Search Results (645)

Accelerated industrialization and surging energy demands have led to continuously rising atmospheric CO₂ concentrations. Developing sustainable methods to reduce atmospheric CO₂ levels is crucial for achieving carbon neutrality. Concurrently, the rapid development of new energy vehicles has driven a significant increase in demand for lithium-ion batteries (LIBs), which are now approaching an end-of-life peak. Efficient recycling of valuable metals from spent LIBs represents a critical challenge. This study employs conventional hydrometallurgical processing to recover valuable metals from spent LIBs. Subsequently, Ni-doped Co₃O₄ (Ni:Co₃O₄) supported on the natural mineral attapulgite (ATP) was synthesized via a sol–gel method. The incorporation of a small amount of Ni into the Co₃O₄ lattice generates oxygen vacancies, inducing a localized surface plasmon resonance (LSPR) effect, which significantly enhances charge carrier transport and separation efficiency. During the photocatalytic reduction of CO₂, the primary product CO generated by the Ni:Co₃O₄/ATP composite achieved a high production rate of 30.1 μmol·g⁻¹·h⁻¹. Furthermore, the composite maintains robust catalytic activity even after five consecutive reaction cycles. Full article

A triphenylphosphine-functionalized silica gel material, optimized for lead adsorption, was synthesized via a one-pot sol–gel reaction and characterized using FTIR and solid-state ¹³C and ²⁹Si NMR and XPS spectroscopy. The interaction between lead cations and phosphine groups was evaluated using the ³¹P NMR chemical shift tensor as a sensor. Two distinct types of phosphine groups, exhibiting different rotational mobility behaviors, were identified, with their ratio influenced by the presence of lead cations. These results suggest that the adsorption behavior of lead on this functionalized silica gel adsorbent can be directly evaluated by its lead–phosphorus interaction. This association was corroborated by the shifting of the binding energies of phosphorus functional groups after lead uptake in the XPS analysis. Full article

The interest in macromolecular alkoxysilyl-functionalized hybrids (self-assembling or nanostructured), which could be used as precursors in biomimetic silica precipitation and for the synthesis of hollow spherical silica particles, is growing. Nevertheless, reports on all-organosilicon systems for bioinspired silica precipitation are scarce. Therefore, a new kind of polyalkoxysilane macromonomer–linear polysilsesquioxane (LPSQ) of ladder-like backbone, functionalized in side chains with trimethoxysilyl groups (LPSQ-R-Si(OMe)₃), was designed following this approach. It was obtained by photoinitiated thiol-ene addition of 3-mercaptopropyltrimethoxysilane to the vinyl-functionalized polysilsesquioxane precursor, carried out in situ in tetraethoxysilane (TEOS). The mixture of LPSQ-R-Si(OMe)₃ and TEOS (co-monomers) was used in a sol–gel process conducted under acidic conditions (0.5 M HCl/NaCl) in the presence of Pluronic^® F-127 triblock copolymer as a template. LPSQ-R-Si(OMe)₃ played a key role for the formation of microparticles of a spherical shape that were formed under the applied conditions, while their size (as low as 3–4 µm) was controlled by the stirring rate. The hybrid materials were hydrophobic and showed good thermal and oxidative stability. Introduction of zinc acetate (Zn(OAc)₂) as an additive in the sol–gel process influenced the pH of the reaction medium, which resulted in structural reinforcement of the hybrid microparticles owing to more effective condensation of silanol groups and a relative increase of the content of SiO₂. The proposed method shows directions in designing the properties of hybrid materials and can be translated to other silicon–organic polymers and oligomers that could be used to produce hollow silica particles. The established role of various factors (macromonomer structure, pH, and stirring rate) allows for the modulation of particle morphology. Full article

The conversion of CO₂ into CH₄ through the Sabatier reaction is one of the key processes that can reduce CO₂ emissions into the atmosphere. This work aims to develop Ni-Al aerogel-based thermo-photocatalysts with large specific surface areas prepared using a sol–gel method and subsequent supercritical drying in CO₂. Different Al/Ni molar ratios were selected for the development of the catalysts, characterized using ICP-OES, N₂ adsorption–desorption isotherms, XRD, H₂-TPR, TEM, UV-Vis DRS, and XPS techniques. Thermo-photocatalytic activity tests were performed in a photoreactor with two different light sources (λ = 365 nm, λ = 470 nm) at a temperature range from 300 °C to 450 °C and a pressure of 10 bar. The catalyst with the highest Ni loading (AG 1/3) produced the best catalytic results, reaching CO₂ conversion and CH₄ selectivity levels of 82% and 100%, respectively, under visible light at 450 °C. In contrast, the catalysts with the lowest nickel loading produced the lowest results, most likely due to their low amounts of active Ni. These results suggest that supercritical drying is an efficient method for developing active thermo-photocatalysts with high Ni dispersion, suitable for Sabatier reactions under mild reaction conditions. Full article

