Search Results (26)

A CO₂-responsive TMPDA–SDS–SiO₂ gel system was developed and evaluated through formulation optimization, structural characterization, rheological testing, and core flooding experiments. The optimal formulation was identified as 7.39 wt% SDS, 1.69 wt% TMPDA, and 0.1 wt% SiO₂, achieving post-CO₂ viscosities above 10³–10⁴ mPa·s. Spectroscopic and microscopic analyses confirmed that CO₂ protonates TMPDA amine groups to form carbamate/bicarbonate species, which drive the micellar transformation into a wormlike network, thereby enhancing gelation and viscosity. Rheological tests showed severe shear-thinning behavior, excellent shear recovery, and reversible viscosity changes under alternating CO₂/N₂ injection. The gel demonstrated rapid responsiveness, reaching stable viscosities within 8 min, and maintained good performance after 60 days of thermal aging at 90 °C and in high-salinity brines. Plugging tests in sand-packed tubes revealed that a permeability reduction of 98.9% could be achieved at 0.15 PV injection. In heterogeneous parallel core flooding experiments, the gel preferentially reduced high-permeability channel conductivity, improved sweep efficiency in low-permeability zones, and increased incremental oil recovery by 14.28–34.38% depending on the permeability contrast. These findings indicate that the CO₂-responsive TMPDA–SDS–SiO₂ gel system offers promising potential as a novel smart blocking gel system for improving the effectiveness of CO₂ flooding in heterogeneous reservoirs. Full article

The limited oxidation resistance of MoSi₂ between 400 °C and 600 °C restricts its aerospace applications. This study develops a silica-sol derived core-shell MoSi₂@SiO₂ composite to enhance the low-temperature oxidation resistance of MoSi₂. Acidic, neutral, and basic silica sols were systematically applied to coat MoSi₂ powders through sol-adsorption encapsulation. Two pathways were used, one was ethanol-mediated dispersion, and the other was direct dispersion of MoSi₂ particles in silica sol. Analysis demonstrated that ethanol-mediated dispersion significantly influenced the coating efficiency and oxidation resistance, exhibited significantly decreased coating weight gains (maximum 27%) and increased oxidation weight gains (10–20%) between 340 °C and 600 °C compared with direct dispersion of MoSi₂ particles with silica sol, ascribe to the kinetic inhibition of hydroxyl group condensation and steric hindrance of MoSi₂-silica sol interface interactions of ethanol. Systematic investigation of silica sol encapsulation of MoSi₂ revealed critical correlations between colloid properties and oxidation resistance of MoSi₂@SiO₂. Basic silica sol coated MoSi₂ (BS-MoSi₂) exhibits the lowest coating efficiency (coating weight gain of 7.74 ± 0.06%) as well as lowest oxidation weight gain (18.45%) between 340 °C and 600 °C compared with those of acid and neutral silica sol coated MoSi₂ (AS-MoSi₂ and NS-MoSi₂), arises from optimal gelation kinetics, enhanced surface coverage via reduced agglomeration, and suppressed premature nucleation through controlled charge interactions under alkaline conditions. Full article

Despite efforts to recycle, boro-alumino-silicate pharmaceutical glass (BASG) results in a significant portion of glass cullet currently landfilled. Highly contaminated fractions of BASG cullet are largely unemployed because of the presence of metals in their composition that prevents recycling. This waste glass can be eligible to produce sustainable alkali-activated materials (AAMs) reducing at the same time consumption of raw materials and CO₂ emissions. The ‘weak’ alkaline attack (NaOH < 3 M) determines the gelation of glass suspensions. Condensation reactions occur in hydrated surface layers, leading to strong bonds (Si-O-Si, Al-O-Si, etc.) between individual glass particles. Alkali are mostly expelled from the gel due to the formation of water-soluble hydrated carbonates. Microwave treatment has been implemented on samples after precuring at 40 °C, saving time and energy and achieving better mechanical properties. To improve the stability and reduce the release of glass components into solution, the consolidated monoliths were subjected to boiling/drying cycles. The chemical stability, cytotoxicity and antibacterial behavior of the final products have been investigated with the purpose of obtaining new competitive and sustainable materials. For further stabilization and for finding new applications, the activated and boiled samples can be fired at low temperature (700 °C) to obtain, respectively, a homogeneous foam or a compact material with glass-like density and microstructure. Full article

