Search Results (141)

The objective of this study was to develop a pectin–tetraethoxysilane (TEOS) hybrid gel with improved functional properties and biocompatibility. The sol–gel process was used to create pectin–TEOS hydrogels containing 0.75, 1.00, 1.25, and 1.50 M TEOS, which were labeled AP-T0.75, AP-T1.00, AP-T1.25, and AP-T1.50. The pectin–TEOS hydrogel AP-T1.50 exhibited a hardness of 631 kPa, a Young’s modulus of 1588 kPa, and an elasticity of 1.95 mm. The degree of swelling decreased as the TEOS content increased. The pectin–TEOS hydrogel AP-T1.25 exhibited the highest strength of adhesion to serosa of 60.6 mN. Serum protein and bovine serum albumin (BSA) adsorption by pectin–TEOS gels was recorded in the range of 2–43 µg/mg after 6 h of incubation at pH 5.0, 7.4, and 8.0. Pectin–TEOS gels demonstrated low rates of hemolysis and complement activation. Leukocyte adhesion on the surface of pectin–TEOS gels depends on TEOS content. Consequently, the mechanical characteristics, serosal adherence, and biocompatibility of pectin–TEOS gel position it as a strong contender for the advancement of smart biomaterials. Full article

This work describes the straightforward synthesis of a novel heterogeneous palladium catalyst immobilized on magnetic Janus-type silica particles coated with an amphiphilic ionic liquid (IL) layer. The material was prepared via a one-pot process wherein TEOS (tetraethoxysilane) and a bis(triethoxysilane) IL precursor are combined to form hollow shells. The IL motifs are selectively located on the outer surface of the hollow particles and serve as centers for the immobilization of palladium species on the material’s surface. The outer surface also hosts magnetic nanoparticles in close proximity to the palladium sites. Thanks to the uniform coverage of the surface with the amphiphilic IL functionality, the material exhibits a well-balanced wettability with reaction components of different polarities. The catalyst’s activity was tested in the Sonogashira cross-coupling reaction of terminal acetylenes and iodobenzene derivatives in water as the solvent. The results show that the mixed palladium–iron oxide catalyst exhibits higher activity than materials containing either immobilized palladium or iron oxide alone, suggesting a synergistic effect in this reaction. Additionally, the reaction proceeds well in the absence of expensive organic ligands and commonly employed additives such as copper co-catalysts or phase transfer catalysts. Furthermore, the material was also used in the oxidative Sonogashira coupling reaction of phenylboronic acid and phenylacetylene. The catalyst can be easily separated using an external magnet and can be reused several times. The feasibility of producing diphenylacetylene on a gram scale via the Sonogashira cross-coupling reaction was also investigated. Full article

Wood is one of the most widely used sustainable lignocellulosic materials, with numerous applications in consumer goods and the construction sector. Despite its positive properties, such as a high strength-to-weight ratio, thermal insulation, and low density, wood’s natural thermal degradation can limit its potential applications. In composite applications like wood–plastic composites, the particle morphology and surface topography must be preserved to support intimate polymer–wood contact and mechanical interlocking. This study investigated the efficacy of a thin silica coating for thermal protection, which was applied via an in situ sol–gel method using the precursor tetraethoxysilane (TEOS). The wood particles and treatments were characterized using particle size analysis, physisorption, FTIR, SEM, XRD, and TGA analyses. After treatment, the specific and microporous surface area of wood particles increased by 118% and 97%, respectively, an effect of the porosity of silica itself. FTIR spectra of the silica-treated wood displayed peaks corresponding to Si stretching, and SEM micrographs confirmed a successful silica coating formation. TGA showed that the silica coating increased the temperatures needed to degrade the underlying hemicellulose and cellulose by 16 °C for all treatment levels. This particle-scale coating provided a promising method for producing thermally protected, functionalizable wood fillers for composites that maintain the filler geometry and potential mechanical interlocking, offering an attractive upcycling pathway for wood residues. Full article

