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Sample records for alkoxide-based sol-gel route

  1. Preparation and characterization of lead zirconate titanate ceramic fibers with alkoxide-based sol-gel route

    NASA Astrophysics Data System (ADS)

    Mai, Manfang; Lin, Cheng; Xiong, Zhaoxian; Xue, Hao; Chen, Lifu

    2009-03-01

    Lead zirconate titanate (PZT) fibers with diameters from 10μm to 40μm were prepared via a sol-gel route. Several kinds of chemicals were used, including lead acetate trihydrate, zirconium n-butoxide and titanium n-butoxide, in addition to butanol as a solvent. As a water source for hydrolysis reaction, Pb(CH3COO)2·3H2O was directly used without further adding of water or catalyst conventionally. Acetylacetonate and acetate were added as stabilization agents to obtain stable sols for fiber drawing. The gel-to-ceramic conversion was characterized with thermal analysis, infrared spectroscopy and X-ray diffraction. A pure perovskite phase was obtained after heat treatment at 650°C for 1h. By using scanning electron microscope (SEM), it was observed that a lower rate of heat treatment resulted in a denser microstructure of the fibers. The relative permittivity and the P-E hysteresis loop of the crystalline PZT fibers were also measured and discussed in the paper.

  2. The effect of refluxing on the alkoxide-based sodium potassium niobate sol-gel system: Thermal and spectroscopic studies

    SciTech Connect

    Chowdhury, Anirban; Bould, Jonathan; Londesborough, Michael G.S.; Milne, Steven J.

    2011-02-15

    A study on the effects of prolonged heating under reflux conditions of up to 70 h on alkoxides of sodium, potassium and niobium dissolved in 2-methoxyethanol for the synthesis of sols of composition Na{sub 0.5}K{sub 0.5}NbO{sub 3} (NKN) has been carried out using combined thermogravimetric-Fourier transform infrared spectroscopic analyses. Extended refluxing increases the homogeneity of the Na{sub 0.5}K{sub 0.5}NbO{sub 3} (NKN) system. Spectroscopic analyses on the non-refluxed and 70 h refluxed NKN gels reveal the existence of inorganic hydrated carbonates and bicarbonates, which we propose arise from the hydration and carbonation of the samples on standing in air. The X-ray diffraction patterns of these two types of gels show orthorhombic NKN phase evolutions at higher temperatures. -- Graphical abstract: Total organic evolution plots over time for NKN dried gels obtained under different refluxing times show different thermochemical behaviours and these were investigated by thermal and spectroscopic analysis tools to find a correlation between the extent of -M-O-M- chain link formation and the amount of solvent vapour (methoxyethanol) evolution. Display Omitted Research highlights: > Prolonged refluxing of sol-gel NKN precursor solutions improves final properties of an NKN system. > An NKN process thermo-chemistry with thermal and spectroscopic analysis tools was explored. > An FTIR of NKN gels reveals tendency of NKN systems for rehydration and recarbonation on standing.

  3. Synthesis of nano-titanium dioxide by sol-gel route

    NASA Astrophysics Data System (ADS)

    Kaler, Vandana; Duchaniya, R. K.; Pandel, U.

    2016-04-01

    Nanosized titanium dioxide powder was synthesised via sol-gel route by hydrolysis of titanium tetraisopropoxide with ethanol and water mixture in high acidic medium. The synthesized nanopowder was further characterized by X-ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and Ultraviolet Visible Spectroscopy in order to determine size, morphology and crystalline structure of the material. The synthesis of nano-TiO2 powder in anatase phase was realized by XRD. The optical studies of nano-TiO2 powder was carried out by UV-Vis spectroscopy and band gap was calculated as 3.5eV, The SEM results with EDAX confirmed that prepared nano-TiO2 particles were in nanometer range with irregular morphology. The FTIR analysis showed that only desired functional groups were present in sample. These nano-TiO2 particles have applications in solar cells, chemical sensors and paints, which are thrust areas these days.

  4. Synthesis of cobalt aluminate nanopigments by a non-aqueous sol-gel route.

    PubMed

    Karmaoui, Mohamed; Silva, Nuno J O; Amaral, Vitor S; Ibarra, Alfonso; Millán, Ángel; Palacio, Fernando

    2013-05-21

    Here we report the chemical synthesis of cobalt aluminum oxide (CoAl2O4) nanoparticles by a non-aqueous sol-gel route. The one-pot procedure is carried out at mild temperatures (in the 150 to 300 °C range), and consists of the reaction between cobalt acetate and aluminium isopropoxide in benzyl alcohol. The resulting CoAl2O4 nanoparticles show an unusually low average size, between 2.5 and 6.2 nm, which can be controlled by the synthesis temperature. The colorimetric properties of the nanoparticles are also determined by the synthesis temperature and the characteristic blue color of CoAl2O4 pigments is achieved in samples prepared at T ≥ 200 °C. The nanoparticles are antiferromagnetically ordered below ∼27 K with an uncompensated configuration. The uncompensated moment shows the typical features of strongly interacting superparamagnetic nanoparticles and spin-glass systems.

  5. Porous titania films fabricated via sol gel rout - Optical and AFM characterization

    NASA Astrophysics Data System (ADS)

    Karasiński, Paweł; Gondek, Ewa; Drewniak, Sabina; Kajzer, Anita; Waczyńska-Niemiec, Natalia; Basiaga, Marcin; Izydorczyk, Weronika; Kouari, Youssef E. L.

    2016-06-01

    Mesoporous titania films of low refractive index ∼1.72 and thickness within the range of 57-96 nm were fabricated via sol-gel rout and dip-coating technique on a soda-lime glass substrate. Tetrabutylorthotitanate Ti(OBu)4 was used as a titania precursor. High porosity and consequently low refractive index were achieved using the polyethylene glycol (PEG 1100) as a template. Based on transmittance, using Tauc's relations, the optical energy band gaps and the Urbach energy were determined. The research shows that in the fabricated titania films there are two types of optical energy band gaps, connected with direct and indirect electron transitions and brought about by the presence of amorphous and crystalline phase respectively. Based on the quantum size effect, the diameters of nanocrystals versus film thickness were determined. AFM studies of the titania films have demonstrated that there are changes of surface morphology taking place with the change of thickness. We have demonstrated that the surface morphology of titania films has influence on wettability.

  6. Analytical Chemistry with Silica Sol-Gels: Traditional Routes to New Materials for Chemical Analysis

    NASA Astrophysics Data System (ADS)

    Walcarius, Alain; Collinson, Maryanne M.

    2009-07-01

    The versatility of sol-gel chemistry enables us to generate a wide range of silica and organosilica materials with controlled structure, composition, morphology and porosity. These materials’ hosting and recognition properties, as well as their wide-open structures containing many easily accessible active sites, make them particularly attractive for analytical purposes. In this review, we summarize the importance of silica sol-gels in analytical chemistry by providing examples from the separation sciences, optical and electrochemical sensors, molecular imprinting, and biosensors. Recent work suggests that manipulating the structure and composition of these materials at different scales (from molecular to macromolecular states and/or from micro- to meso- and/or macroporous levels) promises to generate chemical and biochemical sensing devices with improved selectivity and sensitivity.

  7. Production and characterization of spodumene dosimetric pellets prepared by a sol-gel route

    NASA Astrophysics Data System (ADS)

    Lima, H. R. B. R.; Nascimento, D. S.; Bispo, G. F. C.; Teixeira, V. C.; Valério, M. E. G.; Souza, S. O.

    2014-11-01

    Spodumene is an aluminosilicate that has shown good results for high-dose TL dosimetry for beta or gamma rays. Due to its chemical composition (LiAlSi2O6) it has potential to be used as a neutron dosimeter. The synthetic spodumene is usually produced by solid state reaction and conventional sol-gel, whose shortcomings arise from the need to employ high temperatures and high cost reagents, respectively. Proteic sol-gel method is promising, because it can reduce production costs and the possibility of environmental contamination. This work reports the production of the spodumene by the proteic sol-gel method using edible unflavored gelatin as a precursor. The product is characterized physically and morphologically, and investigated its applicability as a TL dosimeter. Two sets of samples were prepared using different sources of silicon, one with TEOS (Si(OC3H5)4) and one with SILICA (SiO2). The materials produced were characterized by X-ray diffraction, differential thermal analysis and thermogravimetry in order to evaluate the structural properties, as well as possible changes in physical or chemical properties depending on the temperature. The production of spodumene was successful, with generation of the crystals in the β-phase with tetragonal structure. Sintered pellets produced from these crystals were irradiated with a 90Sr-90Y source and their TL glow curves were evaluated. Although the samples prepared by the proteic sol-gel method with TEOS presented a lower forming temperature, the samples produced with SILICA showed higher sensitivity to radiation.

  8. An interesting sol-gel route to prepare oxyfluoride Sr 2CuO 2F 2+δ superconductors

    NASA Astrophysics Data System (ADS)

    Fujihara, S.; Masuda, Y.; Jin, J.-S.; Kimura, T.; Tanabe, K.

    1997-02-01

    The oxyfluoride superconductor, Sr 2CuO 2F 2+δ, was prepared by a sol-gel method. Two different routes were examined; one was an attempt to prepare the Sr 2CuO 2F 2+δ phase directly from fluorine-containing sols, and the other was the fluorination of sol-gel-derived Sr 2CuO 3 fine powders by F 2 gas. The former route did not lead to the formation of oxyfluorides because of the precipitation of SrF 2 by the heat treatments of the gel. The latter route led to the formation of the Sr 2CuO 2F 2+δ phase. The amount of the Sr 2CuO 2F 2+δ phase and superconducting properties of the powders depended on the fluorinating condition such as F 2 gas concentration and fluorinating time. The Tc values reached 45-47 K by annealing the fluorinated samples in vacuo. The magnetization hysteresis loop was measured for the first time in the oxyfluoride superconductors.

  9. Low-temperature deposition of the high-performance anatase-titania optical films via a modified sol gel route

    NASA Astrophysics Data System (ADS)

    Sheng, Yonggang; Liang, Liping; Xu, Yao; Wu, Dong; Sun, Yuhan

    2008-04-01

    Anatase-titania films with high optical performances have been deposited via a modified sol-gel route. This involved several precisely controlled processes including a sufficient hydrolysis of titanium tetraisopropoxide (TTIP) with excessive water, a peptization at pH value of 1-2, a restrained condensation under the hydrothermal conditions at 373 K, and finally a spin-coating process at 293 K. A full characterization of the sols and films indicated that such a well-controlled hydrolysis and condensation of TTIP enabled the formation of high-quality precursor sols consisting of anatase-titania colloidal particles with the mean hydrodynamic diameter of about 17.2 nm, and then endowed the as-deposited films with nanocrystalline structure and the corresponding high refractive index of 1.92 (at 632.8 nm). Moreover, the prepared films exhibited large optical bandgap of 3.38 eV and high laser-induced damage threshold of 16.3 J/cm 2 (at 1064 nm, 3 ns pulse duration and R/1 testing mode), which must be closely related to their homogeneous and nearly defect-free network structures derived from the low-temperature sol-gel deposition route.

  10. New sol-gel synthetic route to transition and main-group metal oxide aerogels using inorganic salt precursors

    SciTech Connect

    Gash, A E; Tillotson, T M; Satcher Jr, J H; Hrubesh, L W; Simpson, R L

    2000-09-12

    We have developed a new sol-gel route to synthesize several transition and main-group metal oxide aerogels. The approach is straightforward, inexpensive, versatile, and it produces monolithic microporous materials with high surface areas. Specifically, we report the use of epoxides as gelation agents for the sol-gel synthesis of chromia aerogels and xerogels from simple Cr(III) inorganic salts. The dependence of both gel formation and its rate was studied by varying the solvent used, the Cr(III) precursor salt, the epoxide/Cr(III) ratio, as well as the type of epoxide employed. All of these variables were shown to affect the rate of gel formation and provide a convenient control of this parameter. Dried chromia aerogels were characterized by high-resolution transmission electron microscopy (HRTEM) and nitrogen adsorption/desorption analyses, results of which will be presented. Our studies have shown that rigid monolithic gels can be prepared from many different metal ions salts, provided the formal oxidation state of the metal ion is greater than or equal to +3. Conversely, when di-valent transition metal salts are used precipitated solids are the products.

  11. Structural and magnetic properties of hexagonal barium ferrite synthesized through the sol-gel combustion route

    NASA Astrophysics Data System (ADS)

    Zahari, Muhammad Hanif bin; Guan, Beh Hoe; Chuan, Lee Kean

    2016-11-01

    Single-phased barium ferrite with the chemical formula of BaFe12O19 was synthesized through the sol-gel combustion method by using stoichiometric amounts of the precursor materials Structural characterizations were done through X-ray diffraction (XRD) analysis. The magnetic properties were determined through vibrating sample magnetometer (VSM) measurement. Pure single-phased BaFe12O19 was successfully obtained at 850°C without any accompanying secondary phases. This was reflected in the magnetic measurements where a prominent hysteresis was displayed by the synthesized powder. Values as high as 50.37 emu/g, 2984.9 G and 26.15 emu/g was observed for the magnetic saturation, coercivity and remanence respectively.

  12. Thermo-optic characterization of neodymium/nickel doped silica glasses prepared via sol-gel route.

    PubMed

    Manuel, Ancy; Kumar, B Rajesh; Basheer, N Shemeena; Kumari, B Syamala; Paulose, P I; Kurian, Achamma; George, Sajan D

    2012-12-01

    Intrinsic as well as rare earth (Neodymium) doped silica glasses with various molar ratio of dopant and a metallic (Nickel) co-dopant is prepared via sol-gel route. The structural characterization of the sample is carried out using X-ray diffraction and Fourier Transform Infrared Spectroscopy. The influence of dopant and doping concentration on the optical properties of silica matrix is investigated via UV-VIS absorption spectroscopy. Effect of dopant on thermal effusivity value of the host matrix is carried out by laser induced open cell photoacoustic technique. Analysis of the results showed that doping affect the thermal effusivity value and results are interpreted in terms of structural modification of the lattice and phonon assisted heat transport mechanism.

  13. Sol-gel synthesis of macroporous barium zirconate monoliths from ionic precursors via a phase separation route

    NASA Astrophysics Data System (ADS)

    Guo, Xingzhong; Wang, Zichen; Song, Jie; Yang, Hui

    2017-03-01

    Monolithic macroporous barium zirconate derived from ionic precursors has been successfully prepared via a phase separation route in the presence of poly(ethylene oxide) (PEO) and propyleneoxide (PO). Poly(ethylene oxide) (PEO) acts as a phase separation inducer, while propyleneoxide (PO) acts as a gelation accelerant in the sol-gel process. Appropriate choice of poly(ethylene oxide) (PEO) and propyleneoxide (PO) allows the production of continuous macroporous monolithic gel with a porosity of ca. 63% and a macropore size of 1.8 μm. Some BaCl2 recrystallizes in the dried gel, and subsequently tetragonal ZrO2 phase precipitates after heat-treated at 800 °C. The crystalline phase barium zirconate forms after heat treatment at 1100 °C in air, while the macroporous structure is preserved with a slight increase of porosity and a decrease of macropore size.

  14. Synthesis of Yttria-Stabilized Zirconia Aerogels by a Non-Alkoxide Sol-Gel Route

    SciTech Connect

    Chervin, C N; Clapsaddle, B J; Chiu, H W; Gash, A E; Satcher, Jr., J H; Kauzlarich, S M

    2005-02-11

    Homogeneous, nanocrystalline powders of yttria-stabilized zirconia were prepared using a nonalkoxide sol-gel method. Monolithic gels, free of precipitation, were prepared by addition of propylene oxide to aqueous solutions of Zr{sup 4+} and Y{sup 3+} chlorides at room temperature. The gels were dried with supercritical CO{sub 2}(l), resulting in amorphous aerogels that crystallized into cubic stabilized ZrO{sub 2} following calcination at 500 C. The aerogels and resulting crystalline products were characterized using in-situ temperature profile X-ray diffraction, thermal analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and nitrogen adsorption/desorption analysis. TEM and N{sub 2} adsorption/desorption analysis of an aerogel indicated a porous network structure with a high surface area (409 m{sup 2}/g). The crystallized yttria-stabilized zirconia maintained high surface area (159 m{sup 2}/g) upon formation of homogeneous, nanoparticles ({approx}10 nm). Ionic conductivity at 1000 C of sintered YSZ (1500 C, 3 hours) prepared by this method, was 0.13 {+-} 0.02 {Omega}{sup -1} cm{sup -1}. Activation energies for the conduction processes from 1000-550 C and 550-400 C, were 0.95 {+-} 0.09 and 1.12 {+-} 0.05 eV, respectively. This is the first reported synthesis and characterization of yttria-stabilized zirconia via an aerogel precursor.

  15. Physical properties of NxTiO2 prepared by sol-gel route

    NASA Astrophysics Data System (ADS)

    Brahimi, Razika; Bessekhouad, Yassine; Trari, Mohamed

    2012-09-01

    The compounds NxTiO2(x=0, 0.05, 0.1, 0.2) with the anatase structure have been synthesized by Sol-Gel method using Tri-ethyl Amine as nitrogen source and their optical, electrical and electrochemical properties are investigated. The electrical conductivity and thermoelectric power are measured in the temperature rang 300-600 K. The samples exhibit p-type behavior in contrast to TiO2. The doped-samples exhibit two optical transitions (2.35≤Eh-Vis(eV)≤2.55; 1.97≤El-Vis (eV)≤2.06) directly allowed in the visible region, while only one transition is observed in UV region (EUV∼3.00 eV). Pure TiO2 shows direct band gap transition of 3.17 eV. The results confirm experimentally the calculations of Di. Valentin et al. [42]. The transitions Eh-Vis and El-Vis are attributed respectively to the promotion of electrons from the localized N 2p and π* N-O bond to the conduction band. In all cases, EUV is associated to the forbidden band energy. Though that the conductivity is generally improved by doping process, only N0.05TiO2 and N0.1TiO2 shows an enhanced mobility. The mechanism of conduction takes place by small polaron hopping. The band edge positions of NxTiO2 (x=0, 0.05, 0.1, 0.2) at room temperature is predicted from the obtained physical properties. This study proves experimentally the principal role of nitrogen in doping process and permits the electronic states localization associated with N-impurities in TiO2 anatase.

  16. Effects of the sol-gel route on the structural characteristics and antibacterial activity of silica-encapsulated gentamicin.

    PubMed

    Corrêa, G G; Morais, E C; Brambilla, R; Bernardes, A A; Radtke, C; Dezen, D; Júnior, A V; Fronza, N; Santos, J H Z Dos

    2014-04-01

    The effects of sol-gel processes, i.e., acid-catalyzed gelation, base-catalyzed gelation and base-catalyzed precipitation routes, on the encapsulation of gentamicin were investigated. The resulting xerogels were characterized using a series of complementary instrumental techniques, i.e., the adsorption/desorption of nitrogen, small-angle X-ray scattering, Fourier transform infrared spectroscopy, diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy and scanning electron microscopy. The encapsulated gentamicin samples were tested against a series of Gram-positive and Gram-negative bacterial strains. The best antimicrobial activity was observed with the encapsulated gentamicin that was prepared via the precipitation route, even in comparison with the neat antibiotic, especially in the case of the Gram-positive strain Staphylococcus aureus. The gentamicin concentration on the outermost surface and the zeta potential were identified as factors that affected the highest efficiency, as observed in the case of encapsulation via the base-catalyzed process.

  17. Structural analysis of fluorine-containing bioactive glass nanoparticles synthesized by sol-gel route assisted by ultrasound energy.

    PubMed

    C Lins, Carolina E; R Oliveira, Agda A; Gonzalez, Ismael; A A Macedo, Waldemar; M Pereira, Marivalda

    2017-02-02

    In the last decades, studies about the specific effects of bioactive glass on remineralization of dentin were the focus of attention, due to their excellent regenerative properties in mineralized tissues. The incorporation of Fluorine in bioactive glass nanoparticles may result in the formation of fluorapatite (FAP), which is chemically more stable than hydroxyapatite or carbonated hydroxyapatite, and therefore is of interest for dental applications. The aim of this study was to synthesize and characterize a new system of Fluorine-containing bioactive glass nanoparticles (BGNPF). A sol-gel route assisted by ultrasound was used for the synthesis of BGNPF. The particles obtained were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), atomic force microscopy (AFM), X-ray diffraction (XRD), dynamic light scattering (DLS), nitrogen adsorption, and X-ray photoelectron spectroscopy (XPS). SEM micrographs showed that the particles are quite uniform spherical nanostructures, occurring agglomeration or partial sinterization of the particulate system after heat treatment. XRD and XPS analysis results suggest the formation of fluorapatite crystals embedded within the matrix of the bioactive glass nanoparticles. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2017.

  18. A new synthesis route to high surface area sol gel bioactive glass through alcohol washing: a preliminary study.

    PubMed

    Mukundan, Lakshmi M; Nirmal, Remya; Vaikkath, Dhanesh; Nair, Prabha D

    2013-01-01

    Bioactive glass is one of the widely used bone repair material due to its unique properties like osteoconductivity, osteoinductivity and biodegradability. In this study bioactive glass is prepared by the sol gel process and stabilized by a novel method that involves a solvent instead of the conventional calcinations process. This study represents the first attempt to use this method for the stabilization of bioactive glass. The bioactive glass stabilized by this ethanol washing process was characterized for its physicochemical and biomimetic property in comparison with similar composition of calcined bioactive glass. The compositional similarity of the two stabilized glass powders was confirmed by spectroscopic and thermogravimetric analysis. Other physicochemical characterizations together with the cell culture studies with L929 fibroblast cells and bone marrow mesenchymal stem cells proved that the stabilization was achieved with the retention of its inherent bioactive potential. However an increase in the surface area of the glass powder was obtained as a result of this ethanol washing process and this add up to the success of the study. Hence the present study exhibits a promising route for high surface area bioactive glass for increasing biomimicity.

  19. Low-temperature synthesis of SrAl{sub 2}O{sub 4} by a modified sol-gel route: XRD and Raman characterization

    SciTech Connect

    Escribano, Purificacion; Marchal, Monica; Luisa Sanjuan, Maria; Alonso-Gutierrez, Pablo; Julian, Beatriz; Cordoncillo, Eloisa . E-mail: cordonci@qio.uji.es

    2005-06-15

    Among other alkaline-earth aluminates, the monoclinic (M) polymorph of SrAl{sub 2}O{sub 4} can be used as host material for Eu{sup 2+} luminescence based phosphors. With the aim of reducing the synthesis temperature of this polymorph, we have produced and characterized by XRD and Raman scattering solid solutions of the SrAl{sub 2-x}B{sub x}O{sub 4} system (x=<0.3) obtained by two different methods, a ceramic route and a modified sol-gel synthesis. Though the addition of boron lowers the temperature of obtention of the M polymorph in both type of samples, lower B contents are needed to stabilize the M form as single phase for samples prepared by the sol-gel method than through the ceramic route. In the sol-gel method, the M polymorph can be obtained at temperatures as low as 1200 deg. C, with a Boron content of just 1%. Rietveld profile analysis allows us to conclude that coexistence of the monoclinic and hexagonal polymorphs of SrAl{sub 2}O{sub 4} occurs for samples synthesized below an onset temperature of about 1000-1100 deg. C, that depends on the sample composition. Above those temperatures, only the monoclinic phase is formed.

  20. Thin Films Derived by a Particulate Sol-Gel Route with Various Cr:Ti Molar Ratios

    NASA Astrophysics Data System (ADS)

    Mohammadi, M. R.; Fray, D. J.

    2014-11-01

    Nanocrystalline and nanostructured TiO2-Cr2O3 thin films and powders were prepared by a facile and straightforward aqueous particulate sol-gel route at low temperature of 400°C. The prepared sols showed a narrow particle size distribution with hydrodynamic diameter in the range of 17.7 nm to 19.0 nm. Moreover, the sols were stable over 4 months, with constant zeta potential measured during this period. The effect of the Cr:Ti molar ratio on the crystallization behavior of the products was studied. X-ray diffraction (XRD) analysis revealed that the powders crystallized at low temperature of 400°C, containing anatase-TiO2, rutile-TiO2, and Cr2O3 phases, depending on the annealing temperature and Cr:Ti molar ratio. Furthermore, it was found that Cr2O3 retarded the anatase to rutile transformation up to 800°C. The activation energy of crystallite growth was calculated to be in the range of 1.3 kJ/mol to 2.9 kJ/mol. Transmission electron microscopy (TEM) imaging showed that one of the smallest crystallite sizes was obtained for TiO2-Cr2O3 binary mixed oxide, being 5 nm at 500°C. Field-emission scanning electron microscopy (FESEM) analysis revealed that the deposited thin films had nanostructured morphology with average grain size in the range of 20 nm to 40 nm at 500°C. Thin films produced under optimized conditions showed excellent microstructural properties for gas sensing applications. They exhibited a remarkable response towards low concentrations of NO2 gas at low operating temperature of 200°C, resulting in increased thermal stability of sensing films as well as a decrease in their power consumption. Furthermore, calibration curves revealed that TiO2-Cr2O3 sensors followed the power law (where S is the sensor response, the coefficients A and B are constants, and [gas] is the gas concentration) for two types of gas, exhibiting excellent capability for detection of low gas concentrations.

  1. The sol-gel route: A versatile process for up-scaling the fabrication of gas-tight thin electrolyte layers

    NASA Astrophysics Data System (ADS)

    Viazzi, Céline; Rouessac, Vincent; Lenormand, Pascal; Julbe, Anne; Ansart, Florence; Guizard, Christian

    2011-03-01

    Sol-gel routes are often investigated and adapted to prepare, by suitable chemical modifications, submicronic powders and derived materials with controlled morphology, which cannot be obtained by conventional solid state chemistry paths. Wet chemistry methods provide attractive alternative routes because mixing of species occurs at the atomic scale. In this paper, ultrafine powders were prepared by a novel synthesis method based on the sol-gel process and were dispersed into suspensions before processing. This paper presents new developments for the preparation of functional materials like yttria-stabilized-zirconia (YSZ, 8% Y2O3) used as electrolyte for solid oxide fuel cells. YSZ thick films were coated onto porous Ni-YSZ substrates using a suspension with an optimized formulation deposited by either a dip-coating or a spin-coating process. The suspension composition is based on YSZ particles encapsulated by a zirconium alkoxide which was added with an alkoxide derived colloidal sol. The in situ growth of these colloids increases significantly the layer density after an appropriated heat treatment. The derived films were continuous, homogeneous and around 20 μm thick. The possible up-scaling of this process has been also considered and the suitable processing parameters were defined in order to obtain, at an industrial scale, homogeneous, crack-free, thick and adherent films after heat treatment at 1400 °C.

  2. Gravure-Printed Sol-Gels on Flexible Glass: A Scalable Route to Additively Patterned Transparent Conductors.

    PubMed

    Scheideler, William J; Jang, Jaewon; Ul Karim, Muhammed Ahosan; Kitsomboonloha, Rungrot; Zeumault, Andre; Subramanian, Vivek

    2015-06-17

    Gravure printing is an attractive technique for patterning high-resolution features (<5 μm) at high speeds (>1 m/s), but its electronic applications have largely been limited to depositing nanoparticle inks and polymer solutions on plastic. Here, we extend the scope of gravure to a new class of materials and on to new substrates by developing viscous sol-gel precursors for printing fine lines and films of leading transparent conducting oxides (TCOs) on flexible glass. We explore two strategies for controlling sol-gel rheology: tuning the precursor concentration and tuning the content of viscous stabilizing agents. The sol-gel chemistries studied yield printable inks with viscosities of 20-160 cP. The morphology of printed lines of antimony-doped tin oxide (ATO) and tin-doped indium oxide (ITO) is studied as a function of ink formulation for lines as narrow as 35 μm, showing that concentrated inks form thicker lines with smoother edge morphologies. The electrical and optical properties of printed TCOs are characterized as a function of ink formulation and printed film thickness. XRD studies were also performed to understand the dependence of electrical performance on ink composition. Printed ITO lines and films achieve sheet resistance (Rs) as low as 200 and 100 Ω/□, respectively (ρ≈2×10(-3) Ω-cm) for single layers. Similarly, ATO lines and films have Rs as low as 700 and 400 Ω/□ with ρ≈7×10(-3) Ω-cm. High visible range transparency is observed for ITO (86-88%) and ATO (86-89%). Finally, the influence of moderate bending stress on ATO films is investigated, showing the potential for this work to scale to roll-to-roll (R2R) systems.

  3. Optical properties of undoped and Mg doped CuCrO{sub 2} powders synthesized by sol-gel route

    SciTech Connect

    Srinivasan, Radhakrishnan; Bolloju, Satish

    2014-01-28

    In this work, CuCrO{sub 2} was synthesized by sol-gel method using citric acid as a gelling agent. The different parameters like ratio of citric acid to metal ions, calcination temperature, and duration were studied. A green colored powder with particle size around 300 nm was formed at the calcination temperature of 800 °C for four hours duration. The increase in temperature has a profound impact on crystallite size and in turn effected the optical properties. Band gap of the obtained CuCrO{sub 2} has varied from 2.3 to 1.7 eV by increasing the temperature from 800 °C to 900 °C. Doping studies were performed by introducing Mg{sup 2+} ion to substitute Cr{sup 3+} in CuCrO{sub 2}. X-ray powder diffraction and SEM studies on 2% Mg doped samples indicated a clear formation of side phases. According to the X-ray powder patterns, the reflections from side phases were increasing with the increase in doping concentrations of Mg from 2 to 5%. The side phases were found to be MgCr{sub 2}O{sub 4} spinel and CuO. The band gap has decreased for doped samples in comparison to undoped one. In this paper, sol-gel synthesis and characterization by Xray powder diffraction, SEM studies and UV-Vis-Diffuse Reflectance spectra are presented.

