Sol-gel synthesis and in vitro bioactivity of copper and zinc-doped silicate bioactive glasses and glass-ceramics.

Science.gov (United States)

Bejarano, Julian; Caviedes, Pablo; Palza, Humberto

2015-03-11

Metal doping of bioactive glasses based on ternary 60SiO2-36CaO-4P2O5 (58S) and quaternary 60SiO2-25CaO-11Na2O-4P2O5 (NaBG) mol% compositions synthesized using a sol-gel process was analyzed. In particular, the effect of incorporating 1, 5 and 10 mol% of CuO and ZnO (replacing equivalent quantities of CaO) on the texture, in vitro bioactivity, and cytocompatibility of these materials was evaluated. Our results showed that the addition of metal ions can modulate the textural property of the matrix and its crystal structure. Regarding the bioactivity, after soaking in simulated body fluid (SBF) undoped 58S and NaBG glasses developed an apatite surface layer that was reduced in the doped glasses depending on the type of metal and its concentration with Zn displaying the largest inhibitions. Both the ion release from samples and the ion adsorption from the medium depended on the type of matrix with 58S glasses showing the highest values. Pure NaBG glass was more cytocompatible to osteoblast-like cells (SaOS-2) than pure 58S glass as tested by 3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide (MTT) assay. The incorporation of metal ions decreased the cytocompatibility of the glasses depending on their concentration and on the glass matrix doped. Our results show that by changing the glass composition and by adding Cu or Zn, bioactive materials with different textures, bioactivity and cytocompatibility can be synthesized.

Processamento e caracterização de espumas vitrocerâmicas do sistema sncp (Sio2-Na2o-Cao-P2 O5 Processing and characterization of sncp (Sio2-Na2o-Cao-P2o5 glass-ceramic foams

Directory of Open Access Journals (Sweden)

Karoline Bastos Mundstock

2010-01-01

Full Text Available Glass-ceramics foams prepared from glasses of the SiO2-Na2O-CaO-P2O5 by replication process were obtained and characterized in terms of their chemical and physical properties by X-ray fluorescence, X-ray diffraction, laser diffraction, thermal analysis, density, mechanical strength, microstructural and cytotoxic analysis. The results showed that it is possible to produce glass-ceramic foams by the replication method with optimized properties but cytotoxic analysis indicates that the glass-ceramic foams are not bioactive materials. Mechanical strength values varying from 0.5 to 1.0 MPa and from 0.8 to 2.3 MPa were reached for mean particle sizes of 10 and 6 µm, respectively.

Luminescence and circularly polarized luminescence of macrocyclic Eu(III) and Tb(III) complexes embedded in xerogel and sol-gel SiO2 glasses

International Nuclear Information System (INIS)

Morita, M.; Rau, D.; Kai, T.

2002-01-01

Luminescence, time-resolved luminescence, circularly polarized luminescence (CPL) and decay profiles of Ln(III)(15-crownether-5) (Ln=Ce, Sm, Eu, Tb) and Tb(III)-(R),(S)-cyclen derivative complexes doped in xerogel and sol-gel silica glasses are measured at temperatures down to 10 K to characterize luminescence properties and the electronic structure in the excited states. Luminescence spectral profiles and calculation of crystal field parameters (B 0 (2) ,B 2 (2) ) in the 5 D 0 → 7 F J (J=1,2) transition give evidence of the fact that the pentagonal and planar structure of Eu(III) (15-crownether-5) does hold in xerogel and sol-gel glasses prepared at temperatures below 100 deg. C. As annealing temperatures are increased from 80 deg. C to 750 deg. C, Eu(III) complexes in sol-gel glasses are found to decompose gradually to SiO 2 :Eu 3+ . Tb(III)-(R) and (S)-cyclen derivative complexes in xerogel reveal at room temperature and 10 K sharp CPL spectra with luminescence dissymmetry factors g lum =-0.1 and 0.1, respectively. These complexes doped in sol-gel glasses represent luminescence characteristics of rare earth ions encapsulated in the nano-porous host

The influence of precursor addition order on the porosity of sol-gel bioactive glasses.

Science.gov (United States)

Fernando, Delihta; Colon, Pierre; Cresswell, Mark; Journet, Catherine; Pradelle-Plasse, Nelly; Jackson, Phil; Grosgogeat, Brigitte; Attik, Nina

2018-06-16

The superior textural properties of sol-gel derived bioactive glasses compared to conventional melt quench glasses accounts for their accelerated bioactivity in vitro. Several studies have explored ways to improve the surface properties of sol-gel glasses in order to maximise their efficiency for bone and tooth regeneration. In this study, we investigated the effect of order of network modifying precursor addition on the textural properties of sol-gel derived bioactive glasses. The effect of precursor addition order on the glass characteristics was assessed by switching the order of network modifying precursor (calcium acetate monohydrate and sodium acetate anhydrous) addition for a fixed composition of bioactive glass (75SiO 2 :5CaO:10Na 2 O:10P 2 O 5 ). The results of this study showed that the order of precursor addition does influence the porosity of these glasses. For the glasses of a fixed composition and preparation conditions we achieved a doubling of surface area, a 1.5 times increase in pore volume and a 1.2 times decrease in pore size just by the mixing the network modifying precursors and adding them together in the sol-gel preparation. This simple and straightforward route adaptation to the preparation of bioactive glasses would allow us to enhance the textural properties of existing and novel composition of bioactive glasses and thus accelerate their bioactivity. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

Biological influence of Ca/P ratio on calcium phosphate coatings by sol-gel processing.

Science.gov (United States)

Catauro, M; Papale, F; Sapio, L; Naviglio, S

2016-08-01

The objective of this work has been to develop low temperature sol-gel glass coatings to modify the substrate surface and to evaluate their bioactivity and biocompatibility. Glasses, based on SiO2·CaO·P2O5, were synthesized by the sol-gel technique using tetraethyl orthosilicate, calcium nitrate tetrahydrate and triethyl phosphate as precursors of SiO2, CaO and P2O5, respectively. Those materials, still in the sol phase, have been used to coat substrates by means of the dip-coating technique. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) has been used for characterize coatings and a microstructural analysis has been obtained using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated substrate was immersed in simulated body fluid (SBF) for 21days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. In order to study the cell behavior and response to our silica based materials, prepared via the sol-gel method, with various Ca/P ratio and coating substrate, we have used the human osteoblast-like U2OS cell line. Copyright © 2016 Elsevier B.V. All rights reserved.

Electronic states of SiO2-MxOy (MxOy=P205, TiO2 and ZrO2) glasses

Energy Technology Data Exchange (ETDEWEB)

Kowada, Y [Hyogo Univ. of Teacher Education, Hyogo (Japan); Adachi, H [Kyoto Univ. (Japan). Faculty of Engineering; Minami, T [Univ. of Osaka Prefecture, Osaka (Japan). Faculty of Engineering

1993-12-01

Using the sol-gel method the surface of metal and glass substrates can be modified. For example, stainless steel sheets coated with the SiO2-ZrO2 glass films have higher resistance to corrosion and oxidation. The coating films contain high concentration of alkali ions diffusing from the glass substrates. It suggests that the sodium ions are trapped strongly within the coating films and are blocked to further diffuse to the surface. This behavior must be associated with the chemical bonding around the sodium ions in the SiO2-TiO2 and SiO2-ZrO2 films. For better understanding of the chemical bonding in the glasses, the electronic states of the SiO2-MxOy glasses were calculated by means of the DV-Xa cluster method. In this paper, the calculation method is explained, the results are discussed and the conclusion is stated. 17 refs., 6 figs.

Investigation of the effect of doping of Cr2O3 on bioactivity properties of the SiO2-CaO-P2O5 bioceramics

Science.gov (United States)

Sarin, Nonita; Singh, K. J.; Kaur, Kulwinder; Anand, Vikas; Kaur, Raminderjit; Singh, Jatinder

2018-05-01

Due to better biocompatibility among various types of biomaterials, bioceramics have been found to be useful for the repair of damaged bone tissues. Authors have prepared bioceramics of the composition xCr2O3-(40-x) SiO2- 40CaO-20P2O5(where, x = 0 and 2 mole %) by using sol gel technique. Prepared samples have been assessed for their bioactivity and cell viability with the help of X-ray diffraction, Fourier transform infrared and MG63 cell line. The aim of this study is to estimate the practical utility of the prepared samples as successful implant materials in human body.

The influence of SiO2 Addition on 2MgO-Al2O3-3.3P2O5 Glass

DEFF Research Database (Denmark)

Larsen, P.H.; Poulsen, F.W.; Berg, Rolf W.

1999-01-01

2MgO-Al2O3-3.3P2O5 glasses with increasing amounts of SiO2 are considered for sealing applications in Solid Oxide Fuel Cells (SOFC). The change in chemical durability under SOFC anode conditions and the linear thermal expansion is measured as functions of the SiO2 concentration. Raman spectroscopy...... analysis of the glasses reveals no sign of important changes in the glass structure upon SiO2 addition. Some increase in glass durability with SiO2 concentration is reported and its cause is discussed....

Making MgO/SiO2 Glasses By The Sol-Gel Process

Science.gov (United States)

Bansal, Narottam P.

1989-01-01

Silicon dioxide glasses containing 15 mole percent magnesium oxide prepared by sol-gel process. Not made by conventional melting because ingredients immiscible liquids. Synthesis of MgO/SiO2 glass starts with mixing of magnesium nitrate hexahydrate with silicon tetraethoxide, both in alcohol. Water added, and transparent gel forms. Subsequent processing converts gel into glass. Besides producing glasses of new composition at lower processing temperatures, sol-gel method leads to improved homogeneity and higher purity.

First Measurements of Time-Dependent Nucleation as a Function of Composition in Na2O.2CaO.3SiO2 Glasses

Science.gov (United States)

Kelton, K. F.; Narayan, K. Lakshmi

1996-01-01

The first measurements in any system of the composition dependence of the time-dependent nucleation rate are presented Nucleation rates of the stoichiometric crystalline phase, Na2O.2CaO.3SiO2, from quenched glasses made with different SiO2 concentrations were determined as a function of temperature and glass composition. A strong compositional dependence of the nucleation rates and a weak dependence for the induction times are observed. Using measured values of the liquidus temperatures and growth velocities as a function of glass composition, these data are shown to be consistent with predictions from the classical theory of nucleation, assuming a composition-dependent interfacial energy.

Gels and gel-derived glasses in the system Na2O-B2O3-SiO2

Science.gov (United States)

Mukherjee, S. P.

1983-01-01

The containerless melting of high-purity multicomponent homogeneous gels and gel monoliths offers a unique approach to making ultrapure multicomponent optical glasses in the reduced gravity environment of space. Procedures for preparing and characterizing gels and gel-derived glasses in the system Na2O-B2O3-SiO2 are described. Preparation is based on the polymerization reactions of alkoxysilane with trimethyl borate or boric acid and a suitable sodium compound. The chemistry of the gelling process is discussed in terms of process parameters and the gel compositions. The physicochemical nature of gels prepared by three different procedures was found to be significantly different. Infrared absorption spectra indicate finite differences in the molecular structures of the different gels. The melting of the gel powders and the transformation of porous gel monoliths to transparent 'glass' without melting are described.

Synthesis and characterization of erbium-doped SiO2-TiO2 thin films prepared by sol-gel and dip-coating techniques onto commercial glass substrates as a route for obtaining active GRadient-INdex materials

International Nuclear Information System (INIS)

Gómez-Varela, Ana I.; Castro, Yolanda; Durán, Alicia; De Beule, Pieter A.A.; Flores-Arias, María T.; Bao-Varela, Carmen

2015-01-01

In this work, SiO 2 -TiO 2 films doped with erbium were prepared by dip-coating sol-gel process onto commercial glass substrates. The surface morphology of the films was characterized using atomic force microscopy, while thickness, refractive index, extinction coefficient and porosity of the films were determined by ellipsometric measurements in a wavelength region of 400-1000 nm. Optical constants and porosity were found to vary with erbium concentration. The proof of principle presented in this paper is applicable to systems of different nature by tailoring the sol-gel precursors in such a way that active GRadient-INdex media described by a complex, parabolic-like refractive index distribution for beam shaping purposes is obtained. - Highlights: • Sol-gel route for preparation of active GRadient-INdex materials is proposed. • SiO 2 -TiO 2 films doped with erbium were prepared by dipping onto commercial glasses. • Morphological and optical characterization of the samples was performed. • Optical constants and porosity were found to vary with erbium concentration. • Refractive index diminishes with dopant content; the contrary occurs for porosity

Ultralow-density SiO2 aerogels prepared by a two-step sol-gel process

International Nuclear Information System (INIS)

Wang Jue; Li Qing; Shen Jun; Zhou Bin; Chen Lingyan; Jiang; Weiyang

1996-01-01

Low density SiO 2 gels are prepared by a two-step sol-gel process from TEOS. The influence of various solution ratios on the gelation process is investigated. The comparative characterization of gels using different solvent, such as ethanol, acetone and methyl cyanide, is also given. The ultralow-density SiO 2 aerogels with density less than 10 kg/m 3 are prepared by CO 2 supercritical drying technique. The structure difference between SiO 2 aerogels prepared by conventional single-step process and the two-step process is also presented

Sol-gel synthesis of TiO2-SiO2 photocatalyst for β-naphthol photodegradation

International Nuclear Information System (INIS)

Qourzal, S.; Barka, N.; Tamimi, M.; Assabbane, A.; Nounah, A.; Ihlal, A.; Ait-Ichou, Y.

2009-01-01

Silica gel supported titanium dioxide particles (TiO 2 -SiO 2 ) prepared by sol-gel method was as photocatalyst in the degradation of β-naphthol in water under UV-illumination. The prepared sample has been characterized by powder X-ray diffraction (XRD), infrared spectroscopy (IR) and scanning electron microscopy (SEM). The supported catalyst had large surface area and good sedimentation ability. The photodegradation rate of β-naphthol under UV-irradiation depended strongly on adsorption capacity of the catalyst, and the photoactivity of the supported catalyst was much higher than that of the pure titanium dioxides. The experiments were measured by high performance liquid chromatography (HPLC). The photodegradation rate of β-naphthol using 60% TiO 2 -SiO 2 particles was faster than that using TiO 2 'Degussa P-25', TiO 2 'PC-50' and TiO 2 'Aldrich' as photocatalyst by 2.7, 4 and 7.8 times, respectively. The kinetics of photocatalytic β-naphthol degradation was found to follow a pseudo-first-order rate law. The effect of the TiO 2 loading on the photoactivity of TiO 2 -SiO 2 particles was also discussed. With good photocatalytic activity under UV-irradiation and the ability to be readily separated from the reaction system, this novel kind of catalyst exhibited the potential effective in the treatment of organic pollutants in aqueous systems.

Resistencia al desgaste de recubrimientos sol-gel de SiO2 y SiO2 - ZrO2 sobre materiales vitrocerámicos obtenidos por sinterización

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Soares, V. O.

2013-10-01

Full Text Available The sol-gel process is widely used to obtain coatings on glass-ceramic substrates in order to improve the scratch and abrasion resistance, also providing a bright and homogeneous appearance of a glaze avoiding expensive final polishing treatments. This paper describes the preparation of silica and silica / zirconia coatings by sol-gel method on Li2O-Al2O3-SiO2 (LAS glassceramic substrates produced by sintering. The coatings were deposited by dip-coating on LAS substrates and characterized by optical microscopy and spectral ellipsometry. On the other hand, hardness and elastic modulus, coefficient of friction and abrasion and scratch resistance of the coatings were determined and compared with the substrate properties. Coatings deposited on LAS glass-ceramic confere the substrate a bright and homogeneous aspect, similar to a glaze, improving the appearance and avoiding the final polishing. However these coatings do not increase the scratch resistance of the substrate only equaling the properties of the glass-ceramic.El proceso sol-gel es un método interesante para la producción de recubrimientos vítreos sobre sustratos vitrocerámicos con el fin de mejorar su resistencia al rayado y al desgaste, y proporcionando además un aspecto homogéneo, vidriado y brillante que evite los costosos tratamientos finales de pulido. Este trabajo describe la preparación de recubrimientos de sílice y sílice/ circona por el método sol-gel sobre sustratos vitrocerámicos del sistema Li2O-Al2O3-SiO2 (LAS producidos por sinterización. Los recubrimientos se depositaron por la técnica de inmersión y se caracterizaron mediante microscopía óptica de luz reflejada y elipsometría espectral. Por otro lado, se determinó la dureza y el módulo de elasticidad, además del coeficiente de fricción, la resistencia al desgaste y al rayado de los recubrimientos. Estos resultados se compararon con las propiedades del sustrato sin recubrir. Las capas depositadas

Structural studies of gels and gel-glasses in the SiO2-GeO2 system using vibrational spectroscopy

Science.gov (United States)

Mukherjee, Shyama P.; Sharma, Shiv K.

1986-01-01

GeO2 gel and gels in the SiO2-GeO2 system synthesized by the hydrolytic polycondensation of metal alkoxides have been studied by infrared and Raman spectroscopic techniques. The molecular structures, hydroxyl contents, and crystallinity of gels and gel-glasses in relation to the thermal history and GeO2 concentration were investigated. The binary compositions having up to 70 mol percent GeO2 were examined.

Sol-Gel synthesis of MgO-SiO2 glass compositions having stable liquid-liquid immiscibility

Science.gov (United States)

Bansal, Narottam P.

1987-01-01

MgO-SiO2 glasses containing up to 15 mol % MgO, which could not have been prepared by the conventional glass melting method due to the presence of stable liquid-liquid immiscibility, were synthesized by the sol-gel technique. Clear and transparent gels were obtained from the hydrolysis and polycondensation of silicon tetraethoxide (TEOS) and magnesium nitrate hexahydrate when the water/TEOS mole ratio was four or more. The gelling time decreased with increase in magnesium content, water/TEOS ratio, and reaction temperature. Magnesium nitrate hexahydrate crystallized out of the gels containing 15 and 20 mol % MgO on slow drying. This problem was partially alleviated by drying the gels quickly at higher temperatures. Monolithic gel samples were prepared using glycerol as the drying control additive. The gels were subjected to various thermal treatments and characterized by several methods. No organic groups could be detected in the glasses after heat treatments to approx. 800 C, but trace amounts of hydroxyl groups were still present. No crystalline phase was found from X-ray diffraction in the gel samples to approx. 890 C. At higher temperatures, alpha quartz precipitated out as the crystalline phase in gels containing up to 10 mol % MgO. The overall activation energy for gel formation in 10MgO-90SiO2 (mol %) system for water/TEOS mole ratio of 7.5 was calculated to be 58.7 kJ/mol.

Microstructural dependence on relevant physical-mechanical properties on SiO2-Na2O-CaO-P2O5 biological glasses.

Science.gov (United States)

Rajendran, V; Begum, A Nishara; Azooz, M A; el Batal, F H

2002-11-01

Bioactive glasses of the system SiO2-Na2O-CaO-P2O5 have been prepared by the normal melting and annealing technique. The elastic moduli, attenuation, Vickers hardness, fracture toughness and fracture surface energy have been obtained using the known method at room temperature. The temperature dependence of elastic moduli and attenuation measurements have been extended over a wide range of temperature from 150 to 500 K. The SiO2 content dependence of velocities, attenuation, elastic moduli, and other parameters show an interesting observation at 45 wt% of SiO2 by exhibiting an anomalous behaviour. A linear relation is developed for Tg, which explores the influence of Na2O on SiO2-Na2O-CaO-P2O5 bioactive glasses. The measured hardness, fracture toughness and fracture surface energy show a linear relation with Young's modulus. It is also interesting to note that the observed results are functions of polymerisation and the number of non-bridging oxygens (NBO) prevailing in the network with change in SiO2 content. The temperature dependence of velocities, attenuation and elastic moduli show the existence of softening in the glass network structure as temperature increases.

Evaluation of sol-gel based magnetic 45S5 bioglass and bioglass-ceramics containing iron oxide.

Science.gov (United States)

Shankhwar, Nisha; Srinivasan, A

2016-05-01

Multicomponent oxide powders with nominal compositions of (45-x)·SiO2·24.5CaO·24.5Na2O·6P2O5xFe2O3 (in wt.%) were prepared by a modified sol-gel procedure. X-ray diffraction (XRD) patterns and high resolution transmission electron microscope images of the sol-gel products show fully amorphous structure for Fe2O3 substitutions up to 2 wt.%. Sol-gel derived 43SiO2·24.5CaO·24.5Na2O·6P2O5·2Fe2O3 glass (or bioglass 45S5 with SiO2 substituted with 2 wt.% Fe2O3), exhibited magnetic behavior with a coercive field of 21 Oe, hysteresis loop area of 33.25 erg/g and saturation magnetization of 0.66 emu/g at an applied field of 15 kOe at room temperature. XRD pattern of this glass annealed at 850 °C for 1h revealed the formation of a glass-ceramic containing sodium calcium silicate and magnetite phases in nanocrystalline form. Temperature dependent magnetization and room temperature electron spin resonance data have been used to obtain information on the magnetic phase and distribution of iron ions in the sol-gel glass and glass-ceramic samples. Sol-gel derived glass and glass-ceramic exhibit in-vitro bioactivity by forming a hydroxyapatite surface layer under simulated physiological conditions and their bio-response is superior to their melt quenched bulk counterparts. This new form of magnetic bioglass and bioglass ceramics opens up new and more effective biomedical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Optical properties of ZrO2, SiO2 and TiO2-SiO2 xerogels and coatings doped with Eu3+ and Eu2+

Directory of Open Access Journals (Sweden)

Gonçalves Rogéria R.

1999-01-01

Full Text Available Eu3+ doped bulk monoliths and thin films were obtained by sol-gel methods in the ZrO2, SiO2 and SiO2-TiO2 systems. Eu3+ 5D0 ® 7FJ emission and decay time characteristics were measured during the entire experimental preparation route from the initial sol to the final xerogels. The crystalline phases identified were tetragonal ZrO2 and mixtures of rutile and anatase TiO2 at high temperature treatments in bulk samples. Good quality thin films were obtained for all systems by dip-coating optical glasses (Schott BK270. The same spectroscopic features were observed either for the bulk monoliths or the films. By appropriate heat treatments under H2 atmosphere Eu2+ containing samples could be obtained in the SiO2-TiO2 system.

The effect of serum proteins on apatite growth for 45S5 Bioglass and common sol-gel derived glass in SBF

Directory of Open Access Journals (Sweden)

Lin Sen

2018-02-01

Full Text Available The inhibitive effects of serum proteins on apatite growth was compared between melt-derived 45S5 Bioglass® and sol-gel derived bioactive glass of the 70S30C (70 mol% SiO2, 30 mol% CaO. By using techniques of XRD, TEM and Raman spectroscopy, the transformation of amorphous calcium phosphate to crystalline apatite, and the resulting size and aspect ratio of the crystals, in simulated body fluid (SBF, was seen to decrease in the presence of serum. XRD showed more rapid HA formation on Bioglass particles, compared to that forming on 70S30C particles, however TEM showed similar size and frequency of the needle-like crystals. Phosphate reduction in SBF was similar for Bioglass and 70S30C. Calcium carbonate formation was more likely on the phosphate-free sol-gel glass than on Bioglass.

Gels and gel-derived glasses in the Na2O-B2O3-SiO2 system. [containerless melting in space

Science.gov (United States)

Mukherjee, S. P.

1982-01-01

The containerless melting of high-purity multicomponent homogeneous gels and gel-monoliths offers a unique approach to making ultrapure multicomponent optical glasses in the reduced gravity environment of space. Procedures for preparing and characterizing gels and gel-derived glasses in the Na2O-B2O3-SiO2 system are described. Preparation is based on the polymerization reactions of alkoxysilane with trimethyl borate or boric acid and a suitable sodium compound. The chemistry of the gelling process is discussed in terms of process parameters and the gel compositions. The physicochemical nature of gels prepared by three different procedures were found to be significantly different. IR absorption spectra indicate finite differences in the molecular structures of the different gels. The melting of the gel powders and the transformation of porous gel-monoliths to transparent 'glass' without melting are described.

Incorporation of sol-gel SnO2:Sb into nanoporous SiO2

International Nuclear Information System (INIS)

Canut, B.; Blanchin, M.G.; Ramos-Canut, S.; Teodorescu, V.; Toulemonde, M.

2006-01-01

Silicon oxide films thermally grown on Si(1 0 0) wafers were irradiated with 200 MeV 197 Au ions in the 10 9 -10 1 cm -2 fluence range. The targets were then etched at room temperature in aqueous HF solution (1 vol.%) for various durations. Atomic force microscopy (AFM) in the tapping mode was used to probe the processed surfaces. Conical holes with a low size dispersion were evidenced. Their surface diameter varies between 20 and 70 nm, depending on the etching time. Sol-gel dip coating technique, associated with a further annealing treatment performed at 500 o C for 15 min, was used to fill the nanopores created in SiO 2 with a transparent conductive oxide (SnO 2 doped with antimony). Transmission electron microscopy (TEM) performed on cross-sectional specimen showed that SnO 2 :Sb crystallites of ∼5 nm mean size are trapped in the holes without degrading their geometry

Investigation of bioactive CaO-P2O5-MgO-SiO2 ceramic composition for orthopedic applications

Science.gov (United States)

Kaur, Pardeep; Singh, K. J.; Sood, Henna; Arora, Daljit Singh

2017-05-01

Bioactive sample of the composition 41CaO-8P2O5-17MgO-34SiO2 has been prepared in the laboratory by quick alkali mediated sol-gel method. 1M ammonia solution has been used to form the gel. Bioactivity of the sample has been analyzed by soaking the samples in simulated body fluid. Degradation study has also undertaken to check the degradation behavior of the sample. MTT cytotoxic test has also been done to know the toxicity of the sample and results show that samples has good percentage of cell viability in the cell culture media. Formation of the hydroxyapatite has been confirmed by the XRD, Raman spectroscopy and FESEM-EDX study.

Analysis of bioactive glasses obtained by sol-gel processing for radioactive implants

Directory of Open Access Journals (Sweden)

Roberto Wanderley dos Santos

2003-01-01

Full Text Available This paper presents the chemical and physical characterizations of SiO2 and SiO2-CaO bioactive glasses incorporated with samarium atoms, produced by sol-gel synthesis. The objective is to provide biocompatible and biodegradable radioactive seeds as an alternative to be used in Brachytherapy for the treatment of prostate cancer. The glasses were produced and analyzed by X-ray fluorescence spectroscopy (XRF, energy dispersive X-ray spectroscopy (EDS, scanning electron microscopy (SEM, He picnometry and nitrogen adsorption analysis. A theoretical evaluation of the specific activity of the samples upon neutron activation is proposed. The XRF and EDS results demonstrate the incorporation of samarium atoms in the glass matrix. The experimental data coupled with the theoretical studies in neutron activation suggest that it is possible to obtain radioactive seeds with activities equivalent to 125I seeds used in brachytherapy prostatic.

Sol-Gel Glasses

Science.gov (United States)

Mukherjee, S. P.

1985-01-01

Multicomponent homogeneous, ultrapure noncrystalline gels/gel derived glasses are promising batch materials for the containerless glass melting experiments in microgravity. Hence, ultrapure, homogeneous gel precursors could be used to: (1) investigate the effect of the container induced nucleation on the glass forming ability of marginally glass forming compositions; and (2) investigate the influence of gravity on the phase separation and coarsening behavior of gel derived glasses in the liquid-liquid immiscibility zone of the nonsilicate systems having a high density phase. The structure and crystallization behavior of gels in the SiO2-GeO2 as a function of gel chemistry and thermal treatment were investigated. As are the chemical principles involved in the distribution of a second network former in silica gel matrix being investigated. The procedures for synthesizing noncrystalline gels/gel-monoliths in the SiO2-GeO2, GeO2-PbO systems were developed. Preliminary investigations on the levitation and thermal treatment of germania silicate gel-monoliths in the Pressure Facility Acoustic Levitator were done.

Heat treatment of Na2O-CaO-P2O5-SiO2 bioactive glasses: densification processes and postsintering bioactivity.

Science.gov (United States)

Sola, A; Bellucci, D; Raucci, M G; Zeppetelli, S; Ambrosio, L; Cannillo, V

2012-02-01

Because of their excellent bioactivity, bioactive glasses are increasingly diffused to produce biomedical devices for bone prostheses, to face the dysfunctions that may be caused by traumatic events, diseases, or even natural aging. However, several processing routes, such as the production of scaffolds or the deposition of coatings, include a thermal treatment to apply or sinter the glass. The exposure to high temperature may induce a devetrification phenomenon, altering the properties and, in particular, the bioactivity of the glass. The present contribution offers an overview of the thermal behavior and properties of two glasses belonging to the Na2O-CaO-P2O5-SiO2 system, to be compared to the standard 45S5 Bioglass(®). The basic goal is to understand the effect of both the original composition and the thermal treatment on the performance of the sintered glasses. The new glasses, the one (BG_Na) with a high content of Na2O, the other (BG_Ca) with a high content of CaO, were fully characterized and sintering tests were performed to define the most interesting firing cycles. The sintered samples, treated at 880°C and 800°C respectively, were investigated from a microstructural point of view and their mechanical properties were compared to those of the bulk (not sintered) glass counterparts. The effect of sintering was especially striking on the BG_Ca material, whose Vickers hardness increased from 598.9 ± 46.7 HV to 1053.4 ± 35.0 HV. The in vitro tests confirmed the ability of the glasses, both in bulk and sintered form, of generating a hydroxyapatite surface layer when immersed in a simulated body fluid. More accurate biological tests performed on the sintered glasses proved the high bioactivity of the CaO-rich composition even after a heat treatment. Copyright © 2011 Wiley Periodicals, Inc.

Bending strength of glass-ceramics based on 3CaO.P2O5-SiO2-MgO glass system

International Nuclear Information System (INIS)

Daguano, J.K.M.F.; Suzuki, P.A.; Santos, C.; Fernandes, M.H.V.; Elias, C.N.