Silica aerogels are extensively used as catalyst supports due to their mesoporous structure and chemical inertness. In this study, SiO₂–AuNP aerogels containing gold nanoparticles (AuNPs) were synthesized using the sol-gel method followed by supercritical CO₂ drying. The inclusion of polyvinyl pyrrolidone (PVP) as a stabilizing agent preserved the gold particle sizes during the gelation process. In contrast, aerogels synthesized without PVP contained enlarged AuNP aggregates, resulting in a shift in the plasmon resonance color from red to bluish or blue–grey. Thermal treatment of these bluish-colored aerogels at high temperatures restored their red coloration, visually indicating the breakdown of large gold clusters into individual nanoparticles. Both types of aerogels were characterized using SEM, TEM, 3D optical microscopy, UV–vis and ATR-IR spectroscopy, and N₂ porosimetry, with their properties analyzed as a function of annealing temperature. Their catalytic activity was evaluated through the reduction of 4-nitrophenol with sodium borohydride, and both aerogel types demonstrated catalytic activity. This thermal conversion of large clusters into individual nanoparticles within an aerogel matrix introduces a new and promising approach for creating catalytically active nanogold-containing aerogel catalysts. Full article

By way of the sol–gel chemical synthesis method, it is possible to synthesize SiO₂ nanoparticles with a defined specific particle size, a surface area, and a defined crystal structure that can be effectively used as a nanoadsorbent to remove various organic dyes. SiO₂ nanoparticles were synthesized by the sol–gel method using sodium silicate (Na₂SiO₃) by a green method without using a tetraethyl orthosilicate (TEOS) precursor, which is very expensive and highly toxic. This sol–gel process involves the formation of a colloidal suspension (sol) and solid gelation to form a network in a continuous liquid phase (gel). In addition, it requires controlled atmospheres. XRD indicates the presence of an amorphous phase with a diffraction angle of 2θ = 23°, associated with SiO₂. UV-Vis spectroscopy reveals an absorbance value in the region of 200 nm to 300 nm, associated with SiO₂ nanoparticles. The application as a nanoadsorbent to remove dyes was measured, and it was found that the nanoparticles with the best performance were those that were synthesized with pH 7, showing a 97% removal with 20 mg of SiO₂ nanoparticles in 60 min. Therefore, SiO₂ nanoparticles can be used as a nanoadsorbent, using a low-cost and scalable method for application to remove methylene blue in an aqueous medium. Full article

Alkaline sodium hydroxide/sodium silicate-activating high-purity metakaolin geopolymerization is described in terms of metakaolin deconstruction in tetrahedral hydrate silicate [O[Si(OH)₃]]⁻ and aluminate [Al(OH)₄]⁻ ionic precursors followed by their reassembling in linear and branched sialates monomers that randomly copolymerize into an irregular crosslinked aluminosilicate network. The novelty of the approach resides in the concurrent thermo-calorimetric (differential scanning calorimetry, DSC) and rheological (dynamic mechanical analysis, DMA) characterizations of the liquid slurry during the transformation into a gel and a structural glassy solid. Tests were run either in temperature scan (1 °C/min) or isothermal (20 °C, 30 °C, 40 °C) cure conditions. A Gaussian functions deconvolution method has been applied to the DSC multi-peak thermograms to separate the kinetic contributions of the oligomer’s concurrent reactions. DSC thermograms of all tested materials are well-fitted by a combination of three overlapping Gaussian curves that are associated with the initial linear low-molecular-weight (Mw) oligomers (P1) formation, oligomers branching into alumina-rich and silica-rich gels (P2), and inter- and intra-molecular crosslinking (P3). The loss factor has been used to define viscoelastic behavioral zones for each DMA rheo-thermogram operated in the same DSC thermal conditions. Macromolecular evolution and viscoelastic properties have been obtained by pairing the deconvoluted DSC thermograms with the viscoelastic behavioral zones of the DMA rheo-thermograms. Two main chemorheological behaviors have been identified relative to pre- and post-gelation separation of the viscoelastic liquid from the viscoelastic solid. Each comprises three behavioral zones, accounting for the concurrently occurring linear and branching oligomerization, aluminate-rich and silica-rich gel nucleations, crosslinking, and vitrification. A “rubbery plateau” in the loss factor path, observed for all the testing conditions, identifies a large behavioral transition zone dividing the incipient gelling liquid slurry from the material hard setting and vitrification. Full article

