Search Results (210)

The long-term structural stability of ordered mesoporous silica (OMS) materials—specifically the durability of their pore architecture and pore lattice over time—is critical for their performance in catalysis, separation, drug carrier and nanoconfinement applications. SBA-15-type silica materials are synthesized via two different routes, namely the conventional “liquid crystal templating” (LCT) and the much less common “true liquid crystal templating” (TLCT) of micellar structures formed by the amphiphilic block copolymer Pluronic P123 in water. Here, we report that SBA-15 materials age very differently depending on the synthesis route: Under ambient conditions, OMS materials obtained via the LCT route undergo significant structural changes over time, especially in microporous regions, while SBA-15 materials obtained via the TLCT route show less or even no structural changes even after a year of storage. We attribute this enhanced aging stability of TLCT materials to their narrow mesopore size distribution and their much lower degree of microporosity. Full article

Treatment of palladium precursor Pd(PPh₃)Cl₂ with equivalent arylfluorodithiophosphato ligand [PPh₄][(4-EtO-C₆H₄)FPS₂] in chloroform at reflux resulted in a mononuclear palladium(I)–sulfur complex cis-[Pd(PPh₃)₂{κ²-S,S′-(4-EtO-C₆H₄)FPS₂}]. This complex was characterized by UV-Vis and IR spectroscopic analysis, thermogravimetric analysis, and XPS analysis, and its molecular structure has been established by single-crystal X-ray diffraction. SBA-15, as a mesoporous material, was selected as a mesoporous silica substrate to further form a homogeneous catalyst, Pd@SBA-15, which has been characterized by IR spectroscopy, electron microscope and N₂ adsorption–desorption test. In addition, the catalytic activity of Pd@SBA-15 for the Suzuki–Miyaura cross-coupling reaction was also investigated. Full article

The rational design of supported ruthenium catalysts for sustainable energy applications requires precise control over metal nanoparticle size, dispersion, and metal–support interactions. This study investigates the influence of mesoporous silica support topology—SBA-15 (2D hexagonal, cylindrical pores), SBA-12 (3D hexagonal structure), and SBA-3 (2D hexagonal)—on the structure and catalytic performance of 1 wt% ruthenium catalysts in CO₂ methanation and gas-phase toluene hydrogenation. Comprehensive characterization by nitrogen physisorption, low- and high-angle X-ray diffraction (XRD), H₂ temperature-programmed reduction (H₂-TPR), CO chemisorption, and transmission electron microscopy (TEM) revealed that support pore architecture dictates ruthenium particle size (1.2 nm for Ru/SBA-15, 2.8 nm for Ru/SBA-3, 4.3 nm for Ru/SBA-12) and dispersion (80%, 35%, 23%, respectively) through geometric confinement effects. Catalytic testing demonstrated contrasting structure–activity relationships: CO₂ methanation exhibited strong structure sensitivity with turnover frequency (TOF) increasing with particle size (Pearson’s r = 0.96), favoring Ru/SBA-3 and Ru/SBA-12 with near-optimal 3–4 nm particles, while toluene hydrogenation showed weaker structure sensitivity, with Ru/SBA-12 achieving the highest TOF owing to its larger particle size and higher crystallinity. These findings underscore the critical importance of tailoring mesoporous support topology to match reaction-specific structure sensitivity, providing fundamental insights for the design of bifunctional catalysts for hydrogenation reactions. Full article

Ultrafast sonochemical synthesis of SBA-15 performed via the pH-adjustment method at 25 °C was reported. Ultrasound treatment was applied to the entire synthesis process for a period of 90 min. The sonication synthesis was compared with the aging-mediated sonication method. Ultrasound assistance under the studied conditions allows the aging step to be replaced and minimizes the structural deterioration of SBA-15 due to the pH-adjustment effect. In addition, the hydrophilic character and CO₂ adsorption capacity of these materials were studied using contact-angle techniques and CO₂ adsorption, respectively. Ultrasonic synthesis at 25 °C results in the best uniformity of a mesopore structure relative to its peers. Full article