2009-01-01

In this work, the Modulus of Rupture of bioactive glass-ceramic based on 3CaO.P 2 O 5 -SiO 2 -MgO system was investigated, aiming its use in bone-restorations. The mechanical property was correlated with microstructural and crystallographic features of this material. High-purity starting-powders, CaCO 3 , SiO 2 , MgO, Ca (H 2 PO 4 ).H 2 O, were used in this study. The powders were mixed in a stoichiometric ratio, using planetary ball-mill. The suspensions were dried, sieved and melted at 1600 deg C, for 4h. The casting ones were cooled quickly until annealing temperature 700 deg C, in which remained for 2h, with controlled cooling-rate until ambient temperature. Bulks of glass were heat-treated with temperatures varying between 700 deg C and 1100 deg C, for 4h, being after that, cooled at 3 deg C/min. Bioactive glass and glass-ceramic were characterized by HRXRD (high resolution X-ray diffraction), where whitlockite was main phase. The microstructure was analyzed by scanning electronic microscopy. Modulus of Rupture was determined by four-point bending testing using specimens of 1.5 x 2 x 25 mm and glasses presented strength near to 70MPa, while glass ceramics treated at 975 deg C-4h, presented bending strength of 120MPa. (author)

Biological influence of Ca/P ratio on calcium phosphate coatings by sol-gel processing

Energy Technology Data Exchange (ETDEWEB)

Catauro, M., E-mail: michelina.catauro@unina2.it [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Papale, F. [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Sapio, L.; Naviglio, S. [Department of Biochemistry, Biophysics and General Pathology, Second University of Naples, Via L. De Crecchio 7, 80138 Naples (Italy)

2016-08-01

The objective of this work has been to develop low temperature sol-gel glass coatings to modify the substrate surface and to evaluate their bioactivity and biocompatibility. Glasses, based on SiO{sub 2}·CaO·P{sub 2}O{sub 5}, were synthesized by the sol-gel technique using tetraethyl orthosilicate, calcium nitrate tetrahydrate and triethyl phosphate as precursors of SiO{sub 2}, CaO and P{sub 2}O{sub 5}, respectively. Those materials, still in the sol phase, have been used to coat substrates by means of the dip-coating technique. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) has been used for characterize coatings and a microstructural analysis has been obtained using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated substrate was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. In order to study the cell behavior and response to our silica based materials, prepared via the sol-gel method, with various Ca/P ratio and coating substrate, we have used the human osteoblast-like U2OS cell line. - Highlights: • Coatings consisting of SiO{sub 2}·CaO·P{sub 2}O{sub 5} glasses were prepared via sol-gel dip coating. • Ca/P molar ratio affects the film morphology and biocompatibility. • Higher cell proliferation was found in response to higher Ca/P ratios coatings. • A growth cell proliferation inhibition was observed in response to lower Ca/P ratio.

Crystallization behaviour of nanostructured hybrid SiO2-TiO2 gel glasses to nanocomposites.

Science.gov (United States)

Tsvetelina, Gerganova; Yordanka, Ivanova; Yuliya, Vueva; Miranda, Salvado Isabel M; Helena, Fernandes Maria

2010-04-01

The crystallization behaviour of hybrid SiO2-TiO2 nanocomposites derived from titanosiloxanes by sol-gel method has been investigated depending on the type of siloxane precursor and the pirolysis temperature. The resulting hybrid titanosiloxanes, crosslinked with trimethylsilil isocyanate (nitrogen-modified) or methyltrietoxisilane (carbon-modified), were pirolyzed in an inert atmosphere in the temperature range between 600 to 1100 degrees C in order to form C-(N)-Si-O-TiO2 nanocomposites. By means of XRD, FTIR, 29Si NMR, SEM, TEM and AFM investigations have been established that the transformation of the nanostructured SiO2-TiO2 hybrid materials into nanocomposites as well as the crystalline size depend on the titanium content and the type of cross-linking agents used in the synthesizes.

Study of absorption, emission and EDS properties of Pr3+ incorporated in a SiO2 matrix by sol-gel method

International Nuclear Information System (INIS)

Gómez-Miranda, M; Fonseca, R Sosa; Ordoñez, C Velásquez

2015-01-01

The optical response of the Pr 3+ ions doped monolith of SiO 2 prepared by sol-gel method was investigated by absorption and emission spectra. The absorption spectrum shows some typical lines of Pr 3+ , with these data was made the diagram levels corresponding to SiO 2 : Pr 3+ . The emission spectra were taken at 225 nm and 240 nm of wavelength of excitation was measured. In that there are reabsorption line at 423 of the Pr 3+ ions in the emission host, that means that some kind of host-ion interactions exist. Red and NIR emission at 612 nm, 652 nm, 711 and 728 nm, respectively, from Pr 3+ ions in SiO 2 was observed. The transition 1 S 0 → 3 P 2 at 425 nm is observed because an effective radiative transfer between the silicate glasses host and the praseodymium ions is observed and discussed

Structural aspects of B2O3-substituted (PbO)0.5(SiO2)0.5 glasses

International Nuclear Information System (INIS)

Sudarsan, V.; Kulshreshtha, S.K.; Shrikhande, V.K.; Kothiyal, G.P.

2002-01-01

Lead borosilicate glasses having general formulae (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 ) x with 0.0≤x≤0.4 and (PbO) 0.5 (SiO 2 ) 0.5-y (B 2 O 3 ) y with 0.0≤y≤0.5 have been prepared by a conventional melt-quench method and characterized by 29 Si, 11 B magic angle spinning (MAS) NMR techniques and infrared spectroscopy, as regards their structural features. From 29 Si NMR results, it has been inferred that with increasing concentration of boron oxide, (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 )x glasses exhibit a systematic increase in the number of Q 4 structural units of Si at the expense of Q 2 structural units, along with the formation of Si-O-B linkages. On the other hand, for (PbO) 0.5 (SiO 2 ) 0.5-y (B 2 O 3 ) y glasses, there is no direct interaction between SiO 2 and B 2 O 3 in the glass network, as revealed by the 29 Si MAS NMR studies. Boron exists in both trigonal and tetrahedral configurations for these two series of glasses and for the (PbO) 0.5 (SiO 2 ) 0.5-y (B 2 O 3 ) y series of glasses; the relative concentration of these two structural units remains almost constant with increasing B 2 O 3 concentration. In contrast, for (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 ) x glasses, there is a slight increase in the number of BO 3 structural units above x = 0.2, as there is a competition between SiO 2 and B 2 O 3 for interaction with Pb 2+ , thereby leading to the formation of BO 3 structural units. For both series of glasses, the thermal expansion coefficient is found to decrease with increasing B 2 O 3 concentration, the effect being more pronounced for the (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 ) x series of glasses due to the increased concentration of Q 4 structural units of silicon and better cross-linking as a result of the formation of Si-O-B-type linkages. (author)

Photoluminescence analysis of Ce3+:Zn2SiO4 & Li++ Ce3+:Zn2SiO4: phosphors by a sol-gel method

Science.gov (United States)

Babu, B. Chandra; Vandana, C. Sai; Guravamma, J.; Rudramadevi, B. Hemalatha; Buddhudu, S.

2015-06-01

Here, we report on the development and photoluminescence analysis of Zn2SiO4, Ce3+:Zn2SiO4 & Li+ + Ce3+: Zn2SiO4 novel powder phosphors prepared by a sol-gel technique. The total amount of Ce3+ ions was kept constant in this experiment at 0.05 mol% total doping. The excitation and emission spectra of undoped (Zn2SiO4) and Ce3+ doped Zn2SiO4 and 0.05 mol% Li+ co-doped samples have been investigated. Cerium doped Zn2SiO4 powder phosphors had broad blue emission corresponding to the 2D3/2→2FJ transition at 443nm. Stable green-yellow-red emission has been observed from Zn2SiO4 host matrix and also we have been observed the enhanced luminescence of Li+ co-doped Zn2SiO4:Ce3+. Excitation and emission spectra of these blue luminescent phosphors have been analyzed in evaluating their potential as luminescent screen coating phosphors.

Effect of SiO2/B2O3 Ratio on the Crystallization Behavior and Dielectric Properties of Barium Strontium Titanate Glass-Ceramics Prepared by Sol-Gel Process

Science.gov (United States)

Chen, Yongzhou; Zhang, Yong; Song, Xiaozhen; Shen, Ziqin; Zhang, Tianyuan

2018-05-01

Ferroelectric glass-ceramics, with a basic composition 90 wt.% (Ba0.65Sr0.35)TiO3-10 wt.% (B2O3-nSiO2) (n = 0.5, 1, 3, 5) were synthesized by the sol-gel method and their phase development and dielectric properties were investigated by differential thermal analysis, x-ray diffraction, field emission scanning electron microscopy, dielectric temperature curves and impedance spectroscopy. From the differential thermal analysis, glass transition and crystallization behavior can be observed. From the x-ray diffraction study, two crystalline phases (Ba,Sr)TiO3 and Ba2TiSi2O8 were formed over the entire composition range of the glass-ceramics. In addition, the main crystal phase has undergone a transformation from (Ba,Sr)TiO3 to Ba2TiSi2O8 with the increase of n. A typical structure in which the crystal phase was surrounded by a glassy matrix has been observed in the scanning electron microscope images. As a result of temperature dependent dielectric property measurements, the dielectric constant increased obviously with the increase of n from 0.5 to 1. Further increasing n led to a reduction of the dielectric constant, which is in coincidence with the variation of the intensity of (Ba,Sr)TiO3 phase with n. According to the impedance spectroscopy analysis and the activation energy calculation, the relaxation peak in both Z″ and M″ data should be attributed to the crystal-glass interface, and the change of conduction mechanism with the increase of SiO2/B2O3 ratio may be attributed to the corresponding transition of the main crystal phase.

Investigation on the utilization of ZrO2-SiO2 composite microspheres for Sr+2 sorption synthesized via sol-gel method

International Nuclear Information System (INIS)

Sert, S.; Tel, H.; Altas, Y.; Eral, M.; Cetinkaya, B.; Inan, S.; Kasap, S.

2009-01-01

Multivalence metal ion's oxides and hydro oxides show high adsorption capacity. These are selective to some kind of ions and show thermal, chemical and radiation resistance. Because of these properties they can be used as a adsorbent for radioactive waste management. It is known that the mix oxide's acidic and basic surface sides and textural (surface area, por side and volume) properties related to mix oxide composition. The previously works shown that the ZrO 2 have high adsorption capacity for Sr + 2. Additionally ZrO 2 is used in production of heat resistance materials, glass and ceramic industries due to it's high melting point. Generally inorganic adsorbents which are crystal forms have low surface area. It is needed that the materials have high surface area and appropriate por size to targeted molecules for take inside adsorbent, in the practical adsorption proses. It is thought that the addition of oxide which has high surface area ( SiO 2 etc.) to between material layer increase it's surface area. Some works showed that the silica increase surface area when mixed Ti in materials structure. Sol-jell proses is a method which is show homogen hetero metal oxide bounds distribution and give advantages to prepare multicomponent oxide materials. In this study, ZrO 2 -SiO 2 -TiO 2 composite microspheres were synthesized by sol-gel method. In synthesis proses; peristaltic pump, nozzle-vibrator system and glass column were used. The optimum Sr 2 + adsorption conditions were determined by 'Central Composite Design' (CCD). Thermodynamic parameters related to adsorption such as ΔHo, ΔSo and ΔGo were calculated. The adsorption data have been interpreted in terms of Langmuir, Freundlich and D-R isotherms.

Sol-Gel Synthesis and Luminescence of Green Light Emitting Phosphors Zn2SiO4/Mn2+

Institute of Scientific and Technical Information of China (English)

无

2006-01-01

Mn2+ doped Zn2SiO4 phosphors were synthesized by sol-gel method, and the influence of zinc source, Mn2+ dopant concentration and annealing temperature were investigated. Results show that zinc nitrate based precursor with strong green emission intensities is better than zinc acetate based precursor. The intensity of green light emission reaches a peak at 254 nm when the Mn2+ dopant concentration is about 5%( molar percentage). Structural details of the phosphors were examined through X-ray diffractometry, thermogravimetric and differential thermal analysis. The result indicates that they are both rhombohedral structures, which remain amorphous below 700 ℃and crystallize completely around 1 000℃. The luminescent properties of Zn2SiO4/Mn2+ phosphors were characterized by excitation and emission spectra.

Fe-Doped Sol-Gel Glasses and Glass-Ceramics for Magnetic Hyperthermia

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Francesco Baino

2018-01-01

Full Text Available This work deals with the synthesis and characterization of novel Fe-containing sol-gel materials obtained by modifying the composition of a binary SiO2-CaO parent glass with the addition of Fe2O3. The effect of different processing conditions (calcination in air vs. argon flowing on the formation of magnetic crystalline phases was investigated. The produced materials were analyzed from thermal (hot-stage microscopy, differential thermal analysis, and differential thermal calorimetry and microstructural (X-ray diffraction viewpoints to assess both the behavior upon heating and the development of crystalline phases. N2 adsorption–desorption measurements allowed determining that these materials have high surface area (40–120 m2/g and mesoporous texture with mesopore size in the range of 18 to 30 nm. It was assessed that the magnetic properties can actually be tailored by controlling the Fe content and the environmental conditions (oxidant vs. inert atmosphere during calcination. The glasses and glass-ceramics developed in this work show promise for applications in bone tissue healing which require the use of biocompatible magnetic implants able to elicit therapeutic actions, such as hyperthermia for bone cancer treatment.

Reflection Enhancement Using TiO2/SiO2 Bilayer Films Prepared by Cost-Effective Sol-gel Method

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R. Ajay Kumar

2017-04-01

Full Text Available Multilayer dielectric thin film structure has been demanded for its application in optoelectronic devices such as optical waveguides, vertical cavity surface-emitting devices, biosensors etc. In this paper, we present the fabrication and characterization of bilayer thin films of TiO2/SiO2 using sol-gel spin coating method. Ellipsometer measurement showed refractive index values 1.46, 2.1 corresponding to the SiO2 and TiO2 films respectively. The FTIR transmittance peaks observed at ~970 cm-1, ~1100 cm-1 and ~1400 cm-1 are attributed to the Ti-O-Si, Si-O-Si and Ti-O-Ti bonds respectively. Maximum reflectance is observed from two bilayer film structure which can be further optimized to get the high reflection to a broad wavelength range.

Understanding the magnetic behavior of heat treated CaO-P2O5-Na2O-Fe2O3-SiO2 bioactive glass using electron paramagnetic resonance studies

Science.gov (United States)

Shankhwar, Nisha; Kothiyal, G. P.; Srinivasan, A.

2014-09-01

Bioactive glass of composition 41CaO-44SiO2-4P2O5-8Fe2O3-3Na2O has been heat treated in the temperature (TA) range of 750-1150 °C for time periods (tA) ranging from 1 h to 3 h to yield magnetic bioactive glass ceramics (MBCs). X-ray diffraction studies indicate the presence of bone mineral (hydroxyapatite and wollastonite) and magnetic (magnetite and α-hematite) phases in nanocrystalline form in the MBCs. Electron paramagnetic resonance (EPR) study was carried out to understand the variation in saturation magnetization and coercivity of the MBCs with TA and tA. These studies reveal the nature and amount of iron ions present in the MBCs and their interaction in the glassy oxide matrix as a function of annealing parameters. The deterioration in the magnetic properties of the glass heat treated above 1050 °C is attributed to the crystallization of the non-magnetic α-hematite phase. These results are expected to be useful in the application of these MBCs as thermoseeds in hyperthermia treatment of cancer.

Compositional and microstructural design of highly bioactive P2O5-Na2O-CaO-SiO2 glass-ceramics.

Science.gov (United States)

Peitl, Oscar; Zanotto, Edgar D; Serbena, Francisco C; Hench, Larry L

2012-01-01

Bioactive glasses having chemical compositions between 1Na(2)O-2CaO-3SiO(2) (1N2C3S) and 1.5Na(2)O-1.5CaO-3SiO(2) (1N1C2S) containing 0, 4 and 6 wt.% P(2)O(5) were crystallized through two stage thermal treatments. By carefully controlling these treatments we separately studied the effects on the mechanical properties of two important microstructural features not studied before, crystallized volume fraction and crystal size. Fracture strength, elastic modulus and indentation fracture toughness were measured as a function of crystallized volume fraction for a constant crystal size. Glass-ceramics with a crystalline volume fraction between 34% and 60% exhibited a three-fold improvement in fracture strength and an increase of 40% in indentation fracture toughness compared with the parent glass. For the optimal crystalline concentration (34% and 60%) these mechanical properties were then measured for different grain sizes, from 5 to 21 μm. The glass-ceramic with the highest fracture strength and indentation fracture toughness was that with 34% crystallized volume fracture and 13 μm crystals. Compared with the parent glass, the average fracture strength of this glass-ceramic was increased from 80 to 210 MPa, and the fracture toughness from 0.60 to 0.95 MPa.m(1/2). The increase in indentation fracture toughness was analyzed using different theoretical models, which demonstrated that it is due to crack deflection. Fortunately, the elastic modulus E increased only slightly; from 60 to 70 GPa (the elastic modulus of biomaterials should be as close as possible to that of cortical bone). In summary, the flexural strength of our best material (215 MPa) is significantly greater than that of cortical bone and comparable with that of apatite-wollastonite (A/W) bioglass ceramics, with the advantage that it shows a much lower elastic modulus. These results thus provide a relevant guide for the design of bioactive glass-ceramics with improved microstructure. Copyright © 2011 Acta

The phenomenon of phase separated in Na2O-B2O3-SiO2, Na2O-SiO2-P2O5 glasses

International Nuclear Information System (INIS)

Procyk, B.; Bieniarz, P.; Plichta, E.; Pudelek, B.; Kucinski, G.; Staniewicz-Brudnik, B.

1997-01-01

During the thermal treatment, the phenomenon of phase separation has been observed in the some glasses. The glass has became opaque, due to the opalescence of phase separated. Investigations of the phenomenon of phase separation were conducted using the basic systems: Na 2 O-B 2 O 3 -SiO 2 , Na 2 O-SiO 2 -P 2 O 5 and theirs modifications. The occurrence of binodal and spinodal phase decomposition was observed by TEM. The phase separation inhomogeneities have drop-like character and with higher concentration shows a tendency for coalescence. The influence of the chemical composition, temperature and time on the phenomenon of phase separation in the investigated glasses has been defined. (author)

Synthesis, structural, spectroscopic and thermoanalytical study of sol–gel derived SiO{sub 2}–CaO–P{sub 2}O{sub 5} gel and ceramic materials

Energy Technology Data Exchange (ETDEWEB)

Catauro, Michelina, E-mail: michelina.catauro@unina2.it [Department of Industrial and Information Engineering, Second University of Naples, via Roma 29, Aversa (CE) (Italy); Dell’Era, Alessandro [Department D.M.E., ‘Guglielmo Marconi’ University, via Plinio 44, Roma (Italy); Vecchio Ciprioti, Stefano, E-mail: stefano.vecchio@uniroma1.it [Department S.B.A.I., Sapienza University of Rome, via del Castro Laurenziano 7, Roma (Italy)

2016-02-10

Highlights: • Four different SiO{sub 2}–CaO–P{sub 2}O{sub 5} gel-glasses were synthesized by the sol–gel method. • FTIR, XRD, SEM-EDS and TG/DTA techniques were used to fully characterize the gels. • Integral isoconversional OFW method was used to study dehydration kinetics. • Appropriate temperatures of 600 and 1200 °C were chosen to thermally treat them. • All amorphous gels at 1200 °C crystallize as wollastonite and pseudowollastonite. - Abstract: In the present work bioactive powders of the ternary SiO{sub 2}·CaO·P{sub 2}O{sub 5} systems, which differ in the Ca/P molar ratio, were synthesized by means of a sol–gel route, using tetraethyl orthosilicate (TEOS, Si(OC{sub 2}H{sub 5}){sub 4}), calcium nitrate tetrahydrate (Ca(NO{sub 3}){sub 2}·4H{sub 2}O) and triethyl phosphate (TEP, OP(OC{sub 2}H{sub 5}){sub 3}) as precursors of SiO{sub 2}, CaO and P{sub 2}O{sub 5}, respectively. In order to investigate the influence of the relative amount of each phase (in this study: SiO{sub 2}, CaO and P{sub 2}O{sub 5}) the thermal properties of the synthesized gel-glass materials were studied as a function of the Ca/P molar ratio using thermogravimetric and differential thermal analysis (TG/DTA). After dehydration (in a single step), described from a kinetic point of view as a simple water evaporation without rupture of chemical bonds, all gels undergo a complex multi-step decomposition with endo and exothermic effects, followed by crystallization of calcium silicate phases at about 950 °C. Furthermore, Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD) and Scanning Electron Microscopy, coupled with energy dispersive spectroscopy (SEM/EDS), allowed us to detect the chemical modifications induced by modifying the Ca/P molar ratio and the sintering. This process is obtained by thermal treatment of the gel-glass precursors after analyzing their thermal behavior in the temperature range 600–1000 °C, with the aim to convert them into

Sol-Gel Synthesis of Phosphate-Based Glasses for Hydrophilic Enamel Applications

International Nuclear Information System (INIS)

Kim, Dae-Sung; Ryu, Bong-ki

2017-01-01

In this study, quaternary phosphate-based sol-gel derived glasses were synthesized from a P 2 O 5 -CaO-Na 2 O-TiO 2 system with a high TiO 2 content of up to 50 mol%. The sol-gel method was chosen because incorporating a high percentage of titanium into a phosphate network via traditional melt-quench methods is non-trivial. The structure and thermal properties of the obtained stabilized sol-gel glasses were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and differential scanning calorimetry (DSC). The XRD results confirmed the amorphous nature of all of the stabilized sol–gel derived glasses. The FTIR results revealed that added TiO 2 enters the network as (TiO 6 ), which likely acts as a modifier oxide. Consequently, the number of terminal oxygen atoms increases, leading to an increase in the number of P-OH bonds. In addition, DSC results confirmed a decrease in glass transition and crystallization temperatures with increasing TiO 2 content. This is the first report of a sol-gel synthesis strategy combined with enameling to prepare glass at low processing temperatures and the first use of such a system for both hydrophilic and chemical resistance purposes.

Sol-Gel Synthesis of Phosphate-Based Glasses for Hydrophilic Enamel Applications

Energy Technology Data Exchange (ETDEWEB)

Kim, Dae-Sung; Ryu, Bong-ki [Pusan National University, Busan (Korea, Republic of)

2017-04-15

In this study, quaternary phosphate-based sol-gel derived glasses were synthesized from a P{sub 2}O{sub 5}-CaO-Na{sub 2}O-TiO{sub 2} system with a high TiO{sub 2} content of up to 50 mol%. The sol-gel method was chosen because incorporating a high percentage of titanium into a phosphate network via traditional melt-quench methods is non-trivial. The structure and thermal properties of the obtained stabilized sol-gel glasses were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and differential scanning calorimetry (DSC). The XRD results confirmed the amorphous nature of all of the stabilized sol–gel derived glasses. The FTIR results revealed that added TiO{sub 2} enters the network as (TiO{sub 6}), which likely acts as a modifier oxide. Consequently, the number of terminal oxygen atoms increases, leading to an increase in the number of P-OH bonds. In addition, DSC results confirmed a decrease in glass transition and crystallization temperatures with increasing TiO{sub 2} content. This is the first report of a sol-gel synthesis strategy combined with enameling to prepare glass at low processing temperatures and the first use of such a system for both hydrophilic and chemical resistance purposes.

Ultrapure glass optical waveguide: Development in microgravity by the sol gel process

Science.gov (United States)

Mukherjee, S. P.; Debsikdar, J. C.; Beam, T.

1983-01-01

The sol-gel process for the preparation of homogeneous gels in three binary oxide systems was investigated. The glass forming ability of certain compositions in the selected oxide systems (SiO-GeO2, GeO2-PbO, and SiO2-TiO2) were studied based on their potential importance in the design of optical waveguide at longer wavelengths.

Influence of phosphorous precursors on spectroscopic properties of Er3+-activated SiO2-HfO2-P2O5 planar waveguides

International Nuclear Information System (INIS)

Vasilchenko, I; Carpentiero, A; Chiappini, A; Chiasera, A; Ferrari, M; Vaccari, A; Lukowiak, A; Righini, G C; Vereshagin, V

2014-01-01

(70-x)SiO 2 -30HfO 2 -xP 2 O 5 (x= 5, 10 mol %) glass planar waveguides activated by 0.5 mol% Er 3 + ions were prepared by sol-gel route. Several phosphorous precursors have been investigated for the synthesis of a dielectric stable sol useful for the realization of planar waveguides. The waveguides were investigated by different diagnostic techniques. The optical properties such as refractive index, thickness, number of propagating modes and attenuation coefficient were measured at 632.8 and 543.5 nm by prism coupling technique. Transmission measurements were carried out in order to assess the transparency of the deposited films. Photoluminescence measurements and lifetime decay curves of the Er 3 + transition (4 I 13/2 → 4 I 15/2 ) were performed in order to investigate the role of P 2 O 5

Visible Light Excited Catalysis and Reusability Performances of TiO2@Pr:Y2SiO5 Upconversion Materials

Directory of Open Access Journals (Sweden)

Yan Jiao

2017-01-01

Full Text Available To get high efficiency photodegradation on pollutants under visible light, Pr(III doped Y2SiO5 upconversion materials and anatase TiO2 nanofilm coated Pr:Y2SiO5 composite have been prepared by using a sol-gel method. XRD and SEM test results indicated that TiO2 nanofilm was well coated on Pr:Y2SiO5 to form TiO2@Pr:Y2SiO5 composite particles with the sizes of 0.5–1.0 μm. To avoid secondary pollution resulting from incomplete recovery of catalyst particles, TiO2@Pr:Y2SiO5 was loaded on the glass fiber filters by using a dip-coating method. It is found that the catalyst particles were embedded into the carrier firmly, even after having been reused for 6 times. The luminescence intensities of TiO2@Pr:Y2SiO5 were getting down sharply with the coating contents of TiO2 increased, which was attributed to the adsorption of the luminescence by the TiO2 film in situ. As a result, TiO2@Pr:Y2SiO5 with 4% TiO2, which presented lowest luminescence intensity, showed the highest efficiency on the photodegradation of nitrobenzene wastewater. The catalysts loaded on glass fiber filters showed excellent reusability on the photodegradation of nitrobenzene and presented a photodegradation rate of 95% at the first time and up to 75.9% even after 6 times of reusing by the treatment time of 12 h.

The structural studies of aluminosilicate gels and thin films synthesized by the sol-gel method using different Al2O3 and SiO2 precursors

Directory of Open Access Journals (Sweden)

Adamczyk Anna

2015-12-01

Full Text Available Aluminosilicate materials were obtained by sol-gel method, using different Al2O3 and SiO2 precursors in order to prepare sols based on water and organic solvents. As SiO2 precursors, Aerosil 200TM and tetraethoxysilane TEOS: Si(OC2H54 were applied, while DisperalTM and aluminium secondary butoxide ATSB: Al(OC4H93 were used for Al2O3 ones. Bulk samples were obtained by heating gels at 500 °C, 850 °C and at 1150 °C in air, while thin films were synthesized on carbon, steel and alundum (representing porous ceramics substrates by the dip coating method. Thin films were annealed in air (steel and alundum and in argon (carbon at different temperatures, depending on the substrate type. The samples were synthesized as gels and coatings of the composition corresponding the that of 3Al2O3·2SiO2 mullite because of the specific valuable properties of this material. The structure of the annealed bulk samples and coatings was studied by FT-IR spectroscopy and XRD method (in standard and GID configurations. Additionally, the electron microscopy (SEM together with EDS microanalysis were applied to describe the morphology and the chemical composition of thin films. The analysis of FT-IR spectra and X-ray diffraction patterns of bulk samples revealed the presence of γ-Al2O3 and δ-Al2O3 phases, together with the small amount of SiO2 in the particulate samples. This observation was confirmed by the bands due to vibrations of Al–O bonds occurring in γ-Al2O3 and δ-Al2O3 structures, in the range of 400 to 900 cm−1. The same phases (γ-Al2O3 and δ-Al2O were observed in the deposited coatings, but the presence of particulate ones strongly depended on the type of Al2O3 and SiO2 precursor and on the heat treatment temperature. All thin films contained considerable amounts of amorphous phase.

B2O3/SiO2 substitution effect on structure and properties of Na2O-CaO-SrO-P2O5-SiO2 bioactive glasses from molecular dynamics simulations.

Science.gov (United States)

Ren, Mengguo; Lu, Xiaonan; Deng, Lu; Kuo, Po-Hsuen; Du, Jincheng

2018-05-23

The effect of B2O3/SiO2 substitution in SrO-containing 55S4.3 bioactive glasses on glass structure and properties, such as ionic diffusion and glass transition temperature, was investigated by combining experiments and molecular dynamics simulations with newly developed potentials. Both short-range (such as bond length and bond angle) and medium-range (such as polyhedral connection and ring size distribution) structures were determined as a function of glass composition. The simulation results were used to explain the experimental results for glass properties such as glass transition temperature and bioactivity. The fraction of bridging oxygen increased linearly with increasing B2O3 content, resulting in an increase in overall glass network connectivity. Ion diffusion behavior was found to be sensitive to changes in glass composition and the trend of the change with the level of substitution is also temperature dependent. The differential scanning calorimetry (DSC) results show a decrease in glass transition temperature (Tg) with increasing B2O3 content. This is explained by the increase in ion diffusion coefficient and decrease in ion diffusion energy barrier in glass melts, as suggested by high-temperature range (above Tg) ion diffusion calculations as B2O3/SiO2 substitution increases. In the low-temperature range (below Tg), the Ea for modifier ions increased with B2O3/SiO2 substitution, which can be explained by the increase in glass network connectivity. Vibrational density of states (VDOS) were calculated and show spectral feature changes as a result of the substitution. The change in bioactivity with B2O3/SiO2 substitution is discussed with the change in pH value and release of boric acid into the solution.

SiO2 sol-gel films after ammonia and heat two-step treatments

International Nuclear Information System (INIS)

Zhang Chunlai; Wang Biyi; Tian Dongbin; Yin Wei; Jiang Xiaodong; Yuan Xiaodong; Yan Lianghong; Zhang Hongliang; Zhao Songnan; Lv Haibing

2008-01-01

SiO 2 thin films were deposited using tetraethoxylsilane as precursor, ammonia as catalyst on K9 glass by sol-gel method. These films were post-treated by ammonia and heat. The properties of the coatings were characterized by ellipsometer, UV-vis spectrophotometry, FTIR-spectroscopy, scanning probe microscope and contact angle measurement apparatus. The resuits indicate that the thickness of the films with ammonia and heat treatment tend to decrease. Both the refractive index and water contact angle increase after ammonia treatment. However, they both decrease after heat treatment. The former increases by 0.236 for the first step, then decreases by 0.202 for the second. The latter increases to 58.92 degree, then decreases to 38.07 degree. The transmittance of the coatings turn to be better and continuously shift to short wave by UV-vis spectrophotometry. The surface becomes smoother by AFM after the two-step treatment. (authors)

Effect of calcium source on structure and properties of sol-gel derived bioactive glasses.

