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Keywords = cathode recovery

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16 pages, 3829 KiB  
Article
Process Development for Concentrating Valuable Metals Present in the Non-Valorized Solid Fractions from Urban Mining
by Nour-Eddine Menad and Alassane Traoré
Metals 2025, 15(8), 834; https://doi.org/10.3390/met15080834 (registering DOI) - 26 Jul 2025
Viewed by 231
Abstract
Global resource consumption continues to grow each year, exerting increasing pressure on their availability. This trend could lead to a shortage of raw materials in the coming years. Aware of the risks associated with this situation, the European Union has implemented policies and [...] Read more.
Global resource consumption continues to grow each year, exerting increasing pressure on their availability. This trend could lead to a shortage of raw materials in the coming years. Aware of the risks associated with this situation, the European Union has implemented policies and strategies aimed at diversifying its supply sources, including waste recycling. In this context, the present study was conducted with the objective of developing innovative processes to concentrate valuable metals present in the non-recovered fractions of waste electrical and electronic equipment (WEEE). Three types of samples were studied: washing table residues (WTRs), printed circuit boards (PCBs), and powders from cathode-ray tube screens (CRT powders). Several separation techniques, based on the physical properties of the elements, were implemented, including electrostatic separation, magnetic separation, and density and gravity-based separations. The results obtained are promising. For WTRs and PCBs, the recovery rates of targeted metals (Cu, Al, Pb, Zn, Sn) reached approximately 91% and 80%, respectively. In addition to these metals, other valuable metals, present in significant quantities, deserve further exploration. Regarding CRT powders, the performances are also encouraging, with recovery rates of 54.7% for zinc, 57.1% for yttrium, and approximately 71% for europium. Although these results are satisfactory, optimizations are possible to maximize the recovery of these critical elements. The techniques implemented have demonstrated their effectiveness in concentrating target metals in the treated fractions. These results confirm that recycling constitutes a viable alternative to address resource shortages and secure part of the supplies needed for the European Union’s industry. Full article
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18 pages, 2688 KiB  
Article
Eco-Friendly Leaching of Spent Lithium-Ion Battery Black Mass Using a Ternary Deep Eutectic Solvent System Based on Choline Chloride, Glycolic Acid, and Ascorbic Acid
by Furkan Nazlı, Işıl Hasdemir, Emircan Uysal, Halide Nur Dursun, Utku Orçun Gezici, Duygu Yesiltepe Özçelik, Fırat Burat and Sebahattin Gürmen
Minerals 2025, 15(8), 782; https://doi.org/10.3390/min15080782 - 25 Jul 2025
Viewed by 394
Abstract
Lithium-ion batteries (LiBs) are utilized in numerous applications due to advancements in technology, and the recovery of end-of-life (EoL) LiBs is imperative for environmental and economic reasons. Pyrometallurgical and hydrometallurgical methods have been used in the recovery of metals such as Li, Co, [...] Read more.
Lithium-ion batteries (LiBs) are utilized in numerous applications due to advancements in technology, and the recovery of end-of-life (EoL) LiBs is imperative for environmental and economic reasons. Pyrometallurgical and hydrometallurgical methods have been used in the recovery of metals such as Li, Co, and Ni in the EoL LiBs. Hydrometallurgical methods, which have been demonstrated to exhibit higher recovery efficiency and reduced energy consumption, have garnered increased attention in recent research. Inorganic acids, including HCl, HNO3, and H2SO4, as well as organic acids such as acetic acid and citric acid, are employed in the hydrometallurgical recovery of these metals. It is imperative to acknowledge the environmental hazards posed by these acids. Consequently, solvometallurgical processes, which involve the use of organic solvents with minimal or no water, are gaining increasing attention as alternative or complementary techniques to conventional hydrometallurgical processes. In the context of solvent systems that have been examined for a range of solvometallurgical methods, deep eutectic solvents (DESs) have garnered particular interest due to their low toxicity, biodegradable nature, tunable properties, and efficient metal recovery potential. In this study, the leaching process of black mass containing graphite, LCO, NMC, and LMO was carried out in a short time using the ternary DES system. The ternary DES system consists of choline chloride (ChCl), glycolic acid (GLY), and ascorbic acid (AA). As a result of the leaching process of cathode powders in the black mass without any pre-enrichment process, Li, Co, Ni, and Mn elements passed into solution with an efficiency of over 95% at 60 °C and within 1 h. Moreover, the kinetics of the leaching process was investigated, and Density Functional Theory (DFT) calculations were used to explain the leaching mechanism. Full article
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12 pages, 23410 KiB  
Article
Recycling and Separation of Valuable Metals from Spent Cathode Sheets by Single-Step Electrochemical Strategy
by Neng Wei, Yaqun He, Guangwen Zhang, Jiahao Li and Fengbin Zhang
Separations 2025, 12(7), 178; https://doi.org/10.3390/separations12070178 - 5 Jul 2025
Viewed by 276
Abstract
The conventional spent lithium-ion batteries (LIBs) recycling method suffers from complex processes and excessive chemical consumption. Hence, this study proposes an electrochemical strategy for achieving reductant-free leaching of high-valence transition metals and efficient separation of valuable components from spent cathode sheets (CSs). An [...] Read more.