  4. Structural, Optical and Magnetic Properties of Nickel-Silica Nanocomposite Prepared by a Sol-Gel Route

    NASA Astrophysics Data System (ADS)

    Saha, Mrinal; Soumya Mukherjee; Gayen, Arup; Siddhartha Mukherjee

    2015-10-01

    Nickel-silica nanocomposites have been synthesized by a sol-gel method using dextrose (C6H12O6) as the reducing agent. The dried gel is heat treated at 850 and 900 °C for 30 min in an inert atmosphere by N2 purging to obtain the composite material. The samples have been characterized by powder X-ray diffraction, field emission scanning electron microscopy, atomic force microscopy, transmission electron microscopy and selected area electron diffraction. Pure polycrystalline nickel granular particle has been found to form with face-centered cubic structure and is entrapped in amorphous silica matrix with particle sizes in between 10 and 30 nm and is almost spherical in shape. The strong ferromagnetic nature of Ni-SiO2 composite became evident from the M-H curve which is quite different from the bulk nickel. The band gap of the synthesized Ni-SiO2 nanocomposite is found to be 2.35 eV. The reported sol-gel technique is a convenient and effective method to prepare high purity nanopowders with uniform size distribution.

  5. Rh6G released from solid and nanoporous SiO2 spheres prepared by sol-gel route

    NASA Astrophysics Data System (ADS)

    García-Macedo, J. A.; Francisco S., P.; Franco, A.

    2015-10-01

    Porous silica nanoparticles are considering good systems for drug cargo and liquid separation. In this work we studied the release of rhodamine 6G (Rh6G) from solid and porous silica nanoparticles. Solid and porous SiO2 spheres were prepared by sol-gel method. Nanoporous channels were produced by using a surfactant that was removed by chemical procedure. Rh6G was incorporated into the channels by impregnation. The hexagonal structure of the pores was detected by XRD and confirmed by HRTEM micrographs. Rh6G released from the particles by stirring them in water at controlled speed was studied as function of time by photoluminescence. Released ratio was faster in the solid nanoparticles than in the porous ones. In the last case, a second release mechanism was observed. It was related with rhodamine coming out from the porous.

  6. Structural and cyclic volta metric investigations on BIPBVOX solid electrolyte synthesized by ethylene glycol-citric acid sol-gel route

    NASA Astrophysics Data System (ADS)

    Naqvi, Faria K.; Beg, Saba; Al-Areqi, Niyazi A. S.

    2016-05-01

    Samples of BIPBVOX.x (Bi2V1-xPbxO5.5-x/2) in the composition range 0.05 ≤ x ≤ 0.20 were prepared by ethylene glycol- citric acid sol-gel synthesis route. Structural investigations were carried out by X-ray diffraction, DTA. The highly conducting γ'- phase was effectively stabilized at room temperature for compositions with x ≥ 0.17. Cyclic voltammetric measurements showed reversible redox reactions of vanadium and irreversible redox reaction of Bi3+ in the BIPBVOX system during the first cathodic and anodic sweep. However, a higher stability against the reduction of Bi3+ to metallic bismuth was seen for x=0.20.

  7. Synthesis of mesoporous silica-alumina materials via urea-templated sol-gel route and their catalytic performance for THF polymerization

    NASA Astrophysics Data System (ADS)

    Ge, Yuanyuan; Jia, Zhiqi; Gao, Chunguang; Gao, Pengfei; Zhao, Lili; Zhao, Yongxiang

    2014-10-01

    A series of mesoporous silica-alumina materials was successfully synthesized by using urea as a low-cost template via sol-gel routes. The characterization results showed that the employ of urea enhanced the porosity of the silica-alumina materials and made the pore size distributions become narrower. The specific surface area, pore volume and pore diameter of SAU-X firstly increased and then decreased as the urea concentration increased from 0 to 60 wt %, and the maximums were obtained at 40 wt % urea concentration. All samples were tested for the THF polymerization. Among them, SAU-40 exhibited the highest activity and the longest catalyst life due to its superior porosity.

  8. Controlled synthesis of highly ordered LaFeO{sub 3} nanowires using a citrate-based sol-gel route

    SciTech Connect

    Yang Zhi; Huang Yi; Dong Bin; Li Hulin . E-mail: lihl@lzu.edu.cn

    2006-02-02

    Highly ordered LaFeO{sub 3} nanowires of complex oxide were controlled synthesized with a porous anodic aluminum oxide (AAO) template by a citrate-based sol-gel route. The results of scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed that the LaFeO{sub 3} nanowires formed a uniform length and diameter, which were determined by the thickness and the pore diameter of the AAO template, respectively. The results of X-ray diffraction (XRD) and the selected area electron diffraction (SAED) indicated that the LaFeO{sub 3} nanowires had a perovskite-type crystal structure. Furthermore, X-ray photoelectron spectroscopy (XPS) demonstrated that stoichiometric LaFeO{sub 3} was formed.

  9. Synthesis of CdS/CdSe core/shell ultra small nanostructures using new microwave assisted ultrasonic sol gel route

    SciTech Connect

    Goswami, Y. C. Kumar, Vijay; Sharma, Ranjana; Singh, Rajeev

    2014-04-24

    Core-shell CdS/CdSe nanostructures have been synthesized by new microwave assisted ultrasonic sol gel route. The solution was obtained by dissolving cadmium acetate and Thiourea in the molar ratio 1:1 in Triethlioamine. The solution was Ultrasonically irradiated by Ultrasonic crystal at 40 Hz for 3 hours at 70°C. The sol was kept for another 24 hours for gel formation. Selenium dioxide was used as a selenium source and added separately. The gel was spin coated on Quartz and Glass slides followed by microwave heat treatment. The samples were characterized by structural morphological and optical characterization. XRD studies confirm the zinc blende phase of the CdS nanoparticles. The mean nanocrystal sizes calculated using Scherrer equation is ∼1.2nm. Optical studies show the strong blue shift in the spectra due to very small size of the nanocrystals. TEM and HRTEM confirm the formation of core shell structures.

  10. Structural, optical and morphological analyses of pristine titanium di-oxide nanoparticles--synthesized via sol-gel route.

    PubMed

    Praveen, P; Viruthagiri, G; Mugundan, S; Shanmugam, N

    2014-01-03

    Pure titanium di-oxide nanoparticles (TiO2) were synthesized by sol-gel technique at room temperature with appropriate reactants. The synthesis of anatase phase TiO2 nanoparticles was achieved by tetraisopropyl orthotitanate and 2-propanol as common starting materials and the product was annealed at 450 °C for 4 h. The synthesized product was characterized by X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR), UV-VIS-Diffuse reflectance spectroscopy (DRS), Photoluminescence (PL) spectroscopy and Scanning electron microscopy (SEM) with Energy dispersive X-ray (EDX) analysis. XRD pattern confirmed the crystalline nature and tetragonal structure of synthesized composition. Average grain size was determined from X-ray line broadening, using the Debye-Scherrer relation. The functional groups present in the sample were identified by FTIR spectroscopy. Diffuse reflectance measurement indicated an absorption band edge on UV-region. The allowed direct and indirect band gap energies, as well as the crystallite size of pure TiO2 nanoparticles are calculated from DRS analysis. The microstructure and elemental identification were done by SEM with EDX analysis.

  11. Development of injectable biocomposites from hyaluronic acid and bioactive glass nano-particles obtained from different sol-gel routes.

    PubMed

    Sohrabi, Mehri; Hesaraki, Saeed; Kazemzadeh, Asghar; Alizadeh, Masoud

    2013-10-01

    Bioactive glass nano-powders with the same chemical composition and different particle characteristics were synthesized by acid-catalyzed (the glass is called BG1) and acid-base catalyzed (BG2) sol-gel processes. Morphological characteristics of powders were determined by TEM and BET methods. The powders were separately mixed with 3% hyaluronic acid solution to form a paste. In vitro reactivity of pastes was determined by soaking them in simulated body fluid. Rheological behaviors of paste in both rotation and oscillation modes were also measured. The results showed that BG1 particles was microporous with mean pore diameter of 1.6 nm and particle size of ~300 nm while BG2 was mesoporous with average pore diameter of 8 and 17 nm and particle size of 20-30 nm. The paste made of BG2 revealed better washout resistance and in vitro apatite formation ability than BG1. According to the rheological evaluations, both pastes exhibited shear thinning but non-thixotropic behavior, meanwhile paste of BG2 had higher viscosity than BG1. The oscillatory tests revealed that the pastes were viscoelastic materials with more viscous nature. Both pastes could be completely injected through standard syringe using low compressive load of 5-50 N. Overall, The biocomposites can potentially be used as bioactive paste for the treatment of hard and even soft tissues.

  12. Hydroxyapatite and fluor-hydroxyapatite layered film on titanium processed by a sol-gel route for hard-tissue implants.

    PubMed

    Kim, Hae-Won; Knowles, Jonathan C; Salih, Vehid; Kim, Hyoun-Ee

    2004-10-15

    A double-layered coating, consisting of a hydroxyapatite (HA) outer film and a fluor-hydroxyapatite (FHA) inner film, was produced on a Ti substrate by a sol-gel route to improve the biocompatibility and functionality of the system. Dissolution behavior of and in vitro cellular responses to the layered film were investigated. Calcium nitrate and triethyl phosphite were used for calcium and phosphate precursors, respectively, and ammonium fluoride was added as a fluorine-ion source for FHA. The FHA layer was deposited on Ti by spin coating and subsequent heat treatment at 550 degrees C for 30 min in air, and then the HA layer was laid down over the FHA-coated Ti under the same conditions. After heat treatment, characteristic apatite structures and phases were developed on both FHA and HA films. The cross-section view of the HA/FHA film clearly showed a double-layered structure on Ti with each layer approximately 0.6-0.8-microm thickness. The coating layer was highly uniform and dense, and adhered to Ti substrate strongly with an adhesion strength of about 40 MPa. The in vitro solubility of the HA/FHA layered film in a physiological solution was between that of HA and FHA pure film, and the dissolution profile was quite biphasic, that is, an initial rapid period and a slowdown with increasing time, reflecting the gradient solubility of the fast HA outer structure/slow FHA inner structure. The human osteoblast-like HOS TE85 cells cultured on the HA/FHA layered film attached, spread, and grew favorably. The proliferation rate of the cells on the layered film was significantly higher (considered at p < 0.05 for n = 6) than that on Ti substrate and was similar to that on pure HA film. The alkaline phosphatase (ALP) activity and osteocalcin (OC) produced by the cells on the layered film were significantly higher (considered at p < 0.05 for n = 6) than those on Ti substrate. Moreover, the ALP and OC levels of cells on the layered film showed the trends of HA outer

  13. Magnetic, electrical, and microstructural properties of YBa2Cu3O7 - A comparison of sol-gel, co-precipitated, and solid state processing routes

    NASA Astrophysics Data System (ADS)

    Hayri, E. A.; Greenblatt, M.; Ramanujachary, K. V.; Nagano, M.; Oliver, J.

    1989-10-01

    Samples of YBa2Cu3O7 were prepared by sol-gel, co-precipitation, and solid state processes. Sol-gel samples were prepared from a solution of yttrium, barium, and copper nitrates dissolved in ethylene glycol, co-precipitated samples were made by the amorphous citrate method, and solid state samples were prepared by conventional high temperature reaction of the appropriate metal oxides and carbonates. The sol-gel process was shown to yield superconducting samples of superior Meissner effect, critical current, and critical field. The co-precipitated samples contain impurities that affect the critical properties. The sol-gel and co-precipitated processes yield materials with well-formed, plate-like particles with a fairly uniform size of about 10 microns. The grains in the solid state sample are smaller but have a much wider distribution of sizes than the samples prepared by solution methods.

  14. Thin films of calcium phosphate and titanium dioxide by a sol-gel route: a new method for coating medical implants.

    PubMed

    Piveteau, L D; Girona, M I; Schlapbach, L; Barboux, P; Boilot, J P; Gasser, B

    1999-03-01

    Titanium is a commonly used biomaterial for dental and orthopaedic applications. To increase its ability to bond with bone, some attempts were made to coat its surface with calcium phosphate (CaP). This paper describes a new type of coating. Instead of a pure CaP layer, a mixing of titanium dioxide (TIO2) and CaP is fabricated and deposited as a coating. These layers are deposited by a sol-gel route on pure titanium substrates using various pre-treatments. The method consists of mixing a solution of tetrabutyl ortho-titanate or a sol of titanium dioxide with a solution of calcium nitrate and phosphorous esters. This composite is deposited on to commercially pure titanium plates, mechanically polished or blasted with pure crystalline aluminum oxide, using the spin-coating technique. These coatings are then fired at 650 or 850 degrees C for various times. The samples are characterized by X-ray diffraction for their crystallinity, X-ray photoelectron spectroscopy for their surface chemical composition and scanning electron microscopy for their topography. Samples treated at 850 degrees C present a well-pronounced crystallinity, and a high chemical purity at the surface. The topography is strongly related to the viscosity of the precursor and the substrate pre-treatment. Possibilities to structure the outermost layer are presented.

  15. Effect of annealing on the structural and optical properties of TiO2 powder prepared by sol-gel route

    NASA Astrophysics Data System (ADS)

    Halder, Nilanjan; Misra, Kamakhya Prakash

    2016-05-01

    Using titanium isopropoxide as the precursor, Titanium dioxide (TiO2) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO2 samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increase with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO2 nano powder samples.

  16. Structural and magnetic properties of pure and Ca-doped LaCoO3 nanopowders obtained by a sol-gel route.

    PubMed

    Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Maragno, Cinzia; Tondello, Eugenio; Caneschi, Andrea; Sangregorio, Claudio; Gialanella, Stefano

    2006-04-01

    Pure and Ca-doped LaCoO3 nanopowders were prepared by a non-alkoxidic sol-gel route using cobalt(II) acetate, lanthanum(III) nitrate and calcium(II) acetate as oxide precursors. The structural evolution and magnetic properties of the samples were studied as a function of thermal treatments in air up to 1273 K. In particular, the microstructure and composition of the systems were analyzed by X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), and X-ray Photoelectron Spectroscopy (XPS). Both pure and calcium-doped samples annealing at 973 K resulted in the formation of cubic LaCoO3 (average crystallite size <30 nm). This phase was fully retained in the calcium-doped materials even after annealing at higher temperatures, whereas a transition to the rhomboedral polymorph was detected in the pure samples at 1073 K. The magnetic behavior of the nanopowders was investigated as a function of temperature and applied field using both dynamic and static susceptibility measurements. Pure lanthanum cobaltite samples underwent a transition to an ordered state at 88 K, and their magnetic properties changed as a function of thermal treatments. As concerns calcium-doped samples, they ordered ferromagnetically at 171 and 185 K depending on the annealing temperature and displayed open hysteresis loops with coercive fields as large as 1.75 T at low temperatures.

  17. A simple route utilizing surfactant-assisted templating sol-gel process for synthesis of mesoporous Dy2O3 nanocrystal.

    PubMed

    Sreethawong, Thammanoon; Chavadej, Sumaeth; Ngamsinlapasathian, Supachai; Yoshikawa, Susumu

    2006-08-01

    A simple route of combined sol-gel process with surfactant-assisted templating technique was successfully employed for the first time to synthesize nanocrystalline mesoporous Dy(2)O(3) with narrow monomodal pore size distribution under mild conditions. The nanocrystalline Dy(2)O(3) with monomodal mesoporous characteristic was ultimately achieved by controlling the hydrolysis and condensation steps of dysprosium n-butoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution. The synthesized material was methodically characterized by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), N(2) adsorption-desorption, Brunauer-Emmett-Teller (BET) surface area analysis, and Barrett-Joyner-Halenda (BJH) pore size distribution analysis. The particle size of the synthesized Dy(2)O(3) in nanosized range obtained from the SEM and HRTEM micrographs was in good accordance with the crystallite size estimated from the XRD result. The N(2) adsorption-desorption result exhibited hysteresis pattern with single loop, indicating the existence of monomodal mesopore. The extremely narrow pore size distribution with mean pore diameter in the mesopore region of the synthesized Dy(2)O(3) was also confirmed by the BJH result.

  18. Ultra-high specific capacitance of β-Ni(OH)2 monolayer nanosheets synthesized by an exfoliation-free sol-gel route

    NASA Astrophysics Data System (ADS)

    Cui, Hongtao; Xue, Junying; Ren, Wanzhong; Wang, Minmin

    2014-09-01

    In this work, β-Ni(OH)2 monolayer nanosheets were prepared in benzyl alcohol by a facile exfoliation-free sol-gel route. The hydrolysis reaction of metal ions was started with the ring-opening reaction of epoxide. The in situ modification of benzyl alcohol molecules on the surface of secondary growth unit of hydroxide allowed the formation of β-Ni(OH)2 monolayer nanosheets and 100 % monolayer state of β-Ni(OH)2 in the resultant suspension. As proven in the electrochemical measurement, the maximum specific capacitance of 1735 F g-1 was obtained at scan rate of 5 mV s-1 within potential window of 0.6 V in 6 mol l-1 KOH aqueous solution, which is equal to the theoretical value of β-Ni(OH)2. This high electrochemical performance is attributed to the complete exposure of every structure unit of β-Ni(OH)2 to electrolyte. This work demonstrates that monolayer nanosheets can generate from the brucite-type nickel hydroxide through this bottom-up strategy although it had been theoretically considered to be impossible.

  19. Nanocrystal/sol-gel nanocomposites

    DOEpatents

    Petruska, Melissa A.; Klimov, Victor L.

    2007-06-05

    The present invention is directed to solid composites including colloidal nanocrystals within a sol-gel host or matrix and to processes of forming such solid composites. The present invention is further directed to alcohol soluble colloidal nanocrystals useful in formation of sol-gel based solid composites.

  20. Nanocrystal/sol-gel nanocomposites

    SciTech Connect

    Petruska, Melissa A; Klimov, Victor L

    2012-06-12

    The present invention is directed to solid composites including colloidal nanocrystals within a sol-gel host or matrix and to processes of forming such solid composites. The present invention is further directed to alcohol soluble colloidal nanocrystals useful in formation of sol-gel based solid composites

  1. Gradient Index Lenses From Sol-Gel Layering.

    DTIC Science & Technology

    2008-02-15

    AND SJu ’ jL SGFRADIENT INDEX LENSES FROM SOL - GEL LAYERING F49620-93-1-0364 3484/XS 6. AU1CqQ(s) ) 61103D Dr John D. Mackenzie 4 7. PE’r~Of;M1!?𔃽...applied U to the sol -ge•l process. The sol - gel process has been widely studied in the Uj recent past, as it is an interesting alte’rnative chemical route...REPORT to Air Force Office of Scientific Research for project entitled GRADIENT INDEX LENSES FROM SOL - GEL LAYERING (An AASERT Award) Grant No.: AFOSR

  2. Structural and optical properties of ZnO: K synthesized by sol-gel auto-combustion route

    SciTech Connect

    Krithiga, R. Sankar, S.; Subhashree, G.; Bharathi, R. Niruban

    2015-06-24

    The structural and optical behavior of ZnO and ZnO doped with K synthesized by solution combustion route is reported in this article. The XRD patterns confirm the substitution of K atoms into ZnO lattice. There are no secondary peaks observed in the XRD patterns. The band gap of the K doped samples show a red shift on comparison with the bandgap of ZnO. The photoluminescence spectral study discloses the quenching behavior of UV emission and the aggrandizing blue emission when K content increases. The rich presence of defects is confirmed from the optical analysis and a practical mechanism, involving Zn{sub i} for the origin of the blue emission in ZnO is discussed here.

  3. Low temperature nanocrystalline TiO2-Fe2O3 mixed oxide by a particulate sol-gel route: Physical and sensing characteristics

    NASA Astrophysics Data System (ADS)

    Mohammadi, M. R.; Fray, D. J.

    2012-09-01

    Nanocrystalline TiO2-Fe2O3 thin films and powders were prepared by a straightforward aqueous particulate sol-gel route at the low temperature of 300 °C. Titanium(IV) isopropoxide and iron(III) chloride were used as precursors, and hydroxypropyl cellulose was used as a polymeric fugitive agent in order to increase the specific surface area. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) revealed that the powder crystallised at the low temperature of 300 °C, containing anatase-TiO2 and hematite-Fe2O3 phases. Furthermore, it was found that Fe2O3 retarded the anatase-to-rutile transformation up to 500 °C. The activation energies for crystallite growth of TiO2 and Fe2O3 components in the binary system were calculated 10.62 and 0.67 kJ/mol, respectively. Moreover, one of the smallest crystallite sizes was obtained for TiO2-Fe2O3 binary mixed oxide, being 6 nm at 300 °C. Field emission scanning electron microscope (FE-SEM) analysis revealed that the deposited thin films had nanostructured morphology. Thin films produced under optimized conditions showed excellent microstructural properties for gas sensing applications. They exhibited a remarkable response towards low concentrations of CO gas (i.e., 25 ppm) at low operating temperature of 150 °C, resulting in increased thermal stability of sensing films as well as a decrease in their power consumption. Furthermore, TiO2-Fe2O3 sensors follow the power law for the detection of CO gas.

  4. An efficient adsorption of indigo carmine dye from aqueous solution on mesoporous Mg/Fe layered double hydroxide nanoparticles prepared by controlled sol-gel route.

    PubMed

    Ahmed, M A; Brick, A A; Mohamed, A A

    2017-05-01

    A new approach for removal of indigo carmine blue (IC) dye which is extensively used in jeans manufacture was successfully performed on novel mesoporous [LDH] nanoparticles prepared by sol-gel route using CTAB as shape and pore directing agent. The physicochemical features were monitored by X-ray diffraction (XRD), Fourier transformer infra-red (FTIR), N2 adsorption-desorption isotherm, Field emission electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). The influence of reaction parameters affecting dye adsorption including contact time, initial dye concentration, pH and temperature were investigated. Textural analysis and HRTEM images indicate the existence of mesoporous spherical nanoparticles of size = 26 nm connected to each other's and embedded large numbers of mesopores of average pore radius = 43.5 Å. A successful adsorption of IC on LDH nanoparticles of surface area = 85.6 m(2)/g at various pH with maximum adsorption capacity = 62.8 mg/g at pH = 9.5. Langmuir model is more favorable to describe the adsorption of IC rather than Freundlich model which reflecting the preferential formation of monolayer on the surface of LDH. Both film diffusion and the intraparticle diffusion affect the dye adsorption. The values of enthalpy change (ΔH) for and (ΔS) are + 28.18 and + 0.118 kJ/mol, respectively indicating that the removal process is endothermic. The results indicated that LDH nanoparticles conserved a good activity even after five consecutive cycles of reuse. Our results suggest that mesoporous LDH nanoparticles are considered a potential novel adsorbent for remediation of wastewater containing IC.

  5. The Microscopic Magnetic Properties of W-type Hexaferrite Powder Prepared by A Sol-Gel Route

    SciTech Connect

    Jotania, Rajshree; Chauhan, Chetna; Sharma, Pooja

    2010-12-01

    Magnetic particles of W-type barium-calcium hexaferrite (BaCa{sub 2}Fe{sub 16}O{sub 27}) have been synthesized using a Stearic acid gel route. The gel precursors were dried at 100 deg. C for 2 hrs and then calcinated at 650 deg. C, 750 deg. C, 850 deg. C and 950 deg. C for 4 hrs in a furnace and slowly cooled to room temperature in order to obtain barium-calcium hexaferrite particles. The microscopic magnetic properties of prepared samples studying using Moessbauer spectroscopy. Moessbauer spectra of all samples were recorded at room temperature. Mossbauer parameters like Isomer shift, Quadruple splitting etc. were calculated with respect to iron foil. Barium calcium hexaferrite samples heated at 650 deg. C, 750 deg. C, 850 deg. C show relaxation type Moessbauer spectra along with paramagnetic doublet. The intensity of paramagnetic doublet increases with temperature confirm the presence of ferrous ions in the samples, where as sample calcinated at 950 deg. C confirm the presence of ferrimagnetic phase with partial super paramagnetic nature of prepared hexaferrite sample.

  6. Sol-gel chemistry-based Ucon-coated columns for capillary electrophoresis.

    PubMed

    Hayes, J D; Malik, A

    1997-07-18

    A sol-gel chemistry-based novel approach for the preparation of a Ucon-coated fused-silica capillary column in capillary electrophoresis is presented. In this approach the sol-gel process is carried out inside 25 microm I.D. fused-silica capillaries. The sol solution contained appropriate quantities of an alkoxide-based sol-gel precursor, a polymeric coating material (Ucon), a crosslinking reagent, a surface derivatizing reagent, controlled amounts of water and a catalyst dissolved in a suitable solvent system. The coating procedure involves filling a capillary with the sol solution and allowing the sol-gel process to proceed for an optimum period. Hydrolysis of the alkoxide precursor and polycondensation of the hydrolyzed products with the surface silanol groups and the hydroxy-terminated Ucon molecules lead to the formation of a surface-bonded sol-gel coating on the inner walls of the capillary. The thickness of the coated film can be controlled by varying the reaction time, coating solution composition and experimental conditions. Commercial availability of high purity sol-gel precursors (e.g., TEOS 99.999%), the ease of coating, run-to-run and column-to-column reproducibility, and long column lifetimes make sol-gel coating chemistry very much suitable for being applied in analytical microseparations column technology. Test samples of basic proteins and nucleotides were used to evaluate the column performance. These results show that the sol-gel coating scheme has allowed for the generation of bio-compatible surfaces characterized by high separation efficiencies in CE. For different types of solutes, the sol-gel coated Ucon column consistently provided migration time R.S.D. values of the order of 0.5%.

  7. Bioactive glass-ceramic coatings prepared by pulsed laser deposition from RKKP targets (sol-gel vs melt-processing route)

    SciTech Connect

    Rau, J.V.; Teghil, R.; Fosca, M.; De Bonis, A.; Cacciotti, I.; Bianco, A.; Albertini, V. Rossi; Caminiti, R.; Ravaglioli, A.

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer Bioactive glass-ceramic coatings for bone tissue repair and regeneration. Black-Right-Pointing-Pointer Pulsed Lased Deposition allowed congruent transfer of target composition to coating. Black-Right-Pointing-Pointer Target was prepared by sol-gel process suitable for compositional tailoring. Black-Right-Pointing-Pointer Titanium, widely used for orthopaedics and dental implants, was used as substrate. Black-Right-Pointing-Pointer The physico-chemical properties of the prepared coatings are reported. -- Abstract: The deposition of innovative glass-ceramic composition (i.e. RKKP) coatings by Pulsed Lased Deposition (PLD) technique is reported. RKKP was synthesised following two methodologies: melt-processing and sol-gel, the latter being particularly suitable to tailor the compositional range. The PLD advantage with respect to other deposition techniques is the congruent transfer of the target composition to the coating. The physico-chemical properties of films were investigated by Scanning Electron and Atomic Force Microscopies, Fourier Transform Infrared Spectroscopy, Angular and Energy Dispersive X-ray Diffraction, and Vickers microhardness. The deposition performed at 12 J/cm{sup 2} and 500 Degree-Sign C allows to prepare crystalline films with the composition that replicates rather well that of the initial targets. The 0.6 {mu}m thin melt-processing RKKP films, possessing the hardness of 25 GPa, and the 4.3 {mu}m thick sol-gel films with the hardness of 17 GPa were obtained.

  8. Sol-gel derived sorbents

    DOEpatents

    Sigman, Michael E.; Dindal, Amy B.

    2003-11-11

    Described is a method for producing copolymerized sol-gel derived sorbent particles for the production of copolymerized sol-gel derived sorbent material. The method for producing copolymerized sol-gel derived sorbent particles comprises adding a basic solution to an aqueous metal alkoxide mixture for a pH.ltoreq.8 to hydrolyze the metal alkoxides. Then, allowing the mixture to react at room temperature for a precalculated period of time for the mixture to undergo an increased in viscosity to obtain a desired pore size and surface area. The copolymerized mixture is then added to an immiscible, nonpolar solvent that has been heated to a sufficient temperature wherein the copolymerized mixture forms a solid upon the addition. The solid is recovered from the mixture, and is ready for use in an active sampling trap or activated for use in a passive sampling trap.

  9. Novel route for rapid sol-gel synthesis of hydroxyapatite, avoiding ageing and using fast drying with a 50-fold to 200-fold reduction in process time.

