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Sol-Gel Chemistry. From Molecule to Functional Materials
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Sol-Gel Chemistry. From Molecule to Functional Materials

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

Deadline for manuscript submissions: closed (31 March 2020) | Viewed by 90149

Special Issue Editors

Prof. Dr. Ahmad Mehdi

E-Mail Website
Guest Editor
Institut Charles Gerhardt Montpellier, Montpellier, France
Interests: molecular chemistry; hybrid materials; sol-gel; surface modification; materials for health
Prof. Dr. Sébastien Clément

E-Mail Website
Guest Editor
Institut Charles Gerhardt, Université de Montpellier, Montpellier, France
Interests: conjugated materials; molecular self-assembly; organic electronic; therapy
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

One of the main challenges in materials science is to find effective strategies to organize the matter in terms of properties: Chemical, physical, etc. In this respect, bottom up approaches based on the self-assembly of molecules at the nanometric scale to form larger structures need to be considered. In particular, the sol-gel process (called inorganic polymerization) has emerged as one of the most important routes for preparing organized materials. It is, thus, important for Molecules to dedicate a Special Issue to this process, since it is perfectly compatible with all kinds of chemistry. This Special Issue will contain contributions discussing all the aspects that are broadly indicated by the keywords. Reviews articles by experts in the field of sol-gel, organosilica, porous hybrid materials and self-assembly will be welcome.

Prof. Ahmad Mehdi
Dr. Sébastien Clément
Guest Editors

Manuscript Submission Information

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Keywords

  • Sol-gel
  • Functional oxide
  • Nanoparticles
  • Hybrid materials

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Editorial

Jump to: Research, Review

7 pages, 399 KiB  
Editorial
Sol-Gel Chemistry: From Molecule to Functional Materials
by Sébastien Clément and Ahmad Mehdi
Molecules 2020, 25(11), 2538; https://doi.org/10.3390/molecules25112538 - 29 May 2020
Cited by 7 | Viewed by 2600
Abstract
Through this Special Issue, you will discover the potentiality of inorganic polymerization (sol-gel process) which is a unique and versatile way for the preparation of materials [...] Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)

