Search Results (658)

Molecular-mimetic nanocolloids (MMNCs) are promising for advanced materials, yet self-assembly fabrication faces challenges in purity and programmability. We report a total synthesis strategy for surfactant-mimetic nanocolloids (SMNCs), an amphiphilic MMNC subclass. SMNCs consist of a ~5 nm silica nanoparticle head and a bottlebrush polymer tail. Regioselective silica deposition on linear-block-brush polymers via the modified sol–gel method enables precise control. This strategy is versatile and can be adapted to synthesize other MMNCs with different components. It offers a more controlled alternative to self-assembly methods, advancing MMNC synthesis and enabling their broader use in emerging technologies. Full article

Poly(trimethylene terephthalate) (PTT) is a thermoplastic polyester with a unique structure due to having three methylene groups in the glycol unit. PTT competes with poly(ethylene terephthalate) (PET) and poly(butylene terephthalate) (PBT) in carpets, textiles, and thermoplastic materials, primarily due to the development of economically efficient synthesis methods. PTT is widely utilized in textiles, carpets, and engineering plastics because of its advantageous properties, including quick-drying capabilities and wrinkle resistance. However, its low melting point, resistance to chemicals, and brittleness compared to PET, have limited its applications. To address some of these limitations for targeted applications, PTT nanocomposites incorporating clay, carbon nanotube, silica, and ZnO have been developed. The distribution of nanoparticles within the PTT matrix remains a significant challenge for its potential applications. Several techniques, including sol–gel blending, melt blending, in situ polymerization, and in situ forming methods have been developed to obtain better dispersion. This review discusses advancements in the synthesis of various PTT nanocomposites and the effects of nanoparticles on the isothermal and nonisothermal crystallization of PTT. Full article

Silica-modified electrodes possess physicochemical properties that make them valuable in electrochemical sensing and energy-related applications. Although intrinsically insulating, silica thin films can selectively interact with redox species, producing sieving effects that enhance electrochemical responses. We synthesized Class I hybrid silica matrices incorporating either negatively charged poly(4-styrene sulfonic acid) or positively charged poly(diallyl dimethylammonium chloride). These hybrid films were deposited onto ITO electrodes and evaluated via cyclic voltammetry in aqueous ferrocenium solutions. The polyelectrolyte charge played a key role in the electroassisted incorporation of ferrocene: silica-PSS films promoted accumulation, while silica-PDADMAC films hindered it due to electrostatic repulsion. In situ UV-vis spectroscopy confirmed that only a fraction of the embedded ferrocene was electroactive. Nevertheless, this fraction enabled effective mediated detection of cytochrome c in solution. These findings highlight the crucial role of ionic interactions and hybrid composition in electron transfer to redox proteins, providing valuable insights for the development of advanced bioelectronic sensors. Full article

To address critical technical challenges in coalbed methane fracturing, including the uncontrollable release rate of conventional breaker agents and incomplete gel breaking, this study designs and fabricates an intelligent controlled-release breaker system based on paraffin-coated mesoporous silica nanoparticle carriers. Three types of mesoporous silica (MSN) carriers with distinct pore sizes are synthesized via the sol-gel method using CTAB, P123, and F127 as structure-directing agents, respectively. Following hydrophobic modification with octyltriethoxysilane, n-butanol breaker agents are loaded into the carriers, and a temperature-responsive controlled-release system is constructed via paraffin coating technology. The pore size distribution was analyzed by the BJH model, confirming that the average pore diameters of CTAB-MSNs, P123-MSNs, and F127-MSNs were 5.18 nm, 6.36 nm, and 6.40 nm, respectively. The BET specific surface areas were 686.08, 853.17, and 946.89 m²/g, exhibiting an increasing trend with the increase in pore size. Drug-loading performance studies reveal that at the optimal loading concentration of 30 mg/mL, the loading efficiencies of n-butanol on the three carriers reach 28.6%, 35.2%, and 38.9%, respectively. The release behavior study under simulated reservoir temperature conditions (85 °C) reveals that the paraffin-coated system exhibits a distinct three-stage release pattern: a lag phase (0–1 h) caused by paraffin encapsulation, a rapid release phase (1–8 h) induced by high-temperature concentration diffusion, and a sustained release phase (8–30 h) attributed to nano-mesoporous characteristics. This intelligent controlled-release breaker demonstrates excellent temporal compatibility with coalbed methane fracturing processes, providing a novel technical solution for the efficient and clean development of coalbed methane. 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