The conventional spent lithium-ion batteries (LIBs) recycling method suffers from complex processes and excessive chemical consumption. Hence, this study proposes an electrochemical strategy for achieving reductant-free leaching of high-valence transition metals and efficient separation of valuable components from spent cathode sheets (CSs). An innovatively designed sandwich-structured electrochemical reactor achieved efficient reductive dissolution of cathode materials (CMs) while maintaining the structural integrity of aluminum (Al) foils in a dilute sulfuric acid system. Optimized current enabled leaching efficiencies exceeding 93% for lithium (Li), cobalt (Co), manganese (Mn), and nickel (Ni), with 88% metallic Al foil recovery via cathodic protection. Multi-scale characterization systematically elucidated metal valence evolution and interfacial reaction mechanisms, validating the technology’s tripartite innovation: simultaneous high metal extraction efficiency, high value-added Al foil recovery, and organic removal through single-step electrochemical treatment. The process synergized the dissolution of CM particles and hydrogen bubble-induced physical liberation to achieve clean separation of polyvinylidene difluoride (PVDF) and carbon black (CB) layers from Al foil substrates. This method eliminates crushing pretreatment, high-temperature reduction, and any other reductant consumption, establishing an environmentally friendly and efficient method of comprehensive recycling of battery materials. Full article
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29 pages, 7261 KiB  
Review
Critical Pathways for Transforming the Energy Future: A Review of Innovations and Challenges in Spent Lithium Battery Recycling Technologies
by Zhiyong Lu, Liangmin Ning, Xiangnan Zhu and Hao Yu
Materials 2025, 18(13), 2987; https://doi.org/10.3390/ma18132987 - 24 Jun 2025
Viewed by 720
Abstract
In the wake of global energy transition and the “dual-carbon” goal, the rapid growth of electric vehicles has posed challenges for large-scale lithium-ion battery decommissioning. Retired batteries exhibit dual attributes of strategic resources (cobalt/lithium concentrations several times higher than natural ores) and environmental [...] Read more.
