Mesoporous Silica-based Materials Research Articles

Novel process for facile preparation of mesoporous silica-based materials with controllable pore structure from coal fly ash

Extraction of silica from fly ash to produce mesoporous silica materials is one of the most important utilization approaches. Mesoporous silica could not be synthesized on a large-scale by conventional sol-gel method. In this paper, facile preparation of mesoporous silica with controllable pore structure from fly ash by the template-free process via two steps of mineral phase transformation and selective acid etching was proposed. The influence of crystalline structure and acid etching degree on structure of as-synthesized mesoporous silica materials was revealed, as well as mechanism of crystalline structure transformation and pore structure formation. The results show that mullite and quartz could be transformed into acid-soluble kaliophilite when fly ash reacted with K2CO3 at temperature of 800–1100 °C. The hexagonal kaliophilite would be transformed into orthorhombic KAlSiO4–O1 phase when the temperature is controlled at 1100 °C. Mesoporous silica with specific surface area of 475.93 m2/g and 642.57 m2/g could be synthesized from activated fly ash with kaliophilite and KAlSiO4–O1 phase crystalline structure. By controlling the degree of acid etching, mesoporous silica materials with different pore structures can be obtained. This paper provides a cost-effective and large-scale process for the preparation of mesoporous silica materials with controllable pore structure from solid waste fly ash.

Synthesis, Characterizations, and Recent Applications of the Silica-based Mobil Composition of Mesoporous Material: A Review

Silica-based mesoporous materials are a class of porous materials with unique characteristics such as ordered pore structure, large surface area, and large pore volume. This review covers the different types of porous material (zeolite and mesoporous) and the physical properties of mesoporous materials that make them valuable in industry. Mesoporous materials can be divided into two groups: silica-based mesoporous materials and non-silica-based mesoporous materials. The most well-known family of silica-based mesoporous materials is the Mesoporous Molecular Sieves family, which attracts attention because of its beneficial properties. The family includes three members that are differentiated based on their pore arrangement. In this review, the major applications of the Mobil Mesoporous Molecular Sieves family, such as catalysts, adsorbents, and drug delivery agents, have been surveyed. Furthermore, the synthesis of the Mesoporous Molecular Sieves materials, the silica sources, the importance of templates, and the mechanisms of the synthesis are discussed herein. Members of this material family are characterized by many physicochemical properties that are closely related to their high silica content, crystalline structure, and pore arrangement. Commonly, the members of this family have large surface areas, high pore volumes, small pore sizes, and narrow and uniform particle size distributions. These properties enable numerous industrial applications and opportunities for scientific studies to further develop existing materials or manufacture new ones.

Redox Properties of TiO2 Thin Films Grown on Mesoporous Silica by Atomic Layer Deposition.

The redox properties of titania films grown by ALD on SBA-15, a silica-based mesoporous material, were characterized as a function of thickness (that is, the number of ALD cycles used). 29Si CP/MAS NMR helped to identify the nature of the surface species that form in the initial stages of deposition, and infrared absorption spectroscopy was used to follow the transition from silica to titania surfaces. The reducibility of the titania sites by CO and H2 was studied ex situ using EPR and in situ with ambient-pressure XPS. It was determined that the titania ALD films are amorphous and easier to reduce than crystalline titania and that the reduction is reversible. A transition in the nature of the surface was also observed, with unique mixed Si-O-Ti sites forming during the first few ALD cycles and a more typical titania surface progressively developing as the film grows in thickness.

Tailoring of Mesoporous Silica-Based Materials for Enhanced Water Pollutants Removal.

The adsorptive performance of mesoporous silica-based materials towards inorganic (metal ions) and organic (dyes) water pollutants was investigated. Mesoporous silica materials with different particle size, surface area and pore volume were prepared and tailored with different functional groups. These materials were then characterised by solid-state techniques, namely vibrational spectroscopy, elemental analysis, scanning electron microscopy and nitrogen adsorption-desorption isotherms, allowing the successful preparation and structural modifications of the materials to be confirmed. The influence of the physicochemical properties of the adsorbents towards the removal of metal ions (Ni2+, Cu2+ and Fe3+) and organic dyes (methylene blue and methyl green) from aqueous solutions was also investigated. The results reveal that the exceptionally high surface area and suitable ζ-potential of the nanosized mesoporous silica nanoparticles (MSNPs) seem to favour the adsorptive capacity of the material for both types of water pollutants. Kinetic studies were performed for the adsorption of organic dyes by MSNPs and large-pore mesoporous silica (LPMS), suggesting that the process follows a pseudo-second-order model. The recyclability along consecutive adsorption cycles and the stability of the adsorbents after use were also investigated, showing that the material can be reused. Current results show the potentialities of novel silica-based material as a suitable adsorbent to remove pollutants from aquatic matrices with an applicability to reduce water pollution.

