Search Results (123)

CO₂ methanation is considered a key process in achieving carbon neutrality. Expanding on our previous study of supercritically dried Ni-Al aerogels, this work compares two gel-based catalyst families prepared via two different routes—supercritically dried Ni impregnated Al aerogel-based catalysts and oven-dried one-pot Ni-Al xerogel-based catalysts—to assess how the synthesis route affects catalyst structure and CO₂ methanation performance under light irradiation. The catalysts were subsequently characterized via different techniques, such as ICP-OES, N₂ adsorption–desorption isotherms, XRD, H₂-TPR, UV-vis DRS, XPS, and TEM. Catalytic activity was tested in a photoreactor at a range of temperatures from 300 °C to 450 °C and 10 bar pressure, and two different light sources were used (λ = 365 nm, λ = 470 nm). Both light sources enhanced catalytic activity in most cases; the xerogels with higher Ni loadings were the most active materials. These catalysts reached CO₂ conversions and CH₄ selectivities near 70% and 100%, respectively. The results indicate that drying gels is a promising method for synthesizing catalysts active in the Sabatier reaction, given the properties of the materials. Full article

The structure collapse and performance degradation caused by traditional air-drying technology often hinder the practical application of bio-based xerogels as absorbent pads. In this study, chitosan (CS) and different types of polyanions (carboxymethyl cellulose (CMC), sodium alginate (SA), hyaluronic acid (HA), pectin (PT) and xanthan gum (XG)) in different proportions were used to prepare an xerogel resistant to atmospheric pressure air drying collapse, and its potential as an absorption pad was systematically evaluated. The results showed that among all the treatments, CS/CMC xerogel at an optimal mass ratio of 1:3 demonstrated superior comprehensive properties. It exhibited minimal shrinkage (p < 0.05) and high porosity, coupled with an exceptional water absorption capacity (140% higher than CS/PT) and hardness (96% higher than CS/SA and CS/HA). FTIR and XRD revealed that strong electrostatic interactions and potential amide bond formation between CS and CMC resulted in a dense yet homogeneous network with low crystallinity. SEM imaging further corroborated a uniform thin-walled porous structure. This stable network contributed to high toughness, of CS/CMC significantly surpassing the brittle CS/XG and CS/PT xerogels (p < 0.05). CS/CMC xerogel is an ideal absorbent material with high absorption, stability, and controllable structure. Full article

This study presents an energy-efficient, room-temperature synthesis and characterization of methacrylated pullulan (Pull-MA) hydrogel developed for controlled nutrient delivery in agricultural applications. Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC) analyses confirmed the successful functionalization of pullulan with methacrylate groups, accompanied by a decrease in thermal transition temperatures, indicative of increased polymer chain mobility. The synthesized Pull-MA hydrogel exhibited a high swelling capacity, reaching an equilibrium swelling ratio of 1068% within 5 h, demonstrating its suitability as a carrier matrix. The room-temperature synthesis approach enabled the in situ incorporation of microbial inoculant into the hydrogel network, preserving microbial viability and activity. SEM analysis performed under the different magnifications (1000, 2500, 5000, 10,000, 25,000×) has confirmed brittle nature of xerogels and increasing in structural irregularities with increasing in cultivation broth content.The biological performance of the fertilizer-loaded hydrogels was evaluated through seed germination assays using maize and pepper as model crops. The optimized formulation, T2 (Pull-MA: cultivation broth 1:5 w/w), significantly improved germination efficiency, as evidenced by increased relative seed germination (RSG), root growth rate (RRG), and germination index (GI) compared to both the control and the low-fertilizer formulation (T1, 1:2.5 w/w). These findings highlight the potential of Pull-MA hydrogels as bioactive seed-coating materials that enhance early seedling development through controlled nutrient release. The results lay a solid foundation for further optimization and future application of this system under real field conditions. Full article

We have investigated the structural, morphological, magnetic, and up-conversion luminescence properties of the Yb³⁺/Er³⁺-doped LiGdF₄ nanocrystals precipitated in the silica glassy matrix. Morphological analysis showed uniform distribution of LiGdF₄ nanocrystals (tens of nm in size), embedded in silica glass matrix. FTIR spectroscopy analysis showed trifluoracetates thermolysis with silica lattice formation and structural analysis by XRD is consistent with the LiGdF₄ crystallization process, most likely through an autocatalytic reaction. The stress and crystalline lattice distortion are assigned to the doping and glass matrix environment where the growth process occurs. The EPR spectra associated with the Gd³⁺ ions have shown a well-defined spectrum in the xerogel, associated with the trifluoroacetate ligand environment. In the LiGdF₄ nanocrystals, the broad and unresolved spectrum is due to an envelope of unresolved anisotropic fine structure and a high dipole–dipole interaction between the Gd³⁺/Yb³⁺/Er³⁺ paramagnetic ions. Under 980 nm laser light pumping, we observed the characteristic “blue”, “green” and “red” up-conversion luminescences of the Er³⁺ ions through Yb → Er energy transfer process, that imply three and two-photon process; near UV up-conversion luminescence of Gd³⁺ is observed at about 280–300 nm where Yb → Er and Er → Gd energy transfer is involved. The UC luminescence properties can be improved up to two times by additional Yttrium co-doping due to the induced crystal field distortion. Full article