    PubMed

    Ben-Arfa, Basam A E; Salvado, Isabel M Miranda; Ferreira, José M F; Pullar, Robert C

    2017-01-01

    We have developed an innovative, rapid sol-gel method of producing hydroxyapatite nanopowders that avoids the conventional lengthy ageing and drying processes (over a week), being 200 times quicker in comparison to conventional aqueous sol-gel preparation, and 50 times quicker than ethanol based sol-gel synthesis. Two different sets of experimental conditions, in terms of pH value (5.5 and 7.5), synthesis temperature (45 and 90°C), drying temperature (60 and 80°C) and calcination temperature (400 and 700°C) were explored. The products were characterised by X-ray diffraction (XRD) Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and specific surface area (SSA) measurements. Pure hydroxyapatite (Ca10(PO4)6(OH)2, HAp) was obtained for the powders synthesised at pH7.5 and calcined at 400°C, while biphasic mixtures of HAp/β-tricalcium phosphate (β-Ca3(PO4)2, TCP) were produced at pH5.5 and (pH7.5 at elevated temperature). The novel rapid drying was up to 200 times faster than conventional drying, only needing 1h with no prior ageing step, and favoured the formation of smaller/finer nanopowders, while producing pure HAp or phase mixtures virtually identical to those obtained from the slow conventional drying method, despite the absence of a slow ageing process. The products of this novel rapid process were actually shown to have smaller crystallite sizes and larger SSA, which should result in increased bioactivity.

  10. Nanocrystal/sol-gel nanocomposites

    DOEpatents

    Klimov, Victor L.; Petruska, Melissa A.

    2010-05-25

    The present invention is directed to a process for preparing a solid composite having colloidal nanocrystals dispersed within a sol-gel matrix, the process including admixing colloidal nanocrystals with an amphiphilic polymer including hydrophilic groups selected from the group consisting of --COOH, --OH, --SO.sub.3H, --NH.sub.2, and --PO.sub.3H.sub.2 within a solvent to form an alcohol-soluble colloidal nanocrystal-polymer complex, admixing the alcohol-soluble colloidal nanocrystal-polymer complex and a sol-gel precursor material, and, forming the solid composite from the admixture. The present invention is also directed to the resultant solid composites and to the alcohol-soluble colloidal nanocrystal-polymer complexes.

  11. Sol-gel precursors and products thereof

    DOEpatents

    Warren, Scott C.; DiSalvo, Jr., Francis J.; Weisner, Ulrich B.

    2017-02-14

    The present invention provides a generalizable single-source sol-gel precursor capable of introducing a wide range of functionalities to metal oxides such as silica. The sol-gel precursor facilitates a one-molecule, one-step approach to the synthesis of metal-silica hybrids with combinations of biological, catalytic, magnetic, and optical functionalities. The single-source precursor also provides a flexible route for simultaneously incorporating functional species of many different types. The ligands employed for functionalizing the metal oxides are derived from a library of amino acids, hydroxy acids, or peptides and a silicon alkoxide, allowing many biological functionalities to be built into silica hybrids. The ligands can coordinate with a wide range of metals via a carboxylic acid, thereby allowing direct incorporation of inorganic functionalities from across the periodic table. Using the single-source precursor a wide range of functionalized nanostructures such as monolith structures, mesostructures, multiple metal gradient mesostructures and Stober-type nanoparticles can be synthesized. ##STR00001##

  12. Metal-silica sol-gel materials

    NASA Technical Reports Server (NTRS)

    Stiegman, Albert E. (Inventor)

    2002-01-01

    The present invention relates to a single phase metal-silica sol-gel glass formed by the co-condensation of a transition metal with silicon atoms where the metal atoms are uniformly distributed within the sol-gel glass as individual metal centers. Any transition metal may be used in the sol-gel glasses. The present invention also relates to sensor materials where the sensor material is formed using the single phase metal-silica sol-gel glasses. The sensor materials may be in the form of a thin film or may be attached to an optical fiber. The present invention also relates to a method of sensing chemicals using the chemical sensors by monitoring the chromatic change of the metal-silica sol-gel glass when the chemical binds to the sensor. The present invention also relates to oxidation catalysts where a metal-silica sol-gel glass catalyzes the reaction. The present invention also relates to a method of performing oxidation reactions using the metal-silica sol-gel glasses. The present invention also relates to organopolymer metal-silica sol-gel composites where the pores of the metal-silica sol-gel glasses are filled with an organic polymer polymerized by the sol-gel glass.

  13. Molecular imprinting in sol-gel matrix.

    PubMed

    Gupta, Radha; Kumar, Ashok

    2008-01-01

    Molecular imprinting is a newly developed methodology which provides molecular assemblies of desired structures and properties and is being increasingly used for several applications such as in separation processes, microreactors, immunoassays and antibody mimics, catalysis, artificial enzymes, biosensor recognition elements and bio- and chemo-sensors. The ambient processing conditions and versatility of the sol-gel process makes sol-gel glassy matrix suitable for molecular imprinting. The progress of sol-gel based molecular imprinted polymers (MIPs) for various applications can be seen from the growing number of publications. The main focus of the review is molecular imprinting in sol-gel matrix and applications of molecular imprinted sol-gel derived materials for the development of sensors. Combining sol-gel process with molecular imprinting enables to procure the sensors with greater sensitivity and selectivity necessary for sensing applications. The merits, problems, challenges and factors affecting molecular imprinting in sol-gel matrix have been discussed. Considerable attention has been drawn on recent developments like use of organically modified silane precursors (ORMOSILS) for the synthesis of hybrid molecular imprinted polymers (HMIPs) and applying surface sol-gel process for molecular imprinting. The development of molecular imprinted sol-gel nanotubes for biochemical separation and bio-imprinting is a new advancement and is under progress. Templated xerogels and molecularly imprinted sol-gel films provide a good platform for various sensor applications.

  14. Synthesis of magnetic FexOy@silica-pillared clay (SPC) composites via a novel sol-gel route for controlled drug release and targeting.

    PubMed

    Mao, Huihui; Liu, Xiaoting; Yang, Jihe; Li, Baoshan; Yao, Chao; Kong, Yong

    2014-07-01

    Novel magnetic silica-pillared clay (SPC) materials with an ordered interlayered mesopore structure were synthesized via a two-step method including gallery molecular self-assembly and sol-gel magnetic functionalization, resulting in the formation of FexOy@SPC composites. Small-angle XRD, TEM and N2 adsorption-desorption isotherms results show that these composites conserved a regular layered and ordered mesoporous structure after the formation of FexOy nanoparticles. Wide-angle XRD and XPS analyses confirmed that the FexOy generated in these mesoporous silica-pillared clay hosts is mainly composed of γ-Fe2O3. Magnetic measurements reveal that these composites with different γ-Fe2O3 loading amounts possess super-paramagnetic properties at 300K, and the saturation magnetization increases with increasing Fe ratio loaded. Compared to the pure SPC, the in vitro drug release rate of the FexOy@SPC composites was enhanced due to the fact that the intensities of the SiOH bands on the pore surface of SPC decrease after the generation of FexOy. However, under an external magnetic field of 0.15T, the drug release rate of the FexOy@SPC composites decreases dramatically owing to the aggregation of the magnetic FexOy@SPC particles triggered by non-contact magnetic force. The obtained FexOy@SPC composites imply the possibility of application in magnetic drug targeting.

  15. Effect of synthesis route on electrical and ethanol sensing characteristics for LaFeO3-δ nanoparticles by citric sol-gel method

    NASA Astrophysics Data System (ADS)

    Cao, Ensi; Yang, Yuqing; Cui, Tingting; Zhang, Yongjia; Hao, Wentao; Sun, Li; Peng, Hua; Deng, Xiao

    2017-01-01

    LaFeO3-δ nanoparticles were prepared by citric sol-gel method with different raw material choosing and calcination process. The choosing of polyethylene glycol instead of ethylene glycol as raw material and additional pre-calcination at 400 °C rather than direct calcination at 600 °C could result in the decrease of resistance due to the reduction of activation energy Ea. Meanwhile, the choosing of ethylene glycol as raw material and additional pre-calcination leads to the enhancement of sensitivity to ethanol. Comprehensive analysis on the sensitivity and XRD, SEM, TEM, XPS results indicates that the sensing performance of LaFeO3-δ should be mainly determined by the adsorbed oxygen species on Fe ions, with certain contribution from native active oxygen. The best sensitivity of 46.1-200 ppm ethanol at prime working temperature of 112 °C is obtained by the sample using ethylene glycol as raw material with additional pre-calcination, which originates from its uniformly-sized and well-dispersed particles as well as high atomic ratio of Fe/La at surface region.

  16. Photorefractive sol-gel materials

    SciTech Connect

    Chaput, F.; Boilot, J.P.; Gacoin, T.; Darracq, B.; Riehl, D.; Canva, M.; Levy, Y.; Brun, A.

    1996-12-31

    The authors report the synthesis and characterization of photorefractive sol-gel materials that possess covalently attached push-pull azobenzene and carbazole moieties. Molecular structural characterization of the modified silane monomers was achieved by {sup 1}H NMR and infra red spectroscopy. The second-order nonlinear optical properties of the organic-inorganic hybrid films prepared from modified silane monomers were evaluated by second-harmonic generation. The stabilized value of the second harmonic coefficient, d{sub 33}, of films poled by corona discharge, at 1,064 nm fundamental wavelength was found to be 107 pm/V. Photorefractivity was clearly displayed from a two beam coupling experiment.

  17. Sol-gel chemistry by ring-opening polymerization

    SciTech Connect

    RAHIMIAN,KAMYAR; LOY,DOUGLAS A.

    2000-02-07

    Sol-gel processing of materials is plagued by shrinkage during polymerization of the alkoxide monomers and processing (aging and drying) of the resulting gels. The authors have developed a new class of hybrid organic-inorganic materials based on the solventless ring-opening polymerization (ROP) of monomers bearing the 2,2,5,5-tetramethyl-2,5-disilaoxacyclopentyl group, which permits them to drastically reduce shrinkage in sol-gel processed materials. Because the monomers are polymerized through a chain growth mechanism catalyzed by base rather than the step growth mechanism normally used in sol-gel systems, hydrolysis and condensation products are entirely eliminated. Furthermore, since water is not required for hydrolysis, an alcohol solvent is not necessary. Monomers with two disilaoxacyclopentyl groups, separated by a rigid phenylene group or a more flexible alkylene group, were prepared through disilylation of the corresponding diacetylenes, followed by ring closure and hydrogenation. Anionic polymerization of these materials, either neat or with 2,2,5,5-tetramethyl-2,5-disila-1-oxacyclopentane as a copolymer, affords thermally stable transparent gels with no visible shrinkage. These materials provide an easy route to the introduction of sol-gel type materials in encapsulation of microelectronics, which they have successfully demonstrated.

  18. Sol-gel composite material characteristics caused by different dielectric constant sol-gel phases

    NASA Astrophysics Data System (ADS)

    Kimoto, Keisuke; Matsumoto, Makoto; Kaneko, Tsukasa; Kobayashi, Makiko

    2016-07-01

    Ultrasonic transducers prepared by a sol-gel composite method have been investigated in the field of nondestructive testing (NDT). Sol-gel composite materials could be ideal piezoelectric materials for ultrasonic transducer applications in the NDT field, and a new sol-gel composite with desirable characteristics has been developed. Three kinds of sol-gel composite materials composed of different dielectric constant sol-gel phases, Pb(Zr,Ti)O3 (PZT), Bi4Ti3O12 (BiT), and BaTiO3 (BT), and the same piezoelectric powder phase, PbTiO3 (PT), were fabricated and their properties were compared quantitatively. As a result, the PT/BT, sol-gel composite with the highest dielectric constant sol-gel phase showed the highest d 33 and signal strength. In addition, only PT/BT was successfully poled by room-temperature corona poling with reasonable signal strength.

  19. Preparation of nanostructured La0.7Ca0.3-xBaxMnO3 ceramics by a combined sol-gel and spark plasma sintering route and resulting magnetocaloric properties

    NASA Astrophysics Data System (ADS)

    Ayadi, F.; Regaieg, Y.; Cheikhrouhou-Koubaa, W.; Koubaa, M.; Cheikhrouhou, A.; Lecoq, H.; Nowak, S.; Ammar, S.; Sicard, L.

    2015-05-01

    This work proposes an original, easy to achieve and inexpensive route to synthesize manganite ceramics for magnetic refrigeration, combining sol-gel chemistry to Spark Plasma Sintering (SPS). The target La0.7Ca0.3-xBaxMnO3 (x=0, 0.1, 0.2) compounds are obtained as single phases which crystallize in the orthorhombic structure (Pnma space group). SPS allows a quick sintering at a relatively low temperature (700 °C in this work) compared to the conventional solid state method (≥1100 °C), leading to densified ultrafine grained pellets (85% of compactness). Magnetic studies show that Ba substitution does not affect significantly the relative cooling power (RCP) of these manganites, while it increases their Curie temperature (TC) by several tens of degrees. Typically, RCP values ranging between 267 and 270 J/kg (for a magnetic field change of 5 T) and TC between 205 and 245 K were measured when x was increased from 0 to 0.2, respectively. These results combined to the fact that the synthesis route is economically advantageous makes the obtained ceramics interesting as active refrigerants for magnetic refrigeration technology below room temperature.

  20. Combinatorial methods in sol-gel technology

    NASA Astrophysics Data System (ADS)

    Rantala, Juha T.; Kololuoma, Terho K.; Kivimaki, L.

    2000-05-01

    Sol-gel processing consists several variable parameters during materials synthesis and post processing steps. The sol-gel synthesis is rather sensitive for the parameters such as pH, temperature, type of catalyst, reaction time etc. However, this sensitivity can be taken as an advantage when developing and studying new materials and their properties. Furthermore, since the sol-gel technology mainly describes the fabrication of solid state materials from a liquid phase by applying metal alkoxides or metal salts as precursors, the post processing such as sintering has critical effects on the final form and properties of the solid material. Combinatorial chemistry and methods are valuable tools to estimate the effects of different variables and to build-up combinatorial libraries for the sol-gel technique. This paper generally describes potentials and the usage motivation of combinatorial chemistry in the sol-gel technology by taking into account some major steps in the synthesis and processing which are valuable for the estimation of the final product properties. Different kind of post processing steps in the combinatorial manner are studied in details. As an example the post processing of sol-gel derived semiconductor oxides and photosensitivity of hybrid sol-gel glasses are presented. The combinatorial treatment and measurement methods for these materials are explained.

  1. A combined sol-gel and spark plasma sintering route to produce highly dense and fine-grained La0.65Ca0.20Na0.15MnO3 ceramics for magnetocaloric applications

    NASA Astrophysics Data System (ADS)

    Abdallah-Ben Ammar, Amal; Ayadi, Firas; Nowak, Sophie; Lecoq, Hélène; Cheikrouhou-Koubaa, Wissem; Cheikhrouhou, Abdelwaheb; Ammar, Souad; Sicard, Lorette

    2014-03-01

    Sol-gel chemistry and spark plasma sintering were coupled to produce fine-grained and dense La0.65Ca0.20Na0.15MnO3 ceramics and their magnetic properties were explored in order to evaluate their efficiency for domestic magnetocaloric applications. The obtained manganites crystallize in the rhombohedral symmetry (R-3c). They present grain size in the sub-micrometer range. Their density and their average grain size increase when the sintering temperature increases from 600 to 800 °C. This entails an increase of the Curie temperature (T C) and of the maximum of the magnetic entropy change, even if these values remain smaller than those measured on their bulk counterparts prepared by a conventional solid state route. However, the magnetic transition occurs on a broad temperature range, resulting in a relative cooling power reaching about 265 J Kg-1 for an applied magnetic field of 5 T. This value is very close to that previously measured on bulk La0.65Ca0.20Na0.15MnO3 ceramics and represents about 64% of that measured on the standard Gd. The ceramics produced here by a low-energy and time-consuming method can thus be considered as technically and economically valuable for the desired applications.

  2. Sol-gel antireflective coating on plastics

    DOEpatents

    Ashley, Carol S.; Reed, Scott T.

    1990-01-01

    An antireflection film made from a reliquified sol-gel hydrolyzation, condensation polymeric reaction product of a silicon, alkoxides and/or metal alkoxides, or mixtures thereof. The film is particularly useful for coating plastics.

  3. Sol-gel antireflective coating on plastics

    DOEpatents

    Ashley, C.S.; Reed, S.T.

    1988-01-26

    An antireflection film made from reliquified sol-gel hydrolyzation, condensation polymeric reaction product of a silicon, alkoxides and/or metal alkoxides, or mixtures thereof. The film is particularly useful for coating plastics.

  4. Sol-gel deposited electrochromic coatings

    SciTech Connect

    Ozer, N.; Lampert, C.M.

    1995-06-01

    Electrochromic devices have increasing application in display devices, switchable mirrors and smart windows. A variety of vacuum deposition technologies have been used to make electrochromic devices. The sol- gel process offers an alternative approach to the synthesis of optical quality and low cost electrochromic device layers. This study summarizes the developments in sol-gel deposited electrochromic films. The sol-gel process involves the formation of oxide networks upon hydrolysis-condensation of alkoxide precursors. In this study we cover the sol-gel deposited oxides of WO[sub 3], V[sub 2]O[sub 5], TiO[sub 2], Nb[sub 2]O[sub 5], and NiO[sub x].

  5. Arylene-bridged 2,2,5,5-tetramethyl2,5-disila-1-oxacyclopentanes as precursors to non-shrinking polysiloxanes. A new route to sol-gel type polymers

    SciTech Connect

    Rahimian, K.; Loy, D.A.

    1998-11-01

    Sol-gel chemistry has been the focus of much attention in the design and preparation of highly crosslinked polysiloxane gels. Preparation of sol-gel processed silica or polysilesquioxane gels is carried out by the hydrolysis and condensation of alkoxysilyl monomers, usually in the presence of catalytic acid or base and an excess of water. Removal of the alcohol and water byproducts of the condensation reactions, in addition to the alcohol needed to co-dissolve the hydrophobic monomers with water, leads to substantial shrinkage during drying of the resulting gels. This limits the utility of sol-gel processing for applications requiring net-shape casting of artifacts, crack free coatings, or low vaporous organic contaminants (VOCs). It would be advantageous to have a sol-gel process based on an organosilicon monomer that would not require water as a reactant or produce water and alcohol condensation products and still result in siloxane network polymers capable of forming gels. Here, the authors show the synthesis and preparation of a novel sol-gel monomer which can easily be polymerized by ring opening polymerization to give highly crosslinked polysiloxane gels with no condensation byproducts.

  6. Sol-gel entrapped cobalt complex

    SciTech Connect

    Lima, Omar J. de; Papacidero, Andrea T.; Rocha, Lucas A.; Sacco, Herica C.; Nassar, Eduardo J.; Ciuffi, Katia J.; Bueno, Luciano A.; Messaddeq, Younes; Ribeiro, Sidney J.L

    2003-03-15

    This work describes optimized conditions for preparation of a cobalt complex entrapped in alumina amorphous materials in the form of powder. The hybrid materials, CoNHG, were obtained by a nonhydrolytic sol-gel route through condensation of aluminum chloride with diisopropylether in the presence of cobalt chloride. The materials were calcined at various temperatures. The presence of cobalt entrapped in the alumina matrix is confirmed by ultraviolet visible spectroscopy. The materials have been characterized by X-ray diffraction (XRD), surface area analysis, thermogravimetric analysis (TGA), differential thermal analyses (DTA) and transmission electron microscopy (TEM). The prepared alumina matrix materials are amorphous, even after heat treatment up to 750 deg. C. The XRD, TGA/DTA and TEM data support the increase of sample crystallization with increasing temperature. The specific surface area, pore size and pore diameter changed as a function of the heat treatment temperature employed. Different heat treatment temperatures result in materials with different compositions and structures, and influence their catalytic activity. The entrapped cobalt materials calcined at 750 deg. C efficiently catalyzed the epoxidation of (Z)-cyclooctene using iodozylbenzene as the oxygen donor.

  7. The Influence of Microgravity on Silica Sol-Gel Formation

    NASA Technical Reports Server (NTRS)

    Sibille, L.; Smith, D. D.; Cronise, R.; Hunt, A. J.; Wolfe, D. B.; Snow, L. A.; Oldenberg, S.; Halas, N.; Rose, M. Franklin (Technical Monitor)

    2000-01-01

    We discuss space-flight experiments involving the growth of silica particles and gels. The effect of microgravity on the growth of silica particles via the sol-gel route is profound. In four different recipes spanning a large range of the parameter space that typically produces silica nanoparticles in unit-gravity, low-density gel structures were instead formed in microgravity. The particles that did form were generally smaller and more polydisperse than those grown on the ground. These observations suggest that microgravity reduces the particle growth rate, allowing unincorporated species to form aggregates and ultimately gel. Hence microgravity favors the formation of more rarefied structures, providing a bias towards diffusion-limited cluster-cluster aggregation. These results further suggest that in unit gravity, fluid flows and sedimentation can significantly perturb sol-gel substructures prior to gelation and these deleterious perturbations may be "frozen" into the resulting microstructure. Hence, sol-gel pores may be expected to be smaller, more uniform, and less rough when formed in microgravity.

  8. Titanium (IV) sol-gel chemistry in varied gravity environments

    NASA Astrophysics Data System (ADS)

    Hales, Matthew; Martens, Wayde; Steinberg, Theodore

    Sol-gel synthesis in reduced gravity is a relatively new topic in the literature and further inves-tigation is essential to realise its potential and application to other sol-gel systems. The sol-gel technique has been successfully applied to the synthesis of silica systems of varying porosity for many diverse applications [1-5]. It is proposed that current methods for the synthesis of silica sol-gels in reduced gravity may be applied to titanium sol-gel processing in order to enhance desirable physical and chemical characteristics of the final materials. The physical and chemical formation mechanisms for titanium alkoxide based sol-gels, to date, is not fully understood. However, various authors [6-9] have described potential methods to control the hydrolysis and condensation reactions of titanium alkoxides through the use of chemical inhibitors. A preliminary study of the reaction kinetics of titanium alkoxide sol-gel reaction in normal gravity was undertaken in order to determine reactant mixtures suitable for further testing under varied gravity conditions of limited duration. Through the use of 1H Nuclear Magnetic Resonance spectroscopy (NMR) for structural analysis of precursor materials, Ultra-Violet-Visible spectroscopy (UV-VIS) and viscosity measurements, it was demonstrated that not only could the rate of the chemical reaction could be controlled, but directed linear chain growth within the resulting gel structure was achievable through the use of increased inhibitor concentrations. Two unique test systems have been fabricated to study the effects of varied gravity (reduced, normal, high) on the formation of titanium sol-gels. Whilst the first system is to be used in conjunction with the recently commissioned drop tower facility at Queensland University of Technology in Brisbane, Australia to produce reduced gravity conditions. The second system is a centrifuge capable of providing high gravity environments of up to 70 G's for extended periods of time

  9. Neutron detector using sol-gel absorber

    DOEpatents

    Hiller, John M.; Wallace, Steven A.; Dai, Sheng

    1999-01-01

    An neutron detector composed of fissionable material having ions of lithium, uranium, thorium, plutonium, or neptunium, contained within a glass film fabricated using a sol-gel method combined with a particle detector is disclosed. When the glass film is bombarded with neutrons, the fissionable material emits fission particles and electrons. Prompt emitting activated elements yielding a high energy electron contained within a sol-gel glass film in combination with a particle detector is also disclosed. The emissions resulting from neutron bombardment can then be detected using standard UV and particle detection methods well known in the art, such as microchannel plates, channeltrons, and silicon avalanche photodiodes.

  10. Hybrid sol-gel optical materials

    DOEpatents

    Zeigler, J.M.

    1993-04-20

    Hybrid sol-gel materials comprise silicate sols cross-linked with linear polysilane, polygermane, or poly(silane-germane). The sol-gel materials are useful as optical identifiers in tagging and verification applications and, in a different aspect, as stable, visible light transparent non-linear optical materials. Methyl or phenyl silicones, polyaryl sulfides, polyaryl ethers, and rubbery polysilanes may be used in addition to the linear polysilane. The linear polymers cross-link with the sol to form a matrix having high optical transparency, resistance to thermooxidative aging, adherence to a variety of substrates, brittleness, and a resistance to cracking during thermal cycling.

  11. Hybrid sol-gel optical materials

    DOEpatents

    Zeigler, John M.

    1993-01-01

    Hybrid sol-gel materials comprise silicate sols cross-linked with linear polysilane, polygermane, or poly(silane-germane). The sol-gel materials are useful as optical identifiers in tagging and verification applications and, in a different aspect, as stable, visible light transparent non-linear optical materials. Methyl or phenyl silicones, polyaryl sulfides, polyaryl ethers, and rubbery polysilanes may be used in addition to the linear polysilane. The linear polymers cross-link with the sol to form a matrix having high optical transparency, resistance to thermooxidative aging, adherence to a variety of substrates, brittleness, and a resistance to cracking during thermal cycling.

  12. Hybrid sol-gel optical materials

    DOEpatents

    Zeigler, John M.

    1992-01-01

    Hybrid sol-gel materials comprise silicate sols cross-linked with linear polysilane, polygermane, or poly(silane-germane). The sol-gel materials are useful as optical identifiers in tagging and verification applications and, in a different aspect, as stable, visible light transparent non-linear optical materials. Methyl or phenyl silicones, polyaryl sulfides, polyaryl ethers, and rubbery polysilanes may be used in addition to the linear polysilane. The linear polymers cross-link with the sol to form a matrix having high optical transparency, resistance to thermooxidative aging, adherence to a variety of substrates, brittleness, and a resistance to cracking during thermal cycling.

  13. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna

    1992-01-01

    Application of sol-gel process to synthesis of aluminoborosilicate powders shows potential for control of microstructures of materials. Development of materials having enhanced processing characteristics prove advantageous in extending high-temperature endurance of fibrous refractory composite insulation made from ceramic fibers.

  14. Sol-Gel Derived Hafnia Coatings

    NASA Technical Reports Server (NTRS)

    Feldman, Jay D.; Stackpoole, Mairead; Blum, Yigal; Sacks, Michael; Ellerby, Don; Johnson, Sylvia M.; Venkatapathy, Ethiras (Technical Monitor)

    2002-01-01

    Sol-gel derived hafnia coatings are being developed to provide an oxidation protection layer on ultra-high temperature ceramics for potential use in turbine engines (ultra-efficient engine technology being developed by NASA). Coatings using hafnia sol hafnia filler particles will be discussed along with sol synthesis and characterization.

  15. High specific surface area nickel mixed oxide powders LaNiO{sub 3} (perovskite) and NiCo{sub 2}O{sub 4} (spinel) via sol-gel type routes for oxygen electrocatalysis in alkaline media

    SciTech Connect

    El Baydi, M.; Chartier, P.; Koenig, J.F.; Poillerat, G.; Tiwari, S.K. |; Singh, R.N.; Rehspringer, J.L.

    1995-04-01

    A novel sol-gel process of preparation of oxide electrocatalysts is investigated to prepare Ni-containing mixed oxides LaNiO{sub 3} and NiCo{sub 2}O{sub 4} at moderate temperatures. High surface area (20-55 m{sup 2} g{sup {minus}1}) powders and high roughness electrodes (30-1500) were obtained. Apparent and real electrocatalytical activity are compared and discussed.

  16. Innovative materials based on sol gel technology

    NASA Astrophysics Data System (ADS)

    Reisfeld, Renata; Saraidarov, Tsiala

    2006-01-01

    We review the sol-gel based new materials which were prepared in our laboratory including: tunable lasers, active waveguides, luminescent solar concentrators, electrochromic, photochromic and gasochromic plates for smart windows, chemical and biological sensors, semiconductor quantum dots and complexes of rare earth ions. In this paper we present the firstly obtained results of the Eu sulfide nanocrystalline (NCs) powder material and doped in the sol-gel based zirconia films. The powder and films were studied by high resolution transmittance electron microscopy (HRTEM), energy dispersive X-ray spectroscopy analysis (EDS) and luminescence spectroscopy. Eu sulfide nanocrystals (NCs) ranging between 8 and 10 nm were obtained as powder and 3-4 nm incorporated in zirconia film.

  17. Droplet Spreading with Sol-Gel Transition

    NASA Astrophysics Data System (ADS)

    Jalaal, Maziyar; Stoeber, Boris; Balmforth, Neil J.

    2014-11-01

    The impact and spreading of liquid droplets on a smooth solid substrate is a classical subject with several industrial applications such as ink-jet printing, spray cooling, coating, and many others. For many of these deposition processes, controlling the final shape of the drop is critical. In the current research, a new technique for controlling the spreading of droplets impacting a substrate is presented. This technique exploits the rheology of a thermo-responsive polymer solution that undergoes a reversible sol/gel transition above a critical temperature. Experiments are conducted using a combination of shadowgraphy and micro-PIV to observe spreading drops. It is shown that the final diameter of a droplet can be controlled through the temperature of the substrate and the tunable sol/gel transition temperature of the fluid.A mathematical model is provided to further elucidate the flow dynamics.

  18. Ring-Resonator/Sol-Gel Interferometric Immunosensor

    NASA Technical Reports Server (NTRS)

    Bearman, Gregory; Cohen, David

    2007-01-01

    A proposed biosensing system would be based on a combination of (1) a sensing volume containing antibodies immobilized in a sol-gel matrix and (2) an optical interferometer having a ring resonator configuration. The antibodies would be specific to an antigen species that one seeks to detect. In the ring resonator of the proposed system, light would make multiple passes through the sensing volume, affording greater interaction length and, hence, greater antibody- detection sensitivity.

  19. Sol-Gel Manufactured Energetic Materials

    DOEpatents

    Simpson, Randall L.; Lee, Ronald S.; Tillotson, Thomas M.; Hrubesh, Lawrence W.; Swansiger, Rosalind W.; Fox, Glenn A.