The role of porosity and acidity in the catalytic upcycling of polyethylene

Plastics have become fundamental and widespread materials in our everyday life. Nowadays, the most demanded plastics are polyolefins, accounting for nearly half of the Global plastic production. However, the end-of-life disposal of these materials is an issue inevitably connected to their increased production. Among chemical recycling techniques, the most thoroughly investigated process is the catalytic pyrolysis, showing a vast panorama of different set-ups optimized for the major production of either gaseous or liquid compounds. In this contribution a series of mesoporous silica-based materials, either pure SiO2 or substituted with Zr and Al, were systematically synthetized varying both porous framework and surface acidity, in the attempt of rationalizing the effect of each parameter (deeply characterized by physico-chemical methods) on the catalytic pyrolysis of linear low-density polyethylene (LLDPE). The synthetized materials together with some zeolites and aluminas reference samples were tested towards LLDPE degradation in a batch reactor set-up optimized for the formation and accumulation of the gaseous compounds, coupled with IR spectroscopy for in situ monitoring the evolution of the most abundant species (mostly propylene and branched C4-C6 olefins, together with a minor fraction of ethylene and short hydrocarbons). This work points out the necessity of the presence of Brønsted acid sites for a good activity (in terms of both the yield of gaseous products and lowering of the process temperature), but it also reveals a non-negligible role of the Lewis acid sites and it warns about the importance of controlling not only the amount of acid sites but also their strength.

Surface area per volumetric loading and its practical significance

The surface area of porous materials is a widely-used parameter in catalysis and adsorption. The most-commonly applied model, Brunauer–Emmett–Teller (BET), bases the parameter to the mass of material. Though the model does have its limitations, comparisons among materials are widely done to rank them from low to high surface areas, and to make correlations with other properties. However, in practical terms volume is often more appropriate since the design of reactors and adsorption columns aims at minimizing their volume. Thus, in such cases the surface areas can be better expressed per material bed volume using the bulk density. In this communication, we discuss the concept of volumetric surface area as m2/cm3MatBed, showing remarkable new insights. We applied this concept to two mesoporous silica-based materials with comparable pore size and C values. A material which was far superior in terms of conventional surface area (561 versus 227 m2/gMat), they both became comparable in terms of m2/cm3MatBed (ca. 110 both) due to the much lower density of the former material. In other words, being superior in gravimetric terms does not guarantee to be volumetrically superior. The results highlight the importance of considering the material bulk density when comparing surface areas of porous materials for applications where volume is critical.

Biological Use of Nanostructured Silica-Based Materials Functionalized with Metallodrugs: The Spanish Perspective.

Since the pioneering work of Vallet-Regí's group on the design and synthesis of mesoporous silica-based materials with therapeutic applications, during the last 15 years, the potential use of mesoporous silica nanostructured materials as drug delivery vehicles has been extensively explored. The versatility of these materials allows the design of a wide variety of platforms that can incorporate numerous agents of interest (fluorophores, proteins, drugs, etc.) in a single scaffold. However, the use of these systems loaded with metallodrugs as cytotoxic agents against different diseases and with distinct therapeutic targets has been studied to a much lesser extent. This review will focus on the work carried out in this field, highlighting both the pioneering and recent contributions of Spanish groups that have synthesized a wide variety of systems based on titanium, tin, ruthenium, copper and silver complexes supported onto nanostructured silica. In addition, this article will also discuss the importance of the structural features of the systems for evaluating and modulating their therapeutic properties. Finally, the most interesting results obtained in the study of the potential therapeutic application of these metallodrug-functionalized silica-based materials against cancer and bacteria will be described, paying special attention to preclinical trials in vivo.

Enhanced adsorption-catalysis combination for the removal of sulphur from fuels using polyoxometalates supported on amphipathic hybrid mesoporous silica nanoparticles.