p-toluenesulfonic acid (pTSA) was used for the synthesis of porous silica xerogels while applying different synthesis conditions. Key parameters included acid concentration, drying temperature and the method of acid removal. The resulting organic–inorganic composites were investigated by nitrogen physisorption, X-ray powder diffraction (XRD), solid-state NMR and thermal analysis. The results demonstrated that both the drying temperature and quantity of the pTSA significantly influenced the pore structure of the xerogels. The utilization of such strong acids like pTSA yielded high surface area and pore volume, as well as narrow pore size distribution. Environmentally friendly template removal by solvent extraction produced materials with superior textural properties compared to traditional calcination, enabling the recovery and reuse of pTSA with over 95% efficiency. A selected mesoporous silica xerogel was modified by a simple two-step post-synthesis procedure with 1-(2-Hydroxyethyl) piperazine (HEP). High CO₂ adsorption capacity was determined for the HEP-modified material in dynamic conditions. The isosteric heat of adsorption revealed the stronger interaction between functional groups and CO₂ molecules. Total CO₂ desorption could be achieved at 60 °C. Leaching of the silica functional groups could not be detected even after four consecutive adsorption cycles. These findings provide valuable insights into the sustainable synthesis of tunable piperazine-modified mesoporous silica xerogels with potential applications in CO₂ capture. Full article

The contamination of water resources with heavy metals creates problems for using it as a source of drinking water. Adsorption is one of the most promising methods for heavy metal ion removal from natural and wastewater. The process of removing copper (II) from aqueous solutions using SiO₂ xerogel as an adsorbent has been studied. The xerogel was thoroughly characterized by transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and argon adsorption–desorption isotherms, revealing an amorphous structure with a high surface area (~347 m²/g) and uniform mesoporosity (2–14 nm pore size). The surface chemistry, dominated by silanol groups, was confirmed by XPS analysis. The adsorption process is influenced by electrostatic interactions between the positively charged Cu(II) ions and the negatively charged surface groups, with the optimal performance near neutral pH. Batch adsorption experiments demonstrated that the silica xerogel effectively removes Cu(II) ions from aqueous solutions, with removal efficiency exceeding 99% at pH values above 4.0. The maximum adsorption capacity of copper (II) ions on SiO₂ xerogel is 67.5 mg/L. Full article

Research on hydrogen (H₂) production has been intensively investigated due to the critical need for transitioning from fossil fuels to cleaner energy sources. This study demonstrates a dual-purpose approach where water pollutant degradation and H₂ production occur simultaneously, eliminating the need for sacrificial materials and reducing costs. CuO-TiO₂ calcined xerogels were employed in solutions containing NaOH and acid black dye 1 (AB1). The CuO-TiO₂/AB1/NaOH system successfully degraded recalcitrant pollutants while producing H₂ under optimized conditions. H₂ evolution occurred at the photocatalyst holes due to AB1’s lower potential compared to water, while AB1 decomposition proceeded via O2^•− radical formation. X-ray diffraction (XRD) and Scanning Electron Microscope (SEM) analyses showed sponge-like structures with 20 nm crystals. Polarization curves confirmed H₂ generation in the cathodic region. Bode diagrams of the CuO-TiO₂/AB1/NaOH system (0.3 M NaOH and 60 mg/L AB1) exhibited noble/passive behavior, consistent with the polarization curve data. Using 0.3–0.4 M NaOH and 60 mg/L AB1, 636–647 ppb H₂/g_catalyst was produced in 60 min, and only 0.07 mg/L AB1 was left as indicated by absorbance measurements at 618 nm. H₂ evolution decreased as dye degradation increased. The best system for dye degradation has a k constant of 0.066 min⁻¹ and R² of 0.99, contains 40 mg/L AB1, and runs at 40 °C, whereas the maximum dual performance required 0.5 M NaOH, yielding 5050 ppb H₂/g_catalyst. Full article