    2005-05-17

    Sol-gel chemistry is used for the preparation of energetic materials (explosives, propellants and pyrotechnics) with improved homogeneity, and/or which can be cast to near-net shape, and/or made into precision molding powders. The sol-gel method is a synthetic chemical process where reactive monomers are mixed into a solution, polymerization occurs leading to a highly cross-linked three dimensional solid network resulting in a gel. The energetic materials can be incorporated during the formation of the solution or during the gel stage of the process. The composition, pore, and primary particle sizes, gel time, surface areas, and density may be tailored and controlled by the solution chemistry. The gel is then dried using supercritical extraction to produce a highly porous low density aerogel or by controlled slow evaporation to produce a xerogel. Applying stress during the extraction phase can result in high density materials. Thus, the sol-gel method can be used for precision detonator explosive manufacturing as well as producing precision explosives, propellants, and pyrotechnics, along with high power composite energetic materials.

  20. Sol-gel manufactured energetic materials

    DOEpatents

    Simpson, Randall L.; Lee, Ronald S.; Tillotson, Thomas M.; Hrubesh, Lawrence W.; Swansiger, Rosalind W.; Fox, Glenn A.

    2003-12-23

    Sol-gel chemistry is used for the preparation of energetic materials (explosives, propellants and pyrotechnics) with improved homogeneity, and/or which can be cast to near-net shape, and/or made into precision molding powders. The sol-gel method is a synthetic chemical process where reactive monomers are mixed into a solution, polymerization occurs leading to a highly cross-linked three dimensional solid network resulting in a gel. The energetic materials can be incorporated during the formation of the solution or during the gel stage of the process. The composition, pore, and primary particle sizes, gel time, surface areas, and density may be tailored and controlled by the solution chemistry. The gel is then dried using supercritical extraction to produce a highly porous low density aerogel or by controlled slow evaporation to produce a xerogel. Applying stress during the extraction phase can result in high density materials. Thus, the sol-gel method can be used for precision detonator explosive manufacturing as well as producing precision explosives, propellants, and pyrotechnics, along with high power composite energetic materials.

  1. Sol-gel based optical chemical sensors

    NASA Astrophysics Data System (ADS)

    Lobnik, Aleksandra; Korent Urek, Špela; Turel, Matejka; Frančič, Nina

    2011-05-01

    The growing activity in the field of optical chemical sensors has resulted in numerous sensing schemes, new indicator dyes, various polymeric matrix, size and shapes and highly diversified methods of immobilization. The sensor characteristics are dependent upon the choice of indicator, polymer, immobilization technique, and also size. Sol-gel technology provides a low-temperature method for obtaining porous silicate glass matrices. It enables to obtain material in the form of films, powders, monoliths, fibres or nanoparticles. Organic reagents and molecular receptors can be easily immobilized in the matrices. Moreover, one of the unique features of the sol-gel process is that the properties of the final network structure, such as hydrophobicity, thickness, porosity, flexibility, reactivity and stability can be easily tailored by controlling the process conditions, the type and the size of the precursors and catalysis. Here we will report about several sensor designed over the years based on sol-gel materials for monitoring and controlling different parameters, such as heavy metals, amines, phosphates, organophosphates.

  2. Sol gel-fluorination synthesis of amorphous magnesium fluoride

    NASA Astrophysics Data System (ADS)

    Krishna Murthy, J.; Groß, Udo; Rüdiger, Stephan; Kemnitz, Erhard; Winfield, John M.

    2006-03-01

    The sol-gel fluorination process is discussed for the reaction of magnesium alkoxides with HF in non-aqueous solvents to give X-ray amorphous nano-sized magnesium fluoride with high surface areas in the range of 150-350 m 2/g (HS-MgF 2). The H2 type hysteresis of nitrogen adsorption-desorption BET-isotherms is indicative for mesoporous solids. A highly distorted structure causes quite high Lewis acidity, shown by NH 3 temperature-programmed desorption (NH 3-TPD) and catalytic test reactions. XPS data of amorphous and conventionally crystalline MgF 2 are compared, both show octahedral coordination at the metal site. Thermal analysis, F-MAS NMR- and IR-spectroscopy give information on composition and structure of the precursor intermediate as well as of the final metal fluoride. The preparation of complex fluorides, M +MgF 3-, by the sol-gel route is reported. From the magnesium fluoride gel of the above process thin films for optical application are obtained by, e.g., spin coating.

  3. Ionogel Electrolytes through Sol-Gel Processing

    NASA Astrophysics Data System (ADS)

    Horowitz, Ariel I.

    Electrical energy needs have intensified due to the ubiquity of personal electronics, the decarbonization of energy services through electrification, and the use of intermittent renewable energy sources. Despite developments in mechanical and thermal methods, electrochemical technologies are the most convenient and effective means of storing electrical energy. These technologies include both electrochemical cells, commonly called batteries, and electrochemical double-layer capacitors, or "supercapacitors", which store energy electrostatically. Both device types require an ion-conducting electrolyte. Current devices use solutions of complex salts in organic solvents, leading to both toxicity and flammability concerns. These drawbacks can be avoided by replacing conventional electrolytes with room-temperature molten salts, known as ionic liquids (ILs). ILs are non-volatile, non-flammable, and offer high conductivity and good electrochemical stability. Device mass can be reduced by combining ILs with a solid scaffold material to form an "ionogel," further improving performance metrics. In this work, sol-gel chemistry is explored as a means of forming ionogel electrolytes. Sol-gel chemistry is a solution-based, industrially-relevant, well-studied technique by which solids such as silica can be formed in situ. Previous works used a simple acid-catalyzed sol-gel reaction to create brittle, glassy ionogels. Here, both the range of products that can be accomplished through sol-gel processing and the understanding of interactions between ILs and the sol-gel reaction network are greatly expanded. This work introduces novel ionogel materials, including soft and compliant silica-supported ionogels and PDMS-supported ionogels. The impacts of the reactive formulation, IL identity, and casting time are detailed. It is demonstrated that variations in formulation can lead to rapid gelation and open pore structures in the silica scaffold or slow gelation and more dense silica

  4. Fabrication of Cu2ZnSn(S,Se)4 solar cells via an ethanol-based sol-gel route using SnS2 as Sn source.

    PubMed

    Zhao, Wangen; Wang, Gang; Tian, Qingwen; Yang, Yanchun; Huang, Lijian; Pan, Daocheng

    2014-08-13

    Cu2ZnSn(S,Se)4 semiconductor is a promising absorber layer material in thin film solar cells due to its own virtues. In this work, high quality Cu2ZnSn(S,Se)4 thin films have been successfully fabricated by an ethanol-based sol-gel approach. Different from those conventional sol-gel approaches, SnS2 was used as the tin source to replace the most commonly used SnCl2 in order to avoid the possible chlorine contamination. In addition, sodium was found to improve the short-circuit current and fill factor rather than the open-circuit voltage due to the decrease of the thickness of small-grained layer. The selenized Cu2ZnSn(S,Se)4 thin films showed large densely packed grains and smooth surface morphology, and a power conversion efficiency of 6.52% has been realized for Cu2ZnSn(S,Se)4 thin film solar cell without antireflective coating.

  5. Sol-gel processing to form doped sol-gel monoliths inside hollow core optical fiber and sol-gel core fiber devices made thereby

    NASA Technical Reports Server (NTRS)

    Shaw, Harry C. (Inventor); Ott, Melanie N. (Inventor); Manuel, Michele V. (Inventor)

    2002-01-01

    A process of fabricating a fiber device includes providing a hollow core fiber, and forming a sol-gel material inside the hollow core fiber. The hollow core fiber is preferably an optical fiber, and the sol-gel material is doped with a dopant. Devices made in this manner includes a wide variety of sensors.

  6. Immobilization and characterization of the transmembrane ion channel peptide gramicidin in a sol-gel matrix

    NASA Astrophysics Data System (ADS)

    Esquembre, Rocío; Poveda, José Antonio; Mallavia, Ricardo; Mateo, C. Reyes

    2007-05-01

    Immobilization of ion channels requires of a methodology able to retain the physical properties of the lipid bilayer where their activity is performed. However, most of lipid membrane immobilization methods have been observed to alter the structural properties of the bilayers. Use of sol-gel routes seems to be an interesting alternative, although unstable liposomes were obtained when conventional sol-gel methodology was employed for immobilizing. Recently, we have suggested that use of alcohol-free sol-gel routes combined with negatively charged lipids could minimize effects exerted by host matrix on liposome structure, increasing its stability. Here we confirm this assumption by analysing the physical properties of a series of zwitterionic and anionic liposomes entrapped in a sol-gel matrix and we develop a methodology able to retain the physical properties of the lipid bilayer. This methodology has been successfully used to immobilize the transmembrane ion channel peptide gramicidin. Gramicidin was reconstituted in anionic liposomes and its immobilization was confirmed from changes observed in the photophysical properties of the tryptophan residues. Ion channel activity was determined using the fluorescent dye pyrene-1,3,6,8-tetrasulphonic acid (PTSA) and long term stability of the immobilized system was checked from steady-state fluorescence anisotropy measurements.

  7. The Sol-Gel-Xerogel Transition

    DTIC Science & Technology

    1993-11-01

    cases, on the matrix of the gel. They showed that photofading of methylene blue in thin films prepared from methyltriethoxy-silane is faster than In films...thin films doped with zeolite crystals (>1 pim, ZSM-5) benefit from the size exclusion selectivity of the encased zeolites . 2. Control of the surface...exposed to H2S due to the formation of CdS crystals. Zink and 0 Dunn [33] reported that sol-gel glasses doped with iron(III) produce an intense blue

  8. Substituent effects on the sol-gel chemistry of organotrialkoxysilanes

    SciTech Connect

    LOY, DOUGLAS A.; BAUGHER, BRIGITTA M.; BAUGHER, COLLEEN R.; SCHNEIDER, DUANE A.; RAHIMIAN, KAMYAR

    2000-05-09

    Silsesquioxanes have been the subject of intensive study in the past and are becoming important again as a vehicle for introducing organic functionalities into hybrid organic-inorganic materials through sol-gel processing. Depending on the application, the target hybrid material may be required to be a highly cross-linked, insoluble gel or a soluble polymer that can be cast as a thin film or coating. The former has applications such as catalyst supports and separations media; the latter is an economically important method for surface modification or compatiblization for applying adhesives or introducing fillers. Polysilsesquioxanes are readily prepared through the hydrolysis and condensation of organotrialkoxysilanes, though organotriaminosilane and organotrihalosilane monomers can also be used. This paper explores the kinetics of the preparation route.

  9. Alkali cold gelation of whey proteins. Part I: sol-gel-sol(-gel) transitions.

    PubMed

    Mercadé-Prieto, Ruben; Gunasekaran, Sundaram

    2009-05-19

    The cold gelation of preheated whey protein isolate (WPI) solutions at alkaline conditions (pH>10) has been studied to better understand the effect of NaOH in the formation and destruction of whey protein aggregates and gels. Oscillatory rheology has been used to follow the gelation process, resulting in novel and different gelation profiles with the gelation pH. At low alkaline pH, typical sol-gel transitions are observed, as in many other biopolymers. At pH>11.5, the system gels quickly, after approximately 300 s, followed by a slow degelation step that transforms the gel to a viscous solution. Finally, there is a second gelation step. This results in a surprising sol-gel-sol-gel transition in time at constant gelation conditions. At very high pH (>12.5), the degelation step is very severe, and the second gelation step is not observed, resulting in a sol-gel-sol transition. The first quick gelation step is related to the quick swelling of the WPI aggregates in alkali, as observed from light scattering, which enables the formation of new noncovalent interactions to form a gel network. These interactions are argued to be destroyed in the subsequent degelation step. Disulfide cross-linking is observed only in the second gelation step, not in the first step.

  10. Er3+-activated photonic structures fabricated by sol-gel and rf-sputtering techniques

    NASA Astrophysics Data System (ADS)

    Ferrari, M.; Alombert-Goget, G.; Armellini, C.; Berneschi, S.; Bhaktha, S. N. B.; Boulard, B.; Brenci, M.; Chiappini, A.; Chiasera, A.; Duverger-Arfuso, C.; Féron, P.; Gonçalves, R. R.; Jestin, Y.; Minati, L.; Moser, E.; Nunzi Conti, G.; Pelli, S.; Rao, D. N.; Retoux, R.; Righini, G. C.; Speranza, G.

    2009-05-01

    The realization of photonic structures operating at visible and near infrared frequencies is a highly attractive scientific and technological challenge. Since optical fiber innovation, a huge of activity has been performed leading to interesting results, such as optical waveguides and planar lightwave circuits, microphotonic devices, optical microcavities, nanowires, plasmonic structures, and photonic crystals. These systems have opened new possibilities in the field of both basic and applied physics, in a large area covering Information Communication Technologies, Health and Biology, Structural Engineering, and Environment Monitoring Systems. Several materials and techniques are employed to successfully fabricate photonic structures. Concerning materials, Er3+-activated silica-based glasses still play an important role, although recently interesting results have been published about fluoride glass-ceramic waveguides. As far as regards the fabrication methods sol-gel route and rf sputtering have proved to be versatile and reliable techniques. In this article we will present a review of some Er3+-activated photonic structures fabricated by sol gel route and rf sputtering deposition. In the discussion on the sol-gel approach we focus our attention on the silica-hafnia binary system presenting an overview concerning fabrication protocols and structural, optical and spectroscopic assessment of SiO2-HfO2 waveguides activated by Er3+ ions. In order to put in evidence the reliability and versatility of the sol-gel route for photonics applications four different confined structures are briefly presented: amorphous waveguides, coated microspheres, monolithic waveguide laser, and core-shell nanospheres. As examples of rf sputtering technique, we will discuss Er3+-activated silica-hafnia and silica-germania waveguides, the latter system allowing fabrication of integrated optics structures by UV photo-imprinting. Finally, two examples of photonic crystal structures, one

  11. Sol-gel method for encapsulating molecules

    DOEpatents

    Brinker, C. Jeffrey; Ashley, Carol S.; Bhatia, Rimple; Singh, Anup K.

    2002-01-01

    A method for encapsulating organic molecules, and in particular, biomolecules using sol-gel chemistry. A silica sol is prepared from an aqueous alkali metal silicate solution, such as a mixture of silicon dioxide and sodium or potassium oxide in water. The pH is adjusted to a suitably low value to stabilize the sol by minimizing the rate of siloxane condensation, thereby allowing storage stability of the sol prior to gelation. The organic molecules, generally in solution, is then added with the organic molecules being encapsulated in the sol matrix. After aging, either a thin film can be prepared or a gel can be formed with the encapsulated molecules. Depending upon the acid used, pH, and other processing conditions, the gelation time can be from one minute up to several days. In the method of the present invention, no alcohols are generated as by-products during the sol-gel and encapsulation steps. The organic molecules can be added at any desired pH value, where the pH value is generally chosen to achieve the desired reactivity of the organic molecules. The method of the present invention thereby presents a sufficiently mild encapsulation method to retain a significant portion of the activity of the biomolecules, compared with the activity of the biomolecules in free solution.

  12. Method of making ionic liquid mediated sol-gel sorbents

    DOEpatents

    Malik, Abdul; Shearrow, Anne M.

    2017-01-31

    Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.

  13. Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

    ERIC Educational Resources Information Center

    Kulkarni, Suhasini; Tran, Vu; Ho, Maggie K.-M.; Phan, Chieu; Chin, Elizabeth; Wemmer, Zeke; Sommerhalter, Monika

    2010-01-01

    This experiment was performed in an upper-level undergraduate biochemistry laboratory course. Students learned how to immobilize an enzyme in a sol-gel matrix and how to perform and evaluate enzyme-activity measurements. The enzyme acid phosphatase (APase) from wheat germ was encapsulated in sol-gel beads that were prepared from the precursor…

  14. Schiff base mediated sol-gel polymerization

    SciTech Connect

    Lindquist, D.A.; Harrison, C.M.; Williams, B.; Morris, R.D.

    1996-12-31

    Formation of a Schiff base imine by reacting a primary amine with either an aldehyde or ketone was initiated by an aluminum compound acting as a Lewis acid catalyst. The water byproduct of the reaction then was used as an in situ reagent for subsequent hydrolysis and sol-gel condensation of the aluminum species. These reactions yielded a gel network containing the entrained Schiff base. Two examples of this synthetic approach are described with two different aluminum catalyst/reagents: a diethylaluminum diethylphosphate ester [(CH{sub 3}CH{sub 2}){sub 2}Al-O-P(O)(OCH{sub 2}CH{sub 3}){sub 2}] and triethyl aluminum [Al(CH{sub 3}CH{sub 2}){sub 3}]. Anhydrous ammonia and acetone were used as the Schiff base precursors.

  15. Sol-gel processing of energetic materials

    SciTech Connect

    Tillotson, T.M.; Hrubesh, L.H.; Fox, G.L.; Simpson, R.L.; Lee, R.W.; Swansiger, R.W.; Simpson, L.R.

    1997-08-18

    As part of a new materials effort, we are exploring the use of sol- gel chemistry to manufacture energetic materials. Traditional manufacturing of energetic materials involves processing of granular solids. One application is the production of detonators where powders of energetic material and a binder are typically mixed and compacted at high pressure to make pellets. Performance properties are strongly dependent on particle size distribution, surface area of its constituents, homogeneity of the mix, and void volume. The goal is to produce detonators with fast energy release rate the are insensitive to unintended initiation. In this paper, we report results of our early work in this field of research, including the preparation of detonators from xerogel molding powders and aerogels, comparing the material properties with present state-of-the-art technology.

  16. Sol-Gel Processing Science Using a Sol-Gel Optics Research Facility (SGORF)

    DTIC Science & Technology

    1989-09-10

    property of the sol-gel process can be used to make optics with special shapes and surface features such as lightweight mirrors, Fresnel lenses and...lightweight mirrors, Fresnel lenses and aspheric optical components.I Acknowledgements The authors gratefully acknowledge financial support of Air Force...e.g. Fresnel lenses ) - internal structures3 - reduced grinding - reduced polishing ! Improved Physical Properties (Type V) - lower coefficient of

  17. Investigations of the small-scale thermal behavior of sol-gel thermites.

    SciTech Connect

    Warren, Mial E.; Farrow, Matthew; Tappan, Alexander Smith

    2009-02-01

    Sol-gel thermites, formulated from nanoporous oxides and dispersed fuel particles, may provide materials useful for small-scale, intense thermal sources, but understanding the factors affecting performance is critical prior to use. Work was conducted on understanding the synthesis conditions, thermal treatments, and additives that lead to different performance characteristics in iron oxide sol-gel thermites. Additionally, the safety properties of sol-gel thermites were investigated, especially those related to air sensitivity. Sol-gel thermites were synthesized using a variety of different techniques and there appear to be many viable routes to relatively equivalent thermites. These thermites were subjected to several different thermal treatments under argon in a differential scanning calorimeter, and it was shown that a 65 C hold for up to 200 minutes was effective for the removal of residual solvent, thus preventing boiling during the final thermal activation step. Vacuum-drying prior to this heating was shown to be even more effective at removing residual solvent. The addition of aluminum and molybdenum trioxide (MoO{sub 3}) reduced the total heat release per unit mass upon exposure to air, probably due to a decrease in the amount of reduced iron oxide species in the thermite. For the thermal activation step of heat treatment, three different temperatures were investigated. Thermal activation at 200 C resulted in increased ignition sensitivity over thermal activation at 232 C, and thermal activation at 300 C resulted in non-ignitable material. Non-sol-gel iron oxide did not exhibit any of the air-sensitivity observed in sol-gel iron oxide. In the DSC experiments, no bulk ignition of sol-gel thermites was observed upon exposure to air after thermal activation in argon; however ignition did occur when the material was heated in air after thermal treatment. In larger-scale experiments, up to a few hundred milligrams, no ignition was observed upon exposure to air

  18. Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: structural and optical studies by DRS, FT-IR, XRD, FESEM investigations.

    PubMed

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-25

    Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400°C and 500°C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm(-1) can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm(-1) are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide.

  19. Structural and dielectric/ferroelectric properties of (La{sub 1-x}Nd{sub x}){sub 2}Ti{sub 2}O{sub 7} synthesized by sol-gel route

    SciTech Connect

    Shao Zhenmian; Saitzek, Sebastien; Roussel, Pascal; Mentre, Olivier; Prihor Gheorghiu, Felicia; Mitoseriu, Liliana; Desfeux, Rachel

    2010-07-15

    A series of compounds with the general formula (La{sub 1-x}Nd{sub x}){sub 2}Ti{sub 2}O{sub 7} (0.0{<=}x{<=}1.0) has been prepared by the sol-gel method. The decomposition of the gel was characterized by thermo-gravimetric analysis coupled to mass spectrometry, indicating the reaction is achieved above 850 {sup o}C. The lattice parameters versus x show an expected decrease in the a and b parameters while c and the {beta} angle remain almost unchanged with respect to the monoclinic symmetry conserved for the full solid solution. Dielectric, piezoelectric and ferroelectric properties were measured on the entire series. - Graphical abstract: XRD patterns of (La{sub 1-x}Nd{sub x}){sub 2}Ti{sub 2}O{sub 7} powders for various x values. The (hkl) peaks positions (with h and k{ne}0) change with x values while the (00l) peaks positions remain unaffected.

  20. Structural and optical studies of ZnAl2O4:x% Cu2+(0 < x ≤ 1.25) nanophosphors synthesized via citrate sol-gel route

    NASA Astrophysics Data System (ADS)

    Motloung, S. V.; Dejene, F. B.; Koao, L. F.; Ntwaeaborwa, O. M.; Swart, H. C.; Motaung, T. E.; Ndwandwe, O. M.

    2017-02-01

    Nanocrystalline ZnAl2O4:x% Cu2+(0 < x ≤ 1.25) phosphor powders were prepared via the citrate sol-gel technique. The pure-phase cubic structures in this systems were verified by the powder X-ray diffraction. Energy Dispersive x-ray Spectroscopy analysis confirmed the presence of the expected elements (Zn, Al, O and Cu). Scanning Electron Microscopy showed that the morphology of the phosphor was dependent on the concentration of Cu2+. High-Resolution Transmission Electron Microscopy confirmed that the Cu2+ concentration does not significantly influence the crystallites sizes of the phosphors. Ultraviolet-visible spectroscopy results showed that the Cu2+ concentration influenced the band gap of the host. Photoluminescence results showed that the emission intensity of the powder sample was dependent on the Cu2+ concentration. The emission from the host lattice was observed at 394 nm, while Cu2+ showed major emission at 405 and minor emission at 574 nm. The emission at 405 nm was due to the 3d84s1 → 3d9 transitions of Cu2+. The Commission on Illumination color coordinate evidently showed shifts from the bluewish to the greenish region with an increase in Cu2+ concentration.

  1. Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: Structural and optical studies by DRS, FT-IR, XRD, FESEM investigations

    NASA Astrophysics Data System (ADS)

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-01

    Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400 °C and 500 °C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm-1 can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm-1 are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide.

  2. Solid-state NMR study of geopolymer prepared by sol-gel chemistry

    SciTech Connect

    Tsai, Yi-Ling; Hanna, John V.; Lee, Yuan-Ling; Smith, Mark E.; Chan, Jerry C.C.

    2010-12-15

    Geopolymers are a new class of materials formed by the condensation of aluminosilicates and silicates obtained from natural minerals or industrial wastes. In this work, the sol-gel method is used to synthesize precursor materials for the preparation of geopolymers. The geopolymer samples prepared by our synthetic route have been characterized by a series of physical techniques, including Fourier-transform infrared, X-ray diffraction, and multinuclear solid-state NMR. The results are very similar to those obtained for the geopolymers prepared from natural kaolinite. We believe that our synthetic approach can offer a good opportunity for the medical applications of geopolymer. -- Graphical abstract: Geopolymer prepared by the sol-gel route has the same spectroscopic properties as the sample prepared from the natural kaolinite. Display Omitted

  3. Structural properties and application in lithium cells of Li(Ni0.5Co0.5)1-yFeyO2 (0 ≤ y ≤ 0.25) prepared by sol-gel route: Doping optimization

    NASA Astrophysics Data System (ADS)

    Abdel-Ghany, A. E.; Hashem, A. M.; Elzahany, E. A.; Abuzeid, H. A.; Indris, S.; Nikolowski, K.; Ehrenberg, H.; Zaghib, K.; Mauger, A.; Julien, C. M.

    2016-07-01

    Layered Li(Co0.5Ni0.5)1-yFeyO2 (0.0 ≤ y ≤ 0.25) oxides were prepared by citric-acid assisted sol-gel method. Elemental and structural properties were investigated by energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman scattering (RS) and Mössbauer spectroscopy, and magnetometry. EDX images show a homogeneous distribution of Fe ions. XRD and RS spectroscopy reveal that the materials crystallize as a LiNiO2sbnd LiCoO2sbnd LiFeO2 solid solution with the typical rhombohedral α-NaFeO2 structure (R 3 bar m S.G.) up to y = 0.2 at which composition a secondary phase was observed. For y > 0.2 the XRD results show the appearance of the α-LiFeO2 phase with the cubic structure (Fm3m S.G.). The degree of cation mixing investigated by XRD analysis and magnetic measurements is z < 0.04, for y < 0.2. Electrochemical tests of Li(Co0.5Ni0.5)1-yFeyO2 (0.0 ≤ y ≤ 0.1) oxides in lithium cells show the influence of iron substitution. The best results have been obtained for the composition y(Fe) = 0.05, where the electrical conductivity is maximum. A specific capacity 32 mAh g-1 is maintained at 8C rate.

  4. Sol/Gel Processing Techniques for Glass Matrix Composites.

    DTIC Science & Technology

    1987-11-01

    development of a general technique (i.e., Pyrex is less susceptible to devitrification than SiO2 or TiO2 -SiO 2 ). In addition. the properties of these sol / gel ...of a sol / gel process for SIC 2 and SiO2 - TiO2 - together with a data base for their densification - are prerequisite to the successful fabrication of...S~%ad~ 5~ ~ ~ *~~~~;:>;::L-; 1: ’*~~’~ ’S. AFWL-TN-86-59 AFWL-TN- 86-59 00 SOL / GEL PROCESSING TECHNIQUES FOR GLASS MATRIX COMPOSITES 0) C. G

  5. Oxide Ceramic Fibers by the Sol-Gel Methods

    DTIC Science & Technology

    1989-02-10

    prepared by the sol-gel method . 3 Table 2. List of candidates for fibers via the sol-gel method . 4 Table 3. Solvents, raw materials and catalysts ...reaction chemistry. The synthesis method will be discussed in Section 3.1.3 Using commercially available precursors the production of lanthanum chromite via...AFWAL-TR-88-4199 OXIDE CERAMIC FIBERS BY THE SOL-GEL METHOD J. D. Mackenzie If) K. Ono The Regents of the University of California (Los Angeles) V

  6. Raman and electrochemical impedance studies of sol-gel titanium oxide and single walled carbon nanotubes composite films.

    PubMed

    Rincón, M E; Trujillo-Camacho, M E; Miranda-Hernández, M; Cuentas-Gallegos, A K; Orozco, G

    2007-01-01

    Titanium oxide grown by a sol-gel route on single-walled carbon nanotubes was studied by Raman and Electrochemical Impedance techniques and compared with mixtures obtained by mechanical grinding. In spite of the superior dispersion of single-walled carbon nanotubes bundles in sol-gel composites, the lost of the small-diameter carbon nanotubes in the oxidizing sol-gel bath was inferred from their Raman spectra and the lower capacitive current of the voltammograms in 0.1 M H2SO4. We proposed proton electrosorption as the main charge storage mechanism for sol-gel composites, favoured by the hydroxylation and n-type conductivity of the oxide, while electrodes based on mixtures were dominated by double-layer charging, developing some pseudocapacitance with potential cycling due to the reversible oxidation of carbon nanotubes. Comparsion with TiO2/Carbon Blacks composites shows the effective role of single-walled carbon nanotubes as templates to control the mesoporous nature of sol-gel composite electrodes.

  7. Electrophoretic Porosimetry of Sol-Gels

    NASA Technical Reports Server (NTRS)

    Snow, L. A.; Smith, D. D.; Sibille, L.; Hunt, A. J.; Ng, J.; Rose, M. Franklin (Technical Monitor)

    2000-01-01

    It has been hypothesized that gravity has an effect on the formation and resulting microstructure of sol-gels. In order to more clearly resolve the effect of gravity, pores may be non-destructively analyzed in the wet gel, circumventing the shrinkage and coarsening associated with the drying procedure. We discuss the development of an electrophoretic technique, analogous to affinity chromatography, for the determination of pore size distribution and its application to silica gels. Specifically a monodisperse charged dye is monitored by an optical densitometer as it moves through the wet gel under the influence of an electric field. The transmittance data (output) represents the convolution of the dye concentration profile at the beginning of the run (input) with the pore size distribution (transfer function), i.e. linear systems theory applies. Because of the practical difficulty in producing a delta function input dye profile we prefer instead to use a step function. Average pore size is then related to the velocity of this dye front, while the pore size distribution is related to the spreading of the front. Preliminary results of this electrophoretic porosimetry and its application to ground and space-grown samples will be discussed.

