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15 pages, 7305 KB  
Article
Electrochemical Anodization-Induced {001} Facet Exposure in A-TiO2 for Improved DSSC Efficiency
by Jolly Mathew, Shyju Thankaraj Salammal, Anandhi Sivaramalingam and Paulraj Manidurai
J. Compos. Sci. 2025, 9(9), 462; https://doi.org/10.3390/jcs9090462 (registering DOI) - 1 Sep 2025
Abstract
We developed dye-sensitized solar cells based on anatase–titanium dioxide (A-TiO2) nanotubes (TiNTs) and nanocubes (TiNcs) with {001} crystal facets generated using simple and facile electrochemical anodization. We also demonstrated a simple way of developing one-dimensional, two-dimensional, and three-dimensional self-assembled TiO2 [...] Read more.
We developed dye-sensitized solar cells based on anatase–titanium dioxide (A-TiO2) nanotubes (TiNTs) and nanocubes (TiNcs) with {001} crystal facets generated using simple and facile electrochemical anodization. We also demonstrated a simple way of developing one-dimensional, two-dimensional, and three-dimensional self-assembled TiO2 nanostructures via electrochemical anodization, using them as an electron-transporting layer in DSSCs. TiNTs maintain tubular arrays for a limited time before becoming nanocrystals with {001} facets. Using FESEM and TEM, we observed that the TiO2 nanobundles were transformed into nanocubes with {001} facets and lower fluorine concentrations. Optimizing the reaction approach resulted in better-ordered, crystalline anatase TiNTs/Ncs being formed on the Ti metal foil. The anatase phase of as-grown TiO2 was confirmed by XRD, with (101) being the predominant intensity and preferred orientation. The nanostructured TiO2 had lattice values of a = 3.77–3.82 and c = 9.42–9.58. The structure and morphology of these as-grown materials were studied to understand the growth process. The photoconversion efficiency and impedance spectra were explored to analyze the performance of the designed DSSCs, employing N719 dye as a sensitizer and the I/I3− redox pair as electrolytes, sandwiched with a Pt counter-electrode. As a result, we found that self-assembled TiNTs/Ncs presented a more effective photoanode in DSSCs than standard TiO2 (P25). TiNcs (0.5 and 0.25 NH4F) and P25 achieved the highest power conversion efficiencies of 3.47, 3.41, and 3.25%, respectively. TiNcs photoanodes have lower charge recombination capability and longer electron lifetimes, leading to higher voltage, photocurrent, and photovoltaic performance. These findings show that electrochemical anodization is an effective method for preparing TiNTs/Ncs and developing low-cost, highly efficient DSSCs by fine-tuning photoanode structures and components. Full article
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14 pages, 2652 KB  
Article
Tuning Solid-State Reaction Pathways Using Molecular Sulfur Precursors to Synthesize FeS Anodes of Li-Ion Batteries for Boosted Electrochemical Performance
by Xiaoyang Zhang, Mingxia Xu, Jialiang Tian, Shaorong Cao, Botao Cao, Yongmei Bai, Xiaojie Hu, Cunfeng Yang, Jiliang Zhang and Chuang Dong
Energies 2025, 18(17), 4623; https://doi.org/10.3390/en18174623 (registering DOI) - 30 Aug 2025
Abstract
The solid-state reactions between Fe2O3 and molecular sulfur sources could produce FeS nanoparticles efficiently, while the functions of these molecules have been ignored except for the role as sulfur sources. In this work, thioacetamide and thiourea were employed as sulfur [...] Read more.