In the wake of global energy transition and the “dual-carbon” goal, the rapid growth of electric vehicles has posed challenges for large-scale lithium-ion battery decommissioning. Retired batteries exhibit dual attributes of strategic resources (cobalt/lithium concentrations several times higher than natural ores) and environmental risks (heavy metal pollution, electrolyte toxicity). This paper systematically reviews pyrometallurgical and hydrometallurgical recovery technologies, identifying bottlenecks: high energy/lithium loss in pyrometallurgy, and corrosion/cost/solvent regeneration issues in hydrometallurgy. To address these, an integrated recycling process is proposed: low-temperature physical separation (liquid nitrogen embrittlement grinding + froth flotation) for cathode–anode separation, mild roasting to convert lithium into water-soluble compounds for efficient metal oxide separation, stepwise alkaline precipitation for high-purity lithium salts, and co-precipitation synthesis of spherical hydroxide precursors followed by segmented sintering to regenerate LiNi1/3Co1/3Mn1/3O2 cathodes with morphology/electrochemical performance comparable to virgin materials. This low-temperature, precision-controlled methodology effectively addresses the energy-intensive, pollutive, and inefficient limitations inherent in conventional recycling processes. By offering an engineered solution for sustainable large-scale recycling and high-value regeneration of spent ternary lithium ion batteries (LIBs), this approach proves pivotal in advancing circular economy development within the renewable energy sector. Full article
(This article belongs to the Section Energy Materials)
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20 pages, 2139 KiB  
Article
Optimized Ammonia Leaching and Energy-Efficient Stripping for Lithium and Cobalt Recovery from Spent LiCoO2 Cathodes
by Aisulu Batkal, Kaster Kamunur, Lyazzat Mussapyrova, Bagdatgul Milikhat and Rashid Nadirov
Metals 2025, 15(7), 690; https://doi.org/10.3390/met15070690 - 20 Jun 2025
Viewed by 258
Abstract
This study investigates the optimization of an ammonia-based leaching process for the recovery of lithium and cobalt from spent LiCoO2 cathodes, coupled with an energy-efficient ammonia stripping approach. Kinetic analysis revealed that both lithium and cobalt extraction follow pseudo-first-order kinetics, with activation [...] Read more.
This study investigates the optimization of an ammonia-based leaching process for the recovery of lithium and cobalt from spent LiCoO2 cathodes, coupled with an energy-efficient ammonia stripping approach. Kinetic analysis revealed that both lithium and cobalt extraction follow pseudo-first-order kinetics, with activation energies of 76.54 kJ/mol and 97.22 kJ/mol, respectively, indicating a chemically controlled process. Optimal leaching conditions were established at 6 M NH3, 1.5 M (NH4)2CO3, liquid-to-solid ratio of 10:1, and 70 °C for 5 h, achieving 82.5% lithium and 96.1% cobalt recovery. The ammonia stripping process was optimized for energy efficiency, with operations at 95–98 °C providing the best balance between rapid NH3 removal and energy consumption. At 98 °C, energy demand was reduced to ~282 kJ/mol, a sevenfold improvement over lower temperature operations. A stepwise separation strategy was developed, involving selective lithium precipitation at pH 10.7–10.8, followed by controlled ammonia stripping to precipitate cobalt at pH 8.8–9.0. This integrated approach offers a promising alternative to conventional acid-based recycling methods, combining high metal recovery with improved energy efficiency and reagent recyclability. Full article
(This article belongs to the Section Extractive Metallurgy)
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17 pages, 3264 KiB  
Article
Potential of Textile Wastewater Decolorization Using Cation Exchange Membrane Electrolysis Coupled with Magnesium Salt Precipitation (CEM-MSP)
by Yujing Zhao, Nuo Cheng, Ruihan Jiang, Jian Jiao, Chen Chen, Jiahao Liang, Longfeng Hu, Hesong Wang and Jinlong Wang
Water 2025, 17(12), 1785; https://doi.org/10.3390/w17121785 - 14 Jun 2025
Viewed by 364
Abstract
To overcome the low efficiency, high cost and less environmentally friendly limitations in existing textile wastewater disposal technology, an innovative approach of cation exchange membrane electrolysis coupled with magnesium salt precipitation (CEM-MSP) was implemented. This method simultaneously achieved the high-efficiency adsorption decolorization of [...] Read more.