Research

Jump to: Editorial, Review

16 pages, 8394 KiB  
Article
Periodic Mesoporous Organosilica Nanoparticles with BOC Group, towards HIFU Responsive Agents
by Hao Li, Carolina Gascó, Anthony Delalande, Clarence Charnay, Laurence Raehm, Patrick Midoux, Chantal Pichon, Roser Pleixats and Jean-Olivier Durand
Molecules 2020, 25(4), 974; https://doi.org/10.3390/molecules25040974 - 21 Feb 2020
Cited by 8 | Viewed by 3396
Abstract
Periodic Mesoporous Organosilica Nanoparticles (PMONPs) are nanoparticles of high interest for nanomedicine applications. These nanoparticles are not composed of silica (SiO2). They belong to hybrid organic–inorganic systems. We considered using these nanoparticles for CO2 release as a contrast agent for [...] Read more.
Periodic Mesoporous Organosilica Nanoparticles (PMONPs) are nanoparticles of high interest for nanomedicine applications. These nanoparticles are not composed of silica (SiO2). They belong to hybrid organic–inorganic systems. We considered using these nanoparticles for CO2 release as a contrast agent for High Intensity Focused Ultrasounds (HIFU). Three molecules (P1–P3) possessing two to four triethoxysilyl groups were synthesized through click chemistry. These molecules possess a tert-butoxycarbonyl (BOC) group whose cleavage in water at 90–100 °C releases CO2. Bis(triethoxysilyl)ethylene E was mixed with the molecules Pn (or not for P3) at a proportion of 90/10 to 75/25, and the polymerization triggered by the sol-gel procedure led to PMONPs. PMONPs were characterized by different techniques, and nanorods of 200–300 nm were obtained. These nanorods were porous at a proportion of 90/10, but non-porous at 75/25. Alternatively, molecules P3 alone led to mesoporous nanoparticles of 100 nm diameter. The BOC group was stable, but it was cleaved at pH 1 in boiling water. Molecules possessing a BOC group were successfully used for the preparation of nanoparticles for CO2 release. The BOC group was stable and we did not observe release of CO2 under HIFU at lysosomal pH of 5.5. The pH needed to be adjusted to 1 in boiling water to cleave the BOC group. Nevertheless, the concept is interesting for HIFU theranostic agents. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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20 pages, 3667 KiB  
Article
In Depth Analysis of Photovoltaic Performance of Chlorophyll Derivative-Based “All Solid-State” Dye-Sensitized Solar Cells
by Michèle Chevrier, Alberto Fattori, Laurent Lasser, Clément Kotras, Clémence Rose, Michela Cangiotti, David Beljonne, Ahmad Mehdi, Mathieu Surin, Roberto Lazzaroni, Philippe Dubois, Maria Francesca Ottaviani, Sébastien Richeter, Johann Bouclé and Sébastien Clément
Molecules 2020, 25(1), 198; https://doi.org/10.3390/molecules25010198 - 03 Jan 2020
Cited by 11 | Viewed by 3724
Abstract
Chlorophyll a derivatives were integrated in “all solid-state” dye sensitized solar cells (DSSCs) with a mesoporous TiO2 electrode and 2′,2′,7,7′-tetrakis[N,N-di(4-methoxyphenyl)amino]-9,9′-spirobifluorene as the hole-transport material. Despite modest power conversion efficiencies (PCEs) between 0.26% and 0.55% achieved for these chlorin [...] Read more.
Chlorophyll a derivatives were integrated in “all solid-state” dye sensitized solar cells (DSSCs) with a mesoporous TiO2 electrode and 2′,2′,7,7′-tetrakis[N,N-di(4-methoxyphenyl)amino]-9,9′-spirobifluorene as the hole-transport material. Despite modest power conversion efficiencies (PCEs) between 0.26% and 0.55% achieved for these chlorin dyes, a systematic investigation was carried out in order to elucidate their main limitations. To provide a comprehensive understanding of the parameters (structure, nature of the anchoring group, adsorption …) and their relationship with the PCEs, density functional theory (DFT) calculations, optical and photovoltaic studies and electron paramagnetic resonance analysis exploiting the 4-carboxy-TEMPO spin probe were combined. The recombination kinetics, the frontier molecular orbitals of these DSSCs and the adsorption efficiency onto the TiO2 surface were found to be the key parameters that govern their photovoltaic response. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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10 pages, 2601 KiB  
Article
Encapsulation of Upconversion Nanoparticles in Periodic Mesoporous Organosilicas
by Saher Rahmani, Chiara Mauriello Jimenez, Dina Aggad, Daniel González-Mancebo, Manuel Ocaña, Lamiaa M. A. Ali, Christophe Nguyen, Ana Isabel Becerro Nieto, Nadège Francolon, Erwan Oliveiro, Damien Boyer, Rachid Mahiou, Laurence Raehm, Magali Gary-Bobo, Jean-Olivier Durand and Clarence Charnay
Molecules 2019, 24(22), 4054; https://doi.org/10.3390/molecules24224054 - 09 Nov 2019
Cited by 3 | Viewed by 2825
Abstract
(1) Background: Nanomedicine has recently emerged as a promising field, particularly for cancer theranostics. In this context, nanoparticles designed for imaging and therapeutic applications are of interest. We, therefore, studied the encapsulation of upconverting nanoparticles in mesoporous organosilica nanoparticles. Indeed, mesoporous organosilica nanoparticles [...] Read more.
(1) Background: Nanomedicine has recently emerged as a promising field, particularly for cancer theranostics. In this context, nanoparticles designed for imaging and therapeutic applications are of interest. We, therefore, studied the encapsulation of upconverting nanoparticles in mesoporous organosilica nanoparticles. Indeed, mesoporous organosilica nanoparticles have been shown to be very efficient for drug delivery, and upconverting nanoparticles are interesting for near-infrared and X-ray computed tomography imaging, depending on the matrix used. (2) Methods: Two different upconverting-based nanoparticles were synthesized with Yb3+-Er3+ as the upconverting system and NaYF4 or BaLuF5 as the matrix. The encapsulation of these nanoparticles was studied through the sol-gel procedure with bis(triethoxysilyl)ethylene and bis(triethoxysilyl)ethane in the presence of CTAB. (3) Results: with bis(triethoxysilyl)ethylene, BaLuF5: Yb3+-Er3+, nanoparticles were not encapsulated, but anchored on the surface of the obtained mesoporous nanorods BaLuF5: Yb3+-Er3+@Ethylene. With bis(triethoxysilyl)ethane, BaLuF5: Yb3+-Er3+ and NaYF4: Yb3+-Er3+nanoparticles were encapsulated in the mesoporous cubic structure leading to BaLuF5: Yb3+-Er3+@Ethane and NaYF4: Yb3+-Er3+@Ethane, respectively. (4) Conclusions: upconversion nanoparticles were located on the surface of mesoporous nanorods obtained by hydrolysis polycondensation of bis(triethoxysilyl)ethylene, whereas encapsulation occurred with bis(triethoxysilyl)ethane. The later nanoparticles NaYF4: Yb3+-Er3+@Ethane or BaLuF5: Yb3+-Er3+@Ethane were promising for applications with cancer cell imaging or X-ray-computed tomography respectively. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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17 pages, 4357 KiB  