The present research article investigates the extraction of aluminum (Al) from an engineered CaO-Al₂O₃-SiO₂ slag by leaching with aqueous HCl under atmospheric pressure conditions. The slag is the by-product of an aluminothermic reduction process to produce metallurgical-grade silicon (Si) in a more sustainable way compared to conventional carbothermic reduction. One major challenge in the acidic leaching of aluminosilicate materials, like the slag treated in this study, is the possibility of SiO₂ gel formation during the leaching process. Extensive SiO₂ gel formation can make the separation of pregnant leach solution (PLS) from the leached residue impossible. Consequently, any acid leaching of aluminosilicate materials must be optimized for avoidance of these gelation phenomena. The present study first explores the leaching behavior of the calcium aluminosilicate slag in relation to the S/L ratio, with all other hydrometallurgical factors remaining stable (20.2% wt. HCl solution, 80 °C, optimized stirring rate), to determine at which value of this parameter SiO₂ gelation occurs. After determining the optimum S/L ratio for this system, an analysis of the behavior of Si in the PLS is presented, and the mechanism of SiO₂ gelation is explained based on critical assessment of these results against data provided from the scientific literature. It was found that the value of the pH of the PLS and the concentration of dissolved CaCl₂ and AlCl₃ are critical factors for the formation of filterable amorphous SiO₂. Under the optimum leaching conditions, PLS containing 37 g/L Al was obtained with concurrent avoidance of gelation phenomena. Full article

A novel, one-pot sol–gel preparation scheme leading to reproducible incorporation of 20–40 nm sized gold nanoparticles (AuNPs) in SiO₂ gels is developed based on in situ reduction during gelation using chloroauric acid and ascorbic acid. Variation in the preparation conditions affects the chemical composition, optical properties and size distribution of the AuNPs incorporated in the silica gels. Different organic dopants, i.e., oleic acid, acetic acid or dodecanethiol, are applied to modify the final composite material and to control the rate of reduction and growth of the AuNPs in the gels. The synthesized samples are characterized by UV/Vis/NIR spectroscopy, X-ray diffraction, transmission electron microscopy, thermal conductivity measurements and DTA/TG measurements. The optical properties of the obtained composites are explained using Mie theory. The incorporation of AuNPs leads to an increase in the thermal conductivity of the silica gels. The best process method in this contribution is the use of NaOH as a gelation catalyst and oleic acid as an organic modifier, leading to 20 nm AuNPs dispersed in the silica matrix. Full article

High-performance coating could be used to protect steels in engineering. The GPTMS-TEOS hybrid coatings were successfully prepared using (3-glycidoxypropyl) trimethoxysilane (GPTMS) and tetraethylorthosilicate (TEOS) as reaction raw materials and diethylenetriamine (DETA) as both a curing agent and catalyst at room temperature. The hybrid coating contained amorphous SiO₂ and was characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The DETA content of the hybrid coating has a significant impact on the performance of the coating. As the DETA content increases, the thermal stability of the hybrid coating increases at 400–600 °C due to the production of more SiO₂ in the amine-rich state. However, the gelation time decreases dramatically, preventing the hybrid coating from better infiltrating the surface of the steel substrate. In addition, there are not enough silicon hydroxyl groups to bond with the hydroxyl groups on the surface of carbon steel and adhesion is significantly reduced. Therefore, hybrid coatings with a moderate DETA content (NH:epoxy ratio equivalent to 1:1) show the best corrosion resistance, with a third-order magnitude increase in corrosion resistance compared to that of carbon steel. Full article