The solid-state reactions between Fe2O3 and molecular sulfur sources could produce FeS nanoparticles efficiently, while the functions of these molecules have been ignored except for the role as sulfur sources. In this work, thioacetamide and thiourea were employed as sulfur sources for the solid-state reactions with Fe2O3 to explore their effects on the microstructure and electrochemical performance of the produced FeS. Despite the slight difference in one functional group for two molecules (−CH3 against −NH2), thiourea leads to a more complex reaction pathway with FeS2 as the intermediate phase, while no such an intermediate phase is observed in the reaction with thioacetamide. The former yields FeS of 2D nanoflakes as the final products, compared with the aggregated nanoparticles in reactions with thiourea. As a result, the nanoflakes exhibit a higher discharge capacity with enhanced stability (388.9 mAh∙g−1 vs. 374.7 mAh∙g−1 above 1 V). According to the reaction pathways, the formation of FeS nanoflakes and superior electrochemical performance were addressed, paving a route for the solid-state reactions with molecules to develop high-performance sulfide electrode materials. Full article
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18 pages, 1693 KB  
Article
Multiple Functions of Carbon Additives in NASICON-Type Electrodes for Stabilizing the Sodium Storage Performance
by Trajche Tushev, Sonya Harizanova, Maria Shipochka, Radostina Stoyanova and Violeta Koleva
Molecules 2025, 30(17), 3547; https://doi.org/10.3390/molecules30173547 - 29 Aug 2025
Viewed by 98
Abstract
Recently, there has been increased interest in NASICON-type electrodes for sodium-ion batteries due to their unique combination of intercalation properties, low cost, and safety. However, their commercialization is hindered by the low electrical conductivity. One strategy to overcome this issue is to integrate [...] Read more.
Recently, there has been increased interest in NASICON-type electrodes for sodium-ion batteries due to their unique combination of intercalation properties, low cost, and safety. However, their commercialization is hindered by the low electrical conductivity. One strategy to overcome this issue is to integrate NASICON materials with carbon additives. This study shows that carbon additives improve the sodium storage performance of a NASICON-type electrode in various ways, depending on the additives’ functional groups, texture, and conductivity properties. The proof-of-concept is based on a multi-electron phospho-sulphate electrode, NaFeVPO4(SO4)2 (NFVPS) mixed with carbon black (C) and reduced graphene oxide (rGO). Carbon-coated samples are obtained via a simple ball milling procedure followed by thermal treatment in an argon flow. Sodium storage in the composites occurs through capacitive and Faradaic reactions. The Faradaic reaction is facilitated at the carbon black composite, while the capacitive reaction dominates for the rGO composite. NFVPS operates through two-electron reactions at 20 °C, while the increased temperatures favor the three-electron reaction. The rGO composite outperforms the carbon black composite in terms of cycling stability and rate capability at 20 and 40 °C. The role of the rGO and carbon black in electrochemical performance is discussed based on the different reactivity of hydroxyl/epoxide and carbonyl functional groups with the electrolyte salt, NaPF6, and the solvent, polypropylene carbonate. Full article
(This article belongs to the Special Issue Carbon-Based Electrochemical Materials for Energy Storage)
21 pages, 2978 KB  
Article
Photopolymerization 3D-Printed Dual-Modal Flexible Sensor for Glucose and pH Monitoring
by Shao Lin, Yu Li, Zhenyao Yang, Qiuzheng Li, Bohua Pang, Yin Feng, Jianglin Fu, Guangmeng Ma and Yu Long
Sensors 2025, 25(17), 5358; https://doi.org/10.3390/s25175358 - 29 Aug 2025
Viewed by 152
Abstract
Currently, flexible sensors based on electrochemical principles are predominantly limited to single-parameter detection, making it challenging to meet the demand for synchronous monitoring of multiple analytes in complex physiological environments. This study presents a 3D-printed flexible sensor for synchronous glucose/pH detection. Glucose was [...] Read more.
