Search Results (898)

In this study, an innovative and sustainable strategy for the valorization of olive leaves, an underutilized agro-industrial byproduct, was developed through enzymatic-assisted aqueous extraction to produce a polyphenol-rich olive leaf extract (OLE). The extract contained notable concentrations of hydroxytyrosol (0.53 mg/L), luteolin-7-o-glucoside (0.70 mg/L), apigenin-4-o-glucoside (0.18 mg/L), and oleuropein (4.24 mg/L). For the first time, this OLE was successfully nanoencapsulated into layered double hydroxides (LDHs) synthesized at Zn²⁺/Al³⁺ molar ratios of 1:1, 2:1, and 3:1, resulting in a series of OLE@LDH_Zn/Al_x/1 nanohybrids. Comprehensive structural characterization confirmed the successful intercalation of OLE within the LDH interlayer galleries. Antioxidant activity (via DPPH assay), total polyphenol content (TPC), and antibacterial tests were conducted to evaluate functionality. Among the nanohybrids, OLE@LDH_Zn/Al_1/1 exhibited the highest TPC (606.6 ± 7.0 mg GAE/L), the lowest EC_50,DPPH, EC_50,ABTS, and EC_50,FRAP values (27.88 ± 1.82, 25.70 ± 0.76, and 39.42 ± 2.16 mg/mL), and superior antibacterial performance against E. coli and S. aureus. Moreover, pH-dependent release revealed targeted polyphenol release under acidic conditions (pH = 1), simulating gastric environments. These results highlight LDHs, particularly with a Zn/Al ratio of 1:1, as promising nanocarriers for the stabilization and controlled release of plant-derived polar phenols, with potential applications in nutrition, food preservation, and biomedicine. Full article

Electrochemical water splitting for hydrogen production is considered a key pathway for achieving sustainable energy conversion. However, the sluggish reaction kinetics of the oxygen evolution reaction (OER) and high overpotentials severely hinder the large-scale application of water electrolysis technology. Nickel–iron layered double hydroxide (NiFe-LDH) has gained attention as a promising non-precious metal OER catalyst due to its abundant active sites and good intrinsic activity. However, its relatively low conductivity and charge transfer efficiency limit the improvement of catalytic performance. Therefore, this study used a simple hydrothermal method to generate a NiFe-LDH/Cs_0.32WO₃ heterojunction composite catalyst, relying on the excellent electronic conductivity of Cs_0.32WO₃ to improve overall charge transfer efficiency. According to electrochemical testing results, the modified NiFe-LDH/Cs_0.32WO₃-20 mg achieved a low overpotential of 349 mV at a current density of 10 mA cm⁻², a Tafel slope of 67.0 mV dec⁻¹, and a charge transfer resistance of 65.1 Ω, which represent decreases of 39 mV, 23.1%, and 40%, respectively, compared to pure NiFe-LDH. The key to performance improvement lies in the tightly bonded heterojunction interface between Cs_0.32WO₃ and NiFe-LDH. X-ray photoelectron spectroscopy (XPS) shows a distinct interfacial charge transfer phenomenon, with a notable negative shift of the W4f peak (0.85 eV), indicating the directional transfer of electrons from Cs_0.32WO₃ to NiFe-LDH. Under the influence of the built-in electric field within the heterojunction, this interfacial charge redistribution improved the electronic structure of NiFe-LDH, increased the proportion of high-valent metal ions, and significantly enhanced the OER reaction kinetics. This study provides new insights for the preparation of efficient heterojunction electrocatalysts. Full article