Article
Assessment of Antifouling Potential of Novel Transparent Sol Gel Coatings for Application in the Marine Environment
by Chloe Richards, Ciprian Briciu-Burghina, Matthew R. Jacobs, Alan Barrett and Fiona Regan
Molecules 2019, 24(16), 2983; https://doi.org/10.3390/molecules24162983 - 16 Aug 2019
Cited by 13 | Viewed by 4052
Abstract
In recent years, there has become a growing need for the development of antifouling technology for application in the marine environment. The accumulation of large quantities of biomass on these surfaces cause substantial economic burdens within the marine industry, or adversely impact the [...] Read more.
In recent years, there has become a growing need for the development of antifouling technology for application in the marine environment. The accumulation of large quantities of biomass on these surfaces cause substantial economic burdens within the marine industry, or adversely impact the performance of sensor technologies. Here, we present a study of transparent coatings with potential for applications on sensors or devices with optical windows. The focus of the study is on the abundance and diversity of biofouling organisms that accumulate on glass panels coated with novel transparent or opaque organically modified silicate (ORMOSIL) coatings. The diatom assessment was used to determine the effectiveness of the coatings against biofouling. Test panels were deployed in a marine environment in Galway Bay for durations of nine and thirteen months to examine differences in biofilm formation in both microfouling and macrofouling conditions. The most effective coating is one which consists of precursor, tetraethyl orthosilicate (HC006) that has a water contact angle > 100, without significant roughness (43.52 nm). However, improved roughness and wettability of a second coating, diethoxydimethylsilane (DMDEOS), showed real promise in relation to macrofouling reduction. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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14 pages, 4286 KiB  
Article
Monitoring Silane Sol-Gel Kinetics with In-Situ Optical Turbidity Scanning and Dynamic Light Scattering
by Abul Bashar Mohammad Giasuddin and David W. Britt
Molecules 2019, 24(16), 2931; https://doi.org/10.3390/molecules24162931 - 13 Aug 2019
Cited by 8 | Viewed by 4776
Abstract
Organosilanes (e.g., R’-SiOR3) provide hydrophobic functionality in thin-film coatings, porous gels, and particles. Compared with tetraalkoxysilanes (SiOR4), organosilanes exhibit distinct reaction kinetics and assembly mechanisms arising from steric and electronic properties of the R’ group on the silicon atom. [...] Read more.
Organosilanes (e.g., R’-SiOR3) provide hydrophobic functionality in thin-film coatings, porous gels, and particles. Compared with tetraalkoxysilanes (SiOR4), organosilanes exhibit distinct reaction kinetics and assembly mechanisms arising from steric and electronic properties of the R’ group on the silicon atom. Here, the hydrolysis and condensation pathways of n-propyltrimethoxy silane (nPM) and a tri-fluorinated analog of nPM, 3,3,3-trifluoropropyl trimethoxy silane (3F), were investigated under aqueous conditions at pH 1.7, 2.0, 3.0, and 4.0. Prior to hydrolysis, 3F and nPM are insoluble in water and form a lens at the bottom (3F) or top (nPM) of the solutions. This phase separation was employed to follow reaction kinetics using a Turbiscan instrument to monitor hydrolysis through solubilization of the neat silane lens while simultaneously tracking condensation-induced turbidity throughout the bulk solution. Dynamic light scattering confirmed the silane condensation and particle aggregation processes reported by the turbidity scanning. Employing macroscopic phase separation of the starting reactants from the solvent further allows for control over the reaction kinetics, as the interfacial area can be readily controlled by reaction vessel geometry, namely by controlling the surface area to volume. In-situ turbidity scanning and dynamic light scattering revealed distinct reaction kinetics for nPM and 3F, attributable to the electron withdrawing and donating nature of the fluoro- and organo-side chains of 3F and nPM, respectively. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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9 pages, 4217 KiB  
Article
Microwave Assisted Sol-Gel Synthesis of Silica-Spider Silk Composites
by Abul Bashar Mohammad Giasuddin and David W. Britt
Molecules 2019, 24(14), 2521; https://doi.org/10.3390/molecules24142521 - 10 Jul 2019
Cited by 6 | Viewed by 3432
Abstract
This study introduces a simple and environmentally friendly method to synthesize silica-protein nanocomposite materials using microwave energy to solubilize hydrophobic protein in an aqueous solution of pre-hydrolyzed organo- or fluoro-silane. Sol-gel functionality can be enhanced through biomacromolecule incorporation to tune mechanical properties, surface [...] Read more.
This study introduces a simple and environmentally friendly method to synthesize silica-protein nanocomposite materials using microwave energy to solubilize hydrophobic protein in an aqueous solution of pre-hydrolyzed organo- or fluoro-silane. Sol-gel functionality can be enhanced through biomacromolecule incorporation to tune mechanical properties, surface energy, and biocompatibility. Here, synthetic spider silk protein and organo- and fluoro-silane precursors were dissolved and mixed in weakly acidic aqueous solution using microwave technology. Scanning electron microscopy (SEM) and Atomic force microscopy (AFM) images revealed the formation of spherical nanoparticles with sizes ranging from 100 to 500 nm depending, in part, on silane fluoro- or organo-side chain chemistry. The silane-protein interaction in the nanocomposite was assessed through infrared spectroscopy. Deconvoluted ATR-FTIR (Attenuated total reflectance Fourier-transform infrared spectroscopy) spectra revealed silane chemistry-specific conformational changes in the protein-silane nanocomposites. Relative to microwave-solubilized spider silk protein, the β structure content increased by 14% in the spider silk-organo-silica nanocomposites, but decreased by a net 20% in the spider silk-fluoro-silica nanocomposites. Methods of tuning the secondary structures, and in particular β-sheets that are the cross-linking moieties in spider silks and other self-assembling fibrillar proteins, may provide a unique means to promote protein interactions, favor subsequent epitaxial growth process, and enhance the properties of the protein-silane nanocomposites. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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15 pages, 5577 KiB  
