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Keywords = hydrothermal reactions

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15 pages, 4751 KiB  
Article
Electrocatalytic Oxidation for Efficient Toluene Removal with a Catalytic Cu-MnOx/GF Electrode in a Solid-State Electrocatalytic Device
by Haozhen Liu, Mingxin Liu, Xiqiang Zhao, Ping Zhou, Zhanlong Song, Wenlong Wang, Jing Sun and Yanpeng Mao
Catalysts 2025, 15(8), 749; https://doi.org/10.3390/catal15080749 - 5 Aug 2025
Abstract
A series of Cu-MnOx/GF catalytic electrodes, with graphite felt (GF) pretreated via microwave modification as the catalyst carrier, were prepared under various hydrothermal conditions and characterized using X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), X-ray photoelectron spectroscopy (XPS), N2 adsorption–desorption, [...] Read more.
A series of Cu-MnOx/GF catalytic electrodes, with graphite felt (GF) pretreated via microwave modification as the catalyst carrier, were prepared under various hydrothermal conditions and characterized using X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), X-ray photoelectron spectroscopy (XPS), N2 adsorption–desorption, and Raman spectroscopy. The catalytic oxidation activity of catalytic Cu-MnOx/GF electrodes toward toluene was evaluated in an all-solid-state electrocatalytic device under mild operating conditions. The evaluation results demonstrated that the microwave-modified catalytic electrode exhibited high electrocatalytic activity toward toluene oxidation, with Cu-MnOx/700W-GF exhibiting significantly higher catalytic activity, indicating that an increase in catalyst loading capacity can promote the removal of toluene. Only CO2 and CO were detected, with no other intermediates observed in the reaction process. Moreover, the catalytic effect was significantly affected by the relative humidity. The catalytic oxidation of toluene can be fully realized under a certain humidity, indicating that the conversion of H2O to strongly oxidizing ·OH on the catalytic electrode is a key step in this reaction. Full article
(This article belongs to the Special Issue Catalytic Removal of Volatile Organic Compounds (VOCs))
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13 pages, 2303 KiB  
Article
A Stable Metal Chalcogenide Cluster-Based Framework Decorated with Transition Metal Complexes for an Efficient Electrocatalytic O2 Reduction Reaction
by Xiang Wang, Juan Li and Tao Wu
Nanomaterials 2025, 15(15), 1186; https://doi.org/10.3390/nano15151186 - 1 Aug 2025
Viewed by 129
Abstract
Highly efficient and stable non-Pt-based electrocatalysts for oxygen reduction reactions (ORRs) are highly desirable in energy conversion and storage systems. Herein, we report a hydrothermally synthesized metal chalcogenide cluster-based framework (NCF-3-Mn), which is decorated with transition metal complexes ([Mn(TEPA)]2+, TEPA = [...] Read more.
Highly efficient and stable non-Pt-based electrocatalysts for oxygen reduction reactions (ORRs) are highly desirable in energy conversion and storage systems. Herein, we report a hydrothermally synthesized metal chalcogenide cluster-based framework (NCF-3-Mn), which is decorated with transition metal complexes ([Mn(TEPA)]2+, TEPA = tetraethylenepentamine), for an electrocatalytic O2 reduction reaction (ORR). Benefitting from the abundant Mn-S bonds and Mn-N-C structures in NCF-3-Mn, it was found that NCF-3-Mn displayed a high onset potential (0.90 V) and an efficient four-electron transfer reaction pathway, which are much better than those of its analogue framework (T2-GaSbS). Moreover, NCF-3-Mn also exhibited a considerable long-term stability and methanol resistance toward ORRs. This work will present new opportunities for exploring the utilization of chalcogenide frameworks as novel non-Pt electrocatalysts for ORRs. Full article
(This article belongs to the Collection Micro/Nanoscale Open Framework Materials (OFMs))
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17 pages, 2736 KiB  
Article
Controlled Formation of α- and β-Bi2O3 with Tunable Morphologies for Visible-Light-Driven Photocatalysis
by Thomas Cadenbach, María Isabel Loyola-Plúa, Freddy Quijano Carrasco, Maria J. Benitez, Alexis Debut and Karla Vizuete
Molecules 2025, 30(15), 3190; https://doi.org/10.3390/molecules30153190 - 30 Jul 2025
Viewed by 222
Abstract
Water pollution caused by increasing industrial and human activity remains a serious environmental challenge, especially due to the persistence of organic contaminants in aquatic systems. Photocatalysis offers a promising and eco-friendly solution, but in the case of bismuth oxide (Bi2O3 [...] Read more.