To overcome the low efficiency, high cost and less environmentally friendly limitations in existing textile wastewater disposal technology, an innovative approach of cation exchange membrane electrolysis coupled with magnesium salt precipitation (CEM-MSP) was implemented. This method simultaneously achieved the high-efficiency adsorption decolorization of dyes and the recovery of lye. The results indicated that cation exchange membrane electrolysis with MgSO4 added to the anode chamber (CEM-EA) exhibited excellent decolorization performance on DB86 dye and achieved low residual Mg2+ concentration. Furthermore, the adsorption mechanism of Mg(OH)2 on DB86 was systematically investigated. The adsorption process fitted with the first-order kinetic, where the adsorption of DB86 by Mg(OH)2 was dominated by electrostatic attraction. Detailed comparison of the four systems demonstrated that CEM-EA was superior to the single magnesium addition method (85.24%) or the stand-alone membrane electrolysis method (10.36%), with 99% decolorization efficiency. In comparison to the cation exchange membrane electrolysis with MgSO4 added to the cathode chamber (CEM-EC), the CEM-EA could diminish the Mg2+ concentration in the effluent to facilitate the lye recovery while guaranteeing the decolorization efficiency. In addition, the DB86 adsorption behavior during the formation of Mg(OH)2 in the cathode chamber was investigated. The Mg(OH)2 particles were relatively dense copper-blue agglomerates with a thin lamellar layer on the surface. Notably, only slight mass contamination was observed on the cation exchange membrane (CEM) surface after multiple cycles. Minor CEM contamination illustrated the stable treatment efficiency of the CEM-EA after several cycles. This study constructed a novel approach integrating membrane electrolysis with magnesium salt precipitation, delivering valuable technical solutions for textile wastewater disposal. Full article
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13 pages, 2405 KiB  
Article
A Closed-Loop Process for Rapid and Selective Lithium Extraction and Resynthesis from Spent LiFePO4 Batteries
by Ruijing Liu, Yuxiao Liu, Jianjiang Li, Yuanlin Chen, Yule Zhu, Kunzheng Zhang, Shuxian Zhao, Liang Du, Xiaoyi Zhu and Lei Zhang
Molecules 2025, 30(12), 2587; https://doi.org/10.3390/molecules30122587 - 13 Jun 2025
Viewed by 480
Abstract
The rapid growth of lithium iron phosphate (LiFePO4, LFP)-based lithium-ion batteries in energy storage raises urgent challenges for resource recovery and environmental protection. In this study, we propose a novel method for rapid and selective lithium extraction and the resynthesis of [...] Read more.
The rapid growth of lithium iron phosphate (LiFePO4, LFP)-based lithium-ion batteries in energy storage raises urgent challenges for resource recovery and environmental protection. In this study, we propose a novel method for rapid and selective lithium extraction and the resynthesis of cathodes from spent LFP batteries, aiming to achieve an economically feasible and efficient recycling process. In this process, a selective leaching H2SO4-H2O2 system is employed to rapidly and selectively extract lithium, achieving a leaching efficiency of 98.72% within just 10 min. Through an exploration of the precipitation conditions of the lithium-containing solution, high-purity Li2CO3 is successfully obtained. The recovered FePO4 and Li2CO3 are then used to resynthesize LFP cathode materials through a carbon-thermal reduction method. A preliminary economic analysis reveals that the disposal cost of spent LFP batteries is approximately USD 2.63 per kilogram, while the value of regenerated LFP reaches USD 4.46, highlighting the economic advantages of this process. Furthermore, with an acid-to-lithium molar ratio of only 0.57—just slightly above the stoichiometric 0.5—the process requires minimal acid usage, offering clear environmental benefits. Overall, this work presents a green, efficient, and economically viable strategy for recycling spent LFP batteries, showcasing strong potential for industrial application and contributing significantly to the development of a circular lithium battery economy. Full article
(This article belongs to the Section Electrochemistry)
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19 pages, 289 KiB  
Review
Solvometallurgy as Alternative to Pyro- and Hydrometallurgy for Lithium, Cobalt, Nickel, and Manganese Extraction from Black Mass Processing: State of the Art
by Alessandra Zanoletti, Alberto Mannu and Antonella Cornelio
Materials 2025, 18(12), 2761; https://doi.org/10.3390/ma18122761 - 12 Jun 2025
Viewed by 617
Abstract
The rapid growth in lithium-ion battery (LIB) demand has underscored the urgent need for sustainable recycling methods to recover critical metals such as lithium, cobalt, nickel, and manganese. Traditional pyrometallurgical and hydrometallurgical approaches often suffer from high energy consumption, environmental impact, and limited [...] Read more.
