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1
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Sol-gel bioactive glass-ceramics Part I: Calcium phosphate silicate/wollastonite glass-ceramics

100%
Radev L., Hristov V., Michailova I., Samuneva B.
Open Chemistry
|
2009
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vol. 7
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issue 3
317-321
EN
In this work we present experimental results about synthesis, structure evolution and in vitro bioactivity of new calcium phosphate silicate/wollastonite (CPS/W) glass-ceramics. The samples obtained were synthesized via polystep sol-gel process with different Ca/P+Si molar ratio (R). The structure of the materials obtained was studied by XRD, FTIR spectroscopy and SEM. XRD showed the presence of Ca15(PO4)2(SiO4)6, β-CaSiO3 and α-CaSiO3 for the sample with R=1.89 after thermal treatment at 1200°C/2h. The XRD results are in good agreement with FTIR analysis. SEM denotes that apatite formation can be observed after soaking in simulated body fluid (SBF). [...]
2
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A silica-silver nanocomposite obtained by sol-gel method in the presence of silver nanoparticles

100%
Racles C., Nistor A., Cazacu M.
Open Chemistry
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2013
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vol. 11
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issue 10
1689-1698
EN
Silver nanoparticles (AgNPs) were obtained by a redox reaction, using a glucose-containing cyclosiloxane as a reduction agent and stabilizer. Then the AgNPs aqueous solution was used as the reaction medium for the sol-gel process, starting from tetraethylorthosilicate (TEOS) as silica precursor. The nanocomposite material resulted (SilAg) after solvent removal, aging and calcination and was investigated by infrared spectroscopy (FT-IR), atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-ray system (SEM/EDX), transmission electron microscopy (TEM), energy-dispersive X-ray fluorescence spectroscopy (EDXRF), X-ray diffraction (XRD) and dynamic vapor sorption (DVS). The results were compared to model silicas obtained without silver. A higher condensation degree in SilAg was obtained due to the basic medium used in the first step and was confirmed by a sorption capacity lower than for the model silicas. The solid surface area calculated with GAB analysis using DVS data for the water vapors is 210 m2 g−1. The nanocomposite showed good catalytic activity for hydrogen peroxide decomposition. [...]
3
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Microwave-assisted and conventional sol-gel preparation of photocatalytically active ZnO/TiO2/glass multilayers

100%
Kaneva N., Stambolova I., Blaskov V., Eliyas A., Vassilev S.
Open Chemistry
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2013
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vol. 11
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issue 7
1055-1065
EN
For the first time a combination of microwaves and/or the conventional treatment method was used to dry and heat multilayered sol-gel ZnO/TiO2/glass structures. Compact or porous TiO2 films were deposited as a bottom layer, covered with a ZnO film. The structures were characterized by X-ray Diffraction (XRD), Energy Dispersive X-ray Spectroscopy (EDX) and Scanning Electron Microscopy (SEM). Only peaks of wurtzite ZnO crystalline phase were registered on the X-Ray diffractograms. The microwave irradiation leads to a formation of poorly crystallized multilayers with very small crystallites and enhanced surface roughness. This results in a better photocatalytic activity of these structures than the structures of the samples treated conventionally. It was established that the morphology of the bottom titania layer affects the reaction of photocatalytic degradation of Malachite Green dye (MG). The structures with the compact bottom TiO2 films showed higher activities than those on porous TiO2 films. This study offers an energy saving method of producing ZnO/TiO2/glass multilayered structures of various morphologies and pronounced photocatalytic properties. The method does not involve any calcination step, normally applied to achieve a good degree of crystallization. This makes the method suitable for protecting substrates of low thermal stability. [...]
4
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Hybrid Materials – Past, Present and Future.