  8. Wet powder processing of sol-gel derived mesoporous silica-hydroxyapatite hybrid powders.

    PubMed

    Andersson, Jenny; Johannessen, Espen; Areva, Sami; Järn, Mikael; Lindén, Mika

    2006-08-01

    This paper describes a method by which a porous silica coating layer can be obtained on different apatite particles through a simple sol-gel synthesis route. Sol-gel derived powders of hydroxyapatite (HAP) and beta tricalciumphosphate (beta-TCP) were coated with a mesoporous silica using C16TAB (hexadecyltrimethylammonium bromide) as a template in order to induce mesophase formation. Further calcination of the material removes the template from the mesophase and leaves a highly ordered hexagonal arranged mesoporous silica structure with a core of HAP/beta-TCP. The phase purity of the SiO2/apatite composites has been thoroughly investigated by the means of FT-IR, XRD, and solid state 31P MAS NMR. The phase purity of these materials is shown to be dependent on the solubility properties of the used apatites. The hybrid materials are suitable as a multifunctional biomaterial where osteoconductive properties can be combined with drug delivery.

  9. Production of continuous mullite fiber via sol-gel processing

    NASA Technical Reports Server (NTRS)

    Tucker, Dennis S.; Sparks, J. Scott; Esker, David C.

    1990-01-01

    The development of a continuous ceramic fiber which could be used in rocket engine and rocket boosters applications was investigated at the Marshall Space Flight Center. Methods of ceramic fiber production such as melt spinning, chemical vapor deposition, and precursor polymeric fiber decomposition are discussed and compared with sol-gel processing. The production of ceramics via the sol-gel method consists of two steps, hydrolysis and polycondensation, to form the preceramic, followed by consolidation into the glass or ceramic structure. The advantages of the sol-gel method include better homogeneity and purity, lower preparation temperature, and the ability to form unique compositions. The disadvantages are the high cost of raw materials, large shrinkage during drying and firing which can lead to cracks, and long processing times. Preparation procedures for aluminosilicate sol-gel and for continuous mullite fibers are described.

  10. Electrochemical and spectroscopic characterization of surface sol-gel processes.

    PubMed

    Chen, Xiaohong; Wilson, George S

    2004-09-28

    (3-Mercaptopropyl)trimethoxysilane (MTS) forms a unique film on a platinum substrate by self-assembly and sol-gel cross-linking. The gelating and drying states of the self-assembled MTS sol-gel films were probed by use of electrochemical and spectroscopic methods. The thiol moiety was the only active group within the sol-gel network. Gold nanoparticles were employed to detect the availability of the thiol group and their interaction further indicated the physicochemical states of the sol-gel inner structure. It was found that the thiol groups in the open porous MTS aerogel matrix were accessible to the gold nanoparticles while thiol groups in the compact MTS xerogel network were not accessible to the gold nanoparticles. The characteristics of the sol-gel matrix change with time because of its own irreversible gelating and drying process. The present work provides direct evidence of gold nanoparticle binding with thiol groups within the sol-gel structures and explains the different permeability of "aerogel" and "xerogel" films of MTS on the basis of electrochemical and spectroscopic results. Two endogenous species, hydrogen peroxide and ascorbic acid, were used to test the permeability of the self-assembled sol-gel film in different states. The MTS xerogel film on the platinum electrode was extremely selective against ascorbic acid while maintaining high sensitivity to hydrogen peroxide in contrast to the relatively high permeability of ascorbic acid in the MTS aerogel film. This study showed the potential of the MTS sol-gel film as a nanoporous material in biosensor development.

  11. Prospects of sol-gel technology towards luminescent materials

    NASA Astrophysics Data System (ADS)

    Reisfeld, R.

    2001-02-01

    Sol-gel method for producing glasses or glass films at relatively low temperature allows incorporation of a large number of inorganic and organic additives during the process of glass formation. We outline some of the sophisticated products and devices obtained by the sol-gel method. Luminecence solar concentrators, tunable lasers in the visible part of the spectrum, active waveguides, semiconductor particles and sensors for environmental impurities.

  12. Sol-gel-based biosensing applied to medicinal science.

    PubMed

    Moreira, Felismina T C; Moreira-Tavares, Ana P; Sales, M Goreti F

    2015-01-01

    Biosensors have opened new horizons in biomedical analysis, by ensuring increased assay speed and flexibility, and allowing point-of-care applications, multi-target analyses, automation and reduced costs of testing. This has been a result of many studies merging nanotechnology with biochemistry over the years, thereby enabling the creation of more suitable environments to biological receptors and their substitution by synthetic analogue materials. Sol-gel chemistry, among other materials, is deeply involved in this process. Sol-gel processing allows the immobilization of organic molecules, biomacromolecules and cells maintaining their properties and activities, permitting their integration into different transduction devices, of electrochemical or optical nature, for single or multiple analyses. Sol-gel also allows to the production of synthetic materials mimicking the activity of natural receptors, while bringing advantages, mostly in terms of cost and stability. Moreover, the biocompatibility of sol-gel materials structures of biological nature allowed the use of these materials in emerging in vivo applications. In this chapter, biosensors for biomedical applications based on sol-gel derived composites are presented, compared and described, along with current emerging applications in vivo, concerning drug delivery or biomaterials. Sol-gel materials are shown as a promising tool for current, emerging and future medical applications.

  13. Bi-Sr-Co-O thermoelectrics prepared by sol-gel methods with modified gel decomposition

    NASA Astrophysics Data System (ADS)

    Rubešová, K.; Hlásek, T.; Jakeš, V.; Sedmidubský, D.; Hejtmánek, J.

    2012-02-01

    We prepared misfit Bi2Sr2Co1.8Ox (Bi-222) phase as a member of a Bi-Sr-Co-O family. Two water based sol-gel methods were chosen with regard to the presence of a strongly hydrolysing Bi3+ ion - chelating route combining EDTA (ethylenediaminetetraacetic acid) and TEA (triethanolamine) and, secondly, water soluble polymer method using PEI (polyethylenimine). We focused on the influence of gel decomposition process on the grain size of precursor and, consequently, on the bulk density of the final samples. We tested decomposition in N2 atmosphere followed by a treatment in pure oxygen. The precursors decomposed in "N2/O2" regime were mainly composed of Bi2O3, SrCO3 and cobalt oxides with the grain size of approximately 50-100 nm. The powders arising from gel decomposition in air contained the desired Bi-Sr-Co-O oxide as the major phase independently of the chosen sol-gel method. The final sintered samples were almost single-phase with traces of the other pseudoternary phase Bi2Sr2CoOx independently of the decomposition atmosphere. For comparison, samples were also prepared by solid state reaction. The sol-gel prepared samples were always of higher bulk density with larger grains, moreover partly microstructurally ordered. These facts were also reflected in transport thermoelectric measurements.

  14. Enzyme renaturation to higher activity driven by the sol-gel transition: Carbonic anhydrase

    PubMed Central

    Vinogradov, Vladimir V.; Avnir, David

    2015-01-01

    We describe a so-far unknown route for renaturing denatured enzymes, namely subjecting the denatured enzyme to an oxide sol-gel transition. The phenomenon was revealed in a detailed study of denatured carbonic anhydrase which was subjected to an alumina sol-gel transition, up to the thermally stabilizing entrapment in the final xerogel. Remarkably, not only that the killed enzyme regained its activity during the sol-gel process, but its activity increased to 180% of the native enzyme. To the best of our knowledge, this is the first report of enhanced activity following by renaturing (a “Phoenix effect”). Kinetic study which revealed a five-orders of magnitude (!) increase in the Arrhenius prefactor upon entrapment compared to solution. Circular dichroism analysis, differential scanning calorimetry, zeta potential analyses as well as synchronous fluorescence measurements, all of which were used to characterize the phenomenon, are consistent with a proposed mechanism which is based on the specific orienting interactions of the active site of the enzyme with respect to the alumina interface and its pores network. PMID:26394694

  15. Enzyme renaturation to higher activity driven by the sol-gel transition: Carbonic anhydrase

    NASA Astrophysics Data System (ADS)

    Vinogradov, Vladimir V.; Avnir, David

    2015-09-01

    We describe a so-far unknown route for renaturing denatured enzymes, namely subjecting the denatured enzyme to an oxide sol-gel transition. The phenomenon was revealed in a detailed study of denatured carbonic anhydrase which was subjected to an alumina sol-gel transition, up to the thermally stabilizing entrapment in the final xerogel. Remarkably, not only that the killed enzyme regained its activity during the sol-gel process, but its activity increased to 180% of the native enzyme. To the best of our knowledge, this is the first report of enhanced activity following by renaturing (a “Phoenix effect”). Kinetic study which revealed a five-orders of magnitude (!) increase in the Arrhenius prefactor upon entrapment compared to solution. Circular dichroism analysis, differential scanning calorimetry, zeta potential analyses as well as synchronous fluorescence measurements, all of which were used to characterize the phenomenon, are consistent with a proposed mechanism which is based on the specific orienting interactions of the active site of the enzyme with respect to the alumina interface and its pores network.

  16. Chemical sensing of copper phthalocyanine sol-gel glass through organic vapors

    SciTech Connect

    Ridhi, R.; Gawri, Isha; Abbas, Saeed J.; Saini, G. S. S.; Tripathi, S. K.

    2015-05-15

    The sensitivities of metallophthalocyanine to vapor phase electron donors has gained significance in many areas and disciplines due to their sensing properties and ease of operation. In the present study the interaction mechanism of organic vapors in Copper Phthalocyanine (CuPc) sol-gel glass has been studied. The interaction mechanism is affected by many factors like morphology, electrical or optical properties of film. CuPc sol-gel glass has been synthesized using chemical route sol-gel method. Its structural characterization was conducted using XRD and the amorphous nature of the silicate glass was observed with characteristic α polymorph phase of CuPc at around 6.64° with 13.30Å interplanar spacing. The size of the particle as determined using Debbye Scherre’s formula comes out around 15.5 nm. The presence of α phase of CuPc was confirmed using FTIR with the appearance of crystal parameter marker band at 787 cm-1. Apart from this A2u and Eu symmetry bands of CuPc have also been observed. The UV absorption spectrum of CuPc exhibits absorption peaks owing to π→ π* and n→ π* transitions. A blue shift in the prepared CuPc glass has been observed as compared to the dopant CuPc salt indicating increase of band gap. A split in B (Soret) band and Q band appears as observed with the help of Lorentzian fitting. CuPc sol gel glass has been exposed with chemical vapors of Methanol, Benzene and Bromine individually and the electrical measurements have been carried out. These measurements show the variation in conductivity and the interaction mechanism has been analyzed.

  17. Slow Release of Plant Volatiles Using Sol-Gel Dispensers.

    PubMed

    Bian, L; Sun, X L; Cai, X M; Chen, Z M

    2014-12-01

    The black citrus aphid, also known as the tea aphid, (Toxoptera aurantii Boyer) attacks economically important crops, including tea (Camellia sinensis (L.) O. Kuntze). In the current study, silica sol-gel formulations were screened to find one that could carry and release C. sinensis plant volatiles to lure black citrus aphids in a greenhouse. The common plant volatile trans-2-hexen-1-al was used as a model molecule to screen for suitable sol-gel formulations. A zNose (Electronic Sensor Technology, Newbury Park, CA) transportable gas chromatograph was used to continuously monitor the volatile emissions. A sol-gel formulation containing tetramethyl orthosilicate and methyltrimethoxysilane in an 8:2 (vol:vol) ratio was selected to develop a slow-release dispenser. The half-life of trans-2-hexen-1-al in the sol-gel dispenser increased slightly with the volume of this compound in the dispenser. Ten different volatiles were tested in the sol-gel dispenser. Alcohols of 6-10 carbons had the longest half-lives (3.01-3.77 d), while esters of 6-12 carbons had the shortest (1.53-2.28 d). Release of these volatiles from the dispensers could not be detected by the zNose after 16 d (cis-3-hexenyl acetate) to 26 d (3,7-dimethylocta-1,6-dien-3-ol). In greenhouse experiments, trans-2-hexen-1-al and cis-3-hexen-1-ol released from the sol-gel dispensers attracted aphids for ≍17 d, and release of these volatiles could not be detected by the zNose after ≍24 d. The sol-gel dispensers performed adequately for the slow release of plant volatiles to trap aphids in the greenhouse.

  18. Sol-gel encapsulation for controlled drug release and biosensing

    NASA Astrophysics Data System (ADS)

    Fang, Jonathan

    The main focus of this dissertation is to investigate the use of sol-gel encapsulation of biomolecules for controlled drug release and biosensing. Controlled drug release has advantages over conventional therapies in that it maintains a constant, therapeutic drug level in the body for prolonged periods of time. The anti-hypertensive drug Captopril was encapsulated in sol-gel materials of various forms, such as silica xerogels and nanoparticles. The primary objective was to show that sol-gel silica materials are promising drug carriers for controlled release by releasing Captopril at a release rate that is within a therapeutic range. We were able to demonstrate desired release for over a week from Captopril-doped silica xerogels and overall release from Captopril-doped silica nanoparticles. As an aside, the antibiotic Vancomycin was also encapsulated in these porous silica nanoparticles and desired release was obtained for several days in-vitro. The second part of the dissertation focuses on immobilizing antibodies and proteins in sol-gel to detect various analytes, such as hormones and amino acids. Sol-gel competitive immunoassays on antibody-doped silica xerogels were used for hormone detection. Calibration for insulin and C-peptide in standard solutions was obtained in the nM range. In addition, NASA-Ames is also interested in developing a reagentless biosensor using bacterial periplasmic binding proteins (bPBPs) to detect specific biomarkers, such as amino acids and phosphate. These bPBPs were doubly labeled with two different fluorophores and encapsulated in silica xerogels. Ligand-binding experiments were performed on the bPBPs in solution and in sol-gel. Ligand-binding was monitored by fluorescence resonance energy transfer (FRET) between the two fluorophores on the bPBP. Titration data show that one bPBP has retained its ligand-binding properties in sol-gel.

  19. Investigations into the structural and down-shifting and up-conversion luminescence properties of Ba2Na1-3x Er x Nb5O15 (0 ≤ x ≤ 0.06) nanocrystalline phosphor synthesized via sol-gel route

    NASA Astrophysics Data System (ADS)

    Kundu, Swarup; Bhimireddi, Rajasekhar; Mishra, Kavita; Rai, S. B.; Varma, K. B. R.

    2015-10-01

    The present work deals with the structural and efficient down-shifting (DS) and up-conversion (UC) luminescence properties of erbium ion (Er3+) doped nanocrystalline barium sodium niobate (Ba2Na1-3x Er x Nb5O15, where x = 0, 0.02, 0.04 and 0.06) powders synthesized via novel citrate-based sol-gel route. The monophasic nature of the title compound was confirmed via x-ray powder diffraction followed by FT-IR studies. High-resolution transmission electron microscopy (HRTEM) facilitated the establishment of the nanocrystalline phase and the morphology of the crystallites. The Kubelka-Munk function, based on diffused reflectance studies and carried out on nano-sized crystallites, was employed to obtain the optical band-gap. The synthesized nanophosphor showed efficient DS/PL-photoluminescence and UC luminescence properties, which have not yet been reported so far in this material. The material emits intense DS green emission on excitation with 378 nm radiation. Interestingly, the material gives intense UC emission in the visible region dominated by green emission and relatively weak red emission on 976 nm excitation (NIR laser excitation). Such a dual-mode emitting nanophosphor could be very useful in display devices and for many other applications.

  20. Nonhydrolytic sol-gel approach to facile creation of surface-bonded zirconia organic-inorganic hybrid coatings for sample preparation. Ι. Capillary microextraction of catecholamine neurotransmitters.

    PubMed

    Alhendal, Abdullah; Mengis, Stephanie; Matthews, Jacob; Malik, Abdul

    2016-10-14

    Nonhydrolytic sol-gel (NHSG) route was used for the creation of novel zirconia-polypropylene oxide (ZrO2-PPO) sol-gel hybrid sorbents in the form of surface coatings for the extraction and preconcentration of catecholamine neurotransmitters and molecules structurally related to their deaminated metabolites. In comparison to other sorbents made of inorganic transition metal oxides, the presented hybrid organic-inorganic sorbents facilitated reversible sorption properties that allowed for efficient desorption of the extracted analytes by LC-MS compatible mobile phases. The presented sol-gel hybrid sorbents effectively overcame the major drawbacks of traditional silica- or polymer-based sorbents by providing superior pH stability (pH range: 0-14), and a variety of intermolecular interactions. Nonaqueous sol-gel treatment of PPO with ZrCl4 was employed for the derivatization of the terminal hydroxyl groups on PPO, providing zirconium trichloride-containing end groups characterized by enhanced sol-gel reactivity. NHSG ZrO2-PPO sorbent provided excellent microextraction performance for catecholamines, low detection limits (5.6-9.6pM), high run-to-run reproducibility (RSD 0.6-5.1%), high desorption efficiency (95.0-99.5%) and high enrichment factors (∼1480-2650) for dopamine and epinephrine, respectively, extracted from synthetic urine samples. The presented sol-gel sorbents provided effective alternative to conventional extraction media providing unique physicochemical characteristics and excellent extraction capability.

  1. Sol-gel derived contamination resistant antireflective coatings

    NASA Astrophysics Data System (ADS)

    Shen, Jun; Liu, Yuan; Wu, Guangming; Zhou, Bin; Zhang, Zhihua; Zhu, Yumei

    2011-02-01

    Silica-based sol-gel antireflective (AR) optical coatings are critical components for high peak power laser systems. It is well known that water vapor and volatile organic compounds in both the laser bay and target bay environments will reduce the antireflective efficiency and laser-damage resistance of the sol-gel AR coating. In this study, alkylation with organosilanes in the vapor state was investigated. Sol-gel AR coatings were vapor-phase treated with hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) at room temperature, and the resulting post-treated sol-gel AR coatings were tested for their resistance to contamination by a series of volatile organic compounds. Contact angle measurements were taken to discern the degree of silanization. After the vapor treatment of sol-gel AR coatings with organosilanes, the spectral performance of the coatings were analyzed by spectrophotometer, both before and after the exposure to volatile organic compounds. It is found that the coatings treated with ammonia and HMDS show a better contamination resistant capability. After being contaminated 70 hours with hexane, the transmittance of the coatings presents no obvious decrease. And the vapor treatment produces an increase in their damage threshold at 1064 nm (10ns pulse width) as compared to untreated control samples.

  2. Sol-gel derived contamination resistant antireflective coatings

    NASA Astrophysics Data System (ADS)

    Shen, Jun; Liu, Yuan; Wu, Guangming; Zhou, Bin; Zhang, Zhihua; Zhu, Yumei

    2010-10-01

    Silica-based sol-gel antireflective (AR) optical coatings are critical components for high peak power laser systems. It is well known that water vapor and volatile organic compounds in both the laser bay and target bay environments will reduce the antireflective efficiency and laser-damage resistance of the sol-gel AR coating. In this study, alkylation with organosilanes in the vapor state was investigated. Sol-gel AR coatings were vapor-phase treated with hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) at room temperature, and the resulting post-treated sol-gel AR coatings were tested for their resistance to contamination by a series of volatile organic compounds. Contact angle measurements were taken to discern the degree of silanization. After the vapor treatment of sol-gel AR coatings with organosilanes, the spectral performance of the coatings were analyzed by spectrophotometer, both before and after the exposure to volatile organic compounds. It is found that the coatings treated with ammonia and HMDS show a better contamination resistant capability. After being contaminated 70 hours with hexane, the transmittance of the coatings presents no obvious decrease. And the vapor treatment produces an increase in their damage threshold at 1064 nm (10ns pulse width) as compared to untreated control samples.

  3. Sol-gel technologies for multimode waveguide structures

    NASA Astrophysics Data System (ADS)

    Karioja, Pentti; Kusevic, Maja; Hiltunen, Marianne; Paaso, Janne; Maekinen, Jukka-Tapani; Hiltunen, Jussi A.; Kautio, Kari; Kopola, Harri K.

    2002-06-01

    Lithographic patterning of organic-inorganic hybrid materials processed by the use of sol-gel technology allows for the generation of waveguide structures at low temperatures onto polymer or ceramic substrates. In addition, sol-gel technology provides the possibility to process precision structures, such as, grooves and cavities, which are applicable for the passive alignment of photonic devices. This provides the possibility for the realization of mass-producible photonic circuits onto large-area substrates. At the moment, the most potential applications are systems based on then use of multimode waveguide structures. Actually, when utilizing sol-gel technology, the challenge is how to process homogenous, low-loss and high-aspect-ratio structures. In addition, when aiming to highly mass-producible multimode modules, the key issue is the alignment of photonic devices preferably by the use of passive precision structures. In the future, when the systems need to be more complicated, the modeling of systems requires sophisticated 3D modeling tools. In this paper, the processing of multimode structures with sol-gel technologies is described, and the characterization results of prototype devices are reported. In addition, molding and cofiring technologies potentially applicable for the hybrid integration of photonic modules are reviewed. Finally, the future research aims for the commercialization of photonic modules based on the use of sol-gel technologies are envisioned.

  4. Optical Sensors for Biomolecules Using Nanoporous Sol-Gel Materials

    NASA Technical Reports Server (NTRS)

    Fang, Jonathan; Zhou, Jing C.; Lan, Esther H.; Dunn, Bruce; Gillman, Patricia L.; Smith, Scott M.

    2004-01-01

    An important consideration for space missions to Mars is the ability to detect biosignatures. Solid-state sensing elements for optical detection of biological entities are possible using sol-gel based biologically active materials. We have used these materials as optical sensing elements in a variety of bioassays, including immunoassays and enzyme assays. By immobilizing an appropriate biomolecule in the sol-gel sensing element, we have successfully detected analytes such as amino acids and hormones. In the case of the amino acid glutamate, the enzyme glutamate dehydrogenase was the immobilized molecule, whereas in the case of the hormone cortisol, an anti-cortisol antibody was immobilized in the sensing element. In this previous work with immobilized enzymes and antibodies, excellent sensitivity and specificity were demonstrated in a variety of formats including bulk materials, thin films and fibers. We believe that the sol-gel approach is an attractive platform for bioastronautics sensing applications because of the ability to detect a wide range of entities such as amino acids, fatty acids, hopanes, porphyrins, etc. The sol-gel approach produces an optically transparent 3D silica matrix that forms around the biomolecule of interest, thus stabilizing its structure and functionality while allowing for optical detection. This encapsulation process protects the biomolecule and leads to a more "rugged" sensor. The nanoporous structure of the sol-gel matrix allows diffusion of small target molecules but keeps larger, biomolecules immobilized in the pores. We are currently developing these biologically active sol-gel materials into small portable devices for on-orbit cortisol detection

  5. Sol-gel processing with inorganic metal salt precursors

    DOEpatents

    Hu, Zhong-Cheng

    2004-10-19

    Methods for sol-gel processing that generally involve mixing together an inorganic metal salt, water, and a water miscible alcohol or other organic solvent, at room temperature with a macromolecular dispersant material, such as hydroxypropyl cellulose (HPC) added. The resulting homogenous solution is incubated at a desired temperature and time to result in a desired product. The methods enable production of high quality sols and gels at lower temperatures than standard methods. The methods enable production of nanosize sols from inorganic metal salts. The methods offer sol-gel processing from inorganic metal salts.

  6. Sol-gel derived PZT films doped with vanadium pentoxide

    SciTech Connect

    Shen Hongfang; Guo Qing; Zhao Zhiman; Cao Guozhong

    2009-11-15

    The present research investigated the sol-gel preparation, dielectric and ferroelectric properties of PZT films doped with 5 mol% vanadium oxide. Stable PZTV sols can be readily formed, and homogeneous, micrometer thick and pinhole-free PZTV films were obtained by using spin coating followed with rapid annealing. The X-ray diffraction patterns revealed that no parasitic or secondary phases were formed in the sol-gel PZT films with the addition of vanadium oxide. The material doped with vanadium pentoxide showed enhanced dielectric constant and remanent polarization with reduced loss tangent and coercive field.

  7. Silica scintillating materials prepared by sol-gel methods

    SciTech Connect

    Werst, D.W.; Sauer, M.C. Jr.; Cromack, K.R.; Lin, Y.; Tartakovsky, E.A.; Trifunac, A.D.

    1993-12-31

    Silica was investigated as a rad-hard alternative to organic polymer hosts for organic scintillators. Silica sol-gels were prepared by hydrolysis of tetramethoxysilane in alcohol solutions. organic dyes were incorporated into the gels by dissolving in methanol at the sol stage of gel formation. The silica sol-gel matrix is very rad-hard. The radiation stability of silica scintillators prepared by this method is dye-limited. Transient radioluminescence was measured following excitation with 30 ps pulses of 20 MeV electrons.

  8. Sol-gel preparation of silica and titania thin films

    NASA Astrophysics Data System (ADS)

    Thoř, Tomáš; Václavík, Jan

    2016-11-01

    Thin films of silicon dioxide (SiO2) and titanium dioxide (TiO2) for application in precision optics prepared via the solgel route are being investigated in this paper. The sol-gel process presents a low cost approach, which is capable of tailoring thin films of various materials in optical grade quality. Both SiO2 and TiO2 are materials well known for their application in the field of anti-reflective and also highly reflective optical coatings. For precision optics purposes, thickness control and high quality of such coatings are of utmost importance. In this work, thin films were deposited on microscope glass slides substrates using the dip-coating technique from a solution based on alkoxide precursors of tetraethyl orthosilicate (TEOS) and titanium isopropoxide (TIP) for SiO2 and TiO2, respectively. As-deposited films were studied using spectroscopic ellipsometry to determine their thickness and refractive index. Using a semi-empirical equation, a relationship between the coating speed and the heat-treated film thickness was described for both SiO2 and TiO2 thin films. This allows us to control the final heat-treated thin film thickness by simply adjusting the coating speed. Furthermore, films' surface was studied using the white-light interferometry. As-prepared films exhibited low surface roughness with the area roughness parameter Sq being on average of 0.799 nm and 0.33 nm for SiO2 and TiO2, respectively.

  9. Sol-gel processed Cu2SnS3 films for photovoltaics

    NASA Astrophysics Data System (ADS)

    Dias, Sandra; Banavoth, Murali; Krupanidhi, S. B.

    2013-06-01

    Cu2SnS3 films have been processed by the sol-gel route. Differential Scanning Calorimetry (DSC) study was done to observe the phase transformations and to ascertain the deposition temperature. X-ray diffraction (XRD) confirms the phase formation of Cu2SnS3 . The texture coefficient analysis shows the preferential orientation of the (112) facet. Scanning electron microscopy reveals the morphology of the film. Energy Dispersive Spectroscopy (EDS) was used for compositional studies. Raman spectrum shows the peaks corresponding to the tetragonal phase of Cu2SnS3.

  10. Scanning electron microscopy analysis of sol-gel derived biocompatible glass

    NASA Astrophysics Data System (ADS)

    Holmes-Smith, A. S.; Hungerford, G.; Uttamlal, M.; Amaro, M.; Martins, P.; McBrearty, L.; Love, G.; Ferreira, M. I. C.

    2008-08-01

    Bioactive silica gels/polymer systems have been produced using a sol-gel route and their bio-compatibility has been investigated by immersing them in simulated body fluid (SBF). The porous monoliths have been characterised by SEM and EDX analysis where images obtained show pores on the surface of 10-200 μm. The silica gels are not homogeneous and distinct regions of silicon and calcium are observed. The growth of an apatite layer on the surface of the gels was evident after steeping in SBF.

  11. Aqueous silicates in biological sol-gel applications: new perspectives for old precursors.

    PubMed

    Coradin, Thibaud; Livage, Jacques

    2007-09-01

    Identification of silica sol-gel chemistry with silicon alkoxide hydrolysis and condensation processes is common in modern materials science. However, aqueous silicates exhibit several features indicating that they may be more suitable precursors for specific fields of research and applications related to biology and medicine. In this Account, we illustrate the potentialities of such aqueous precursors for biomimetic studies, bio-hybrid material design, and bioencapsulation routes. We emphasize that the natural relevance, the biocompatibility, and the low ecological impact of silicate chemistry may balance its lack of diversity, flexibility, and processability.

  12. Solid-state NMR study of geopolymer prepared by sol-gel chemistry

    NASA Astrophysics Data System (ADS)

    Tsai, Yi-Ling; Hanna, John V.; Lee, Yuan-Ling; Smith, Mark E.; Chan, Jerry C. C.

    2010-12-01

    Geopolymers are a new class of materials formed by the condensation of aluminosilicates and silicates obtained from natural minerals or industrial wastes. In this work, the sol-gel method is used to synthesize precursor materials for the preparation of geopolymers. The geopolymer samples prepared by our synthetic route have been characterized by a series of physical techniques, including Fourier-transform infrared, X-ray diffraction, and multinuclear solid-state NMR. The results are very similar to those obtained for the geopolymers prepared from natural kaolinite. We believe that our synthetic approach can offer a good opportunity for the medical applications of geopolymer.

  13. Sol-gel matrices for direct colorimetric detection of analytes

    DOEpatents

    Charych, Deborah H.; Sasaki, Darryl; Yamanaka, Stacey

    2000-01-01

    The present invention relates to methods and compositions for the direct detection of analytes using color changes that occur in immobilized biopolymeric material in response to selective binding of analytes to their surface. In particular, the present invention provides methods and compositions related to the encapsulation of biopolymeric material into metal oxide glass using the sol-gel method.

