermeasures to attempts for identity theft and other uninvited attempts for retrieval of information. It could also be applicable to the automotive industry as well as the aerospace industry for collision avoidance and phased array radar systems, respectively

Nessel, James↗

DOE OSTI2024

Plastic Parallel Pathways Platform- 4P Model

The U.S. generates 42 million metric tons of plastic waste each year - the most of any country - of which less than 9% is recycled. This represents an estimated loss of $2.3 billion and 3.4 EJ embodied energy per year. Plastic use reduction, reuse and recycling are thus increasingly important, but making informed policy and research decisions within this space can be challenging given the diverse range of available solutions. Various recycling and waste management options are available for plastics, such as conversion into energy (incineration, pyrolysis, gasification), conversion to lower- or higher-grade plastics (mechanical recycling, chemical or enzymatic depolymerization processes, dissolution) or up-cycling to feedstock chemicals (photo/electro/catalytic methods, pyrolysis, gasification). While many previous publications have investigated a subset of these options, there is currently no modelling platform that can quantitatively assess and compare the economic and environmental impacts of all these different plastic management pathways and their respective products simultaneously. To directly compare the benefits and disadvantages of plastic-to-x technologies, we propose a novel analysis framework: the Plastic Parallel Pathways Platform (4P). 4P will model a systems analysis framework for capturing plastic material flows processed via different waste management scenarios. The total economic cost and greenhouse gas emissions (as well as additional economic, energetic, and environmental metrics indicators) of a given scenario will be calculated enabling comparison to other scenarios, thereby informing decisions on plastic recycling pathways.

circular economy↗

DOE OSTI2021

Investigating the durability of a direct methanol fuel cell equipped with commercial Platinum Group Metal-free cathodic electro-catalysts

For the first time a long-term (500 h) durability study in direct methanol fuel cells (DMFCs) is carried out on a Platinum Group Metal-free (PGM-free) cathodic electro-catalyst commercially available on market. The electro-catalyst is tested for 500 h at a fixed cell voltage (0.3 V), recording the polarization curves during the operation. A drastic decrease in performance is observed after the first 100 h (from 220 to 75 mA cm –2 ); afterwards, the decrease is flatter, passing from 75 to 25 mA cm –2 (at 500 h). The causes of this performance degradation are investigated by postmortem physicochemical analyzes, such as X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with X-ray energy dispersive analysis (EDX). Finally, possible reasons of degradation are indicated to be PGM-free catalyst aggregation, carbon and nitrogen species decrease, Ruthenium dissolution and migration from the anode to the cathode, poisoning both membrane and cathode catalyst.

25 ENERGY STORAGE↗

DOE OSTI2020

Fluorination effect for stabilizing cationic and anionic redox activities in cation-disordered cathode materials

We see that cation-disordered Li-excess cathodes with oxygen redox reactions are promising candidates for high-energy-density Li ion batteries. Nevertheless, the oxygen redox process that is required for the high capacity often comes with the oxygen loss, which leads to severe capacity degradation and voltage decay. In this work, we have successfully synthesized a series of Li-excess cation-disordered cathodes (Li 1.2 Mn 0.4+x Ti 0.4-x O 2-x Fx) (0 ≤ x ≤ 0.2) with different fluorine (F) contents. The electrochemical performance results show that the Li 1.2 Mn 0.55 Ti 0.25 O 1.85 F 0.15 (LMTOF0.15) exhibits the highest reversible capacity (275 mAh g -1 , under 30 mA g -1 ), cyclability, and voltage retentions. The mapping of resonant inelastic X-ray scattering (mRIXS) and differential electrochemical mass spectroscopy (DEMS) results reveal that the fluorination enhances the reversible lattice oxygen redox reaction while suppressing irreversible gas release and surface reactions. The X-ray Absorption Spectroscopy (XAS) during the initial two cycles shows that F-substitution alleviates the reduction of the Mn valence state during the whole (dis)charge processes in the bulk and at the surface of the material, results in higher average discharge voltage. In addition, the introduction of F improves the structural stability and suppresses local lattice distortion of the material. Therefore, LMTOF 0.15 is able to cycle with smaller polarization, less interfacial side reaction and Mn dissolution, and therefore results in enhanced cyclability. This work provides a comprehensive understanding of the fluorination effect on the cationic and anionic redox activities in cation-disordered Li-excess cathodes.

25 ENERGY STORAGE↗

DOE OSTI2024

Metal-facilitated, sustainable nitroarene hydrogenation under ambient conditions

Hydrogenation is a critical reaction in the chemical industry, yielding a range of important compounds such as fine chemicals, pharmachemicals and agrochemicals. However, conventional hydrogenation typically requires pressurized hydrogen, high temperatures and involves noble metal catalysts. Here, we proposed a two-step hydrogenation process, utilizing water as the hydrogen source for the industrially important reduction of nitroarenes to anilines. A metal or reduced metal oxide, which can be obtained from solar thermal or electrochemical reduction, acts as the active site for nitrobenzene adsorption, H 2 O dissociation and in-situ hydrogen generation. Among the 15 metal and reduced metal oxides investigated, Zn and Sn emerged as highly efficient catalysts for the reduction of a broad range of organic nitro compounds under mild conditions, with H 2 utilization efficiency 1-2 orders of magnitude above the state-of-the-art. The presented protocol provides extra dimensions for designing and optimizing conventional hydrogenation process with an alternative pathway. The reactive hydrogen atoms generated in-situ effectively overcome the barriers associated with hydrogen gas dissolution and its subsequent dissociation on the catalyst surface, thereby greatly enhancing the overall effectiveness for the hydrogenation reaction. This research potentially establishes a sustainable, generally applicable alternative to conventional hydrogenation methods, simultaneously presenting a viable solution for renewable energy storage.