Silica/alumina composite particles were synthesized via the sol–gel method to promote fine dispersion and homogenous mixing. Aluminum chloride hydroxide served as the alumina precursor, while amorphous silica, obtained from rice husk, was directly incorporated into the alumina sol. Following synthesis, the material was calcined at 1000 °C, yielding an α-cristobalite form of silica and corundum-phase alumina. These hybrid particles were introduced into polymer composites at reinforcement levels of 1 wt.%, 3 wt.%, and 5 wt.%. Mechanical behavior was evaluated through three-point bending tests, Shore D hardness measurements, and controlled-energy impact testing. Among the formulations, the 3 wt.% composite exhibited optimal performance, displaying the highest flexural modulus and strength, along with enhanced impact resistance. Hardness increased with rising particle content. Fractographic analysis revealed that the 3 wt.% loading produced a notably rougher fracture surface, correlating with improved energy absorption. In contrast, the 5 wt.% composite, although harder than the matrix and other composites, exhibited diminished toughness due to particle agglomeration. Full article

Moroccan oil shale ash (MOSA) represents an underutilized industrial by-product, particularly in the Rif region, where its high mineral content has often led to its neglect in value-added applications. This study highlights the successful conversion of MOSA into amorphous mesoporous silica (AS-Si) using a sol–gel process assisted by polyethylene glycol (PEG-6000) as a soft template. The resulting AS-Si material was extensively characterized to confirm its potential for environmental remediation. FTIR analysis revealed characteristic vibrational bands corresponding to Si–OH and Si–O–Si bonds, while XRD confirmed its amorphous nature with a broad diffraction peak at 2θ ≈ 22.5°. SEM imaging revealed a highly porous, sponge-like morphology composed of aggregated nanoscale particles, consistent with the nitrogen adsorption–desorption isotherm. The material exhibited a specific surface area of 68 m²/g, a maximum in the pore size distribution at a pore diameter of 2.4 nm, and a cumulative pore volume of 0.11 cm³/g for pores up to 78 nm. DLS analysis indicated an average hydrodynamic diameter of 779 nm with moderate polydispersity (PDI = 0.48), while a zeta potential of –34.10 mV confirmed good colloidal stability. Furthermore, thermogravimetric analysis (TGA) and DSC suggested the thermal stability of our amorphous silica. The adsorption performance of AS-Si was evaluated using methylene blue (MB) and ciprofloxacin (Cipro) as model pollutants. Kinetic data were best fitted by the pseudo-second-order model, while isotherm studies favored the Langmuir model, suggesting monolayer adsorption. AS-Si could be used four times for the removal of MB and Cipro. These results collectively demonstrate that AS-Si is a promising, low-cost, and sustainable adsorbent derived from Moroccan oil shale ash for the effective removal of organic contaminants from aqueous media. 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 aim of the present research was to synthesize protective composite layers from biodegradable cellulose and biocompatible, sol–gel-derived silica cryogel. An important task in the present work was to achieve good applicability on distinct (smooth and rough) surfaces of various materials (from metallic to ceramic). The aim was to utilize the composite layers as thermal and electric insulation coating. The investigation put some effort into the enhancement of mechanical strength and the elasticity of the thin layer as well as a reduction in its water solubility. The removal of the alkali content leads successfully to a significant reduction in water solubility (97 wt% → 1–3 wt%). Adhesion properties were measured using a specialized measurement technique developed in our laboratory. Treatments of the substrate surface, such as alkaline or acidic etching (i.e., Na₂CO₃, HF, water glass), mechanical roughening, or the application of a thin alkali-containing primer layer, strongly increase adhesion. SEM analyses revealed the interactions between the matrix and the reinforcement phase and their morphology. Full article