Microporous alumophosphate molecular sieves AlPO₄-n are promising materials for use in catalysis, gas adsorption, and gas separation. However, AlPO₄-n faces problems such as diffusion limitations that lead to a deterioration in mass transfer. To solve this problem, we studied the crystallization of alumophosphate reaction gels prepared using aluminum isopropoxide and various secondary amines as templates, including diethyl-, di-n-propyl-, diisopropyl-, and di-n-butylamines. Using X-ray diffraction, Ramon spectroscopy, and STEM methods, it has been demonstrated that the reaction gels prepared using DPA, DIPA, and DBA are amorphous xerogels consisting of 5–10 nm nanoparticles. The reaction gel prepared with DEA is a combination of a layered phase and an amorphous aluminophosphate. It has been shown that the use of aluminum iso-propoxide allows the production of AlPO₄-11 in the form of 2–4 µm aggregates consisting of primary AlPO₄-11 nanocrystals. The template was found to exert a significant effect upon both the characteristics of the porous structure and the size of AlPO-11 nanocrystals. A template is proposed for the synthesis of hierarchical AlPO₄-11 with a maximum volume of mesopores. The morphology and crystal size of AlPO₄-11 were found to strongly influence its adsorption properties in the adsorption of octane. Full article

Silica fillers have been a cornerstone in chemical technology due to their versatility, availability, and ease of integration into various formulations. Recent advancements, including chlorine-free synthesis of alkoxysilanes, have paved the way for alternative materials like polymethylsilsesquioxane (PMSSO). This study explores the structural evolution and properties of a hydrophobic PMSSO xerogel, synthesized through hydrolytic polycondensation of methyltriethoxysilane (MTEOS). PMSSO exhibits exceptional hydrophobicity, high specific surface area, and compatibility with polymer matrices, making it a promising filler for applications in rubber products, lubricants, and cosmetics. We developed a straightforward synthesis method for producing PMSSO xerogel that avoids toxic solvents and organochlorosilanes, ensuring safety and sustainability. The reaction conditions, particularly the amount of alkali and neutralization parameters, were found to significantly influence the properties of the final xerogels, such as specific surface area. Optimization of the synthesis parameters allow for obtaining PMSSO xerogels with a specific surface area about 600 m²/g. These findings underscore PMSSO’s potential as a versatile, eco-friendly alternative to conventional silica fillers, offering tailored properties for diverse industrial applications. Full article

In this study, the potential to modify the phase structure and morphology of manganese dioxide synthesized via the hydrothermal route was explored. A series of samples were prepared at different synthesis temperatures (100, 120, 140, and 160 °C) using KMnO₄ and MnSO₄·H₂O as precursors. The phase composition and morphology of the materials were analyzed using various physicochemical methods. The results showed that, at the lowest synthesis temperature (100 °C), an intercalation compound with composition K_1.39Mn₃O₆ and a very small amount of α-MnO₂ was formed. At higher temperatures (120–160 °C), the amount of α-MnO₂ increased, indicating the formation of two clearly distinguished crystal structures. The sample obtained at 160 °C exhibited the highest specific surface area (approximately 157 m²/g). These two-phase (α-MnO₂/K_1.39Mn₃O₆) materials, synthesized at the lowest and highest temperatures, respectively, and containing an appropriate amount of carbon xerogel, were tested as active mass for positive electrodes in a solid-state supercapacitor, using a Na₊-form Aquivion^® membrane as the polymer electrolyte. The electrochemical evaluation showed that the composite with the higher specific surface area, containing 75% manganese dioxide, demonstrated improved characteristics, including 96% capacitance retention after 5000 charge/discharge cycles and high energy efficiency (approximately 99%). These properties highlight its potential for application in solid-state supercapacitors. Full article

In sustainable construction and packaging, the development of novel bio-based materials is crucial, driving a re-evaluation of traditional components. Lightweight, biodegradable materials, including xerogels, have great potential in architectural and packaging applications. However, reinforcing these materials to improve their mechanical strength remains a challenge. Alginate is a promising matrix material that may be compatible with inorganic fibrous or particulate materials. In this study, biocomposite xerogel-structured foam materials based on an alginate matrix with expanded perlite reinforcement are improved using certain additives in different weight ratios. The plasticizers used include glycerol and gum arabic, while chitosan was added as an additional reinforcement, and iota carrageenan was added as a stabilizer. The tested specimens, with varying weight ratios of the added components, showed good mechanical behavior that highlights their potential use as packaging and/or architectural materials. The influence of the presence of different components in the composite material specimens on the modulus of elasticity was investigated using SEM images and FTIR analyses of the specimens. The results show that the specimen with the largest improvement in the elastic modulus contained a combination of chitosan and glycerol at a lower percentage (1.96 MPa), and the specimen with the largest improvement in tensile strength was the specimen containing chitosan with no plasticizers (120 kPa), compared to cases where combinations of other materials are present. Full article