Water pollution caused by increasing industrial and human activity remains a serious environmental challenge, especially due to the persistence of organic contaminants in aquatic systems. Photocatalysis offers a promising and eco-friendly solution, but in the case of bismuth oxide (Bi2O3) there is still a limited understanding of how structural and morphological features influence photocatalytic performance. In this work, a straightforward hydrothermal synthesis method followed by controlled calcination was developed to produce phase-pure α- and β-Bi2O3 with tunable morphologies. By varying the hydrothermal temperature and reaction time, distinct structures were successfully obtained, including flower-like, broccoli-like, and fused morphologies. XRD analyses showed that the final crystal phase depends solely on the calcination temperature, with β-Bi2O3 forming at 350 °C and α-Bi2O3 at 500 °C. SEM and BET analyses confirmed that morphology and surface area are strongly influenced by the hydrothermal conditions, with the flower-like β-Bi2O3 exhibiting the highest surface area. UV–Vis spectroscopy revealed that β-Bi2O3 also has a lower bandgap than its α counterpart, making it more responsive to visible light. Photocatalytic tests using Rhodamine B showed that the flower-like β-Bi2O3 achieved the highest degradation efficiency (81% in 4 h). Kinetic analysis followed pseudo-first-order behavior, and radical scavenging experiments identified hydroxyl radicals, superoxide radicals, and holes as key active species. The catalyst also demonstrated excellent stability and reusability. Additionally, Methyl Orange (MO), a more stable and persistent azo dye, was selected as a second model pollutant. The flower-like β-Bi2O3 catalyst achieved 73% degradation of MO at pH = 7 and complete removal under acidic conditions (pH = 2) in less than 3 h. These findings underscore the importance of both phase and morphology in designing high-performance Bi2O3 photocatalysts for environmental remediation. Full article
(This article belongs to the Special Issue Green Catalysis Technology for Sustainable Energy Conversion)
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28 pages, 14491 KiB  
Article
Catalytically Active Oxidized PtOx Species on SnO2 Supports Synthesized via Anion Exchange Reaction for 4-Nitrophenol Reduction
by Izabela Ðurasović, Robert Peter, Goran Dražić, Fabio Faraguna, Rafael Anelić, Marijan Marciuš, Tanja Jurkin, Vlasta Mohaček Grošev, Maria Gracheva, Zoltán Klencsár, Mile Ivanda, Goran Štefanić and Marijan Gotić
Nanomaterials 2025, 15(15), 1159; https://doi.org/10.3390/nano15151159 - 28 Jul 2025
Viewed by 313
Abstract
An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO2 supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO2 supports, namely SnA (synthesized almost at room [...] Read more.