Background/Objectives: Mesoporous silica materials, particularly KIT-6, offer promising features, such as large surface area, tunable pore structures, and biocompatibility, making them ideal candidates for advanced drug delivery systems. The aims of this study were to develop and evaluate an innovative modified-release platform for metformin hydrochloride (MTF), using KIT-6 mesoporous silica as a matrix, to enhance oral antidiabetic therapy. Methods: KIT-6 was synthesized using an ultrasound-assisted sol-gel method and subsequently loaded with MTF via adsorption from alkaline aqueous solutions at two concentrations (1 and 3 mg/mL). The structural and morphological characteristics of the matrices—before and after drug loading—were assessed using SEM-EDX, TEM, and nitrogen adsorption–desorption isotherms (the BET method). In vitro drug release profiles were recorded in simulated gastric and intestinal fluids over 12 h. Kinetic modeling was performed using seven classical models, and a multifractal theoretical framework was used to further interpret the complex release behavior. Results: The loading efficiency increased with increasing drug concentration but nonlinearly, reaching 56.43 mg/g for 1 mg/mL and 131.69 mg/g for 3 mg/mL. BET analysis confirmed significant reductions in the surface area and pore volume upon MTF incorporation. In vitro dissolution showed a biphasic release: a fast initial phase in an acidic medium followed by sustained release at a neutral pH. The Korsmeyer–Peppas and Weibull models best described the release profiles, indicating a predominantly diffusion-controlled mechanism. The multifractal model supported the experimental findings, capturing nonlinear dynamics, memory effects, and soliton-like transport behavior across resolution scales. Conclusions: The study confirms the potential of KIT-6 as a reliable and efficient carrier for the modified oral delivery of metformin. The combination of experimental and multifractal modeling provides a deeper understanding of drug release mechanisms in mesoporous systems and offers a predictive tool for future drug delivery design. This integrated approach can be extended to other active pharmaceutical ingredients with complex release requirements. Full article

Background: The present work is devoted to the biological effects of sol–gel-derived silica (Si)–copper (Cu) nanomaterials. Methods and Results: Tetraethyl orthosilane (TEOS) was used as a silica precursor; copper was introduced as a solution in ethanol with Cu(OH)₂. The obtained samples were denoted as Si/Cu (gel) and Si/Cu/500 (500 °C heat-treated). Their phase formation and morphology were studied by XRD and SEM. The antibacterial activity was tested by two Gram-positive bacteria, three Gram-negative bacteria, and two types of eukaryotic species. Most bacteria were more sensitive to Si/Cu/500 materials than to Si/Cu (gel). The yeasts were more sensitive to Si/Cu (gel). The new nanomaterials were tested for oxidant activity at pH 7.4 (physiological) and pH 8.5 (optimal) in three model systems by the chemiluminescent method. They significantly inhibited the generation of free radicals and ROS. This result underlines their potential as regulators of the free radical processes in living systems. The epithelial tumor cell lines appeared more sensitive than the non-transformed fibroblasts, likely due to their metabolic activity and proliferation rates, leading to greater accumulation of the substances. Using Daphnia magna, the ecotoxicity study showed that the LC₅₀ was reached at 1 mg/L of Si/Cu/500. Si/Cu (gel) was more toxic. Conclusions: Our results reveal the potential of these nanohybrids to be applied in living, eukaryotic systems. The cytotoxicity evaluation showed higher tolerance of normal, non-transformed cells, in concurrence with the oxidation tests. Full article

A composite photocatalyst of ceria–cadmium supported on mesoporous SBA-15 silica was synthesized and employed for the aqueous methylene blue (MB) degradation. The composites were prepared using an incipient wetness impregnation technique and a conventional sol–gel approach with triblock copolymer P123 as a structure-directing agent for SBA-15 preparation, enabling the uniform dispersion of CeO₂ and Cd species within the SBA-15 framework. The physicochemical properties of both CeO₂/SBA-15 and Cd-CeO₂/SBA-15 composites were analyzed using small-angle and wide-angle XRD, FT-IR spectroscopy, SEM, TEM, EDX spectroscopy, N₂ physisorption at 77 K, and UV-Vis spectroscopy. The findings revealed that the SBA-15 support retained its well-ordered hexagonal mesostructure in both the ceria–SBA-15 and SBA-15-supported cadmium–ceria (Cd-CeO₂) composites. The highest degradation efficiency of 96.40% was achieved under optimal conditions, and kinetic analysis using the Langmuir–Hinshelwood model indicated that the MB degradation process followed pseudo-first-order kinetics, with a strong correlation coefficient (R² = 0.9925) and a rate constant (k) of 0.02532 min⁻¹. Under irradiation, the Cd-CeO₂/SBA-15 composites exhibited superior photocatalytic activity compared to the pristine components, owing to the synergistic interaction between ceria and cadmium, enhanced light absorption, and improved charge carrier separation. The recyclability test demonstrated that the degradation efficiency decreased slightly from 96.40% to 94.86% after three cycles, confirming the stability and reusability of Cd-CeO₂/SBA-15 composites. The photocatalytic process demonstrated a favorable electrical energy per order (EE/O) value of 281.8 kWh m⁻³, indicating promising energy efficiency for practical wastewater treatment. These results highlight the excellent photocatalytic performance and durability of the synthesized Cd-CeO₂/SBA-15 composites, making them promising candidates for facilitating the photocatalytic decomposition of MB and other dye molecules in water treatment applications. Full article