Polyoxometalate (POM) mesoporous silica-based materials with a low POM loading have been designed with hydrophilic and hydrophobic properties. These materials act as powerful heterogeneous catalysts in oxidative desulfurization (ODS), owing to their ability to adsorb both H2O2 and sulphur-containing compounds from the model oil simultaneously. The formation of charge transfer salts through ion pair interaction with a choline functionality, available on the hybrid silica support, affords robust and recyclable heterogeneous catalysts for the ODS process under mild conditions (45 min and 40 °C). Besides, the nature of the polyoxometalate anions is highly dependent on the characteristics of the silica surface. The masking of silanol groups present on the silica surface using silylating agents, with diverse reactivity and steric hindrance, influences the silica surface-heteropolyanion interactions, as well as heteropolyanion-heteropolyanion interactions. In addition, it modifies the hydrophobic properties of the surface, which is a determining factor in the adsorption properties of non-polar dibenzothiophene (DBT) by the catalysts. Adsorption, an anterior step to the oxidation reaction, has been demonstrated to be key to the superior activity of POM-SiMe3-Chol-MSN, where the silanol groups have been capped by trimethylsilyl groups. For the first time, and to better understand POM-surface and POM-POM anion interactions, an extensive characterization of the materials has been performed using 13C, 31P, and 95Mo MAS NMR spectroscopy and solid-state electrochemical techniques, among others.

A reflux system for SBA-15 synthesis for the selective hydrogenation of cinnamyl aldehyde

Silica-based mesoporous materials, such as SBA-15, are important supports in the field of catalysis due to their ordered pore channels.

Template-free facile preparation of mesoporous silica from fly ash for shaped composite phase change materials

Traditional sol-gel template preparation method for mesoporous silica has limited its large-scale production and applications due to low production quantity, complex preparation process and high cost. In this paper, we proposed a novel template-free process to prepare mesoporous silica-based materials by acid etching of activated fly ash to improve the support performance for shaped composite phase change materials. The mechanisms of mineral phase transformation and pore formation during preparation of mesoporous silica from fly ash were systematically investigated, and the structure, morphology and thermal properties of as-prepared shaped composite phase change materials (SCPCMs) were characterized and analyzed. The results show that stable mullite and quartz could be transformed into potassium aluminosilicate minerals after calcined with K2CO3, and mesoporous silica-based materials with different pore shapes and specific surface area ranging from 330 to 490 m2/g could be prepared from as-calcined fly ash. The PEG/MS-I (ink bottle-shaped material) achieved the largest loading efficiency of 64.88%, and the highest melting phase change enthalpy of 88.38 J/g, which is 30.7% and 57.7% higher than that of PEG/MS-S (silt-shaped material) and PEG/MS-W (wedge-shaped material), respectively. After 20 thermal cycles, the loss of melting enthalpy for PEG/MS-I was only 3%, and the thermal energy storage and release time were 23.1% and 17.0% shorter than that of pure PEG, respectively. In all, the PEG/MS-I composite exhibited reliable thermal storage performance and temperature regulation ability, which provides the feasibility of application of fly ash-derived composite phase change material in energy storage field.

Novel Antitumor Agents Based on Fluorescent Benzofurazan Derivatives and Mesoporous Silica

Two novel fluorescent mesoporous silica-based hybrid materials were obtained through the covalent grafting of [4-hydrazinyl-7-nitrobenz-[2,1,3-d]-oxadiazole (NBDH) and N1-(7-nitrobenzo[c][1,2,5]-oxadiazol-4-yl) benzene-1,2-diamine (NBD-PD), respectively, inside the channels of mesoporous silica SBA-15. The presence of fluorescent organic compounds (nitrobenzofurazan derivatives) was confirmed by infrared spectroscopy (IR), X-ray photoelectron spectroscopy (XPS), thermal analysis (TG), and fluorescence spectroscopy. The nitrogen physisorption analysis showed that the nitrobenzofurazan derivatives were distributed uniformly on the internal surface of SBA-15, the immobilization process having a negligible effect on the structure of the support. Their antioxidant activity was studied by measuring the ability to reduce free radicals DPPH (free radical scavenging activity), in order to formulate potential applications of the materials obtained. Cytotoxicity of the newly synthesized materials, SBA-NBDH and SBA-NBD-PD, was evaluated on human B16 melanoma cells. The morphology of these cells, internalization and localization of the investigated materials in melanoma and fibroblast cells were examined through fluorescence imaging. The viability of B16 (3D) spheroids after treatment with SBA-NBDH and SBA-NBD-PD was evaluated using MTS assay. The results showed that both materials induced a selective antiproliferative effect, reducing to various degrees the viability of melanoma cells. The observed effect was enhanced with increasing concentration. SBA-NBD-PD exhibited a higher antitumor effect compared to SBA-NBDH starting with a concentration of 125 µg/mL. In both cases, a significantly more pronounced antiproliferative effect on tumor cells compared to normal cells was observed. The viability of B16 spheroids dropped by 40% after treatment with SBA-NBDH and SBA-NBD-PD at 500 µg/mL concentration, indicating a clear cytotoxic effect of the tested compounds. These results suggest that both newly synthesized biomaterials could be promising antitumor agents for applications in cancer therapy.