Currently, flexible sensors based on electrochemical principles are predominantly limited to single-parameter detection, making it challenging to meet the demand for synchronous monitoring of multiple analytes in complex physiological environments. This study presents a 3D-printed flexible sensor for synchronous glucose/pH detection. Glucose was quantified via H2O2 oxidation current (GOD-catalyzed reaction), while pH was measured through polyaniline (PANI) resistance changes. The ionogel-based microneedle electrode ensures mechanical robustness. At 0.2 V, optimal signal decoupling was achieved: glucose oxidation current dominates, while PANI’s polarization effect is minimized. Neutral pH minimally affected glucose oxidase (GOD) activity, and low glucose concentrations induced negligible pH interference, ensuring orthogonality. In artificial interstitial fluid, the sensor showed glucose: linear response (0.5–2.5 g·L−1, 0.288 μA·mM−1·cm−2); pH: piecewise-linear sensitivity (0.155 Ω/pH·cm2 for pH > 7; 0.135 Ω/pH·cm2 for pH < 7). The design enables real-time multiparameter monitoring with high selectivity, addressing current limitations in flexible electrochemical sensors. Full article
(This article belongs to the Section Biosensors)
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14 pages, 2443 KB  
Article
Design of CoMoCe-Oxide Nanostructured Composites as Robust Bifunctional Electrocatalyst for Water Electrolysis Overall Efficiency
by Akbar I. Inamdar, Amol S. Salunke, Jyoti V. Patil, Sawanta S. Mali, Chang Kook Hong, Basit Ali, Supriya A. Patil, Nabeen K. Shrestha, Sejoon Lee and Sangeun Cho
Materials 2025, 18(17), 4052; https://doi.org/10.3390/ma18174052 - 29 Aug 2025
Viewed by 199
Abstract
The development of ternary metal oxide electrocatalysts with optimized electronic structures and surface morphologies has emerged as one of the effective strategies to improve the performance of electrochemical water splitting. In this work, ternary CoMoCe (CMC)-oxide electrocatalysts were successfully synthesized on nickel foam [...] Read more.
The development of ternary metal oxide electrocatalysts with optimized electronic structures and surface morphologies has emerged as one of the effective strategies to improve the performance of electrochemical water splitting. In this work, ternary CoMoCe (CMC)-oxide electrocatalysts were successfully synthesized on nickel foam substrates via a hydrothermal technique and employed for their catalytic activity in an alkaline electrolyte. For comparison, binary counterparts (CoMo, CoCe, and MoCe) were also fabricated under similar conditions. The synthesized catalysts’ electrodes exhibited diverse surface architectures, including microporous-flake hybrids, ultrathin flakes, nanoneedle-assembled microspheres, and randomly oriented hexagonal structures. Among them, the ternary CoMoCe-oxide electrode exhibited outstanding bifunctional electrocatalytic activity, delivering low overpotentials of 124 mV for the hydrogen evolution reaction (HER) at −10 mA cm−2, and 340 mV for the oxygen evolution reaction (OER) at 100 mA cm−2, along with excellent durability. Furthermore, in full water-splitting configuration, the CMC||CMC and RuO2||CMC electrolyzers required cell voltages of 1.69 V and 1.57 V, respectively, to reach a current density of 10 mA cm−2. Remarkably, the CMC-based electrolyzer reached an industrially relevant current density of 1000 mA cm−2 at a cell voltage of 2.18 V, maintaining excellent stability over 100 h of continuous operation. These findings underscore the impact of an optimized electronic structure and surface architecture on design strategies for high-performance ternary metal oxide electrocatalysts. Herein, a robust and straightforward approach is comprehensively presented for fabricating highly efficient ternary metal-oxide catalyst electrodes, offering significant potential for scalable water splitting. Full article
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11 pages, 3841 KB  
Article
Fluoride-Mediated Synthesis of Co(OH)F and Electronic Structure Optimization for Enhanced Water Oxidation Performance
by Qianqian Dong, Yuhao Li, Jihao Liu, Yaru Wen, Junjie Wang, Haining Mo, Qianqian Jin, Shaohui Zhang and Xiong He
Molecules 2025, 30(17), 3529; https://doi.org/10.3390/molecules30173529 - 29 Aug 2025
Viewed by 149
Abstract
This study deciphers the anionic modulation mechanism of halide ions (F/Cl) in cobalt-based hydroxides for oxygen evolution reaction (OER). Phase-pure Co(OH)2, Co(OH)F, and Co2(OH)3Cl were fabricated via substrate-independent hydrothermal synthesis to eliminate conductive [...] Read more.