An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO2 supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO2 supports, namely SnA (synthesized almost at room temperature), SnB (hydrothermally treated at 180 °C), and SnC (annealed at 600 °C), are systematically investigated, all loaded with 1 mol% Pt from H2PtCl6 under identical mild conditions. The chloride ions from the SnCl4 precursors were efficiently removed via a strong-base anion exchange reaction, resulting in highly dispersed, crystalline ~5 nm cassiterite SnO2 particles. All Pt/SnO2 composites displayed mesoporous structures with type IVa isotherms and H2-type hysteresis, with SP1a (Pt on SnA) exhibiting the largest surface area (122.6 m2/g) and the smallest pores (~3.5 nm). STEM-HAADF imaging revealed well-dispersed PtOx domains (~0.85 nm), while XPS confirmed the dominant Pt4+ and Pt2+ species, with ~25% Pt0 likely resulting from photoreduction and/or interactions with Sn–OH surface groups. Raman spectroscopy revealed three new bands (260–360 cm−1) that were clearly visible in the sample with 10 mol% Pt and were due to the vibrational modes of the PtOx species and Pt-Cl bonds introduced due the addition and hydrolysis of H2PtCl6 precursor. TGA/DSC analysis revealed the highest mass loss for SP1a (~7.3%), confirming the strong hydration of the PtOx domains. Despite the predominance of oxidized PtOx species, SP1a exhibited the highest catalytic activity (kapp = 1.27 × 10−2 s−1) and retained 84.5% activity for the reduction of 4-NP to 4-AP after 10 cycles. This chloride-free low-temperature synthesis route offers a promising and generalizable strategy for the preparation of noble metal-based nanocatalysts on oxide supports with high catalytic activity and reusability. Full article
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20 pages, 10028 KiB  
Article
The Fabrication of Cu2O-u/g-C3N4 Heterojunction and Its Application in CO2 Photoreduction
by Jiawei Lu, Yupeng Zhang, Fengxu Xiao, Zhikai Liu, Youran Li, Guiyang Shi and Hao Zhang
Catalysts 2025, 15(8), 715; https://doi.org/10.3390/catal15080715 - 27 Jul 2025
Viewed by 436
Abstract
Over efficient photocatalysts, CO2 photoreduction typically converts CO2 into low-carbon chemicals, which serve as raw materials for downstream synthesis processes. Here, an efficient composite photocatalyst heterojunction (Cu2O-u/g-C3N4) has been fabricated to reduce CO2. [...] Read more.
Over efficient photocatalysts, CO2 photoreduction typically converts CO2 into low-carbon chemicals, which serve as raw materials for downstream synthesis processes. Here, an efficient composite photocatalyst heterojunction (Cu2O-u/g-C3N4) has been fabricated to reduce CO2. Graphitic carbon nitride (g-C3N4) was synthesized via thermal polymerization of urea at 550 °C, while pre-dispersed Cu2O derived from urea pyrolysis (Cu2O-u) was prepared by thermal reduction of urea and CuCl2·2H2O at 180 °C. The heterojunction Cu2O-u/g-C3N4 was subsequently constructed through hydrothermal treatment at 180 °C. This heterojunction exhibited a bandgap of 2.10 eV, with dual optical absorption edges at 485 nm and above 800 nm, enabling efficient harvesting of solar light. Under 175 W mercury lamp irradiation, the heterojunction catalyzed liquid-phase CO2 photoreduction to formic acid, acetic acid, and methanol. Its formic acid production activity surpassed that of pristine g-C3N4 by 3.14-fold and TiO2 by 8.72-fold. Reaction media, hole scavengers, and reaction duration modulated product selectivity. In acetonitrile/isopropanol systems, formic acid and acetic acid production reached 579.4 and 582.8 μmol·h−1·gcat−1. Conversely, in water/triethanolamine systems, methanol production reached 3061.6 μmol·h−1·gcat−1, with 94.79% of the initial conversion retained after three cycles. Finally, this work ends with the conclusions of the CO2 photocatalytic reduction to formic acid, acetic acid, and methanol, and recommends prospects for future research. Full article
(This article belongs to the Section Photocatalysis)
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9 pages, 861 KiB  
Communication
Hydrothermal Carbonization of Pruned Persimmon Tree Branches: Optimization of Process Conditions for Enhanced Energy Recovery
by Hirotaka Maeda and Yuta Ueda
Materials 2025, 18(15), 3425; https://doi.org/10.3390/ma18153425 - 22 Jul 2025
Viewed by 170
Abstract
Pruned branches from persimmon trees are a largely untapped agricultural waste resource. This study explores the conversion of these branches into an enhanced fuel source through hydrothermal carbonization. The branches were subjected to hydrothermal treatment under various conditions to identify the optimal parameters. [...] Read more.