The production of biodiesel from microalgae presents a sustainable and renewable solution to the growing global energy demands, with catalysts playing a critical role in optimizing the transesterification process. This study examines the emerging catalysts and innovative techniques utilized in converting microalgal lipids into fatty acid methyl esters, emphasizing their impact on reaction efficiency, yield, and environmental sustainability. Sulfuric acid demonstrates excellent performance in in situ transesterification, while NaOH/zeolite achieves high biodiesel yields using ultrasound- and microwave-assisted methods. Metal oxides such as CuO, NiO, and MgO supported on zeolite, as well as ZnAl-layered double hydroxides (LDHs), further enhance reaction performance through their high activity and stability. Enzymatic catalysts, particularly immobilized lipases, provide a more environmentally friendly option, offering high yields (>90%) and the ability to operate under mild conditions. However, their high cost and limited reusability pose significant challenges. Ionic liquid catalysts, such as tetrabutylphosphonium carboxylate, streamline the process by eliminating the need for drying and lipid extraction, achieving yields as high as 98% from wet biomass. The key novelty of this work lies in its detailed focus on the use of ionic liquids and nanocatalysts in microalgae-based biodiesel production, which are often underrepresented in previous reviews that primarily discuss homogeneous and heterogeneous catalysts. Full article

The development of low-cost and high-efficiency oxygen evolution reaction (OER) catalysts is essential to enhance the practicality of electrochemical water splitting for green hydrogen production. Layered double hydroxides (LDHs), especially those based on nickel and cobalt, have attracted attention due to their tunable composition, abundant redox-active sites, and earth-abundant constituents. However, their application is hindered by their limited conductivity and sluggish reaction kinetics. In this study, rare-earth-element-doped NiCo LDHs were synthesized directly on nickel foam through a one-step hydrothermal approach to improve the OER activity by modulating the electronic structure and optimizing the surface morphology. Among the representative catalysts, the incorporation of Sm significantly influenced the microstructure and electronic configuration of the catalyst, as confirmed by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). Electrochemical tests showed that the optimized Sm-NiCo LDH achieved a low overpotential of 172 mV at 10 mA cm⁻² and a small Tafel slope of 84 mV dec⁻¹ in 1 M KOH, indicating an expanded electrochemically active surface and improved charge transport. Long-term stability tests further showed its durability. These findings suggest that Sm doping enhances the OER performance by increasing active site exposure and promoting efficient charge transfer, offering a promising strategy for designing rare-earth-modified, non-precious-metal-based OER catalysts. Full article

The development of an economical and efficient method for recovering phosphate (PO₄³⁻-P) and ammonium nitrogen (NH₄⁺-N) is of paramount importance for environmental remediation. The preparation of Mg/Fe-loaded biochar (Mg/Fe-BC) was achieved through chemical precipitation followed by pyrolysis in this study. Single solution adsorption studies indicated that temperature significantly affected how effectively Mg/Fe-BC could adsorb and remove NH₄⁺-N, whereas PO₄³⁻-P adsorption showed minimal temperature sensitivity. In mixed simulated solutions, In the mixed simulated solution, the maximum adsorption capacities of Mg/Fe-BC for PO₄³⁻-P and NH₄⁺-N were 145.97–153.05 mg/g and 112.63–121.51 mg/g, respectively. The optimal dosage for synergistic adsorption was determined to be 3 g/L, while pH values ranging from 3 to 9 exhibited negligible effects on the adsorption of both contaminants. The presence of Ca²⁺ and HCO₃⁻ in the solution may interfere with the simultaneous adsorption of PO₄³⁻-P and NH₄⁺-N. SEM-EDS and XPS analyses revealed that the primary adsorption mechanisms of PO₄³⁻-P and NH₄⁺-N by Mg/Fe-BC involved electrostatic attraction, ion exchange, and hydrogen bonding. In practical applications using chicken manure biogas slurry, Mg/Fe-BC demonstrated synergistic adsorption effects, achieving removal efficiencies of 86.86% for PO₄³⁻-P and 36.86% for NH₄⁺-N, thereby confirming its potential application value in wastewater treatment. Full article