Synthesis and characteristics of mesoporous carbon catalysts via sulfonation process from surfactant residue and their catalytic properties toward gas-phase ethanol dehydrogenation

BackgroundThe several mesoporous materials are captive for applying in the different catalytic application due to its unique characteristics, which directly affected to the different selectivity of catalytic activity. This research aims to consider the possibility of the synthesis, characteristics, and catalytic activity of the different mesoporous carbon materials (SBA-15-C, MCF-C, KIT-6-C, and TMS-C) derived from the corresponding mesoporous silica materials (SBA-15, MCF, KIT-6, and TMS). MethodsMesoporous silica-based materials such as SBA-15, TMS, MCF, and KIT-6 were straightly synthesized and transformed as silica-based materials to mesoporous carbon-based materials denoted as SBA-15/C, TMS/C, MCF/C, and KIT-6/C using the surfactant residue with sulfuric acid as sulfonation process in order to enhance the physicochemical properties. In addition, these carbon catalysts were compared up on characteristics and catalytic performance towards ethanol dehydrogenation to convert ethanol into acetaldehyde. Significant findingsIt revealed that these mesoporous silica-based materials were successfully converted to the promising mesoporous carbon-based materials having appropriate physicochemical properties including acid-base properties owing to the significant existence of the carbon source. The MCF/C exhibited remarkable catalytic activity than any other carbon materials on ethanol dehydrogenation. Moreover, MCF/C is also stable toward ethanol dehydrogenation along the extensive time of the operation with behavioral recyclability. Thus, MCF/C is captivating as a potential catalyst for ethanol dehydrogenation to acetaldehyde owing to the appropriate physicochemical characteristic of the well-defined mesoporous carbon catalyst

Silica-based fibers with axially aligned mesopores from chitin self-assembly and sol-gel chemistry

Polysaccharide nanorods (chitin, cellulose) can be used as colloidal templates to form silica-based mesoporous materials by combining self-assembly and sol-gel chemistry. Chitin nanorods are chosen here for their self-assembly properties, facile preparation from natural resources, and because of the complexing properties of the free amino groups at their surface in view of further functionalization. Electrospinning of ethanolic co-suspensions, containing the chitin nanorods as pore templates, siloxane oligomers as silica precursors and polyvinylpyrrolidone (PVP) as spinning polymer, allows for forming mats of hybrid organic-inorganic fibers with diameters in the 200–300 nm range. The relative proportions of each component can be adjusted to meet specific characteristics (e.g. micro-/mesoporosity ratio). After calcination, the fibers present an open porosity studied by TEM and N2 volumetry. Elongated mesopores (100–200 nm long, 2–4 nm wide) are created by individual chitin monocrystals forming the nanorods. They are highly oriented along the fibers' axes with orientational order parameters P2 > 0.95 for volume chitin contents φchitin* ≥ 0.2. Additional microporosity is provided by the removal of the spinning polymer, PVP. Complementary viscosity measurements on the initial co-suspensions allow discussing the interactions between colloids and their possible impact on the materials’ textures observed. The introduction of a monomeric Ti4+ precursor in the co-suspensions leads to isolated and tetrahedral Ti units, distributed in the calcined porous silica fibers and possibly close to the pores surface. In addition, preliminary investigations on processing the fibers with a Zn xanthate as ZnS precursor leads to carbonized fibers with nanoparticles and a Zn/S molar ratio close to 1.