Article
TiO2-Based Hybrid Nanocomposites Modified by Phosphonate Molecules as Selective PAH Adsorbents
by Nadine Bou Orm, Quoc An Trieu and Stephane Daniele
Molecules 2018, 23(11), 3046; https://doi.org/10.3390/molecules23113046 - 21 Nov 2018
Cited by 10 | Viewed by 3856
Abstract
A robust sol-gel process was developed for the synthesis of surface-functionalized titania nanocrystallites bearing unsaturated groups starting from molecular heteroleptic single-source precursors. Molecules and nanomaterials were thoroughly characterized by multinuclear liquid and solid-state nuclear magnetic resonance (NMR), infra-red (FT-IR, DRIFT) spectroscopies. Nitrogen adsorption-desorption [...] Read more.
A robust sol-gel process was developed for the synthesis of surface-functionalized titania nanocrystallites bearing unsaturated groups starting from molecular heteroleptic single-source precursors. Molecules and nanomaterials were thoroughly characterized by multinuclear liquid and solid-state nuclear magnetic resonance (NMR), infra-red (FT-IR, DRIFT) spectroscopies. Nitrogen adsorption-desorption (BET), thermogravimetric (TG) and elemental analyses demonstrated the reliability and the fine tuning of the surface functionalization in terms of ratio TiO2:ligand. The as-prepared materials were used as nano-adsorbents to remove mixture of 16 polycyclic aromatic hydrocarbon (PAHs) from aqueous solutions. Adsorption kinetic experiments were carried out for 24 h in solutions of one PAH [benzo(a)pyrene, 220 ppb] and of a mixture of sixteen ones [220 ppb for each PAH]. Most kinetic data best fitted the pseudo-second order model. However, in PAHs mixture, a competition process took place during the first hours leading to a remarkable high selectivity between light and heavy PAHs. This selectivity could be fine-tuned depending on the nature of the unsaturated group of the phosphonate framework and on the nanomaterial textures. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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11 pages, 3187 KiB  
Article
Tuning Texture and Morphology of Mesoporous TiO2 by Non-Hydrolytic Sol-Gel Syntheses
by Yanhui Wang, Maroua Bouchneb, Johan G. Alauzun and P. Hubert Mutin
Molecules 2018, 23(11), 3006; https://doi.org/10.3390/molecules23113006 - 17 Nov 2018
Cited by 6 | Viewed by 3995
Abstract
The development of powerful synthetic methodologies is paramount in the design of advanced nanostructured materials. Owing to its remarkable properties and low cost, nanostructured TiO2 is widely investigated for applications such as photocatalysis, energy conversion or energy storage. In this article we [...] Read more.
The development of powerful synthetic methodologies is paramount in the design of advanced nanostructured materials. Owing to its remarkable properties and low cost, nanostructured TiO2 is widely investigated for applications such as photocatalysis, energy conversion or energy storage. In this article we report the synthesis of mesoporous TiO2 by three different non-hydrolytic sol-gel routes, and we investigate the influence of the synthetic route and of the presence and nature of the solvent on the structure, texture and morphology of the materials. The first route is the well-known ether route, based on the reaction of TiCl4 with iPr2O. The second and third routes, which have not been previously described for the synthesis of mesoporous TiO2, involve the reaction of Ti(OiPr)4 with stoichiometric amounts of acetophenone and benzoic anhydride, respectively. All materials are characterized by XRD, N2 physisorption and SEM. By playing with the non-hydrolytic route used and the reaction conditions (presence of a solvent, nature of the solvent, calcination), it is possible to tune the morphology and texture of the TiO2. Depending on the reaction conditions, a large variety of mesoporous TiO2 nanostructures could be obtained, resulting from the spontaneous aggregation of TiO2 nanoparticles, either rounded nanoparticles, platelets or nanorods. These nanoparticle networks exhibited a specific surface area up to 250 m2 g−1 before calcination, or up to 110 m2 g−1 after calcination. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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15 pages, 4927 KiB  
Article
Development of Zinc-Doped Hydroxyapatite by Sol-Gel Method for Medical Applications
by Catalin Constantin Negrila, Mihai Valentin Predoi, Simona Liliana Iconaru and Daniela Predoi
Molecules 2018, 23(11), 2986; https://doi.org/10.3390/molecules23112986 - 15 Nov 2018
Cited by 63 | Viewed by 4612
Abstract
Zinc- (Zn) doped hydroxyapatite (HAp) were prepared by sol-gel method. Zinc-doped hydroxyapatite (ZnHAp) and HAp were analyzed by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The Rietveld analysis revealed that the HAp and 7ZnHAp powders obtained by sol-gel method have a monophasic [...] Read more.
Zinc- (Zn) doped hydroxyapatite (HAp) were prepared by sol-gel method. Zinc-doped hydroxyapatite (ZnHAp) and HAp were analyzed by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The Rietveld analysis revealed that the HAp and 7ZnHAp powders obtained by sol-gel method have a monophasic hydroxyapatite structure belonging to the P63/m spatial group. The results obtained from the ultrasound characterization of HAp and ZnHAp are also presented in this study. The effect of zinc concentration on properties that were deduced from ultrasonic measurements are studied in the case of a significant zinc concentration (xZn = 0.07). From the values of the ultrasonic waves velocities were determined by the pairs of elastic coefficients of the suspensions (Young modulus E, Poisson coefficient ν), which have proven to be similar to those determined by other authors. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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13 pages, 1780 KiB  
Article
New Layered Polythiophene-Silica Composite Through the Self-Assembly and Polymerization of Thiophene-Based Silylated Molecular Precursors
by Marie-José Zacca, Danielle Laurencin, Sébastien Richeter, Sébastien Clément and Ahmad Mehdi
Molecules 2018, 23(10), 2510; https://doi.org/10.3390/molecules23102510 - 30 Sep 2018
Cited by 5 | Viewed by 3221
Abstract
A new layered hybrid polythiophene-silica material was obtained directly by hydrolysis and polycondensation (sol-gel) of a silylated-thiophene bifunctional precursor, and its subsequent oxidative polymerization by FeCl3. This precursor was judiciously designed to guarantee its self-assembly and the formation of a lamellar [...] Read more.