100%
Kickelbick G.
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2015
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vol. 1
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issue 1
EN
Hybrid materials represent one of the most growing new material classes at the edge of technological innovations. Unique possibilities to create novel material properties by synergetic combination of inorganic and organic components on the molecular scale makes this materials class interesting for application-oriented research of chemists, physicists, and materials scientists. The modular approach for combination of properties by the selection of the best suited components opens new options for the generation of materials that are able to solve many technological problems. This review will show in selected examples how science and technological driven approaches can help to design better materials for future applications.
5
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Temperature effect over structure and photochemical properties of nanostructured SnO2 powders

100%
Ungureanu A.-M., Oprea O., Vasile B., Andronescu C., Voicu G., Jitaru I.
Open Chemistry
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2014
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vol. 12
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issue 9
909-917
EN
We successfully synthesized tin dioxide nanoparticles with polyhedral morphology via an ethylene glycol assisted sol-gel approach. The structural characteristics of three tin dioxide samples were investigated after being thermally treated at 400°C, 600°C and 800°C. X-ray diffraction (XRD) patterns clearly show the formation of single phase tin dioxide nanoparticles, with crystallite size of 6–20 nm, in good correlation with Fourier transform infrared (FTIR) spectra. Transmission electron microscopy (TEM) analysis confirms the formation of 6nm polyhedral nanoparticles for the 400°C sample. Ultraviolet-visible (UV-Vis) and photoluminescence (PL) spectra suggest a high concentration of oxygen vacancies. The oxygen vacancy concentration increases with temperature, due to the combined action of the formation of VO and the energetic O compensation. X-ray photoelectron spectroscopy (XPS) analysis also confirms the formation of single phase tin dioxide and the presence of oxygen vacancies in good agreement with UV-VIS and PL data.
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Sol-gel bioactive glass-ceramics Part II: Glass-ceramics in the CaO-SiO2-P2O5-MgO system

100%
Radev L., Hristov V., Michailova I., Samuneva B.
Open Chemistry
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2009
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vol. 7
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issue 3
322-327
EN
Ceramics, with basic composition based on the CaO-SiO2-P2O5-MgO system with different Ca+ Mg/P+Si molar ratio (R), were prepared via polystep sol-gel technique. The structure of the obtained ceramic materials has been studied by XRD, FTIR spectroscopy, and SEM. X-ray diffraction showed the presence of akermanite and HA for the sample with R = 1.68 and Mg substituted β-TCP and silicocarnotite for the sample with R = 2.16, after thermal treatment at 1200°C/2 h. The obtained results are in good agreement with FTIR. In vitro test for bioactivity in static condition proved that the carbonate containing hydroxyapatite (CO3HA) can be formed on the surface of the synthesized samples. CO3HA consisted of both A- and B-type CO 32− ions. SEM micrographs depicted different forms of HA particles, precipitated on the surface after soaking in 1.5 simulated body fluid (SBF). [...]
7
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Methylcellulose/SiO2 hybrids: sol-gel preparation and characterization by XRD, FTIR and AFM

88%
Rangelova N., Radev L., Nenkova S., Miranda Salvado I., Vas Fernandes M., Herzog M.
Open Chemistry
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2011
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vol. 9
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issue 1
112-118
EN
Methylcellulose (MC) / SiO2 organic / inorganic hybrid materials have been prepared from MC and methyltriethoxysilane or ethyltrimethoxysilane, and characterized by XRD, FTIR and AFM. XRD showed peak shifts. FTIR shows intermolecular hydrogen bonding between MC and SiO2. AFM depicts surface roughness which depends on the silica precursor and MC content. [...]
8
Content available remote

Silica-carrageenan hybrids used for cell immobilization realizing high-temperature degradation of nitrile substrates