This study deciphers the anionic modulation mechanism of halide ions (F/Cl) in cobalt-based hydroxides for oxygen evolution reaction (OER). Phase-pure Co(OH)2, Co(OH)F, and Co2(OH)3Cl were fabricated via substrate-independent hydrothermal synthesis to eliminate conductive support interference. Electrocatalytic evaluation on glassy carbon electrodes demonstrates fluoride’s superior regulatory capability over chloride. X-ray photoelectron spectroscopy (XPS) analyses revealed that F incorporation induces charge redistribution through Co → F electron transfer, optimizing the electronic configuration via ligand effects. F incorporation simultaneously guided the anisotropic growth of 1D nanorods and reduced surface energy, thereby enhancing the wettability of Co(OH)F. The engineered Co(OH)F catalyst delivers exceptional OER performance: 318 mV overpotential at 10 mA/cm2 in 1 M KOH with 94% current retention over 20 h operation. This study provides a synthetic strategy for preparing pure-phase Co(OH)F and compares halide ions’ effects on enhancing OER activity through electronic structure modulation and morphological control of basic cobalt salts. Full article
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16 pages, 2535 KB  
Article
Effect of the Microstructure of Carbon Supports on the Oxygen Reduction Properties of the Loaded Non-Noble Metal Catalysts
by Dan Ma, Yudong Zhang, Menghan Liang, Runyu Niu, Yao Ge, Yanan Zou and Xiaorui Dong
Nanomaterials 2025, 15(17), 1327; https://doi.org/10.3390/nano15171327 - 29 Aug 2025
Viewed by 217
Abstract
The development of efficient non-noble metal catalysts is critical for advancing sustainable fuel-cell technologies. This study investigates the effect of carbon support microstructure on the oxygen reduction reaction (ORR) performance of Fe-N-C catalysts. By precisely tuning the pyrolysis temperature of activated carbon (AC) [...] Read more.
The development of efficient non-noble metal catalysts is critical for advancing sustainable fuel-cell technologies. This study investigates the effect of carbon support microstructure on the oxygen reduction reaction (ORR) performance of Fe-N-C catalysts. By precisely tuning the pyrolysis temperature of activated carbon (AC) between 600 and 1000 °C, we elucidate the mechanistic influence of the physicochemical characteristics of the carbon support on the ORR activity of the supported catalyst. Increasing the pyrolysis temperature enhanced the electrical conductivity of the carbon support, thereby improving the ORR performance of the catalyst. However, while the defect density and specific surface area of the carbon support initially increased with increasing pyrolysis temperature, they declined when elevated temperatures were used (e.g., 1000 °C), leading to reduced ORR activity. The AC-900 support, pyrolyzed at 900 °C, exhibited an optimal balance of a high surface area, abundant defects, and superior conductivity. An Fe phthalocyanine/AC-900 catalyst synthesized using the AC-900 support exhibited excellent ORR activity (E1/2: 0.89 V and Eon: 0.95 V vs. reversible hydrogen electrode (RHE)) in 0.1 M KOH. This work highlights the pivotal role of carbon support microstructure in governing the ORR activity of the supported catalyst and provides a rational strategy for designing high-performance non-noble metal electrocatalysts. Full article
(This article belongs to the Section Energy and Catalysis)
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22 pages, 6310 KB  
Article
A Green Electroslag Technology for Cadmium Recovery from Spent Ni-Cd Batteries Under Protective Flux with Electromagnetic Stirring by Electrovortex Flows
by Ervīns Blumbergs, Michail Maiorov, Artur Bogachov, Ernests Platacis, Sergei Ivanov, Pavels Gavrilovs and Vladimir Pankratov
Metals 2025, 15(9), 959; https://doi.org/10.3390/met15090959 - 29 Aug 2025
Viewed by 207
Abstract
The recycling of nickel–cadmium batteries poses a significant environmental challenge due to cadmium’s high biotoxicity. This study proposes a green method for recovering cadmium from cadmium oxide (CdO) using carbon (coal) in the presence of a molten binary flux (KCl:NaCl = 0.507:0.493, melting [...] Read more.
