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Special Issue "Microporous/Mesoporous Inorganic Materials"

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Inorganic Chemistry".

Deadline for manuscript submissions: closed (31 May 2020).

Special Issue Editors

Dr. Bénédicte Lebeau
Website
Guest Editor
Equipe Matéraiux à Porosité Contrôlée, Institut de Science des Matériaux de Mulhouse, CNRS LRC 7228, Université de Haute Alsace, 68093 Mulhouse, France
Interests: mesoporous oxides; materials with hierarchized porosity; sol-gel synthesis; mechanisms of formation; organic and inorganic functionalization; shaping, encapsulation/vectorization; adsorption; catalysis; thermal insulation
Special Issues and Collections in MDPI journals
Prof. Dr. T. Jean Daou
Website1 Website2
Guest Editor
Axe Matériaux à Porosité Contrôlée (MPC), Institut de Science des Matériaux de Mulhouse (IS2M), Université de Haute Alsace (UHA), CNRS, UMR 7361, 68093 Mulhouse, France
Interests: zeolites; hierarchical materials; synthesis and characterization of porous materials; textural properties; structural properties; shaping of zeolites; molecular decontamination; energy storage or adsorption; catalysis
Special Issues and Collections in MDPI journals

Special Issue Information

Dear Colleagues,

Porous materials having inorganic or hybrid frameworks delimiting a regular porous structure are promising candidates for different applications, such as catalysis, separation, ion exchange, gas storage, molecular decontamination, etc. In particular, microporous materials and mesoporous materials have exciting properties due to the size of their pore openings, their large specific surface areas and pore volumes. Recently, another class of porous materials, called hierarchical porous materials, has emerged. These materials contain at least two different types of interconnected porosities (micro/mesopores, etc.), which are known, for example, to improve the performances of the microporous counterpart thanks to an efficient mass transfer kinetics through mesopores. Porous materials are of great scientific importance from a fundamental point of view due to their ability to interact with atoms, ions, and molecules on their sizeable interior surfaces and porosity. This growing interest in porous materials has led to progress in characterization techniques and modelling studies to better understand the structure/property relationships, in order to improve the design of tailor-made porous materials with high performances. This Special Issue proposes a state-of-the-art in recent advances made in the field of inorganic and hybrid porous materials, with a focus on:

  •       New methods for the synthesis of porous materials and the control of particle size and morphology
  •       Methods for textural and structural characterization of porous materials
  •       Shaping of porous materials (films, pellets, beads, extrudates, etc.)
  •       Known applications:
          -Molecular decontamination (water and air treatments)
          -Gas storage
          -Ion-exchange
          -Molecular sieving (molecule separation, gas purification)
          -Catalysis (biomass conversion, etc.)
  •       Emerging applications:
          -Energy storage
          -Sensors
          -Health (biomedical applications)
          -Photovoltaic

Dr. Bénédicte Lebeau
Prof. Dr. T. Jean Daou
Guest Editors

Manuscript Submission Information

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Published Papers (13 papers)