Pruned branches from persimmon trees are a largely untapped agricultural waste resource. This study explores the conversion of these branches into an enhanced fuel source through hydrothermal carbonization. The branches were subjected to hydrothermal treatment under various conditions to identify the optimal parameters. Higher temperatures and longer treatment durations increased the carbon content to 69.2% and reduced the oxygen content to 20.4%. A Van Krevelen diagram showed that dehydration was the primary reaction, with decarboxylation occurring at 250 °C. The energy value increased from 18.2 MJ/kg for raw branches to 28.5 MJ/kg under the optimal conditions, indicating a 57% improvement. These findings demonstrate that hydrothermal carbonization effectively utilizes persimmon pruning waste, offering a sustainable method for converting biomass into energy and aiding agricultural waste management. Full article
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11 pages, 2972 KiB  
Article
ZnCu Metal–Organic Framework Electrocatalysts for Efficient Ammonia Decomposition to Hydrogen
by Mingguang Ouyang, Geng Chen, Weitao Ning, Xiaoyang Wang, Xiaojiang Mu and Lei Miao
Energies 2025, 18(14), 3871; https://doi.org/10.3390/en18143871 - 21 Jul 2025
Viewed by 332
Abstract
The electrocatalytic decomposition of ammonia represents a promising route for sustainable hydrogen production, yet current systems rely heavily on noble metal catalysts with prohibitive costs and limited durability. A critical challenge lies in developing non-noble electrocatalysts that simultaneously achieve high active site exposure, [...] Read more.
The electrocatalytic decomposition of ammonia represents a promising route for sustainable hydrogen production, yet current systems rely heavily on noble metal catalysts with prohibitive costs and limited durability. A critical challenge lies in developing non-noble electrocatalysts that simultaneously achieve high active site exposure, optimized electronic configurations, and robust structural stability. Addressing these requirements, this study strategically engineered Cu-doped ZIF-8 architectures via in situ growth on nickel foam (NF) substrates through a facile room-temperature hydrothermal synthesis approach. Systematic optimization of the Cu/Zn molar ratio revealed that Cu0.7Zn0.3-ZIF/NF achieved optimal performance, exhibiting a distinctive nanoflower-like architecture that substantially increased accessible active sites. The hybrid catalyst demonstrated superior electrocatalytic performance with a current density of 124 mA cm−2 at 1.6 V vs. RHE and a notably low Tafel slope of 30.94 mV dec−1, outperforming both Zn-ZIF/NF (39.45 mV dec−1) and Cu-ZIF/NF (31.39 mV dec−1). Combined XPS and EDS analyses unveiled a synergistic electronic structure modulation between Zn and Cu, which facilitated charge transfer and enhanced catalytic efficiency. A gas chromatography product analysis identified H2 and N2 as the primary gaseous products, confirming the predominant occurrence of the ammonia oxidation reaction (AOR). This study not only presents a noble metal-free electrocatalyst with exceptional efficiency and durability for ammonia decomposition but also demonstrates the significant potential of MOF-derived materials in sustainable hydrogen production technologies. Full article
(This article belongs to the Special Issue Advanced Energy Conversion Technologies Based on Energy Physics)
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11 pages, 1808 KiB  
Article
CdZnS Nanowire Decorated with Graphene for Efficient Photocatalytic Hydrogen Evolution
by Zemeng Wang, Yunsheng Shen, Qingsheng Liu, Tao Deng, Kangqiang Lu and Zhaoguo Hong
Molecules 2025, 30(14), 3042; https://doi.org/10.3390/molecules30143042 - 20 Jul 2025
Viewed by 285
Abstract
Harnessing abundant and renewable solar energy for photocatalytic hydrogen production is a highly promising approach to sustainable energy generation. To realize the practical implementation of such systems, the development of photocatalysts that simultaneously exhibit high activity, cost-effectiveness, and long-term stability is critically important. [...] Read more.