  14. Sol-Gel Matrices For Direct Colorimetric Detection Of Analytes

    DOEpatents

    Charych, Deborah H.; Sasaki, Darryl; Yamanaka, Stacey

    2002-11-26

    The present invention relates to methods and compositions for the direct detection of analytes using color changes that occur in immobilized biopolymeric material in response to selective binding of analytes to their surface. In particular, the present invention provides methods and compositions related to the encapsulation of biopolymeric material into metal oxide glass using the sol-gel method.

  15. Process of forming a sol-gel/metal hydride composite

    DOEpatents

    Congdon, James W.

    2009-03-17

    An external gelation process is described which produces granules of metal hydride particles contained within a sol-gel matrix. The resulting granules are dimensionally stable and are useful for applications such as hydrogen separation and hydrogen purification. An additional coating technique for strengthening the granules is also provided.

  16. ARSENIC REMOVAL USING SOL-GEL SYNTHESIZED TITANIUM DIOXIDE NANOPARTICLES

    EPA Science Inventory

    In this study, the effectiveness of TiO2 nanoparticles in arsenic adsorption was examined. TiO2 particles (LS) were synthesized via sol-gel techniques and characterized for their crystallinity, surface area and pore volume. Batch adsorption studies were perf...

  17. Protein interactions with nanoporous sol-gel derived bioactive glasses.

    PubMed

    Lin, Sen; Van den Bergh, Wouter; Baker, Simon; Jones, Julian R

    2011-10-01

    Sol-gel derived bioactive glasses are excellent candidates for bone regenerative implant materials as they bond with bone, stimulate bone growth and degrade in the body. Their interactions with proteins are critical to understanding their performance after implantation. This study focuses on the interactions between fibrinogen and sol-gel glass particles of the 70S30C (70 mol.% SiO(2), 30 mol.% CaO composition). Sol-gel silica and melt-derived Bioglass® were also used for comparison. Fibrinogen penetration into the nanoporous glasses was observed by live tracking the fluorescent-labelled fibrinogen with confocal microscopy. The effect of pore size on protein penetration was investigated. Nanoporous networks with modal pore diameters larger than 6 nm were accessible to fibrinogen. When the modal nanopore diameter was decreased to 2 nm or less, the penetration of fibrinogen was inhibited. The surface properties of the glasses, which can be modulated by media pH, glass composition and final stabilisation temperature in the sol-gel process, have effects on fibrinogen adsorption via long-range Coulombic forces before the adsorption and via short-range interactions such as hydrogen bonding after the adsorption.

  18. Photolithography fabrication of sol-gel ridge waveguides

    NASA Astrophysics Data System (ADS)

    Sara, Rahmani; Touam, Tahar; Blanchetiere, Chantal; Saddiki, Z.; Saravanamuttu, Kalaichelvi; Du, Xin M.; Chrostowski, Jacek; Andrews, Mark P.; Najafi, S. Iraj

    1998-07-01

    We report on fabrication of ridge waveguides in UV-light sensitive glass sol-gel thin films, deposited on silicon substrate, using a simple photolithography process. The single-layer films are prepared at low temperature and deep UV-light (DUV) is employed to make the waveguides. The effect of fabrication parameters on waveguide shape is investigated.

  19. Inorganic Sensing Using Organofunctional Sol-Gel Materials

    PubMed Central

    Carrington, Nathan A.; Xue, Zi-Ling

    2007-01-01

    This Account describes recent work in the development and applications of sol-gel sensors for concentrated strong acids/bases and metal ions. The use of sol-gel films doped with organic indicators for the optical sensing of concentrated strong acids (HCl 1-10 M) and bases (NaOH 1-10 M) has been explored, and the development of dual optical sensor approaches for ternary systems (HCl-salt-H2O and NaOH-alcohol-H2O) to give acid and salt as well as base and alcohol concentrations is discussed. The preparation of transparent, ligand-grafted sol-gel monoliths is also described, and their use in the analysis of both metal cations (Cu2+) and anions [Cr(VI)] is presented. A new model using both metal ion diffusion and immobilization by the ligands in such monoliths has been developed to give metal concentrations using the optical monolith sensors. In addition to optical sensing, a method utilizing ligand-grafted sol-gel films for analyte preconcentration in the electrochemical determination of Cr(VI) has been explored and is discussed. PMID:17465520

  20. Bioactive glass nanoparticles obtained through sol-gel chemistry.

    PubMed

    Lukowiak, Anna; Lao, Jonathan; Lacroix, Josephine; Nedelec, Jean-Marie

    2013-07-28

    Different sol-gel strategies based on the Stöber method are proposed enabling preparation of nanoparticles of SiO2-CaO bioactive glass with different size, narrow size distribution and good dispersion capability. Eu(3+)-doped glass nanoparticles with luminescent properties can also be obtained.

  1. Safe and Environmentally Acceptable Sol-gel Derived Pyrophoric Pyrotechnics

    SciTech Connect

    Simspon, R L; Satcher, J H; Gash, A

    2004-06-10

    It was demonstrated that highly porous sol-gel derived iron (III) oxide materials could be reduced to sub-micron-sized metallic iron by heating the materials to intermediate temperatures in a hydrogen atmosphere. Through a large number of experiments complete reduction of the sol-gel based materials was realized with a variety of hydrogen-based atmospheres (25-100% H{sub 2} in Ar, N{sub 2}, CO{sub 2}, or CO) at intermediate temperatures (350 C to 700 C). All of the resulting sol-gel-derived metallic iron powders were ignitable by thermal methods, however none were pyrophoric. For comparison several types of commercial micron sized iron oxides Fe2O3, and NANOCAT were also reduced under identical conditions. All resulting materials were characterized by thermal gravimetric analysis (TGA), differential thermal analysis (DTA), powder X-ray diffraction (PXRD), as well as scanning and transmission electron microscopies (SEM and TEM). In addition, the reduction of the iron oxide materials was monitored by TGA. In general the sol-gel materials were more rapidly reduced to metallic iron and the resulting iron powders had smaller particle sizes and were more easily oxidized than the metallic powders derived from the micron sized materials. The lack of pyrophoricity of the smaller fine metallic powders was unexpected and may in part be due to impurities in the materials that create a passivation layer on the iron. Several recommendations for future study directions on this project are detailed.

  2. Sol-gel derived planar waveguides for sensor applications

    NASA Astrophysics Data System (ADS)

    Karasinski, Pawel; Zielonka, Iwona

    2003-09-01

    The paper presents investigation results on the application of sol-gel technology for the production of planar waveguides. These waveguides are produced in a two-component system SiO2:TiO2. We discussed application potentials of the produced layers and presented the results of theoretical analysis involving future structures.

  3. Application of energy-dispersive X-ray elemental mapping to probe the homogeneity of sol-gel derived YBa{sub 2}Cu{sub 3}O{sub 7-{delta}} and related phases

    SciTech Connect

    Houk, C.S.; Burgoine, G.A.; Page, C.J.

    1995-04-01

    The authors describe results obtained using energy dispersive X-ray (EDX) elemental mapping to probe the homogeneity of YBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}. Sol-gel synthesis and conventional solid-state synthesis of the ceramic with firing to 950{degrees}C and sol-gel synthesis with firing at 700{degrees}C are the synthetic routes considered. It was found that the low temperature sol-gel method yields high-quality YBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} provided the firing stage is of sufficient duration.

  4. A general nonaqueous sol-gel route to g-C3N4-coupling photocatalysts: the case of Z-scheme g-C3N4/TiO2 with enhanced photodegradation toward RhB under visible-light.

    PubMed

    Liu, Xu; Chen, Nan; Li, Yuxiu; Deng, Dongyang; Xing, Xinxin; Wang, Yude

    2016-12-22

    The g-C3N4-coupling TiO2 photocatalysts with controllable particle size as well as the interface contact were prepared by a general nonaqueous sol-gel method. The structural and morphological features of g-C3N4/TiO2 were investigated through the X-ray diffraction, Fourier transformed infrared spectra, scanning electron microscopy and transmission electron microscopy, respectively. It is found the TiO2 nanoparticles with a size of 7.3 ± 1.6 nm are uniformly anchored on the surface of the g-C3N4 nanosheets in isolation. The photocatalytic properties of as-prepared g-C3N4/TiO2 were tested by degradation of Rhodamine B (RhB) under visible light, and an enhanced activity is observed. The mechanism of the enhanced activity was further investigated through N2 adsorption-desorption isotherms, UV-vis spectra, photoluminescence spectra, photoelectrochemical measurements, radical trapping experiments and X-ray photoelectron spectroscopy. Furthermore, the photocatalytic performances of obtained g-C3N4/TiO2 under sunlight were also evaluated in aspects of degradation efficiency and stability. The results indicate that the obtained g-C3N4/TiO2 is one promising photocatalyst for practical applications. The study of as-prepared g-C3N4/TiO2 also implies that the present method could be a general route of g-C3N4-coupling photocatalysts.

  5. A general nonaqueous sol-gel route to g-C3N4-coupling photocatalysts: the case of Z-scheme g-C3N4/TiO2 with enhanced photodegradation toward RhB under visible-light

    PubMed Central

    Liu, Xu; Chen, Nan; Li, Yuxiu; Deng, Dongyang; Xing, Xinxin; Wang, Yude

    2016-01-01

    The g-C3N4-coupling TiO2 photocatalysts with controllable particle size as well as the interface contact were prepared by a general nonaqueous sol-gel method. The structural and morphological features of g-C3N4/TiO2 were investigated through the X-ray diffraction, Fourier transformed infrared spectra, scanning electron microscopy and transmission electron microscopy, respectively. It is found the TiO2 nanoparticles with a size of 7.3 ± 1.6 nm are uniformly anchored on the surface of the g-C3N4 nanosheets in isolation. The photocatalytic properties of as-prepared g-C3N4/TiO2 were tested by degradation of Rhodamine B (RhB) under visible light, and an enhanced activity is observed. The mechanism of the enhanced activity was further investigated through N2 adsorption-desorption isotherms, UV-vis spectra, photoluminescence spectra, photoelectrochemical measurements, radical trapping experiments and X-ray photoelectron spectroscopy. Furthermore, the photocatalytic performances of obtained g-C3N4/TiO2 under sunlight were also evaluated in aspects of degradation efficiency and stability. The results indicate that the obtained g-C3N4/TiO2 is one promising photocatalyst for practical applications. The study of as-prepared g-C3N4/TiO2 also implies that the present method could be a general route of g-C3N4-coupling photocatalysts. PMID:28004826

  6. A general nonaqueous sol-gel route to g-C3N4-coupling photocatalysts: the case of Z-scheme g-C3N4/TiO2 with enhanced photodegradation toward RhB under visible-light

    NASA Astrophysics Data System (ADS)

    Liu, Xu; Chen, Nan; Li, Yuxiu; Deng, Dongyang; Xing, Xinxin; Wang, Yude

    2016-12-01

    The g-C3N4-coupling TiO2 photocatalysts with controllable particle size as well as the interface contact were prepared by a general nonaqueous sol-gel method. The structural and morphological features of g-C3N4/TiO2 were investigated through the X-ray diffraction, Fourier transformed infrared spectra, scanning electron microscopy and transmission electron microscopy, respectively. It is found the TiO2 nanoparticles with a size of 7.3 ± 1.6 nm are uniformly anchored on the surface of the g-C3N4 nanosheets in isolation. The photocatalytic properties of as-prepared g-C3N4/TiO2 were tested by degradation of Rhodamine B (RhB) under visible light, and an enhanced activity is observed. The mechanism of the enhanced activity was further investigated through N2 adsorption-desorption isotherms, UV-vis spectra, photoluminescence spectra, photoelectrochemical measurements, radical trapping experiments and X-ray photoelectron spectroscopy. Furthermore, the photocatalytic performances of obtained g-C3N4/TiO2 under sunlight were also evaluated in aspects of degradation efficiency and stability. The results indicate that the obtained g-C3N4/TiO2 is one promising photocatalyst for practical applications. The study of as-prepared g-C3N4/TiO2 also implies that the present method could be a general route of g-C3N4-coupling photocatalysts.

  7. New insights into uranium (VI) sol-gel processing

    SciTech Connect

    King, C.M.; Thompson, M.C.; Buchanan, B.R. ); King, R.B. . Dept. of Chemistry); Garber, A.R. . Dept. of Chemistry)

    1990-01-01

    Nuclear Magnetic Resonance (NMR) investigations on the Oak Ridge National Laboratory process for sol-gel synthesis of microspherical nuclear fuel (UO{sub 2}), has been extremely useful in sorting out the chemical mechanism in the sol-gel steps. {sup 13}C, {sup 15}N, and {sup 1}H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C{sub 6}H{sub 12}N{sub 4}) has revealed near quantitative stability of this adamantane-like compound in the sol-gel process, contrary to its historical role as an ammonia source for gelation from the worldwide technical literature. {sup 17}O NMR of uranyl (UO{sub 2}{sup ++}) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, ((UO{sub 2}){sub 3}({mu}{sub 3}-O)({mu}{sub 2}-OH){sub 3}){sup +}, induced by basic hydrolysis with the HMTA gelation agent. Spectroscopic results will be presented to illustrate that trimer condensation occurs during sol-gel processing leading to layered polyanionic hydrous uranium oxides in which HMTAH{sup +} is occluded as an intercalation'' cation. Subsequent sol-gel processing of microspheres by ammonia washing results in in-situ exchange and formation of a layered hydrous ammonium uranate with a proposed structural formula of (NH{sub 4}){sub 2} ((UO{sub 2}){sub 8} O{sub 4} (OH){sub 10}) {center dot} 8H{sub 2}O. This compound is the precursor to sintered UO{sub 2} ceramic fuel. 23 refs., 10 figs.

  8. Microstructural and antibacterial properties of zinc-substituted cobalt ferrite nanopowders synthesized by sol-gel methods

    NASA Astrophysics Data System (ADS)

    Sanpo, Noppakun; Berndt, Christopher C.; Wang, James

    2012-10-01

    Zinc-substituted cobalt ferrite nanopowders were prepared via a sol-gel route using citric acid as a chelating agent. The influence of zinc concentration on the microstructure, crystal structure, surface wettability, surface roughness, and antibacterial property of zinc-substituted cobalt ferrite nanopowders was investigated systematically. The substitution of zinc influences slightly the microstructure, surface wettability, surface roughness, and crystal structure but strongly affects the antibacterial property of the cobalt ferrite nanopowders.

  9. A new approach to prepare nanoscopic rare earth metal fluorides: the fluorolytic sol-gel synthesis of ytterbium fluoride.

    PubMed

    Schmidt, L; Dimitrov, A; Kemnitz, E

    2014-06-25

    A new approach for the preparation of approx. 5 nm sized ytterbium fluoride nanoparticles based on the fluorolytic sol-gel route is reported. DLS, TEM, IR and XRD were used to characterize the particles as well as the aging behavior of the sols. Furthermore, a new Yb(III) complex was isolated from the precursor solution and characterized by X-ray single crystal structure determination.

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

    NASA Technical Reports Server (NTRS)

    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.

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

    NASA Technical Reports Server (NTRS)

    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.

  12. Calcium hydroxyapatite, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2} ceramics prepared by aqueous sol-gel processing

    SciTech Connect

    Bogdanoviciene, Irma; Beganskiene, Aldona; Tonsuaadu, Kaia; Glaser, Jochen; Meyer, H.-Juergen . E-mail: juergen.meyer@uni-tuebingen.de; Kareiva, Aivaras . E-mail: aivaras.kareiva@chf.vu.lt

    2006-09-14

    Aqueous sol-gel chemistry routes based on ammonium-hydrogen phosphate as the phosphorus precursor and calcium acetate monohydrate as source of calcium ions have been developed to prepare calcium hydroxyapatite samples with different morphological properties. In the sol-gel processes, an aqueous solutions of ethylene diamine tetra-acetic acid (EDTA) or tartaric acid (TA) as complexing agents were added to the reaction mixture. The monophasic Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2} samples were obtained by calcination of precursor gels for 5 h at 1000 deg. C. The phase transformations, composition and micro-structural features in the polycrystalline samples were studied by thermoanalytical methods (TGA/DTA), infrared spectroscopy (IR), X-ray powder diffraction analysis (XRD) and scanning electron microscopy (SEM). It was shown that adjusting the nature of complexing agent in the aqueous sol-gel processing can be used to control the morphology of the ceramic samples.

  13. Molecularly imprinted sol-gel nanotubes membrane for biochemical separations.

    PubMed

    Yang, Huang-Hao; Zhang, Shu-Qiong; Yang, Wei; Chen, Xiao-Lan; Zhuang, Zhi-Xia; Xu, Jin-Gou; Wang, Xiao-Ru

    2004-04-07

    In this study, we report a simple procedure for applying molecular imprinting functional groups to the inner surfaces of the template-synthesized sol-gel nanotubes for chemical separation of estrone. The silica nanotubes were synthesized within the pores of nanopore alumina template membranes using a sol-gel method by simultaneous hydrolysis of a silica monomer-imprinted molecule complex and tetraethoxysilane (TEOS). A covalent imprinting strategy was employed by generating a sacrificial spacer through the reaction of the isocyanate group of 3-(triethoxysilyl)propyl isocyanate and a phenol moiety of estrone to form a thermally cleavable urethane bond. This allowed us to remove the imprinted estrone by simple thermal reaction and to simultaneously introduce functional groups into the cavity formed by the silica nanotubes. Experiments indicated that estrone could be bound selectively by such an approach and have a binding affinity of 864 +/- 137 (n = 3).

  14. Optical detection of parasitic protozoa in sol-gel matrices

    NASA Astrophysics Data System (ADS)

    Livage, Jacques; Barreau, J. Y.; Da Costa, J. M.; Desportes, I.

    1994-10-01

    Whole cell parasitic protozoa have been entrapped within sol-gel porous silica matrices. Stationary phase promastigote cells of Leishmania donovani infantum are mixed with a silica sol before gelation occurs. They remain trapped within the growing oxide network and their cellular organization appears to be well preserved. Moreover protozoa retain their antigenic properties in the porous gel. They are still able to detect parasite specific antibodies in serum samples from infected patients via an enzyme linked immunosorbent assay (ELISA). Antigen- antibody associations occurring in the gel are optically detected via the reactions of a peroxidase conjugate with ortho-phenylenediamine leading to the formation of a yellow coloration. A clear-cut difference in optical density is measured between positive and negative sera. Such an entrapment of antigenic species into porous sol-gel matrices avoids the main problems due to non specific binding and could be advantageously used in diagnostic kits.

  15. Tunable Optical Properties of Metal Nanoparticle Sol-Gel Composites

    NASA Technical Reports Server (NTRS)

    Smith, David D.; Snow, Lanee A.; Sibille, Laurent; Ignont, Erica

    2001-01-01

    We demonstrate that the linear and non-linear optical properties of sol-gels containing metal nanoparticles are highly tunable with porosity. Moreover, we extend the technique of immersion spectroscopy to inhomogeneous hosts, such as aerogels, and determine rigorous bounds for the average fractional composition of each component, i.e., the porosity of the aerogel, or equivalently, for these materials, the catalytic dispersion. Sol-gels containing noble metal nanoparticles were fabricated and a significant blue-shift in the surface plasmon resonance (SPR) was observed upon formation of an aerogel, as a result of the decrease in the dielectric constant of the matrix upon supercritical extraction of the solvent. However, as a result of chemical interface damping and aggregation this blue-shift does not strictly obey standard effective medium theories. Mitigation of these complications is achieved by avoiding the use of alcohol and by annealing the samples in a reducing atmosphere.

  16. Nanostructured Energetci Matreials with sol-gel Chemistry

    SciTech Connect

    Gash, A; Satcher, J; Simpson, R; Clapsaddle, B

    2003-11-18

    The utilization of nanomaterials in the synthesis and processing of energetic materials (i.e., pyrotechnics, explosives, and propellants) is a relatively new area of science and technology. Previous energetic nanomaterials have displayed new and potentially beneficial properties, relative to their conventional analogs. Unfortunately some of the energetic nanomaterials are difficult and or expensive to produce. At LLNL we are studying the application of sol-gel chemical methodology to the synthesis of energetic nanomaterials components and their formulation into energetic nanocomposites. Here sol-gel synthesis and formulation techniques are used to prepare Fe{sub 2}O{sub 3}/Al pyrotechnic nanocomposites. The preliminary characterization of their thermal properties and the degree of mixing between fuel and oxidizer phases is contrasted with that of a conventional pyrotechnic mixture.

  17. Synthesis of zirconium oxide nanoparticle by sol-gel technique

    SciTech Connect

    Lim, H. S.; Ahmad, A.; Hamzah, H.

    2013-11-27

    Zirconium oxide nanoparticle is synthesized using sol-gel technique. Various mole ratio of ammonia solution and nitric acid relative to zirconium propoxide is added in the reaction to study the effect on the crystallinity and particle size on zirconium oxide particle. Zirconium oxide synthesized with nitric acid have the smallest particle size under FESEM image and show the increasing formation of crystalline tetragonal phase under XRD diffractogram.

  18. Sol-Gel Thin Films for Plasmonic Gas Sensors.

    PubMed

    Della Gaspera, Enrico; Martucci, Alessandro

    2015-07-13

    Plasmonic gas sensors are optical sensors that use localized surface plasmons or extended surface plasmons as transducing platform. Surface plasmons are very sensitive to dielectric variations of the environment or to electron exchange, and these effects have been exploited for the realization of sensitive gas sensors. In this paper, we review our research work of the last few years on the synthesis and the gas sensing properties of sol-gel based nanomaterials for plasmonic sensors.

  19. Sol-Gel Thin Films for Plasmonic Gas Sensors

    PubMed Central

    Della Gaspera, Enrico; Martucci, Alessandro

    2015-01-01

    Plasmonic gas sensors are optical sensors that use localized surface plasmons or extended surface plasmons as transducing platform. Surface plasmons are very sensitive to dielectric variations of the environment or to electron exchange, and these effects have been exploited for the realization of sensitive gas sensors. In this paper, we review our research work of the last few years on the synthesis and the gas sensing properties of sol-gel based nanomaterials for plasmonic sensors. PMID:26184216

  20. New developments for sol-gel film and fiber processing

    SciTech Connect

    Hurd, A.J.

    1995-03-01

    New insights into the development of microstructure in sol-gel films have recently been revealed by several diagnostic techniques, including imaging ellipsometry, {open_quotes}chemical imaging{close_quotes} by fluorescent tracers, light scattering from capillary waves, and finite-element modeling. The evolution of porosity during the continuous transition from dilute sol to porous solid in restricted geometries such as films and fibers is becoming clearer through fundamental understanding of evaporation dynamics and capillarity.

  1. Sol-gel synthesis and characterization of undoped and Al-doped ZnO thin films for memristive application

    NASA Astrophysics Data System (ADS)

    Ayana, Dawit G.; Prusakova, Valentina; Collini, Cristian; Nardi, Marco V.; Tatti, Roberta; Bortolotti, Mauro; Lorenzelli, Leandro; Chiappini, Andrea; Chiasera, Alessandro; Ferrari, Maurizio; Lunelli, Lorenzo; Dirè, Sandra

    2016-11-01

    The Sol-gel route is a versatile method to fabricate multi-layer, dense and homogeneous ZnO thin films with a controlled thickness and defects for a memristive application. In this work, sol-gel derived multi-layer undoped and Al-doped ZnO thin films were prepared by a spin-coating technique on SiO2/Ti/Pt and silica glass substrates. The effect of both Al doping and curing conditions on the structural and morphological features of ZnO films was investigated by complementary techniques, including electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, micro-Raman spectroscopy, and X-ray diffraction analysis. Electrical measurements were performed on SiO2/Ti/Pt/ZnO/Pt(dishes) and SiO2/Ti/Pt/ZnO(Al)/Pt(dishes) fabricated memristive cells and preliminary current-voltage curves were acquired.

  2. Synthesis of 45S5 Bioglass® via a straightforward organic, nitrate-free sol-gel process.

    PubMed

    Rezabeigi, Ehsan; Wood-Adams, Paula M; Drew, Robin A L

    2014-07-01

    More than four decades after the discovery of 45S5 Bioglass® as the first bioactive material, this composition is still one of the most promising materials in the tissue engineering field. Sol-gel-derived bioactive glasses generally possess improved properties over other bioactive glasses, because of their highly porous microstructure and unique surface chemistry which accelerate hydroxyapatite formation. In the current study, a new combination of precursors with lactic acid as the hydrolysis catalyst have been employed to design an organic, nitrate-free sol-gel procedure for synthesizing of 45S5 Bioglass®. This straightforward route is able to produce fully amorphous submicron particles of this glass with an appropriately high specific surface area on the order of ten times higher than that of the melt-derived glasses. These characteristics are expected to lead to rapid hydroxyapatite formation and consequently more efficient bone bonding.

  3. Structural investigations of sol-gel-derived LiYF{sub 4} and LiGdF{sub 4} powders

    SciTech Connect

    Lepoutre, S.; Boyer, D. Potdevin, A.; Dubois, M.; Briois, V.; Mahiou, R.

    2007-11-15

    A soft synthesis route based on the sol-gel process was used for preparing rare-earth tetrafluoride powders from alkoxide precursors. In-situ fluorination was performed by decomposition of a fluorine containing organic compound named 1,1,1-trifluoro-5-methyl-2,4-hexanedione when sintering the as-prepared xerogel to produce crystallized samples. Both to insure complete departure of organic residues as well as to avoid any oxidation into oxyfluoride, annealing treatment was carried out under fluorine atmosphere. Free-oxygen content of resulting samples was evidenced by infrared and Raman spectroscopies. X-ray absorption spectroscopies (XAS) and {sup 19}F nuclear magnetic resonance (NMR) studies showed that samples heat treated at 300 deg. C are already crystallized but for a full crystallization in LiGdF{sub 4} and LiYF{sub 4} a thermal treatment at 550 deg. C is needed. Temperature dependence of powder morphology was analyzed by scanning electron microscopy (SEM). - Graphical abstract: The sol-gel route is a soft process, which allows developing versatile-shaped compounds. A fluorine organic compound named 1,1,1-trifluoro-5-methyl-2,4-hexadione was used to synthesis LiGdF{sub 4} and LiYF{sub 4} powders based on the sol-gel method. These materials can be used as host lattices for rare-earth ions to provide phosphors.

  4. Sol-Gel Processing of Neodymia-Silica Glass

    NASA Astrophysics Data System (ADS)

    Pope, Edward John Andrew

    Silica glass containing neodymium is a potentially important laser glass because of its low thermal expansion, and high temperature stability. The sol-gel method is highly advantageous in that it permits the uniform distribution of relatively large concentrations of neodymium in a silica host with respect to conventional processing techniques. In the research herein described, the formation of neodymia-silica gels and glasses and the evolution of structure as a function of heat treatment temperature from the liquid state to the glassy state is discussed. A thorough review of the fundamentals of sol-gel processing, many of which were developed as direct result of this research effort, is presented with an emphasis on gel structural evolution. Inasmuch as sol-gel is an aqueous solution based process, the significant problem of hydroxyl contamination is explored. Two methods of OH removal, by chlorination at elevated temperatures and "In Situ dehydroxylization" are examined and compared. The fluorescence and optical properties of neodymia -silica glass is presented and compared with other laser glasses doped with neodymium. For the first time a tentative structural model of the local environment of neodymium in silica glass is proposed.

  5. Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

    NASA Technical Reports Server (NTRS)

    Chu, Chung-tse; Zheng, Haixing

    1996-01-01

    Advanced materials play an important role in the development of electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. The sol-gel process is a versatile solution for use in the fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. This processing technique is particularly useful in producing porous materials with high surface area and low density, two of the most desirable characteristics for electrode materials. In addition,the porous surface of gels can be modified chemically to create tailored surface properties, and inorganic/organic micro-composites can be prepared for improved material performance device fabrication. Applications of several sol-gel derived electrode materials in different energy storage devices are illustrated in this paper. V2O5 gels are shown to be a promising cathode material for solid state lithium batteries. Carbon aerogels, amorphous RuO2 gels and sol-gel derived hafnium compounds have been studied as electrode materials for high energy density and high power density electrochemical capacitors.

  6. Piezoelectric Sol-Gel Composite Film Fabrication by Stencil Printing.

    PubMed

    Kaneko, Tsukasa; Iwata, Kazuki; Kobayashi, Makiko

    2015-09-01

    Piezoelectric films using sol-gel composites could be useful as ultrasonic transducers in various industrial fields. For sol-gel composite film fabrication, the spray coating technique has been used often because of its adaptability for various substrates. However, the spray technique requires multiple spray coating processes and heating processes and this is an issue of concern, especially for on-site fabrication in controlled areas. Stencil printing has been developed to solve this issue because this method can be used to fabricate thick sol-gel composite films with one coating process. In this study, PbTiO3 (PT)/Pb(Zr,Ti)O3 (PZT) films, PZT/PZT films, and Bi4Ti3O12 (BiT)/PZT films were fabricated by stencil printing, and PT/ PZT films were also fabricated using the spray technique. After fabrication, a thermal cycle test was performed for the samples to compare their ultrasonic performance. The sensitivity and signal-to-noise-ratio (SNR) of the ultrasonic response of PT/PZT fabricated by stencil printing were equivalent to those of PT/PZT fabricated by the spray technique, and better than those of other samples between room temperature and 300°C. Therefore, PT/PZT films fabricated by stencil printing could be a good candidate for nondestructive testing (NDT) ultrasonic transducers from room temperature to 300°C.