The recycling of nickel–cadmium batteries poses a significant environmental challenge due to cadmium’s high biotoxicity. This study proposes a green method for recovering cadmium from cadmium oxide (CdO) using carbon (coal) in the presence of a molten binary flux (KCl:NaCl = 0.507:0.493, melting point 667 °C). The flux’s relatively low density and conductivity enable cadmium reduction beneath and through the flux layer. Brown coal (5–25 mm) served as the reductant. The reduction of cadmium from cadmium oxide with carbon (brown coal) took place in the temperature range from 667 °C to 700 °C. To enhance the process, electrovortex flows (EVF) were employed—generated by the interaction between non-uniform AC electric currents and their self-induced magnetic fields resembling conditions in a fluidised bed reactor. The graphite crucible acted as both one of the electrodes, with a graphite rod as the second electrode. As Cd and CdO are denser than both the flux and coal, the reduction proceeded below the flux layer. The flux facilitated CdO transport to the reductant, speeding up the reaction. X-ray diffraction (XRD) and scanning electron microscopy (SEM) confirmed the formation of metallic cadmium beneath and within the flux layer. This method demonstrates the feasibility of flux-assisted cadmium recovery without prior mixing and offers a foundation for further optimisation of sustainable battery recycling. Full article
(This article belongs to the Special Issue Green Technologies in Metal Recovery)
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13 pages, 1876 KB  
Article
Fe Species Intercalation Confined by the Interlayer Environment of V2CTx MXene for Lithium-Ion Storage
by Jiaxin Li, Miao Liu, Jiaming Li, Wenjuan Han, Shichong Xu, Haibo Li and Ming Lu
Inorganics 2025, 13(9), 290; https://doi.org/10.3390/inorganics13090290 - 28 Aug 2025
Viewed by 224
Abstract
This work successfully achieved pre-intercalation of Fe species in V2CTx MXene through an annealing method. The crystallographic structure, microscopic morphology, and functional groups of the samples before and after pre-intercalation were analyzed by XRD, SEM, and FTIR, and the electrochemical performance of MXene [...] Read more.
This work successfully achieved pre-intercalation of Fe species in V2CTx MXene through an annealing method. The crystallographic structure, microscopic morphology, and functional groups of the samples before and after pre-intercalation were analyzed by XRD, SEM, and FTIR, and the electrochemical performance of MXene electrodes was studied. Research has shown that the interlayer spacing of pre-intercalated MXene increases with an increase in annealing temperature. The interlayer spacing of MXene annealed at 800 °C is 13.1% higher than that of the original MXene. However, the morphology of the samples was damaged by excessively high annealing temperatures, which also weakened the lithium-ion storage performance. In contrast, the cycling performance of MXene electrodes annealed at 400 °C showed the greatest improvement, reaching 71.65%. This is because iron species, acting as a pillar support structure, expand the interlayer spacing and broaden the transport channels for lithium ions. Meanwhile, high-temperature annealing generates more oxygen-containing functional groups, which provide additional active sites for lithium-ion transport, promote the kinetics of electrode reactions, and thus enhance its lithium-ion storage performance. Full article
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20 pages, 3429 KB  
Article
Insights into the Electrocatalytic Activity of Mixed-Valence Mn3+/Mn4+ and Fe2+/Fe3+ Transition Metal Oxide Materials
by Bogdan-Ovidiu Taranu, Paula Svera, Gabriel Buse and Maria Poienar
Solids 2025, 6(3), 48; https://doi.org/10.3390/solids6030048 - 26 Aug 2025
Viewed by 401
Abstract
Hydrogen generation has become a popular research subject in light of currently pressing issues, such as the rapidly increasing environmental pollution, the depleting fossil fuel reserves, and the looming energy crisis. Sustainable electrochemical water splitting is regarded as one of the most desirable [...] Read more.