Harnessing abundant and renewable solar energy for photocatalytic hydrogen production is a highly promising approach to sustainable energy generation. To realize the practical implementation of such systems, the development of photocatalysts that simultaneously exhibit high activity, cost-effectiveness, and long-term stability is critically important. In this study, a Cd0.8Zn0.2S nanowire photocatalytic system decorated with graphene (GR) was prepared by a simple hydrothermal method. The introduction of graphene increased the reaction active area of Cd0.8Zn0.2S, promoted the separation of photogenerated charge carriers in the semiconductor, and improved the photocatalytic performance of the Cd0.8Zn0.2S semiconductor. The results showed that Cd0.8Zn0.2S loaded with 5% graphene exhibited the best photocatalytic activity, with a hydrogen production rate of 1063.4 µmol·g−1·h−1. Characterization data revealed that the graphene cocatalyst significantly enhances electron transfer kinetics in Cd0.8Zn0.2S, thereby improving the separation efficiency of photogenerated charge carriers. This study demonstrates a rational strategy for designing high-performance, low-cost composite photocatalysts using earth-abundant cocatalysts, advancing sustainable hydrogen production. Full article
(This article belongs to the Section Photochemistry)
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5 pages, 665 KiB  
Proceeding Paper
Opportunities of Coupling Hydrothermal Liquefaction with Wet Oxidation: Significance of Appropriate Thermodynamic Model Selection in Process Modeling
by Arif Hussain, Bertram Thoning Hvass Søgaard and Konstantinos Anastasakis
Proceedings 2025, 121(1), 7; https://doi.org/10.3390/proceedings2025121007 - 17 Jul 2025
Viewed by 183
Abstract
This study examines the significance of thermodynamic model selection to improve predictions when modeling a wet oxidation (WO) process. WO is a promising technology for treating the highly concentrated process water stream from hydrothermal liquefaction (HTL) while generating heat, due to the exothermic [...] Read more.
This study examines the significance of thermodynamic model selection to improve predictions when modeling a wet oxidation (WO) process. WO is a promising technology for treating the highly concentrated process water stream from hydrothermal liquefaction (HTL) while generating heat, due to the exothermic oxidation reactions, leading to a potential integrated HTL-WO autothermal process. However, the harsh process conditions employed fail to describe oxygen solubility accurately, leading to major deviations in predicted COD reduction, heat generation, vapor fraction, and final design. To accurately capture oxygen solubility at elevated temperatures and pressures, experimental oxygen solubility data were regressed using activity coefficient models. This yielded improved oxygen solubility predictions at 280–350 °C, more realistic vapor fractions and heat outputs, and COD reduction close to experimental values. Full article
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19 pages, 4090 KiB  
Article
The Behavior of Divalent Metals in Double-Layered Hydroxides as a Fenton Bimetallic Catalyst for Dye Decoloration: Kinetics and Experimental Design
by Edgar Oswaldo Leyva Cruz, Diana Negrete Godínez, Deyanira Angeles-Beltrán and Refugio Rodríguez-Vázquez
Catalysts 2025, 15(7), 687; https://doi.org/10.3390/catal15070687 - 16 Jul 2025
Viewed by 547
Abstract
This study investigates the influence of divalent metals—(Mg(II), Co(II), and Ni(II)) in layered double hydroxides (LDHs), with a constant trivalent Fe(III) component—on the decoloration of crystal violet and methyl blue dyes via a Fenton-type oxidation reaction. The catalysts, synthesized by co-precipitation and hydrothermal [...] Read more.