Thermosensitive hydrogels undergo reversible sol-gel phase transitions in response to changes in temperature. Owing to their excellent biocompatibility, mild reaction conditions, and controllable gelation properties, these hydrogels represent a promising class of biomaterials suitable for minimally invasive treatment systems in diverse biomedical applications. This review systematically summarizes the gelation mechanisms of thermosensitive hydrogels and optimization strategies to enhance their performance for broader application requirements. In particular, we highlight recent advances in injectable thermosensitive hydrogels as a carrier within stem cells, bioactive substances, and drug delivery for treating various tissue defects and diseases involving bone, cartilage, and other tissues. Furthermore, we propose challenges and directions for the future development of thermosensitive hydrogels. These insights provide new ideas for researchers to explore novel thermosensitive hydrogels for tissue repair and disease treatment. Full article

Polyethersulfone (PES) membranes are essential in separation processes; however, their inherent hydrophobicity can limit their effectiveness in water-intensive applications. This study aims to enhance PES membranes by modifying them with a NiFe₂O₄–nanoclay composite nanoparticle to improve both their hydrophilicity and photocatalytic potential as a photocatalytic membrane. The nanoparticles were synthesized using the sol–gel auto-combustion method and incorporated into PES membranes through mixed-matrix embedding (1 wt% and 3 wt%) and surface coating. X-ray diffraction confirmed the cubic spinel structure of the composite nanoparticles, which followed the second order kinetic reaction during the photodegradation–adsorption of crystal violet. The mixed-matrix membranes displayed a remarkable 170% increase in water flux and a 25% improvement in mechanical strength, accompanied by a slight decrease in contact angle at 1 wt% of nanoparticle loading. In contrast, the surface-coated membranes demonstrated a significant reduction in contact angle to 18°, indicating a highly hydrophilic surface and increased roughness. All membranes achieved high dye removal rates of 98–99%, but only the coated membrane system exhibited approximately 50% photocatalytic degradation, following mixed kinetics. These results highlight the critical importance of surface modification in advancing PES membranes, as it significantly reduces fouling and enhances water–material interaction qualities essential for future filtration and photocatalytic applications. Exploring hybrid strategies that combine both embedding and coating approaches may yield even greater synergies in membrane functionality. Full article

There is currently an effort to scale up sol–gel nanomaterials without compromising quality, and microwave heating can pave the way for this due to its heating efficiency, resulting in a fast and homogeneous process. In this work, the sol–gel synthesis of transition metal aerogels, specifically iron-based aerogels, is studied using a microwave-assisted sol–gel methodology in an open-system multimode device as a potential route to scale-up production. Different approaches were tested to evaluate the best way to increase yield per batch, with different vessel shapes and volumes. It is shown that the shape and size of the vessel can be determinant in the interaction with microwaves and, thus, in the heating process, influencing the sol–gel reactions and the characteristics and homogeneity of the obtained nanomaterials. It has been found that a wide vessel is preferable to a tall and narrow one since the heating process is more homogeneous in the former and the sol–gel and cross-linking reactions take place earlier, which improves the mechanical properties of the final nanomaterial. For mass production of nanomaterials, the interaction of the reagents with the microwave field must be considered, and this depends not only on their nature but also on their volume, shape, and arrangement inside the cavity. Full article

The sol–gel synthesis of titanium dioxide (TiO₂) nanostructures is investigated in the present work in order to optimize synthesis parameters and enhance the optical properties and cost-effectiveness of the obtained materials. TiO₂ is widely used in photocatalysis, photovoltaics, and environmental applications due to its high stability, tunable band gap, and strong light absorption. The sol–gel method offers a scalable, cost-effective route for producing nanostructured TiO₂, although the precise control over particle morphology remains challenging. For this reason, in the present work, a statistical design of experiments (DOE) approach is employed to systematically refine reaction conditions through the manipulation of precursor concentrations, solvent ratios, and reaction volume. The experimental results obtained indicate that acetic acid is a key catalyst and stabilizing agent, significantly improving nucleation control and particle formation. Moreover, it is also shown that solvent dilution, particularly with acetic acid, leads to the formation of TiO₂ nanorods with enhanced optical properties. Additionally, scanning electron micrographs revealed that controlled synthesis conditions can reduce the particle size distribution and improve structural uniformity. Moreover, X-ray diffraction analyses confirmed the formation of a pure anatase crystalline phase, while ultraviolet–visible spectroscopy analyses indicated the existence of an optimal band gap for photocatalytic applications. Finally, the cost analysis showed that acetic acid-assisted synthesis can reduce production costs and simultaneously maintain high optical properties. Therefore, the present study highlights that proper manipulation and control of reaction conditions during sol–gel syntheses can allow the manufacture of high-performance TiO₂ nanomaterials for advanced technological applications, also providing a foundation for the development of cost-effective materials. Full article