A new layered hybrid polythiophene-silica material was obtained directly by hydrolysis and polycondensation (sol-gel) of a silylated-thiophene bifunctional precursor, and its subsequent oxidative polymerization by FeCl3. This precursor was judiciously designed to guarantee its self-assembly and the formation of a lamellar polymer-silica structure, exploiting the cooperative effect between the hydrogen bonding interactions, originating from the ureido groups and the π-stacking interactions between the thiophene units. The lamellar structure of the polythiophene-silica composite was confirmed by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM) analyses. The solid-state nuclear magnetic resonance (NMR), UV-Vis, and photoluminescence spectra unambiguously indicate the incorporation of polythiophene into the silica matrix. Our work demonstrates that using a polymerizable silylated-thiophene precursor is an efficient approach towards the formation of nanostructured conjugated polymer-based hybrid materials. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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15 pages, 6746 KiB  
Article
Silica/Polyethylene Glycol Hybrid Materials Prepared by a Sol-Gel Method and Containing Chlorogenic Acid
by Michelina Catauro, Elisabetta Tranquillo, Alessia Salzillo, Lucia Capasso, Michela Illiano, Luigi Sapio and Silvio Naviglio
Molecules 2018, 23(10), 2447; https://doi.org/10.3390/molecules23102447 - 25 Sep 2018
Cited by 21 | Viewed by 3530
Abstract
Chlorogenic acid (CGA) is a very common dietary polyphenolic compound. CGA is becoming very attractive due to its potential use as preventive and therapeutic agent in many diseases, including cancer. Inorganic/organic hybrid materials are gaining considerable attention in the biomedical field. The sol-gel [...] Read more.
Chlorogenic acid (CGA) is a very common dietary polyphenolic compound. CGA is becoming very attractive due to its potential use as preventive and therapeutic agent in many diseases, including cancer. Inorganic/organic hybrid materials are gaining considerable attention in the biomedical field. The sol-gel process provides a useful way to obtain functional organic/inorganic hybrids. The aim of this study was to synthesize silica/polyethylene glycol (PEG) hybrids with different percentages of CGA by sol-gel technique and to investigate their impact on the cancer cell proliferation. Synthesized materials have been chemically characterized through the FTIR spectroscopy and their bioactivity evaluated looking by SEM at their ability to produce a hydroxyapatite layer on their surface upon incubation with simulated body fluid (SBF). Finally, their effects on cell proliferation were studied in cell lines by direct cell number counting, MTT, flow cytometry-based cell-cycle and cell death assays, and immunoblotting experiments. Notably, we found that SiO2/PEG/CGA hybrids exhibit clear antiproliferative effects in different tumor, including breast cancer and osteosarcoma, cell lines in a CGA dependent manner, but not in normal cells. Overall, our results increase the evidence of CGA as a possible anticancer agent and illustrate the potential for clinical applications of sol-gel synthesized SiO2/PEG/CGA materials. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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15 pages, 3739 KiB  
Article
Antioxidant and Fluorescence Properties of Hydrogenolyzised Polymeric Proanthocyanidins Prepared Using SO42−/ZrO2 Solid Superacids Catalyst
by Liwen Ni, Fanbin Zhao, Bolun Li, Tong Wei, Hang Guan and Shixue Ren
Molecules 2018, 23(10), 2445; https://doi.org/10.3390/molecules23102445 - 25 Sep 2018
Cited by 13 | Viewed by 3267
Abstract
Larix bark oligomeric proanthocyanidins (LOPC) were prepared from larix bark polymeric proanthocyanidins (LPPC) by catalytic hydrogenolysis using SO42−/ZrO2 solid superacid as the catalyst. The catalyst to polymeric proanthocyanidins ratio was 0.2:1 (m/m). The LOPC, obtained [...] Read more.
Larix bark oligomeric proanthocyanidins (LOPC) were prepared from larix bark polymeric proanthocyanidins (LPPC) by catalytic hydrogenolysis using SO42−/ZrO2 solid superacid as the catalyst. The catalyst to polymeric proanthocyanidins ratio was 0.2:1 (m/m). The LOPC, obtained after hydrogenolysis at 100 °C for 4 h under 3 MPa hydrogen pressure, retained the structural characteristics of proanthocyanidins. The average degree of polymerization was reduced from 9.50% to 4.76% and the depolymerization yield was 53.85%. LOPC has good antioxidant properties and, at the same concentration, the reducing ability of LOPC was much higher than that of LPPC. The IC50 values of LOPC for scavenging DPPH• and ABTS•+ radicals were 0.046 mg/mL and 0.051 mg/mL, respectively. LOPC is biocompatible and has fluorescent properties that are affected by external factors, such as solvent polarity, pH and the presence of different metal ions. These features indicate that LOPC could be developed as a new biological fluorescent marker. The depolymerization of low-value polymeric proanthocyanidins to provide high-value oligomeric proanthocyanidins and the development of new applications for proanthocyanidins represent significant advances. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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13 pages, 1261 KiB  
Article
Sol-Gel Immobilisation of Lipases: Towards Active and Stable Biocatalysts for the Esterification of Valeric Acid
by Soledad Cebrián-García, Alina M. Balu, Araceli García and Rafael Luque
Molecules 2018, 23(9), 2283; https://doi.org/10.3390/molecules23092283 - 06 Sep 2018
Cited by 21 | Viewed by 3589
Abstract
Alkyl esters are high added value products useful in a wide range of industrial sectors. A methodology based on a simple sol-gel approach (biosilicification) is herein proposed to encapsulate enzymes in order to design highly active and stable biocatalysts. Their performance was assessed [...] Read more.
Alkyl esters are high added value products useful in a wide range of industrial sectors. A methodology based on a simple sol-gel approach (biosilicification) is herein proposed to encapsulate enzymes in order to design highly active and stable biocatalysts. Their performance was assessed through the optimization of valeric acid esterification evaluating the effect of different parameters (biocatalyst load, presence of water, reaction temperature and stirring rate) in different alcoholic media, and comparing two different methodologies: conventional heating and microwave irradiation. Ethyl valerate yields were in the 80–85% range under optimum conditions (15 min, 12% m/v biocatalyst, molar ratio 1:2 of valeric acid to alcohol). Comparatively, the biocatalysts were slightly deactivated under microwave irradiation due to enzyme denaturalisation. Biocatalyst reuse was attempted to prove that good reusability of these sol-gel immobilised enzymes could be achieved under conventional heating. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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14 pages, 2200 KiB  