TiO₂ is the most used material for the photocatalytic removal of organic pollutants in aqueous media. TiO₂, specifically its anatase phase, is well-known for its great performance under UV irradiation, high chemical stability, low cost and non-toxicity. Nevertheless, TiO₂ presents two main drawbacks: its limited absorption of the visible spectrum; and its relatively low specific surface area and pore volume. Regarding the latter, several works in the literature have addressed the issue by developing new synthesis approaches in which anatase is dispersed and supported on the surface of porous materials. In the present work, two series of materials have been prepared where anatase has been supported on mesoporous silica (MSTiR%) in situ through a hydrothermal synthesis approach, where, in addition to using tetraethoxysilane (TEOS) as a silicon precursor, three organotriethoxysilanes [RTEOS, where R = methyl (M), propyl (P) or phenyl (Ph)] were used at a RTEOS:TEOS molar percentage of 10 and 30%. The materials were thoroughly characterized by several techniques to determine their morphological, textural, chemical, and UV-vis light absorption properties and then the most promising materials were used as photocatalysts in the photodegradation of the emerging contaminant and antiepileptic carbamazepine (CBZ) under UV irradiation. The materials synthesized using 10% molar percentage of RTEOS (MSTiR10) were able to almost completely degrade (~95%), 1 mg L⁻¹ of CBZ after 1 h of irradiation using a 275 nm LED and 0.5 g L⁻¹ of catalyst dose. Therefore, this new synthesis approach has proven useful to develop photoactive TiO₂ composites with enhanced textural properties. Full article

Colloidal quantum dots (QDs) are semiconductor crystals a few nanometers in size. Due to their vibrant colors and unique photoluminescence (PL), QDs are widely utilized in displays, where barrier films provide essential shielding. However, one of the primary challenges of QD applications remains achieving sufficient robustness while keeping costs low. Over the past two decades, significant progress has been made in the encapsulation of QDs within silica matrices, aiming to preserve their original PL properties. Research efforts have evolved from bulk forms to thin films. Silica nanoparticles containing multiple embedded QDs have emerged as particularly promising candidates for practical applications. This review highlights recent advancements in silica-based QD encapsulation, incorporating findings from both the authors’ investigations and those of other research groups within the field. Silica glass possesses inherent shielding capabilities, but silane coupling agents such as (3-aminopropyl)trimethoxysilane and (3-mercaptopropyl)trimethoxysilane tend to negatively impact this functionality when they are used alone, partly because of the limited formation of a well-developed glass network structure. However, when judiciously controlled, they can serve as mediators between the QD surface and the surrounding pure silica glass matrix, helping to preserve PL properties and control the morphology of silica particles. This review discusses the potential for achieving exceptional shielding properties through sol–gel glass fabrication at low temperatures, utilizing both tetraethoxysilane and other silane coupling agents. 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 global market for flame-retardant materials is expected to grow steadily, from USD 7.0 billion in 2022 to USD 16.6 billion in 2030, driven by increasing demand for environment-friendly fire safety solutions in transportation, construction, and electronics. Polylactic acid (PLA), a biodegradable polymer which possesses excellent mechanical properties, is increasingly being considered for future mobility applications. However, it is characterized by high heat release and toxic smoke during combustion, which are significant drawbacks. In order to address this, the chemical modification of Kraft lignin was achieved through a phenolation and subsequent silylation with tetraethoxysilane, aiming to mitigate the degradation of PLA’s mechanical properties while utilizing its inherent char-forming ability. The modified lignins were combined with ammonium polyphosphate (APP) and melt-mixed with PLA using an injection-mixing molder to prepare test specimens. Analysis by FT-IR, NMR spectroscopy, and SEM-EDS confirmed successful grafting of phenolic and silane functionalities, and thermogravimetric analysis demonstrated enhanced thermal stability of the modified lignins compared to unmodified ones. Vertical burning tests and limiting oxygen index (LOI) measurements showed that the PLA/APP/SPKL composite material achieved a V-0 UL-94 rating and 31.95% LOI, demonstrating the highest level of flame retardancy. This compares to the LOI of neat PLA, 19 to 21%. Despite the enhancement in flame retardancy to the V-0 level, the decline in tensile strength was limited, and the composite retained comparable mechanical strength to PLA-APP composites with V-2 flame retardancy. The findings indicate that the combination of phenolation and silylation of lignin with APP, a flame-retardant material, offers a viable and sustainable methodology for the fabrication of PLA composites that exhibit both flame retardancy and mechanical strength. Full article