CO₂ methanation offers a sustainable route to reduce greenhouse gas emissions by converting carbon dioxide into methane, a valuable renewable fuel. This exothermic reaction not only mitigates its environmental impact but also provides energy-efficient benefits, as the heat generated can be reused in industrial applications. In this study, CO₂ methanation was carried out in a continuous flow reactor with a CO₂:H₂ molar ratio of 1:4 and a gas hourly space velocity (GHSV) of 12,000 h⁻¹, using a Ni-Al-LDH catalyst with a molar ratio of 2.3. The research focused on how calcination and reduction conditions affect catalyst structure and activity. Characterization techniques such as BET, XRD, TPR, H₂-TPD, and CO₂-TPD revealed that these conditions significantly influence surface area, crystallinity, phase composition, and metal dispersion. A higher reduction temperature decreased the surface area and increased both the crystallite size and basicity. The findings highlight that thermal treatment play a crucial role in optimizing the catalytic properties of NiAl catalyst. The sample calcined at 600 °C showed greater activity at lower reaction temperatures, while the catalyst calcined at 400 °C performed better above 300 °C. Additionally, the evaluation of the effect of the reduction atmosphere during catalyst activation showed that H₂ is a more effective reducing gas at lower reaction temperatures, whereas biogas showed a better performance at higher temperatures. Importantly, XRD results showed the catalysts maintained their structural integrity post-reaction, with no significant carbon deposition in the H₂ atmosphere, confirming their potential for long-term application in CO₂ methanation. Full article

A facile and versatile strategy to obtain NPs@ZnAlO nanocomposite materials, comprising controlled-size nanoparticles (NPs) within a ZnAlO matrix is reported. The mono-(Au, Ni) and bimetallic (Ni-Au) NPs serving as an active phase were prepared by the polyol-alkaline method, while the ZnAlO support was obtained via the thermal decomposition of its corresponding layered double hydroxide (LDH) precursors. X-ray diffraction (XRD) patterns confirmed the successful fabrication of the nanocomposites, including the synthesis of the metallic NPs, the formation of LDH-like structure, and the subsequent transformation to ZnO phase upon LDH calcination. The obtained nanostructures confirmed the nanoplate-like morphology inherited from the original LDH precursors, which tended to aggregate after the addition of gold NPs. According to the UV-Vis spectroscopy, loading NPs onto the ZnAlO support enhanced the light absorption and reduced the band gap energy. ATR-DRIFT spectroscopy, H₂-TPR measurements, and XPS analysis provided information about the functional groups, surface composition, and reducibility of the materials. The catalytic performance of the developed nanostructures was evaluated by the photodegradation of bisphenol A (BPA), under simulated solar irradiation. The conversion of BPA over the bimetallic Ni-Au@ZnAlO reached up to 95% after 180 min of irradiation, exceeding the monometallic Ni@ZnAlO and Au@ZnAlO catalysts. Its enhanced activity was correlated with good dispersion of the bimetals, narrower band gap, and efficient charge carrier separation of the photo-induced e⁻/h⁺ pairs. Full article

Maritime corrosion is a global problem often retarded through protective coatings containing corrosion inhibitors (CIs). ZnAl layered double hydroxides (LDH) have been used to immobilize CIs, which can reduce their early leaching and, thus, foster long-term corrosion protection. However, the environmental behavior of these nanomaterials remains largely unknown, particularly in the context of global changes. The present study aims to assess the environmental behavior of four anti-corrosion nanomaterials in an ocean acidification scenario (IPCC SSP3-7.0). Three different concentrations of the nanostructured CIs (1.23, 11.11, and 100 mg L⁻¹) were prepared and maintained at 20 °C and 30 °C in artificial salt water (ASW) at two pH values, with and without the presence of organic matter. The nanomaterials’ particle size and the release profiles of Al³⁺, Zn²⁺, and anions were monitored over time. In all conditions, the hydrodynamic size of the dispersed nanomaterials confirmed that the high ionic strength favors their aggregation/agglomeration. In the presence of organic matter, dissolved Al³⁺ increased, while Zn²⁺ decreased, and increased in the ocean acidification scenario at both temperatures. CIs were more released in the presence of humic acid. These findings demonstrate the influence of the tested parameters in the nanomaterials’ environmental behavior, leading to the release of metals and CIs. Full article