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Research

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Open AccessArticle
Efficient Removal of Volatile Organic Compounds by FAU-Type Zeolite Coatings
Molecules 2020, 25(15), 3336; https://doi.org/10.3390/molecules25153336 - 23 Jul 2020
Abstract
Silicone and pure organic binders were used to develop FAU-type zeolite coatings applied on pre-treated aluminum substrates by using a spraying method and then cured under specific conditions. The influence of the amount of binder on adhesion properties of zeolite coatings was first [...] Read more.
Silicone and pure organic binders were used to develop FAU-type zeolite coatings applied on pre-treated aluminum substrates by using a spraying method and then cured under specific conditions. The influence of the amount of binder on adhesion properties of zeolite coatings was first investigated to determine the optimum ratio between zeolite and binder. Zeolite coatings were then elaborated with a high zeolite content (between 70 and 80 wt.%) to ensure high adsorption capacities. The amount of binders involved in different zeolite coatings was sufficient to achieve interesting adhesion and cohesion properties. The accessibility of zeolite microporosity was studied by nitrogen adsorption-desorption measurements, which revealed a very small or no loss of the micropore volume for the optimized coatings. Volatile Organic Compounds (VOCs) adsorption measurements were carried out using n-hexane as probe molecule. FAU-type zeolite in powder form adsorbs 180 mg/ganhydrous zeolite, whereas the amounts of n-hexane adsorbed by zeolite coatings ranged from 131 to 175 mg/ganhydrous zeolite. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
Synthesis of Hierarchical Zeolites with Morphology Control: Plain and Hollow Spherical Beads of Silicalite-1 Nanosheets
Molecules 2020, 25(11), 2563; https://doi.org/10.3390/molecules25112563 - 31 May 2020
Cited by 1
Abstract
Binderless pure silica zeolites (zeosils) spheres and hollow spheres with a diameter of 20 µm composed of silicalite-1 nanosheets particles were prepared by pseudomorphic transformation of spherical silica beads using different temperatures (110, 130, and 150 °C) and treatment times (1–5 days) in [...] Read more.
Binderless pure silica zeolites (zeosils) spheres and hollow spheres with a diameter of 20 µm composed of silicalite-1 nanosheets particles were prepared by pseudomorphic transformation of spherical silica beads using different temperatures (110, 130, and 150 °C) and treatment times (1–5 days) in order to adapt the local dissolution rate of silica to the crystallization rate of silicalite-1 nanosheets allowing to preserve the initial morphology of the silica beads. Fully crystalline beads of 20 µm were obtained at 110 °C for 5 days, whereas hollow spheres similar in size were synthesized at higher temperatures. The crystallization process seems to begin at the outer surface of the amorphous silica beads and spreads with the time in the interior of the beads leading to a dissolution of the inner amorphous part of the beads to create zeosil hollow spheres for the highest treatment temperatures (130 and 150 °C). The dissolution rate of the inner amorphous part of the beads increases by increasing the hydrothermal treatment temperature from 130 to 150 °C. The silicalite-1 beads synthesized at 110 °C for 5 days showed to be promising for rapid molecular decontamination by adsorbing n-hexane in larger amount than the silicalite-1 conventional big crystals in powder forms. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
Influence of the Compensating Cation Nature on the Water Adsorption Properties of Zeolites
Molecules 2020, 25(4), 944; https://doi.org/10.3390/molecules25040944 - 20 Feb 2020
Cited by 3
Abstract
The influence of the compensating cation (Na+, Li+, Mg2+) nature on the water adsorption properties of LTA and FAU-type zeolites was investigated. Cation exchanges were performed at 80 °C for 2 h using 1 M aqueous solutions [...] Read more.
The influence of the compensating cation (Na+, Li+, Mg2+) nature on the water adsorption properties of LTA and FAU-type zeolites was investigated. Cation exchanges were performed at 80 °C for 2 h using 1 M aqueous solutions of lithium chloride (LiCl) or magnesium chloride (MgCl2). XRF and ICP-OES analyses indicate that the cation exchange yields reach values between 59 to 89% depending on the number of exchange cycles and the nature of the zeolite and cation, while both zeolites structures are preserved during the process, as shown by XRD and solid state NMR analyses. Nitrogen adsorption-desorption experiments indicate a higher available microporous volume when sodium cations are replaced by smaller monovalent lithium cations or by divalent magnesium cations because twice less cations are needed compared to monovalent cations. Up to 15% of gain in the available microporous volume is obtained for FAU-type zeolites exchanged with magnesium cation. This improvement facilitates the adsorption of water with an increase in the water uptake up to 30% for the LTA and FAU type zeolites exchanged with magnesium. These exchanged zeolites are promising for uses in water decontamination because a smaller amount is needed to trap the same amount of water compared to their sodium counterparts. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
Nanostructured Nickel Aluminate as a Key Intermediate for the Production of Highly Dispersed and Stable Nickel Nanoparticles Supported within Mesoporous Alumina for Dry Reforming of Methane
Molecules 2019, 24(22), 4107; https://doi.org/10.3390/molecules24224107 - 14 Nov 2019
Cited by 7
Abstract
Two routes of preparation of mesoporous Ni-alumina materials favoring the intermediate formation of nanostructured nickel-aluminate are presented. The first one involves an aluminum containing MOF precursor used as sacrificial template to deposit nickel while the second is based on a one-pot synthesis combined [...] Read more.