88%
Kabaivanova L., Chernev G., Miranda Salvado I., Fernandes M.
Open Chemistry
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2011
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vol. 9
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issue 2
232-239
EN
In this work the application of hybrid materials, containing TEOS as source of SiO2 and k-carrageenan in different percentage, synthesized by the sol-gel method at room temperature was studied. They were used as matrices for entrapment of whole Bacillus sp. UG-5B cells, producers of thermostable nitrilase. The effect of the surface area and size and quantity of pores in the synthesized materials on the enzyme activity was evaluated. The process of biodegradation of different concentrations of toxic, potentially carcinogenic and mutagenic substrates by the obtained biocatalysts was investigated. The enzyme reaction takes place by the nitrilase pathway, catalysing nitrile hydrolysis directly to the corresponding carboxylic acid, forming ammonia. At batch experiments the influence of the substrate concentration of different nitriles was tested and 20 mM concentration was found most suitable. A two-step biodegradation process in a laboratory-scale column bioreactor of o-, m- and p-tolunitrile as a mixture was followed. After operation of the system for nine hours for the mixture of substrates at a flow rate of 45 mL h−1 and at 60°C, the overall conversion realized was above 90%, showing a good efficiency of the investigated process.
9
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Removal of cadmium and copper ions by Trichosporon cutaneum R57 cells immobilized onto polyvinyl alcohol/tetraethoxysilane hybrid matrices

88%
Bryaskova R., Georgieva N., Peshev D.
Open Chemistry
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2010
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vol. 8
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issue 5
1053-1058
EN
Polyvinyl alcohol (PVA) and tetraethoxysilane (TEOS) hybrid materials were prepared by sol-gel methods and tested as matrices for immobilization of Trichosporon cutaneum R57, capable of removing cadmium and copper ions from aqueous solutions. A kinetic model was applied and the effects of matrix TEOS content on the copper and cadmium uptake equilibria and rate constants were investigated. [...]
10
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The influence of the chelating/combustion agents on the structure and magnetic properties of zinc ferrite

88%
Slatineanu T., Diana E., Nica V., Oancea V., Caltun O., Iordan A., Palamaru M.
Open Chemistry
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2012
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vol. 10
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issue 6
1799-1807
EN
The present study is reporting the influence of the chelating/combustion agents on the magnetic properties of Zn ferrite. Six chelating/combustion agents, citric acid, egg white, tartaric acid, glycine, glucose and urea, were used to obtain monophase zinc nanoferrite via a sol-gel auto-combustion method. The samples were subjected to a comparative study of structural features and magnetic properties by means of infrared spectroscopy, X-ray diffractometry, scanning electron microscopy and vibrating sample magnetometry. Significant influence of fuel and combustion mode was observed in the magnetic behavior of as-obtained samples. Values of the structural parameters were discovered to vary as a function of fuel choice, and to obtain crystallite size between 38 and 62 nm, inversion degree between 0.239 and 0.807, lattice parameter between 8.4125 and 8.4432 Å. The optimization of sol-gel method synthesis of zinc ferrite nanoparticles by chosing the appropriate fuel is providing structural and magnetic properties of zinc nanoferrite as potential materials to be used in biomedical applications. [...]
11
Content available remote

Organic-inorganic hybrid materials based on N=C=O functionalised silan modified with titanium and zirconium

88%
Ivanova Y., Dimitriev Y., Gerganova T., Bryaskova R., Fernandes M., Miranda Salvado I.
|
EN
This work investigates the influence of the precursor trimethylsilil isocyanate on the sol-gel synthesis of hybrid materials. The obtained Si−O−C−N network is additionally modified by titanium and zirconium alcoxypropoxides in the range of 10 to 30 wt. %. The structure of the obtained hybrid materials before and after pyrolysis up to 1100°C was investigated by methods of XRD, FTIR and 29Si MAS NMR. We established that the hybrid structure was stable up to 600°C based on IR study. The structural transformation of the hybrid materials into oxycarbonitrogen system started at 800°C. The network of the hybrids modified by titanium remained stable and amorphous up to the final temperature of the pyrolysis (1100°C) compared to the gels modified by more than 10 wt.% Zr. It was confirmed by XRD analysis that the last mentioned are nanocomposite materials, built from carbooxynitrogen vitreous matrix and ZrO2-nanocrystals (tetragonal). The NMR method verified the presence of heterometallic bonds (Si−O−Ti and Si−O−Zr) and Q4, ZrQ3 or TiQ3, NSiO3 and D structural units in the gels.
12
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Synthesis of SnO2 nanopowders by a sol-gel process using propanol-isopropanol mixture