The rapid growth in lithium-ion battery (LIB) demand has underscored the urgent need for sustainable recycling methods to recover critical metals such as lithium, cobalt, nickel, and manganese. Traditional pyrometallurgical and hydrometallurgical approaches often suffer from high energy consumption, environmental impact, and limited metal selectivity. As an emerging alternative, solvometallurgy, and in particular the use of low-melting mixtures solvents, including deep eutectic solvents, offers a low-temperature, tunable, and potentially more environmentally compatible pathway for black mass processing. This review presents a comprehensive assessment of the recent advances (2020–2025) in the application of LoMMSs for metal recovery from LCO and NCM cathodes, analyzing 71 reported systems across binary, ternary, hydrated, and non-ChCl-based solvent families. Extraction efficiencies, reaction kinetics, coordination mechanisms, and solvent recyclability are critically evaluated, highlighting how solvent structure influences performance and selectivity. Particular attention is given to the challenges of lithium recovery, solvent degradation, and environmental trade-offs such as energy usage, waste generation, and chemical stability. A comparative synthesis identifies the most promising systems based on their mechanistic behavior and industrial relevance. The future outlook emphasizes the need for greener formulations, enhanced lithium selectivity, and life-cycle integration to support circular economy goals in battery recycling. Full article
(This article belongs to the Special Issue Systems and Materials for Recycling Spent Lithium-Ion Batteries)
20 pages, 1982 KiB  
Article
Hydrogen Production from Winery Wastewater Through a Dual-Chamber Microbial Electrolysis Cell
by Ana Baía, Alonso I. Arroyo-Escoto, Nuno Ramos, Bilel Abdelkarim, Marta Pereira, Maria C. Fernandes, Yifeng Zhang and Annabel Fernandes
Energies 2025, 18(12), 3043; https://doi.org/10.3390/en18123043 - 9 Jun 2025
Viewed by 526
Abstract
This study explores the feasibility of producing biohydrogen from winery wastewater using a dual-chamber microbial electrolysis cell (MEC). A mixed microbial consortium pre-adapted to heavy-metal environments and enriched with Geobacter sulfurreducens was anaerobically cultivated from diverse waste streams. Over 5000 h of development, [...] Read more.
This study explores the feasibility of producing biohydrogen from winery wastewater using a dual-chamber microbial electrolysis cell (MEC). A mixed microbial consortium pre-adapted to heavy-metal environments and enriched with Geobacter sulfurreducens was anaerobically cultivated from diverse waste streams. Over 5000 h of development, the MEC system was progressively adapted to winery wastewater, enabling long-term electrochemical stability and high organic matter degradation. Upon winery wastewater addition (5% v/v), the system achieved a sustained hydrogen production rate of (0.7 ± 0.3) L H2 L−1 d−1, with an average current density of (60 ± 4) A m−3, and COD removal efficiency exceeding 55%, highlighting the system’s resilience despite the presence of inhibitory compounds. Coulombic efficiency and cathodic hydrogen recovery reached (75 ± 4)% and (87 ± 5)%, respectively. Electrochemical impedance spectroscopy provided mechanistic insight into charge transfer and biofilm development, correlating resistive parameters with biological adaptation. These findings demonstrate the potential of MECs to simultaneously treat agro-industrial wastewaters and recover energy in the form of hydrogen, supporting circular resource management strategies. Full article
(This article belongs to the Special Issue Advanced Materials and Technologies for Hydrogen Evolution)
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15 pages, 2067 KiB  
Article
Innovative Integration of Citric Acid Leaching and Electrodialysis for Selective Lithium Recovery from NMC Cathode Material
by Soukayna Badre-Eddine, Laurence Muhr and Alexandre Chagnes
Metals 2025, 15(6), 598; https://doi.org/10.3390/met15060598 - 27 May 2025
Viewed by 669
Abstract
With the growing demand for metals driven by technological advancements and population growth, recycling lithium-ion batteries has become vital for protecting the environment and recovering valuable materials. Developing sustainable recycling technologies is now more essential than ever. This paper focuses on using electrodialysis [...] Read more.