We present a crack-free optically active SiO₂ glass-composite material containing YAG:Ce synthesized via a modified sol–gel technique. A glass-composite material consisting of yttrium aluminum garnet doped with Ce³⁺ (YAG:Ce) was entrapped into a SiO₂ xerogel. This composite material was prepared using a sol–gel technique with modified gelation and a drying process to obtain crack-free optically active SiO₂ glass. The concentration of the YAG:Ce was from 0.5 to 2.0 wt%. All synthesized samples were characterized via X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques, confirming their exceptional quality and structural integrity. The luminescence properties of the obtained materials were studied. Overall, the prepared samples’ excellent structural and optical quality makes them great candidates for further investigation, or even potential practical application. Furthermore, boron-doped YAG:Ce glass was synthesized for the first time. Full article

To reduce the harm caused by industrial solid waste to the environment, and solve the problem of excavated soil disposal in buried pipeline management projects, this study proposes a method to produce soil-based controlled low strength materials (CLSM) by using industrial solid wastes (including fly ash and red mud) as partial replacements for cement. The properties of CLSM were characterized in terms of flowability, unconfined compressive strength, phase composition and microstructure. The test results showed that fly ash could significantly improve the flowability of CLSM, while red mud had more advantages for the strength development. When 20% fly ash and 30% red mud were combined to replace cement, the fluidity of CLSM was 248 mm, and the unconfined compressive strength (UCS) at 3, 7 and 28 days was 1.08, 1.49 and 3.77 MPa, respectively. The hydration products of CLSM were mainly calcium silicate hydrate gels, ettringite and calcite. Fly ash provided nucleation sites for cement hydration, while the alkali excitation of red mud promoted the dissolution of SiO₂ and Al₂O₃ in fly ash. The filling and gelation of hydration products make the microstructure dense, which improves the mechanical properties of the mixture. Full article

Condensation reactions of chlorosilanes (SiCl₄ and CH₃SiCl₃) and bis(trimethylsilyl)ethers of rigid, quasi-linear diols (CH₃)₃SiO–AR–OSi(CH₃)₃ (AR = 4,4′-biphenylene (1) and 2,6-naphthylene (2)), with release of (CH₃)₃SiCl as a volatile byproduct, afforded novel hybrid materials that feature Si–O–C bridges. The precursors 1 and 2 were characterized using FTIR and multinuclear (¹H, ¹³C, ²⁹Si) NMR spectroscopy as well as single-crystal X-ray diffraction analysis in case of 2. Pyridine-catalyzed and non-catalyzed transformations were performed in THF at room temperature and at 60 °C. In most cases, soluble oligomers were obtained. The progress of these transsilylations was monitored in solution with ²⁹Si NMR spectroscopy. Pyridine-catalyzed reactions with CH₃SiCl₃ proceeded until complete substitution of all chlorine atoms; however, no gelation or precipitation was found. In case of pyridine-catalyzed reactions of 1 and 2 with SiCl₄, a Sol–Gel transition was observed. Ageing and syneresis yielded xerogels 1A and 2A, which exhibited large linear shrinkage of 57–59% and consequently low BET surface area of 10 m²⋅g⁻¹. The xerogels were analyzed using powder-XRD, solid state ²⁹Si NMR and FTIR spectroscopy, SEM/EDX, elemental analysis, and thermal gravimetric analysis. The SiCl₄-derived amorphous xerogels consist of hydrolytically sensitive three-dimensional networks of SiO₄-units linked by the arylene groups. The non-hydrolytic approach to hybrid materials may be applied to other silylated precursors, if the reactivity of the corresponding chlorine compound is sufficient. Full article