Science.gov (United States)

Yu, Bobo; Turdean-Ionescu, Claudia A; Martin, Richard A; Newport, Robert J; Hanna, John V; Smith, Mark E; Jones, Julian R

2012-12-18

The aim was to determine the most effective calcium precursor for synthesis of sol-gel hybrids and for improving homogeneity of sol-gel bioactive glasses. Sol-gel derived bioactive calcium silicate glasses are one of the most promising materials for bone regeneration. Inorganic/organic hybrid materials, which are synthesized by incorporating a polymer into the sol-gel process, have also recently been produced to improve toughness. Calcium nitrate is conventionally used as the calcium source, but it has several disadvantages. Calcium nitrate causes inhomogeneity by forming calcium-rich regions, and it requires high temperature treatment (>400 °C) for calcium to be incorporated into the silicate network. Nitrates are also toxic and need to be burnt off. Calcium nitrate therefore cannot be used in the synthesis of hybrids as the highest temperature used in the process is typically 40-60 °C. Therefore, a different precursor is needed that can incorporate calcium into the silica network and enhance the homogeneity of the glasses at low (room) temperature. In this work, calcium methoxyethoxide (CME) was used to synthesize sol-gel bioactive glasses with a range of final processing temperatures from 60 to 800 °C. Comparison is made between the use of CME and calcium chloride and calcium nitrate. Using advanced probe techniques, the temperature at which Ca is incorporated into the network was identified for 70S30C (70 mol % SiO(2), 30 mol % CaO) for each of the calcium precursors. When CaCl(2) was used, the Ca did not seem to enter the network at any of the temperatures used. In contrast, Ca from CME entered the silica network at room temperature, as confirmed by X-ray diffraction, (29)Si magic angle spinning nuclear magnetic resonance spectroscopy, and dissolution studies. CME should be used in preference to calcium salts for hybrid synthesis and may improve homogeneity of sol-gel glasses.

Homogeneity of peraluminous SiO2-B2O3-Al2O3-Na2O-CaO-Nd2O3 glasses: Effect of neodymium content

International Nuclear Information System (INIS)

Gasnier, E.; Bardez-Giboire, I.; Massoni, N.; Montouillout, V.; Pellerin, N.; Allix, M.; Ory, S.; Cabie, M.; Poissonnet, S.; Massiot, D.

2014-01-01

Considering the interest of developing new glass matrices able to immobilize higher concentration of high level nuclear wastes than currently used nuclear borosilicate compositions, glasses containing high rare earth contents are of particular interest. This study focuses on a peraluminous alumino borosilicate system SiO 2 -B 2 O 3 -Al 2 O 3 -Na 2 O-CaO-Nd 2 O 3 defined by a per-alkaline/peraluminous ratio RP = ([Na 2 O] + [CaO])/ ([Na 2 O] + [CaO] + [Al 2 O 3 ]) ≤ 0.5. Samples with various contents of Nd 2 O 3 from 0 to 10 mol% were studied using DSC, XRD, SEM, TEM, STEM and EMPA methods. The glasses present a high thermal stability even after a slow cooling treatment from the melt. Only a slight mullite crystallization is detected for low Nd 2 O 3 content (≤2.3 mol%) and crystallization of a neodymium borosilicate crystalline phase combined to a phase separation occurred at high Nd 2 O 3 content (≥8 mol%). The solubility of neodymium in the presence of aluminum is demonstrated, with higher neodymium incorporation amounts than in per-alkaline glasses. (authors)

Optical Properties of Malachite Green Dye Doped SiO2 Glasses: Effect of Transition Metal (Fe-I Used as a Codopant

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Dulen Bora

2014-01-01

Full Text Available Enhanced luminescence properties of Malachite Green (MG (oxalate in Fe-MG codoped SiO2 glasses compared to its values in MG doped SiO2 glasses are reported here. The enhancement is chiefly attributed to a resonance nonradiative energy transfer between Fe and MG. The quantum yield of Malachite Green (MG, in presence of Iron, trapped in sol-gel derived SiO2 glass increases by an order of ~103 compared to that in low viscous solvent while a lifetime of 3.29 ns is reported.

Porous Silica Sol-Gel Glasses Containing Reactive V2O5 Groups

Science.gov (United States)

Stiegman, Albert E.

1995-01-01

Porous silica sol-gel glasses into which reactive vanadium oxide functional groups incorporated exhibit number of unique characteristics. Because they bind molecules of some species both reversibly and selectively, useful as chemical sensors or indicators or as scrubbers to remove toxic or hazardous contaminants. Materials also oxidize methane gas photochemically: suggests they're useful as catalysts for conversion of methane to alcohol and for oxidation of hydrocarbons in general. By incorporating various amounts of other metals into silica sol-gel glasses, possible to synthesize new materials with broad range of new characteristics.

Synthesis and photocatalytic properties of porous TiO2 films prepared by ODA/sol-gel method

International Nuclear Information System (INIS)

Zhang Wenjie; Bai Jiawei

2012-01-01

Porous TiO 2 films were deposited on SiO 2 pre-coated glass-slides by sol-gel method using octadecylamine (ODA) as template. The amount of ODA in the sol played an important role on the physicochemical properties and photocatalytic performance of the TiO 2 films. The films prepared at different conditions were all composed of anatase titanium dioxide crystals, and TiO 2 crystalline size got larger with increasing ODA amount. The maximum specific surface area of 41.5 m 2 /g was obtained for TiO 2 powders prepared from titanium sol containing 2.0 g ODA. Methyl orange degradation rate was enhanced along with increasing ODA amount and reached the maximal value at 2.0 g addition of ODA. After 40 min of UV-light irradiation, methyl orange degradation rate reached 30.5% on the porous film, which was about 10% higher than that on the smooth film. Porous TiO 2 film showed almost constant activity with slight decrease from 30.5% to 28.5% after 4 times of recycles.

Thermal Annealing Effect on Optical Properties of Binary TiO2-SiO2 Sol-Gel Coatings

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Xiaodong Wang

2012-12-01

Full Text Available TiO2-SiO2 binary coatings were deposited by a sol-gel dip-coating method using tetrabutyl titanate and tetraethyl orthosilicate as precursors. The structure and chemical composition of the coatings annealed at different temperatures were analyzed by Raman spectroscopy and Fourier Transform Infrared (FTIR spectroscopy. The refractive indices of the coatings were calculated from the measured transmittance and reflectance spectra. An increase in refractive index with the high temperature thermal annealing process was observed. The Raman and FTIR results indicate that the refractive index variation is due to changes in the removal of the organic component, phase separation and the crystal structure of the binary coatings.

Synthesis and Characterization of SiO2@Y2MoO6:Eu3+ Core-Shell Structured Spherical Phosphors by Sol-Gel Process.

Science.gov (United States)

Li, G Z; Liu, F H; Chu, Z S; Wu, D M; Yang, L B; Li, J L; Wang, M N; Wang, Z L

2016-04-01

SiO2@Y2MoO6:Eu3+ core-shell phosphors were prepared by the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as kinetic decays were used to characterize the resulting SiO2@Y2MoO6:Eu3+ core-shell phosphors. The XRD results demonstrated that the Y2MoO6:Eu3+ layers on the SiO2 spheres crystallized after being annealed at 700 °C and the crystallinity increased with raising the annealing temperature. The obtained core-shell phosphors have spherical shape with narrow size distribution (average size ca. 640 nm), non-agglomeration, and smooth surface. The thickness of the Y2MoO6:Eu3+ shells on the SiO2 cores could be easily tailored by varying the number of deposition cycles (70 nm for four deposition cycles). The Eul+ shows a strong PL emission (dominated by 5D0-7F2 red emission at 614 nm) under the excitation of 347 nm UV light. The PL intensity of Eu3+ increases with increasing the annealing temperature and the number of coating cycles.

Sol-gel synthesis and characterization of single-phase Ni ferrite nanoparticles dispersed in SiO2 matrix

International Nuclear Information System (INIS)

Nadeem, K.; Traussnig, T.; Letofsky-Papst, I.; Krenn, H.; Brossmann, U.; Wuerschum, R.

2010-01-01

Nanoparticles of NiFe 2 O 4 dispersed in SiO 2 (25 wt%) matrix were synthesized by sol-gel method using tetraethyl orthosilicate (TEOS), as a precursor for SiO 2 . The sol-gel method for nanocomposites normally provides multi-phase nanoparticles. We investigated by a synopsis of different analysis methods, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and SQUID-magnetometry, how the various chemical phases are transformed to a single-phase spinel structure during the various stages of annealing from 300 to 900 o C. We have developed a full phase diagram of chemical phases as a function of annealing temperature. The average particle size lies in the range 16-27 nm. The chemical phases formed below 900 o C are NiFe, NiO, γ-Fe 2 O 3 , α-Fe 2 O 3 , and NiFe 2 O 4 , respectively. The role of the TEOS prepared SiO 2 matrix is to restrict the particle size in a small range in order to rule out particle size effects. In the mid-infrared, a shift of the vibrational Fe-O bond is observed from 568 to 586 cm -1 for annealing between 500 and 700 o C which indicates an increasing NiFe 2 O 4 phase formation. A systematic study of coercivity field (ranging from 32 to 200 Oe) and saturation magnetic moment (ranging from 12.2 to 32.1 emu/g) for differently annealed samples supports our findings about the evolution of single-phase NiFe 2 O 4 at 900 o C. The opposite trend of saturation magnetic moment and coercivity with respect to annealing temperature clearly separates the different phases of metallic, antiferromagnetic, and finally single-phase spinel NiFe 2 O 4 .

Synthesis of ceramic powders of La9,56 (SiO4)6O2,34 and La9,8Si5,7MgO,3O26,4 by modified sol-gel process

International Nuclear Information System (INIS)

Lira, Sabrina Lopes; Paiva, Mayara Rafaela Soares; Misso, Agatha Matos; Elias, Daniel Ricco; Yamagata, Chieko

2012-01-01

Lanthanum silicate oxyapatite materials are promising for application as electrolyte in solid oxide fuel cells because of high ionic conductivity at temperatures between 600 deg C and 800 deg C. In this work, oxyapatites with the composition La 9,56 (SiO 4 ) 6 O 2,34 , and La 9,8 Si 5,7 Mg 0,3 O 26,4 were synthesized by using the sol-gel method, followed by precipitation. Initially, the gel of silica was synthesized from sodium silicate solution, by acid catalysis using lanthanum and magnesium chloride solution. Then, the La and Mg hydroxides were precipitated with NaOH in the gel. The powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and measurements of specific surface area. The crystalline oxyapatite phase of La 9,56 (SiO 4 ) 6 O 2,34 , and was La 9,8 Si 5,7 Mg 0,3 O 26,4 obtained by calcination at 900 deg C for 2 and 1h respectively (author)

Effects of cobalt doping on structural, morphological, and optical properties of Zn2SiO4 nanophosphors prepared by sol-gel method

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Norhafizah Mohd Rasdi

Full Text Available In this paper, undoped and cobalt (II (3, and 5 mol % doped zinc silicate nanophosphors prepared by a sol-gel method which were heated at 1000 °C were studied in detail. From the XRD result, undoped and Co2+ doped zinc silicate sample yields α- and β-Zn2SiO4. This also shows that α-Zn2SiO4 acts as the primary phase in the crystal structure of the sample. For FESEM, the grain size decreases as the dopant increases where undoped sample indicates average grain size of 181 nm while 3 and 5 mol % exhibits containing ones 136.89 nm and 176.22 nm respectively. With FTIR transmission a major peak at range of 1100 cm−1, 880, 550, and 350 assigning as Si-O-Si asymmetric stretching, SiO4 asymmetric stretching, ZnO4 symmetric stretching, and Si-O asymmetric deformation vibration were observed respectively. The absorption band of doped Zn2SiO4 exhibited a higher absorbance intensity in the UV region compared to undoped Zn2SiO4. Besides, all the samples depict that the sample was having a red shift in which the band shifted to the longer wavelength. The energy band gap value of undoped sample shows 3.07 eV and when Co2+ dopant (3 and 5 mol % was introduced, the energy band gap started to decrease (2.46 and 2.42 eV respectively. PL emission presents two peaks at blue emissions (420 and 480 nm and a green emission (525 nm. The result present that Co2+:Zn2SiO4 is potentially good to use as blue and green phosphors for luminescent optical material. Keywords: Cobalt (II doped zinc silicate, Transition metal, Sol-gel method, Nanophosphors, Photoluminescence

Sol-Gel Production; Proceedings of the First International Conference on Application and Commercialization of Sol-Gel Processing Held in Saarbruecken, Germany on 24-25 May 1993

National Research Council Canada - National Science Library

Schmidt, Helmut

1998-01-01

...; Sol-Gel Coatings on Large Glass Substrates for Multilayer Interference Systems; A SiO2-ZrO2 Gel Film doped with Organic Pigments Made by the Sol-Gel Method for Contrast Enhancement of Color Picture Tubes...

PENGUJIAN AKTIVITAS KOMPOSIT Fe2O3-SiO2 SEBAGAI FOTOKATALIS PADA FOTODEGRADASI 4-KLOROFENOL (The Activity Test of Fe2O3-SiO2 Composite As Photocatalyst on 4-Chlorophenol Photodegradation

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Eko Sri Kunarti

2009-03-01

Full Text Available ABSTRAK  Pada penelitian ini telah dilakukan pengujian aktivitas komposit Fe2O3-SiO2 sebagai fotokatalis pada fotodegradasi 4-klorofenol. Penelitian diawali dengan preparasi dan karakterisasi fotokatalis Fe2O3-SiO2. Preparasi dilakukan dengan metode sol-gel pada temperatur kamar menggunakan tetraetil ortosilikat (TEOS dan besi (III nitrat sebagai prekursor diikuti dengan perlakuan termal pada temperature 500 oC. Karakterisasi dilakukan dengan metode spektrometri inframerah, difraksi sinar-X dan spektrometri fluoresensi sinar-X. Uji aktivitas komposit untuk fotodegradasi 4-klorofenol dilakukan dalam reaktor tertutup yang dilengkapi dengan lampu UV. Pada uji ini telah dipelajari pengaruh waktu penyinaran dan pH larutan terhadap efektivitas fotodegradasi 4-klorofenol. Hasil penelitian menunjukkan bahwa komposit Fe2O3-SiO2 dapat dipreparasi dengan metode sol-gel pada temperatur kamar diikuti perlakuan termal. Komposit Fe2O3-SiO2 dapat meningkatkan efektivitas fotodegradasi 4-klorofenol dari 11,86 % menjadi 55,38 %. Efektivitas fotodegradasi 4- klorofenol dipengaruhi waktu penyinaran dan pH larutan yang semakin lama waktu penyinaran efektifitas fotodegradasi semakin tinggi, namun waktu penyinaran yang lebih lama dari 4 jam dapat menurunkan efektivitasnya. pH larutan memberikan pengaruh yang berbeda-beda pada efektivitas fotodegradasi 4-klorofenol.   ABSTRACT The activity test of Fe2O3-SiO2 composite as photocatalyst on 4-chlorophenol photodegradation has been studied. The research was initiated by preparation of Fe2O3-SiO2 photocatalyst and followed by characterization. The preparation was conducted by sol-gel method at room temperature using tetraethylorthosilicate (TEOS and iron (III nitrate as precursors followed by thermal treatment at a temperature of 500oC. The characterizations were performed by X-ray Diffraction (XRD, Infrared and X-ray Fluorescence Spectrophotometry. The photocatalytic activity test of composites for 4 chlorophenol

Imprinted sol-gel electrochemical sensor for the determination of benzylpenicillin based on Fe3O4/SiO2 multi-walled carbon nanotubes-chitosans nanocomposite film modified carbon electrode

International Nuclear Information System (INIS)

Hu Yufang; Li Jiaxing; Zhang Zhaohui; Zhang Huabin; Luo Lijuan; Yao Shouzhuo

2011-01-01

Graphical abstract: A novel imprinted sol-gel electrochemical sensor based on Fe 3 O 4 /SiO 2 -MWNTs-CTS nanocomposite film and a thin MIP film has been developed on a carbon electrode. Highlights: → A novel imprinted sol-gel electrochemical sensor based on Fe 3 O 4 /SiO 2 -MWNTs-CTS nanocomposites has been developed. → Fe 3 O 4 /SiO 2 -MWNTs-CTS nanocomposites act as 'electronic wires' to enhance the electron transfer. → The inherent specificity of the MIPs brings about highly selectivity. The imprinted sensor detects benzylpenicillin in real samples successfully. - Abstract: Herein, a novel imprinted sol-gel electrochemical sensor based on multi-walled carbon nanotubes (MWNTs) doped with chitosan film on a carbon electrode has been developed. Prior to doped, the MWNTs have been decorated with Fe 3 O 4 nanoparticles which have been coated uniformly with SiO 2 layer. The characterization of imprinted sensor has been carried out by X-ray diffraction and scanning electron microscopy. The performance of the proposed imprinted sensor has been investigated using cyclic voltammetry and differential pulse voltammetry. The imprinted sensor offers a fast response and sensitive benzylpenicillin quantification. The fabricated benzylpenicillin imprinted sensor exhibits a linear response from 5.0 x 10 -8 to 1.0 x 10 -3 mol L -1 with a detection limit of 1.5 x 10 -9 mol L -1 . For samples analysis, perfect recoveries of the imprinted sensor for benzylpenicillin indicated that the imprinted sensor was able to detect benzylpenicillin in real samples successfully.

Microstructure, Thermal, Mechanical, and Dielectric Properties of BaO-CaO-Al2O3-B2O3-SiO2 Glass-Ceramics

Science.gov (United States)

Li, Bo; Bian, Haibo; Fang, Yi

2017-12-01

BaO-CaO-Al2O3-B2O3-SiO2 (BCABS) glass-ceramics were prepared via the method of controlled crystallization. The effect of CaO modification on the microstructure, phase evolution, as well as thermal, mechanical, and dielectric properties was investigated. XRD identified that quartz is the major crystal phase; cristobalite and bazirite are the minor crystal phases. Moreover, the increase of CaO could inhibit the phase transformation from quartz to cristobalite, but excessive CaO would increase the porosity of the ceramics. Additionally, with increasing the amount of CaO, the thermal expansion curve tends to be linear, and subsequently the CTE value decreases gradually, which is attributed to the decrease of cristobalite with high CTE and the formation of CaSiO3 with low CTE. The results indicated that a moderate amount of CaO helps attaining excellent mechanical, thermal, and dielectric properties, that is, the specimen with 9 wt% CaO sintered at 950 °C has a high CTE value (11.5 × 10-6/°C), a high flexural strength (165.7 MPa), and good dielectric properties (ɛr = 6.2, tanδ = 1.8 × 10-4, ρ = 4.6 × 1011 Ω•cm).

The effect of rare earth dopants on the structure, surface texture and photocatalytic properties of TiO2-SiO2 prepared by sol-gel method

International Nuclear Information System (INIS)

Mohamed, R.M.; Mkhalid, I.A.

2010-01-01

The sol-gel method was successfully used to prepare a series of TiO 2 -SiO 2 and rare earth (RE) (La 3+ , Nd 3+ , Sm 3+ , Gd 3+ )-doped TiO 2 -SiO 2 nanoparticles at a doping level of 3 atomic percent. The structural features of parent TiO 2 -SiO 2 and RE-TiO 2 -SiO 2 fired at 550 o C have been investigated by XRD, UV-diffuse reflection, SEM and nitrogen adsorption measurements at -196 o C. XRD data verified the formation of typical characteristic anatase form in all the prepared RE-doped TiO 2 -SiO 2 samples. In comparison with the pure TiO 2 -SiO 2 samples (ca. 35 nm in diameter), the RE-TiO 2 -SiO 2 samples have relatively small particle size indicating that the doping with RE metal ions can improve the particle morphology, and retard the grain growth of TiO 2 -SiO 2 during heat treatment. The results indicated that Gd 3+ doped TiO 2 -SiO 2 has the lowest bandgap and particle size compared with pure TiO 2 -SiO 2 and other nanoparticles of RE-doped TiO 2 -SiO 2 . The highest surface area (S BET ) and pore volume (V p ) values were recorded for Gd-TiO 2 -SiO 2 as well. The effect of doping on the photoactivity was evaluated by the photocatalytic degradation of EDTA as a probe reaction. Among all the pure and RE-doped TiO 2 -SiO 2 , Gd 3+ -TiO 2 -SiO 2 performed the highest catalytic activity towards the tested reaction. That might be due to its special characteristics of particle size, surface texture and bandgap properties. Details of the synthesis procedure and results of the characterization studies of the produced RE-TiO 2 -SiO 2 are presented in this paper.

Are the phosphorus-rich Na2O–CaO–B2O3–SiO2–P2O5 glasses bioactive and what is an influence of doping with manganese oxide?

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Bragiel P.

2018-03-01

Full Text Available A series of glasses of the composition 20Na2-O-15CaO-5B2O3-5SiO2-(55 - x P2O5:xMnO2, was prepared and characterized by XRD, DSC, SEM, and Raman techniques. The samples were later immersed in simulated body fluid (SBF for checking the potential growth of hydroxyapatite layer (HA. Experiments confirmed that addition of manganese oxide leads to structural changes of the glasses. With increasing content of MnO2, the surface of the samples became more congenial for improving the growth of HA. The formation of HA layer on the surface of the samples was confirmed just after seven days of immersion. The growth rate of HA has gradually increased with the increase of MnO2 content.

Evaluation of micro-abrasion-corrosion on SiO2-TiO2-ZrO2 coatings synthesized by the sol-gel method

Science.gov (United States)

Bautista Ruiz, J.; Aperador, W.; Caballero Gómez, J.

2016-02-01

The medical science and the engineering, work to improve the materials used in the manufacture of joint implants, since they have a direct impact on the quality of people life. The surgical interventions are increasing worldwide with a high probability of a second or even a third intervention. Around these circumstances, it was evaluated the behaviour against microabrasion-corrosion phenomena on SiO2 TiO2 ZrO2 coatings, synthesized by the sol-gel method with concentration of the Si/Ti/Zr precursors: 10/70/20 and 10/20/70. The coatings were deposited on AISI 316 LVM stainless steel substrates. The morphological characterization of the wear was made by AFM techniques. It was observed that the coatings with higher levels of titanium have a good response to the phenomena of microabrasion-corrosion.

In-vitro study of copper doped SiO2-CaO-P2O5 system for bioactivity and antimicrobial properties

Science.gov (United States)

Kaur, Kulwinder; Singh, K. J.; Anand, Vikas; Kaur, Harpreet; Arora, Daljit Singh

2015-08-01

Samples of the xCuO-(45-x)CaO-10P2O5-45SiO2 system (x varies from 0 to 4 mole%) have been synthesized for application as biomaterials to slow or inhibit the growth of living organisms (fungi and other pathogenic microorganisms) by the combination of sol-gel and co-precipitation processes. Prepared samples have been characterized by X-Ray Diffraction, Fourier Transform Infra-Red and Field Emission Scanning Electron Microscopy techniques before and after immersion in simulated body fluid. Antimicrobial activity of samples has been investigated against Staphylococcus aureus. Releasing of Cu2+and other ions in the simulated body fluid has been determined by Atomic Absorption Spectroscopy to ensure the use of prepared material as biomaterial with good antibacterial properties.

Synthesis and Characterization of V2O5/SiO2 Nanoparticles as Efficient Catalyst for Aromatization 1,4 Dihydropyridines

International Nuclear Information System (INIS)

Farzaneh, F.; Zamanifar, E.; Jafari Foruzin, L.; Ghandi, M.

2012-01-01

V 2 O 5 /SiO 2 nanoparticles was prepared via an one-pot sol gel method from vanadyl- acetylacetonate and tetraethyl orthosilicate in refluxing MeOH, followed by calcination at 700 °C for 2 hours. The resultant nanoparticles was characterized by means of scanning electron microscopy, transmission electron microscopy, X-ray diffraction, TGA and FTIR techniques. Rapid and efficient aromatization of 1,4-dihydropyridines catalyzed by V 2 O 5 /SiO 2 nanoparticles is described in this presentation.

LOW-TEMPERATURE SINTERED (ZnMg2SiO4 MICROWAVE CERAMICS WITH TiO2 ADDITION AND CALCIUM BOROSILICATE GLASS

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BO LI

2011-03-01

Full Text Available The low-temperature sintered (ZnMg2SiO–TiO2 microwave ceramic using CaO–B2O3–SiO2 (CBS as a sintering aid has been developed. Microwave properties of (Zn1-xMgx2SiO4 base materials via sol-gel method were highly dependent on the Mg-substituted content. Further, effects of CBS and TiO2 additives on the crystal phases, microstructures and microwave characteristics of (ZnMg2SiO4 (ZMS ceramics were investigated. The results indicated that CBS glass could lower the firing temperature of ZMS dielectrics effectively from 1170 to 950°C due to the liquid-phase effect, and significantly improve the sintering behavior and microwave properties of ZMS ceramics. Moreover, ZMS–TiO2 ceramics showed the biphasic structure and the abnormal grain growth was suppressed by the pinning effect of second phase TiO2. Proper amount of TiO2 could tune the large negative temperature coefficient of resonant frequency (tf of ZMS system to a near zero value. (Zn0.8Mg0.22SiO4 codoped with 10 wt.% TiO2 and 3 wt.% CBS sintered at 950°C exhibits the dense microstructure and excellent microwave properties: εr = 9.5, Q·f = 16 600 GHz and tf = −9.6 ppm/°C.

Scratch resistance of SiO{sub 2} and SiO{sub 2} - ZrO{sub 2} sol-gel coatings on glass-ceramic obtained by sintering; Resistencia al desgaste de recubrimientos sol-gel de SiO{sub 2} y SiO{sub 2} - ZrO{sub 2} sobre materiales vitroceramicos obtenidos por sinterizacion

Energy Technology Data Exchange (ETDEWEB)

Soares, V. O.; Soares, P.; Peitl, O.; Zanotto, E. D.; Duran, A.; Castro, Y.

2013-10-01

The sol-gel process is widely used to obtain coatings on glass-ceramic substrates in order to improve the scratch and abrasion resistance, also providing a bright and homogeneous appearance of a glaze avoiding expensive final polishing treatments. This paper describes the preparation of silica and silica / zirconia coatings by sol-gel method on Li{sub 2}O-Al{sub 2}O3-SiO{sub 2} (LAS) glassceramic substrates produced by sintering. The coatings were deposited by dip-coating on LAS substrates and characterized by optical microscopy and spectral ellipsometry. On the other hand, hardness and elastic modulus, coefficient of friction and abrasion and scratch resistance of the coatings were determined and compared with the substrate properties. Coatings deposited on LAS glass-ceramic confere the substrate a bright and homogeneous aspect, similar to a glaze, improving the appearance and avoiding the final polishing. However these coatings do not increase the scratch resistance of the substrate only equaling the properties of the glass-ceramic. (Author)

In vitro evaluation of bioactivity of SiO2-CaO-P2O5-Na2O-CaF2-ZnO glass-ceramics

Science.gov (United States)

Riaz, Madeeha; Zia, Rehana; Saleemi, Farhat; Bashir, Farooq; Hossain, Tousif; Kayani, Zohra

2014-09-01

Zinc is an essential trace element that stimulates bone formation but it is also known as an inhibitor of apatite crystal growth. In this work addition of ZnO to SiO2-CaO-P2O5-Na2O-CaF2 glass-ceramic system was made by conventional melt-quenching technique. DSC curves showed that the addition of ZnO moved the endothermic and exothermic peaks to lower temperatures. X-ray diffraction analysis did not reveal any additional phase caused by ZnO addition and showed the presence of wollastonite and hydroxyapatite crystalline phases only in all the glass-ceramic samples. As bio-implant apatite forming ability is an essential condition, the surface reactivity of the prepared glass-ceramic specimens was studied in vitro in Kokubo's simulated body fluid (SBF) [1] with ion concentration nearly equal to human blood plasma for 30 days at 37 °C under static condition. Atomic absorption spectroscopy (AAS) was used to study the changes in element concentrations in soaking solutions and XRD, FT-IR and SEM were used to elucidate surface properties of prepared glass-ceramics, which confirmed the formation of HCAp on the surface of all glass-ceramics. It was found that the addition of ZnO had a positive effect on bioactivity of glass-ceramics and made it a potential candidate for restoration of damaged bones.

Sol–gel hybrid membranes loaded with meso/macroporous SiO{sub 2}, TiO{sub 2}–P{sub 2}O{sub 5} and SiO{sub 2}–TiO{sub 2}–P{sub 2}O{sub 5} materials with high proton conductivity

Energy Technology Data Exchange (ETDEWEB)

Castro, Yolanda, E-mail: castro@icv.csic.es [Instituto de Cerámica y Vidrio, Consejo Superior de Investigaciones Científicas (ICV-CSIC), Campus de Cantoblanco, 28049 Madrid (Spain); Mosa, Jadra, E-mail: jmosa@icv.csic.es [Instituto de Cerámica y Vidrio, Consejo Superior de Investigaciones Científicas (ICV-CSIC), Campus de Cantoblanco, 28049 Madrid (Spain); Aparicio, Mario [Instituto de Cerámica y Vidrio, Consejo Superior de Investigaciones Científicas (ICV-CSIC), Campus de Cantoblanco, 28049 Madrid (Spain); Pérez-Carrillo, Lourdes A.; Vílchez, Susana; Esquena, Jordi [Instituto de Química Avanzada de Cataluña, Consejo Superior de Investigaciones Científicas (IQAC-CSIC), CIBER de Bioingeniería, Biomateriales y Nanomedicina (CIBER-BBN), Jordi Girona 18-26, 08034 Barcelona (Spain); Durán, Alicia [Instituto de Cerámica y Vidrio, Consejo Superior de Investigaciones Científicas (ICV-CSIC), Campus de Cantoblanco, 28049 Madrid (Spain)

2015-01-15

In this work, highly conductive hybrid organic–inorganic membranes loaded with SiO{sub 2}, TiO{sub 2}–P{sub 2}O{sub 5} and SiO{sub 2}–TiO{sub 2}–P{sub 2}O{sub 5} meso/macroporous particles were prepared via a sol–gel process. Meso/macroporous particles were incorporated to hybrid membranes, for improving water retention and enhancing electrochemical performance. These particles with a polymodal pore size distribution were prepared by templating in highly concentrated emulsions, the particles showed a specific surface area between 50 m{sup 2}/g (TiO{sub 2}–P{sub 2}O{sub 5}) and 300 m{sup 2}/g (SiO{sub 2}–TiO{sub 2}–P{sub 2}O{sub 5}). The particles were dispersed in a hybrid silica sol and further sprayed onto glass paper. The films were polymerized and sintered; those loaded with meso/macroporous particles had a homogenous distribution. High temperature proton conductivity measurements confirmed a high water retention. Conductivity of these materials is higher than that of Nafion{sup ®} at higher temperatures (120 °C) (2·10{sup −2} S/cm). This study provides processing guideline to achieve hybrid electrolytes for efficient conduction of protons due to their high surface area and porous structure. - Highlights: • Hybrid electrolyte with meso/macroporous particles were synthesized by sol–gel. • Depositions of hybrid solutions by spraying onto glass substrates were performed. • Proton conductivity was evaluated as a function of composition and porous structure.