With the growing demand for metals driven by technological advancements and population growth, recycling lithium-ion batteries has become vital for protecting the environment and recovering valuable materials. Developing sustainable recycling technologies is now more essential than ever. This paper focuses on using electrodialysis to process a leach solution of LiNi0.33Mn0.33Co0.33O2 (NMC 111) cathode materials leached with citric acid. This study demonstrates that the complexing properties of citrate anions contribute to the efficient separation of Li from Ni, Co, and Mn by electrodialysis. This is achieved by promoting the formation of anionic species for Ni, Co, and Mn while maintaining Li in its cationic form. The leach solution was produced under the following optimal experimental conditions to reach a final pH of 5 and high leaching efficiency: a citric acid concentration of 1 mol L−1, a leaching temperature of 45 °C, a leaching time of 5 h, a liquid/solid ratio of 100 g/L, and 8 vol.% H2O2. These conditions resulted in leaching efficiencies of 89.3% for Ni, 95.1% for Co, 77.1% for Mn, and 92.9% for Li. This solution led to the formation of a lithium-rich supernatant and a precipitate. The supernatant was then used as the feed solution for electrodialysis. Pure lithium was successfully separated with a faradic efficiency of 71.4% with a commercial cation-exchange membrane. This strategy enables selective lithium recovery while minimizing membrane fouling during the process. Full article
(This article belongs to the Special Issue Feature Papers in Extractive Metallurgy)
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15 pages, 3012 KiB  
Article
Efficient Extraction of Lithium, Cobalt, and Nickel from Nickel-Manganese-Cobalt Oxide Cathodes with Cholin Chloride/Pyrogallol-Based Deep Eutectic Solvent
by Aisulu Batkal, Kaster Kamunur, Lyazzat Mussapyrova, Yerzhan Mukanov and Rashid Nadirov
Recycling 2025, 10(3), 88; https://doi.org/10.3390/recycling10030088 - 3 May 2025
Viewed by 918
Abstract
This study explores the use of a deep eutectic solvent (DES) composed of choline chloride and pyrogallol (1:1 molar ratio) for the recovery of lithium, cobalt, and nickel from spent lithium-ion battery cathodes based on LiNi0.33Co0.33Mn0.33O2 [...] Read more.
This study explores the use of a deep eutectic solvent (DES) composed of choline chloride and pyrogallol (1:1 molar ratio) for the recovery of lithium, cobalt, and nickel from spent lithium-ion battery cathodes based on LiNi0.33Co0.33Mn0.33O2 (NMC111). The DES exhibits moderate viscosity, intrinsic redox activity, and strong complexation ability, enabling efficient metal dissolution under mild conditions. The effects of both temperature (50–80 °C) and time (up to 12 h) on leaching efficiency were systematically investigated. Optimal leaching parameters—80 °C, 8 h, and a liquid-to-solid ratio of 50—yielded extraction efficiencies of 92% for Li, 85% for Co, and 88% for Ni. Kinetic modeling indicated pseudo-first-order behavior with activation energies of 26.6, 22.1, and 25.2 kJ/mol for Li, Co, and Ni, respectively. Mechanistic analysis confirmed the dual role of pyrogallol as both reducing agent (facilitating Co3+ to Co2+ conversion) and chelating ligand. Full article
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19 pages, 5650 KiB  
Article
Study of Operational Parameters on Indium Electrowinning Using a Ti Cathode
by Carla Lupi, Erwin Ciro and Alessandro Dell’Era
Materials 2025, 18(9), 2089; https://doi.org/10.3390/ma18092089 - 2 May 2025
Viewed by 468
Abstract
Indium, widely used as indium-tin oxide (ITO), has been recognized as a strategical metal for audiovisual, optoelectronic systems, semiconductors and photovoltaic fields. An increasing shortage and unflexible mineral supply have led indium to be recovered from secondary sources, such as waste electrical and [...] Read more.