Nanostructured bimetallic IrSn composites deposited on the natural aluminosilicate montmorillonite were synthesized and evaluated as anode electrocatalysts for polymer electrolyte membrane electrolysis cells (PEMECs). The test series prepared via the sol–gel method consisted of samples with 30 wt. % total metal content and varying Ir:Sn ratio. The performed X-ray diffraction analysis and high-resolution transmission electron icroscopy registered very fine nanostructure of the composites with metal particles size of 2–3 nm homogeneously dispersed on the support surface and also intercalated in the basal space of its layered structure. The electrochemical behavior was investigated by cyclic voltammetry and steady-state polarization techniques. The initial screening was performed in 0.5 M H₂SO₄. Then, the catalysts were integrated as anodes in membrane electrode assemblies (MEAs) and tested in a custom-made PEMEC. The electrochemical tests revealed that the catalysts with Ir:Sn ratio 15:15 and 18:12 wt. % demonstrated high efficiency toward the oxygen evolution reaction during repetitive potential cycling and sustainable performance with current density in the range 140–120 mA cm⁻² at 1.6 V vs. RHE during long-term stability tests. The results obtained give credence to the studied IrSn/MMT nanocomposites to be considered promising, cost-efficient catalysts for the oxygen evolution reaction (OER). Full article

To develop eco-friendly low-temperature NH₃-SCR catalysts for the non-electric industry, a series of CeMn-modified Ba₂Ti₅O₁₂ catalysts were synthesized using the sol-gel method to achieve denitrification. Activity tests revealed that Ce-Mn-modified Ba₂Ti₅O₁₂ catalysts exhibit excellent low-temperature denitrification performance with a broad operational temperature window. Characterization through XRD, XPS, BET, NH₃-TPD, and EPR indicated that Ce-Mn modification enhances surface oxygen chemisorption and increases acidity, significantly improving NO_x reduction. Notably, the optimal catalyst achieved NO_x conversion rates exceeding 90% within the temperature range of 90 to 240 °C under a gas hourly space velocity (GHSV) of 28,000 h⁻¹. In particular, the coexistence of Ce and Mn species promotes the oxidation of NO to NO₂, facilitating the “fast SCR” reaction. The abundance of valence states further enhances the catalyst’s ultra-low-temperature NH₃-SCR denitration performance. Full article

In this study, platinum (Pt) nanocatalysts were synthesized via a sol-gel method over the non-stoichiometric, Magnéli phase titanium oxides (TinO_2n−1) at varying Pt loadings (10–40 wt.%). Their structural and morphological properties were characterized, and after preliminary electrochemical screening, the catalysts were integrated into commercially available gas diffusion electrodes (GDEs) with a three-layer structure to enhance mass transport and catalyst utilization. Membrane electrode assemblies (MEAs) were fabricated using a Nafion^® 117 polymer membrane and tested in a laboratory PEM cell under controlled conditions. The electrochemical activity toward the hydrogen reduction reaction (HRR) was evaluated at room temperature and at elevated temperatures to determine the catalytic efficiency and stability. The optimal Pt loading was determined to be 30 wt.%, achieving a current density of approximately 0.12 A cm⁻² at 0.25 V, demonstrating a balance between catalyst efficiency and material utilization. The chronoamperometry tests showed minimal degradation over prolonged operation, suggesting that the catalysts were durable. These findings highlight the potential of Pt-based catalysts supported on Magnéli phase titanium oxides (TinO_2n−1) for efficient HRRs in electrochemical hydrogen pumps/compressors, offering a promising approach for improving hydrogen compression efficiency and advancing sustainable energy technologies. Full article

Combining the properties of organic and inorganic components with high surface areas and large pore volumes opens up countless possibilities for designing materials tailored to a wide range of advanced applications. As the majority of mesoporous hybrid materials are siliceous, the development of cost-effective synthetic approaches to produce water-stable hybrids with controlled porosity and functionality remains essential. Herein, we describe an original strategy for the synthesis of bridged mesoporous titania–bisphosphonate hybrids based on a one-step, template-free, non-hydrolytic sol–gel process. The reaction between Ti(OiPr)₄ and several flexible or rigid bisphosphonate esters, in the presence of acetic anhydride (Ac₂O) leads to the formation of TiO₂ anatase nanorods interconnected by fully condensed bisphosphonate groups. The general method that we depict is quantitative and low cost. All materials are mesoporous with very high specific surface areas (up to 520 m²·g⁻¹) and pore volumes (up to 0.93 cm³·g⁻¹). Full article