Two routes of preparation of mesoporous Ni-alumina materials favoring the intermediate formation of nanostructured nickel-aluminate are presented. The first one involves an aluminum containing MOF precursor used as sacrificial template to deposit nickel while the second is based on a one-pot synthesis combined to an EISA method. As shown by a set of complementary techniques, the nickel-aluminate nanospecies formed after calcination are homogeneously distributed within the developed mesoporous alumina matrices whose porous characteristics vary depending on the preparation method. A special attention is paid to electron-microscopy observations using especially STEM imaging with high chemical sensitivity and EDS elemental mapping modes that help visualizing the extremely high nickel dispersion and highlight the strong metal anchoring to the support that persists after reduction. This leads to active nickel nanoparticles particularly stable in the reaction of dry reforming of methane. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
Electrical Behavior of a Catalyst Composed of Laminar Manganese Oxide Supported on γ-Al2O3
Molecules 2019, 24(16), 2984; https://doi.org/10.3390/molecules24162984 - 16 Aug 2019
Abstract
The electrical characterization of catalysts composed of layered manganese oxide in the form of birnessite supported on γ-Al2O3, which have been successfully used in the combustion of soot, is presented. The results indicate that the electrical conduction and ion [...] Read more.
The electrical characterization of catalysts composed of layered manganese oxide in the form of birnessite supported on γ-Al2O3, which have been successfully used in the combustion of soot, is presented. The results indicate that the electrical conduction and ion conduction processes are influenced by the amount of the active phase. There was also evidence of Grotthuss-type proton conductivity favored by the presence of surface water on the exposed alumina surface. The above is supported by the porous nature of the catalyst in which the surface area varied between 125.2 ± 1.2 and 159.0 ± 1.1 m2/g, evidencing changes in the alumina surface. The conductivity, determined from measurements of impedance spectroscopy, at low frequency showed changes associated with the amount of the active phase. The values ranged from 2.61 × 10−8 ± 2.1 × 10−9 Ω−1·cm−1 (pure alumina) to 7.33 × 10−8 ± 5.9 × 10−9 Ω−1·cm−1, 7.21 × 10−8 ± 5.8 × 10−9 Ω−1·cm−1 and 4.51 × 10−7 ± 3.6 × 10−8 Ω−1·cm−1 at room temperature for catalysts with nominal active phase contents of 5.0, 10.0 and 20.0%, respectively. Such results indicate that it is possible to modulate the electrical properties with variations in the synthesis parameters. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
Incorporation of Brazilian Diatomite in the Synthesis of An MFI Zeolite
Molecules 2019, 24(10), 1980; https://doi.org/10.3390/molecules24101980 - 23 May 2019
Cited by 3
Abstract
The need for greener procedures is a fact to reduce residues, to decrease industrial costs, and to accomplish the environmental agreements. In an attempt to address this question, we propose the addition of a natural resource, Brazilian diatomite, to an MFI zeolite traditional [...] Read more.
The need for greener procedures is a fact to reduce residues, to decrease industrial costs, and to accomplish the environmental agreements. In an attempt to address this question, we propose the addition of a natural resource, Brazilian diatomite, to an MFI zeolite traditional synthesis. We have characterized the resulting product with different techniques, such as X-ray diffraction, microscopy, and gas sorption, and, afterwards, we evaluate the greenness of the process by the Green Star method. The results were promising: We obtained the desired topology in the form of small crystallites aggregated and a pore diameter of 0.8 nm. In conclusion, the product has the necessary characteristics for an adsorption or catalytic future tests and escalation to industrial production. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
First-Principles Study of AlPO4-H3, a Hydrated Aluminophosphate Zeotype Containing Two Different Types of Adsorbed Water Molecules
Molecules 2019, 24(5), 922; https://doi.org/10.3390/molecules24050922 - 06 Mar 2019
Cited by 4
Abstract
Porous aluminophosphate zeotypes (AlPOs) are promising materials for heat transformation applications using water as a working fluid. Two “types” of adsorbed water molecules can be distinguished in hydrated AlPOs: Water molecules adsorbed in the direct proximity of framework aluminium atoms form bonds to [...] Read more.
Porous aluminophosphate zeotypes (AlPOs) are promising materials for heat transformation applications using water as a working fluid. Two “types” of adsorbed water molecules can be distinguished in hydrated AlPOs: Water molecules adsorbed in the direct proximity of framework aluminium atoms form bonds to these Al atoms, with the coordination number of Al increasing from four to five or six. The remaining water molecules that are adsorbed in other parts of the accessible pore space are not strongly bonded to any framework atom, they interact with their environment exclusively through hydrogen bonds. The APC-type small-pore aluminophosphate AlPO4-H3 contains both types of H2O molecules. In the present work, this prototypical hydrated AlPO is studied using dispersion-corrected density functional theory (DFT) calculations. After validating the computations against experimental crystal structure and Raman spectroscopy data, three interrelated aspects are addressed: First, calculations for various partially hydrated models are used to establish that such partially hydrated phases are not thermodynamically stable, as the interaction with the adsorbed water molecules is distinctly weaker than in fully hydrated AlPO4-H3. Second, IR and Raman spectra are computed and compared to those of the dehydrated analogue AlPO4-C, leading to the identification of a few “fingerprint” modes that could be used as indicators for the presence of Al-coordinated water molecules. Finally, DFT-based molecular dynamics calculations are employed to study the dynamics of the adsorbed water molecules. All in all, this in-depth computational study of AlPO4-H3 contributes to the fundamental understanding of hydrated AlPOs, and should therefore provide valuable information for future computational and experimental studies of these systems. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