Hydrogen generation has become a popular research subject in light of currently pressing issues, such as the rapidly increasing environmental pollution, the depleting fossil fuel reserves, and the looming energy crisis. Sustainable electrochemical water splitting is regarded as one of the most desirable methods for obtaining green hydrogen. Considering this state of affairs, the water splitting electrocatalytic activity of glassy carbon electrodes modified with birnessite-type K2Mn4O8 and mixed-valence iron phosphate Fe3(PO3OH)4(H2O)4 materials were evaluated in electrolyte solutions having different pH values. Both compounds were characterized by X-ray diffraction and FT-IR spectroscopy in order to analyze their phase purity and their structural features. The most catalytically active birnessite-type K2Mn4O8-based electrode was manufactured using a catalyst ink containing only the electrocatalyst dispersed in ethanol and Nafion solution. In 0.1 M H2SO4, it exhibited an oxygen evolution reaction (OER) overpotential of 1.07 V and a hydrogen evolution reaction (HER) overpotential of 0.957 V. The Tafel slopes obtained in the OER and HER experiments were 0.180 and 0.142 V/dec, respectively. The most catalytically active mixed-valence iron phosphate Fe3(PO3OH)4(H2O)4-based electrode was obtained with a catalyst ink containing the specified material mixed with carbon black and dispersed in ethanol and Nafion solution. In a strongly alkaline medium, it displayed a HER overpotential of 0.515 V and a Tafel slope value of 0.122 V/dec. The two electrocatalysts have not been previously investigated in this way, and the acquired data provide insights into their electrocatalytic activity and improve the scientific understanding of their properties and applicative potential. Full article
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10 pages, 1211 KB  
Communication
Enhanced Rate Capability in B-Site High-Entropy Perovskite Oxide Ceramics: The Case of La(Co0.2Cr0.2Ni0.2Ga0.2Ge0.2)O3
by Boon-How Mok, Tengfa Yao, Longchao Fu, Cheng-Tsung Lu, Haoxian Ouyang, Zongying Pan and Changan Tian
Materials 2025, 18(17), 3966; https://doi.org/10.3390/ma18173966 - 25 Aug 2025
Viewed by 368
Abstract
This study employed the solid-state method to prepare perovskite-type high-entropy oxide materials La(Co0.2Cr0.2Fe0.2Mn0.2Ni0.2)O3 and La(Co0.2Cr0.2Ni0.2Ga0.2Ge0.2)O3 with equimolar ratios at the B-site [...] Read more.
This study employed the solid-state method to prepare perovskite-type high-entropy oxide materials La(Co0.2Cr0.2Fe0.2Mn0.2Ni0.2)O3 and La(Co0.2Cr0.2Ni0.2Ga0.2Ge0.2)O3 with equimolar ratios at the B-site and explored the effects of sintering temperature on the phase structure and electrochemical properties of high-entropy oxide ceramics. The results show that after sintering at 1300°C, both samples exhibit orthorhombic perovskite structures. Both have a relative density of >97%, while La(Co0.2Cr0.2Ni0.2Ga0.2Ge0.2)O3 has a significantly larger grain size. Using these materials as electrodes, the cyclic voltammetry (CV) and galvanostatic charge–discharge (GCD) results indicate that the working electrode made of La(Co0.2Cr0.2Ni0.2Ga0.2Ge0.2)O3 shows higher oxidation reaction activity in CV measurements and achieved a specific capacitance of 74.3 F/g at a current density of 1 A/g in GCD measurements, which still maintained 73% of its initial specific capacitance (54.3 F/g) when the current density was increased to 10 A/g. Its capacitance retention rate is 10 percentage points higher than that of La(Co0.2Cr0.2Fe0.2Mn0.2Ni0.2)O3 at high current densities, demonstrating superior rate performance. Full article
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26 pages, 5061 KB  
Article
Mechanism and Kinetic Parameters of Functionalized Composite Carbon-Based Electrocatalyst During Oxidation of Glycerol Using Dynamic Electrochemical Impedance Spectroscopy
by Faisal Abnisa, Pater Adeniyi Alaba and Ramesh Kanthasamy
Catalysts 2025, 15(9), 805; https://doi.org/10.3390/catal15090805 - 25 Aug 2025
Viewed by 373
Abstract
This research investigates the glycerol oxidation reaction on carbon-functionalized composites using Tafel behavior, exchange current density (ECD), rate constant, and dynamic electrochemical impedance spectroscopy (DEIS) data fitting. The aim is to gather essential data for fabricating glycerol electrooxidation electrodes in an alkaline medium. [...] Read more.