Indium, widely used as indium-tin oxide (ITO), has been recognized as a strategical metal for audiovisual, optoelectronic systems, semiconductors and photovoltaic fields. An increasing shortage and unflexible mineral supply have led indium to be recovered from secondary sources, such as waste electrical and electronic equipment (WEEE). The main step for indium hydrometallurgical recovery from WEEE is the electrowinning process using sulfate baths, giving lower environmental impact and improved workplace safety conditions. In this investigation, a titanium cathode has been employed for the study of the indium electrowinning process in a sulfate-based bath. This study was focused on analyzing current efficiency (CE), specific energy consumption (SEC) and deposit morphology and structure as the temperature, current density, pH and electrolyte composition were varied. Prior to conducting electrowinning tests, a conventional three-electrode cell was used to perform cyclic voltametric assessments of the electrodeposition reactions on the Ti electrode at room temperature. The indium electrowinning tests on Ti cathodes presented CE values higher than 90%, with low energy consumption at low current densities, showing a negligible influence of additive agents in the bath, different from results obtained with other cathodes in other works. Moreover, the increase of the current density beyond 75 A/m2 produced significant effects by etching the electrode surface with 1M HF. In particular, at the conclusion of this investigation, good results are obtained without additives, by etching the titanium cathode and operating at higher current density between 100 and 200 A/m2 at pH 2.3 and different temperatures (40 °C and 60 °C). Finally, indium deposits were analyzed by XRD and SEM in order to determine the influence of operative conditions on the structure and surface morphology. Full article
(This article belongs to the Special Issue Advances in Electronic and Photonic Materials)
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14 pages, 2848 KiB  
Article
Development of Fluorine Fixation Processes for the Horizontal Recycling of Lithium
by Kazuki Fujiwara, Kaisei Ito, Shunsuke Kuzuhara, Osamu Terakado, Natsuki Hosoya, Hideo Hayashi and Ryo Kasuya
Materials 2025, 18(9), 2050; https://doi.org/10.3390/ma18092050 - 30 Apr 2025
Viewed by 319
Abstract
In order to effectively recover Li from cathode active materials of lithium-ion batteries, model samples of LiCoO2 mixed with polyvinylidene fluoride (PVDF) were calcined at temperatures of 350–700 °C under an Ar or air atmosphere. Complete Li recovery was achieved by calcining [...] Read more.
In order to effectively recover Li from cathode active materials of lithium-ion batteries, model samples of LiCoO2 mixed with polyvinylidene fluoride (PVDF) were calcined at temperatures of 350–700 °C under an Ar or air atmosphere. Complete Li recovery was achieved by calcining the model sample at 400 °C under an Ar atmosphere, followed by water leaching. Additionally, to immobilize PVDF-derived F, an impurity in Li purification, we explored the use of calcium compounds (Ca(OH)2 and CaCO3) and a layered double hydroxide in both dry and wet processing methods. In the wet process, F was fixed by adding Ca(OH)2 to an aqueous LiF solution containing 1000 ppm of F. We confirmed that 98.6% of F was successfully removed from the solution after repeated fixation procedures. Furthermore, the unreacted Ca in the solution was separated and removed as CaCO3 by concentrating the solution. Full article
(This article belongs to the Special Issue Low Dimensional Materials for Batteries and Supercapacitors)
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13 pages, 4881 KiB  
Article
Electrochemiluminescence/Electrochemistry Dual-Mode Synchronous Sensing of Pb2+ Based on G4–hemin DNAzyme Complex During One-Step Scan
by Rukai Wei, Lei Shang, Wei Zhang, Xiaojian Li, Liping Jia, Rongna Ma and Huaisheng Wang
Molecules 2025, 30(9), 1951; https://doi.org/10.3390/molecules30091951 - 28 Apr 2025
Viewed by 440
Abstract
Electrochemiluminescence (ECL)/electrochemistry (EC) dual-mode sensors have garnered significant interest for their enhanced analytical reliability through the cross-verification of dual-signal outputs. However, conventional approaches necessitate two potential scans to acquire ECL and EC signals independently, resulting in temporal and environmental discrepancies between the two [...] Read more.