Article
Europium-Doped Sol-Gel SiO2-Based Glasses: Effect of the Europium Source and Content, Magnesium Addition and Thermal Treatment on Their Photoluminescence Properties
by Hussein Fneich, Nathalie Gaumer, Stéphane Chaussedent, Wilfried Blanc and Ahmad Mehdi
Molecules 2018, 23(7), 1768; https://doi.org/10.3390/molecules23071768 - 19 Jul 2018
Cited by 14 | Viewed by 4288
Abstract
Rare-earth doped silica-based glasses lead the optical materials due to their tailorable spectroscopic and optical properties. In this context, we took advantage of the sol-gel process to prepare various Eu-doped silica glasses to study their luminescent properties before and after annealing at 900 [...] Read more.
Rare-earth doped silica-based glasses lead the optical materials due to their tailorable spectroscopic and optical properties. In this context, we took advantage of the sol-gel process to prepare various Eu-doped silica glasses to study their luminescent properties before and after annealing at 900 °C. The effect of magnesium on these properties was studied in comparison with Mg-free-glass. Using TEM, nitrogen sorption, XRD and FT-IR, we confirmed that the magnesium modifies the glass structure and the thermal treatment eliminates the aqueous environment, modifying the structure ordering. The emission spectra and the decay time curves show the advantages of the Mg addition and the annealing on the photoluminescent properties. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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20 pages, 3568 KiB  
Article
Photonic Band Gap and Bactericide Performance of Amorphous Sol-Gel Titania: An Alternative to Crystalline TiO2
by M. Clara Gonçalves, José Carlos Pereira, Joana C. Matos and Helena Cristina Vasconcelos
Molecules 2018, 23(7), 1677; https://doi.org/10.3390/molecules23071677 - 10 Jul 2018
Cited by 36 | Viewed by 7272
Abstract
In addition to its traditional application in white pigments, nanocrystalline titania (TiO2) has optoelectronic and photocatalytic properties (strongly dependent on crystallinity, particle size, and surface structure) that grant this naturally occurring oxide new technological applications. Sol-gel is one of the most [...] Read more.
In addition to its traditional application in white pigments, nanocrystalline titania (TiO2) has optoelectronic and photocatalytic properties (strongly dependent on crystallinity, particle size, and surface structure) that grant this naturally occurring oxide new technological applications. Sol-gel is one of the most widely used methods to synthesize TiO2 films and NPs, but the products obtained (mostly oxy-hydrated amorphous phases) require severe heat-treatments to promote crystallization, in which control over size and shape is difficult to achieve. In this work, we obtained new photocatalytic materials based on amorphous titania and measured their electronic band gap. Two case studies are reported that show the enormous potential of amorphous titania as bactericide or photocatalyst. In the first, amorphous sol-gel TiO2 thin films doped with N (TiO2−xNx, x = 0.75) were designed to exhibit a photonic band gap in the visible region. The identification of Ti-O-N and N-Ti-O bindings was achieved by XPS. The photonic band gaps were found to be 3.18 eV for a-TiO2 and 2.99 eV for N-doped a-TiO2. In the second study, amorphous titania and amine-functionalized amorphous titania nanoparticles were synthetized using a novel base-catalysed sol-gel methodology. All the synthesized amorphous TiO2 nanoparticles exhibit bactericide performance (E. coli, ASTME 2149-13). Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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18 pages, 6922 KiB  
Article
Tubular and Spherical SiO2 Obtained by Sol Gel Method for Lipase Immobilization and Enzymatic Activity
by Crina Anastasescu, Silviu Preda, Adriana Rusu, Dana Culita, Gabriel Plavan, Stefan Strungaru, Jose Maria Calderon-Moreno, Cornel Munteanu, Catalina Gifu, Mirela Enache, Radu Socoteanu, Daniel Angelescu, Mihai Anastasescu, Mariuca Gartner, Ioan Balint and Maria Zaharescu
Molecules 2018, 23(6), 1362; https://doi.org/10.3390/molecules23061362 - 05 Jun 2018
Cited by 13 | Viewed by 4105
Abstract
A wide range of hybrid biomaterials has been designed in order to sustain bioremediation processes by associating sol-gel SiO2 matrices with various biologically active compounds (enzymes, antibodies). SiO2 is a widespread, chemically stable and non-toxic material; thus, the immobilization of enzymes [...] Read more.
A wide range of hybrid biomaterials has been designed in order to sustain bioremediation processes by associating sol-gel SiO2 matrices with various biologically active compounds (enzymes, antibodies). SiO2 is a widespread, chemically stable and non-toxic material; thus, the immobilization of enzymes on silica may lead to improving the efficiency of biocatalysts in terms of endurance and economic costs. Our present work explores the potential of different hybrid morphologies, based on hollow tubes and solid spheres of amorphous SiO2, for enzyme immobilization and the development of competitive biocatalysts. The synthesis protocol and structural characterization of spherical and tubular SiO2 obtained by the sol gel method were fully investigated in connection with the subsequent immobilization of lipase from Rhizopus orizae. The immobilization is conducted at pH 6, lower than the isoelectric point of lipase and higher than the isoelectric point of silica, which is meant to sustain the physical interactions of the enzyme with the SiO2 matrix. The morphological, textural and surface properties of spherical and tubular SiO2 were investigated by SEM, nitrogen sorption, and electrokinetic potential measurements, while the formation and characterization of hybrid organic-inorganic complexes were studied by UV-VIS, FTIR-ATR and fluorescence spectroscopy. The highest degree of enzyme immobilization (as depicted from total organic carbon) was achieved for tubular morphology and the hydrolysis of p-nitrophenyl acetate was used as an enzymatic model reaction conducted in the presence of hybrid lipase–SiO2 complex. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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10 pages, 1982 KiB  
Article
Cast-In-Situ, Large-Sized Monolithic Silica Xerogel Prepared in Aqueous System
by Wenhui Ding, Xiaodong Wang, Dong Chen, Tiemin Li and Jun Shen
Molecules 2018, 23(5), 1178; https://doi.org/10.3390/molecules23051178 - 15 May 2018
Cited by 3 | Viewed by 3792
Abstract
