Search Results (97)

A binder-free Co₃O₄ nanoneedle electrode grown directly on nickel foam (Co₃O₄@NF) was fabricated by hydrothermal synthesis followed by calcination and evaluated for electrocatalytic nitrate reduction to ammonium. The integrated three-dimensional architecture combines the catalytic activity of Co₃O₄ with the high conductivity and open porosity of nickel foam, thus exposing abundant active sites, shortening electron-transfer pathways, and facilitating mass transport. Among the electrodes prepared at different calcination temperatures, Co₃O₄@NF calcined at 400 °C delivered the best performance. Under the optimal conditions of −1.4 V vs. Ag/AgCl, pH 7, and an initial NO₃⁻-N concentration of 50 mg L⁻¹, the electrode achieved 83.4% nitrate removal within 480 min together with 98.7% ammonium selectivity. Electrochemical measurements revealed a markedly enlarged electrochemically active surface area and reduced charge-transfer resistance after Co₃O₄ loading. Mechanistic analyses via TBA quenching experiments and DFT calculations revealed that both the direct pathway and the hydrogen-assisted indirect pathway were operative, with the indirect pathway being dominant due to its lower free energy barrier while maintaining negligible nitrite accumulation. The electrode also showed good cycling stability and retained high ammonium selectivity in real water matrices. These results demonstrate that binder-free Co₃O₄ nanoneedles supported on nickel foam constitute a promising cathode architecture for coupling nitrate removal with ammonia recovery. Full article

This study investigates the hydrothermal modification of commercial titanium dioxide (TiO₂) in the presence of a natural licorice root extract (Glycyrrhiza glabra L.), serving as a stabilizing and growth-modulating agent. The experimental framework combines hydrothermal treatment in a Teflon-lined autoclave with subsequent thermal calcination to elucidate the structural, morphological, and chemical evolution of the material. The plant-based extract significantly influences particle assembly during synthesis, fostering the formation of an initial organic–inorganic hybrid system that results in enhanced morphological homogeneity compared to pristine TiO₂. Thermal analyses (TGA and DSC) demonstrated the progressive decomposition of the organic components with increasing temperature, yielding a thermally stable, predominantly inorganic material at 600 °C. Scanning Electron Microscopy (SEM) observations confirmed a more uniform particle distribution in the modified samples. X-ray diffraction (XRD) patterns corroborated that the primary crystalline phase of TiO₂ remains intact across all conditions, with structural variations limited to peak definition and long-range organization. Furthermore, FTIR spectroscopy supported the preservation of characteristic TiO₂ vibrational features while indicating a gradual depletion of weakly bound surface species following thermal treatment. In conclusion, these findings demonstrate that natural extracts can effectively function as growth-modulating agents, steering material organization without altering its intrinsic chemical properties. This approach aligns with the principles of Green Chemistry and the circular economy, highlighting the potential of renewable plant-based resources as functional additives for the sustainable processing of inorganic materials. Rather than seeking to outperform commercial benchmarks, this work establishes a viable and low-environmental-impact strategy for morphological and structural modulation. Full article

Despite exhibiting exceptional structural stability, spinel lithium titanate (Li₄Ti₅O₁₂, LTO) suffers from inherent limitations in both electronic conductivity and ionic diffusion kinetics, limiting its high-rate application. In this study, pringle-shaped Li₄Ti₅O₁₂/carbon (LTO/C) composite was synthesized using low-cost sucrose as the organic carbon source, using a facile hydrothermal-calcination method. Each pringle-shaped nanosheet was composed of Li₄Ti₅O₁₂ nanoparticles that are 15 nm in size, which can shorten lithium-ion diffusion distances as well as better the contact between electrolyte and active materials. Meanwhile, the uniform carbon cladding improves the material’s electronic conductivity. Owing to the synergistic effects between the mesoporous LTO nanosheets and carbon coating, LTO/C-6.31 wt% presented remarkable rate capability and cycling stability, delivering 145.5 mAh g⁻¹ at 20 C over 1000 cycles with 93.93% capacity retention. This work demonstrates an effective synthesis route to developing high-rate capability and long-cycle-life anode materials for LIBs. Full article