Functional mesoporous silica decorated with Ag nanoparticles as chemo-photothermal agents

This work reports the synthesis, characterization, and evaluation of the photothermal effect of silica-based mesoporous materials (SBA-15), functionalized and decorated with silver nanoparticles (AgNP) for photothermal analysis and drug delivery applications. The synthesis of SBA-15 occurred by the hydrothermal method following functionalization with APTS amino silanes, resulting in the SBA15-NH2 sample. The AgNP were synthesized by reduction method, using hemiaminal groups on the surface of SBA15-NH2 modifiers as reduction agents (SBA15-xAg with x = 4, and 10 mM of AgNO3). FTIR, XRD, N2 Sorption, SEM, TEM, zeta potential, diffuse reflectance, and UV–Vis spectroscopy characterized the materials. The samples were explored in applications such as photothermal agents and drug delivery. The photothermal analysis showed temperature variations above 22 °C. Besides, most suspensions prepared exhibit good photothermal stability. These features indicate that materials are promising as photothermal agents. The release tests indicated that only the SBA15-4Ag sample showed an increasing trend in curcumin release after being exposed to a 785 nm laser. It confirms that the smaller amount of silver nanospheres in the aforementioned sample was more effective in propagating the heat. Therefore, the results showed promising materials as nano heaters, especially the SBA15-4 Ag sample, which presents the good formation of silver nanorods, high heat degree, high photothermal efficiency values (η), and time-dependent.

Anchoring of 10-phenylphenothiazine to mesoporous silica materials: A water compatible organic photocatalyst for the degradation of pollutants

• An organic photocatalyst (PTH) has been anchored onto mesoporous silica-based materials. • The PTH-containing materials have been fully characterized by different methods. • The photocatalytic activity of the materials has been tested for degradation of pollutants in water. • The SBA-15-AP-PTH was the most efficient for degrading acetaminophen and diclofenac. The application of organic photocatalysts towards the oxidation of pollutants in water is hampered by different limitations such as their insolubility in the media. Herein, we report that the grafting of a photo-organocatalyst into mesoporous silica materials is an ideal approach to obtain effective catalysts. Thereby, the photocatalyst 10-phenylphenothiazine (PTH) was easily anchored into three different mesoporous silica-based materials (MSN, MSU-2 and SBA-15) with different particle sizes and pore sizes through an amide bond formation. The materials were characterized using IR analysis, solid-state X-ray diffraction, porosity and microscopy (SEM and TEM) techniques, showing that PTH is immobilized inside the pores of the materials and its optical properties are maintained after the anchoring. Although homogeneous PTH was inactive in water media, the three photocatalytic materials were active for the degradation of pollutants. SBA-15-AP-PTH exhibited the highest catalytic performance towards the degradation of acetaminophen and diclofenac under solar irradiation, finding in this manner a new strategy for the decontamination of pollutants.

APTES-Modified SBA-15 as a Non-Toxic Carrier for Phenylbutazone.

Improvement of the bioavailability of poorly soluble medicinal substances is currently one of the major challenges for pharmaceutical industry. Enhancing the dissolution rate of those drugs using novel methods allows to increase their bioavailability. In recent years, silica-based mesoporous materials have been proposed as drug delivery systems that augment the dissolution rate. The aim of this study was to analyse the influence of phenylbutazone adsorption on SBA-15 on its dissolution rate. Moreover, we examined the cytotoxicity of the analyzed silica. The material was characterized by SEM, TEM, DSC, 1H-NMR, XRD, and FT-IR. The phenylbutazone did not adsorb on unmodified SBA-15, while the adsorption on APTES-modified SBA-15 resulted in 50.43 mg/g of loaded phenylbutazone. Phenylbutazone adsorbed on the APTES-modified SBA-15 was then released in the hydrochloric acidic medium (pH 1.2) and phosphate buffer (pH 7.4) and compared to the dissolution rate of the crystalline phenylbutazone. The release profiles of the amorphous form of adsorbed phenylbutazone are constant in different pH, while the dissolution rate of the crystalline phenylbutazone depends on the pH. The cytotoxicity assays were performed using the Caco-2 cell line. Our results indicate that the analyzed material ensured phenylbutazone adsorption in an amorphous state inside the mesopores and increased its dissolution rate in various pH levels. Furthermore, the cytotoxicity assay proved safety of studied material. Our study demonstrated that APTES-modified SBA-15 can serve as a non-toxic drug carrier that improves the bioavailability of phenylbutazone.