Acrylic resin composites with a high filler loading, consisting of a fluoride-containing hydrotalcite incorporated into silica nanoparticles, were prepared. The filler was obtained by a multi-step process. First, ZnAl hydrotalcite in fluoride form (HTlc/F) was functionalised with tetraethoxysilane to form Si-O-M bonds (M = Al or Zn) with the brucitic layers. The ethoxysilane groups exposed on the layers were used as nucleation seeds for silica nanoparticles. The composite, named SiO₂@HTlc/F, was then functionalised with 3-(trimethoxysilyl)-propyl methacrylate groups and used as a filler for acrylic resins. The methacrylate groups on the surface of the inorganic composite participated in the polymerisation process of the resin by minimising the phase separation between inorganic and polymer through the formation of chemical bonds at the polymer–inorganic interface. The filler in the resin increases the degree of polymerisation, bringing it to values very close to 100%. Finally, preliminary studies on the release of fluoride anions showed that they are released slowly over time. Full article

Maghemite (γ-Fe₂O₃) nanoparticles are widely used in biomedical, catalytic, and environmental applications owing to their superparamagnetic properties and surface tunability. Functionalization with primary amine groups via 3-aminopropyltriethoxysilane (APTES) is commonly employed to enable the covalent immobilization of biomolecules and other functional species. The efficiency of this silanization process depends significantly on the density of surface hydroxyl groups, which serve as reactive sites for silane coupling. In this study, the impact of acid and base pretreatments on the surface hydroxylation of γ-Fe₂O₃ nanoparticles and the subsequent APTES grafting performance was systematically evaluated. Intermediate modification using tetraethoxysilane (TEOS) was explored as a strategy to enhance silanization by forming a hydroxyl-rich silica interlayer. Fourier transform infrared spectroscopy and zeta-potential measurements were performed to assess surface chemistry and functional-group incorporation. The results indicate that acid pretreatment significantly increases the availability of reactive –OH groups, while TEOS-assisted silanization improves the uniformity and density of surface-bound amine groups. These findings highlight the critical role of surface conditioning and sequential modification in achieving the controlled and robust amine functionalization of iron oxide nanoparticles. The developed approach provides a foundation for the rational design of surface engineering protocols for high-performance magnetic nanomaterials. Full article

Hybrid silane-based coatings were developed via the sol–gel process using two precursors, vinyltrimethoxysilane (VTMS) and tetraethoxysilane (TEOS), and subsequently deposited onto three titanium-based substrates: commercially pure titanium Grade 2, Ti6Al4V, and Ti13Nb13Zr. Comprehensive physicochemical characterization was performed, including microstructural (optical and SEM), topographical (3D roughness), spectroscopic (FTIR), and electrochemical (potentiodynamic) analyses. The coatings were continuous, transparent, smooth, and exhibited high gloss with no visible cracks or surface defects. Surface roughness (Sa ≈ 0.3 μm) was consistent across all samples and remained unaffected by both the VTMS to TEOS ratio and the substrate type. Coating thickness ranged from 8 to 15 μm, as confirmed by both digital microscopy and thickness gauge measurements. All coatings demonstrated strong adhesion to the substrates. FTIR analysis confirmed the presence of key functional groups, such as CH₂, C=C, C–H, Si–O–Si, Si–OH, Si–O–Ti, CH=CH₂, and O–Si–O, regardless of the substrate type. Electrochemical tests in Ringer’s solution showed excellent corrosion resistance, particularly for coatings with a VTMS to TEOS ratio of 1:1. Post-corrosion imaging confirmed the integrity of the coatings and their effectiveness as protective barriers in simulated physiological environments. These findings support the potential of VTMS/TEOS sol–gel coating as a surface modification strategy for biomedical titanium implants. Full article

A sol-gel approach was used to prepare a thin hydrogel membrane based on an organic-inorganic polymer matrix embedded with pre-synthesized gold nanoparticles (AuNPs). The organic polymers utilized were poly(vinyl alcohol) (PVA) and poly(ethylene oxide) 400 (PEO) while tetraethoxysilane (TEOS) served as a precursor for the inorganic silica polymer. AuNPs were synthesized using D-glucose as a reducing agent and starch as a capping agent. A mixture of PVA, PEO, pre-hydrolyzed TEOS, and AuNP dispersions was cast and dried at 50 °C to obtain the hybrid hydrogel membrane. The structure, morphology, and optical properties of the nanocomposite membrane were analyzed using TEM, SEM, XRD, and UV-Vis spectroscopy. The newly designed hybrid hydrogel membrane was utilized as an efficient sorbent for the simultaneous speciation analysis of valence species of chromium and manganese in water samples via solid-phase extraction. This study revealed that Cr(III) and Mn(II) could be simultaneously adsorbed onto the PVA/PEO/SiO₂/AuNP membrane at pH 9 while Cr(VI) and Mn(VII) remained in solution due to their inability to bind under these conditions. Under optimized parameters, detection limits and relative standard deviations were determined for chromium and manganese species. The developed analytical method was successfully applied for the simultaneous speciation analysis of chromium and manganese in drinking water and wastewater samples. Full article