Two mineral-based solid residues, namely coal gangue (CG) and phosphorus tailings (PT), two of the largest solid waste streams in the mining industry, were used as the sole metal feedstocks to fabricate a novel MgCaFeAl layered double hydroxide (LDH-GT) via a 700 °C calcination, acid leaching and hydrothermal coprecipitation route, with simultaneous synthesis of white carbon black from the reaction byproducts. Under optimized conditions (total metal load is 150 mg kg⁻¹, LDH-GT dose is 0.09 g, pH from 6 to 7), the synthesized material achieved concurrent immobilization efficiencies of 76.28%, 99.96%, and 99.95% for Cr (VI), Cd (II) and Ni (II), respectively, within a 24 h reaction period. TCLP leachability decreased by 82 to 91% relative to the untreated soil. After three wetting, drying and freeze–thaw cycles, the leached concentrations of all three metals remained below 0.3 mg L⁻¹, confirming excellent long-term stability. Mechanistic analyses revealed that Cr (VI) was mainly sequestered through interlayer anion exchange and surface complexation, whereas Cd (II) and Ni (II) were immobilized via isomorphic substitution into the LDH lattice, precipitation as carbonates, and incorporation into Fe/Mn oxides. A 7-day mung bean bioassay showed that LDH-GT amendment increased seed germination from 50% to 73%, enhanced root and shoot biomass by 1.1- to 1.6-fold, and decreased plant Cr, Cd, and Ni contents by over 80%. The 16S rRNA sequencing further demonstrated that LDH-GT reversed the decline in microbial α diversity induced by heavy metal stress, restored aerobic chemoheterotrophic and sulfur cycling functional guilds, and reduced pathogenic signatures. This study provides the demonstration of a waste-to-resource LDH that achieves efficient, durable remediation of multi-metal-contaminated soils, offering a scalable route for coupling solid waste valorization with in situ site restoration. Full article

The NiCo₂O₄/nickel cobalt sulfide (NiCoS) electrode was constructed on a nickel foam (NF) substrate using a combination of hydrothermal synthesis and constant potential electrodeposition. The NiCo₂O₄ prepared via an in situ hydrothermal method followed by calcination served as an intermediate layer, providing structural support and abundant active sites for the subsequent electrodeposition of the NiCoS top layer. The NiCoS loading amount was optimized by adjusting the deposition time. The optimized NiCo₂O₄/NiCoS electrode delivered an areal specific capacitance (Cs) of 6.94 F cm⁻² at a discharge current density of 2 mA cm⁻² with a coulombic efficiency of 98.85%. It retained 64.52% of its initial capacitance as the current density increased from 2 to 80 mA cm⁻² and exhibited an equivalent series resistance (R_ESR) of 1.06 Ω cm⁻². Furthermore, the NiCo₂O₄/NiCoS electrode retained 88.24% of its initial capacitance after 700 charge/discharge cycles, eventually stabilizing at 81.25% within 4000 cycles. Full article

Contamination of water bodies caused by increasing human and industrial activities poses a serious threat to human health and environmental sustainability, highlighting the need for green and efficient remediation strategies. In this study, a facile hydrothermal synthesis followed by controlled calcination was developed to fabricate phase-pure α- and β-Bi₂O₃ with a unique coral-like hierarchical morphology as visible-light-active photocatalysts. Phase selectivity was achieved by tuning the calcination temperature, yielding pure β-Bi₂O₃ while preserving the hierarchical structure. Optical characterization revealed a narrower bandgap for β-Bi₂O₃ (2.24 eV) compared to α-Bi₂O₃ (2.75 eV), favoring visible-light absorption. Photocatalytic performance was evaluated using Rhodamine B as a model pollutant, where β-Bi₂O₃ achieved complete degradation within 240 min, significantly outperforming α-Bi₂O₃. The degradation followed pseudo-first-order kinetics, and the catalyst exhibited excellent robustness and reusability. To further demonstrate applicability toward persistent contaminants, Methyl Orange (MO) and the antibiotic ciprofloxacin (CIP) were employed as additional model pollutants. The coral-like β-Bi₂O₃ showed high visible-light activity toward MO, including complete removal under acidic conditions. Moreover, efficient degradation of CIP was achieved at neutral pH, with 90% removal within 150 min and complete degradation after 240 min. Overall, these results highlight coral-like β-Bi₂O₃ as an efficient standalone photocatalyst for visible-light-driven degradation of dye and pharmaceutical pollutants. Full article

The study investigates the structural and thermal properties of zirconia ceramics doped with Sm₂O₃. The powders were prepared via a mild hydrothermal synthesis route at a temperature of 200 °C, for 2 h with a pressure of 60–100 atm, starting from ZrO₂-Sm₂O₃ compositions. Structural and physicochemical characterization was performed using XRD, SEM-EDAX, BET and FT-IR analyses after synthesis and subsequent heat treatments up to 1500 °C. The results indicate good thermal stability of the materials, while a single cubic phase is achieved after calcination at 1500 °C. The ceramics show low thermal conductivity (0.41 W·m⁻¹·K⁻¹), reduced heat capacity (0.26 J·g⁻¹·K⁻¹), and low thermal diffusivity (0.34 mm²·s⁻¹), with all measured parameters lower than those commonly reported for conventional rare-earth-stabilized zirconia. Full article