The Role of Transmission Electron Microscopy in the Early Development of Mesoporous Materials for Tissue Regeneration and Drug Delivery Applications.

For the last 20 years, silica-based mesoporous materials have provided a sound platform for the development of biomedical technology applied to tissue engineering and drug delivery. Their unique structural and textural characteristics, chiefly, the ordered distribution of homogeneous and tunable pores with high surface areas and large pore volume, and their excellent biocompatibility provide an excellent starting point for bone tissue regeneration on the mesoporous surface, and also to load species of interest inside the pores. Adequate control of the synthesis conditions and functionalization of the mesoporous surface are critical factors in the design of new systems that are suitable for use in specific medical applications. Simultaneously, the use of appropriate characterization techniques in the several stages of design and manufacture of mesoporous particles allows us to ascertain the textural, structural and compositional modifications induced during the synthesis, functionalization and post-in vitro assays processes. In this scenario, the present paper shows, through several examples, the role of transmission electron microscopy and associated spectroscopic techniques in the search for useful information in the early design stages of mesoporous systems, with application in the fields of tissue regeneration and drug delivery systems.

Nanoantibiotics Based in Mesoporous Silica Nanoparticles: New Formulations for Bacterial Infection Treatment.

This review focuses on the design of mesoporous silica nanoparticles for infection treatment. Written within a general context of contributions in the field, this manuscript highlights the major scientific achievements accomplished by professor Vallet-Regí’s research group in the field of silica-based mesoporous materials for drug delivery. The aim is to bring out her pivotal role on the envisage of a new era of nanoantibiotics by using a deep knowledge on mesoporous materials as drug delivery systems and by applying cutting-edge technologies to design and engineer advanced nanoweapons to fight infection. This review has been divided in two main sections: the first part overviews the influence of the textural and chemical properties of silica-based mesoporous materials on the loading and release of antibiotic molecules, depending on the host–guest interactions. Furthermore, this section also remarks on the potential of molecular modelling in the design and comprehension of the performance of these release systems. The second part describes the more recent advances in the use of mesoporous silica nanoparticles as versatile nanoplatforms for the development of novel targeted and stimuli-responsive antimicrobial nanoformulations for future application in personalized infection therapies.

Surface functionalization of handleable silica-based mesoporous materials for CO2 sequestration: Synthesis, characterization and performance.

Two different types of silica monolith based on commercial hydrophobic Aerosil200 and hydrophilic Sipernat320 (Evonik) were successfully covalently functionalized with different amines as CO2 sequestrants. 3-aminopropyltriethoxysilane (AMPS) was used for a first functionalization and applied as it is or as linker to extend the chain length with diglycine (diGly) and triglycine (triGly). The physico-chemical characterization of the samples comprehends nitrogen adsorption at -196 °C to determine surface area and porosity and thermogravimetric analysis (TGA) to evaluate the thermal stability of the materials and quantify the extent of functionalization. CO2 and N2 adsorption microcalorimetry, coupled with FTIR spectroscopy, was used to evaluate the ability of the materials to selectively sequestrate CO2 against N2 in post-combustion procedures and the reversibility of the process. The comparison with a powdery commercial activated carbon, taken as reference, evidences the good adsorption capacity (comparable to that of the carbon reference) of monoliths from Sipernat 320 bringing a short aliphatic chain and terminal -NH2 groups (more than 700 μmol/g of CO2 sequestrated at 30 °C), and the advantages in term of easy storage and recoverability, with respect to powdery adsorbents.

Rapid pore expansion of mesoporous silica-based materials using microwave irradiation and pore swelling agents

In the present work we analyze the use of microwave radiation in the presence of pore swelling agents as a post-synthesis treatment for expanding the pore size of non-calcined SiO2-based mesoporous materials. In comparison with traditional hydrothermal treatments, using microwaves decreases significantly the time required for this process and is compatible with both ionic and non-ionic surfactant pore templates (e.g. cetyltrimethylammonium bromide (CTAB) and polypropyleneglycol-based surfactants). The evolution of the mesostructural parameters has been followed with small angle X-ray scattering (SAXS), X-ray diffraction (XRD), field-emission Scanning electron microscopy (FESEM) and N2 porosimetry. In particular, this strategy allows an easy approach for post-processing non-calcined templated siliceous materials and tailoring their final pore dimensions.