Polymer gel plugging is an effective technique for gas mobility control in flue gas flooding reservoirs. However, the performance of polymer gels is extremely susceptible to the injected flue gas. A reinforced chromium acetate/partially hydrolyzed polyacrylamide (HPAM) gel, using thiourea as the oxygen scavenger and nano-SiO₂ as the stabilizer, was formulated. The related properties were evaluated systematically, including gelation time, gel strength, and long-term stability. The results indicated that the degradation of polymers was effectively suppressed by oxygen scavengers and nano-SiO₂. The gel strength would be increased by 40% and the gel kept desirable stability after aging for 180 days at elevated flue gas pressures. Dynamic light scattering (DLS) analysis and Cryo-scanning electron microscopy (Cryo-SEM) revealed that nano-SiO₂ was adsorbed on polymer chains by hydrogen bonding, which improved the homogeneity of gel structure and thus enhanced the gel strength. Besides, the compression resistance of gels was studied by creep and creep recovery tests. The failure stress of gel with the addition of thiourea and nanoparticles could reach up to 35 Pa. The gel retained a robust structure despite extensive deformation. Moreover, the flow experiment indicated that the plugging rate of reinforced gel still maintained up to 93% after flue gas flooding. It is concluded that the reinforced gel is applicable for flue gas flooding reservoirs. Full article

Protection of concrete against aggressive influences from the surrounding environment becomes an important step to increase its durability. Today, alkali silicate solutions are advantageously used as pore-blocking treatments that increase the hardness and impermeability of the concrete’s surface layer. Among these chemical substances, known as concrete densifiers, lithium silicate solutions are growing in popularity. In the present study, the chemical composition of the lithium silicate densifiers is put into context with the properties of the newly created insoluble inorganic gel responsible for the micro-filling effect. Fourier-transform infrared spectroscopy was used as a key method to describe the structure of the formed gel. In this context, the gelation process was studied through the evolution of viscoelastic properties over time using oscillatory measurements. It was found that the gelation process is fundamentally controlled by the molar ratio of SiO₂ and Li₂O in the densifier. The low SiO₂ to Li₂O ratio promotes the gelling process, resulting in a rapidly formed gel structure that affects macro characteristics, such as water permeability, directly related to the durability of treated concretes. Full article

Polymer gels have been widely used in high water cut oilfields for profile control and water plugging. It is urgent to develop a gel suitable for the Tahe Oilfield (Temperature: 130 °C, salinity: 2.2 × 10⁵ mg/L) in China. A stable gel was prepared by using an acrylamide (AM)/2-acrylamide-2-methyl propanesulfonic acid (AMPS) copolymer crosslinked with urotropin (HMTA), hydroquinone (HQ), thiourea and Nano-SiO₂. This paper covers a step-by-step process for designing gels based on experience with preparing gels. A wide range of combinations between polymers and crosslinking agents with and without stabilizers were investigated, and the results indicated that there is an optimal value of AMPS content of AM/AMPS copolymers in the preparation of gels. Increasing the mass fraction of copolymer and using stabilizer enhanced the performance of gel, but an excessive amount of crosslinking agent was not conducive to the stability of gel. The work optimized the formula of plugging agent suitable for the high temperature and high salt (HTHS) condition in the Tahe Oilfield. The gelling solution had a long gelation time of 20 h. The gel had high strength (Sydansk’s gel-strength code of “G”) with storage modulus of 12.9 Pa and could be stable for half a year at 130 °C and 2.2 × 10⁵ mg/L of salinity. The plate model that could be heated and pressurized was used to simulate the oil flooding and profile modification under the condition of the Tahe Oilfield for the first time. The experiment results showed that the oil recovery could be increased by 13.22% by subsequent water flooding under heterogeneous formation condition. Therefore, it was fully confirmed that the plugging performance of AM/AMPS phenolic gel prepared in the work was excellent. The information provided in the study could be used as a reference for the design and evaluation of polymer gels in other HTHS reservoirs. Full article