This paper introduces a streamlined three-step synthesis method for crafting porous Fe₂O₃/ZnO nanofibers (NFs). Initially, Fe₂O₃ nanoparticles (NPs) were synthesized using the hydrothermal method. Subsequently, PVP NFs laden with Fe₂O₃ NPs and zinc salt were synthesized via an electrospinning method. Finally, porous Fe₂O₃/ZnO NFs were fabricated through calcination, resulting in an average diameter of approximately 100 nm. Gas-sensing experiments illuminate that the porous Fe₂O₃/ZnO NFs exhibit outstanding sensitivity, selectivity, and robust long-term stability. Although the response magnitude decreased under high relative humidity (RH) due to competitive adsorption, the sensor maintained distinct detectable responses towards NO₂ vapor at an optimum temperature of 225 °C. Particularly noteworthy is the substantial enhancement in NO₂ sensing properties observed in the Fe₂O₃/ZnO composite compared to pure ZnO NFs. This enhancement can be ascribed to the distinctive microstructure and heterojunction formed between Fe₂O₃ and ZnO. Full article

The aim of the presented work is to develop a more energy- and time-saving modification of a well-known hydrothermal synthesis method by reducing the time of the synthesis regime and drying step, as well as the possible removal of the calcination procedure. The structure and morphology of Gd-doped ceria (Ce_1−xGd_xO_2−x/2, where x = 0, 0.1, 0.2, 0.3, and 0.5), synthesized via the optimized hydrothermal method, were thoroughly investigated. Phase composition was analyzed using X-ray diffraction (XRD), while the structural units of the materials were identified by Fourier-transform infrared spectroscopy (FTIR). Chemical composition was studied using energy-dispersive X-ray spectroscopy (EDS) and further confirmed by energy-dispersive X-ray fluorescence (EDXRF). Transmission electron microscopy (TEM) was employed to analyze the size and shape of the nanoparticles. Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) confirmed the presence of Ce³⁺ ions in both doped and undoped CeO₂ samples. Full article

The eco-toxicological impacts caused by organic pollutants in aquatic environments have emerged as a global concern in recent decades, resulting from the potential hazards they present to ecosystem integrity and human health. Decorating active components on mesoporous silica is considered a popular approach by which to obtain synergistic effects in persulfate activation for sustainable water decontamination. However, at present there has been no review focusing solely, specifically and comprehensively on this field. Therefore, this paper places an emphasis on the latest research progress on the synthesis and physicochemical properties of functionalized mesoporous silica materials as well as their catalytic performance. The preparation methods included co-condensation, impregnation, grinding–calcination, hydrothermal synthesis and chemical precipitation, and their synthesis parameters played a major role in the characterization of materials, thereby affecting pollutant elimination. Metal redox cycles, nonmetallic activation and confinement effects contributed to persulfate activation. Targeted pollutants were degraded via radical pathways, non-radical pathways, or a combination of the two. The effects and causes of operational conditions (catalyst and persulfate dosage, initial pollutant concentration, temperature, initial pH, co-existing anions, and natural organic matter) varied across the degradation systems, and they were categorized and summarized in detail. Furthermore, functionalized mesoporous silica presented excellent reusability, stability and applicability in practical application. Finally, current potential directions for further research and sustainable development in this field were also prospected. This critical analysis aims to fuel the evolution of functionalized mesoporous silica catalyst-driven persulfate system application in water treatment and to bridge prevailing knowledge gaps. Full article

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

Bimetallic catalysts can effectively enhance the catalytic degradation efficiency of peroxymonosulfate (PMS), which is usually attributed to the enhancement of electron transfer, but currently, there is no clear explanation of the mechanism of how the electron transfer is enhanced. A nitrogen-doped Fe/Mn composite biochar (FeMn-NBC) was co-constructed by hydrothermal synthesis and high-temperature calcination. The FeMn-NBC activated PMS more efficiently than the monometallic one due to the enhanced electron transfer between Fe and Mn. The FeMn-NBC/PMS system activated PMS with Mn as the active center, and the high oxidation state of Mn⁴⁺ promoted the acceleration of the PMS adsorption of the generation of Mn²⁺/Mn³⁺. This gaining effect accelerated the electron cycling between Fe²⁺/Fe³⁺ and Mn²⁺/Mn³⁺/Mn⁴⁺, which enhanced the PMS catalysis to generate free radicals (•OH, SO₄^•− and •O₂⁻) and non-radicals (¹O₂) for the efficient degradation of diisobutyl phthalate (DIBP). Benefiting from this gaining effect, the degradation rate of DIBP by the FeMn-NBC/PMS system was increased by 2.43 and 3.38 times compared to Fe-NBC and Mn-NBC. The bimetallic-enhanced electron transfer mechanism proposed in this study facilitated the development of efficient catalysts for more efficient and selective removal of organic pollutants. Full article