Electrochemiluminescence (ECL)/electrochemistry (EC) dual-mode sensors have garnered significant interest for their enhanced analytical reliability through the cross-verification of dual-signal outputs. However, conventional approaches necessitate two potential scans to acquire ECL and EC signals independently, resulting in temporal and environmental discrepancies between the two detection modes. In this paper, we present a novel synchronous ECL/EC dual-mode sensing platform for lead ion (Pb2+) detection via a one-step potential scan (0.2 to −0.4 V vs. Ag/AgCl) utilizing a G-quadruplex (G4)–hemin DNAzyme complex. This complex synergistically catalyzed the electrochemical reduction of dissolved oxygen, concurrently generating a distinct cathodic ECL emission from Ru(bpy)32+ and a synchronous reduction current peak at −0.25 V. Pb2+ quantification was achieved through its dose-dependent suppression of DNAzyme activity by destabilizing the G4–hemin interaction, thereby proportionally attenuating both ECL intensity and EC signal (reduction current). The integrated sensor demonstrated high sensitivity (detection limits of 1.51 nM for ECL detection and 2.03 nM for EC detection), robust anti-interference capability, and satisfactory reproducibility, with recoveries ranging from 95.5 to 103.1% in environmental water analysis. This work established a paradigm for one-step dual-mode sensor design, offering new prospects for environmental monitoring. Full article
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16 pages, 4986 KiB  
Article
Performance of 3D Network-Structured LiFePO4@Li3V2(PO4)3/Carbon Nanofibers via Coaxial Electrospinning as Self-Supporting Cathode for Lithium-Ion Batteries
by Ruixia Chu, Hongtao Zhang, Wanyou Huang, Fangyuan Qiu, Yan Wang, Zhenyu Li and Xiaoyue Jin
Materials 2025, 18(9), 1969; https://doi.org/10.3390/ma18091969 - 26 Apr 2025
Viewed by 606
Abstract
Lithium-ion batteries (LIBs) with high power, high capacity, and support for fast charging are increasingly favored by consumers. As a commercial electrode material for power batteries, LiFePO4 was limited from further wide application due to its low conductivity and lithium-ion diffusion rate. [...] Read more.
Lithium-ion batteries (LIBs) with high power, high capacity, and support for fast charging are increasingly favored by consumers. As a commercial electrode material for power batteries, LiFePO4 was limited from further wide application due to its low conductivity and lithium-ion diffusion rate. The development of advanced architectures integrating rational conductive networks with optimized ion transport pathways represents a critical frontier in optimizing the performance of cathode materials. In this paper, a novel self-supporting cathode material (designated as LFP@LVP-CES) was synthesized through an integrated coaxial electrospinning and controlled pyrolysis strategy. This methodology directly converts LiFePO4, Li3V2(PO4)3, and polyacrylonitrile (PAN)) into flexible, binder-free cathodes with a hierarchical structural organization. The 3D carbon nanofiber (CNF) matrix synergistically integrates LiFePO4 (Li/Fe/POx) and Li3V2(PO4)3 (Li/V/POx) nanoparticles, where CNFs act as a conductive scaffold to enhance electron transport, while the POx polyanionic frameworks stabilize Li+ diffusion pathways. Morphological characterizations (SEM and TEM) revealed a 3D cross-connected carbon nanofiber matrix (diameter: 250 ± 50 nm) uniformly embedded with active material particles. Electrochemical evaluations demonstrated that the LFP@LVP-CES cathode delivers an initial specific capacity of 165 mAh·g−1 at 0.1 C, maintaining 80 mAh·g−1 at 5 C. Notably, the material exhibited exceptional rate capability and cycling stability, demonstrating a 96% capacity recovery after high-rate cycling upon returning to 0.1 C, along with 97% capacity retention over 200 cycles at 1 C. Detailed kinetic analysis through EIS revealed significantly reduced Rct and increased Li+ diffusion. This superior electrochemical performance can be attributed to the synergistic effects between the 3D conductive network architecture and dual active materials. Compared with traditional coating processes and high-temperature calcination, the preparation of controllable electrospinning and low-temperature pyrolysis to some extent avoid the introduction of harmful substances and reduce raw material consumption and carbon emissions. This original integration strategy establishes a paradigm for designing freestanding electrode architectures through 3D structural design combined with a bimodal active material, providing critical insights for next-generation energy storage systems. Full article
(This article belongs to the Section Advanced Nanomaterials and Nanotechnology)
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