  7. Sol-gel optical coatings for lasers, 3

    SciTech Connect

    Floch, H.G.; Belleville, P.F.; Priotton, J.J.; Pegon, P.M.; Dijonneau, C.S.; Guerain, J.

    1995-12-01

    The planned megajoule-class neodymium-glass laser system will be the world`s largest. The proposed CEL-V design, based on the use of 240 beams, will use 50--150 times more optical material than did Phebus. Almost 10,000 m{sup 2} of coated area are required for optical coatings; this is a factor of almost 500 increase over Phebus. Lens, flashlamp, blastshield, harmonic converter, debris shield, window and cavity-end mirror coatings by the sol-gel process represent >96% of the entire coated area. The remaining <4% are high-rejection-ratio polarizers, pick-off cavity mirrors and transport mirrors. Cost estimates show that, for coating deposition, the sol-gel technique provides considerable saving compared to the more conventional e-beam deposition technique. Highly reflective and polarizing sol-gel-derived optical coatings have been prepared and tested for the proposed French megajoule neodymium-glass laser. Laser damage studies are reported here.

  8. Development of polymeric materials for sol-gel waveguides

    NASA Astrophysics Data System (ADS)

    Kusevic, Maja; Hiltunen, Marianne

    2002-06-01

    The scalability to mass production and low cost are two driving forces towards multimode waveguide technologies. Organic-inorganic hybrid materials realized by sol-gel technology are promising choices for the fabrication of integrated optical circuits. This paper describes fabrication and characterization of the photo-patternable materials that are based on the sol-gel technology. The materials can be processed directly, using UV lithographic processing. Tailored polymeric materials are achieved, avoiding the use of the previously developed pre-hydrolyzed zirconium sol-gel precursors, which exhibit a lack of environmental stability. Films, which behave as a negative tone photoresist under UV-exposure, are fabricated by the spin-coating method on various substrates. The procedure shows the possibility for tailoring the refractive index and birefringence of the materials by varying the composition concentrations of the hybrid polymer system. Refractive indices vary from 1.4770 to 1.4950. The synthesized material also exhibits the possibility for birefringence optimization depending on the composition concentrations. The direct lithography process was demonstrated on various substrate materials (i.e., silicon wafer, glass, quartz, as well as flexible plastics, LTCC and semiconductor materials). The film waveguides are characterized by using of prism coupling technique at various wavelengths. The morphology of the optical structures is measured with a white-light interferometer.

  9. Encapsulation of biomaterials in porous glass-like matrices prepared via an aqueous colloidal sol-gel process

    DOEpatents

    Liu, Dean-Mo; Chen, I-Wei

    2001-01-01

    The present invention provides a process for the encapsulation of biologically important proteins into transparent, porous silica matrices by an alcohol-free, aqueous, colloidal sol-gel process, and to the biological materials encapsulated thereby. The process is exemplified by studies involving encapsulated cytochrome c, catalase, myoglobin, and hemoglobin, although non-proteinaceous biomaterials, such as active DNA or RNA fragments, cells or even tissues, may also be encapsulated in accordance with the present methods. Conformation, and hence activity of the biomaterial, is successfully retained after encapsulation as demonstrated by optical characterization of the molecules, even after long-term storage. The retained conformation of the biomaterial is strongly correlated to both the rate of gelation and the subsequent drying speed of the encapsulatng matrix. Moreover, in accordance with this process, gelation is accelerated by the use of a higher colloidal solid concentration and a lower synthesis pH than conventional methods, thereby enhancing structural stability and retained conformation of the biomaterials. Thus, the invention also provides a remarkable improvement in retaining the biological activity of the encapsulated biomaterial, as compared with those involved in conventional alkoxide-based processes. It further provides new methods for the quantitative and qualitative detection of test substances that are reactive to, or catalyzed by, the active, encapsulated biological materials.

  10. Comparative study of nanocrystalline titanium dioxide obtained through sol-gel and sol-gel-hydrothermal synthesis.

    PubMed

    Seck, E I; Doña-Rodríguez, J M; Pulido Melián, E; Fernández-Rodríguez, C; González-Díaz, O M; Portillo-Carrizo, D; Pérez-Peña, J

    2013-06-15

    TiO2 particles were prepared by sol-gel method alone and by sol-gel method combined with hydrothermal treatment. The structural and photocatalytic properties of the two series of photocatalysts were compared. XRD studies revealed that rutilization was faster in the series of photocatalysts, which had been additionally subjected to a hydrothermal process (SG-HT). The hydrothermally treated photocatalysts also displayed a higher specific surface area than those which had only been synthesized using the sol-gel process (SG) and subjected to low calcination temperatures of up to 873 K, while this tendency was inverted at higher temperatures. In accordance with the above observation, the hydrothermally treated series of photocatalysts had a lower particle size than the SG series calcined immediately after the sol-gel process up to 873 K, with this relation being inverted for the highest two temperatures which were studied (973 K and 1023 K) and which saw the commencement of rutilization. Increases in average particle size were observed for both series, with a polyhedral morphology seen as calcination temperature rose. FTIR studies highlighted the presence of the band at 2351 cm(-1) in the SG-HT photocatalysts, characteristic of surface-adsorbed CO2. This was not seen in the SG or P25 photocatalysts. In terms of photoreactivity, the best photocatalyst in the SG-HT series was that calcined at 923 K and in the SG series at 1023 K (SG-1023). Comparing these two photocatalysts and the commercial P25 photocatalyst, SG-1023 was found to be the most photoactive in both the photodegradation and the mineralization of phenol.

  11. Phenyl Functionalized Sol-gel Silica Sorbent for Capillary Microextraction and Chromia-Based Sol-gel Ucon Stationary Phase for Capillary Gas Chromatography

    NASA Astrophysics Data System (ADS)

    McLean, Michael M.

    The first chapter of this thesis presents an introduction to sol-gel methodology whose usefulness as a synthetic route will be demonstrated with two applications in chromatography. The first application involves the fabrication of a capillary micro-extraction (CME) device by coating a phenyl functionalized extracting phase on the inner surface of a fused silica capillary for analyte pre-concentration. The device was coupled on-line to a RP-HPLC system and practicality was demonstrated using allergens as target analytes. The allergens chosen as model analytes are typically found in fragrance products and food. Most of the 26 fragrance allergens that are monitored by various government authorities have a phenyl organic moiety (a strong chromophore), thus making them appropriate probes for exploring the extraction efficiency of the coating using a UV detector. The CME device showed ppt level limit of detection which makes it suitable for trace analyses of allergens and similar compounds in a variety of matrices. The second application explores the feasibility of using sol-gel derived chromia-based stationary phase in gas chromatographic columns. The organic moiety of the stationary phase was derived from Ucon 75-H-90,000 while the inorganic backbone was prepared using chromium(III) dichloride hydroxide - methacrylic acid - aqua complex, 40% in isopropanol/acetone . Usefulness of prepared chromia-based GC stationary phase was examined for petrochemical application. Promising results were obtained using aliphatic-aromatics, polyaromatic hydrocarbons, BTEX test mixture, cycloalkanes, branched alkanes and akylbenzenes. The column was able to perform without degradation despite being rinsed multiples times sequentially with the following solvents: dichloromethane, methanol, water and finally methanol again. Maximum theoretical plate number calculated is around 2,400 plates/m. The plate number clearly needs improvement but is a promising result for the newly explored

  12. Synthesis of phthalocyanine doped sol-gel materials

    NASA Technical Reports Server (NTRS)

    Dunn, Bruce

    1993-01-01

    The synthesis of sol-gel silica materials doped with three different types of metallophthalocyanines has been studied. Homogeneous materials of good optical quality were prepared and the first optical limiting measurements of dyes in sol-gel hosts were carried out. The properties of these solid state limiters are similar to limiters based on phthalocyanine (Pc) in solution. Sol-gel silica materials containing copper, tin and germanium phthalocyanines were investigated. The initial step in all cases was to prepare silica sols by the sonogel method using tetramethoxy silane (TMOS), HCl and distilled water. Thereafter, the synthesis depended upon the specific Pc and its solubility characteristics. Copper phthalocyanine tetrasulfonic acid tetra sodium salt (CuPc4S) is soluble in water and various doping levels (1 x 10 (exp -4) M to 1 x 10 (exp -5) M) were added to the sol. The group IV Pc's, SnPc(OSi(n-hexyl)3)2 and GePc(OSi(n-hexyl)3)2, are insoluble in water and the process was changed accordingly. In these cases, the compounds were dissolved in THF and then added to the sol. The Pc concentration in the sol was 2 x 10(exp -5)M. The samples were then aged and dried in the standard method of making xerogel monoliths. Comparative nanosecond optical limiting experiments were performed on silica xerogels that were doped with the different metallophthalocyanines. The ratio of the net excited state absorption cross section (sigma(sub e)) to the ground state cross section (sigma(sub g)) is an important figure of merit that is used to characterize these materials. By this standard the SnPc sample exhibits the best limiting for the Pc doped sol-gel materials. Its cross section ratio of 19 compares favorably with the value of 22 that was measured in toluene. The GePc materials appear to not be as useful as those containing SnPc. The GePc doped solids exhibit a higher onset energy (2.5 mj and lower cross section ratio, 7. The CuPc4S sol-gel material has a still lower cross

  13. New insights in the structural and morphological properties of sol-gel deposited ZnO multilayer films

    NASA Astrophysics Data System (ADS)

    Demes, T.; Ternon, C.; Riassetto, D.; Roussel, H.; Rapenne, L.; Gélard, I.; Jimenez, C.; Stambouli, V.; Langlet, M.

    2016-08-01

    This study shows how the structural and morphological properties of sol-gel deposited ZnO films can be precisely tuned and selectively controlled. For that purpose, ZnO films have been deposited through a multilayer sol-gel route using solutions of zinc acetate dihydrate (ZAD) diluted in 1-butanol. The opto-geometrical, morphological, and structural properties of these films have been thoroughly studied in relation to the ZAD concentration in butanol, number of deposited single-layers, and heat-treatment conditions. On this basis, different physical processes occurring over the multilayer deposition procedure have been discussed to explain how the experimental parameters influence the film properties and enable to tune the grain size, texture coefficient, and surface coverage rate in a wide range of values. This work is a first step toward the optimized growth of ZnO nanowires on sol-gel films and their subsequent integration in 2D or 3D nanowire-based biosensors.

  14. High-coercivity CoFe2O4 thin films on Si substrates by sol-gel

    NASA Astrophysics Data System (ADS)

    Tang, Xianwu; Jin, Linghua; Wei, Renhuai; Zhu, Xiaoguang; Yang, Jie; Dai, Jianming; Song, Wenhai; Zhu, Xuebin; Sun, Yuping

    2017-01-01

    CoFe2O4 (CFO) thin films with high coercivity HC are desirable in applications. The difficulty in achieving large-area CFO thin films with high coercivity by sol-gel has hindered the development of CFO thin films. Herein, polycrystalline CFO thin films with the room temperature out-of-plane and in-plane coercivity HC respectively reached ~5.9 and 3.6 kOe has been achieved on the silicon substrate by sol-gel. The room-temperature maximum magnetic energy product (BH)max and remanence ratio Mr/Ms are of 1.66 MG Oe and 0.58 respectively, which are also the largest values amongst the CFO thin films prepared by solution methods. At the same time, annealing temperature and thickness effects on the HC, (BH)max and Mr/Ms of the derived CFO thin films have been investigated. It is observed that grain size and residual tensile strain in the derived films play an important role in the variations of HC and Mr/Ms. These results will provide an effective route for fabricating larger-area high-coercivity CFO thin films with low-cost by sol-gel on silicon wafers.

  15. Comparing nanostructured hydroxyapatite coating on AZ91 alloy samples via sol-gel and electrophoretic deposition for biomedical applications.

    PubMed

    Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan

    2014-12-01

    Magnesium is one of the most critical elements in hard tissues regeneration and therefore causes speeding up the restoration of harmed bones, while high deterioration rate of magnesium in body fluid restricts it to be used as biodegradable implants. Alloying magnesium with some relatively nobler metals such as aluminium, zinc, rare earth elements, magnesium-bioceramics composites, and surface modification techniques are some of the routes to control magnesium corrosion rate. In this study AZ91 magnesium alloy had been coated by nanostructured hydroxyapatite via sol-gel dip coating and electrophoretical methods to survey the final barricade properties of the obtained coatings. In order to perform electrophoretic coating, powders were prepared by sol-gel method, and then the powders deposited on substrates utilizing direct current electricity. Zeta potentials of the electrophoresis suspensions were measured to determine a best mode for good quality coatings. Transmission Electron Microscopy (TEM), and Scanning Electron Microscopy (SEM) were used to confirm nanoscale dimension, and the uniformity of the nanostructured hydroxyapatite coating, respectively. Fourier Transform-Infrared and X-ray diffraction analysis were utilized for functional group and phase structure evaluation of the prepared coatings, correspondingly. Electrochemical corrosion tests were performed in SBF at 37±1 (°)C which revealed considerable increase in corrosion protection resistivity and corrosion current density for electrophoretic coated specimens versus sol-gel coated specimens. Results showed that both sol-gel and electrophoretical techniques seem to be suitable to coat magnesium alloys for biomedical applications but electrophoretic coating technique is a better choice due to the more homogeneity and more crystalline structure of the coating.

  16. Sol-gel derived polymer composites for energy storage and conversion

    NASA Astrophysics Data System (ADS)

    Han, Kuo

    Sol-gel process is a simple chemistry to convert the small precursor molecules into an inorganic polymer, which could be applied to synthesize inorganic materials, modify the interface of materials, bridge the organic and inorganic materials, etc. In this dissertation, novel sol-gel derived composites have been developed for high dielectric breakdown capacitors, low high frequency loss capacitors and flexible piezoelectrics. Numerous efforts have been made in the past decades to improve the energy storage capability of composite materials by incorporating nanometer scale ceramic addictives with high dielectric permittivity into dielectric polymers with high breakdown strength. However, most composites suffer from the low breakdown strength and make the potential gain in energy density small. Here, a new chemical strategy is proposed that, through sol-gel reactions between ceramic precursors and functional groups at the end of the functionalized Poly(vinylidene fluoride -co-chlorotrifluoroethylene) chains, amorphous low permittivity ceramics was in-situ generated in the polymer matrix and cross-linked the polymer chains simultaneously. By carefully tuning precursors, the polymer/precursors feeding ratios, a series of nanocomposites were systematically designed. All the samples are comprehensively characterized and the structure-property correlations are well investigated. The optimal samples exhibit higher breakdown strength than the pristine polymer. The enhanced breakdown strength ascribed to low contrast in permittivity, great dispersion and improved electrical and mechanical properties. This newly developed approach has shown great promise for new composite capacitors. The percolative polymer composites have recently exhibited great potential in energy storage due to their high dielectric permittivities at the neighborhood of the percolation threshold. Yet high energy dissipation and poor voltage endurance of the percolative composites resulted from electrical

  17. Sol-Gel Synthesis and Characterization of Neodymium-Ion Doped Nanostructured Titania Thin Films

    DTIC Science & Technology

    2001-11-01

    ABSTRACT Nd doped TiO2 nanostructured thin films were prepared by sol - gel technique on quartz and Si substrates using TiCl 4 precursor. As-deposited...making TiO2 nanostructured thin films on quartz substrates via sol - gel method. The purpose of this study was to determine the effects of preparation...UNCLASSIFIED Defense Technical Information Center Compilation Part Notice ADP012201 TITLE: Sol - Gel Synthesis and Characterization of Neodymium-Ion

  18. Silica fibers doped with erbium ions obtained by the sol gel method

    NASA Astrophysics Data System (ADS)

    Pawlik, Elzbieta; Strek, Wieslaw; Wojcik, Jan; Wojciechowski, C.; Malashkevich, G. E.; Melnichenko, I. M.; Poddenezhny, E. N.

    1997-08-01

    The paper presents the optical properties of glasses and optical fibers from quartz glass, obtained by the sol-gel method. A new technique of sol-gel glass preparation is described. Rods were formed from the glass thus produced from which PCS-type fibers were next drawn. Using the same sol-gel technology, the erbium-doped quartz glasses were obtained. The transmission and luminescence characteristics were measured for the glasses as well as for fibers drawn from them.

  19. Durable hydrophobic sol-gel finishing for textiles

    NASA Astrophysics Data System (ADS)

    Vihodceva, S.; Kukle, S.; Bitenieks, J.

    2015-03-01

    The surface of cotton textile was modified to create a water-repellent finishing by depositing a modifying coatings using the sol-gel technique. Treated textiles evaluated using scanning electron microscopy, X-Ray powder diffraction (XRD). The wettability of treated fabrics was characterized by water contact angle and drop test. The results showed that the cotton textile treated with 7.5 wt.% zinc acetate dihydrate sol showed excellent hydrophobic properties, water contact angle could reach 145°C without decreasing after 50 hydrothermal treatment cycles.

  20. Sol Gel-Derived SBA-16 Mesoporous Material

    PubMed Central

    Rivera-Muñoz, Eric M.; Huirache-Acuña, Rafael

    2010-01-01

    The aim of this article is to review current knowledge related to the synthesis and characterization of sol gel-derived SBA-16 mesoporous silicas, as well as a review of the state of the art in this issue, to take stock of knowledge about current and future applications. The ease of the method of preparation, the orderly structure, size and shape of their pores and control, all these achievable through simple changes in the method of synthesis, makes SBA-16 a very versatile material, potentially applicable in many areas of science and molecular engineering of materials. PMID:20957080

  1. Sol-gel-derived AR coatings for solar receivers

    NASA Astrophysics Data System (ADS)

    Ashley, C. S.; Reed, S. T.

    1984-09-01

    A process for applying sol-gel antireflection (AR) coatings to solar receiver envelopes is investigated. The process consists of applying a porous film which is subsequently etched to achieve the optimum AR effect. The result is a single-layer interference film with a reflectance minimum at 550 nm. The solar transmittance of coated tubes is typically increased to 0.05 to 0.97, as compared with 0.91 for uncoated tubes. Coated tubes showed no significant decrease in solar transmittance after 16 weeks of operation in a parabolic trough collector system. Recommendations are included for process improvement before industrial scale-up.

  2. Uncooled microbolometer IR FPA based on sol-gel VOx

    NASA Astrophysics Data System (ADS)

    Ovsyuk, V. N.; Shashkin, V. V.; Dem'yanenko, M. A.; Fomin, B. I.; Vasil'ieva, L. L.; Soloviev, A. P.

    2005-06-01

    The technology of high-quality uncooled focal plane arrays (FPA) fabrication has been developed. Simple and cheap sol-gel technology of thermosensitive vanadium oxide layers preparation is underlain in its basis. Uncooled 160x120 and 320x240 FPA for 8-14 microns spectral range have been fabricated. The noise equivalent temperature difference less than 8OmK has been achieved at frame rate 60 Hz for 160x120 FPA and at use of optics with 1/1 relative aperture.

  3. Preparation and characterisation of novel thick sol-gel titania film photocatalysts.

    PubMed

    Mills, Andrew; Elliott, Nicholas; Hill, George; Fallis, David; Durrant, James R; Willis, Richard L

    2003-05-01

    The preparation and characterization of thick (9 microns), clear, mechanically robust and photocatalytically active films of nanocrystalline anatase titania are described. XRD and SEM analysis show the films comprise 13 nm particles of anatase TiO2. Thin (54 nm) films of the 'paste' TiO2, along with sol-gel titania films made by a more traditional route are also prepared and characterised. All titania films mediate the photocatalytic destruction of stearic acid with a quantum yield of 0.0016 +/- 0.0003, using either 365 nm (i.e. BLB) or 254 nm (germicidal) light. P25 TiO2 films also appear to mediate the same process with a similar formal quantum efficiency. Of all the films tested, the thick paste TiO2 films are the most ideally suited for use with near UV light, for reasons which are discussed. All the titania films tested exhibit photoinduced superhydrophilicity.

  4. Green synthesis of magnetic chitosan nanocomposites by a new sol-gel auto-combustion method

    NASA Astrophysics Data System (ADS)

    Ansari, Fatemeh; Sobhani, Azam; Salavati-Niasari, Masoud

    2016-07-01

    The Fe2O3/CuFe2O4/chitosan nanocomposites have been successfully synthesized via a new sol-gel auto-combustion route. To prepare the nanocomposites, copper ferrite (CuFe2O4) and iron (II) oxide (Fe2O3) nanostructures were first prepared utilizing onion as a green reductant for the first time, and characterized by SEM, TEM, XRD, IR and VSM. Then chitosan was added into the nanostructures dispersed in water. Chitosan was used to functionalize and modify the nanostructures and also to improve surface properties. The nanocomposites were also characterized by several techniques including SEM, TEM, XRD, IR and VSM. The effects of amount of onion and chitosan on the morphology and particle size of nanocomposites were evaluated.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. Sol-gel processes and materials. (Latest citations from the Aerospace database). Published Search

    SciTech Connect

    Not Available

    1994-11-01

    The bibliography contains citations concerning design and development of sol-gel processes and sol-gel derived materials. Sol-gel derived materials include protective and transparent films, ceramic coatings, nanocomposites and microcomposites, porous and dense composites, fiber reinforced composites, oxides, and ductile ceramics. Topics include preparation of high temperature superconducting oxides and films, glass-ceramic composites and ceramic matrix composites for high temperature applications, sol-gel processes for advanced ceramics, coatings on semiconductors, infrared optical coatings, and coatings on carbon/carbon composites. (Contains 250 citations and includes a subject term index and title list.)

  7. Ultrafast Sol-Gel Synthesis of Graphene Aerogel Materials

    SciTech Connect

    Lim, Mathew; Hu, Matthew; Manandhar, Sandeep; Sakshaug, Avery; Strong, Adam; Riley, Leah; Pauzauskie, Peter J.

    2015-12-01

    Graphene aerogels derived from graphene-oxide (GO) starting materials recently have been shown to exhibit a combination of high electrical conductivity, chemical stability, and low cost that has enabled a range of electrochemical applications. Standard synthesis protocols for manufacturing graphene aerogels require the use of sol-gel chemical reactions that are maintained at high temperatures for long periods of time ranging from 12 hours to several days. Here we report an ultrafast, acid-catalyzed sol-gel formation process in acetonitrile in which wet GO-loaded gels are realized within 2 hours at temperatures below 45°C. Spectroscopic and electrochemical analysis following supercritical drying and pyrolysis confirms the reduction of the GO in the aerogels to sp2 carbon crystallites with no residual carbon–nitrogen bonds from the acetonitrile or its derivatives. This rapid synthesis enhances the prospects for large-scale manufacturing of graphene aerogels for use in numerous applications including sorbents for environmental toxins, support materials for electrocatalysis, and high-performance electrodes for electrochemical capacitors and solar cells.

  8. Electrospun sol-gel fibers for fluorescence-based sensing

    NASA Astrophysics Data System (ADS)

    Memisevic, Jasenka; Riley, Lela; Grant, Sheila A.

    2009-05-01

    Fluorescence based biosensors have the ability to provide reliable pathogen detection. However, the performance could be improved by enhancing the effective surface area of the biosensor. We report on a new nanofibrous fluorescencebased biosensor, whereas a sol-gel platform mesh was constructed by utilizing electrospinning techniques. Furthermore, incorporating cetyltrimethylammonium bromide (CTAB) and conducting pore-forming techniques resulted in a high surface area material suitable for biosensor immobilization. The biosensor was designed to detect Helicobacter hepaticus bacterium by sandwiching the pathogen between two antibodies, one labeled with Alexa Fluor 546 fluorescent dye and the other with 20nm Au nanoparticles. In the presence of pathogen, the close proximity of Au nanoparticles quenched the Alexa Fluor fluorescence, suggesting that the electrospun fiber platforms are suitable for sensing H. Hepaticus. Additionally, sol-gel fibers used as biosensor platform have the added benefit of increased immobilization, as fluorescence intensity from immobilized biosensors is 8.5x106 cps higher on fibers than on a flat, non-porous substrate.

  9. Novel hybrid sol-gel materials for smart sensor windows

    NASA Astrophysics Data System (ADS)

    Wencel, Dorota; Higgins, Clare; Guckian, Adrian; McDonagh, Colette; MacCraith, Brian D.

    2005-06-01

    Current sensor trends, such as multianalyte capability, miniaturisation and patternability are important drivers for materials requirements in optical chemical sensors. In particular, issues such as enhanced sensitivity and printablity are key in developing optimised sensor materials for smart windows for bioprocessing applications. This study focuses on combining novel sol-gel-based hybrid matrices with engineered luminescent complexes to produce stable luminescence-based optical sensors with enhanced sensitivity for a range of analytes including oxygen, pH and carbon dioxide. As well as optimising sensor performance, issues such as surface modification of the plastic substrate and compatibility with different deposition techniques were addressed. Hybrid sol-gel matrices were developed using a range of precursors including tetraethoxysilane (TEOS), methyltriethoxysilane (MTEOS), ethyltriethoxysilane (ETEOS), n-propyltriethoxysilane (PTEOS), phenyltriethoxysilane (PhTEOS), and n-octyltriethoxysilane (C8TEOS). Oxygen sensing, based on luminescence quenching of ruthenium phenanthroline complexes, has been realised with each of these hybrid materials. Furthermore, the possibility of immobilising pH-indicators for pH and carbon dioxide sensing has been investigated with some success. In the context of in-situ monitoring of bioprocesses, issues such as humidity interference as well as the chemical robustness of the multianalyte platform, were addressed.

  10. Sol-gel optical coatings for lasers, 2

    SciTech Connect

    Floch, H.G.; Belleville, P.F.; Priotton, J.J.; Pegon, P.M.; Dijonneau, C.S.; Guerain, J.

    1995-11-01

    There are three basic types of antireflective (AR) coatings. The first is a single-layer coating in which the coating index is equal to the square root of the index of the substrate, assuming air is the external medium. The second type is a system of two or more layers of different indexes. The third type is a graded-index system, where the index is uniformly and continuously graded from the substrate to the external medium. Low reflection ranges from narrow for the single-layer to broad for the graded-layer and multilayered with a large number of layers. Four types of sol-gel AR coatings have been developed at CEL-V. They are based on single-layer or multilayer designs. They consist mainly of amorphous silica in the polymeric and/or colloidal state, combined in certain cases with other metallic oxides, binders, fillers, hydrophobic and lubricating agents, and adhesion promoters. These antireflective sol-gel-derived optical coatings have been prepared and tested for the proposed French megajoule neodymium-glass laser.

  11. Processing and Characterization of Sol-Gel Cerium Oxide Microspheres

    SciTech Connect

    McClure, Zachary D.; Padilla Cintron, Cristina

    2016-09-27

    Of interest to space exploration and power generation, Radioisotope Thermoelectric Generators (RTGs) can provide long-term power to remote electronic systems without the need for refueling or replacement. Plutonium-238 (Pu-238) remains one of the more promising materials for thermoelectric power generation due to its high power density, long half-life, and low gamma emissions. Traditional methods for processing Pu-238 include ball milling irregular precipitated powders before pressing and sintering into a dense pellet. The resulting submicron particulates of Pu-238 quickly accumulate and contaminate glove boxes. An alternative and dust-free method for Pu-238 processing is internal gelation via sol-gel techniques. Sol-gel methodology creates monodisperse and uniform microspheres that can be packed and pressed into a pellet. For this study cerium oxide microspheres were produced as a surrogate to Pu-238. The similar electronic orbitals between cerium and plutonium make cerium an ideal choice for non-radioactive work. Before the microspheres can be sintered and pressed they must be washed to remove the processing oil and any unreacted substituents. An investigation was performed on the washing step to find an appropriate wash solution that reduced waste and flammable risk. Cerium oxide microspheres were processed, washed, and characterized to determine the effectiveness of the new wash solution.

  12. Sol-gel applications for ceramic membrane preparation

    NASA Astrophysics Data System (ADS)

    Erdem, I.

    2017-02-01

    Ceramic membranes possessing superior properties compared to polymeric membranes are more durable under severe working conditions and therefore their service life is longer. The ceramic membranes are composed of some layers. The support is the layer composed of coarser ceramic structure and responsible for mechanical durability under filtration pressure and it is prepared by consolidation of ceramic powders. The top layer is composed of a finer ceramic micro-structure mainly responsible for the separation of components present in the fluid to be filtered and sol-gel method is a versatile tool to prepare such a tailor-made ceramic filtration structure with finer pores. Depending on the type of filtration (e.g. micro-filtration, ultra-filtration, nano-filtration) aiming separation of components with different sizes, sols with different particulate sizes should be prepared and consolidated with varying precursors and preparation conditions. The coating of sol on the support layer and heat treatment application to have a stable ceramic micro-structure are also important steps determining the final properties of the top layer. Sol-gel method with various controllable parameters (e.g. precursor type, sol formation kinetics, heat treatment conditions) is a practical tool for the preparation of top layers of ceramic composite membranes with desired physicochemical properties.

  13. Optical materials by a modified sol-gel nanoparticle process

    NASA Astrophysics Data System (ADS)

    Schmidt, Helmut K.; Mennig, Martin

    2000-05-01

    Optical sol-gel materials have been of interest for many years. The reason is that through the preparation of sold with nanoparticulate liquid structures, transparent coatings of many inorganic oxides can be produced. By using oxides for example, with different refractive indices, reflective or antireflective coatings can be fabricated. To obtain stable layers, the gel coating have to be densified at higher temperatures, in general between 400 and 600 degrees C. This may be suitable for glass surfaces, but not for temperature sensitive substrates like plastics. In addition to this, if multilayer coatings have to be produced, between each step a densification process has to be carried out before the net coating step takes place. This leads to an unsatisfying situation if industrial low cost processing is required. In addition to this, the dip coating process is not suitable for high speed or large area coating techniques. This is one of the reasons whey the sol-gel process never has gained a real high significance for industrial coatings on glass and is limited to special products so far.