The present study demonstrates, for the first time, the fundamental possibility of producing electrode materials for sodium-ion batteries through low-temperature carbothermic smelting of ilmenite concentrate fluxed with calcined soda and diatomite, followed by aqueous refining of titanium slag. The primary phase composition of the slag includes Na₂Ti₃O₇ (48.2%), Na_0.23TiO₂ (22.0%), Na₂TiSiO₅ (11%), and Na_0.67Al_0.1Mn_0.9O₂ (8.5%), which, upon hydrolysis, transform into a monophase titanium dioxide with intercalated sodium—Na_0.23TiO₂. Thermodynamic analysis of the heat effects of chemical reactions among raw materials and resulting products substantiates the role of silicon and sodium oxides, carbon, oxygen, and water in the formation of various electrode materials during carbothermic flux conversion and aqueous refining. Insights into the mechanisms of thermochemical formation and hydrothermal phase transformations offer a scientific basis for the development of intercalation systems from abundant and low-cost natural raw materials, bypassing the need for expensive precursor synthesis. Full article

Developing efficient bifunctional electrocatalysts with excellent stability at high current densities for overall water splitting is a challenging yet essential objective. However, transition metal phosphides encounter issues such as poor dispersibility, low specific surface area, and limited electronic conductivity, which hinder the achievement of satisfactory performance. Therefore, this study presents the highly efficient bifunctional electrocatalyst of CeO₂-modified NiFe phosphide on nickel foam (CeO₂/Ni₂P/Fe₂P/NF). Ni₂P/Fe₂P coupled with CeO₂ was deposited on nickel foam through hydrothermal synthesis and sequential calcination processes. The electrocatalytic performance of the catalyst was evaluated in an alkaline solution, and it exhibited an HER overpotential of 87 mV at the current density of 10 mA cm⁻² and an OER overpotential of 228 mV at the current density of 150 mA cm⁻². Furthermore, the catalyst demonstrated good stability, with a retention rate of 91.2% for the HER and 97.3% for the OER after 160 h of stability tests. The excellent electrochemical performance can be attributed to the following factors: (1) The interface between Ni₂P/Fe₂P and CeO₂ facilitates electron transfer and reactant adsorption, thereby improving catalytic activity. (2) The three-dimensional porous structure of nickel foam provides an ideal substrate for the uniform distribution of Ni₂P, Fe₂P, and CeO₂ nanoparticles, while its high conductivity facilitates electron transport. (3) The incorporation of larger Ce³⁺ ions in place of smaller Fe³⁺ ions leads to lattice distortion and an increase in defects within the NiFe-layered double hydroxide structure, significantly enhancing its catalytic performance. This research finding offers an effective strategy for the design and synthesis of low-cost, high-potential catalysts for water electrolysis. Full article

Mixed oxides were obtained via calcination at 550 °C from layered double hydroxides (LDHs), which were synthesized in a previous study via co-precipitation and co-precipitation followed by hydrothermal treatment using aluminum residues as the source of this element. After characterization, these oxides (Mg-Al-_LDH-CP and Mg-Al-_LDH-H, named according to the synthesis methods of the precursor LDHs) were applied as heterogeneous catalysts in the methyl transesterification of ethyl acetate (EA). The formation of mixed oxides was confirmed by the absence of basal peaks associated with the layered LDH structure in the XRD analysis, due to calcination. Further characterization revealed that Mg-Al-_LDH-CP exhibited the highest number of acidic sites, while Mg-Al-_LDH-H had the highest number of basic sites. The transesterification activity was evaluated in the reaction between ethyl acetate (EA) and methanol (MeOH). The best result, obtained under a molar ratio of 1:5:0.005 (EA:MeOH:catalyst) at 120 °C, was a 63% conversion after 360 min of reaction for the Mg-Al-_LDH-CP catalyst, which had a higher number of acidic sites and fewer basic sites. Additionally, the catalysts demonstrated robustness, maintaining catalytic activity over four cycles without a significant decrease in performance. These results indicate the feasibility of using mixed oxides derived from LDH, synthesized from aluminum residues, as heterogeneous catalysts in transesterification reactions, highlighting their potential for advancing more sustainable catalyst development. Full article