This study investigates the influence of divalent metals—(Mg(II), Co(II), and Ni(II)) in layered double hydroxides (LDHs), with a constant trivalent Fe(III) component—on the decoloration of crystal violet and methyl blue dyes via a Fenton-type oxidation reaction. The catalysts, synthesized by co-precipitation and hydrothermal treatment, were tested in both hydroxide and oxide forms under varying agitation conditions (0 and 280 rpm). A 22 × 3 factorial design was used to analyze the effect of the divalent metal type, catalyst phase, and stirring. The Mg/Fe oxide, with the highest BET surface area (144 m2/g) and crystallite size (59.7 nm), showed superior performance—achieving up to 98% decoloration of crystal violet and 97% of methyl blue within 1 h. The kinetic analysis revealed pseudo-second-order and pseudo-first-order fits for crystal violet and methyl blue, respectively. These findings suggest that LDH-based catalysts provide a fast, low-cost, and effective option for dye removal in aqueous systems. Full article
(This article belongs to the Section Environmental Catalysis)
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22 pages, 7389 KiB  
Article
FeCo-LDH/CF Cathode-Based Electrocatalysts Applied to a Flow-Through Electro-Fenton System: Iron Cycling and Radical Transformation
by Heng Dong, Yuying Qi, Zhenghao Yan, Yimeng Feng, Wenqi Song, Fengxiang Li and Tao Hua
Catalysts 2025, 15(7), 685; https://doi.org/10.3390/catal15070685 - 15 Jul 2025
Viewed by 344
Abstract
In this investigation, a hierarchical FeCo-layered double hydroxide (FeCo-LDH) electrochemical membrane material was prepared by a simple in situ hydrothermal method. The prepared material formed a 3D honeycomb-structured FeCo-LDH-modified carbon felt (FeCo-LDH/CF) catalytic layer with uniform open pores on a CF substrate with [...] Read more.
In this investigation, a hierarchical FeCo-layered double hydroxide (FeCo-LDH) electrochemical membrane material was prepared by a simple in situ hydrothermal method. The prepared material formed a 3D honeycomb-structured FeCo-LDH-modified carbon felt (FeCo-LDH/CF) catalytic layer with uniform open pores on a CF substrate with excellent catalytic activity and was served as the cathode in a flow-through electro-Fenton (FTEF) reactor. The electrocatalyst demonstrated excellent treatment performance (99%) in phenol simulated wastewater (30 mg L−1) under the optimized operating conditions (applied voltage = 3.5 V, pH = 6, influent flow rate = 15 mL min−1) of the FTEF system. The high removal rate could be attributed to (i) the excellent electrocatalytic oxidation performance and low interfacial charge transfer resistance of the FeCo-LDH/CF electrode as the cathode, (ii) the ability of the synthesized FeCo-LDH to effectively promote the conversion of H2O2 to •OH under certain conditions, and (iii) the flow-through system improving the mass transfer efficiency. In addition, the degradation process of pollutants within the FTEF system was additionally illustrated by the •OH dominant ROS pathway based on free radical burst experiments and electron paramagnetic resonance tests. This study may provide new insights to explore reaction mechanisms in FTEF systems. Full article
(This article belongs to the Special Issue Environmentally Friendly Catalysis for Green Future)
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18 pages, 3880 KiB  
Article
Sustainable Synthesis of Adipic Acid via MnOx-Catalyzed Electrooxidation of Cyclohexanol in Neutral Electrolyte
by Jiaming Shi, Guiling Zhang, Shiying Yang, Dan Yang, Yuguang Jin, Xiaoyue Wan, Yihu Dai, Yanhui Yang and Chunmei Zhou
Molecules 2025, 30(14), 2937; https://doi.org/10.3390/molecules30142937 - 11 Jul 2025
Viewed by 325
Abstract
Adipic acid (AA), a pivotal precursor for nylon-6,6 and polyurethane, was synthesized via an innovative catalytic electrocatalytic oxidation strategy in this study. Four distinct MnOx/CNT nanocatalysts were prepared by hydrothermal and co-precipitation methods and fabricated into electrodes for the oxidation of [...] Read more.