This research investigates the glycerol oxidation reaction on carbon-functionalized composites using Tafel behavior, exchange current density (ECD), rate constant, and dynamic electrochemical impedance spectroscopy (DEIS) data fitting. The aim is to gather essential data for fabricating glycerol electrooxidation electrodes in an alkaline medium. Corrected net current analysis reveals that the nitrogen-doped activated carbon black composite electrode (ACB-N2) exhibits the highest instantaneous catalytic activity, with a net current density of 1.3 mA cm−2 at 1.0 V vs. SCE. However, the dual-doped nitrogen and fluorine composite (ACB-N2F2) demonstrates the lowest Tafel slope (177.97 mV dec−1), indicating faster kinetics, and it maintains superior electrochemical stability during chronoamperometric testing. ACB-N2F2 exhibits the highest ECD (1.0129 mA cm−2) and the lowest Ts and rate constant (2.62 × 109 cm s−1), indicating the fastest electron transfer. These findings suggest that while ACB-N2 offers the highest net GOR activity, ACB-N2F2 combines kinetic efficiency and long-term durability, making it a promising candidate for practical GOR applications. The rate-determining step is water adsorption at low overpotentials (0.55 V, 0.5 V, and 0.4 V vs. SCE for ACB-F2, ACB-N2, and ACB-N2F2, respectively). Full article
(This article belongs to the Section Electrocatalysis)
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26 pages, 1505 KB  
Review
Application of Electrochemical Oxidation for Urea Removal: A Review
by Juwon Lee, Jeongbeen Park, Intae Shim, Jae-Wuk Koo, Sook-Hyun Nam, Eunju Kim, Seung-Min Park and Tae-Mun Hwang
Processes 2025, 13(8), 2660; https://doi.org/10.3390/pr13082660 - 21 Aug 2025
Viewed by 508
Abstract
The consistent quality control of ultrapure water (UPW) in semiconductor manufacturing depends on removing trace organonitrogen compounds such as urea. Due to its high solubility, chemical stability, and neutral polarity, urea is inadequately removed by conventional processes. Even at low concentrations, it elevates [...] Read more.
The consistent quality control of ultrapure water (UPW) in semiconductor manufacturing depends on removing trace organonitrogen compounds such as urea. Due to its high solubility, chemical stability, and neutral polarity, urea is inadequately removed by conventional processes. Even at low concentrations, it elevates total organic carbon (TOC) and reduces electrical resistivity. The use of reclaimed water as a sustainable feed stream amplifies this challenge because its nitrogen content is variable and persistent. Conventional methods such as reverse osmosis, ultraviolet oxidation, and ion exchange remain limited in treating urea due to its uncharged, low-molecular-weight nature. This review examines the performance and limitations of these processes and explores electrochemical oxidation (EO) as an alternative. Advances in EO are analyzed with attention to degradation pathways, electrode design, reaction selectivity, and operational parameters. Integrated systems combining EO with membrane filtration, adsorption, or chemical oxidation are also reviewed. Although EO shows promise for selectively degrading urea, its application in UPW production is still in its early stages. Challenges such as low conductivity, byproduct formation, and energy efficiency must be addressed. The paper first discusses urea in reclaimed water and associated removal challenges, then examines both conventional and emerging treatment technologies. Subsequent sections delve into the mechanisms and optimization of EO, including electrode materials and operational parameters. The review concludes with a summary of main findings and a discussion of future research directions, aiming to provide a comprehensive foundation for validating EO as a viable technology for producing UPW from reclaimed water. Full article
(This article belongs to the Special Issue Addressing Environmental Issues with Advanced Oxidation Technologies)
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18 pages, 1808 KB  
Article
Holmium Metal Nanoparticle PbO2 Anode Formed by Electrodeposition for Efficient Removal of Insecticide Acetamiprid and Improved Oxygen Evolution Reaction
by Milica Kaludjerović, Sladjana Savić, Danica Bajuk-Bogdanović, Aleksandar Jovanović, Lazar Rakočević, Goran Roglić, Jadranka Milikić and Dalibor Stanković
Micromachines 2025, 16(8), 960; https://doi.org/10.3390/mi16080960 - 20 Aug 2025
Viewed by 413
Abstract
This work examines the possibility of using a PbO2-based electrode doped with the rare-earth metal holmium in the field of oxygen evolution and the development of an efficient method for the degradation of acetamiprid. Acetamiprid is a widely used insecticide and, [...] Read more.