This study compared the chemical, structural, and luminescent properties of xerogel-based ceramic powders (CPs) with those of a new series of crystallized aerogels (CAs) synthesized by the epoxy-assisted sol–gel process. Materials with different proportions of Eu³⁺ (2, 5, 8, and 10 mol%) were synthesized in Lu₂O₃ host matrices, as well as a Eu₂O₃ matrix for comparative purposes. The products were analyzed by infrared spectroscopy (IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS), transmission electron microscopy (TEM), photoluminescence analysis, and by the Brunauer–Emmett–Teller (BET) technique. The results show a band associated with the M-O bond, located at around 575 cm⁻¹. XRD enabled us to check two ensembles: matrices (Lu₂O₃ or Eu₂O₃) and doping (Lu₂O₃:Eu³⁺) with appropriate chemical compositions featuring C-type crystal structures and intense reflections by the (222) plane, with an interplanar distance of around 0.3 nm. Also, the porous morphology presented by the materials consisted of interconnected particles that formed three-dimensional networks. Finally, emission bands due to the energy transitions (⁵D_J, where J = 0, 1, 2, and 3) were caused by the Eu³⁺ ions. The samples doped at 10 mol% showed orange-pink photoluminescence and had the longest disintegration times and greatest quantum yields with respect to the crystallized Eu₂O₃ aerogel. Full article

Metal oxides containing La, Mn, and Co cations can catalyze oxygen reduction reactions (ORRs) in electrochemical processes. However, these materials require carbon support and optimal interactions between both compounds to be active. In this work, two approaches to prepare composites of La-Mn-Co-based compounds over carbon xerogel were developed. Using sol-gel methods, either the metal-based material was deposited on the existing carbon xerogel or vice versa. The metal oxide selected was the LaMn_0.7Co_0.3O₃ perovskite, which has good catalytic behavior and selectivity towards direct ORRs. All the as-prepared composites were tested for ORRs in alkaline liquid electrolytes and characterized by diverse physicochemical techniques such as XRD, XPS, SEM, or N₂ adsorption. Although the perovskite structure either decomposed or failed to form using those in situ methods, the materials exhibited great catalytic activity, which can be ascribed to the strengthening of the interactions between oxides and the carbon support via C-O-M covalent bonds and to the formation of new active sites such as the MnO/Co heterointerfaces. Moreover, Co-N_x-C species are formed during the synthesis of the metal compounds over the carbon xerogel. These species possess a strong catalytic activity towards ORR. Therefore, the composites formed by synthesizing metal compounds over the carbon xerogel exhibit the best performance in the ORR, which can be ascribed to the presence of the MnO/Co heterointerfaces and Co-N_x-C species and the strong interactions between both compounds. Moreover, the small nanoparticle size leads to a higher number of active sites available for the reaction. Full article

Chitosan, alginate, and chitosan–alginate (50:50) mixed hydrogels were prepared by freeze casting, freeze-drying, and subsequent physical cross-linking. Chitosan was cross-linked with citrate and alginate with calcium ions, while the mixed gels were cross-linked with both cross-linking agents. Both cryogels and xerogels were obtained by lyophilization and drying of the hydrogels. We investigated the effect of the chemical composition and the physical state of gels on the gel structure and sorption of model dyes. Alginate and mixed gels cross-linked with Ca²⁺ ions sorbed 80–95% of cationic dye from the solutions. The chitosan gels are primarily capable of adsorbing anionic dyes, but at near-neutral pH, their capacity is lower than that of alginate gels, showing 50–60% dye sorption. In the case of alginate gels, the dye sorption capacity of xerogels, cryogels, and hydrogels was the same, but for chitosan gels, the hydrogels adsorbed slightly less dye than the dried gels. Full article

Solid-state supercapacitors with gel electrolytes have emerged as a promising field for various energy storage applications, including electronic devices, electric vehicles, and mobile phones. In this study, nanocomposite gel membranes were fabricated using the solution casting method with perfluorosulfonic acid (PFSA) ionomer dispersion, both with and without the incorporation of 10 wt.% montmorillonite (MMT). MMT, a natural clay known for its high surface area and layered structure, is expected to enhance the properties of supercapacitor systems. Manganese oxide, selected for its pseudocapacitive behavior in a neutral electrolyte, was synthesized via direct co-precipitation. The materials underwent structural and morphological characterization. For electrochemical evaluation, a two-electrode Swagelok cell was employed, featuring a carbon xerogel negative electrode, a manganese dioxide positive electrode, and a PFSA polymer membrane serving as both the electrolyte and separator. The membrane was immersed in a 1 M Na₂SO₄ solution before testing. A comprehensive electrochemical analysis of the hybrid cells was conducted and compared with a symmetric carbon/carbon supercapacitor. Cyclic voltammetric curves were recorded, and galvanostatic charge–discharge tests were conducted at various temperatures (20, 40, 60 °C). The hybrid cell with the PFSA/MMT 10 wt.% exhibited the highest specific capacitance and maintained its hybrid profile after prolonged cycling at elevated temperatures, highlighting the potential of the newly developed membrane. Full article