Adipic acid (AA), a pivotal precursor for nylon-6,6 and polyurethane, was synthesized via an innovative catalytic electrocatalytic oxidation strategy in this study. Four distinct MnOx/CNT nanocatalysts were prepared by hydrothermal and co-precipitation methods and fabricated into electrodes for the oxidation of cyclohexanol (Cy-OH) in a K2SO4 neutral solution. Comprehensive characterization revealed that the catalytic performance depended on both crystalline phase configuration and manganese valence states. MnO(OH) and MnOx were identified as the main active species, with the synergy between MnO species and carbon nanotubes significantly enhancing catalytic activity. Mechanistic investigations demonstrated that under Mn4+-dominant conditions, low-valence manganese species facilitated Cy-OH-to-cyclohexanone (Cy=O) conversion, while an optimal Oads/Olat ratio (≈1) effectively promoted subsequent Cy=O oxidation to AA. Under optimized conditions (1.25 V vs. Ag/AgCl, 80 °C, 15 h), complete Cy-OH conversion was achieved with 56.4% AA yield and exceptional Faradaic efficiency exceeding 94%. This work elucidates manganese-based electrocatalytic oxidation mechanisms, proposes a sequential reaction pathway, and establishes an environmentally benign synthesis protocol for AA, advancing sustainable industrial chemistry. Full article
(This article belongs to the Special Issue Nanomaterials for Catalytic Upcycling/Conversion of Plastics/Biomass)
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15 pages, 2499 KiB  
Article
Constructing Sulfur Vacancy-Rich NiCo2S4@MoS2 Core@shell Heterostructure via Interface Engineering for Enhanced HER Electrocatalysis
by Ziteng Song, Yuan Liu, Peng Yin, Jie Dai, Yingying Xu, Rongming Wang and Sibin Duan
Nanomaterials 2025, 15(14), 1061; https://doi.org/10.3390/nano15141061 - 9 Jul 2025
Viewed by 351
Abstract
The rational design of heterointerfaces with optimized charge dynamics and defect engineering remains pivotal for developing advanced non-noble metal-based electrocatalysts for water splitting. A comparative study of NiCo2S4–MoS2 heterostructures was conducted to elucidate the impact of interfacial architecture [...] Read more.
The rational design of heterointerfaces with optimized charge dynamics and defect engineering remains pivotal for developing advanced non-noble metal-based electrocatalysts for water splitting. A comparative study of NiCo2S4–MoS2 heterostructures was conducted to elucidate the impact of interfacial architecture and defect engineering on hydrogen evolution reaction (HER) performance. A core@shell NiCo2S4@MoS2 heterostructure was synthesized via a facile hydrothermal growth method, inducing lattice distortion and strong interfacial coupling, while supported NiCo2S4/MoS2 heterostructures were prepared by ultrasonic-assisted deposition. A detailed structural and spectroscopic characterization and theoretical calculation demonstrated that the core@shell configuration promotes charge redistribution across the NiCo2S4–MoS2 interface and generates abundant sulfur vacancies, thereby increasing the density of electroactive sites. Electrochemical measurements reveal that NiCo2S4@MoS2 markedly outperforms the supported heterostructure, single-component NiCo2S4, and MoS2 when serving as the HER catalyst in acid solution. These findings establish a dual-optimization strategy—combining interfacial design with vacancy modulation—that provides a generalizable paradigm for the deliberate design of high-efficiency non-noble metal-based electrocatalysts for water splitting reactions. Full article
(This article belongs to the Special Issue Nanostructured Materials for Electrocatalysis)
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18 pages, 3089 KiB  
Article
Biomass-Derived Catalysts with Dual Functions for Electrochemical Water Splitting
by Wangchuang Zhu, Xinghua Zhang, Qi Zhang, Lungang Chen, Xiuzheng Zhuang and Longlong Ma
Energies 2025, 18(14), 3592; https://doi.org/10.3390/en18143592 - 8 Jul 2025
Viewed by 247
Abstract
With the continuous consumption of fossil energy and the related environmental problems, clean energy, especially the hydrogen energy-derived water electrolysis, has attracted wide attention. However, as a result of the high energy consumption of water electrolysis and the limitations of single-function catalysts, there [...] Read more.