Films of a Ni/Al-layered double hydroxide intercalated with reduced graphene oxide were deposited, by means of a simple and rapid electrochemical synthesis, on Pt electrodes previously submitted to a special cleaning procedure. The aim of the research was to determine whether the better electrocatalytic properties of the Ni(III)/Ni(II) couple, due to the presence of the carbon nanomaterial, as compared to the Ni/Al-LDH alone, could allow glucose detection at physiological pHs, as normally LDHs work as redox mediators in basic solutions. Chronoamperometric experiments were carried out by applying a potential of 1.0 V vs. SCE to the electrode soaked in solutions buffered at pHs from 5.0 to 9.0 to which glucose was continuously added. The steady-state currents increased as the pH solution increased, but at pH = 7.0 the modified electrode exhibited a fast and rather sensitive response, which was linear up to 10.0 mM glucose, with a sensitivity of 0.56 A M⁻¹ cm⁻² and a limit of detection of 0.05 mM. Our results suggest the potential application of Ni/Al-LDH(ERGO) composite for the non-enzymatic detection of glucose or other oxidizable analytes under biological conditions. Full article

This review article compiled previous reports in the fabrication of hydroquinone (HQ) electrochemical sensors using differently modified electrodes. The electrode materials, which are also called electrocatalysts, play a crucial role in electrochemical detection of biomolecules and toxic substances. Metal oxides, MXenes, carbon-based materials such as reduced graphene oxide (rGO), carbon nanotubes (CNTs), layered double hydroxides (LDH), metal sulfides, and hybrid composites were extensively utilized in the fabrication of HQ sensors. The electrochemical performance, including limit of detection, linearity, sensitivity, selectivity, stability, reproducibility, repeatability, and recovery for real-time sensing of the HQ sensors have been discussed. The limitations, challenges, and future directions are also discussed in the conclusion section. It is believed that the present review article may benefit researchers who are involved in the development of HQ sensors and catalyst preparation for electrochemical sensing of other toxic substances. Full article

To date, one of the main problems associated with the engineering application of metallic materials is corrosion protection. To increase their durability and reduce damage, a variety of protection methods have been studied and applied. In recent decades, coating techniques have become increasingly important. Among these coatings, Layered Double Hydroxides (LDHs) have shown unique properties, such as ion exchange, high adhesion, and hydrophobicity, particularly useful for biomedical applications. In this review, after a detailed exposition of the LDHs’ synthesis processes, the most recent corrosion protection methods are illustrated. Intercalation of corrosion inhibitors and release kinetics of intercalates are presented. Although this work is mainly focused on laboratory-scale investigations and fundamental research, the problems inherent to large-scale industrial manufacturing and application are outlined and briefly discussed. Full article

Recently, it has been found that electrochemical sensing technology is one of the significant approaches for the monitoring of toxic and hazardous substances in food and the environment. Nitrofurazone (NFZ) and nitrofurantoin (NFT) possess a hazardous influence on the environment, aquatic life, and human health. Thus, various advanced materials such as graphene, carbon nanotubes, metal oxides, MXenes, layered double hydroxides (LDHs), polymers, metal–organic frameworks (MOFs), metal-based composites, etc. are widely used for the development of nitrofurazone and nitrofurantoin sensors. This review article summarizes the progress in the fabrication of electrode materials for nitrofurazone and nitrofurantoin sensing applications. The performance of the various electrode materials for nitrofurazone and nitrofurantoin monitoring are discussed. Various electrochemical sensing techniques such as square wave voltammetry (SWV), differential pulse voltammetry (DPV), linear sweep voltammetry (LSV), amperometry (AMP), cyclic voltammetry (CV), and chronoamperometry (CA) are discussed for the determination of NFZ and NFT. It is observed that DPV, SWV, and AMP/CA are more sensitive techniques compared to LSV and CV. The challenges, future perspectives, and limitations of NFZ and NFT sensors are also discussed. It is believed that present article may be useful for electrochemists as well materials scientists who are working to design electrode materials for electrochemical sensing applications. Full article

The structural memory effect is normally considered one of the most important properties of LDHs. However, certain anions can have adverse effects on it. In this study, three types of CLDHs (Mg2Al1-CLDH, Mg2Al0.5Fe0.5-CLDH, Mg2Fe1-CLDH) were obtained and used to observe their regeneration behaviors in the presence of sulfate, silicate, and phosphate, respectively, at initial pH values of 10 and 13. The samples were characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTG), scanning electron microscope (SEM), and N2 adsorption–desorption isotherm (BET). The results suggested that silicate and phosphate have significant impacts on the regeneration of CLDHs, while sulfate does not. Specifically, phosphate and silicate reacted with MgO to generate magnesium silicate and magnesium phosphate dibasic, which were covered on the surface of particles and hindered the hydroxylation of metal oxides. However, a higher pH can suppress the formation of new substances and promote the regeneration of LDHs. Moreover, the CLDHs with high specific surface area had a stronger anti-interference performance regarding the effects of phosphate and silicate. Full article