The overreliance on non-renewable phosphate fertilizers necessitates sustainable alternatives for phosphorus recycling in agriculture. This study aimed to characterize and enhance the metabolic activity of phosphate-solubilizing microorganisms isolated from compost by eliciting them with two distinct mesoporous silica nanoparticles: standard SBA-15-S and short-pore SBA-15-C. Bacterial strains with broad-spectrum P solubilization and mineralization capacities were isolated from the mesophilic phases of tomato greenhouse and cow manure composts. These isolates received treatment with nanoparticle concentrations of 0.1, 10, and 100 ppm. The results demonstrated that nanoparticle elicitation significantly altered microbial growth, solubilization halos on tricalcium phosphate, and the specific activity of acid, neutral, and alkaline phosphatases in a strain- and nanoparticle-dependent manner. Notably, SBA-15-C at 100 ppm consistently enhanced multiple P-recycling properties across several strains, including Proteus and Myroides species. Principal component analysis revealed distinct behavioral clusters between composting phases and isolation methods. The findings indicate that tailored silicon oxide nanostructures can serve as eustressors to modulate and enhance the P-solubilizing and mineralizing functions of compost-derived microbiota, offering a promising nanobiostimulation strategy for developing enhanced biofertilizers. Full article

The incorporation of drugs into nanostructured silica has proven to be an effective strategy for delaying drug release, protecting against enzymatic degradation, and enhancing therapeutic efficacy. Specifically, crotoxin, a component derived from the venom of Crotalus durissus terrificus, exhibits notable analgesic and immunomodulatory properties. Previous studies have demonstrated that encapsulating crotoxin within SBA-15 nanostructured mesoporous silica not only reduces its toxicity and enhances its analgesic effects but also enables effective oral administration. Given its promising efficacy and the expanding interest in its application across various experimental models and potential therapeutic uses, this study aimed to conduct a detailed analysis of the physicochemical properties of crotoxin when incorporated into SBA-15 silica. Following characterization, the crotoxin–SBA-15 complex was orally administered to mice in an experimental model of ulcerative colitis (UC). The most widely adopted experimental model for studying UC involves the administration of dextran sodium sulfate (DSS) in drinking water to induce colonic inflammation in susceptible animals. In this study, we hypothesized that crotoxin incorporated into ordered mesoporous silica (SBA-15) could modulate DSS-induced UC. Crotoxin was successfully incorporated into SBA-15 and administered orally, as its physicochemical properties supported this route of delivery. Mice received the crotoxin–SBA-15 complex either at the onset of UC induction or on days 1 and 4 after DSS exposure. Seven days after the start of DSS administration, we observed a substantial reduction (approximately 50%) in Disease Activity Index (DAI) scores, accompanied by marked improvements in the histopathological features of the colon. These findings indicate for the first time that crotoxin incorporated into SBA-15 exhibits significant therapeutic potential in the treatment of experimentally induced ulcerative colitis. Full article

AgI and ZnI₂ nanocrystals are key components for AgI-ZnI₂-SiO₂ hybrid powders (HPs), which could be potentially important for atmospheric artificial precipitation technology. HPs were created by the “Hydrothermal template cocondensation” method (“HTC” method). Mesoporous silica dioxide (MCM48, MCM41, SBA15, SBA16), silver iodides, and zinc iodides were simultaneously grown under specific conditions. The influence of silica dioxide on AgI and ZnI₂ nanocrystals characteristics (phase, size, and thermal stability) were studied using various physicochemical analysis methods. In addition to crystal features, some structural and textural properties of the AgI-ZnI₂-SiO₂ hybrid as an individual agglomerate and its morphology were determined. This showed that nanocrystal features were dependent on synthesis condition. The influence of the nature of the reagent, which is pH-forming, was manifested at the initial stage of the process, and the morphology of the silica dioxide matrix controlled the crystal properties during the post-synthesis phase. It was established that the thermal stability of AgI and ZnI₂ nanocrystals increased due to the protective shielding function of that SiO₂ matrix. Full article

Mesoporous silica and its derivatives might enable applications ranging from biomedicine to petrochemical processing. Transmission electron microscopy (TEM), X-ray diffraction (XRD) and N₂ adsorption–desorption measurements are usually used to characterize the ordered porous system. However, none of these methods convey the full surface information. In this work, a low-voltage scanning electron microscope (LVSEM) with beam deceleration technology was employed to image detailed surface structures of ~2 nm pore size silica (MCM-41), SBA-15, KIT-6, and mesoporous silica nanospheres (MSNSs). The prospects for the development of this application of ultra-high-resolution scanning electron microscopy (SEM) are discussed in the characterization of the ordered porous materials. We demonstrate that the complete dimension range of the mesoscopic surface structure (2–50 nm) could be resolved by current low-voltage SEM technology. Full article