Aerogels have gained much interest in the last decades due to their specific properties, such as high porosity, high surface area, and low density, which have caused them to be used in multiple and varied fields. As the applicability of aerogels is tightly correlated to their morpho-structural features, special consideration must be allocated to the fabrication method. An emerging technique for producing nanostructured materials with tailored morphology and dimensions is represented by continuous-flow microfluidics. In this context, this work explores the synergic combination of aerogel-based materials with microfluidic synthesis platforms to generate advanced nanocomposite adsorbents for water decontamination. Specifically, this study presents the novel synthesis of a magnetic silica-based aerogel using a custom-designed 3D microfluidic platform, offering enhanced control over nanoparticle incorporation and gelation compared to conventional sol–gel techniques. The resulting gel was further dried via supercritical CO₂ extraction to preserve its unique nanostructure. The multi-faceted physicochemical investigations (XRD, DLS, FT-IR, RAMAN, SEM, and TEM) confirmed the material’s uniform morphology, high porosity, and surface functionalization. The HR-MS FT-ICR analysis has also demonstrated the advanced material’s adsorption capacity for various pesticides, suggesting its adequacy for further environmental applications. An exceptional 93.7% extraction efficiency was registered for triazophos, underscoring the potential of microfluidic synthesis approaches in engineering advanced, eco-friendly adsorbent materials for water decontamination of relevant organic pollutants. Full article

Despite their high porosity and wide applicability, silica xerogels face mechanical strength limitations for high-performance applications. This study presents an ambient-pressure sol-gel strategy utilizing calcium-glycerol synergy to produce robust xerogels with enhanced properties. Physicochemical analyses reveal that controlled Ca²⁺ incorporation (optimal at 6 wt.%) accelerates gelation kinetics while establishing a hybrid network through ionic complexation and hydrogen bonding. The resulting xerogels achieve exceptional compressive strength (30.8 MPa) while maintaining uniform mesoporosity (50–90 nm pore size). Remarkably, the as-prepared silica xerogels demonstrate outstanding thermal insulation, maintaining a 220 °C temperature differential in 300 °C environments. These results prove that the ambient-pressure sol-gel strategy utilizing calcium-glycerol synergy can enhance the mechanical performance and thermal insulation performance of silica xerogels with the dual actions of Ca²⁺-induced network reinforcement via silanol coordination and glycerol-mediated stress relief during ambient drying. Overall, this work can offer a scalable, energy-efficient approach to produce high-performance silica xerogels with huge potential in building envelopes and aerospace systems. Full article

Porous silica gel powders, doped with gold nanoparticles (AuNPs), were obtained by heating silica gels containing 1-dodecanethiol and tetrachloroauric acid at temperatures of 450 °C, 700 °C and 900 °C, and characterized using X-ray diffraction, TEM/EDS studies, UV/Vis reflectance spectroscopy and DTA/TG investigations. The color and microstructure of the obtained samples with a composition SiO₂:AuNPs (about 0.03% Au) depend on the heating temperature. The UV/Vis reflection spectra of the samples are explained using Mie’s theory. The thermal stability of the obtained samples, as well as the processes occurring in the sol–gel matrix upon heating, were monitored by DTA/TG. The textural properties of the obtained materials were described based on adsorption–desorption isotherms. The obtained nanocomposites are promising pigments for ceramic glazes, similar to the Purple of Cassius. The textural properties of certain samples, S_BET = 200–350 m²/g, a mean pore diameter (D_AV) of approximately 10 nm and a specific pore volume (V_t) between 0.5 and 0.8 cm³/g, make them promising candidates for catalytic applications, comparable to aerogel-like materials. Full article