Preparation of Raspberry-like Superhydrophobic SiO2 Particles by Sol-gel Method and Its Potential Applications

Directory of Open Access Journals (Sweden)

Xu Gui-Long

2011-12-01

Full Text Available Raspberry‐like SiO2 particles with a nano‐micro‐binary structure were prepared by a simple sol‐gel method using tetraethoxysilane (TEOS and methyltriethoxysilane (MTES as precursors. The chemical components and morphology of the SiO2 particles were characterized by Fourier transform infrared spectroscopy (FT‐IR and a Transmission electron microscope (TEM. The surface topography and wetting behaviour of the raspberry‐like SiO2 surface were observed with a Scanning electron microscope (SEM and studied by the water/oil contact angle (CA, respectively. The thermal stability of the prepared SiO2 particles was characterized by TGA analysis. The results show that the highly dispersed SiO2 particles initially prepared by the sol‐gel method turn into raspberry‐like particles with during the aging process. The raspberry‐like SiO2 particles show superhydrophobicity and superoleophilicity across a wide range of pH values. The SiO2 particles were thermally stable up to 475°C, while above this temperature the hydrophobicity decreases and finally becomes superhydrophobic when the temperature reaches 600°C. The raspberry‐like SiO2 particles which were prepared have potential applications in the fields of superhydrophobic surfaces, water‐oil separation, anti‐corrosion and fluid transportation.

Sol-gel synthesis of magnesium oxide-silicon dioxide glass compositions

Science.gov (United States)

Bansal, Narottam P.

1988-01-01

MgO-SiO2 glasses containing up to 15 mol pct MgO, which could not have been prepared by the conventional glass melting method due to the presence of stable liquid-liquid immiscibility, were synthesized by the sol-gel technique. Clear and transparent gels were obtained from the hydrolysis and polycondensation of silicon tetraethoxide (TEOS) and magnesium nitrate hexahydrate when the water/TEOS mole ratio was four or more. The gelling time decreased with increase in magnesium content, water/TEOS ratio, and reaction temperature. Magnesium nitrate hexahydrate crystallized out of the gels containing 15 and 20 mol pct MgO on slow drying. This problem was partially alleviated by drying the gels quickly at higher temperatures. Monolithic gel samples were prepared using glycerol as the drying control additive. The gels were subjected to various thermal treatments and characterized by several methods. No organic groups could be detected in the glasses after heat treatments to approx. 800 C, but trace amounts of hydroxyl groups were still present. No crystalline phase was found from X-ray diffraction in the gel samples to approx. 890 C. At higher temperatures, alpha quartz precipitated out as the crystalline phase in gels containing up to 10 mol pct MgO. The overall activation energy for gel formation in 10MgO-90SiO2 (mol pct) system for water/TEOS mole ratio of 7.5 was calculated to be 58.7 kJ/mol.

Efectos de fotodegradación propiciados por recubrimientos de TiO2 y TiO2-SiO2 obtenidos por Sol-Gel

Directory of Open Access Journals (Sweden)

Rodriguez Paez, J. E.

2008-10-01

Full Text Available Photodegradation effect is widely used for water purification this contributes to preservation and protection of environment. Titanium oxide, (TiO2, is a compound that shows up this phenomenon. TiO2 is a semiconductor which may degradate pollutants through of a oxidation process. It permit the treatment of the residual water. It this work we has conformed coatings of TiO2 y TiO2-SiO2, utilized Sol-Gel method and investigated the degradation of the blue Methylene. For this, we introduced these coatings in the blue methylene solution which was illuminated with radiation of λ=365nm to activate its photocatilist properties. The structures of the coatings were characterized using Atomic Force Microscopy (AFM and X-ray Photoelectron Spectroscopy (XPS.El efecto de fotodegradación es ampliamente utilizado para la purificación del agua, acción que contribuye a la conservación y protección del medio ambiente; el óxido de titanio (TiO2 es uno de los semiconductores que pueden degradar contaminantes mediante procesos de oxidación, lo que lo hace apto para el tratamiento de aguas residuales. En este trabajo se conformaron recubrimientos de TiO2 y TiO2-SiO2, por el método Sol-Gel, y se estudio la degradación que experimentaba una solución de azul de metileno al introducirle estos recubrimientos e iluminarlos con una radiación de λ=365nm para activar su propiedad fotocatalítica. Los recubrimientos fueron caracterizados microestructuralmente utilizando Microscopía de Fuerza Atómica (MFA y Espectroscopía de Fotoelectrones de rayos X (XPS. Los resultados obtenidos de los ensayos de fotodegradación indican que los recubrimientos con una cantidad pequeña de silicio presentan un mayor efecto de fotodegradación indicando que el silicio puede generar puntos de anclaje que facilitan las reacciones de fotocatálisis. Por otro lado, la formación de centros activos, constituidos principalmente por carbono, también contribuyeron al desarrollo de estas

Role of the Short Distance Order in Glass Reactivity

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María Vallet-Regi

2018-03-01

Full Text Available In 2005, our group described for the first time the structural characterization at the atomic scale of bioactive glasses and the influence of the glasses’ nanostructure in their reactivity in simulated body fluids. In that study, two bioactive sol-gel glasses with composition 80%SiO2–20%CaO and 80%SiO2–17%CaO–3%P2O5 (in mol-% were characterized by High-Resolution Transmission Electron Microscopy (HRTEM. Such characterization revealed unknown features of the glasses’ structure at the local scale that allowed the understanding of their different in vitro behaviors as a consequence of the presence or absence of P2O5. Since then, the nanostructure of numerous bioactive glasses, including melt-prepared, sol-gel derived, and mesoporous glasses, was investigated by HRTEM, Nuclear Magnetic Resonance (NMR spectroscopy, Molecular Dynamics (MD simulations, and other experimental techniques. These studies have shown that although glasses are amorphous solids, a certain type of short distance order, which greatly influences the in vitro and in vivo reactivity, is always present. This paper reviews the most significant advances in the understanding of bioactive glasses that took place in the last years as a result of the growing knowledge of the glasses’ nanostructure.

Role of the Short Distance Order in Glass Reactivity

Science.gov (United States)

2018-01-01

In 2005, our group described for the first time the structural characterization at the atomic scale of bioactive glasses and the influence of the glasses’ nanostructure in their reactivity in simulated body fluids. In that study, two bioactive sol-gel glasses with composition 80%SiO2–20%CaO and 80%SiO2–17%CaO–3%P2O5 (in mol-%) were characterized by High-Resolution Transmission Electron Microscopy (HRTEM). Such characterization revealed unknown features of the glasses’ structure at the local scale that allowed the understanding of their different in vitro behaviors as a consequence of the presence or absence of P2O5. Since then, the nanostructure of numerous bioactive glasses, including melt-prepared, sol-gel derived, and mesoporous glasses, was investigated by HRTEM, Nuclear Magnetic Resonance (NMR) spectroscopy, Molecular Dynamics (MD) simulations, and other experimental techniques. These studies have shown that although glasses are amorphous solids, a certain type of short distance order, which greatly influences the in vitro and in vivo reactivity, is always present. This paper reviews the most significant advances in the understanding of bioactive glasses that took place in the last years as a result of the growing knowledge of the glasses’ nanostructure. PMID:29534481

The application of Cu/SiO2 catalytic system in chemical mechanical planarization based on the stability of SiO2 sol

International Nuclear Information System (INIS)

Li Yan; Liu Yuling; Wang Aochen; Yang Zhixin; Sun Mingbin; Cheng Chuan; Zhang Yufeng; Zhang Nannan

2014-01-01

There is a lot of hydroxyl on the surface of nano SiO 2 sol used as an abrasive in the chemical mechanical planarization (CMP) process, and the chemical reaction activity of the hydroxyl is very strong due to the nano effect. In addition to providing a mechanical polishing effect, SiO 2 sol is also directly involved in the chemical reaction. The stability of SiO 2 sol was characterized through particle size distribution, zeta potential, viscosity, surface charge and other parameters in order to ensure that the chemical reaction rate in the CMP process, and the surface state of the copper film after CMP was not affected by the SiO 2 sol. Polarization curves and corrosion potential of different concentrations of SiO 2 sol showed that trace SiO 2 sol can effectively weaken the passivation film thickness. In other words, SiO 2 sol accelerated the decomposition rate of passive film. It was confirmed that the SiO 2 sol as reactant had been involved in the CMP process of copper film as reactant by the effect of trace SiO 2 sol on the removal rate of copper film in the CMP process under different conditions. In the CMP process, a small amount of SiO 2 sol can drastically alter the chemical reaction rate of the copper film, therefore, the possibility that Cu/SiO 2 as a catalytic system catalytically accelerated the chemical reaction in the CMP process was proposed. According to the van't Hoff isotherm formula and the characteristics of a catalyst which only changes the chemical reaction rate with out changing the total reaction standard Gibbs free energy, factors affecting the Cu/SiO 2 catalytic reaction were derived from the decomposition rate of Cu (OH) 2 and the pH value of the system, and then it was concluded that the CuSiO 3 as intermediates of Cu/SiO 2 catalytic reaction accelerated the chemical reaction rate in the CMP process. It was confirmed that the Cu/SiO 2 catalytic system generated the intermediate of the catalytic reaction (CuSiO 3 ) in the CMP process

Micro-ion beam analysis of physico-chemical reactions in vitro induced by nano-structured sol-gel derived bioactive glasses

International Nuclear Information System (INIS)

Lao, J.

2007-07-01

The study of bioactive glasses is a multi-field area of research aiming at a major goal: the development of new generation biomaterials that would be able to bond with host tissues through the formation of a strong interfacial bond, together with helping the body heal itself through the stimulation of specific cellular responses. Thus clinical applications of bioactive glasses mainly concern dental surgery and orthopedics, for filling osseous defects. For this purpose, we have elaborated bioactive glasses in the binary SiO 2 -CaO system, ternary SiO 2 -CaO-P 2 O 5 system, and for the first time, to our knowledge, strontium-doped SiO 2 -CaO-SrO and SiO 2 -CaO-P 2 O 5 -SrO glasses. The materials were elaborated using the sol-gel process, which allowed the synthesis of nano-porous materials with great purity and homogeneity. The bio-activity of the glasses was clearly demonstrated in vitro: in contact with biological fluids, the whole lot of mate-rials were able to induce the formation of a Ca-P-Mg layer a few microns thick at their surface. Our work is characterized by the use of PIXE-RBS nuclear microprobes to study the bioactive glass/biological fluids interface. Thanks to these methods we obtained chemical maps that made possible the analysis of major and trace elements concentrations at the interface. Moreover, quantitative information regarding the local reactivity of glasses were acquired. These data are important to evaluate the kinetics and amplitude of the physico-chemical reactions involved in the bio-activity process. Thus, we highlighted that the binary glass is the highest reactive regarding the dissolution of the glassy matrix as well as the first appearance of the Ca-P rich layer. However the Ca/P atomic ratio calculated at the glass/biological fluids interface decreases slowly, indicating that the Ca-P-Mg layer encounters difficulties to be changed into a more stable apatitic phase. For the P-containing glasses, the de-alkalinization of the matrix and

The ceramic SiO2 and SiO2-TiO2 coatings on biomedical Ti6Al4VELI titanium alloy

International Nuclear Information System (INIS)

Surowska, B.; Walczak, M.; Bienias, J.

2004-01-01

The paper presents the study of intermediate SiO 2 and SiO 2 -TiO 2 sol-gel coatings and dental porcelain coatings on Ti6Al4VELI titanium alloy. Surface microstructures and wear behaviour by pin-on-disc method of the ceramic coatings were investigated. The analysis revealed: (1) a compact, homogeneous SiO 2 and SiO 2 -TiO 2 coating and (2) that intermediate coatings may provide a durable joint between metal and porcelain, and (3) that dental porcelain on SiO 2 and TiO 2 coatings shows high wear resistance. (author)

Optical properties of BaO added bioactive Na2O-CaO-P2O5 glasses

Science.gov (United States)

Edathazhe, Akhila B.; Shashikala, H. D.

2018-04-01

This paper deals with the effect of BaO addition on the optical properties of bioactive Na2O-CaO-P2O5 glasses for biomedical optics applications. The phosphate glasses with composition (26-x)Na2O-xBaO-29CaO-45P2O5 (x = 0, 5, 10, 15 mol%) have been prepared by melt-quenching technique at 1100°C. The refractive index of glasses increased with BaO content. The optical band gap and Urbach energy of synthesized glasses were derived from the optical absorption spectra by using UV-Visible spectrometer. The addition of 5 mol% of BaO increased the band gap energy of glasses due to the formation of ionic cross-links in the glass structure. The defect and interstitial bonds formation in theglasses decreased with BaO additions as indicated by reductions in the Urbach energy values. No such variations in the band gap and Urbach energy values of glasses were observed with BaO content from 5 to 15 mol%. The molar and oxide ion polarizability values were calculated from the band gap and molar volume of glasses. The increase in the calculated optical basicity and metallization criteria of glasses supported the rise in band gap energy values with BaO additions. As the melting temperature of glasses decreased from 1200 to 1100°C, the refractive index increased as supported by the measured density values. The band gap energy is not changed with melting temperature. The Urbach energy decreased with decrease in melting temperature in case of BaO-free Na2O-CaO-P2O5 glasses, whereas it increased in case of BaO added glasses due to the role of BaO as modifying oxide.

Preliminary study in development of glass-ceramic based on SiO2-LiO2 system, starting of different SiO2 starting powders

International Nuclear Information System (INIS)

Daguano, J.K.M.F.; Santos, F.A.; Santos, C.; Marton, L.F.M.; Conte, R.A.; Rodrigues Junior, D.; Melo, F.C.L.

2009-01-01

In this work, lithium disilicate glass-ceramics were developed starting of the rice ash- SiO 2 and Li 2 CO 3 powders. The results were compared with glass ceramics based on the lithium disilicate obtained by commercial SiO 2 powders. Glass were melted at 1580 deg C, and annealed at 850 deg C. X-Ray diffraction and scanning electron microscopy were used for characterization of the materials, and hardness and fracture toughness were evaluated using Vickers indentation method. Glasses with amorphous structure were obtained in both materials. After annealing, 'rice-ash' samples presented Li 2 SiO 3 and residual SiO 2 as crystalline phases. On the other side, commercial SiO 2 - Samples presented only Li 2 Si 2 O 5 as crystalline phases and the better results of hardness and fracture toughness. (author)

Phonon spectra in SiO2 glasses

International Nuclear Information System (INIS)

Perez R, J.F.; Jimenez S, S.; Gonzalez H, J.; Vorobiev, Y.V.; Hernandez L, M.A.; Parga T, J.R.

1999-01-01

Phonon spectra in SiO 2 sol-gel made glasses annealed under different conditions are investigated using infrared absorption and Raman scattering. These data are compared with those obtained in commercial optical-quality quartz. All the materials exhibit the same phonon bands, the exact position and the intensity depend on the measuring technique and on the sample preparation method. The phonon spectra in this material are interpreted on the basis of a simple quasi-linear description of elastic waves in an O-Si-O chain. It is shown that the main features observed in the range 400-1400 cm -1 can be predicted using a quasi-linear chain model in which the band at 1070 cm -1 is assigned to the longitudinal optical waves in the O-Si-O chain with the smallest possible wavelength at the Brillouin zone boundary, the band located around 450 cm -1 is assigned to the transversal optical waves and the band at 800 cm -1 to the longitudinal acoustical waves with the same wavelength. The degree of structural disorder can be also deduced within the framework of the proposed model. (Author)

Effect of phase transformation and partial crystallization on the mechanical properties of glass and glass-ceramics based on 3CaO.P_2O_5-SiO_2-MgO system

International Nuclear Information System (INIS)

Daguano, J.K.M.F.; Simba, B.G.; Santos, C.

2011-01-01

In this work, glass and glass-ceramics of the 3CaO.P_2O_5-SiO_2-MgO system were developed aiming to produce different crystallization degrees. Glasses were melted at 1600 deg C and heat treated at 700 deg C. Part of the glasses was crystallized using heat treatments at 770 deg C and 1150 deg C for 4h. The partial crystallization and phase transformations were responsible for different mechanical properties (bending strength, young modulus, fracture toughness and hardness) in each temperature. The mechanical response of the material is discussed in relation to the microstructure, crystalline phases, and porosity of the materials. (author)

Composition and crystallization kinetics of R2O-Al2O3-SiO2 glass-ceramics

International Nuclear Information System (INIS)

Xiong, Dehua; Cheng, Jinshu; Li, Hong

2010-01-01

The crystallization behavior and microstructure of R 2 O-Al 2 O 3 -SiO 2 (R means K, Na and Li) glass were investigated by means of differential scanning calorimeter (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystallization kinetic parameters including the crystallization apparent activation energy (E a ), the Avrami parameter (n), glass transition temperature (T g ) and the activity energy of glass transition (E t ) were also measured with different methods. The results have shown that: the DSC traces of composition A parent glass have two different precipitation crystallization peaks corresponding to E a1 (A) = 151.4 kJ/mol (Li 2 SiO 3 ) and E a2 (A) = 623.1 kJ/mol (Li 2 Si 2 O 5 ), the average value of n = 1.70 (Li 2 Si 2 O 5 ) for the surface crystallization and E t (A) = 202.8 kJ/mol. And E a (B) = 50.7 kJ/mol (Li 2 SiO 3 ), the average value of n = 3.89 (Li 2 SiO 3 ) for the bulk crystallization and E t (B) = 220.4 kJ/mol for the composition B parent glass. Because of the content of R 2 O is bigger than composition A, composition B parent glass has a lower E a , T g and a larger n, E t .

Preparation of orthophosphate glasses in the MgO-CaO-SiO2-Nb2O5-P2O5 system.

Science.gov (United States)

Lee, Sungho; Ueda, Kyosuke; Narushima, Takayuki; Nakano, Takayoshi; Kasuga, Toshihiro

2017-01-01

Niobia/magnesia-containing orthophosphate invert glasses were successfully prepared in our earlier work. Orthophosphate groups in the glasses were cross-linked by tetrahedral niobia (NbO4) and magnesia. The aim of this work is to prepare calcium orthophosphate invert glasses containing magnesia and niobia, incorporating silica, and to evaluate their structures and releasing behaviors. The glasses were prepared by melt-quenching, and their structures and ion-releasing behaviors were evaluated. 31P solid-state nuclear magnetic resonance (NMR) and Raman spectroscopies showed the glasses consist of orthophosphate (PO4), orthosilicate (SiO4), and NbO4 tetrahedra. NbO4 and MgO in the glasses act as network formers. By incorporating SiO2 into the glasses, the chemical durability of the glasses was slightly improved. The glasses reheated at 800°C formed the orthophosphate crystalline phases, such as β-Ca3(PO4)2, Mg3(PO4)2 and Mg3Ca3(PO4)4 in the glasses. The chemical durability of the crystallized glasses was slightly improved. Orthosilicate groups and NbO4 in the glasses coordinated with each other to form Si-O-Nb bonds. The chemical durability of the glasses was slightly improved by addition of SiO2, since the field strength of Si is larger than that of Ca or Mg.

Synthesis of CaO-SiO2-P2O5 mesoporous bioactive glasses with high P2O5 content by evaporation induced self assembly process.

Science.gov (United States)

Zhao, Shan; Li, Yanbao; Li, Dongxu

2011-02-01

Mesoporous bioactive glasses (MBGs) of the CaO-SiO(2)-P(2)O(5) system containing relatively high P(2)O(5) contents (10-30 mol%) were prepared from a sol-gel. An evaporation-induced self-assembly (EISA) technique was used with poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide) (EO(20)-PO(70)-EO(20), P123) acting as a template. The structural, morphological and textural properties of MBGs were investigated by small-angle X-ray diffraction (SAXRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy and a N(2) sorption/desorption technique. SAXRD and TEM results display the reduced long-range ordering of mesopores with increasing P(2)O(5) content. N(2) sorption/desorption analysis shows that all three samples exhibit a type IV isotherm with type H1 hysteresis loops, characteristic of independent cylindrical slim pore channels and this material has a Barret-Joyner-Halenda (BJH) model pore size of ~4 nm and BET specific surface area ~430 m(2)/g. NMR results indicate a more condensed framework for samples with 30 mol% P(2)O(5) than samples with 10 mol% P(2)O(5). For in vitro bioactivity tests where samples were soaked in simulated body fluid (SBF), samples with 30 mol% P(2)O(5) showed higher crystallinity than those with lower P(2)O(5) contents Silicon concentration increased in SBF solution during the soaking period, which indicates MBGs can be degradable in SBF solution.

SiO2 Glass Density to Lower-Mantle Pressures

DEFF Research Database (Denmark)

Petitgirard, Sylvain; Malfait, Wim J.; Journaux, Baptiste

2017-01-01

and present Earth. SiO2 is the main constituent of Earth's mantle and is the reference model system for the behavior of silicate melts at high pressure. Here, we apply our recently developed x-ray absorption technique to the density of SiO2 glass up to 110 GPa, doubling the pressure range...... for such measurements. Our density data validate recent molecular dynamics simulations and are in good agreement with previous experimental studies conducted at lower pressure. Silica glass rapidly densifies up to 40 GPa, but the density trend then flattens to become asymptotic to the density of SiO2 minerals above 60...... GPa. The density data present two discontinuities at similar to 17 and similar to 60 GPa that can be related to a silicon coordination increase from 4 to a mixed 5/6 coordination and from 5/6 to sixfold, respectively. SiO2 glass becomes denser than MgSiO3 glass at similar to 40 GPa, and its density...

Investigation on the utilization of ZrO2-SiO2 composite microspheres for Sr+2 sorption synthesized via sol-gel method

International Nuclear Information System (INIS)

Inan, S.; Tel, H.; Altas, Y.; Eral, M.; Sert, S.; Cetinkaya, B.; Kaplan, U.

2009-01-01

Sr-90 is a typical fission product with a half life of approximately 30 years. The removal of long lived radiotoxic strontium from liquid radioactive waste is an important issue for the health safety. Besides, it reduces the storage problems and facilitates the disposal of the waste. Several methods are utilized for the removal of strontium from liquid radioactive waste. One of the important methods is adsorption processes using metal oxides. Especially, sorbents such as hydrous oxides of titanium, silicium and zirconium and their mixtures, titanium and zirconium phosphates, crystalline silico-titanate(CST) have a good thermal and radiation stability, chemical stability even in strong acidic media, high sorption capacity and compatibility to immobilisation step. The major disadvantage of synthetic inorganic sorbents is their unsuitable granulometric and mechanical properties to use in column applications. Preparation of homogen and uniform spherical particles of these composite sorbents by sol-gel method improves the flow dynamics for column operation and extends its practical applications in industry. In this study, ZrO 2 -SiO 2 composite microspheres were synthesized by sol-gel method. for the sorption of Sr 2 +. The optimum Sr 2 + adsorption conditions were determined by 'Central Composite Design' (CCD). Thermodynamic parameters related to adsorption such as ΔHo, ΔSo and ΔGo were calculated. The adsorption data have been interpreted in terms of Langmuir, Freundlich and D-R isotherms.

Nanocrystal in Er3+-doped SiO2-ZrO2 Planar Waveguide with Yb3+ Sensitizer

International Nuclear Information System (INIS)

Razaki, N. Iznie; Jais, U. Sarah; Abd-Rahman, M. Kamil; Bhaktha, S. N. B.; Chiasera, A.; Ferrari, M.

2010-01-01

Higher doping of Er 3+ in glass ceramic waveguides would cause concentration and pair-induced quenching which lead to inhomogeneous line-width of luminescence spectrum thus reduce output intensity. Concentration quenching can be overcome by introducing ZrO 2 in the glass matrix while co-doping with Yb 3+ which acts as sensitizer would improve the excitation efficiency of Er 3+ . In this study, SiO 2 -ZrO 2 planar waveguides having composition in mol percent of 70SiO 2 -30ZrO 2 doped with Er 3+ and co-doped with Yb 3+ , were prepared via sol-gel route. Narrower and shaper peaks of PL and XRD shows the formation of nanocrystals. Intensity is increase with addition amount of Yb 3+ shows sensitizing effect on Er 3+ .

Sol-gel synthesis of bioactive glass porous scaffolds with addition of porogen agent

International Nuclear Information System (INIS)

Guimaraes, F.B.A.P.; Barrioni, B.R.; Oliveira, A.C.X.; Oliveira, A.A.R.; Pereira, M.M.

2016-01-01

The use of biomaterials capable of generating a biological response has been one of the biggest progresses in regenerative medicine, due to their ability to support growth stimulation and damaged tissue regeneration. In this context, bioceramics, particularly bioactive glass (BG), were the subject of many studies. The technique of porogen agent addition for the synthesis of scaffolds is an interesting procedure, because several types of porogen agents can be used. The aim of the present work was to obtain scaffolds using four porogen agents and to evaluate the effects that a change in treatment temperature can have on their crystallinity. Scaffolds of sol-gel bioactive glass 100S (100% SiO 2 ) using as porogen agents paraffin 1, paraffin 2, wax and CMC (carboxymethyl cellulose) were synthesized and characterized. As the best results were obtained with paraffin 1, scaffolds 58S (60%SiO 2 -36%CaO-4%P 2 O 5 ) and 100S using paraffin 1 as porogen agent were prepared. The scaffolds were submitted to different treatment temperatures to evaluate the effect on their crystallinity. Pore structure was analyzed by scanning electron microscopy and micro-computed tomography. Scaffolds presented satisfactory pore size and pore size distribution, important characteristics for scaffolds because they allow cell migration, nutrient transport, vascularisation and tissue ingrowth. X-ray powder diffraction showed the amorphous nature of the scaffolds. At 900 °C, scaffolds BG 58S and 100S showed a small increase in crystallinity. BET analysis (N 2 -adsorption) indicated a mesoporous structure. The specific surface area varied from 73.2 m 2 /g for scaffold 58S treated at 800 °C to 331.2 m 2 /g for scaffold 100S treated at 800 °C. The materials obtained showed no toxic effects by MTT cytotoxicity assays. Results showed that the development of scaffolds is possible using porogen agents, with 3D interconnected porous structure and might therefore be a potential biomaterial for bone

Study on spectroscopic properties and effects of tungsten ions in 2Bi2O3-3GeO2/SiO2 glasses.

Science.gov (United States)

Yu, Pingsheng; Su, Liangbi; Cheng, Junhua; Zhang, Xia; Xu, Jun

2017-04-01

The 2Bi 2 O 3 -3GeO 2 /SiO 2 glass samples have been prepared by the conventional melt quenching technique. XRD patterns, absorption spectra, excitation-emission spectra and Raman measurements were utilized to characterize the synthesized glasses. When substitute SiO 2 for GeO 2 , the 0.4Bi 2 O 3 -(0.4-0.1)GeO 2 -(0.2-0.5)SiO 2 glasses exhibit strong emission centered at about 475nm (under 300nm excitation), and the decay constants are within the scope of 20-40ns. W doping into 2Bi 2 O 3 -3SiO 2 glass could increase the emission intensity of 470nm, and the W-doped 2Bi 2 O 3 -3SiO 2 glass has shown another emission at about 433nm with much shorter decay time (near 10ns). The 2Bi 2 O 3 -3GeO 2 /SiO 2 glass system could be the possible candidate for scintillator in high energy physics applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Crack-resistant Al2O3-SiO2 glasses.

Science.gov (United States)

Rosales-Sosa, Gustavo A; Masuno, Atsunobu; Higo, Yuji; Inoue, Hiroyuki

2016-04-07

Obtaining "hard" and "crack-resistant" glasses have always been of great important in glass science and glass technology. However, in most commercial glasses both properties are not compatible. In this work, colorless and transparent xAl2O3-(100-x)SiO2 glasses (30 ≤ x ≤ 60) were fabricated by the aerodynamic levitation technique. The elastic moduli and Vickers hardness monotonically increased with an increase in the atomic packing density as the Al2O3 content increased. Although a higher atomic packing density generally enhances crack formation in conventional oxide glasses, the indentation cracking resistance increased by approximately seven times with an increase in atomic packing density in binary Al2O3-SiO2 glasses. In particular, the composition of 60Al2O3 • 40SiO2 glass, which is identical to that of mullite, has extraordinary high cracking resistance with high elastic moduli and Vickers hardness. The results indicate that there exist aluminosilicate compositions that can produce hard and damage-tolerant glasses.

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Science.gov (United States)

Bansal, Narottam P.; Hyatt, Mark J.

1989-01-01

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Preparation and characterization of Sio2CaCl2 nanocomposite by the sol-gel method

International Nuclear Information System (INIS)

Tohidi, S. H.; Ziaie, F.; Abdolmaleki, A.

2009-01-01

The SiO 2 CaCl 2 hybrid porous materials were prepared by the sol-gel method. This process was conducted by the hydrolysis and condensation of Tetraethyl orthosilicate by replacement of ethanol from alcogel and drying at the ambient temperature to obtain xerogel structure. The alcogel samples were synthesized from Tetraethyl orthosilicate, EtOH, H 2 O, HCl, NH 4 OH and CaCl 2 , while the total molar ratio of the compounds was 1: 9: 4: 8 x 10 -4 , 8 x 10 -3 , respectively. Xerogel containing 30 wt % of CaCl 2 (dry matter) was prepared and characterized by Scanning Electron Microscopy, Transmission Electron Microscopy, Fourier Transmittance Infra Red spectrum, Energy Dispersive X-ray and Thermal Gravimetric Analysis systems. The results obtained from Scanning Electron Microscopy and Energy Dispersive X-ray showed the micrograph of CaCl 2 on the silica and chemical elemental analysis, respectively. On the other hand, The Transmission Electron Microscopy micrograph confirmed average particle size of SiO 2 -CaCl 2 about 50 nm and Fourier Transmittance Infra Red spectrum described the functional groups of the nano composite. The thermal analysis of SiO 2 -CaCl 2 nano composite was performed using Thermal Gravimetric Analysis system and the results showed that the suitable temperature for initial thermal treatment was about 200 d eg C .

Study of a Mixed Alkaline–Earth Effect on Some Properties of Glasses of the CaO-MgO-Al2O3-SiO2 System

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Valle-Fuentes, J. F.