This paper reports the preparation of cast-in-situ, large-sized monolithic silica xerogels by a two-step acid–base catalyzed approach under ambient pressure drying. Low-cost industrial silica sol and deionized water were used as the silicon source and the solvent, respectively. Hexadecetyltrimethylammonium bromide (CTAB) was used [...] Read more.
This paper reports the preparation of cast-in-situ, large-sized monolithic silica xerogels by a two-step acid–base catalyzed approach under ambient pressure drying. Low-cost industrial silica sol and deionized water were used as the silicon source and the solvent, respectively. Hexadecetyltrimethylammonium bromide (CTAB) was used as a modification agent. Different amounts of polyethylene glycol 400 (PEG400) was added as a pore-forming agent. The prepared silica xerogels under ambient pressure drying have a mesoporous structure with a low density of 221 mg·cm−3 and a thermal conductivity of 0.0428 W·m−1·K−1. The low-cost and facile preparation process, as well as the superior performance of the monolithic silica xerogels make it a promising candidate for industrial thermal insulation materials. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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15 pages, 3595 KiB  
Article
Innovative Formulation Combining Al, Zr and Si Precursors to Obtain Anticorrosion Hybrid Sol-Gel Coating
by Clément Genet, Marie-Joëlle Menu, Olivier Gavard, Florence Ansart, Marie Gressier and Robin Montpellaz
Molecules 2018, 23(5), 1135; https://doi.org/10.3390/molecules23051135 - 10 May 2018
Cited by 7 | Viewed by 5018
Abstract
The aim of our study is to improve the aluminium alloy corrosion resistance with Organic-Inorganic Hybrid (OIH) sol-gel coating. Coatings are obtained from unusual formulation with precursors mixing: glycidoxypropyltrimethoxysilane (GPTMS), zirconium (IV) propoxide (TPOZ) and aluminium tri-sec-butoxide (ASB). This formulation was characterized and [...] Read more.
The aim of our study is to improve the aluminium alloy corrosion resistance with Organic-Inorganic Hybrid (OIH) sol-gel coating. Coatings are obtained from unusual formulation with precursors mixing: glycidoxypropyltrimethoxysilane (GPTMS), zirconium (IV) propoxide (TPOZ) and aluminium tri-sec-butoxide (ASB). This formulation was characterized and compared with sol formulations GPTMS/TPOZ and GPTMS/ASB. In each formulation, a corrosion inhibitor, cerium (III) nitrate hexahydrate, is employed to improve the corrosion performance. Coatings obtained from sol based on GPTMS/TPOZ/ASB have good anti-corrosion performances with Natural Salt Spray (NSS) resistance of 500 h for a thickness lower than 4 µm. Contact angle measurement showed a coating hydrophobic behaviour. To understand these performances, nuclear magnetic resonance (NMR) analyses were performed, results make sol-gel coating condensation evident and are in very good agreement with previous results. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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9 pages, 3101 KiB  
Article
Fabrication of Refractive Index Tunable Coating with Moisture-Resistant Function for High-Power Laser Systems Based on Homogeneous Embedding of Surface-Modified Nanoparticles
by Wei Yang, Xiangyang Lei, Haohao Hui, Qinghua Zhang and Xueran Deng
Molecules 2018, 23(5), 1105; https://doi.org/10.3390/molecules23051105 - 07 May 2018
Cited by 11 | Viewed by 3465
Abstract
Moisture-resistant silicone coatings were prepared on the surface of potassium dihydrogen phosphate (KDP) crystal by means of spin-coating, in which hydrophobic-modified SiO2 nanoparticles were embedded in a certain proportion. The refractive index of such coating can be tuned arbitrarily in the range [...] Read more.
Moisture-resistant silicone coatings were prepared on the surface of potassium dihydrogen phosphate (KDP) crystal by means of spin-coating, in which hydrophobic-modified SiO2 nanoparticles were embedded in a certain proportion. The refractive index of such coating can be tuned arbitrarily in the range of 1.21–1.44, which endows the KDP optical component with excellent transmission capability as well as the moisture proof effect. A dual-layer anti-reflective coating system was obtained by covering this silicone coating with a porous SiO2 coating which is specially treated to enhance the moisture resistance. Transmittance of such a dual-layer coating system could reach 99.60% and 99.62% at 1064 nm and 532 nm, respectively, by precisely matching the refractive index of both layers. Furthermore, the long-term stability of this coating system has been verified at high humidity ambient of 80% RH for 27 weeks. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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13 pages, 4933 KiB  
Article
Improvement of Adhesion Properties and Corrosion Resistance of Sol-Gel Coating on Zinc
by Pauline Savignac, Marie-Joëlle Menu, Marie Gressier, Bastien Denat, Yacine El Khadir, Stephan Manov and Florence Ansart
Molecules 2018, 23(5), 1079; https://doi.org/10.3390/molecules23051079 - 03 May 2018
Cited by 12 | Viewed by 3664
Abstract
Corrosion is a major problem for durability of many metals and alloys. Among the efficient classical surface treatments, chromate-based treatments must be banished from industrial use due to their toxicity. At the same time, sol-gel routes have demonstrated high potential to develop an [...] Read more.
Corrosion is a major problem for durability of many metals and alloys. Among the efficient classical surface treatments, chromate-based treatments must be banished from industrial use due to their toxicity. At the same time, sol-gel routes have demonstrated high potential to develop an efficient barrier effect against aggressive environments. By this process, the anti-corrosion property can be also associated to others in the case of the development of multi-functional hybrid coatings. In this paper, the main goal is precisely to improve both the corrosion resistance and the adhesion properties of phosphated zinc substrates by the deposition of a hybrid (organic-inorganic) sol-gel layer. To reach this double objective, a choice between two formulations 3-glycidoxypropyltrimethoxysilane (GPTMS)/aluminum-tri-sec-butoxide (ASB) and 3-(trimethoxysilyl)propylmethacrylate (MAP)/tetraethylorthosilicate (TEOS) was firstly made based on the results obtained by microstructural characterizations using SEM, optical analysis, and mechanical characterization such as shock and/or scratch tests (coupled to climatic chamber and salt spray exposure). Several investigations were performed in this study, and the best formulation and performances of the system were obtained by adding a new precursor (1-[3-(trimethoxysilyl)propyl]ureido-UPS) under controlled conditions, as detailed in this paper. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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Review