In response to the urgent need for sustainable antibacterial solutions against antibiotic-resistant pathogens, this study presents a facile dendritic polymer-assisted approach for synthesizing highly active ZnO/mesoporous silica nanocomposites (SBA-15, SBA-16, KIT-6, MSU-X). Two hyperbranched polymers—polyethyleneimine (PEI) and carboxy-methylated polyethyleneimine (Trilon-P, TrP)—were employed as templating and metal-trapping agents. The influence of pore geometry, polymer functionality, and polymer-loading method (wet or dry impregnation) on ZnO nanoparticle (NP) formation was systematically examined. All nanocomposites exhibited high structural homogeneity, incorporating ultrasmall or amorphous ZnO NPs (1–10 nm) even at 8 wt.% Zn loading. Zn uptake was strongly dependent on polymer end groups, while the spatial distribution of ZnO NPs was dictated by the silica host structure. Antibacterial assays against Staphylococcus aureus revealed remarkable activity, particularly for ZnO/SBA-15_PEI, ZnO/SBA-16_PEI, and ZnO/MSU-X_TrP nanocomposites, with minimum inhibitory concentrations of 1–2.5 μg mL⁻¹ Zn and over 90% mammalian cell viability. Life Cycle Assessment identified energy use as the main environmental factor, with ZnO/SBA-15_PEI_WI displaying the lowest impact. Overall, the interplay between silica pore architecture, polymer type, and impregnation method governs ZnO accessibility and bioactivity, establishing a versatile strategy for designing next-generation ZnO/SiO₂ nanocomposites with tunable antibacterial efficacy and minimal cytotoxic and environmental footprint. Full article

Biofuels are critical drop-in replacement energy sources to support the decarbonisation of hard-to-abate sectors such as aviation and marine shipping. Transesterification of non-edible oils is a well-established route to biodiesel as a versatile liquid transport fuel, but is challenging to scale using existing homogeneous liquid base catalysts. In this work, we report the synthesis, characterisation, and application of silica-supported MgO solid base catalysts for triglyceride transesterification with methanol and highlight the impact of silica pore structure on performance. True liquid crystal templating enables the one-pot synthesis of mesoporous MgO/SBA-15 catalysts with variable Mg content, or hierarchical macroporous–mesoporous MgO/SBA-15 analogues through the addition of polystyrene nanospheres. Both MgO/SBA-15 families exhibit highly ordered pore networks; however, ~280 nm macropores stabilise Mg-O-Si interfacial species even at high Mg loading, in contrast to the mesoporous support that permits sintering of ~14 nm MgO nanocrystals. Hierarchical porous MgO/SBA-15 catalysts exhibit higher specific activity and conversion of tributyrin to methyl butyrate than their mesoporous analogues (3 mmol⋅h⁻¹⋅g⁻¹ versus 2 mmol⋅h⁻¹⋅g⁻¹ at 60 °C and 11 wt% Mg). The magnitude of this rate enhancement increases with triglyceride chain length, being approximately three-fold for trilaurin (C₁₂) transesterification at 90 °C, attributed to superior in-pore mass transport of bulky reactants through the hierarchical porous catalyst. Full article

Mesoporous materials have attracted increasing attention due to their ordered pore systems; tunable surface chemistry; and versatile applications in catalysis, adsorption, and environmental technologies. Among them, SBA-15 stands out for its large surface area, uniform mesopores, and high hydrothermal stability, which make it a promising platform for gas adsorption and mass transport studies. This review examines the functionalization of SBA-15 through strategies such as post-synthesis grafting and co-condensation, focusing on the introduction of amines, thiols, and organometallic species that enhance selectivity, adsorption capacity, and thermal stability. The discussion integrates classical diffusion models, including Fickian and Knudsen transport, with more advanced approaches such as the Maxwell–Stefan formalism, to describe molecular transport within mesoporous networks and highlight the role of van der Waals interactions in gas capture processes. Special emphasis is placed on the relationship between structural features and diffusive behavior, supported by recent advances in computational modeling and spectroscopic validation. Applications in CO₂ capture, heterogeneous catalysis, drug delivery, and environmental remediation are critically assessed to illustrate the versatility of functionalized SBA-15. This review concludes by outlining future perspectives on the rational design of hierarchical and multifunctional mesoporous materials for clean energy conversion, pollutant removal, and biomedical applications. Full article