2007-06-01

Full Text Available In the present work, we studied a “Mixed Alkaline–Earth Effect”, i.e. the non-linear behaviour showed by the glass transition temperature as well as by the compressive strength of glasses of the CaO-MgO-Al2O3-SiO2 system, when a part of the CaO contained in them was substituted by a BaO/SrO mixture, in variable molar proportions. An important factor for the occurrence of this phenomenon was the difference in atomic weight, ionic radii and field strength of the Ba2+ and Sr2+ ions in comparison with those corresponding to the Ca2+ ion. Another factor considered was the likely occurrence of a microphase separation caused by the addition of BaO and/or SrO, together with the presence of F- and Mg2+ in the glasses. Other glass properties studied as a function of the CaO substitution level were density, glass molar volume, oxygen molar volume, packing fraction, and chemical resistance in neutral, basic and acidic aqueous media. In general, the structural reinforcement of the glass network caused by the partial substitution of CaO by a BaO/SrO mixture was accompanied by an improvement in the alkaline resistance of the materials, which were found to be suitable for applications in corrosive environments, especially in basic media. Keywords: Mixed alkaline–earth effect; CaO-MgO-Al2O3-SiO2 system; glass properties.En el presente trabajo, se estudia el comportamiento no lineal mostrado por la temperatura de transición vítrea y por la resistencia a la compresión de vidrios del sistema CaO-MgO-Al2O3-SiO2, cuando una parte del CaO contenido en los mismos es sustituido por una mezcla de BaO/SrO, en relación molar variable. Factores importantes para que se de este comportamiento son la diferencia entre pesos atómicos, radios iónicos e intensidad de campo de los iones Ba2+ y Sr2+ y los del propio ión Ca2+. Otro factor considerado ha sido la probable existencia de una separación de microfases originada por la adición de BaO y/o SrO, junto con la

Characterisation and Properties of Lithium Disilicate Glass Ceramics in the SiO2-Li2O-K2O-Al2O3 System for Dental Applications

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Naruporn Monmaturapoj

2013-01-01

Full Text Available This work proposes four different glass formulas derived from the SiO2-Li2O-K2O-Al2O3 system to investigate the effect of glass composition on their crystal formations and properties. Glass LD1 was SiO2-Li2O-K2O-Al2O3 system with the addition of P2O5 and CaF2 as nucleating agents. In Glass LD2, a slight amount of MgO was mixed in order to increase the viscosity of the melting glass. Finally, the important factor of Si : Li ratio was increased in Glasses LD3 and LD4 with compositions otherwise the same as LD1 and LD2. The results found that P2O5 and CaF2 served as a nucleating site for lithium phosphate and fluorapatite to encourage heterogenous nucleation and produce a fine-grained interlocking microstructure of lithium disilicate glass ceramics. MgO content in this system seemed to increase the viscosity of the melting glass and thermal expansion coefficient including the chemical solubility. Increasing the Si : Li ratio in glass compositions resulted in the change of the microstructure of Li2Si2O5 crystals.

Raman and optical absorption spectroscopic investigation of Yb-Er codoped phosphate glasses containing SiO2

Institute of Scientific and Technical Information of China (English)

Youkuo Chen; Lei Wen; Lili Hu; Wei Chen; Y. Guyot; G. Boulon

2009-01-01

Yb-Er codoped Na2O-Al2O3-P2Os-xSiO2 glasses containing 0 鈥? 20 mol% SiO2 were prepared successfully. The addition of SiO2 to the phosphate glass not only lengthens the bond between P5+ and non-bridging oxygen but also reduces the number of P=O bond. In contrast with silicate glass in which there is only four-fold coordinated Si4+, most probably there coexist [SiO4] tetrahedron and [SiO6] octahedron in our glasses. Within the range of 0 鈥? 20 mol% SiO2 addition, the stimulated emission cross-section of Er3+ ion only decreases no more than 10%. The Judd-Ofelt intensity parameters of Er3+, 惟.2 does not change greatly, but 惟74 and 惟6 decrease obviously with increasing SiO2 addition, because the bond between Er + and O2- is more strongly covalently bonded.

Effects of Al/P composition ratio on the crystallization of MgO-CaO-Al203-SiO2-P2O5 bioglass-ceramic system

Energy Technology Data Exchange (ETDEWEB)

Wu, Shihching; Hon, Minhsiung [National Cheng-Kung Univ., Taiwan (Taiwan, Province of China)

1993-06-01

Effects of Al/P composition ratio on the crystallization of apatite and anorthite were investigated by differential thermal analysis ( DTA ) using series of glasses with the nominal composition of 3.0wt% MgO, 35.0wt% CaO, 41.4wt% SiO2 and 20.6wt%(Al2O3+P205). With the decrease of Al/P ratio, the activation energy for apatite crystallization is decreased and the apatite exotherm is shifted to the lower temperature. On the other hand, anorthite crystallized from the specimen surface, the activation energy for anorthite is increased with the decrease of Al/P ratio, however the exotherm is not shifted significantly. Roughly estimated values of Avrami parameters, n, which is related to the directionality of crystal growth, for apatite and anorthite have been 2 and 1 respectively. This had shown that apatite implies bulk crystallization and anorthite signifies surface crystallization. Also the SEM observations of the crystals revealed that there was one dimensional crystal growth for anorthite and spherulitic growth for apatite. 17 refs., 6 figs., 2 tabs.

Effect of calcium fluoride on sintering behaviour of SiO2-CaO-Na2O-MgO glass-ceramic system

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Bahman Mirhadi

2012-09-01

Full Text Available The crystallization characteristics of glasses based on the SiO2-CaO-Na2O-MgO (SCNM system containing calcium fluoride (CaF2 have been investigated by differential thermal analysis (DTA, X-ray diffraction (XRD and scanning electron microscopy (SEM. The partial replacement of CaO by CaF2 in the studied glass-ceramics led to the development of different crystalline phase assemblages, including wollastonite and diopside using various heat-treatment processes. With the increase of CaF2 content, the crystallization temperature of the glass and the strength of the crystallization peak temperature decreases. Addition of CaF2 up to 6.0 mol%, as expected, improved the sinterability. This sample reached to maximum density by sintering at 950 °C.

Modulation of the thermoluminescence glow curve of sol-gel synthesized SiO2 and Si O-2:Eu through thermal annealing

International Nuclear Information System (INIS)

Salas J, Ch. J.; Cruz V, C.; Bernal, R.; Castano, V. M.

2015-10-01

Full text: Due to the increasing use of ionizing radiations, is necessary to monitor the radiation fields and exposure doses in facilities in which they are used. Different facilities or applications involve the use of different radiation and doses, and the sort of needed dosimetry also varies. Sometimes a conventional thermoluminescence (Tl) dosimetry satisfy the requirements since the record of the accumulated dose in a time interval is enough, but other cases could require for real-time measurement of a radiation field, being required a non-Tl dosimetric technique. On the other hand, different applications involve the use of different dose ranges, and so dosimeters with different sensitivities are needed. To solve the diverse needs of radiation detectors and dosimeters, a lot of phosphors materials has been characterized concerning their dosimetric capabilities. For medical application, biocompatible materials are desirable. In this work, we present experimental evidence that Sol-Gel synthesized SiO 2 and SiO 2 :Eu phosphors exhibit Tl glow curves composed by the superposition of several individual glow peaks each located at different temperature ranging from values below 100 up to temperatures greater than 400 degrees C, whose relative sensitivities can be modified by subjecting the phosphors to different thermal annealing. By modulating the relative intensities of the individual Tl peaks, glow curves with different shapes are obtained in such a way that SiO 2 and SiO 2 :Eu can be used to develop dosimeters useful for different dose ranges, and for both, conventional thermoluminescence dosimetry and non-thermoluminescence afterglow-based) dosimetry. (Author)

Non-isothermal crystallization kinetics of Fe{sub 2}O{sub 3}–CaO–SiO{sub 2} glass containing nucleation agent P{sub 2}O{sub 5}/TiO{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Li, Bin, E-mail: stra-ceo@163.com; Wang, Yongya; Luo, Wenqin; Li, Jingfen [Huzhou University, Department of Material Chemistry (China); Li, Jianyou [Huzhou Central Hospital, Orthopedic Department (China)

2017-03-15

Fe{sub 2}O{sub 3}–CaO–SiO{sub 2} glass ceramics containing nucleation agent P{sub 2}O{sub 5}/TiO{sub 2} were prepared by sol-gel method. The samples were characterized by X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The activation energy and kinetic parameters for crystallization of the samples were calculated by the Johnson-Mehi-Avrami (JMA) model and Augis-Bennett method according to the results of DSC. The results showed that the crystallization mechanism of Fe{sub 2}O{sub 3}–CaO–SiO{sub 2} glass, whose non-isothermal kinetic parameter n = 2.3, was consistent with surface crystallization of the JMA model. The kinetics model function of Fe{sub 2}O{sub 3}–CaO–SiO{sub 2} glass, f(α) = 2.3(1–α)[–ln(1–α)]{sup 0.57}, was also obtained. The addition of nucleation agent P{sub 2}O{sub 5}/TiO{sub 2} could reduce the activation energy, which made the crystal growth modes change from onedimensional to three-dimensional.

Effect of B2O3 and P2O5 on fluorosilicic mica glass-ceramic sintering process

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Wu S.

2010-01-01

Full Text Available To study the effect of B2O3 and P2O5 on fluorosilicic mica glass-ceramic sintering process, six sets of K2O-MgO-SiO2-F glasses were prepared by using B2O3 and P2O5 as sintering aid, respectively. Green bodies of the glass powder were formed by gel casting and sintered at 800, 850, 900, 950, 1000oC for 6 hours, resectively. The sintering and crystallization behavior were studied by thermal shrinkage , X-ray diffraction and SEM. The results showed that the shrinkage rate of the glass with 2wt% B2O3 and P2O5 was highest, while the rate of the glass with 5wt% P2O5 was lowest. An additional crystal other than fluorosilicic mica was precipitated in the glass ceramics generated by sintering of glass powder. The present results confirmed that the glass powder of pure K2O-MgO-SiO2-Fsystem had poor sinterability, while glass powder with minor addition of P2O5 and/or B2O3 showed good sinterability. This result was also verified by SEM.

Characterization and toxicity studies of bioglass by Sol-gel method for prostate cancer therapy

International Nuclear Information System (INIS)

Roberto, Wanderley S.; Veloso, Gabriela A.; Silva, Luciana; Campos, Tarcísio P.R.

2017-01-01

One of the most advanced methods for the treatment of prostate cancer in the initial stage is brachytherapy, which uses titanium seeds, incorporated with 125 I, which is radioactive, and which is implanted in the prosthetic volume. In recent studies, we investigated the possibility of applying the Sol-Gel (SG) method for the production of bioactive seeds, incorporated with radioactive Sm in silica glasses for the treatment of cancer. In this project three compositions of the glasses of the SiO 2 -CaO system were synthesized using the SG method. The chemical and physical composition of the seeds were analyzed by X-ray diffraction and Atomic Absorption Analysis. A pilot study of in vivo and in vitro toxicity was conducted in rabbit and PC-3 lineage cells. The results showed that the ceramic matrices in the SiO 2 - CaO - Sm system present no toxicity in the in vivo model presenting no post-implant inflammatory process. None restriction of in vitro cell growth was found. In conclusion, there is no toxicity in seeds and the radiotoxicity will occur only in the period in which the seeds present activity coming from 153 Sm

Photocatalytic hydrogen production using visible-light-responsive Ta 3N5 photocatalyst supported on monodisperse spherical SiO2 particulates

KAUST Repository

Liu, Xiaoming; Zhao, Lan; Domen, Kazunari; Takanabe, Kazuhiro

2014-01-01

Fine nanoparticles of Ta3N5 (10-20 nm) were synthesized on the surfaces of SiO2 spheres with a diameter of ∼550 nm. A sol-gel method was used to modify the surface of SiO2 with Ta2O5 from TaCl5 dissolved in ethanol in the presence of citric acid

Research of the lime rich portions of the CaO-SiO2-P2O5 system

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Puertas, F.

1995-03-01

Full Text Available A detailed study has been carried out to explain the influence of Pp^ in silicate phases and in industrial raw meals upon their mineralogical compositions. Some compositions in the lime rich portion of the CaO-SiO2-P2O5 system are studied using laboratory reactants. The results showed that the compositions lying in the range of CaO = 69,5-70,1; P2O5= 16,2-19,5; SiO2 = 11,1-13,6 (wt% give, at 1000 °C, the mineralogical composition (HAp, β-C2S, C5PS which can develop a high strength in chemically bonded ceramics. At high temperature (1400 ºC these compositions give a large amount of silicocarnotite (C5PS and 2C2.C3P phase. A selected composition of the industrial raw meal with added phosphate: CaO = 62,66; SiO2 -= 17,33; Al2O3 = 4,88; Fe2O3 = 4,29; P2O5 = 8,73; MgO = 2,09 (wt% forms at 1350 ºC a clinker containing high amount of α-C2S to replace C3S. Such a clinker may have good applications in the synthesis of active belite cement.Se estudia con detalle la influencia del P2O5 sobre las composiciones mineralógicas en fases silicato y en un crudo industrial. Asimismo se estudian algunas composiciones de la zona rica en cal del sistema CaO-SiO2-P2O5 utilizando reactivos químicos. Los resultados demuestran que, a presión atmosférica y recinto abierto, las composiciones dentro de los límites CaO = 69,5-70,1; P2O5= 16,2-19,5; SiO2 = 11,1-13,6 (% en peso dan a 1000ºC la composición mineralógica siguiente: HAp, β-C2S, C5PS; pueden desarrollar una alta resistencia química en "chemically bonded ceramics". A altas temperaturas (1400°C producen una elevada proporción de silicocarnotita (C5PS S y la fase 2C2.C3P. Con la adición de fosfato a una determinada dosificación de crudo industrial (CaO = 62,66; SiO2 = 17,33; Al2O3 = 4,88; Fe2O3 = 4,29; P2O5 = 8,73; MgO = 2,09 -% en peso- se forma, a 1350°C, un clinker que contiene una alta proporción de α-C2S que reemplaza al C3S. Este clinker puede tener buenas aplicaciones en la obtención de

Stabilization/Solidification of Radioactive LiCl-KCl Waste Salt by Using SiO2-Al2O3-P2O5(SAP) Inorganic Composite: Part 1. Dechlorination Behavior of LiCl-KCl and Characteristics of Consolidation

International Nuclear Information System (INIS)

Cho, In Hak; Park, Hwan Seo; Ahn, Soo Na; Kim, In Tae; Cho, Yong Zun

2012-01-01

The metal chloride wastes from a pyrochemical process to recover uranium and transuranic elements has been considered as a problematic waste difficult to apply to a conventional solidification method due to the high volatility and low compatibility with silicate glass. In this study, a dechlorination approach to treat LiCl-KCl waste for final disposal was adapted. In this study, a SiO 2 -Al 2 O 3 -P 2 O 5 (SAP) inorganic composite as a dechlorination agent was prepared by a conventional sol-gel process. By using a series of SAPs, the dechlorination behavior and consolidation of reaction products were investigated. Different from LiCl waste, the dechlorination reaction occurred mainly at two temperature ranges. The thermogravimetric test indicated that the first reaction range was about 400 degree C for LiCl and the second was about 700 degree C for KCl. The SAP 1071 (Si/Al/P=1/0.75/1 in molar) was found to be the most favorable SAP as a dechlorination agent under given conditions. The consolidation test revealed that the bulk shape and the densification of consolidated forms depended on the SAP/Salt ratios. The leaching test by PCT-A method was performed to evaluate the durability of consolidated forms. This study provided the basic information on the dechlorination approach. Based on the experimental results, the dechlorination method using a SiO 2 -Al 2 O 3 -P 2 O 5 (SAP) could be considered as one of alternatives for the immobilization of waste salt.

Photocatalytic Removal of Phenol under Natural Sunlight over N-TiO2-SiO2 Catalyst: The Effect of Nitrogen Composition in TiO2-SiO2

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Viet-Cuong Nguyen

2009-01-01

Full Text Available In this present work, high specific surface area and strong visible light absorption nitrogen doped TiO2-SiO2 photocatalyst was synthesized by using sol-gel coupled with hydrothermal treatment method. Nitrogen was found to improve the specific surface area while it also distorted the crystal phase of the resulting N-TiO2-SiO2 catalyst. As the N/ (TiO2-SiO2 molar ratio was more than 10%, the derived catalyst presented the superior specific surface area up to 260 m2/g. Nevertheless, its photoactivity towards phenol removal was observed to significantly decrease, which could results from the too low crystallinity. The nitrogen content in N-TiO2-SiO2 catalyst was therefore necessary to be optimized in terms of phenol removal efficiency and found at ca. 5%. Under UVA light and natural sunlight irradiation of 80 min, N(5%-TiO2-SiO2 catalyst presented the phenol decomposition efficiencies of 68 and 100%, respectively. It was also interestingly found in this study that the reaction rate was successfully expressed using a Langmuir-Hinshelwood (L-H model, indicating the L-H nature of photocatalytic phenol decomposition reaction on the N-TiO2-SiO2 catalyst.

Structural study of some gadolinium glass ceramics obtained by sol-gel method

International Nuclear Information System (INIS)

Coroiu, Ilioara; Simiti, Vida I.; Bratu, I.; Borodi, Gh.; Darabont, Al.

2004-01-01

Increased interest in silicate systems containing different rare earth oxides has resulted from their important applications in various fields of technology including laser, optical fiber and optical waveguides in telecommunication applications, microelectronics and catalysis. Glass-ceramics of 0.95 SiO 2 -0.05 Na 2 O composition containing up to 15% molar Gd 2 O 3 were obtained by the sol-gel method. We chose the sol-gel method because this offers the advantage of a good chemical homogeneity and a better control of physical and chemical properties in comparison with traditional methods used to obtain glasses and ceramics. The obtained samples were pressed at 200 kgf/cm 2 as disks with a diameter of Φ=22 mm and a thickness of around 1 mm. Then, they were heat-treated at 250 deg C, 500 deg C and 1000 deg C for about 48 hours. The structural study was made using X-ray diffraction, scanning electron microscopy (SEM) and IR spectroscopy. The X-ray diffraction patterns show that addition of Gd 2 O 3 exerts an important influence on the crystallization process of the studied samples. The crystalline phase decreases with increasing the Gd 2 O 3 concentration. SEM data support this assertion. IR spectra point out also that the increasing of the gadolinium oxide content and the thermal treatment temperature produce the strengthening of the glass ceramic network. Thus, the gadolinium ions play the role of network modifier of the glass ceramic structure. (authors)

Natural CaO-TiO2-SiO2 based ceramics

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Jelena Pantić

2011-06-01

Full Text Available Lešnica river deposits consist of a large number of minerals of different grain sizes including sphene. Since it is very difficult to obtain pure monophase titanite by different synthetic routes (sol-gel, coprecipitation, combustion, spray pyrolysis and hydrothermal method, the aim of this work was to study the structure of the sphene from the Lešnica river deposits and possibility of using it as a natural precursor for CaO-TiO2-SiO2 based ceramics. The sphene from Lešnica was analyzed by different methods: tristimulus colorimetry, infrared spectroscopy, electron microprobe and X-ray single crystal diffraction. It was confirmed that Al, Fe, Mn and P are present in the sphene structure and proposed that corresponding structural formula could be: (Ca2+1.008 Mn2+0.0021.010(Ti4+0.901 Fe3+0.033 Al3+0.060 P5+0.0010.995 Si4+1.024 O2-5.

Liquidus Temperature of SrO-Al2O3-SiO2 Glass-Forming Compositions

DEFF Research Database (Denmark)

Abel, Brett M.; Morgan, James M.; Mauro, John C.

2013-01-01

. In the composition range of interest for industrial glasses, Tliq tends to decrease with increasing strontium-to-alumina ratio. We find that cristobalite, mullite, and slawsonite are the dominant devitrification phases for the compositions with high SiO2, SiO2+Al2O3, and SrO contents, respectively. By comparison...... with the phase diagrams for CaO-Al2O3-SiO2 and MgO-Al2O3-SiO2 systems, we have found that for the highest [RO]/[Al2O3] ratios, Tliq exhibits a minimum value for R = Ca. Based on the phase diagram established here, the composition of glass materials, for example, for liquid crystal display substrates, belonging...... to the SrO-Al2O3-SiO2 family may be designed with a more exact control of the glass-forming ability by avoiding the regions of high liquidus temperature....

P2O5-doping in waste glasses: evolution of viscosity and crystallization processes

Science.gov (United States)

Tarrago, Mariona; Espuñes, Alex; Garcia-Valles, Maite; Martinez, Salvador

2015-04-01

Current concern for environmental preservation is the main motive for the study of new, more sustainable materials. Increasing amounts of sewage sludge are produced in wastewater treatment plants over the world every day. This fact represents a major problem for the municipalities and industries due to the volume of waste and also to the contaminant elements it may bear, which require expensive conditions for disposal in landfills. Vitrification is an established technique in the inertization of different types of toxic wastes (such as nuclear wastes and contaminated soils) that has been used successfully for sewage sludge. Glasses of basaltic composition (43.48SiO2-14.00Al2O3-12.86Fe2O3-10.00CaO-9.94MgO-3.27Na2O-1.96K2O-0.17MnO-0.55P2O5-2.48TiO2) are used as a laboratory analogous of wastes such as sewage sludge and galvanic sludge to study the properties of the inertization matrix. This basaltic matrix is doped by adding 1%, 2%, 3%, 4% and 20% of P5O5 in order to cover the compositional range of phosphate in sewage sludge encountered in the literature. In this study, the focus has been placed in the effect of the concentration of phosphate (P2O5) in glass stability, thermal properties and evolution of viscosity with temperature. The dependence of viscosity on temperature and the thermal behaviour of these glasses are critical parameters in the design of their production process. Regarding the compositional limits of the mixture, it has been observed that melt reactivity is much increased when P2O5 content is over 4%, hindering the glass conformation process. Moreover, stanfieldite (calcium and magnesium phosphate) crystallized during glass making when phosphate concentration approached 20%, hence establishing the upper limit for glass stability. Viscosity is also dramatically increased in this range, hence requiring production amends. Differential thermal analysis has provided nucleation and crystallization temperatures of the glasses around 915°C and 1050�

Magnetic nanoparticles induced dielectric enhancement in (La, Gd)2O3: SiO2 composite systems

Science.gov (United States)

Kao, T. H.; Mukherjee, S.; Yang, H. D.

2013-11-01

Magnetic Gd2O3 and non-magnetic La2O3 nanoparticles (NPs) have been synthesized together with different doping concentrations in SiO2 matrix via sol-gel route calcination at 700 °C and above. Properly annealed NP-glass composite systems show enhancement of dielectric constant and magnetodielectric effect (MDE) near room temperature, depending on superparamagnetic NPs concentrations. From application point of view, the enhancement of dielectric constant along with MDE can be achieved by tuning the NPs size through varying calcination temperature and/or increasing the doping concentration of magnetic rare earth oxide.

Structural and optical properties of sol-gel deposited proton conducting Ta{sub 2}O{sub 5} films

Energy Technology Data Exchange (ETDEWEB)

Ozer, N.; Lampert, C.M.

1995-08-01

Proton conducting tantalum oxide films were deposited by spin coating using a sol-gel process. The coating solutions were prepared using Ta(OC{sub 2}H{sub 5}){sub 5} as a precursor. X-ray diffraction studies determined that the sol-gel films, heat treated at temperatures below 400 C, were amorphous. Films heat treated at higher temperatures were crystalline Ta{sub 2}O{sub 5}. The solar transmission values (T{sub s}) of tantala films on glass generally range from 0.8--0.9 depending on thickness. The refractive index and the extinction coefficient were evaluated from transmittance characteristics in the UV-VIS-NIR regions. The refractive index values calculated at 550 nm increased from 1.78 to 1.97 with increasing heat treatment from 150 to 450 C. The films heat treated at different temperatures showed low absorption with extinction coefficients of less than k=1x10{sup -3} in the visible range. Spectrophotometric and impedance spectroscopic investigations performed on Ta{sub 2}O{sub 5} films revealed that these films have protonic conductivity of 3.2x10{sup -6} S/cm. The films are suitable for proton conducting layers in electrochromic (EC) devices.

Synthesis and Luminescence Properties of Yellow-emitting SiO2/Zn2SiO4: Mn Nanocomposite

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Karim OMRI

2014-05-01

Full Text Available Yellow light emitting Mn2+-doped b-Zn2SiO4 phosphor nanoparticles embedded in SiO2 host matrix, were prepared by a simple solid-phase reaction under natural atmosphere at 1500 °C for 2 hours after the incorporation of manganese doped zinc oxide nanoparticles in silica using sol-gel method. The SiO2/Zn2SiO4:Mn nanocomposite was characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy (SEM and photoluminescence (PL. The nanopowder was crystallized in triclinic b-Zn2SiO4 phase with a particles size varies between 70 nm and 84 nm. The SiO2/b-Zn2SiO4:Mn nanocomposite exhibited a broad yellow emission band at 575 nm under UV excitation light. The dependence of the intensity and energy position of the obtained PL band on measurement temperature and power excitation will be discussed.

Effects of four step sintering on Y2O3: SiO2 nanocomposite

International Nuclear Information System (INIS)

Ahlawat, Rachna

2015-01-01

Need for high performance materials for advanced applications have led to the development of new concepts in materials design processing and their fabrication. The development of nanocrystalline materials with improved and novel properties is an important turning point in materials research. In present work, we report synthesis and structural characterization of Y 2 O 3 : SiO 2 nanocomposite. Sol-gel technique is being used to prepare-Y 2 O 3 SiO 2 nanocomposite due to its effectiveness in preparing samples with good mixing of starting materials and at relatively low reaction temperature. We have used Y(NO 3 ) 3 .4H 2 O and TEOS as precursors and followed usual approach of sol-gel technique, the final product of Y 2 O 3 : SiO 2 nanocomposite is obtained in the form of powder. The powder samples were sintered at different temperature for different time durations in programmable muffle furnace. The samples were characterized by complementary techniques as X-Ray Diffraction (XRD), Fourier Transforms Infrared Spectroscopy (FTIR) and Transmission Electron Microscopy (TEM). (author)

Sol-gel prepared B2O3-SiO2 thin films for protection of copper substrates

International Nuclear Information System (INIS)

Gouda, M.; Ahmed, M.S.; Shahin, M.A.

2000-01-01

Full text.Borosilicate coating has potential for applications in the field of electronics, e.g., as passivation layers. One of the main difficulties for applying these films by the conventional melting process is the extensive volatilization of B 2 O 3 from the melt. In this work transparent borosilicate films of 2OB 2 O3.8OSiO 2 (in mole %). Prepared by the sole gel method, were applied onto copper substrates by dip-coating technique. The transparency of these films was very sensitive to the humidity of the atmosphere during the coating process. Transparent films were obtained below 20% relative humidity at 20 celsius degree. High temperature oxidation tests, at about 585 celsius degree stream of air, showed that the sol-gel prepared 2OB 2 O 3 .8OSiO 2 thin films are protective coating for copper substrates under fairly severe temperature gradient and oxidizing atmosphere. It was found that the protective action of these films depends on the film thickness

Fabrication and characterization of Er+3 doped SiO2/SnO2 glass-ceramic thin films for planar waveguide applications

Science.gov (United States)

Guddala, S.; Chiappini, A.; Armellini, C.; Turell, S.; Righini, G. C.; Ferrari, M.; Narayana Rao, D.

2015-02-01

Glass-ceramics are a kind of two-phase materials constituted by nanocrystals embedded in a glass matrix and the respective volume fractions of crystalline and amorphous phase determine the properties of the glass-ceramics. Among these properties transparency is crucial in particular when confined structures, such as, dielectric optical waveguides, are considered. Moreover, the segregation of dopant rare-earth ions, like erbium, in low phonon energy crystalline medium makes these structures more promising in the development of waveguide amplifiers. Here we are proposing a new class of low phonon energy tin oxide semiconductor medium doped silicate based planar waveguides. Er3+ doped (100-x) SiO2-xSnO2 (x= 10, 20, 25 and 30mol%), glass-ceramic planar waveguide thin films were fabricated by a simple sol-gel processing and dip coating technique. XRD and HRTEM studies indicates the glass-ceramic phase of the film and the dispersion of ~4nm diameter of tin oxide nanocrystals in the amorphous phase of silica. The spectroscopic assessment indicates the distribution of the dopant erbium ions in the crystalline medium of tin oxide. The observed low losses, 0.5±0.2 dB/cm, at 1.54 μm communication wavelength makes them a quite promising material for the development of high gain integrated optical amplifiers.

Effect of V2O5 on SrO-ZnO-B2O3-SiO2 glass-ceramics for high temperature sealant application

Science.gov (United States)

Tiwari, Babita; Bhatacharya, S.; Dixit, A.; Gadkari, S. C.; Kothiyal, G. P.

2012-06-01

Glasses in the SrO-ZnO-B2O3-SiO2 (SZBS) system with and without V2O5 were prepared by melt-quench method and transformed into glass-ceramics by controlled crystallization. Investigated glasses and glass-ceramics have thermal expansion coefficients (TEC) in the range of 95-120 × 10-7/°C (30-600 °C), which match closely with TEC of other components of solid oxide fuel cell (SOFC). Study of thermo-physical properties of SZBS glasses revealed the network modifying effect of V2O5. Addition of V2O5 increases the TEC and decreases the viscosity of the glass which is beneficial for making seal with Crofer-22-APU. Microstructural investigations have shown good bonding of SZBS glasses with Crofer-22-APU. Elemental line scans indicate that inter-diffusion of Fe, Cr and Si across interface, which is thought to be responsible for good bonding with Crofer-22-APU.

Evaluation of sol-gel derived Eu2+ activated SrMgAl2SiO7 as a novel nanostructure luminescent pigment

International Nuclear Information System (INIS)

Sameie, H.; Salimi, R.; Sabbagh Alvani, A.A.; Sarabi, A.A.; Moztarzadeh, F.; Tahriri, M.

2010-01-01

A novel nanostructure pigment of Eu 2+ doped SrMgAl 2 SiO 7 was prepared via the sol-gel route. The phase composition and condition of crystallites during heating were characterized by X-ray diffraction (XRD) analysis. Investigation of optical properties by spectrophotometer illustrated that under short ultraviolet excitation wavelength, the main emission peak occurred at about 415-420 nm. Also, relatively pure purplish blue color was observed that can be ascribed to the 4f 6 5d 1 ( 2 D)→4f 7 ( 8 S 7/2 ) transition of Eu 2+ . The effect of calcination temperature on the luminescence properties of the phosphors was evaluated and, also in this case, scanning electron microscope (SEM) was employed. From colorimetry results, color coordinations of phosphor shift towards the deep blue region as calcination temperature increases. Finally, grain size of products at optimum calcination temperature was estimated to be about 20-30 nm using Scherrer's equation, which was consistent with transmission electron microscopy (TEM) observations.

UV-VUV laser induced phenomena in SiO2 glass

International Nuclear Information System (INIS)

Kajihara, Koichi; Ikuta, Yoshiaki; Oto, Masanori; Hirano, Masahiro; Skuja, Linards; Hosono, Hideo

2004-01-01

Creation and annihilation of point defects were studied for SiO 2 glass exposed to ultraviolet (UV) and vacuum UV (VUV) lights to improve transparency and radiation toughness of SiO 2 glass to UV-VUV laser light. Topologically disordered structure of SiO 2 glass featured by the distribution of Si-O-Si angle is a critical factor degrading transmittance near the fundamental absorption edge. Doping with terminal functional groups enhances the structural relaxation and reduces the number of strained Si-O-Si bonds by breaking up the glass network without creating the color centers. Transmittance and laser toughness of SiO 2 glass for F 2 laser is greatly improved in fluorine-doped SiO 2 glass, often referred as 'modified silica glass'. Interstitial hydrogenous species are mobile and reactive at ambient temperature, and play an important role in photochemical reactions induced by exposure to UV-VUV laser light. They terminate the dangling-bond type color centers, while enhancing the formation of the oxygen vacancies. These findings are utilized to develop a deep-UV optical fiber transmitting ArF laser photons with low radiation damage

Synthesis of bioactive poly(ethylene glycol)/SiO2-CaO-P2O5 hybrids for bone regeneration

International Nuclear Information System (INIS)

Liu Wei; Wu Xiaohong; Zhan Hongbing; Yan Fuhua

2012-01-01

Poly(ethylene glycol) (PEG)/SiO 2 -CaO-P 2 O 5 hybrid xerogels were prepared using a room temperature sol-gel process. The advantage of this hybrid material over conventional composites is the molecular scale interactions between the bioactive inorganic components and the biodegradable organic components. Since PEG was added into the sol when the hydrolysis of tetraethoxysilane occurred, the molecular chain of PEG was penetrated into the SiO 2 networks to form a semi-IPN structure. Due to the excellent biocompatibility and aqueous solubility of PEG molecules, as well as the bioactivity of the inorganic components, the biological and mechanical properties of this hybrid xerogel exhibit great potential for bone regeneration applications. The formation of hydroxyapatite was observed when the xerogel was immersed into simulated body fluid, demonstrating good bioactivity of the hybrid. The cell toxicity test also demonstrated that the hybrid material is suitable for the proliferation of MC3T3-E1 cells. Thus, the PEG/SiO 2 -CaO-P 2 O 5 hybrid xerogel has great potential to meet the demands of bone regeneration materials. - Highlights: ► PEG was penetrated into the SiO 2 networks to form a semi-IPN structure. ► This hybrid xerogel exhibit great potential for bone regeneration applications. ► SEM micrographs confirm the bioactivity of the samples.