Direct Air Capture (DAC) is emerging as a critical climate change mitigation strategy, offering a pathway to actively remove atmospheric CO₂. This comprehensive review synthesizes advancements in DAC technologies, with a particular emphasis on the pivotal role of nanostructured solid sorbent materials. The work critically evaluates the characteristics, performance, and limitations of key nanomaterial classes, including metal–organic frameworks (MOFs), covalent organic frameworks (COFs), zeolites, amine-functionalized polymers, porous carbons, and layered double hydroxides (LDHs), alongside solid-supported ionic liquids, highlighting their varied CO₂ uptake capacities, regeneration energy requirements, and crucial water sensitivities. Beyond traditional temperature/pressure swing adsorption, the review delves into innovative DAC methodologies such as Moisture Swing Adsorption (MSA), Electro Swing Adsorption (ESA), Passive DAC, and CO₂-Binding Organic Liquids (CO₂ BOLs), detailing their unique mechanisms and potential for reduced energy footprints. Despite significant progress, the widespread deployment of DAC faces formidable challenges, notably high capital and operational costs (currently USD 300–USD 1000/tCO₂), substantial energy demands (1500–2400 kWh/tCO₂), water interference, scalability hurdles, and sorbent degradation. Furthermore, this review comprehensively examines the burgeoning global DAC market, its diverse applications, and the critical socio-economic barriers to adoption, particularly in developing countries. A comparative analysis of DAC within the broader carbon removal landscape (e.g., CCS, BECCS, afforestation) is also provided, alongside an address to the essential, often overlooked, environmental considerations for the sustainable production, regeneration, and disposal of spent nanomaterials, including insights from Life Cycle Assessments. The nuanced techno-economic landscape has been thoroughly summarized, highlighting that commercial viability is a multi-faceted challenge involving material performance, synthesis cost, regeneration energy, scalability, and long-term stability. It has been reiterated that no single ‘best’ material exists, but rather a portfolio of technologies will be necessary, with the ultimate success dependent on system-level integration and the availability of low-carbon energy. The review paper contributes to a holistic understanding of cutting-edge DAC technologies, bridging material science innovations with real-world implementation challenges and opportunities, thereby identifying critical knowledge gaps and pathways toward a net-zero carbon future. Full article

Sulfion oxidation reaction (SOR) has great potential in replacing oxygen evolution reaction (OER) and boosting highly efficient hydrogen evolution. The development of highly active and stable SOR electrocatalysts is crucial for assisting hydrogen production with low energy consumption. In this work, multiphase NiCoFe-based layered double hydroxide (namely NiCoFe-LDH) has been synthesized via a facile seed-assisted heterogeneous nucleation method. Benefiting from its unique microsized hydrangea-like structure and synergistic active phases, the catalyst delivers substantial catalytic interfaces and reactive centers for SOR. Consequently, NiCoFe-LDH electrode achieves a remarkably low potential of 0.381 V at 10 mA cm⁻² in 1 M KOH + 0.1 M Na₂S, representing a significant reduction of 0.98 V compared to conventional OER. Notably, under harsh industrial conditions (6 M KOH + 0.1 M Na₂S, 80 °C), the electrolysis system based on NiCoFe-LDH||NF pair exhibits a cell potential of only 0.71 V at 100 mA cm⁻², which shows a greater decreasing amplitude of 1.05 V compared with that of traditional OER/HER systems. Meanwhile, the NiCoFe-LDH||NF couple could maintain operational stability for 100 h without obvious potential fluctuation, as well as possessing a lower energy consumption of 1.42 kWh m⁻³ H₂. Multiphase eletrocatalysis for SOR could indeed produce hydrogen with low-energy consumption. Full article