This work examines the possibility of using a PbO2-based electrode doped with the rare-earth metal holmium in the field of oxygen evolution and the development of an efficient method for the degradation of acetamiprid. Acetamiprid is a widely used insecticide and, as such, it very often reaches waterways, where it can cause many problems for wildlife and the environment. X-ray powder diffraction analysis, Raman spectroscopy, and energy-dispersive X-ray spectroscopy results confirmed the structure of Ti/SnO2-Sb2O3/Ho-PbO2, while the morphology of its surface was investigated by scanning electron microscopy with energy-dispersive X-ray spectroscopy. Ti/SnO2-Sb2O3/Ho-PbO2 showed good OER activity in alkaline media with a Tafel slope of 138 mV dec−1. The Ti/SnO2-Sb2O3/Ho-PbO2 electrode shows very good efficiency in removing acetamiprid. By optimizing the degradation procedure, the following operating conditions were obtained: a current density of 20 mA cm−2, a pH value of the supporting electrolyte (sodium sulfate) of 2, and a concentration of the supporting electrolyte of 0.035 M. After optimization, the maximum efficiency of removing acetamiprid (10 mg L−1, 4.5 × 10−5 mol) from water was achieved, 96.8%, after only 90 min of treatment, which represents an efficiency of 1.125 mol cm−2 of the electrode. Additionally, it was shown that the degradation efficiency is strictly related to the concentration of the treated substance. Full article
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18 pages, 1918 KB  
Article
Sustainable Degradation of Acetaminophen by a Solar-Powered Electro-Fenton Process: A Green and Energy-Efficient Approach
by Sonia Herrera-Chávez, Silvia Gutierrez, Miguel A. Sandoval, Enric Brillas, Martin Pacheco-Álvarez and Juan M. Peralta-Hernández
Processes 2025, 13(8), 2633; https://doi.org/10.3390/pr13082633 - 20 Aug 2025
Viewed by 619
Abstract
The presence of acetaminophen (ACTP) in aquatic environments has become a significant concern due to its environmental persistence and the potential formation of toxic transformation products. This study systematically compares the performance of three electrochemical advanced oxidation processes (EAOPs), electro-oxidation (EO), electro-Fenton (EF), [...] Read more.
The presence of acetaminophen (ACTP) in aquatic environments has become a significant concern due to its environmental persistence and the potential formation of toxic transformation products. This study systematically compares the performance of three electrochemical advanced oxidation processes (EAOPs), electro-oxidation (EO), electro-Fenton (EF), and solar photo-electro-Fenton (SPEF), for the degradation and mineralization of ACTP in aqueous media using boron-doped diamond (BDD) electrodes. Reactions were conducted under varying operational parameters, including current densities (15–60 mA cm−2), initial ACTP concentrations (10–30 mg L−1), and Fe2+ dosages. In the SPEF system, natural sunlight was utilized as the source of UV-A irradiation (30–35 W m−2). Among the evaluated processes, SPEF exhibited the highest degradation efficiency, achieving up to 97% ACTP removal and 78% chemical oxygen demand (COD) reduction within 90 min. High-performance liquid chromatography (HPLC) analysis identified phenol and catechol as major intermediates, suggesting a degradation pathway involving hydroxylation, aromatic ring cleavage, and subsequent oxidation into low-molecular-weight carboxylic acids. Kinetic modeling revealed pseudo-first-order behavior, with a maximum rate constant of 0.0865 min−1 under optimized conditions determined via Box–Behnken experimental design. Additionally, SPEF demonstrated enhanced energy efficiency (~0.052 kWh gCOD−1) and improved oxidant regeneration under solar radiation, highlighting its potential as an environmentally friendly and cost-effective alternative for pharmaceutical wastewater treatment. These results support the implementation of SPEF as a sustainable strategy for mitigating the environmental impact of emerging contaminants, especially in regions with high solar availability and limited technological resources. Full article
(This article belongs to the Special Issue Modeling and Optimization for Multi-scale Integration)
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