Ultrasound-assisted sol-gel synthesis of ZrO2.

Science.gov (United States)

Guel, Marlene Lariza Andrade; Jiménez, Lourdes Díaz; Hernández, Dora Alicia Cortés

2017-03-01

Synthesis of tetragonal ZrO 2 by both conventional sol-gel and ultrasound-assisted sol-gel methods and using a non-ionic surfactant Tween-20, was performed. A porous microstructure composed of nanometric particles was observed. Tetragonal ZrO 2 was obtained using a low heat treatment temperature of powders, 500°C by both methods. A higher crystallinity and a shorter reaction time were observed when ultrasound was used in the sol-gel method due to the cavitation phenomenon. Copyright © 2016 Elsevier B.V. All rights reserved.

Recubrimientos meso-porosos de SiO2-TiO2-P2O5 para aplicaciones en pilas de combustible de intercambio protónico

Directory of Open Access Journals (Sweden)

Castro, Y.

2014-08-01

Full Text Available The article describes the preparation of mesoporous SiO2-TiO2-P2O5 coatings by Sol-Gel process combined to EISA method for using as proton exchange membranes fuel cells. Tetraethylorthosilicate (TEOS, methyl triethoxysilane (MTES, titanium tetrachloride (TiCl4 and phosphorus trichloride (PCl3 have used as precursors and cetyl trimethylammonium bromide (CTAB as porous generator agent. Films were deposited by immersion technique controlling the relative humidity at 40 and 20-70% and treated at 400 to 500° C for 15, 30, 45 and 60 min. The variation of the refractive index and thickness have studied as a function of temperature and sintering time as well as the pore volume and density of the coatings by spectroscopic ellipsometry. Moreover, the hydrophobic/hydrophilic character of the coatings has been studied by Transform Infrared Spectroscopy (FTIR and by contact angle measurements, following the loss of methyl groups with the temperature and sintering time. The results show that these parameters are crucial to obtain coatings with high porosity and low contact angle, important to obtain high proton conductivity conditions. The sintering conditions were fixed to 400°C / 60 min. Conductivity measurements at four points show high proton conductivity, 0,16 and 0,85 S/cm, up and down ramp, respectively, at 80°C and 80 % of humidity. These coatings are good candidates for PEMFC membranes, if they are deposited onto electrodes.El artículo describe la preparación de recubrimientos mesoporosos de SiO2-TiO2-P2O5 por el método sol-gel combinado con el método EISA para su aplicación como membranas en pilas de intercambio protónico. Se han utilizado como precursores el tetraetilortosilicato (TEOS, metil-trietoxi-silano (MTES, tetracloruro de titanio (TiCl4 y el tricloruro de fosforo (PCl3 y como agente generador de porosidad el bromuro de cetil trimetilamonio (CTAB. Los recubrimientos se depositaron mediante la técnica de inmersión controlando la

Erbium-doped borosilicate glasses containing various amounts of P2O5 and Al2O3: Influence of the silica content on the structure and thermal, physical, optical and luminescence properties

International Nuclear Information System (INIS)

Bourhis, Kevin; Massera, Jonathan; Petit, Laeticia; Koponen, Joona; Fargues, Alexandre; Cardinal, Thierry; Hupa, Leena; Hupa, Mikko; Dussauze, Marc; Rodriguez, Vincent; Ferraris, Monica

2015-01-01

Highlights: • Er 3+ doped borosilicate glasses were processed with different compositions and characterizations. • An increase in the SiO 2 content leads to a silicate-rich environment around the Er 3+ site. • An increase in the SiO 2 content decreases the Er 3+ absorption cross-section at 980 nm. • Glasses with 60 mol% of SiO 2 exhibit a stronger emission intensity at 1530 nm than glasses with x = 50. • Highest 1.5 μm emission intensity was achieved for the Al and P containing glass with 60 mol% of SiO 2 . - Abstract: The influence of the silica content on several properties of Er-doped borosilicate glasses in the presence of various amounts of P 2 O 5 and Al 2 O 3 has been investigated. The introduction of P 2 O 5 and/or Al 2 O 3 are responsible for structural modifications in the glass network through a charge-compensation mechanism related to the formation of negatively-charged PO 4 and AlO 4 groups or through the formation of AlPO 4 -like structural units. In this paper, we show that an increase in the SiO 2 content leads to a silicate-rich environment around the Er 3+ site, resulting in an increased dependence of the Er 3+ ions optical and luminescence properties on the P 2 O 5 and/or Al 2 O 3 concentration. The highest emission intensity at 1.5 μm was achieved for the glass with an equal proportion of P and Al in the glass system with 60 mol% of SiO 2

Influence of fluoride additions on biological and mechanical properties of Na2O-CaO-SiO2-P2O5 glass-ceramics.

Science.gov (United States)

Li, H C; Wang, D G; Hu, J H; Chen, C Z

2014-02-01

Two series of Na2O-CaO-SiO2-P2O5 glass-ceramics doped with NH4HF2 (G-NH4HF2) or CaF2 (G-CaF2) have been prepared by sol-gel method. The glass-ceramic phase composition and morphology were characterized by X-ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS). The mechanical properties and thermal expansion coefficient were measured by a microhardness tester, an electronic tensile machine and a thermal expansion coefficient tester. The structure difference between these two glass-ceramics was investigated by Fourier transform infrared spectroscopy (FTIR), and the in vitro bioactivity of the glass-ceramics was determined by in vitro simulated body fluid (SBF) immersion test. The hemolysis test, in vitro cytotoxicity test, systemic toxicity test and the implanted experiment in animals were used to evaluate the biocompatibility of the glass-ceramics. The mechanical properties of sample G-NH4HF2 are lower than that of sample G-CaF2, and the bioactivity of sample G-NH4HF2 is better than that of sample G-CaF2. The thermal expansion coefficients of these two glass-ceramics are all closer to that of Ti6Al4V. After 7 days of SBF immersion, apatites were induced on glass-ceramic surface, indicating that the glass-ceramics have bioactivity. The hemolysis test, in vitro cytotoxicity test and systemic toxicity test demonstrate that the glass-ceramics do not cause hemolysis reaction, and have no toxicity to cell and living animal. The implanted experiment in animals shows that bone tissue can form a good osseointegration with the implant after implantation for two months, indicating that the glass-ceramics are safe to serve as implants. Copyright © 2013 Elsevier B.V. All rights reserved.

SiO2-TiO2-P2O5 meso porous coatings for proton exchange membranes fuel cells

International Nuclear Information System (INIS)

Castro, Y.; Mosa, J.; Duran, A.

2014-01-01

The article describes the preparation of meso porous SiO 2 -TiO 2 -P 2 O 5 coatings by Sol-Gel process combined to EISA method for using as proton exchange membranes fuel cells. Tetraethyl orthosilicate (TEOS), methyl triethoxysilane (MTES), titanium tetrachloride (TiCl 4 ) and phosphorus trichloride (PCl 3 ) have used as precursors and cetyl trimethylammonium bromide (CTAB) as porous generator agent. Films were deposited by immersion technique controlling the relative humidity at 40 and 20-70% and treated at 400 to 500 degree centigrade for 15, 30, 45 and 60 min. The variation of the refractive index and thickness have studied as a function of temperature and sintering time as well as the pore volume and density of the coatings by spectroscopic ellipsometry. Moreover, the hydrophobic/hydrophilic character of the coatings has been studied by Transform Infrared Spectroscopy (FTIR) and by contact angle measurements, following the loss of methyl groups with the temperature and sintering time. The results show that these parameters are crucial to obtain coatings with high porosity and low contact angle, important to obtain high proton conductivity conditions. The sintering conditions were fixed to 400 degree centigrade/60 min. Conductivity measurements at four points show high proton conductivity, 0,16 and 0,85 S/cm, up and down ramp, respectively, at 80 degree centigrade and 80 % of humidity. These coatings are good candidates for PEMFC membranes, if they are deposited onto electrodes. (Author)

Sol-gel derived manganese-releasing bioactive glass as a therapeutical approach for bone tissue engineering

Energy Technology Data Exchange (ETDEWEB)

Barrioni, B.R.; Oliveira, A.C.; Leite, M.F.; Pereira, M.M. [Universidade Federal de Minas Gerais (UFMG), MG (Brazil)

2016-07-01

Full text: Bioactive glasses (BG) have been highlighted in tissue engineering, due to their high bioactivity and biocompatibility, being potential materials for bone tissue repair. Its composition is variable and quite flexible, allowing the incorporation of therapeutic metallic ions, which has been regarded as a promising approach in the development of BG with superior properties for tissue engineering. These ions can be released in a controlled manner during the dissolution process of the glass, having the advantage of being released at the exactly implant site where they are needed, thus optimizing the therapeutic efficacy and reducing undesired side effects in the patient. Among several ions that have been studied, Manganese (Mn) has been shown to favor osteogenic differentiation. Besides, this ion is also a cofactor for several enzymes involved in remodeling of extracellular matrix, presenting an important role in cell adhesion. Therefore, it is very important to study the Mn role in the BG network and its influence on the glass bioactivity. In this context, new bioactive glass compositions derived from the 58S (60%SiO2-36%CaO-4%P2O5, mol%) were synthesized in this work, using the sol-gel method, by the incorporation of Mn into their structure. FTIR and Raman spectra showed the presence of typical BG chemical groups, whereas the amorphous structure typical of these materials was confirmed by XRD analysis, which also indicated that the Mn incorporation in the glass network was well succeeded, as its precursor did not recrystallize. The role of Mn in the glass network was also evaluated by XPS. The influence of Mn on carbonated hydroxyapatite layer formation after different periods of immersion of the BG powder in Simulated Body Fluid was evaluated using zeta potential, SEM, EDS and FTIR, whereas the controlled ion release was measured through ICP-OES. MTT assay revealed that Mn-containing BG showed no cytotoxic effect on cell culture. All these results indicate

Sol-gel derived manganese-releasing bioactive glass as a therapeutical approach for bone tissue engineering

International Nuclear Information System (INIS)

Barrioni, B.R.; Oliveira, A.C.; Leite, M.F.; Pereira, M.M.

2016-01-01

Full text: Bioactive glasses (BG) have been highlighted in tissue engineering, due to their high bioactivity and biocompatibility, being potential materials for bone tissue repair. Its composition is variable and quite flexible, allowing the incorporation of therapeutic metallic ions, which has been regarded as a promising approach in the development of BG with superior properties for tissue engineering. These ions can be released in a controlled manner during the dissolution process of the glass, having the advantage of being released at the exactly implant site where they are needed, thus optimizing the therapeutic efficacy and reducing undesired side effects in the patient. Among several ions that have been studied, Manganese (Mn) has been shown to favor osteogenic differentiation. Besides, this ion is also a cofactor for several enzymes involved in remodeling of extracellular matrix, presenting an important role in cell adhesion. Therefore, it is very important to study the Mn role in the BG network and its influence on the glass bioactivity. In this context, new bioactive glass compositions derived from the 58S (60%SiO2-36%CaO-4%P2O5, mol%) were synthesized in this work, using the sol-gel method, by the incorporation of Mn into their structure. FTIR and Raman spectra showed the presence of typical BG chemical groups, whereas the amorphous structure typical of these materials was confirmed by XRD analysis, which also indicated that the Mn incorporation in the glass network was well succeeded, as its precursor did not recrystallize. The role of Mn in the glass network was also evaluated by XPS. The influence of Mn on carbonated hydroxyapatite layer formation after different periods of immersion of the BG powder in Simulated Body Fluid was evaluated using zeta potential, SEM, EDS and FTIR, whereas the controlled ion release was measured through ICP-OES. MTT assay revealed that Mn-containing BG showed no cytotoxic effect on cell culture. All these results indicate

Crystallization and chemical durability of glasses in the system Bi2O3-SiO2

International Nuclear Information System (INIS)

Fredericci, C.

2011-01-01

The crystallization of the Bi 2 O 3 -SiO 2 -TiO 2 -Al 2 O 3 -Na 2 O-K 2 O and Bi 2 O 3 -SiO 2 -ZnO-Al 2 O 3 -B 2 O 3 -Na 2 O glasses was studied using glass samples prepared by traditional melt-quench method. Differential thermal analysis (DTA) curves suggested that surface crystallization played a major role in the crystallization of the glass samples. X-ray diffraction (XRD) analysis revealed the crystallization of bismuth silicate for both glasses and bismuth silicate and zinc silicate for the glass containing ZnO. Through scanning electron microscopy (MEV) and energy dispersive spectroscopy (EDS), it was possible to observe that the crystals of zinc silicate (Zn 2 SiO 4 ) were readily attacked by hot 0,1 N sulfuric acid, whereas bismuth silicate crystals were more resistant to acidic attack etching. (author)

Flexural strength and translucent characteristics of lithium disilicate glass-ceramics with different P2O5 content

International Nuclear Information System (INIS)

Wang, Fu; Gao, Jing; Wang, Hui; Chen, Ji-hua

2010-01-01

Lithium disilicate glass-ceramics derived from the SiO 2 -Li 2 O-K 2 O-Al 2 O 3 -ZrO 2 -P 2 O 5 system with different P 2 O 5 content (from 0.5 mol.% to 2.0 mol.% at a step of 0.5 mol.%) were prepared for dental restorative application. Flexural strength of final glass-ceramics and translucent characteristics expressed in term of contrast ratio (CR) were measured. The interrelations between P 2 O 5 content, microstructure and properties were discussed. Glass-ceramic with a P 2 O 5 content of 1.0 mol.%, in which elongated rod-like Li 2 Si 2 O 5 crystals formed an interlocking microstructure, showed the highest flexural strength and suitable contrast ratio for dental restorative application.

Preparation and characterization of sol-gel derived (Th{sub x}Ce{sub 1-x})O{sub 2} microspheres

Energy Technology Data Exchange (ETDEWEB)

Cetinkaya, Berkan; Tel, Hueseyin [Ege Univ., Izmir (Turkey). Inst. of Nuclear Sciences

2018-04-01

(Th{sub x}Ce{sub 1-x})O{sub 2} microspheres (x = 0.50, 0.75 and 0.95) with high homogeneity were prepared via sol-gel technique, starting from the initial chemical materials Th(NO{sub 3}){sub 4} . 5H{sub 2}O and (NH{sub 4}){sub 2}[Ce(NO{sub 3}){sub 6}]. The sols were prepared by addition of ammonia under pH and temperature control. Sols were gelated to spherical form in a gelation system consisting of peristaltic pump, flow regulator, nozzle and a glass column. To obtain crack-free spheres suitable for gelation, source sols neutralization conditions, drop formation and pre-hardening medium were investigated and the optimum conditions were determined. After aging, washing and drying steps, gel microspheres were characterized. For this purpose, thermal behaviors of spheres were investigated with TG/DTA analysis. Dried microspheres at 80 C were calcined at three different temperatures, namely 450 C, 800 C and 1150 C, and crystal parameters were calculated from XRD data. BET specific surface area and BJH porosity analyses were also carried out.

Low-temperature sol-gel synthesis of NaZr2P3O12

International Nuclear Information System (INIS)

Agrawal, D.K.; Adair, J.H.

1990-01-01

The NZP family of new low-expansion materials has attracted wide interest for its potential in advanced technological applications. NaZr 2 P 3 O 12 , which is the parent composition of this family, has been synthesized by the solution sol-gel method using special precursor solutions, which led to its formation (although poorly crystalline) at temperatures as low as 120 degrees C. The lowest temperature of formation of a single phase of NaZr 2 P 3 O 12 with a high degree of crystallinity was found to be 600 degrees C

Structure-Dependent Spectroscopic Properties of Yb3+-Doped Phosphosilicate Glasses Modified by SiO2

Directory of Open Access Journals (Sweden)

Ling Wang

2017-02-01

Full Text Available Yb3+-doped phosphate glasses containing different amounts of SiO2 were successfully synthesized by the conventional melt-quenching method. The influence mechanism of SiO2 on the structural and spectroscopic properties was investigated systematically using the micro-Raman technique. It was worth noting that the glass with 26.7 mol % SiO2 possessed the longest fluorescence lifetime (1.51 ms, the highest gain coefficient (1.10 ms·pm2, the maximum Stark splitting manifold of 2F7/2 level (781 cm−1, and the largest scalar crystal-field NJ and Yb3+ asymmetry degree. Micro-Raman spectra revealed that introducing SiO2 promoted the formation of P=O linkages, but broke the P=O linkages when the SiO2 content was greater than 26.7 mol %. Based on the previous 29Si MAS NMR experimental results, these findings further demonstrated that the formation of [SiO6] may significantly affect the formation of P=O linkages, and thus influences the spectroscopic properties of the glass. These results indicate that phosphosilicate glasses may have potential applications as a Yb3+-doped gain medium for solid-state lasers and optical fiber amplifiers.

Structure-Dependent Spectroscopic Properties of Yb3+-Doped Phosphosilicate Glasses Modified by SiO2

Science.gov (United States)

Wang, Ling; Zeng, Huidan; Yang, Bin; Ye, Feng; Chen, Jianding; Chen, Guorong; Smith, Andew T.; Sun, Luyi

2017-01-01

Yb3+-doped phosphate glasses containing different amounts of SiO2 were successfully synthesized by the conventional melt-quenching method. The influence mechanism of SiO2 on the structural and spectroscopic properties was investigated systematically using the micro-Raman technique. It was worth noting that the glass with 26.7 mol % SiO2 possessed the longest fluorescence lifetime (1.51 ms), the highest gain coefficient (1.10 ms·pm2), the maximum Stark splitting manifold of 2F7/2 level (781 cm−1), and the largest scalar crystal-field NJ and Yb3+ asymmetry degree. Micro-Raman spectra revealed that introducing SiO2 promoted the formation of P=O linkages, but broke the P=O linkages when the SiO2 content was greater than 26.7 mol %. Based on the previous 29Si MAS NMR experimental results, these findings further demonstrated that the formation of [SiO6] may significantly affect the formation of P=O linkages, and thus influences the spectroscopic properties of the glass. These results indicate that phosphosilicate glasses may have potential applications as a Yb3+-doped gain medium for solid-state lasers and optical fiber amplifiers. PMID:28772601

Modeling the Onset of Phase Separation in CaO-SiO2-CaCl2 Chlorine-Containing Silicate Glasses.

Science.gov (United States)

Swansbury, Laura A; Mountjoy, Gavin; Chen, Xiaojing; Karpukhina, Natalia; Hill, Robert

2017-06-08

The addition of chlorine into a bioactive glass composition is expected to reduce its abrasiveness and increase its bioactivity, which is important for dental applications such as toothpastes. There is a lack of information and understanding regarding the structural role of chlorine in chlorine-containing bioactive silicate glasses. This has prompted classical core-shell model molecular dynamics simulations of (50 - x/2)CaO-(50 - x/2)SiO 2 -xCaCl 2 glasses to be performed, where x ranges from x = 0.0 to 43.1 mol % CaCl 2 . These ternary glasses are advantageous for a fundamental study because they do not have additional network formers (e.g., phosphorus pentoxide) or modifiers (e.g., sodium) typically found in bioactive glass compositions. The (50 - x/2)CaO-(50 - x/2)SiO 2 -xCaCl 2 glasses were seen to become phase-separated around the x = 16.1 mol % CaCl 2 composition, and chlorine predominantly coordinated with calcium. These findings provide a solid foundation for further computational modeling work on more complex chlorine-containing bioactive glass compositions.

Foldable and Cytocompatible Sol-gel TiO2 Photonics.

Science.gov (United States)

Li, Lan; Zhang, Ping; Wang, Wei-Ming; Lin, Hongtao; Zerdoum, Aidan B; Geiger, Sarah J; Liu, Yangchen; Xiao, Nicholas; Zou, Yi; Ogbuu, Okechukwu; Du, Qingyang; Jia, Xinqiao; Li, Jingjing; Hu, Juejun

2015-09-07

Integrated photonics provides a miniaturized and potentially implantable platform to manipulate and enhance the interactions between light and biological molecules or tissues in in-vitro and in-vivo settings, and is thus being increasingly adopted in a wide cross-section of biomedical applications ranging from disease diagnosis to optogenetic neuromodulation. However, the mechanical rigidity of substrates traditionally used for photonic integration is fundamentally incompatible with soft biological tissues. Cytotoxicity of materials and chemicals used in photonic device processing imposes another constraint towards these biophotonic applications. Here we present thin film TiO2 as a viable material for biocompatible and flexible integrated photonics. Amorphous TiO2 films were deposited using a low temperature (<250 °C) sol-gel process fully compatible with monolithic integration on plastic substrates. High-index-contrast flexible optical waveguides and resonators were fabricated using the sol-gel TiO2 material, and resonator quality factors up to 20,000 were measured. Following a multi-neutral-axis mechanical design, these devices exhibit remarkable mechanical flexibility, and can sustain repeated folding without compromising their optical performance. Finally, we validated the low cytotoxicity of the sol-gel TiO2 devices through in-vitro cell culture tests. These results demonstrate the potential of sol-gel TiO2 as a promising material platform for novel biophotonic devices.

Intensely emitting CdTe nanocrystals retained initial photoluminescence efficiency in sol-gel derived Si1-xZrxO2 glass

International Nuclear Information System (INIS)

Yang, P.; Murase, N.

2007-01-01

Emitting CdTe nanocrystals (NCs) were embedded in pure glass matrices (Si 1-x Zr x O 2 , x≤0.15) using a controlled sol-gel method, where the pre-hydrolyzed condition, the molar ratio of Zr/Si, the gelation time, the pH, and the amount of alcohol were judiciously optimized considering the surface condition of the NCs and the mechanism of the glass formation. As a result, the prepared glass phosphor exhibited high photoluminescence efficiencies (40% for green and 60% for red when Zr/Si was 5-10%) by retaining their initial values as in CdTe colloidal solution. To our knowledge, these values are the highest among those ever obtained for any solid matrices containing NCs. Because of the existence of Zr, the prepared glasses exhibit much better resistance against the ambient atmosphere, heat-treatment, and boiling water compared with pure silica glass (x=0) or the glass prepared from our other methods using a silane coupling agent. Thus, the obtained glass is promising for applications such as optical devices. (orig.)

De-chlorination and solidification of radioactive LiCl waste salt by using SiO_2-Al_2O_3-P_2O_5 (SAP) inorganic composite including B_2O_3 component

International Nuclear Information System (INIS)

Lee, Ki Rak; Park, Hwan-Seo; Cho, In-Hak; Choi, Jung-Hoon; Eun, Hee-Chul; Lee, Tae-Kyo; Han, Seung Youb; Ahn, Do-Hee

2017-01-01

SAP (SiO_2-Al_2O_3-P_2O_5) composite has been recently studied in KAERI to deal with the immobilization of radioactive salt waste, one of the most problematic wastes in the pyro-chemical process. Highly unstable salt waste was successfully converted into stable compounds by the dechlorination process with SAPs, and then a durable waste form with a high waste loading was produced when adding glassy materials to dechlorination product. In the present study, U-SAP composite which is SAP bearing glassy component (Boron) was synthesized to remove the adding and mixing steps of glassy materials for a monolithic wasteform. With U-SAPs prepared by a sol-gel process, a series of wasteforms were fabricated to identify a proper reaction condition. Physical and chemical properties of dechlorination products and U-SAP wasteforms were characterized by XRD, DSC, SEM, TGA and PCT-A. A U-SAP wasteform showed suitable properties as a radioactive wasteform such as dense surface morphology, high waste loading, and high durability at the optimized U-SAP/salt ratio 2.

Formation of SiO2/polytetrafluoroethylene hybrid superhydrophobic coating

International Nuclear Information System (INIS)

Zheng Yansheng; He Yi; Qing Yongquan; Zhuo Zhihao; Mo Qian

2012-01-01

Highlights: ► The coating showed the water contact angle of 165° and the water sliding angle of 6°. ► The hierarchical structure with the low surface energy leads to surface superhydrophobicity. ► We demonstrated a simple yet efficient approach to preparing superhydrophobic surface. - Abstract: Superhydrophobic coating has been fabricated on the glass substrates with modified SiO 2 sol and polytetrafluoroethylene emulsion through a sol–gel process. SiO 2 sol was modified with γ-glycidoxypropyl trimethoxysilane. The coatings were characterized by water contact angle measurement, Scanning electron microscope, Fourier transform infrared spectrometry, X-ray photoelectron spectroscopy and thermal synthetic analysis. The experimental results show that coatings exhibited superhydrophobic and heat-resistant property with a water average contact angle of 156° and sliding angle of 6°, coating has a rough surface with both micro- and nanoscale structures, γ-glycidoxypropyl trimethoxysilane enhanced the hydrophobicity of the coatings. Low surface energy of polymer and special structure of the coatings were responsible for the hydrophobic of the surfaces.

Crystallization behavior of (1 - x)Li2O.xNa2O.Al2O3.4SiO2 glasses

International Nuclear Information System (INIS)

Wang, Moo-Chin; Cheng, Chih-Wei; Chang, Kuo-Ming; Hsi, Chi-Shiung

2010-01-01

The crystallization behavior of the (1 - x)Li 2 O.xNa 2 O.Al 2 O 3 .4SiO 2 glasses has been investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED) and energy dispersive spectroscopy (EDS). The crystalline phase was composed of β-spodumene. The isothermal crystallization kinetics of β-spodumene from the (1 - x)Li 2 O.xNa 2 O.Al 2 O 3 .4SiO 2 glasses has also been studied by a quantitative X-ray diffraction method. The activation energy of β-spodumene formation decreases from 359.2 to 317.8 kJ/mol when the Na 2 O content increases from 0 to 0.4 mol and it increases from 317.8 to 376.9 kJ/mol when the Na 2 O content increases from 0.4 to 0.6 mol. The surface nucleation and plate-like growth were dominant in the crystallization of the (1 - x)Li 2 O.xNa 2 O.Al 2 O 3 .4SiO 2 glasses.

Structural evolution of the SiO2-Ag system prepared by the Sol-gel process with incorporation of Ag particles

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Garcia-Gonzalez, L.

2011-02-01

Full Text Available Structural evolution of Sol-Gel glasses in powder form and coatings with incorporation of Ag particles at the starting solution showed an evolution from SiO2 amorphous matrix to the cristobalite phase with the annealing treatment at around 800 ºC for one hour. This structural evolution was obtained at lower Ag concentration up 0.7 %vol. Two series of samples were studied, A series using HNO3 and B series using HCl as catalytic agent; in both series grenetine was used as a dispersing agent to avoid the precipitation of Ag particles. We found the incorporation of silver in the xerogeles matrix promotes the devitrification process at relatively low temperatures with the presence of partial crystallization in form of cistobalite. This structure was produced by controlling the catalytic agent quoted in the preparation process. The EPR and UV-Vis absorption spectra show the presence of Fe3+ ions as a contaminant in the source of the Ag particles, due to the process to obtain these particles. By means the IR spectra a high (OH- concentration at higher temperatures was observed in this system, until 600 ºC at difference of the sol-gel glasses made with incorporation of Ag particles by nitrates. The color evolution of the coating samples with the annealing temperature varies from a light brown at 100 ºC to yellow at 500 ºC.La evolución estructural de vidrios de Sol-Gel en forma de polvos y recubrimientos preparados con la incorporación de partículas de Ag a partir de la solución precursora muestra la evolución de la matriz amorfa de SiO2 a la fase cristobalita utilizando tratamientos térmicos alrededor de 800 °C por un tiempo de una hora. Dicha evolución estructural fue obtenida en concentraciones bajas a partir de 0.7% de Ag. Dos series de muestras fueron estudiadas, la serie A usando HNO3 y la serie B usando HCl como agente catalítico; en ambas series se uso grenetina como agente dispersante para evitar la precipitación de las part

Synthesis of hybrid cellulose nanocomposite bonded with dopamine SiO2/TiO2 and its antimicrobial activity

Science.gov (United States)

Ramesh, Sivalingam; Kim, Gwang-Hoon; Kim, Jaehwan; Kim, Joo-Hyung

2015-04-01

Organic-inorganic hybrid material based cellulose was synthesized by the sol-gel approach. The explosion of activity in this area in the past decade has made tremendous progress in industry or academic both fundamental understanding of sol-gel process and applications of new functionalized hybrid materials. In this present research work, we focused on cellulose-dopamine functionalized SiO2/TiO2 hybrid nanocomposite by sol-gel process. The cellulose-dopamine hybrid nanocomposite was synthesized via γ-aminopropyltriethoxysilane (γ-APTES) coupling agent by in-situ sol-gel process. The chemical structure of cellulose-amine functionalized dopamine bonding to cellulose structure with covalent cross linking hybrids was confirmed by FTIR spectral analysis. The morphological analysis of cellulose-dopamine nanoSiO2/TiO2 hybrid nanocomposite materials was characterized by XRD, SEM and TEM. From this different analysis results indicate that the optical transparency, thermal stability, control morphology of cellulose-dopamine-SiO2/TiO2 hybrid nanocomposite. Furthermore cellulose-dopamine-SiO2/TiO2 hybrid nanocomposite was tested against pathogenic bacteria for antimicrobial activity.