The aim of this research was to prepare pH sensor films based on litmus using the sol–gel method with tetraethoxysilane (TEOS) and phenyltrimethoxysilane (PTMS) as precursors. The pH sensor film was then applied to millireactors to evaluate its performance on the intricate geometries of static mixers commonly found in millireactor designs. Millireactors were made from Formlabs High Temp resin using stereolithography (SLA) and from Anycubic Basic resin using digital light processing (DLP) technology. The performance of the pH sensor films was evaluated by tracking color changes in the pH sensor films and analyzing RGB (red, green, blue) and hue values through a smartphone application. The experiment involved mixing solutions with different pH values at varying flow rates within the millireactor channels. Furthermore, along with analyzing the hue values, characterization techniques involved measuring contact angles with water and diiodomethane. A film combining a litmus indicator with titanium dioxide (TiO₂) displayed a color change within one minute and maintained this color throughout the study, confirming its reusability. Sensor films exhibited excellent reversibility (RSD = 2.4–3.3%) and stability. The findings demonstrate that the pH-sensitive films perform robustly across varying geometries, paving the way for their integration into advanced millireactor systems with static mixers and continuous chemical monitoring within Industry 4.0. Full article

This study investigates the synthesis and characterization of SiO₂-Gd₂O₃-Eu₂O₃ nanomaterials. The sol–gel method was employed using tetraethoxysilane (TEOS), gadolinium nitrate, and europium nitrate as precursors. The influence of rare earth oxide concentration on the hydrolysis kinetics and activation energy was evaluated. Additionally, the acid-base properties of the synthesized materials were examined using the Hammett indicator adsorption method. The results revealed that the addition of Gd₂O₃ and Eu₂O₃ oxides to the system accelerated the hydrolysis process and reduced the activation energy. The formation of a layered structure, consisting of a central Si(OH)₄ nucleus, a Si-O-Si polymer layer, and hydrated metal ion layers, was observed. The acid-base properties of the synthesized nanomaterials were influenced by the drying method and the composition of the system. The findings provide valuable insights into the synthesis and properties of SiO₂-Gd₂O₃-Eu₂O₃ nanomaterials, which have potential applications in various fields such as optoelectronics and catalysis. Full article

Silicon oxide (SiOx) coatings are attracting significant attention and are widely used in industrial applications. They can be prepared by plasma-assisted chemical vapor deposition (PACVD). PACVD at atmospheric pressure (AP-PACVD) is often employed to synthesize SiOx coatings, but it has generally not been scaled up to an industrially viable level. In the present work, a SiOx coating was continuously deposited onto a polyethylene terephthalate film using industrial-scale roll-to-roll type AP-PACVD. 1,1,3,3-Tetramethyldisiloxane (TMDSO) and tetraethoxysilane (TEOS) were selected as precursors. The elemental compositions and chemical structures of the SiOx coatings were characterized, and oxygen and water-vapor transmission rates were measured. The SiOx coating using TEOS exhibited better barrier properties than that using TMDSO, corresponding to the high oxygen content, high SiO₂ content, and high siloxane network content in the SiOx coating. Full article

Methylotrophic yeast Ogataea polymorpha BKM Y-2559 was immobilized in organosilicon sol–gel matrices using precursors isobutyltriethoxysilane (iBTES) and tetraethoxysilane (TEOS) to create an effective biocatalyst. The analytical and metrological performance of the biosensor permitted the determination of the optimum ratio of iBTES and TEOS, which was found to be 20/80 vol.%. The results of the scanning electron microscopy method demonstrated the formation of organosilicon material around microorganisms, as well as the ease with which metabolic products of yeast cells and substrates could diffuse through the obtained pores. A laboratory model of the biofilter was developed, exhibiting an oxidative capacity that varied from 0.14 to 1.25 gO₂/(m³ × cycle) in accordance with the initial level of water pollution and the degree of purification of moderately polluted water. The latter was found to be 20%, which aligns with the norm for drip biofilters operating in cyclic mode. Full article