In recent years CO₂ reforming of methane has attracted great interest as it produces high CO/H₂ ratio syngas suitable for the synthesis of higher hydrocarbons and oxygenated derivatives since it is a way for disposing and recycling two greenhouse gases with high environmental impact, CH₄ and CO₂, and because it is regarded as a potential route to store and transmit energy due to its strong endothermic effect. Along with noble metals, all the group VIII metals except for osmium have been studied for catalytic CO₂ reforming of methane. It was found that the catalytic activity of Ni, though lower than those of Ru and Rh, was higher than the catalytic activities of Pt and Pd. Although noble metals have been proven to be insensitive to coke, the high cost and restricted availability limit their use in this process. It is therefore valuable to develop stable Ni-based catalysts. In this contribution, we show how their activity and coking resistivity are greatly related to the size and dispersion of Ni particles. Well-dispersed Ni nanoparticles were achieved by multistep impregnation on a mesoporous silica support, namely SBA-15, obtained through a sol-gel method, using acetate as a nickel precursor and keeping the Ni loading between 5% and 11%. Significant catalytic activity was obtained at temperatures as low as 450 °C, a temperature well below their deactivation temperature, i.e., 700 °C. For the pre-reduced samples, a CO₂ conversion higher than 99% was obtained at approximately 680 °C. As such, their deactivation by sintering and coke formation was prevented. To the best of our knowledge, no Ni-based catalysts with complete CO₂ conversion at temperatures lower than 800 °C have been reported so far. Full article

The fabrication of highly loaded and uniformly dispersed metal oxide nanoparticles (NPs) is much desired but still remains a great challenge. Herein, the NiO NPs exclusively confined in mesoporous silica SBA-15 were obtained by using nickel nitrate hydrate as a precursor through a facile solvent-free preparation method, which comprised manual grinding of Ni(NO₃)₂·6H₂O with SBA-15 and subsequent air calcination. Characterization results from X-ray diffraction (XRD) and transmission electron microscope (TEM) revealed that aggregation-free NiO nanoparticles with sizes of 3–5 nm were obtained at loading as high as 20 wt.% (weight%). Further increasing the NiO loading to 30 wt.% led to partial agglomeration of discrete nanoparticles to rod-like particles, while no external particles were observed. By comparing the sample derived from nickel acetate with exclusively external NiO particles, it was established that the pore confinement provided NiO nanoparticles with high thermal stability. Lastly, the catalytic performance of the prepared sample was evaluated in the model reaction of ammonia decomposition to CO_x-free H₂, and the stable NH₃ conversion of 93.7% was achieved at the weight hourly space velocity (WHSV) value of 30,000 mL·g⁻¹·h⁻¹ and at high temperature of 650 °C for 60 h, demonstrating the great potential of the solvent-free method in preparing thermally stable and robust supported catalysts. Full article

This study introduces a novel approach for analyzing theoretical Raman spectra, designed to facilitate spectral interpretation, particularly for complex systems such as functional mesoporous silica-based thin films. The proposed methodology relies on spectral decomposition supported by theoretical calculations, representing a step toward the development of autonomous research laboratories. The method assigns vibrational shifts to individual atoms within a molecular model and uses this information to generate partial spectra corresponding to specific atomic groupings. Unlike separate calculations for isolated components, this approach preserves the mutual interactions within the entire molecular structure, providing a more accurate representation of the vibrational environment. Decomposing the theoretical spectrum into contributions from atomic groups significantly simplifies the assignment of Raman bands to specific structural units, thereby enhancing the interpretative power of theoretical spectra and their correlation with experimental data. The method was demonstrated using real Raman spectroscopic data obtained from mesoporous SBA-15 silica thin films containing copper phosphonate groups. This work also highlights the critical role of molecular modeling and DFT calculations in Raman spectral analysis and outlines future perspectives for the use of artificial intelligence to automate and optimize the spectral interpretation process. Full article

Furfural and 5-hydroxymethylfurfural are considered as essential platform molecules for the chemical industry, acting as precursors and intermediates of numerous products. They are produced from pentoses and hexoses, respectively, in an acid medium. In this work, biomass from a green macroalgae, Ulva rigida, was treated under acidic conditions provided by heterogeneous catalysts in order to promote the dehydration of its monosaccharides into furfural and 5-hydroxymethylfurfural. Particularly, two functionalized mesoporous silicas, HMS and SBA-supported metal oxides (Nb₂O₅ and ZrO₂), were used as catalysts. Their textural, structural, and acid properties were deeply studied, providing excellent BET surface areas (ranging 424 to 1204 m²/g) and a high concentration of acid sites (220–460 µmol/g), which then translated into great catalytic performances (77.8% and 64.1% of furfural and HMF molar yields, respectively, using HMS-Nb) after a 4 h of reaction time at 180 and 160 °C, respectively. The catalyst showed excellent stability and recyclability as it could be reused for up to five reaction runs with only a slight decrease in performance. Full article