This work studies the effect of mesostructured silica–zirconia–tungstophosphoric acid (SiO₂-ZrO₂-TPA) composites used as catalysts in the synthesis of nifedipine by the Hantzsch methodology. The selectivity for nifedipine is determined, along with that of secondary products that may form depending on the reaction conditions. The materials were synthesized via the sol–gel method and characterized by N₂ adsorption–desorption isotherms, infrared spectroscopy (FT-IR), ³¹P solid-state nuclear magnetic resonance (NMR-MAS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), X-ray photoelectron spectra (XPS), and potentiometric titration. The characterization results from the XPS spectra showed that as the Si/Zr ratio drops, the Si-O-Si signal size decreases, while the Zr-O signal size increases. Characterization by titration indicated that an increase in the total acidity of the material, resulting from support modification with tungstophosphoric acid (H₃PW₁₂O₄₀, TPA), enhances the reaction yield. The catalytic activity in the solvent-free Hantzsch reaction was evaluated under thermal heating and microwave irradiation. The experiments conducted at 80 °C achieved a maximum yield of 57% after 4 h of reaction using the Si20Zr80TPA30 catalyst (50 mg), while by microwave heating, the yield significantly improved, reaching 77% in only 1 h of reaction. This catalyst exhibited stability and reusability without significant loss of activity up to the third cycle. Depending on the type of material and the reaction conditions, it is possible to modify the selectivity of the reaction, obtaining a 1,2-dihydropyridine isomeric to nifedipine. Reaction intermediates and other minor secondary products that may be formed in the process were also evaluated. Full article

NASICON-type titanium and zirconium phosphates doped with rare-earth cations, A_0.33M₂(PO₄)₃ (M = Ti, Zr; A = Dy, Y, Yb), were synthesized using the sol–gel method and investigated as catalysts for ethanol dehydration at 300–400 °C. The catalysts were characterized via XRD, SEM, BET, and FTIR spectroscopy. The relationships between the catalyst composition, acidity and the dehydration activity were evaluated. Diethyl ether (DEE) formation is promoted by the presence of the zirconium phosphates (ZrP), while the presence of titanium phosphate (TiP) catalyzes the formation of both ethylene and diethyl ether (DEE). The application of Fourier-transform infrared (FTIR) spectroscopy to the analysis of adsorbed C₆H₆ has revealed the presence of hydroxyl groups exhibiting varying degrees of proton-donating mobility. This finding has enabled the correlation of the structure of the active sites with the process’s selectivity. The results underscore the key function of OH-group localization and framework geometry in the control of form-selective reactions. Full article

Recently, aquatic life and human health are seriously threatened by the release of pharmaceutical drugs. For a sustainable ecosystem, emerging contaminants like antibiotics must be removed from drinking water and wastewater. To address this issue pure and cerium-doped titanium dioxide (CeT) nanoparticles were produced with stable tetragonal (anatase) lattices by room temperature sol–gel method and employing the inorganic titanium oxysulfate (TiOSO₄) as titanium precursor. The structural analysis by X-ray diffraction (XRD) revealed that at calcination temperature of 600 °C all (un and doped) powders were composed of crystalline anatase TiO₂ with the crystallite sizes in the range of 13.5–11.3 nm. UV–vis DRS spectroscopy revealed that the most narrowed bandgap value of 2.75 eV was calculated for the 0.5CeT sample containing the optimum dopant content of 0.5 weight ratio. X-ray spectroscopy (XPS) confirmed the presence of the impurity level Ce³⁺/Ce⁴⁺, which became responsible for the decrease in bandgap as well as for the photoinduced carriers recombination rate. Photocatalytic tests showed that the maximum decomposition of the model spiramycin (SPR) antibiotic pollutant was 88.0% and 77.0%, under UV and visible light, respectively. According to the reaction kinetics, SPR decomposition adhered to the Langmuir–Hinshelwood (L–H) model and via ROS experiments mainly hydroxyl radicals (OH^•) followed by photogenerated holes (h⁺s) become responsible for the pollutant degradation. In summary, this study elaborates on the role of xCeT nanoparticles as an efficient photocatalyst for the elimination of organic contaminants in wastewater. Full article