25 ENERGY STORAGE↗

DOE OSTI2024

Topological Considerations in Electrolyte Additives for Passivating Silicon Anodes with Hybrid Solid–Electrolyte Interphases

Unlike most anodes used in high energy density batteries, lithiated Si does not form long-lasting passivating solid-electrolyte interphases (SEI) during formation or on charge due to SEI delamination, reconstruction, or dissolution. As a result, electrolyte degradation is continuous and results in a permanent loss of the Li inventory, shortening the useful life of the battery. Here, in this study, we show that perfluoroether electrolyte additives featuring either sulfonyl fluorides or trifluorovinyl ethers, when introduced in prescribed amounts to locally superconcentrated electrolytes, exhibit preferential reactivity at Si during formation due to their higher reduction potential than salts and solvents, creating a hybrid SEI that is simultaneously enriched with LiF and organics tethered to the reactive functionality. While both reactive motifs are effective in creating a hybrid SEI, perfluoroether additives bearing sulfonyl fluorides show more substantial integration. More important, however, is the combined influence of additive topology on anchoring efficacy and tether flexibility between anchoring sites on SEI resiliency. Top-performing Si|LFP cells featuring ditopic additive-enriched SEI improve capacity retention by as much as 45% over 100 cycles when compared to additive-free cells.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Pt–Co truncated octahedral nanocrystals: a class of highly active and durable catalysts toward oxygen reduction

We report a facile and scalable synthesis of Pt–Co truncated octahedral nanocrystals (TONs) by employing Pt(acac) 2 and Co(acac) 2 as precursors, together with CO molecules and Mn atoms derived from the decomposition of Mn 2 (CO) 10 as a reductant and a {111} facet-directing agent, respectively. Both the composition and yield of the Pt–Co TONs could be varied through the introduction of CHCl 3 . When tested at 80 °C using membrane electrode assembly (MEA), the 4 nm Pt 2.6 Co TONs gave a mass activity of 294 A g Pt –1 at beginning-of-life (BOL) and it increased to 384 A g Pt –1 during recovery cycles. The mass activity at BOL only dropped by 24% after 30 000 voltage cycles at end-of-life (EOL) in a metal dissolution accelerated stress test. The Pt 2.6 Co/C catalyst outperformed the commercial TKK Pt 3 Co/C (230 A g Pt –1 at BOL and 40% loss after 30 000 cycles at EOL) in terms of both activity and durability. Our systematic analysis suggested that the enhancement in activity can be attributed to the combination of small, uniform size and well-defined {111} facets. This new class of catalysts holds promise for applications in proton-exchange membrane fuel cells.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Silver Electrolysis for Disinfection of Spacecraft Potable Water: 2023 Update

Anodic dissolution of silver electrodes, or “silver electrolysis,” is being investigated as a means of introducing biocidal silver into potable water on exploration spacecraft. Last year’s paper reported a fault condition termed “electrode bridging,” in which silver deposits on interelectrode wetted materials, eventually bridging the electrode gap and providing an alternate conduction pathway that diminishes the silver output of the reactor. Since then, two strategies have been developed that prevent this fault from occurring: 1) increasing the frequency of polarity reversal and 2) separating the active surface of the electrode from the interelectrode wetted material. These strategies were tested independently, and in both cases, the reactor performed as expected with no occurrence of bridging for at least one crew-year equivalent of cumulative operation. Additional tests were conducted at varying levels of influent dissolved oxygen to better understand the nature of the cathode reaction and its impact on reactor performance. Results indicate that the primary cathode reaction is the reduction of dissolved oxygen, which could imply a dependence of reactor performance on dissolved oxygen concentration. However, it was found that at the typical oxygen concentrations anticipated for spacecraft processed water, the impact on silver electrolysis performance was negligible. Finally, multiphysics modelling of the reactor fluid mechanics and electrochemistry was undertaken to provide the capability to optimize the design of a future reactor prototype.

silver electrolysis↗

NASA NTRSDate not supplied

Silver Electrolysis for Disinfection of Spacecraft Potable Water: 2023 Update

silver electrolysis↗

DOE OSTI2021

In Situ Polymerization of Polypyrrole and Polyaniline on the Surface of Magnetic Molybdenum Trioxide Nanoparticles: Implications for Water Treatment

Photocatalyst dissolution greatly diminishes the usability of photocatalysts in water treatments. Coating conductive polymers on the surface of photocatalysts can reduce dissolution without compromising the photocatalytic properties of the material. In this investigation, polypyrrole (PPy) and polyaniline (PANI) were used to coat two magnetic MoO 3 nanoparticles with different surface chemistries. The polymer-coated MoO 3 @Fe 3 O 4 nanoparticles were synthesized by optimizing the mole fractions of PPy or PANI, MoO 3 , and Fe 3 O 4 . The optimized PPy@ MoO 3 @Fe 3 O 4 (PMF1) and PANI@MoO 3 @Fe 3 O 4 (PMF2) resulted in 95.39 and 75.98% methylene blue dye removal, respectively. MoO 3 dissolutions of 4.12 and 5.6% were obtained for PMF1 and PMF2, respectively, demonstrating the reduced solubility of the coated nanoparticles as compared to their uncoated counterparts (7.87% for MF1 and 18.1% for MF2). In situ small-angle neutron scattering (SANS) was utilized to investigate the polymerization kinetics of PPy and PANI on nanoparticles. The results revealed that an increase in base material oxygen vacancies resulted in the reduction of both the polymer size and the polymerization rate. Furthermore, this study demonstrated that SANS provides valuable insights into the polymer growth mechanisms on nanoparticle surfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