Processing and optical properties of Nd3+-doped SiO2-TiO2-Al2O3 planar waveguides

Science.gov (United States)

Xiang, Qing; Zhou, Yan; Ooi, Boon Siew; Lam, Yee Loy; Chan, Yuen Chuen; Kam, Chan Hin

2000-05-01

We report here the processing and optical characterization of Nd3+-doped SiO2-TiO2-Al2O3 planar waveguides deposited on SOS substrates by the sol-gel route combined with spin-coating and rapid thermal annealing. The recipes used for preparing the solutions by sol-gel route are in mole ratio of 93SiO2:20AlO1.5: x ErO1.5. In order to verify the residual OH content in the films, FTIR spectra were measured and the morphology of the material by the XRD analysis. Five 2-layer films annealed at a maximum temperature of 500 degrees C, 700 degrees C, 900 degrees, 1000 degrees C, 1100 degrees C respectively were fabricated on silicon. The FTIR and XRD curves show that annealing at 1050 degrees C for 15s effectively removes the OH in the materia and keeps the material amorphous. The propagation loss of the planar waveguides was measured by using the method based on scattering in measurements and the result was obtained to be 1.54dB/cm. The fluorescence spectra were measured with 514nm wavelength of Ar+ laser by directly shining the pump beam on the film instead of prism coupling. The results show that the 1 mole Nd3+ content recipe has the strongest emission efficiency among the four samples investigated.

Effect of heat treatment on the properties of SiO2-CaO-MgO-P 2O 5 bioactive glasses.

Science.gov (United States)

Zhou, Yue; Li, Hongying; Lin, Kaili; Zhai, Wanying; Gu, Weiming; Chang, Jiang

2012-09-01

Since the invention of 45S5 Bioglass, researchers never stopped exploring new generation bioactive glass (BG) materials for wider applications in regenerative medicine, among which a novel SiO(2)-CaO-MgO-P(2)O(5) bioactive glass (BG20) is an excellent candidate. However, apart from their biocompatibility and bioactivity, a porous structure is also a must for a tissue engineering scaffold in successfully fixing bone defect. The porosity is the outcome of the high temperature (500-1,000 °C) treatment in the fabricating process of the bioglass scaffold. Under the high temperature, the amorphous glass material will become crystallized at certain percentage in the glass matrix, and possibly leading to consequent changes in the mechanical strength, biodegradability and bioactivity. To elucidate the effect of phase transition on the change of the properties of BG20, the experiments in this report were designed to fine-tuning the heat treating temperatures to fabricate a series of BG20 powders with different crystallization structures. X-ray diffraction revealed a positive correlation between the heating temperature and the crystallization, as well as the compressive strength of the materials. In vitro degradation and ion analysis by ICP-AES demonstrated a similar releasing behavior of different ions including Mg(2+), Ca(2+) and Si(4+), which in common is the tendency of decreasing of the ion concentration along with the increasing of the treating temperature. Cell proliferation assay using both mouse fibroblasts (NIH3T3) and bone marrow stromal cells (BMSCs) showed little toxicity of the ionic extract of the BG20 powders at all the treating temperatures, while fibroblasts demonstrated a significant promoting in the percentage of proliferation. Furthermore, reverse-transcription and polymerase chain reaction analysis on two representative marker genes for early osteogenesis and endochondral ossification, respectively, type I collagen alpha 1 and Indian Hedge-hog, showed

Eu-doped ZnO-HfO2 hybrid nanocrystal-embedded low-loss glass-ceramic waveguides

Science.gov (United States)

Ghosh, Subhabrata; N, Shivakiran Bhaktha B.

2016-03-01

We report on the sol-gel fabrication, using a dip-coating technique, of low-loss Eu-doped 70SiO2 -(30-x) HfO2-xZnO (x = 2, 5, 7 and 10 mol%) ternary glass-ceramic planar waveguides. Transmission electron microscopy and grazing incident x-ray diffraction experiments confirm the controlled growth of hybrid nanocrystals with an average size of 3 nm-25 nm, composed of ZnO encapsulated by a thin layer of nanocrystalline HfO2, with an increase of ZnO concentration from x = 2 mol% to 10 mol% in the SiO2-HfO2 composite matrix. The effect of crystallization on the local environment of Eu ions, doped in the ZnO-HfO2 hybrid nanocrystal-embedded glass-ceramic matrix, is studied using photoluminescence spectra, wherein an intense mixed-valence state (divalent as well as trivalent) emission of Eu ions is observed. The existence of Eu2+ and Eu3+ in the SiO2-HfO2-ZnO ternary matrix is confirmed by x-ray photoelectron spectroscopy. Importantly, the Eu{}2+,3+-doped ternary waveguides exhibit low propagation losses (0.3 ± 0.2 dB cm-1 at 632.8 nm) and optical transparency in the visible region of the electromagnetic spectrum, which makes ZnO-HfO2 nanocrystal-embedded SiO2-HfO2-ZnO waveguides a viable candidate for the development of on-chip, active, integrated optical devices.

Effect of pH values on surface modification and solubility of phosphate bioglass-ceramics in the CaO-P 2O 5-Na 2O-SrO-ZnO system

Science.gov (United States)

Li, Xudong; Cai, Shu; Zhang, Wenjuang; Xu, Guohua; Zhou, Wei

2009-08-01

The bioactive glass-ceramics in the CaO-P 2O 5-Na 2O-SrO-ZnO system were synthesized by the sol-gel technique, and then chemically treated at different pH values to study the solubility and surface modification. Samples sintered at 650 °C for 4 h consisted of the crystalline phase β-Ca 2P 2O 7 and the glass matrix. After soaking in the solution at pH 1.0, the residual glass matrix on the surface appeared entirely dissolved and no new phase could be detected. Whereas at pH 3.0, web-like layer exhibiting peaks corresponding to CaP 2O 6 was formed and covered the entire surface of the sample. When conducted at pH 10.0, only part of the glass matrix was dissolved and a new phase Ca 4P 6O 19 was precipitated, forming the petaline layer. The chemical treatment can easily change the surface morphologies and phase composition of this bioactive glass-ceramics. The higher level of surface roughness resulting from the new-formed layer would improve the interface bonding and benefit for cell adhesion.

Sol-gel process for preparation of YBa2Cu4O8 from acidic acetates/ammonia/ascorbic acid systems

International Nuclear Information System (INIS)

Deptula, A.; Lada, W.; Olczak, T.; Goretta, K.C.

1997-01-01

YBa 2 Cu 4 O x sols were prepared by addition of ammonia to acidic acetate solutions of Y 3+ , Ba 2+ , and Cu 2+ . Ascorbic acid was added to part of the sol. The resultant sols were gelled to a shard or a coating by evaporation at 60 C. Addition of ethanol to the sols facilitated formation of gel coatings, fabricated by a dipping technique, on Ag or glass or substrates. At 100 C, gels formed in the presence of ascorbic acid were perfectly amorphous, in contrast to crystalline acetate gels. The quality of coatings prepared from ascorbate gels was superior to that of acetate gel coatings

Preparation and encapsulation performance of Al_2O_3-SiO_2-B_2O_3 glass-ceramic for high temperature thermal storage

International Nuclear Information System (INIS)

Li, Ruguang; Zhu, Jiaoqun; Zhou, Weibing; Cheng, Xiaomin; Liu, Fengli

2017-01-01

Highlights: • Al_2O_3-B_2O_3-SiO_2 has good chemical durability, corrosion resistance and dense structure. • The material rarely used in high temperature thermal storage. • The material was prepared and characterized in the paper. - Abstract: In this paper, Al_2O_3-SiO_2-B_2O_3 glass-ceramic was prepared and characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), further, the porosity was detected by Archimedes principle, thermo physical properties were investigated by differential scanning calorimeter (DSC), respectively. The phase composition was detected by XRD, and the morphology was observed by SEM. The results indicated that the thermal conductivities of the Al_2O_3-SiO_2-B_2O_3 glass-ceramic were between 1.3 and 1.5 W·(m·K)"−"1, and the material had good thermal stability in the range of 300–900 °C. The porosity and apparent density were increased with the temperature. The porosity of Al_2O_3-SiO_2-B_2O_3 glass-ceramic in ranging from 1.2 to 9.6%, the apparent density were between 2.12 and 2.67 g·cm"−"3, and heat capacities were between 0.64 and 0.79 kJ/(kg·K). All the results indicated that the Al_2O_3-SiO_2-B_2O_3 glass-ceramic can be applied as encapsulation material in high temperature latent thermal energy storage.

Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

Science.gov (United States)

Sibille, L.; Gavira-Gallardo, J. A.; Hourlier-Bahloul, D.

2003-01-01

Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SiO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2,7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil simular in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. The elemental composition and structure of the precursor molecules were characterized. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors.

Enhanced Photocatalytic Activity of ZrO2-SiO2 Nanoparticles by Platinum Doping

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Mohammad W. Kadi

2013-01-01

Full Text Available ZrO2-SiO2 mixed oxides were prepared via the sol-gel method. Photo-assisted deposition was utilized for doping the prepared mixed oxide with 0.1, 0.2, 0.3, and 0.4 wt% of Pt. XRD spectra showed that doping did not result in the incorporation of Pt within the crystal structure of the material. UV-reflectance spectrometry showed that the band gap of ZrO2-SiO2 decreased from 3.04 eV to 2.48 eV with 0.4 wt% Pt doping. The results show a specific surface area increase of 20%. Enhanced photocatalysis of Pt/ZrO2-SiO2 was successfully tested on photo degradation of cyanide under illumination of visible light. 100% conversion was achieved within 20 min with 0.3 wt% of Pt doped ZrO2-SiO2.

Sol-gel derived porous bioactive nanocomposites: Synthesis and in vitro bioactivity

Science.gov (United States)

Shankhwar, Nisha; Kothiyal, G. P.; Srinivasan, A.

2013-06-01

Porous bioactive composites consisting of SiO2-CaO-Na2O-P2O5 bioactive glass-ceramic and synthetic water soluble polymer Polyvinylpyrrolidone [PVP (C6H9NO)n, MW˜40000 g/mol] have been synthesized by sol-gel route. As-prepared polymeric composites were characterized by X-ray diffraction (XRD) technique. Two major bone mineral phases, viz., hydroxyapatite [Ca10(PO4)6(OH)2] and wollastonite [calcium silicate (CaSiO3)] have been identified in the XRD patterns of the composites. Presence of these bone minerals indicates the bioactive nature of the composites. In vitro bioactivity tests confirm bioactivity in the porous composites. The flexibility offered by these bioactive polymer composites is advantageous for its application as implant material.

Femtosecond double proton transfer dynamics in [2,2'-bipyridyl]-3,3'-diol in sol-gel glasses

NARCIS (Netherlands)

Prosposito, P.; Marks, D.R.A.; Zhang, H.; Glasbeek, M.

1998-01-01

Abstract: Intramolecular excited state double proton-transfer dynamics has been studied for [2,2'-bipyridyl]-3,3'-diol (BP(OH)2) in sol-gel glass. By means of the femtosecond fluorescence up-conversion technique, the spectral dependence of the fluorescence transients obtained for BP(OH)2 in a few

Low Loss Sol-Gel TiO2 Thin Films for Waveguiding Applications

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Alexis Fischer

2013-03-01

Full Text Available TiO2 thin films were synthesized by sol-gel process: titanium tetraisopropoxide (TTIP was dissolved in isopropanol, and then hydrolyzed by adding a water/isopropanol mixture with a controlled hydrolysis ratio. The as prepared sol was deposited by “dip-coating” on a glass substrate with a controlled withdrawal speed. The obtained films were annealed at 350 and 500 °C (2 h. The morphological properties of the prepared films were analyzed by Scanning Electron Microscopy (SEM and Atomic Force Microscopy (AFM. The optical waveguiding properties of TiO2 films were investigated for both annealing temperature using m-lines spectroscopy. The refractive indices and the film thickness were determined from the measured effective indices. The results show that the synthesized planar waveguides are multimodes and demonstrate low propagation losses of 0.5 and 0.8 dB/cm for annealing temperature 350 and 500 °C, respectively.

Crystallization and characterization of Y2O3-SiO2 glasses

Science.gov (United States)

Drummond, Charles H., III; Lee, William E.; Sanders, W. A.; Kiser, J. D.

1991-01-01

Glasses in the yttria-silica system with 20 to 40 mol pct Y2O3 were subjected to recrystallization studies after melting at 1900 to 2100 C in W crucibles in 1 and 50 atm N2. The TEM and XRD results obtained indicate the presence of the delta, gamma, gamma prime, and beta-Y2Si2O7 crystalline phases, depending on melting and quenching conditions. Heat treatment in air at 1100 to 1600 C increased the amount of crystallization, and led to the formation of Y2SiO5, cristabalite, and polymorphs of Y2Si2O7. Also investigated were the effects of 5 and 10 wt pct zirconia additions.

Li+ ions diffusion into sol-gel V2O5 thin films: electrochromic properties

Science.gov (United States)

Benmoussa, M.; Outzourhit, A.; Bennouna, A.; Ihlal, A.

2009-10-01

V{2}O{5} thin films were prepared by the sol-gel spin coating process. The Li+ ions insertion effect on optical and electrochromic properties of those films was studied. The diffusion coefficient was calculated using both cyclic voltammograms and chronoamperometric curves. The amount x of Li+ ions in LixV{2}O{5} was also calculated. Finally, the electrochromic performance evolution characteristics such as the reversibility, coloration efficiency, coloration memory stability and response time were studied.

Luminescence and energy transfer of Tb3+-doped BaO-Gd2O3-Al2O3-B2O3-SiO2 glasses.

Science.gov (United States)

Zuo, Chenggang; Huang, Jinze; Liu, Shaoyou; Xiao, Anguo; Shen, Youming; Zhang, Xiangyang; Zhou, Zhihua; Zhu, Ligang

2017-12-05

Transparent Tb 3+ -doped BaO-Gd 2 O 3 -Al 2 O 3 -B 2 O 3 -SiO 2 glasses with the greater than 4g/cm 3 were prepared by high temperature melting method and its luminescent properties have been investigated by measured UV-vis transmission, excitation, emission and luminescence decay spectra. The transmission spectrum shows there are three weak absorption bands locate at about 312, 378 and 484nm in the glasses and it has good transmittance in the visible spectrum region. Intense green emission can be observed under UV excitation. The effective energy transfer from Gd 3+ ion to Tb 3+ ion could occur and sensitize the luminescence of Tb 3+ ion. The green emission intensity of Tb 3+ ion could change with the increasing SiO 2 /B 2 O 3 ratio in the borosilicate glass matrix. With the increasing concentration of Tb 3+ ion, 5 D 4 → 7 F J transitions could be enhanced through the cross relaxation between the two nearby Tb 3+ ions. Luminescence decay time of 2.12ms from 546nm emission is obtained. The results indicate that Tb 3+ -doped BaO-Gd 2 O 3 -Al 2 O 3 -B 2 O 3 -SiO 2 glasses would be potential scintillating material for applications in X-ray imaging. Copyright © 2017 Elsevier B.V. All rights reserved.

Radiation hardening in sol-gel derived Er3+-doped silica glasses

International Nuclear Information System (INIS)

Hari Babu, B.; León Pichel, Mónica; Ollier, Nadège; El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed; Poumellec, Bertrand; Lancry, Matthieu; Ibarra, Angel

2015-01-01

The aim of the present paper is to report the effect of radiation on the Er 3+ -doped sol-gel silica glasses. A possible application of these sol-gel glasses could be their use in harsh radiation environments. The sol-gel glasses are fabricated by densification of erbium salt-soaked nanoporous silica xerogels through polymeric sol-gel technique. The radiation-induced attenuation of Er 3+ -doped sol-gel silica is found to increase with erbium content. Electron paramagnetic resonance studies reveal the presence of E′ δ point defects. This happens in the sol-gel aluminum-silica glass after an exposure to γ-rays (kGy) and in sol-gel silica glass after an exposure to electrons (MGy). The concentration levels of these point defects are much lower in γ-ray irradiated sol-gel silica glasses. When the samples are co-doped with Al, the exposure to γ-ray radiation causes a possible reduction of the erbium valence from Er 3+ to Er 2+ ions. This process occurs in association with the formation of aluminum oxygen hole centers and different intrinsic point defects

Effect of SiO2 addition and gamma irradiation on the lithium borate glasses

Science.gov (United States)

Raut, A. P.; Deshpande, V. K.

2018-01-01

The physical properties like density, glass transition temperature (Tg), and ionic conductivity of lithium borate (LB) glasses with SiO2 addition were measured before and after gamma irradiation. Remarkable changes in properties have been obtained in the physical properties of LB glasses with SiO2 addition and after gamma irradiation. The increase in density and glass transition temperature of LB glasses with SiO2 addition has been explained with the help of increase in density of cross linking due to SiO4 tetrahedra formation. The increase in ionic conductivity with SiO2 addition was explained with the help of ‘mixed glass former effect’. The increase in density and Tg of LB glasses with SiO2 addition after gamma irradiation has been attributed to fragmentation of bigger ring structure into smaller rings, which increases the density of cross linking and hence compaction. The exposure of gamma irradiation has lead to decrease in ionic conductivity of LB glasses with SiO2 addition. The atomic displacement caused by gamma irradiation resulted in filling of interstices and decrease in trapping sites. This explains the obtained decrease in ionic conductivity after gamma irradiation of glasses. The obtained results of effect of SiO2 addition and gamma irradiation on the density, Tg and ionic conductivity has been supported by FTIR results.

Investigating the Effect of Glass Ion Release on the Cytocompatibility, Antibacterial Eflcacy and Antioxidant Activity of Y2O3 / CeO2 doped SiO2-SrO-Na2O glasses

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Placek L. M.

2018-02-01

Full Text Available The effect on ion release and cytocompatibility of Yttrium (Y and Cerium (Ce are investigated when substituted for Sodium (Na in a 0.52SiO2-0.24SrO-0.24-Na2OMOglass series (where MO= Y2O3 or CeO2. Glass leaching was evaluated through pH measurements and Inductive Coupled Plasma-Optical Emission Spectrometry (ICP-OES analysiswhere the extract pH increased during incubation (11.2 - 12.5. Ion release of Silicon (Si, Na and Strontium (Sr from the Con glass was at higher than that of glasses containing Y or Ce, and reached a limit after 1 day. Ion release from Y and Ce containing glasses reached a maximum of 1800 μg/mL, 1800 μg/mL, and 10 μg/mL for Si, Na, and Sr, respectively. Release of Y and Cewas below the ICP- OES detection limit 75% of bacteria at a 9% extract concentration. Antioxidant capacity (mechanism for neuroprotection was evaluated using the ABTS assay. All glasses had inherent radical oxygen species (ROS scavenging capability with Con reaching 9.5 mMTE.

Synthesis and characterization of erbium-doped SiO{sub 2}-TiO{sub 2} thin films prepared by sol-gel and dip-coating techniques onto commercial glass substrates as a route for obtaining active GRadient-INdex materials

Energy Technology Data Exchange (ETDEWEB)

Gómez-Varela, Ana I. [Microoptics and GRIN Optics Group, Department of Applied Physics, Faculty of Optics and Optometry and Faculty of Physics, Universidade de Santiago de Compostela, Campus Vida s/n, Santiago de Compostela E-15782 (Spain); Castro, Yolanda, E-mail: castro@icv.csic.es [Instituto de Cerámica y Vidrio (CSIC), Kelsen 5, Campus de Cantoblanco, Madrid 28049 (Spain); Durán, Alicia [Instituto de Cerámica y Vidrio (CSIC), Kelsen 5, Campus de Cantoblanco, Madrid 28049 (Spain); De Beule, Pieter A.A. [Applied Nano-Optics Laboratory, International Iberian Nanotechnology Laboratory, Braga 4715-330 (Portugal); Flores-Arias, María T. [Microoptics and GRIN Optics Group, Department of Applied Physics, Faculty of Optics and Optometry and Faculty of Physics, Universidade de Santiago de Compostela, Campus Vida s/n, Santiago de Compostela E-15782 (Spain); Bao-Varela, Carmen, E-mail: carmen.bao@usc.es [Microoptics and GRIN Optics Group, Department of Applied Physics, Faculty of Optics and Optometry and Faculty of Physics, Universidade de Santiago de Compostela, Campus Vida s/n, Santiago de Compostela E-15782 (Spain)

2015-05-29

In this work, SiO{sub 2}-TiO{sub 2} films doped with erbium were prepared by dip-coating sol-gel process onto commercial glass substrates. The surface morphology of the films was characterized using atomic force microscopy, while thickness, refractive index, extinction coefficient and porosity of the films were determined by ellipsometric measurements in a wavelength region of 400-1000 nm. Optical constants and porosity were found to vary with erbium concentration. The proof of principle presented in this paper is applicable to systems of different nature by tailoring the sol-gel precursors in such a way that active GRadient-INdex media described by a complex, parabolic-like refractive index distribution for beam shaping purposes is obtained. - Highlights: • Sol-gel route for preparation of active GRadient-INdex materials is proposed. • SiO{sub 2}-TiO{sub 2} films doped with erbium were prepared by dipping onto commercial glasses. • Morphological and optical characterization of the samples was performed. • Optical constants and porosity were found to vary with erbium concentration. • Refractive index diminishes with dopant content; the contrary occurs for porosity.

[Influence of La2O3 and Li2O on glass powder for infiltrating ZTA all-ceramic dental material formed by gel-casting].

Science.gov (United States)

Jin, Qiong; Wang, Xiao-fei; Yang, Zheng-yu; Tong, Yi-ping; Zhu, Li; Ma, Jian-feng

2012-10-01

The influence of La2O3 and Li2O on glass powder was studied in this paper, which is to infiltrate ZTA all-ceramic dental material formed by gel-casting. The performance of different component was analyzed to optimize glass formula. Six groups of glass powder were designed and prepared by conventional melt-quenching method. ZTA ceramic blocks were covered with glass paste, which were formed by gel-casting and sintered in 1200 degrees centigrade, then infiltrated in 1150 degrees centigrade for twice to make glass/ZTA ceramic composites. By detecting differential thermal analysis and melting range of infiltration glass power, as well as flexural strength, linear shrinkage, SEM and EDS of glass/ZTA ceramic composites, the optimized glass group was determined out. Statistical analysis was performed using SPSS 13.0 software package by means of paired t test or one way ANOVA. The bending strength of group Li1 was (291.2±27.9) MPa, significantly higher than group Li2 and group La2(Pglass of group Li1 can lubricate ZTA ceramics well, their structure was compact and had a few small pores. Intergranular fracture existed on cross surface as well as transgranular fracture. The results showed that Li1(30%La2O3-15%Al2O3-15%SiO2-15%B2O3-5%Li2O) glass infiltrated ZTA ceramic composite had the best capability. Glass/ZTA composite material can be prepared by gel-casting and infiltrating way, and this process is simple and economically suitable for general dental laboratory.

Sol-gel synthesis and characterization of lithiummolybdosilicate glass

International Nuclear Information System (INIS)

Prakash, I.; Nallamuthu, N.; Muralidharan, P.; Satyanarayana, N.; Venkateswarlu, M.; Balasubramanyam, S.

2008-01-01

10 % Li 2 O + 0.9 % MoO 3 + 89.1 %SiO 2 (LMS) glassy sample was prepared using Sol-gel process and was characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Differential scanning calorimetry (DSC) techniques. The ion conducting mechanism was studied through impedance technique at various temperatures. The conductivity of the sample was found to be 4.1257 x 10 -8 Scm -1 at 613 K. The activation energy was calculated from the log (sT) vs. 1000/T plot and it was found to be (0.1466 ± 0.012) eV. (author)

Synthesis of Titania-Silica Materials by Sol-Gel

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Rubia F. S. Lenza

2002-10-01

Full Text Available In this work TiO2-SiO2 glasses containing as much as 20 mol % of TiO2 were prepared via sol-gel process using titanium and silicon alkoxides, in the presence of chlorine, in the form of titanium tetrachloride or HCl. The gels were heat-treated until 800 °C. X-ray diffraction and Fourier transform infrared spectroscopy were used to understand the structural properties of TiO2-SiO2 oxides calcined at different temperatures and to evaluate the homogeneity of these materials. The degree of the compactness of the silica network is inferred from the frequency of the asymmetric stretching vibrations of Si-O-Si bonds. Formation of Si-O-Ti bridges, as monitored by the intensity of characteristic 945 cm-1 ¾ 960 cm-1 vibration, is particularly prominent if the method of basic two-step prehydrolysis of silicon alkoxide, addition of titanium alkoxide and completion of hydrolysis was used.

Estimation of silver nanoparticles size in SiO2 sol-gel layers by use of UV-VIS spectroscopy

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Marek Novotný

2011-12-01

Full Text Available Silica glass layers containing silver nanoparticles were prepared by the sol-gel method. The layers were deposited on a glass substrate by the dip-coating method, dried and heat treated at various temperatures. The average silver particle size was determined from absorption spectra according to Mie’s theory. A good correlation was found between the calculated values and analysis of HRTEM images. A very narrow size distribution was obtained by this procedure. The average particle size of silver particles fell between 1 and 2 nm for dried samples; in case of glasses treated at 500 and 550°C the size ranged between 2 and 4 nm.

Structure and crystallization of SiO2 and B2O3 doped lithium disilicate glasses from theory and experiment.

Science.gov (United States)

Erlebach, Andreas; Thieme, Katrin; Sierka, Marek; Rüssel, Christian

2017-09-27

Solid solutions of SiO 2 and B 2 O 3 in Li 2 O·2SiO 2 are synthesized and characterized for the first time. Their structure and crystallization mechanisms are investigated employing a combination of simulations at the density functional theory level and experiments on the crystallization of SiO 2 and B 2 O 3 doped lithium disilicate glasses. The remarkable agreement of calculated and experimentally determined cell parameters reveals the preferential, kinetically controlled incorporation of [SiO 4 ] and [BO 4 ] at the Li + lattice sites of the Li 2 O·2SiO 2 crystal structure. While the addition of SiO 2 increases the glass viscosity resulting in lower crystal growth velocities, glasses containing B 2 O 3 show a reduction of both viscosities and crystal growth velocities. These observations could be rationalized by a change of the chemical composition of the glass matrix surrounding the precipitated crystal phase during the course of crystallization, which leads to a deceleration of the attachment of building units required for further crystal growth at the liquid-crystal interface.

Adsorption of uranyl in SiO2 porous glass

International Nuclear Information System (INIS)

Benedetto, F. E.; Prado, M. O.

2013-01-01

Vitreous SiO 2 porous matrices can be used in many applications involving the uptake of chemical species on its solid surface. In this work, vitreous silica sponges were prepared from a sodium borosilicate glass manufactured in our laboratory. The product obtained was then separated into phases with subsequent leaching of the soluble phase rich in B and Na. The resulting porous matrices have a specific surface of 35 m2/gr. Adsorption of uranyl ions onto the SiO 2 porous surface was studied to evaluate the use of this material as a filter for treatment of uranium containing water. The effects of contact time, adsorbent mass and equilibrium concentration of solution were studied. The porous adsorbent exhibits a pseudo-second-order kinetic behavior. The sponges with adsorbed uranium were thermally sealed as a way of U immobilization. Retention of uranium was confirmed during the matrix sealing by TGA. Uranium concentration before and after adsorption tests were made by means of ICP-OES. For uranium concentration of 800 ppm, 72 hours contact time and pH of 3.5, the amount of uranium adsorbed was 21.06 ± 0.02 mg U per gram of vitreous porous SiO 2 . (author)

TiO2/SiO2 prepared via facile sol-gel method as an ideal support for green synthesis of Ag nanoparticles using Oenothera biennis extract and their excellent catalytic performance in the reduction of 4-nitrophenol

Directory of Open Access Journals (Sweden)

Bahar Khodadadi

2017-01-01

Full Text Available In the present study, the extract of the plant of Oenothera biennis was used to green synthesis of silver nanoparticles (Ag NPs as an environmentally friendly, simple and low cost method. And Additionally, TiO2/SiO2 was prepared via facile sol-gel method using starch as an important, naturally abundant organic polymer as an ideal support. The Ag NPs/TiO2/SiO2 as an effective catalyst was prepared through reduction of Ag+ ions using Oenothera biennis extract as the reducing and stabilizing agent and Ag NPs immobilization on TiO2/SiO2 surface in the absence of any stabilizer or surfactant. Several techniques such as FT-IR spectroscopy, UV-Vis spectroscopy, X-ray Diffraction (XRD, sScanning eElectron mMicroscopy (FE-SEM, Eenergy dDispersive X-ray sSpectroscopy (EDS, and Ttransmission Eelectron Mmicroscopy (TEM were used to characterize TiO2/SiO2, silver nanoparticles (Ag NPs, and Ag NPs/TiO2/SiO2. Moreover, the catalytic activity of the Ag NPs/ TiO2/SiO2 was investigated in the reduction of 4-nitrophenol (4-NP at room temperature. On the basis of the results, the Ag NPs/TiO2/SiO2 was found to be high catalytic activity highly active catalyst according to the experimental results in this study. In addition, Ag NPs/TiO2/SiO2 can be recovered and reused several times in the reduction of 4-NP with no significant loss of catalytic activity.

Transparent Glass-Ceramics Produced by Sol-Gel: A Suitable Alternative for Photonic Materials

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Giulio Gorni

2018-01-01

Full Text Available Transparent glass-ceramics have shown interesting optical properties for several photonic applications. In particular, compositions based on oxide glass matrices with fluoride crystals embedded inside, known as oxyfluoride glass-ceramics, have gained increasing interest in the last few decades. Melt-quenching is still the most used method to prepare these materials but sol-gel has been indicated as a suitable alternative. Many papers have been published since the end of the 1990s, when these materials were prepared by sol-gel for the first time, thus a review of the achievements obtained so far is necessary. In the first part of this paper, a review of transparent sol-gel glass-ceramics is made focusing mainly on oxyfluoride compositions. Many interesting optical results have been obtained but very little innovation of synthesis and processing is found with respect to pioneering papers published 20 years ago. In the second part we describe the improvements in synthesis and processing obtained by the authors during the last five years. The main achievements are the preparation of oxyfluoride glass-ceramics with a much higher fluoride crystal fraction, at least double that reported up to now, and the first synthesis of NaGdF4 glass-ceramics. Moreover, a new SiO2 precursor was introduced in the synthesis, allowing for a reduction in the treatment temperature and favoring hydroxyl group removal. Interesting optical properties demonstrated the incorporation of dopant ions in the fluoride crystals, thus obtaining crystal-like spectra along with higher efficiencies with respect to xerogels, and hence demonstrating that these materials are a suitable alternative for photonic applications.

Transparent Glass-Ceramics Produced by Sol-Gel: A Suitable Alternative for Photonic Materials

Science.gov (United States)

Gorni, Giulio; Mosa, Jadra; Balda, Rolindes; Fernández, Joaquin; Durán, Alicia; Castro, Yolanda

2018-01-01

Transparent glass-ceramics have shown interesting optical properties for several photonic applications. In particular, compositions based on oxide glass matrices with fluoride crystals embedded inside, known as oxyfluoride glass-ceramics, have gained increasing interest in the last few decades. Melt-quenching is still the most used method to prepare these materials but sol-gel has been indicated as a suitable alternative. Many papers have been published since the end of the 1990s, when these materials were prepared by sol-gel for the first time, thus a review of the achievements obtained so far is necessary. In the first part of this paper, a review of transparent sol-gel glass-ceramics is made focusing mainly on oxyfluoride compositions. Many interesting optical results have been obtained but very little innovation of synthesis and processing is found with respect to pioneering papers published 20 years ago. In the second part we describe the improvements in synthesis and processing obtained by the authors during the last five years. The main achievements are the preparation of oxyfluoride glass-ceramics with a much higher fluoride crystal fraction, at least double that reported up to now, and the first synthesis of NaGdF4 glass-ceramics. Moreover, a new SiO2 precursor was introduced in the synthesis, allowing for a reduction in the treatment temperature and favoring hydroxyl group removal. Interesting optical properties demonstrated the incorporation of dopant ions in the fluoride crystals, thus obtaining crystal-like spectra along with higher efficiencies with respect to xerogels, and hence demonstrating that these materials are a suitable alternative for photonic applications. PMID:29385706

Synthesis of unidirectional structures of SiO2-Ag using Au nanoparticles as nucleation centers

International Nuclear Information System (INIS)

Villa S, G.; Mendoza A, D.; Gutierrez W, C.; Perez H, R.