With the continuous consumption of fossil energy and the related environmental problems, clean energy, especially the hydrogen energy-derived water electrolysis, has attracted wide attention. However, as a result of the high energy consumption of water electrolysis and the limitations of single-function catalysts, there is an urgent need for cheap and simple-to-make bifunctional catalysts. In this work, based on the NiFe-LDH that is usually used for OER (Oxygen Evolution Reaction), doping of heteroatoms was carried out and a bifunctional catalyst could be then prepared using biomass as the carbon source. The preparation of catalyst precursors and in situ reduction were performed through the coupling process of hydrothermal and pyrolysis to enhance the electrolytic activity of the catalyst. Results showed that the overpotentials required to reach a current density of 10 mA·cm−2 for the HER and OER processes were 305.2 mV and 310.4 mV, respectively, which are superior to the commercial catalysts. In the subsequent characterization, the structural characteristics of the catalyst support and their structure–activity correlation with active metals were systematically investigated by TEM, XRD, and XPS analysis, providing mechanistic insights into the catalytic behavior. The basic catalytic mechanisms of HER and OER were also obtained: the HER process was due to the formation of a Ni3Fe alloy structure during catalyst preparation, which changed the electronic structure of the catalyst, while the OER process was induced by the formation of a NiOOH intermediate. The research results are expected to provide new ideas and data support for the preparation of bifunctional catalysts. Full article
(This article belongs to the Section A4: Bio-Energy)
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14 pages, 3884 KiB  
Article
Self-Supported Tailoring of Nickel Sulfide/CuCo Nanosheets into Hierarchical Heterostructures for Boosting Urea Oxidation Reaction
by Prince J. J. Sagayaraj, Aravind Senthilkumar, Juwon Lee, Eun-Kyeong Byeon, Hyoung-il Kim, Sulakshana Shenoy and Karthikeyan Sekar
Catalysts 2025, 15(7), 664; https://doi.org/10.3390/catal15070664 - 7 Jul 2025
Viewed by 635
Abstract
Electro-oxidation of urea (UOR) in alkaline medium is one of the most effective alternative ways of producing green hydrogen, as the oxidation potential in UOR is less and thermodynamically more favorable than conventional water oxidation. The development of cost-effective materials in catalyzing UOR [...] Read more.
Electro-oxidation of urea (UOR) in alkaline medium is one of the most effective alternative ways of producing green hydrogen, as the oxidation potential in UOR is less and thermodynamically more favorable than conventional water oxidation. The development of cost-effective materials in catalyzing UOR is recently seeking more attention in the research hotspot. Suitably modifying the Ni-based catalysts towards active site creation and preventing surface passivation is much important in this context, following which we reported the synthesis of Ni3S2 (NS) supported with CuCo (CC) bimetallic (NSCC). A simple hydrothermal route for NS synthesis and the electrodeposition method for CuCo (CC) deposition is adapted in a self-supported manner. The NS and CC catalysts exhibited sheet-like morphology, as confirmed by SEM and TEM analysis. The bimetallic CC deposition prevented the surface passivation of nickel sulfide (NS) over oxygen evolution reaction (OER) and improved the charge-transfer kinetics. The NSCC catalyst catalyzed UOR in an alkaline medium, which required a lower potential of 1.335 V vs. RHE to attain the current density of 10 mAcm−2, with a lower Tafel slope value of 131 mVdec−1. In addition, a two-electrode cell setup is constructed with an operating cell voltage of 1.512 V for delivering 10 mAcm−2 current density. This study illustrates the new strategy of designing heterostructure catalysts for electrocatalytic UOR. Full article
(This article belongs to the Special Issue Homogeneous and Heterogeneous Catalytic Oxidation and Reduction)
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