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12 pages, 2149 KiB  
Review
Recent Applications of Molecularly Imprinted Sol-Gel Methodology in Sample Preparation
by Mohammad Mahdi Moein, Abbi Abdel-Rehim and Mohamed Abdel-Rehim
Molecules 2019, 24(16), 2889; https://doi.org/10.3390/molecules24162889 - 09 Aug 2019
Cited by 53 | Viewed by 6418
Abstract
Due to their selectivity and chemical stability, molecularly imprinted polymers have attracted great interest in sample preparation. Imprinted polymers have been applied for the extraction and the enrichment of different sorts of trace analytes in biological and environmental samples before their analysis. Additionally, [...] Read more.
Due to their selectivity and chemical stability, molecularly imprinted polymers have attracted great interest in sample preparation. Imprinted polymers have been applied for the extraction and the enrichment of different sorts of trace analytes in biological and environmental samples before their analysis. Additionally, MIPs are utilized in various sample preparation techniques such as SPE, SPME, SBSE and MEPS. Nevertheless, molecularly imprinted polymers suffer from thermal (stable only up to 150 °C) and mechanical stability issues, improper porosity and poor capacity. The sol-gel methodology as a promising alternative to address these limitations allowing the production of sorbents with controlled porosity and higher surface area. Thus the combination of molecularly imprinted technology and sol-gel technology can create influential materials with high selectivity, high capacity and high thermal stability. This work aims to present an overview of molecularly imprinted sol-gel polymerization methods and their applications in analytical and bioanalytical fields. Full article
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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