2008-01-01

This paper reports a method to synthesize Ag unidirectional structures covered with SiO 2 by sol-gel technique using Au nanoparticles as nucleation centers of the unidirectional structures. In the first phase unidirectional structures of SiO 2 -Ag CI are obtained by sol-gel, using TEOS as a precursor of metallic structures (Ag) and the incorporation of Au nanoparticles as nucleation centers for growth of unidirectional structures. In the second stage, one-way systems are subjected to thermal treatment in H 2 atmosphere for obtain AG 0 particles through mechanisms that diffusion and coalescence of silver to form structures that have a thin cover of SiO 2 . Analysis by scanning electron microscopy, transmission and atomic force microscopy allowed to determine the chemical composition and microstructural properties of unidirectional systems SiO 2 -Ag. (Author)

Pd/Nb2O5/SiO2 catalyst for the direct hydrodeoxygenation of biomass-related compounds to liquid alkanes under mild conditions.

Science.gov (United States)

Shao, Yi; Xia, Qineng; Liu, Xiaohui; Lu, Guanzhong; Wang, Yanqin

2015-05-22

A simple Pd-loaded Nb2 O5 /SiO2 catalyst was prepared for the hydrodeoxygenation of biomass-related compounds to alkanes under mild conditions. Niobium oxide dispersed in silica (Nb2 O5 /SiO2 ) as the support was prepared by the sol-gel method and characterized by various techniques, including N2 adsorption, XRD, NH3 temperature-programmed desorption (TPD), TEM, and energy-dispersive X-ray spectroscopy (EDAX) atomic mapping. The characterization results showed that the niobium oxide species were amorphous and well dispersed in silica. Compared to commercial Nb2 O5 , Nb2 O5 /SiO2 has significantly more active niobium oxide species exposed on the surface. Under mild conditions (170 °C, 2.5 MPa), Pd/10 %Nb2 O5 /SiO2 was effective for the hydrodeoxygenation reactions of 4-(2-furyl)-3-buten-2-one (aldol adduct of furfural with acetone), palmitic acid, tristearin, and diphenyl ether (model compounds of microalgae oils, vegetable oils, and lignin), which gave high yields (>94 %) of alkanes with little CC bond cleavage. More importantly, owing to the significant promotion effect of NbOx species on CO bond cleavage and the mild reaction conditions, the CC cleavage was considerably restrained, and the catalyst showed an excellent activity and stability for the hydrodeoxygenation of palmitic acid with almost no decrease in hexadecane yield (94-95 %) in a 150 h time-on-stream test. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterizing the residual glass in a MgO/Al2O3/SiO2/ZrO2/Y2O3 glass-ceramic

Science.gov (United States)

Seidel, Sabrina; Patzig, Christian; Wisniewski, Wolfgang; Gawronski, Antje; Hu, Yongfeng; Höche, Thomas; Rüssel, Christian

2016-01-01

The non-isochemical crystallization of glasses leads to glass-ceramics in which the chemical composition of the amorphous matrix differs from that of the parent glass. It is challenging to solely analyse the properties of these residual glassy phases because they frequently contain finely dispersed crystals. In this study, the composition of the residual glass matrix after the crystallization of a glass with the mol% composition 50.6 SiO2 · 20.7 MgO · 20.7 Al2O3 · 5.6 ZrO2 · 2.4 Y2O3 is analysed by scanning transmission electron microscopy (STEM) including energy dispersive X-ray analysis (EDXS). A batch of the residual glass with the determined composition is subsequently melted and selected properties are analysed. Furthermore, the crystallization behaviour of this residual glass is studied by X-ray diffraction, scanning electron microscopy including electron backscatter diffraction and STEM-EDXS analyses. The residual glass shows sole surface crystallization of indialite and multiple yttrium silicates while bulk nucleation does not occur. This is in contrast to the crystallization behaviour of the parent glass, in which a predominant bulk nucleation of spinel and ZrO2 is observed. The crystallization of the residual glass probably leads to different crystalline phases when it is in contact to air, rather than when it is enclosed within the microstructure of the parent glass-ceramics. PMID:27734918

Glass formation and properties of glasses in V/sub 2/O/sub 5/-B/sub 2/O/sub 3/-P/sub 2/O/sub 5/ system

Energy Technology Data Exchange (ETDEWEB)

Sedmale, G P; Vajvad, Ya A; Arkhipova, S E; Laukmanis, L A

1987-01-01

The glass formation in the system V/sub 2/O/sub 5/-B/sub 2/O/sub 3/-P/sub 2/O/sub 5/ and the properties of the obtained glasses have been studied by methods including that of the mathematical design and the treatment of the obtained data on ECM. The glass formation region is limited by the molar content of V/sub 2/O/sub 5/ 30-80%, B/sub 2/O/sub 3/ 0-45%, P/sub 2/O/sub 5/ 20-65%. The chemical stability data show that at the molar content of V/sub 2/O/sub 5/ 45-50% the transfer of vanadium from the state of the modificator to the glass-forming agent takes place. For the studied glasses the electron mechanism of conductivity is the dominating one.

Quantitative analysis of crystalline and remaining glass phases in CaO-B2O3-SiO2 ternary system glass ceramics

International Nuclear Information System (INIS)

He Ming; Wu Mengqiang; Zhang Shuren; Zhou Xiaohua; Zhang Ting; Chen Song

2010-01-01

Research highlights: → As for CBS ternary system glass ceramics, due to the complex phase compositions, many methods could be difficult to determine quantitatively the absolute amounts of crystalline and remaining oxides. In this study, an available method based on the Rietveld method was used to quantitatively analyze the relative weight fraction and densities of crystalline phases. These above data are used to obtain a table of both relative weight fraction of crystalline phases and densities of all phases including CBS LTCC. Using volume additivity rule, it is possible to analysis quantitatively the absolute weight fraction of crystalline phases and also the oxides molar content in the remaining glass. - Abstract: Based on Rietveld method of X-ray techniques and volume additivity rule, a new method was developed to quantitatively analyze the phase composition of CaO-B 2 O 3 -SiO 2 ternary system glass ceramics. Lattice parameters, densities and relative weight fractions of crystalline phases in CaO-B 2 O 3 -SiO 2 ternary system were obtained by X-ray diffraction (XRD) refinement. According to the relative weight fraction of crystalline phases and densities of various components, the volume additivity rule was revealed by calculating the absolute weight fraction of crystalline phases of CaO-B 2 O 3 -SiO 2 glass ceramics. In addition, molar contents of the oxides in the remaining glass can also be determined by this method. Comparing this method with internal standard method, it is found that the maximum deviations of the crystallinity and the absolute weight fraction of crystalline phases are less than 2.6% and 2.9%, respectively. As a result, quantitative evaluation of CaO-B 2 O 3 -SiO 2 ternary system glass ceramics can be achieved using this method.

Internal Friction of (SiO2)1-x (GeO2)x Glasses

OpenAIRE

Kosugi , T.; Kobayashi , H.; Kogure , Y.

1996-01-01

Internal friction of (SiO2)1-x (GeO2)x glasses (x = 0, 5, 10, 24 and 100 mole%) is measured at temperatures between 1.6 and 280 K. The data are filted with the equations for thermally activated relaxation with distributing activation energies in symmetrical double-well potentials. From the determined relaxation strength spectra for each sample, the contributions from each type of microscopic structural units are calculated assuming that transverse motion of the bridging O atom in Si-O-Si, Si-...

Synthesis of ZrO2-TiO2 mixed oxide spheres by sol-gel method and investigation of Sr adsorption behaviours by experimental design approach

International Nuclear Information System (INIS)

Cetinkaya, B.; Tel, H.; Altas, Y.; Eral, M.; Sert, S.; Inan, S.; Talip, Z.

2009-01-01

ZrO 2 -TiO 2 gel spheres were synthesized by sol-gel method. Zr-Ti sol solution was prepared from ZrCl 4 and TiCl 4 (1:1 mol ratio) via partial neutralization by ammonia to obtain 0.5M final metal concentration. ZrO 2 -TiO 2 sol was transferred to vibrating nozzle system by peristaltic pump. Vibrating nozzle system was designed and produced in Institute of Nuclear Sciences. Sol drops formed by nozzle were gelled in gelation column. Synthesized ZrO 2 -TiO 2 spheres were aged for 24h then washed with deionized water and dried in oven. Sr + 2 adsorption behaviors of ZrO 2 -TiO 2 mixed oxides were investigated with central composite design (CCD). Four independent parameters (pH, initial Sr + 2 concentration, temperature and contact time) were investigated with 7 replicates at central points. Sorption data have been interpreted in terms of Langmuir, Freundlich and Dubinin Radushkevich equations. Thermodynamic parameters for the sorption system have been determined.

Effect of SiO2 concentration in silica sol on interface reaction during titanium alloy investment casting

Directory of Open Access Journals (Sweden)

Ya-meng Wei

2018-01-01

Full Text Available Using silica sol as a binder for titanium investment casting is very attractive due to its good stability and reasonable cost as compared with yttrium sol and zirconium sol. However, the mechanism of interface reaction in the related system remains unclear. In this investigation, the interface reaction between Y2O3-SiO2 (Y-Si shell mold and titanium alloys was studied. A group of shell molds were prepared by using Y2O3 sand and silica sol with different contents of SiO2. Ti-6Al-4V alloy was cast under vacuum by gravity casting through cold crucible induction melting (CCIM method. Scanning electron microscopy (SEM and energy dispersive x-ray spectroscopy (EDS were employed to characterize the micromorphology and composition of the reaction area, respectively. X-ray photoelectron spectroscopy (XPS was used to confirm the valence state of relevant elements. White light interferometer (WLI was used to obtain the surface topography of Y-Si shells. The results show that the thickness of reaction layers is below 3 μm when the SiO2 content of silica sol is below 20wt.%. Whereas, when the SiO2 content increases to 25wt.%, the thickness of the reaction layer increases sharply to about 15 μm. There is a good balance between chemical inertness and mechanical performance when the SiO2 content is between 15 and 20wt.%. Moreover, it was found that the distribution of SiO2 and the roughness at the surface of the shell are the key factors that determine the level of reaction.

Study and fabrication of ZnNb2O6 thin films by sol-gel method

International Nuclear Information System (INIS)

Hsu, Cheng-Hsing; Yang, Pai-Chuan; Yang, Hsi-Wen; Yan, Shu-Fong; Tung, Hsin-Han

2011-01-01

Zinc niobium oxide (ZnNb 2 O 6 ) thin films were grown on ITO/glass substrate by sol-gel process. Microstructure and surface morphology of the ZnNb 2 O 6 thin films have been studied by X-ray diffraction and scanning electron microscopy. Optical properties of the ZnNb 2 O 6 thin films were obtained by UV-visible recording spectrophotometer. The dependence of the microstructure, optical transmittance spectra, optical band gap on annealing temperature was also investigated.

New sol-gel bioactive glass and titania composites with enhanced physico-chemical and biological properties.

Science.gov (United States)

Pawlik, Justyna; Widziołek, Magdalena; Cholewa-Kowalska, Katarzyna; Łączka, Maria; Osyczka, Anna Maria

2014-07-01

We developed TiO2 matrix composites modified by sol-gel bioactive glasses (SBG) of either high CaO content (A2) or high SiO2 content (S2). The latter were mixed with titanium dioxide (TiO2) at 75:25, 50:50, and 25:75 weight ratios and sintered at 1250°C for 2 h. We examined the effects of various types (A2 or S2) and compositional TiO2 :SBG ratios on the mechanical properties of resulting composites, their bioactivity and human bone marrow mesenchymal stem cells (MSC) response. The chemistry of SBGs influenced the phase composition, mechanical and biological properties of the composites. Rutile and titanite prevailed in A2-TiO2 composites, and rutile and crystobalite in S2-TiO2 composites. Compressive strength increased significantly for 25A2-TiO2 composites (140 MPa) compared to matrix TiO2 (58 MPa). Composites containing 50-75 wt % of either SBG displayed bioactive properties as determined by simulated body fluid test. Compared to TiO2, human bone marrow stromal cell (BMSC) viability was enhanced on the composites containing 25 wt % of either SBG, whereas the composites modified by 25 wt % of S2 enhanced alkaline phosphatase activity and mineralization in cultures treated with osteogenic inducers-dexamethasone (Dex) or bone morphogenetic protein. Increasing amounts of A2 in TiO2 matrix decreased cell viability but increased collagen deposition and mineralized matrix production by BMSC. Considering the physico-chemical and biological properties of the presented composites, the modification of TiO2 with SBG may prove useful strategy in several bone tissue related regeneration strategies. © 2013 Wiley Periodicals, Inc.

Analyses of desorbed H2O with temperature programmed desorption technique in sol-gel derived HfO2 thin films

International Nuclear Information System (INIS)

Shimizu, H.; Nemoto, D.; Ikeda, M.; Nishide, T.

2009-01-01

Hafnium oxide (HfO 2 ) is a promising material for the gate insulator in highly miniaturized silicon (Si) ultra-large-scale-integration (ULSI) devices (32 nm and beyond). In the field chemistry, a sol-gel processing has been used to fabricate HfO 2 thin film with the advantages of low cost, relative simplicity, and easy control of the composition of the layers formed. Temperature-programmed desorption (TPD) has been used not only for analyzing adsorbed gases on the surfaces of bulk sol-gel-derived HfO 2 of sol-gel-derived HfO 2 thin film fired at 350, 450, 550 and 700 deg C in sol-gel derived HfO 2 films in air is investigated using TPD, and also the material characterization of HfO 2 thin films is evaluated by X-ray diffraction (XRD) method. The dielectric constant of the films was also estimated using the capacitance-voltage (C-V) method. TPD is essentially a method of analyzing desorped gases from samples heated by infra-red light as a function of temperature under vacuum conditions using a detector of quadruple mass spectroscopy (QMS). Sol-gel-derived HfO 2 films were fabricated on 76-mm-diameter Si(100) wafers as follows. Hafnia sol solutions were prepared by dissolving HfCl 4 in NH 4 OH solution, followed by the of HCOOH. (author)

TiO2 effect on crystallization mechanism and physical properties of nano glass-ceramics of MgO-Al2O3-SiO2 glass system.

Science.gov (United States)

Jo, Sinae; Kang, Seunggu

2013-05-01

The effect of TiO2 on the degree of crystallization, thermal properties and microstructure for MgO-Al2O3-SiO2 glass-ceramics system containing 0-13 wt% TiO2 and 0-1.5 wt% B2O3 in which the cordierite is the main phase was studied. Using Kissinger and Augis-Bennett equations, the activation energy, 510 kJ/mol and Avrami constant, 1.8 were calculated showing the surface-oriented crystallization would be preferred. The alpha-cordierite phase was generated in the glass-ceramics of containing TiO2 of 0-5.6 wt%. However, for the glass-ceramics of TiO2 content above 7 wt%, an alpha-cordierite disappeared and micro-cordierite phase was formed. The glass-ceramics of no TiO2 added had spherical crystals of few tens nanometer size spread in the matrix. As TiO2 content increased up to 5.6 wt%, a lump of dendrite was formed. In the glass-ceramics containing TiO2 7-13 wt%, in which the main phase is micro-cordierite, the dendrite crystal disappeared and a few hundred nanometer sized crystal particles hold tightly each other were generated. The thermal conductivity of glass-ceramics of both a-cordierite and micro-cordierite base decreased with TiO2 contend added. The thermal conductivity of glass-ceramics of 1.5 wt% TiO2 added was 3.4 W/mK which is 36% higher than that of glass-ceramics of no TiO2 added. The sintering temperature for 1.5 wt% TiO2 glass-ceramics was 965 degrees C which could be concluded as to apply to LTCC process for LED packaging.

Seed-mediated photodeposition route to Ag-decorated SiO2@TiO2 microspheres with ideal core-shell structure and enhanced photocatalytic activity

Science.gov (United States)

Ma, Jianqi; Guo, Xiaohua; Ge, Hongguang; Tian, Guanghui; Zhang, Qiang

2018-03-01

Ag-decorated SiO2@TiO2 microspheres (SiO2@TiO2-Ag) with ideal core-shell structure and enhanced photocatalytic activity were successfully fabricated by combining both coating anatase TiO2 on the surface of SiO2 spheres and subsequent depositing face-centered cubic Ag nanoparticles (NPs) on the coated TiO2 surface via novel sol-gel method and Ag-seed-mediated photodeposition (PD) route, respectively. The morphology, structure, composition and optical properties of the resulting composites were characterized in detail. The results reveal that the monodisperse SiO2 spheres of ∼260 nm were covered uniformly and perfectly by the TiO2 nanoparticle coating layer with the thickness of ca. 55 nm by the novel sol-gel method. Further, homogeneously and highly dispersed Ag NPs with an average size of 8 ± 1.5 nm were strongly anchored onto the TiO2 surface in SiO2@TiO2 core-shell spheres by the modified PD process (Ag-seed-mediated PD route), whereas polydispersed Ag aggregates and detached Ag NPs were irregularly deposited over the TiO2 surface in previous works, which is the inherent problem and has not been effectively solved for depositing noble metal NPs such as Au, Ag, Pt, Pd on TiO2 surface by conventional PD method. The formation mechanism of small and uniformly dispersed Ag NPs with narrow size distribution via the modified PD method is tentatively explained by both nucleation kinetics and growth kinetics. The key reason is that the pre-deposited seeds firmly tethered on SiO2@TiO2 spheres served as nucleation sites and anchoring points for the further nucleation and subsequent growth of Ag via photoreduction of Ag+.

Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

Science.gov (United States)

Sibille, L.; Gavira-Gallardo, J. A.; Hourlier-Bahloul, D.

2004-01-01

Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil similar JSC-1 in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. Characterization of the precursor molecules and efforts to further concentrate and hydrolyze the products to obtain gel materials will be presented for evaluation as ceramic precursors.

Structural Modification of Sol-Gel Synthesized V2O5 and TiO2 Thin Films with/without Erbium Doping

Directory of Open Access Journals (Sweden)

Fatma Pınar Gökdemir

2014-01-01

Full Text Available Comparative work of with/without erbium- (Er- doped vanadium pentoxide (V2O5 and titanium dioxide (TiO2 thin films were carried out via sol-gel technique by dissolving erbium (III nitrate pentahydrate (Er(NO33·5H2O in vanadium (V oxoisopropoxide (OV[OCH(CH32]3 and titanium (IV isopropoxide (Ti[OCH(CH32]4. Effect of Er doping was traced by Fourier transform IR (FTIR, thermogravimetric/differential thermal (TG/DTA, and photoluminescence measurements. UV-Vis transmission/absorption measurement indicated a blue shift upon Er doping in V2O5 film due to the softening of V=O bond while appearance of typical absorption peaks in Er-doped TiO2 film. Granule size of the films increased (reduced upon Er substitution on host material compared to undoped V2O5 and TiO2 films, respectively.

Preparation and characterization of new glasses from the TeO2-CdO-Al2O3-SiO2 system

OpenAIRE

Zayas, Mª. E.; Espinoza-Beltrán, F. J.; Romero, Maximina; Rincón López, Jesús María

1998-01-01

A new family of glasses from the TeO2-CdO-Al2O3-SiO2 system obtained from CdS-TeO2 mixtures melted in fireclay crucibles have been prepared and characterized. The density values of these glasses are in the 3.30-3.46 gcm-3 range. The viscosity-temperature variation shows that glasses with high TeO2 content depict the typical variation of `short glasses' for a molding operation. Microstructural observations by TEM (replica method) and SEM microscopies have shown that these glasses contain very ...

PDMS-SiO{sub 2}-TiO{sub 2}-CaO hybrid materials – Cytocompatibility and nanoscale surface features

Energy Technology Data Exchange (ETDEWEB)

Almeida, J. Carlos [CICECO - Aveiro Institute of Materials, Department of Materials and Ceramic Engineering, University of Aveiro, 3810-193 Aveiro (Portugal); Wacha, András [Research Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar Tudósok körútja 2, Budapest 1117 (Hungary); Gomes, Pedro S.; Fernandes, M. Helena R. [Laboratory for Bone Metabolism and Regeneration, Faculdade de Medicina Dentária, Universidade do Porto (Portugal); Fernandes, M. Helena Vaz [CICECO - Aveiro Institute of Materials, Department of Materials and Ceramic Engineering, University of Aveiro, 3810-193 Aveiro (Portugal); Salvado, Isabel M. Miranda, E-mail: isabelmsalvado@ua.pt [CICECO - Aveiro Institute of Materials, Department of Materials and Ceramic Engineering, University of Aveiro, 3810-193 Aveiro (Portugal)

2016-07-01

Two PDMS-SiO{sub 2}-TiO{sub 2}-CaO porous hybrid materials were prepared using the same base composition, precursors, and solvents, but following two different sol-gel procedures, based on the authors' previous works where for the first time, in this hybrid system, calcium acetate was used as calcium source. The two different procedures resulted in monolithic materials with different structures, microstructures, and surface wettability. Even though both are highly hydrophobic (contact angles of 127.2° and 150.6°), and present different filling regimes due to different surface topographies, they have demonstrated to be cytocompatible when tested with human osteoblastic cells, against the accepted idea that high-hydrophobic surfaces are not suitable to cell adhesion and proliferation. At the nanoscale, the existence of hydrophilic silica domains containing calcium, where water molecules are physisorbed, is assumed to support this capability, as discussed. - Highlights: • Two hybrid materials were prepared following two different sol-gel procedures. • Both are highly hydrophobic but demonstrated to be cytocompatible. • Different filling regimes were observed.

Preparation of sol-gel TiO2/purified Na-bentonite composites and their photovoltaic application for natural dye-sensitized solar cells

International Nuclear Information System (INIS)

Saelim, Ni-on; Magaraphan, Rathanawan; Sreethawong, Thammanoon

2011-01-01

Highlights: → Natural dye from red cabbage was successfully employed in DSSC. → A fast sol-gel method to produce TiO 2 /clay thin film was proposed. → The sol-gel-prepared TiO 2 /clay was applied as the scattering layer on top of TiO 2 electrode. → Thicker sol-gel-prepared TiO 2 /clay electrode showed higher DSSC efficiency. - Abstract: The sol-gel TiO 2 /purified natural clay electrodes having Ti:Si molar ratios of 95:5 and 90:10 were initially prepared, sensitized with natural red cabbage dye, and compared to the sol-gel TiO 2 electrode in terms of physicochemical characteristics and solar cell efficiency. The results showed that the increase in purified Na-bentonite content greatly increased the specific surface area and total pore volume of the prepared sol-gel TiO 2 /purified Na-bentonite composites because the clay platelets prevented TiO 2 particle agglomeration. The sol-gel TiO 2 /5 mol% Si purified Na-bentonite and sol-gel TiO 2 /10 mol% Si purified Na-bentonite composites could increase the film thickness of solar cells without cracking when they were coated as a scattering layer on the TiO 2 semiconductor-based film, leading to increasing the efficiency of the natural dye-sensitized solar cells in this work.

CoO-doped MgO-Al2O3-SiO2-colored transparent glass-ceramics with high crystallinity

Science.gov (United States)

Tang, Wufu; Zhang, Qian; Luo, Zhiwei; Yu, Jingbo; Gao, Xianglong; Li, Yunxing; Lu, Anxian

2018-02-01

To obtain CoO-doped MgO-Al2O3-SiO2 (MAS)-colored transparent glass-ceramics with high crystallinity, the glass with the composition 21MgO-21Al2O3-54SiO2-4B2O3-0.2CoO (in mol %) was prepared by conventional melt quenching technique and subsequently thermal treated at several temperatures. The crystallization behavior of the glass, the precipitated crystalline phases and crystallinity were analyzed by X-ray diffraction (XRD). The microstructure of the glass-ceramics was characterized by field emission scanning electron microscopy (FSEM). The transmittance of glass-ceramic was measured by UV spectrophotometer. The results show that a large amount of α-cordierite (indianite) with nano-size was precipitated from the glass matrix after treatment at 1020 °C for 3 h. The crystallinity of the transparent glass-ceramic reached up to 97%. Meanwhile, the transmittance of the glass-ceramic was 74% at 400 nm with a complex absorption band from 450 nm to 700 nm. In addition, this colored transparent glass-ceramic possessed lower density (2.469 g/cm3), lower thermal expansion coefficient (1.822 × 10-6 /℃), higher Vickers hardness (9.1 GPa) and higher bending strength (198 MPa) than parent glass.

Surface chemistry and durability of borosilicate glass

International Nuclear Information System (INIS)

Carroll, S.A.; Bourcier, W.L.; Phillips, B.L.

1994-01-01

Important glass-water interactions are poorly understood for borosilicate glass radioactive waste forms. Preliminary results show that glass durability is dependent on reactions occurring at the glass-solution interface. CSG glass (18.2 wt. % Na 2 O, 5.97 wt. % CaO, 11.68 wt. % Al 2 O 3 , 8.43 wt. % B 2 O 3 , and 55.73 wt. % SiO 2 ) dissolution and net surface H + and OH - adsorption are minimal at near neutral pH. In the acid and alkaline pH regions, CSG glass dissolution rates are proportional to [H + ] adsorbed 2 and [OH - ] adsorbed 0.8 , respectively. In contrast, silica gel dissolution and net H + and OH - adsorption are minimal and independent of pH in acid to neutral solutions. In the alkaline pH region, silica gel dissolution is proportional to [OH - ] adsorbed 0.9 adsorbed . Although Na adsorption is significant for CSG glass and silica gel in the alkaline pH regions, it is not clear if it enhances dissolution, or is an artifact of depolymerization of the framework bonds

Spectroscopic features of Ni(2+) ion in PbO-Bi2O3-SiO2 glass system.

Science.gov (United States)

Suresh, B; Srinivasa Reddy, M; Siva Sesha Reddy, A; Gandhi, Y; Ravi Kumar, V; Veeraiah, N

2015-04-15

Glasses of the composition (30-x)PbO-5Bi2O3-65SiO2: xNiO (with x ranging from 0 to 1.0 mol%) were synthesized. A variety of spectroscopic studies, viz., IR, Raman optical absorption and luminescence properties of these glasses have been carried out as a function of NiO concentration. The analysis of results of all these studies has indicated that the nickel ions occupy both octahedral and tetrahedral positions. However, with the increase of NiO concentration the octahedral occupancy of Ni(2+) ions prevailed over the tetrahedral ions. The luminescence spectra of these glasses have exhibited a broad NIR emission band in region 1100-1500 nm. This band is identified as being due to (3)T2(3F)→(3)A2(3F) octahedral transition of Ni(2+) ions. The luminescence efficiency and cross section have been found to be the highest for the glass containing the highest concentration of NiO. The reasons for such high luminescence efficiency have been discussed in the light of structural variations taking place in the host glass network. Copyright © 2015 Elsevier B.V. All rights reserved.

Optical properties of transparent Li2O-Ga2O3-SiO2 glass-ceramics embedding Ni-doped nanocrystals

International Nuclear Information System (INIS)

Suzuki, Takenobu; Murugan, Ganapathy Senthil; Ohishi, Yasutake

2005-01-01

Transparent Li 2 O-Ga 2 O 3 -SiO 2 (LGS) glass-ceramics embedding Ni:LiGa 5 O 8 nanocrystals were fabricated. An intense emission centered around 1300 nm with the width of more than 300 nm was observed by 976 nm photoexcitation of the glass-ceramics. The lifetime was more than 900 μs at 5 K and 500 μs at 300 K. The emission could be attributed to the 3 T 2g ( 3 F)→ 3 A 2g ( 3 F) transition of Ni 2+ in distorted octahedral sites in LiGa 5 O 8 . The product of stimulated emission cross section and lifetime for the emission was about 3.7x10 -24 cm 2 s and was a sufficiently practical value

Silver effect on the structure of SiO2-CaO-P2O5 ternary system

International Nuclear Information System (INIS)

Vulpoi, Adriana; Baia, Lucian; Simon, Simion; Simon, Viorica

2012-01-01

In this study are reported results obtained from the structural, morphological and textural investigations of 56SiO 2 ∙(40-x)CaO·4P 2 O 5 ·xAg 2 O system, where 0 ≤ x ≤ 10 mol%. The samples obtained by sol–gel method were annealed and then characterized by X-ray diffraction (XRD), differential thermal analysis (DTA), thermal gravimetric analysis (TGA), vibrational spectroscopy (Raman, FTIR), N 2 -adsorption measurements, and transmission electron microscopy (TEM). XRD patterns of the investigated samples exhibit tricalcium phosphate (TCP) nanostructured phase and show the existence of metallic silver as dispersed phase. The presence of apatite-like phase is underlined by the recorded Raman and especially FT-IR spectra. TEM pictures indicate the presence of silver nanoparticles of almost spherical shapes and various sizes inside the matrix, depending on the Ag 2 O content. Regarding the textural properties, it was observed both a decrease of the specific surface area as well as a progressive change of the mesoporous characteristics with the silver addition, the latter behavior recommending the potential use of these samples for applications, where the morphology control is required.

Gel electrolytes based on poly(acrylonitrile)/sulpholane with hybrid TiO2/SiO2 filler for advanced lithium polymer batteries

International Nuclear Information System (INIS)

Kurc, Beata

2014-01-01

Highlights: • Paper describes properties of gel electrolyte based on PAN with TMS and TiO 2 -SiO 2 . • The TiO 2 -SiO 2 oxide composite was precipitated in the emulsion system and used as the fillers. • The capacity of the graphite anode depends on the current rate and the amount of TiO 2 -SiO 2 . • For PE3 electrolyte was obtained practical capacity more than 90% of the theoretical capacity. - Abstract: This paper describes the synthesis and properties of a new type of ceramic fillers for composite polymer gel electrolytes. Hybrid TiO 2 -SiO 2 ceramic powders have been obtained by co-precipitation from titanium(IV) sulfate solution using sodium silicate as the precipitating agent. The resulting submicron-size powders have been applied as fillers for composite polymer gel electrolytes for Li-ion batteries based on polyacrylonitrile (PAN) membranes. The powders and gel electrolytes have been examined structurally and electrochemically, showing favorable properties in terms of electrolyte uptake and electrochemical characteristics in Li-ion cells

Raman and infrared investigations of glass and glass-ceramics with composition 2Na2O·1CaO·3SiO2