88%
Hassanzadeh A., Moazzez B., Haghgooie H., Nasseri M., Golzan M., Sedghi H.
Open Chemistry
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2008
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vol. 6
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issue 4
651-656
EN
A simple sol-gel process is proposed for synthesizing SnO2 nanopowders utilizing normal propanol and isopropanol mixture instead of just using normal alcohols such as ethanol, propanol or butanol for Sol preparation. No surfactant was used in this Sol preparation process. The structure of sol is studied by FT-IR-ATR technique. On altering propanol to isopropanol ratio, three different nanopowders were obtained. X-ray powder diffraction, high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction pattern (SAED) and BET techniques were used to characterize prepared powders. Results show that smaller grain size was obtained via altering alcohols ratio. In addition, Merck commercial SnO2 powder was also used as a reference material for comparing purposes; because it has nanometer scale (ca. 60 nm). HRTEM images show that obtained nanopowders were polycrystalline and their average diameters fall into the range of 6–80 nm. Finally, the effect of alkoxide ligand size through sol-gel synthesis on product particle size is discussed. [...]
13
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Alginate/porous silica matrices for the encapsulation of living organisms: tunable properties for biosensors, modular bioreactors, and bioremediation devices

75%
Perullini M., Calcabrini M., Jobbágy M., Bilmes S. A.
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EN
The encapsulation of living cells within inorganic silica hydrogels is a promising strategy for the design of biosensors, modular bioreactors, and bioremediation devices, among other interesting applications, attracting scientific and technological interest. These hostguest multifunctional materials (HGFM) combine synergistically specific biologic functions of their guest with those of the host matrix enhancing their performance. Although inorganic immobilization hosts present several advantages over their (bio)polymer-based counterparts in terms of chemical and physical stability, the direct contact of cells with silica precursors during synthesis and the constraints imposed by the inorganic host during operating conditions have proved to influence their biological response. Recently, we proposed an alternative two-step procedure including a pre-encapsulation in biocompatible polymers such as alginates in order to confer protection to the biological guest during the inorganic and more cytotoxic synthesis. By means of this procedure, whole cultures of microorganisms remain confined in small liquid volumes generated inside the inorganic host, providing near conventional liquid culture conditions.Moreover, the fact of protecting the biological guest during the synthesis of the host, allows extending the synthesis parameters beyond biocompatible conditions, tuning the microstructure of the matrix. In turn, the microstructure (porosity at the nanoscale, radius of gyration of particles composing the structure, and fractal dimension of particle clusters) is determinant of macroscopic parameters, such as optical quality and transport properties that govern the encapsulation material’s performance. Here, we review the most interesting applications of the two-step procedure, making special emphasis on the optimization of optical, transport and mechanical properties of the host as well as in the interaction with the guest during operation conditions.
14
Content available remote

Structural and optical properties of WO3 electrochromic layers prepared by the sol-gel method

63%
Novinrooz A., Sharbatdaran M., Noorkojouri H.
Open Physics
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2005
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vol. 3
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issue 3
456-466
EN
Thin layers of tungsten trioxide have been prepared from an aqueous solution of peroxotungstic acid (PTA) using the sol-gel method. Compositional, structural and optical characteristics of WO3 coated on indium tin oxide (ITO) conductive glass substrates were studied using X-ray diffractometery (XRD), cyclic voltammetery (CV), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). Monoclinic and triclinic crystalline structures for thin film and powdered WO3 were confirmed by XRD analysis. SEM micrograph of annealed samples revealed micro cracks due to a decrease in density and a contraction of layers. EDX analysis showed that 1∶2 ratio of oxygen and tungsten atoms in the prepared films is obtained at heat treatment temperatures higher than 200 °C. Furthermore, the annealed samples showed very good electrochromic behavior in cyclic voltammetery studies. Refractive index “n” and extinction coefficient “k” values were found to be reduced by increasing the wavelength and decreasing the temperature.
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