A Spectroscopic Study of Tautomeric Equilibrium of Salicylideneaniline in ZSM-5 Zeolites
Molecules 2019, 24(4), 795; https://doi.org/10.3390/molecules24040795 - 22 Feb 2019
Abstract
Salicylideneaniline (SA) sorbed in cation-exchanged M-ZSM-5 (M = H+, Li+, Na+, K+, Rb+, Cs+ and Zn2+) zeolites was studied by spectroscopic techniques assisted by quantum-chemical calculations. The nature of extra-framework [...] Read more.
Salicylideneaniline (SA) sorbed in cation-exchanged M-ZSM-5 (M = H+, Li+, Na+, K+, Rb+, Cs+ and Zn2+) zeolites was studied by spectroscopic techniques assisted by quantum-chemical calculations. The nature of extra-framework cations present in the zeolite void was found to affect the spectral signature of the sorbed SA molecule that points to the shift of tautomeric equilibrium between the enol and keto forms. Small size cations, such as H+ and Li+, stabilize a cis-keto SA tautomer along with a enol one in the zeolite structure. The calculations indicate that the sorbed cis-keto tautomer may have the dipole large enough to be considered as a zwitterion. New features appearing in the spectra with the increase of the cation size were attributed to the presence of trans-keto SA tautomer, which up to now has been observed only in time-resolved spectroscopic experiments. A strong interaction of the molecule with cations in Zn-ZSM-5 zeolite results in the chelation of enol SA with the divalent Zn2+ ions. The results of the study suggest that the tautomeric equilibrium of molecules belonging to the Schiff base family can be tuned by the confinement in the nanoporous materials via a choice of topology of zeolite framework and the nature of extra-framework cations. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
Synthesis of Mesoporous TiO2/Boron-Doped Diamond Photocatalyst and Its Photocatalytic Activity under Deep UV Light (λ = 222 nm) Irradiation
Molecules 2018, 23(12), 3095; https://doi.org/10.3390/molecules23123095 - 27 Nov 2018
Cited by 6
Abstract
There is a need for highly efficient photocatalysts, particularly for water purification. In this study, we fabricated a mesoporous TiO2 thin film on a boron-doped diamond (BDD) layer by a surfactant-assisted sol-gel method, in which self-assembled amphiphilic surfactant micelles were used as [...] Read more.
There is a need for highly efficient photocatalysts, particularly for water purification. In this study, we fabricated a mesoporous TiO2 thin film on a boron-doped diamond (BDD) layer by a surfactant-assisted sol-gel method, in which self-assembled amphiphilic surfactant micelles were used as an organic template. Scanning electron microscopy revealed uniform mesopores, approximately 20 nm in diameter, that were hexagonally packed in the TiO2 thin film. Wide-angle X-ray diffraction and Raman spectroscopy clarified that the framework crystallized in the anatase phase. Current–voltage (I–V) measurements showed rectification features at the TiO2/BDD heterojunction, confirming that a p–n hetero-interface formed. The as-synthesized mesoporous TiO2/BDD worked well as a photocatalyst, even with a small volume of TiO2 (15 mm × 15 mm × c.a. 1.5 µm in thickness). The use of deep UV light (λ = 222 nm) as a light source was necessary to enhance photocatalytic activity, due to photo-excitation occurring in both BDD and TiO2. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessFeature PaperArticle
Synthesis of Binderless ZK-4 Zeolite Microspheres at High Temperature
Molecules 2018, 23(10), 2647; https://doi.org/10.3390/molecules23102647 - 16 Oct 2018
Cited by 5
Abstract
Binderless zeolite macrostructures in the form of ZK-4 microspheres were prepared using anion-exchange resin beads as shape-directing macrotemplates. The particles were synthesized under hydrothermal conditions at different temperatures and treatment times. The influence of the different synthesis parameters was investigated by X-ray diffraction, [...] Read more.
Binderless zeolite macrostructures in the form of ZK-4 microspheres were prepared using anion-exchange resin beads as shape-directing macrotemplates. The particles were synthesized under hydrothermal conditions at different temperatures and treatment times. The influence of the different synthesis parameters was investigated by X-ray diffraction, scanning electron microscopy, fluorescence X, nitrogen adsorption measurements and 29Si solid-state NMR. Fully crystalline spheres similar in size and shape to the original resin beads were obtained by a hydrothermal treatment at the highest temperatures (150–180 °C) for a short treatment time of 24 h. The synthesized microspheres showed to be promising in the molecular decontamination of volatile organic compounds (VOCs). Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessArticle
Influence of Synthesis Method on LTA Time-Dependent Stability
Molecules 2018, 23(9), 2122; https://doi.org/10.3390/molecules23092122 - 23 Aug 2018
Cited by 7
Abstract
Time-stability of LTA zeolite formed by hydrothermal method with or without the action of ultrasonic irradiation was investigated by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). The results show that 6 months after the synthesis by hydrothermal process with continuous sonication, [...] Read more.
Time-stability of LTA zeolite formed by hydrothermal method with or without the action of ultrasonic irradiation was investigated by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). The results show that 6 months after the synthesis by hydrothermal process with continuous sonication, LTA evolves into a more stable sodalite, whereas no differences are detected 12 months after LTA synthesis by conventional pre-fused hydrothermal process. These data confirm that using the two approaches, different mechanisms control both zeolite crystallization and time-stability of the newly-formed mineral at solid state. The results are particularly important in the light of the synthetic zeolite application. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Review

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Open AccessReview
Energetic Performance of Pure Silica Zeolites under High-Pressure Intrusion of LiCl Aqueous Solutions: An Overview
Molecules 2020, 25(9), 2145; https://doi.org/10.3390/molecules25092145 - 04 May 2020
Abstract
An overview of all the studies on high-pressure intrusion—extrusion of LiCl aqueous solutions in hydrophobic pure silica zeolites (zeosils) for absorption and storage of mechanical energy is presented. Operational principles of heterogeneous lyophobic systems and their possible applications in the domains of mechanical [...] Read more.
An overview of all the studies on high-pressure intrusion—extrusion of LiCl aqueous solutions in hydrophobic pure silica zeolites (zeosils) for absorption and storage of mechanical energy is presented. Operational principles of heterogeneous lyophobic systems and their possible applications in the domains of mechanical energy storage, absorption, and generation are described. The intrusion of LiCl aqueous solutions instead of water allows to considerably increase energetic performance of zeosil-based systems by a strong rise of intrusion pressure. The intrusion pressure increases with the salt concentration and depends considerably on zeosil framework. In the case of channel-type zeosils, it rises with the decrease of pore opening diameter, whereas for cage-type ones, no clear trend is observed. A relative increase of intrusion pressure in comparison with water is particularly strong for the zeosils with narrow pore openings. The use of highly concentrated LiCl aqueous solutions instead of water can lead to a change of system behavior. This effect seems to be related to a lower formation of silanol defects under intrusion of solvated ions and a weaker interaction of the ions with silanol groups of zeosil framework. The influence of zeosil nanostructure on LiCl aqueous solutions intrusion–extrusion is also discussed. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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Open AccessReview
Mesoporous Silica-Based Materials for Electronics-Oriented Applications
Molecules 2019, 24(13), 2395; https://doi.org/10.3390/molecules24132395 - 28 Jun 2019
Cited by 8
Abstract
Electronics, and nanoelectronics in particular, represent one of the most promising branches of technology. The search for novel and more efficient materials seems to be natural here. Thus far, silicon-based devices have been monopolizing this domain. Indeed, it is justified since it allows [...] Read more.
Electronics, and nanoelectronics in particular, represent one of the most promising branches of technology. The search for novel and more efficient materials seems to be natural here. Thus far, silicon-based devices have been monopolizing this domain. Indeed, it is justified since it allows for significant miniaturization of electronic elements by their densification in integrated circuits. Nevertheless, silicon has some restrictions. Since this material is applied in the bulk form, the miniaturization limit seems to be already reached. Moreover, smaller silicon-based elements (mainly processors) need much more energy and generate significantly more heat than their larger counterparts. In our opinion, the future belongs to nanostructured materials where a proper structure is obtained by means of bottom-up nanotechnology. A great example of a material utilizing nanostructuring is mesoporous silica, which, due to its outstanding properties, can find numerous applications in electronic devices. This focused review is devoted to the application of porous silica-based materials in electronics. We guide the reader through the development and most crucial findings of porous silica from its first synthesis in 1992 to the present. The article describes constant struggle of researchers to find better solutions to supercapacitors, lower the k value or redox-active hybrids while maintaining robust mechanical properties. Finally, the last section refers to ultra-modern applications of silica such as molecular artificial neural networks or super-dense magnetic memory storage. Full article
(This article belongs to the Special Issue Microporous/Mesoporous Inorganic Materials)
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