  14. Sol - Gel synthesis and characterization of magnesium peroxide nanoparticles

    NASA Astrophysics Data System (ADS)

    Jaison, J.; Ashok raja, C.; Balakumar, S.; Chan, Y. S.

    2015-04-01

    Magnesium peroxide is an excellent source of oxygen in agriculture applications, for instance it is used in waste management as a material for soil bioremediation to remove contaminants from polluted underground water, biological wastes treatment to break down hydrocarbon, etc. In the present study, sol-gel synthesis of magnesium peroxide (MgO2) nanoparticles is reported. Magnesium peroxide is odourless; fine peroxide which releases oxygen when reacts with water. During the sol-gel synthesis, the magnesium malonate intermediate is formed which was then calcinated to obtain MgO2 nanoparticles. The synthesized nanoparticles were characterized using Thermo gravimetric -Differential Thermal Analysis (TG- DTA), X-Ray Diffraction studies (XRD) and High Resolution Transmission Electron Microscope (HRTEM). Our study provides a clear insight that the formation of magnesium malonate during the synthesis was due to the reaction between magnesium acetate, oxalic acid and ethanol. In our study, we can conclude that the calcination temperature has a strong influence on particle size, morphology, monodispersity and the chemistry of the particles.

  15. Nanostructured Energetic Materials with Sol-Gel Methods

    SciTech Connect

    Gash, A; Satcher, J; Simpson, R; Clapsaddle, B

    2003-11-25

    The utilization of sol-gel chemical methodology to prepare nanostructured energetic materials as well as the concepts of nanoenergetics is described. The preparation and characterization of two totally different compositions is detailed. In one example, nanostructured aerogel and xerogel composites of sol-gel iron (III) oxide and ultra fine grained aluminum (UFG Al) are prepared, characterized, and compared to a conventional micron-sized Fe{sub 2}O{sub 3}/Al thermite. The exquisite degree of mixing and intimate nanostructuring of this material is illustrated using transmission and scanning electron microscopies (TEM and SEM). The nanocomposite material has markedly different energy release (burn rate) and thermal properties compared to the conventional composite, results of which will be discussed. Small-scale safety characterization was performed aerogels and xerogels of the nanostructured thermite. The second nanostructured energetic material consists of a nanostructured hydrocarbon resin fuel network with fine ammonium perchlorate (NH{sub 4}ClO{sub 4}) oxidizer present.

  16. Nanostructured energetic materials derived from sol-gel chemistry

    SciTech Connect

    Simpson, R L; Tillotson, T M; Hrubesh, L W; Gash, A E

    2000-03-15

    Initiation and detonation properties are dramatically affected by an energetic material's microstructural properties. Sol-gel chemistry allows intimacy of mixing to be controlled and dramatically improved over existing methodologies. One material goal is to create very high power energetic materials which also have high energy densities. Using sol-gel chemistry we have made a nanostructured composite energetic material. Here a solid skeleton of fuel, based on resorcinol-formaldehyde, has nanocrystalline ammonium perchlorate, the oxidizer, trapped within its pores. At optimum stoichiometry it has approximately the energy density of HMX. Transmission electron microscopy indicated no ammonium perchlorate crystallites larger than 20 nm while near-edge soft x-ray absorption microscopy showed that nitrogen was uniformly distributed, at least on the scale of less than 80 nm. Small-angle neutron scattering studies were conducted on the material. Those results were consistent with historical ones for this class of nanostructured materials. The average skeletal primary particle size was on the order of 2.7 nm, while the nanocomposite showed the growth of small 1 nm size crystals of ammonium perchlorate with some clustering to form particles greater than 10 nm.

  17. Sol-gel derived ceramic electrolyte films on porous substrates

    SciTech Connect

    Kueper, T.W.

    1992-05-01

    A process for the deposition of sol-gel derived thin films on porous substrates has been developed; such films should be useful for solid oxide fuel cells and related applications. Yttria-stabilized zirconia films have been formed from metal alkoxide starting solutions. Dense films have been deposited on metal substrates and ceramic substrates, both dense and porous, through dip-coating and spin-coating techniques, followed by a heat treatment in air. X-ray diffraction has been used to determine the crystalline phases formed and the extent of reactions with various substrates which may be encountered in gas/gas devices. Surface coatings have been successfully applied to porous substrates through the control of substrate pore size and deposition parameters. Wetting of the substrate pores by the coating solution is discussed, and conditions are defined for which films can be deposited over the pores without filling the interiors of the pores. Shrinkage cracking was encountered in films thicker than a critical value, which depended on the sol-gel process parameters and on the substrate characteristics. Local discontinuities were also observed in films which were thinner than a critical value which depended on the substrate pore size. A theoretical discussion of cracking mechanisms is presented for both types of cracking, and the conditions necessary for successful thin formation are defined. The applicability of these film gas/gas devices is discussed.

  18. Sol-gel hydroxyapatite coatings on stainless steel substrates.

    PubMed

    Liu, Dean-Mo; Yang, Quanzu; Troczynski, Tom

    2002-02-01

    Thin film hydroxyapatite deposits onto sandblasted 316L stainless steel substrates were prepared using water-based sol-gel technique recently developed in our lab. The coatings were annealed in air at 375 degrees C, 400 degrees C, and 500 degrees C. Phase formation, surface morphology, interfacial microstructure, and interfacial bonding strength of the coatings were investigated. Apatitic structure developed within the coatings while annealing at temperatures > or = 400 degrees C, while those heat-treated at 375 degrees C showed poor crystallinity. The coatings were dense and firmly attached to the underlying substrates, reaching an average bonding strength (as determined through the pull-out test) of 44 MPa. Nano-porous structure was found for the coatings annealed at 500 degrees C, believed to result from grain growth, and causing a slight decrease in the bonding strength. Surface microcracking, although not extensive, occurred after annealing at temperatures > or = 400 degrees C, and was linked to non-uniform thickness of the coating due to roughness of the substrate. A contraction of the coatings as a result of sintering, and phase transition from amorphous (or poor crystalline) to reasonably good crystalline apatite, may be responsible for the loss of structural integrity of the thicker sections of the coatings. It seems quite promising that a dense and adhesive apatite coating can be achieved through water-based sol gel technology after short-term annealing at around 400 degrees C in air.

  19. Preparation of superhydrophobic surface with a novel sol-gel system

    NASA Astrophysics Data System (ADS)

    Su, Dong; Huang, Chengya; Hu, You; Jiang, Qiangwei; Zhang, Long; Zhu, Yunfeng

    2011-11-01

    Sol-gel method is a simple and cheap way to prepare superhydrophobic coatings or films, however, most of the researches on sol-gel focus on silica or ZnO sol-gel. The present paper proposes a novel sol-gel which is made from hydrolysis and condensation of the by-product of polymethylhydrosiloxane (PMHS) reacting with γ-aminopropyltriethoxysilane (KH550). The mechanism of formation of the by-product and the sol-gel is discussed and the by-product is characterized by FT-IR. The mass ratio of KH550/PMHS of the sol-gel influences the water contact angle (WCA) and water sliding angle (WSA) of the film made of spraying the sol-gel to microscope glass. When the mass ratio of KH550/PMHS of the sol-gel reaches 0.25, WCA of the corresponding film is 157° and WSA of it is less than 1°. The mechanism of formation of the sol-gel is discussed, and the size of the sol-gel is characterized by polarization microscope as well. The morphology of the film made of the sol-gel is analyzed by means of scanning electron microscope (SEM). It was found that the diameter of the particle of the superhydrophobic film is about 40 μm, nevertheless, from the larger magnification picture, the particle is found to be composed of micro-balls whose diameter is about 2 μm, and the micro-ball is composed of nano-sphere whose diameter is less than 200 nm.

  20. Manipulation and characterization of thin-film interfacial chemistry: Sol-gel deposition and single molecule tracking experiments

    NASA Astrophysics Data System (ADS)

    Barhoum, Moussa

    Single molecule trajectories of 1,1'-dioctadecyl-3,3,3'3'-tetramethylindocarbo - cyanine perchlorate (DiI) fluorophores diffusing on planar supported 1,2-dimyristoyl-snglycero- 3-phosphocholine (DMPC) lipid bilayers imaged through total internal reflection fluorescence (TIRF) microscopy at different temperatures are investigated. The spatial resolution limit for detecting molecular motion is evaluated by characterizing the apparent motion which arises from the limited signal-to-noise ratio (S/N) of imaged and simulated stationary DiI molecules. Statistical criteria for reliably distinguishing molecular motion from stationary molecules using F-test statistics, including the computation of local signal-to-noise ratios are then established and used for reliably detecting subdiffraction motion of DiI molecules on DMPC. The same single molecule tracking concept is used in investigating the temperature dependence of subdiffraction diffusional confinement of single Rhodamine 6G molecules in polymer brushes of poly (N-isopropylacrylamide), pNIPAAm, above and below its lower critical solution temperature (LCST) of 32°C. Reliably distinguishing subdiffraction molecular motion from stationary events is crucial in validating the application of single molecule tracking experiment in probing nanometersized hydrophobic environments of polymer structure. A versatile and rapid sol-gel technique for the fabrication of high quality one-dimensional photonic bandgap materials was developed. Silica/titania multilayer materials are fabricated by a sol-gel chemistry route combined with dip-coating onto planar or curved substrate. A shock-cooling step immediately following the thin film heat-treatment process is introduced. The versatility of this sol-gel method is demonstrated by the fabrication of various Bragg stack-type materials with fine-tuned optical properties. Measured optical properties show good agreement with theoretical simulations confirming the high quality of these sol-gel

  1. Calcium and phosphate adsorption as initial steps of apatite nucleation on sol-gel-prepared titania surface.

    PubMed

    Coreño, Juan; Martínez, Antonia; Coreño, Oscar; Bolarín, Ana; Sánchez, Félix

    2003-01-01

    Titania powders have been prepared by the sol-gel route from Ti (IV) ethoxide under acidic conditions. Adsorption experiments of calcium and phosphate ions on gel-derived titania suspensions were performed to suggest a likely initial step of apatite growth on its surface. Experiments were performed as a function of time and pH at 37 degrees C with and without NaCl present in the suspensions. Also, zeta (zeta) potential experiments were performed to determine the kind of calcium adsorption. Results suggest that, apparently, calcium and phosphate adsorption can act as two different initial steps for apatite growth.

  2. Influence of processing parameters on the luminescence of sol-gel derived PrPO{sub 4}

    SciTech Connect

    Chadeyron-Bertrand, G. . E-mail: chadeyr@chimtp.univ-bpclermont.fr; Vial, S.; Cellier, J.; Boyer, D.; Mahiou, R.

    2005-09-01

    PrPO{sub 4} synthesis by the sol-gel process was carried out using an alkoxide route. Powders purity and morphology were analyzed by means of X-ray diffraction, laser granulometry and scanning electron microscopy. Moreover, praseodymium fluorescence in that lattice was recorded by laser induced spectroscopy at room temperature. Upon excitation into the {sup 3}P{sub 0} high energy level, emission in the red wavelength range is observed from this state as well as from the {sup 1}D{sub 2} level. Finally, dependence of the phosphorus precursor and hydrolysis rate on the quantum efficiency was investigated.

  3. Sol-gel microextraction phases for sample preconcentration in chromatographic analysis.

    PubMed

    Segro, Scott S; Tran, Minh Phuong; Kesani, Sheshanka; Alhendal, Abdullah; Turner, Erica B

    2010-10-01

    Sol-gel technology provides a simple and reliable method for solid-phase microextraction (SPME) fiber preparation through in situ creation of surface-bonded organic-inorganic hybrid coatings characterized by enhanced thermal stability and solvent-resistance properties that are important for the coupling of SPME with GC and HPLC, respectively. The sol-gel coating technology has led to the development of an extensive array of sol-gel sorbent coatings for SPME. In this article, sol-gel microextraction coatings are reviewed, with particular attention on their synthesis, characterization, and applications in conjunction with GC and HPLC analyses. In addition, the development of sol-gel-coated stir bars, their inherent advantages, and applications are discussed. Next, the development and applications of sol-gel capillary microextraction (CME) in hyphenation with GC and HPLC is extensively reviewed. The newly emerging germania- and titania-based sol-gel microextraction phases look promising, especially in terms of pH and hot solvent stability. Finally, sol-gel monolithic beds for CME are reviewed. Such monolithic beds are in a position to greatly improve the extracting capabilities and enhanced sensitivity in CME.

  4. Bactericidal micron-thin sol-gel films prevent pin tract and periprosthetic infection.

    PubMed

    Qu, Haibo; Knabe, Christine; Burke, Megan; Radin, Shula; Garino, Jonathan; Schaer, Thomas; Ducheyne, Paul

    2014-08-01

    Orthopedic injuries constitute the majority of wounds sustained by U.S. soldiers in recent conflicts. The risk of infection is considerable with fracture fixation devices. In this pilot study, we examined the use of unique bactericidal micron-thin sol-gel films on fracture fixation devices and their ability to prevent and eradicate infections. External fixation was studied with micron-thin sol-gel coated percutaneous pins releasing triclosan and inserted medially into rabbit tibiae. A total of 11 rabbits received percutaneous pins that were either uncoated or sol-gel/triclosan coated. Internal fracture fixation was also studied using sol-gel coated intramedullary (IM) nails releasing vancomycin in the intramedullary tibiae. Six sheep received IM nails that were coated with a sol-gel film that either contained vancomycin or did not contain vancomycin. All animals were challenged with Staphylococcus aureus around the implant. Animals were euthanized at 1 month postoperative. Rabbits receiving triclosan/sol-gel coated percutaneous pins did not show signs of infection. Uncoated percutaneous pins had a significantly higher infection rate. In the sheep study, there were no radiographic signs of osteomyelitis with vancomycin/sol-gel coated IM nails, in contrast to the observations in the control cohort. Hence, the nanostructured sol-gel controlled release technology offers the promise of a reliable and continuous delivery system of bactericidals from orthopedic devices to prevent and treat infection.

  5. Radiation hardening in sol-gel derived Er{sup 3+}-doped silica glasses

    SciTech Connect

    Hari Babu, B. E-mail: matthieu.lancry@u-psud.fr; León Pichel, Mónica; Ollier, Nadège; El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed; Poumellec, Bertrand; Lancry, Matthieu E-mail: matthieu.lancry@u-psud.fr; Ibarra, Angel

    2015-09-28

    The aim of the present paper is to report the effect of radiation on the Er{sup 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{sup 3+}-doped sol-gel silica is found to increase with erbium content. Electron paramagnetic resonance studies reveal the presence of E′{sub 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{sup 3+} to Er{sup 2+} ions. This process occurs in association with the formation of aluminum oxygen hole centers and different intrinsic point defects.

  6. Organoaluminophosphate sol-gel silica glass thin films for integrated optics

    NASA Astrophysics Data System (ADS)

    Touam, Tahar; Milova, Galina; Saddiki, Z.; Fardad, M. A.; Andrews, Mark P.; Juma, Salim K.; Chrostowski, Jacek; Najafi, S. Iraj

    1997-01-01

    We report on the fabrication and characterization of waveguide thin films on silicon by ultraviolet light imprinting in a new photosensitive, organically modified aluminophosphate sol-gel silica glass prepared by a one-step dip-coating process. Appropriate combinations of ultraviolet light exposure time, sol-gel film thickness and postbake parameters produce waveguides suitable for optical telecommunication applications.

  7. Sol-gel based oxidation catalyst and coating system using same

    NASA Technical Reports Server (NTRS)

    Watkins, Anthony N. (Inventor); Leighty, Bradley D. (Inventor); Oglesby, Donald M. (Inventor); Ingram, JoAnne L. (Inventor); Schryer, Jacqueline L. (Inventor)

    2010-01-01

    An oxidation catalyst system is formed by particles of an oxidation catalyst dispersed in a porous sol-gel binder. The oxidation catalyst system can be applied by brush or spray painting while the sol-gel binder is in its sol state.

  8. Sol-Gel Precursors for Ceramics from Minerals Simulating Soils from the Moon and Mars

    NASA Technical Reports Server (NTRS)

    Sibille, Laurent; Gavira-Gallardo, Jose-Antonio; Hourlier-Bahloul, Djamila

    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 some preliminary 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 A12O3 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 simulant soils. Clear sol-gel precursors have been obtained by dissolution of silica from Lunar simulant soil in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Thermogravimetric Analysis and X-ray Photoelectron Spectroscopy were used to characterize the elemental composition and structure of the precursor molecules. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors. In the second set of experiments, we used the same starting materials to synthesize silicate esters in acidified alcohol mixtures. Preliminary results indicate the presence of silicon alkoxides in the product of distillation.

  9. Alkoxide-based precursors for direct electrospinning of alumina fibers

    NASA Astrophysics Data System (ADS)

    Maneeratana, Vasana

    The vision for space exploration in 2004 reinvigorated excitement that was engendered during the 1960's space race. Looking to assist NASA's agency wide mission to develop new technologies to enhance space travel, it is the ultimate goal of this work to support future missions with a hand-held electrospinning apparatus to instantaneously repair existing crucial ceramic fiber structures, such as spacesuits, insulative foams, and tiles. In this research, a new type of precursor is designed based from aluminum alkoxide-based precursors, since alumina serves as a base material for a majority of high-temperature applications. The structure-processing behavior of these precursors is subsequently studied. New precursors of aluminum alkoxides were prepared by modifying solutions; as a result various types of structures were produced, ranging from continuous hollow fibers, continuous solid fibers, or hollow particles. Direct electrospinning with these alkoxide-based precursors yielded an average of 1.9 g/hr of Al2O3, compared to literature with the highest theoretical yield calculated to be 0.68 g/hr. Further exploration of electrospinning parameters found that flow rate directly related to exposure times; therefore fibers were produced in the atmosphere through hydrolysis/condensation with simultaneous solvent evaporation. Furthermore other processing parameters, including the effect of the microstructure due to processing in an electric field were studied. It was found that electrospinning promotes the reaction of the alkoxide, which thereby reduces trapped solvents. As a result of firing schedules, the fibers' hollow features were preserved, and precursors with volatile species resulted in near net shaped fibers. At low firing temperatures, specific surface areas in the range of 330-345 m 2/g were found electrospun fibers. Additionally modified precursors lowered alpha transitions of fibers down to ˜900°C.

  10. Fabrication of advanced electrochemical energy materials using sol-gel processing techniques

    NASA Technical Reports Server (NTRS)

    Chu, C. T.; Chu, Jay; Zheng, Haixing

    1995-01-01

    Advanced materials play an important role in electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. They are being used as both electrodes and electrolytes. Sol-gel processing is a versatile solution technique used in fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. The application of sol-gel processing in the fabrication of advanced electrochemical energy materials will be presented. The potentials of sol-gel derived materials for electrochemical energy applications will be discussed along with some examples of successful applications. Sol-gel derived metal oxide electrode materials such as V2O5 cathodes have been demonstrated in solid-slate thin film batteries; solid electrolytes materials such as beta-alumina for advanced secondary batteries had been prepared by the sol-gel technique long time ago; and high surface area transition metal compounds for capacitive energy storage applications can also be synthesized with this method.

  11. Optical fiber sensor having a sol-gel fiber core and a method of making

    DOEpatents

    Tao, Shiquan; Jindal, Rajeev; Winstead, Christopher; Singh, Jagdish P.

    2006-06-06

    A simple, economic wet chemical procedure is described for making sol-gel fibers. The sol-gel fibers made from this process are transparent to ultraviolet, visible and near infrared light. Light can be guided in these fibers by using an organic polymer as a fiber cladding. Alternatively, air can be used as a low refractive index medium. The sol-gel fibers have a micro pore structure which allows molecules to diffuse into the fiber core from the surrounding environment. Chemical and biochemical reagents can be doped into the fiber core. The sol-gel fiber can be used as a transducer for constructing an optical fiber sensor. The optical fiber sensor having an active sol-gel fiber core is more sensitive than conventional evanescent wave absorption based optical fiber sensors.

  12. Manufacture of Regularly Shaped Sol-Gel Pellets

    NASA Technical Reports Server (NTRS)

    Leventis, Nicholas; Johnston, James C.; Kinder, James D.

    2006-01-01

    An extrusion batch process for manufacturing regularly shaped sol-gel pellets has been devised as an improved alternative to a spray process that yields irregularly shaped pellets. The aspect ratio of regularly shaped pellets can be controlled more easily, while regularly shaped pellets pack more efficiently. In the extrusion process, a wet gel is pushed out of a mold and chopped repetitively into short, cylindrical pieces as it emerges from the mold. The pieces are collected and can be either (1) dried at ambient pressure to xerogel, (2) solvent exchanged and dried under ambient pressure to ambigels, or (3) supercritically dried to aerogel. Advantageously, the extruded pellets can be dropped directly in a cross-linking bath, where they develop a conformal polymer coating around the skeletal framework of the wet gel via reaction with the cross linker. These pellets can be dried to mechanically robust X-Aerogel.

  13. Holographic gratings in hybrid sol-gel films

    NASA Astrophysics Data System (ADS)

    Raschella, R.; Marino, I.-G.; Lottici, P. P.; Bersani, D.; Lorenzi, A.; Montenero, A.

    2003-08-01

    Organic-inorganic films based on SiO2, containing Disperse Red 1 (DR1), carbazole units and 2,4,7-trinitro-9-fluorenone (TNF), have been prepared by a sol-gel technique. Diffraction gratings have been produced through different effects: photoinduced birefringence and photorefractivity, using 488.0 nm and 632.8 nm light, respectively. Pure polarization holographic birefringence gratings have been investigated and diffraction efficiencies higher than those obtained by light intensity modulation have been measured. The study of the temporal behavior of the diffraction efficiencies makes possible the identification of different processes involved in the DR1 molecular orientation: angular hole burning (AHB), angular redistribution (AR), Cis molecules gain has been determined by two-beam coupling (2BC) measurements. The effect of the polarization of the writing beams on the grating and of a circularly polarized photoisomerizing radiation during grating erasure has been interpreted in terms of an orientation contribution to the grating formation.

  14. Photochromic gratings in sol gel films containing diazo sulfonamide chromophore

    NASA Astrophysics Data System (ADS)

    Kucharski, Stanisław; Janik, Ryszard

    2005-09-01

    The photochromic sol-gel hybrid materials were prepared by incorporation of an azo chromophore containing sulfonamide fragment into polysiloxane cross-linked network. The materials were used to form transparent films on glass by spin-coating and/or casting. The reversible change of refraction index of the films on illumination with white light was observed by ellipsometry. The experiments with two beam coupling (TBC) and four wave mixing (4 WM) arrangement with green or blue laser beams as writing beams showed formation of a diffraction grating. The diffraction efficiency of the first order was 0.025-0.038 which yielded refraction index modulation in the range of up to 0.0066.

  15. Sol-gel multilayers applied by a meniscus coating process

    SciTech Connect

    Britten, J.A.; Thomas, I.M.

    1992-03-19

    We describe a meniscus coating method to produce high-laser damage threshold, silica/alumina sol-gel multilayer reflectors on 30 {plus} cm substrates for laser-fusion applications. This process involves forcing a small suspension flow through a porous applicator tube, forming a falling film on the tube. A substrate contacts this film to form a meniscus. Motion of the substrate relative to the applicator entrains a thin film on the substrate, which leaves behind a porous, optical quality film upon solvent evaporation. We develop a solution for the entrained film thickness as a function of geometry, flow and fluid properties by an analysis similar to that of the classical dip-coating problem. This solution is compared with experimental measurements. Also, preliminary results of multilayer coating experiments with a prototype coater are presented, which focus on coating uniformity and laser damage threshold (LDT).

  16. Sol-Gel Glass Holographic Light-Shaping Diffusers

    NASA Technical Reports Server (NTRS)

    Yu, Kevin; Lee, Kang; Savant, Gajendra; Yin, Khin Swe (Lillian)

    2005-01-01

    Holographic glass light-shaping diffusers (GLSDs) are optical components for use in special-purpose illumination systems (see figure). When properly positioned with respect to lamps and areas to be illuminated, holographic GLSDs efficiently channel light from the lamps onto specified areas with specified distributions of illumination for example, uniform or nearly uniform irradiance can be concentrated with intensity confined to a peak a few degrees wide about normal incidence, over a circular or elliptical area. Holographic light diffusers were developed during the 1990s. The development of the present holographic GLSDs extends the prior development to incorporate sol-gel optical glass. To fabricate a holographic GLSD, one records a hologram on a sol-gel silica film formulated specially for this purpose. The hologram is a quasi-random, micro-sculpted pattern of smoothly varying changes in the index of refraction of the glass. The structures in this pattern act as an array of numerous miniature lenses that refract light passing through the GLSD, such that the transmitted light beam exhibits a precisely tailored energy distribution. In comparison with other light diffusers, holographic GLSDs function with remarkably high efficiency: they typically transmit 90 percent or more of the incident lamp light onto the designated areas. In addition, they can withstand temperatures in excess of 1,000 C. These characteristics make holographic GLSDs attractive for use in diverse lighting applications that involve high temperatures and/or requirements for high transmission efficiency for ultraviolet, visible, and near-infrared light. Examples include projectors, automobile headlights, aircraft landing lights, high-power laser illuminators, and industrial and scientific illuminators.

  17. Sol-Gel processing of silica nanoparticles and their applications.

    PubMed

    Singh, Lok P; Bhattacharyya, Sriman K; Kumar, Rahul; Mishra, Geetika; Sharma, Usha; Singh, Garima; Ahalawat, Saurabh

    2014-11-06

    Recently, silica nanoparticles (SNPs) have drawn widespread attention due to their applications in many emerging areas because of their tailorable morphology. During the last decade, remarkable efforts have been made on the investigations for novel processing methodologies to prepare SNPs, resulting in better control of the size, shape, porosity and significant improvements in the physio-chemical properties. A number of techniques available for preparing SNPs namely, flame spray pyrolysis, chemical vapour deposition, micro-emulsion, ball milling, sol-gel etc. have resulted, a number of publications. Among these, preparation by sol-gel has been the focus of research as the synthesis is straightforward, scalable and controllable. Therefore, this review focuses on the recent progress in the field of synthesis of SNPs exhibiting ordered mesoporous structure, their distribution pattern, morphological attributes and applications. The mesoporous silica nanoparticles (MSNPs) with good dispersion, varying morphology, narrow size distribution and homogeneous porous structure have been successfully prepared using organic and inorganic templates. The soft template assisted synthesis using surfactants for obtaining desirable shapes, pores, morphology and mechanisms proposed has been reviewed. Apart from single template, double and mixed surfactants, electrolytes, polymers etc. as templates have also been intensively discussed. The influence of reaction conditions such as temperature, pH, concentration of reagents, drying techniques, solvents, precursor, aging time etc. have also been deliberated. These MSNPs are suitable for a variety of applications viz., in the drug delivery systems, high performance liquid chromatography (HPLC), biosensors, cosmetics as well as construction materials. The applications of these SNPs have also been briefly summarized.

  18. Ionic liquid-mediated sol-gel coatings for capillary microextraction.

    PubMed

    Shearrow, Anne M; Harris, Glenn A; Fang, Li; Sekhar, Praveen K; Nguyen, Ly T; Turner, Erica B; Bhansali, Shekhar; Malik, Abdul

    2009-07-17

    Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. This opportunity, however, has not yet been explored. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. In this work, we developed a method that overcomes this hurdle and provides IL-mediated advanced sol-gel materials for capillary microextraction (CME). We examined two different ILs: (a) a phosphonium-based IL, trihexyltetradecylphosphonium tetrafluoroborate, and (b) a pyridinium-based ionic liquid, N-butyl-4-methylpyridinium tetrafluoroborate. These ILs were evaluated in conjunction with two types of hydroxy-terminated polymers: (a) two Si-OH terminated polymers (PDMS and BMPO), and (b) two C-OH terminated polymers (PEG and polyTHF) that differ in their sol-gel reactivity. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. The IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions in off-line CME-GC compared to analogous sol-gel coatings prepared without any IL in the sol solution. Contrary to this, the IL-mediated sol-gel coatings prepared with C-OH terminated polymers provided lower extraction efficiencies compared to their IL-free counterparts. These observations were explained by (a) lower sol-gel reactivity of C-OH groups in PEG and polyTHF compared to Si-OH groups in PDMS and in hydrolyzed alkoxysilane precursors and (b) extremely high viscosity of ionic liquids. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics

  19. A silica sol-gel design strategy for nanostructured metallic materials.

    PubMed

    Warren, Scott C; Perkins, Matthew R; Adams, Ashley M; Kamperman, Marleen; Burns, Andrew A; Arora, Hitesh; Herz, Erik; Suteewong, Teeraporn; Sai, Hiroaki; Li, Zihui; Werner, Jörg; Song, Juho; Werner-Zwanziger, Ulrike; Zwanziger, Josef W; Grätzel, Michael; DiSalvo, Francis J; Wiesner, Ulrich

    2012-03-18

    Batteries, fuel cells and solar cells, among many other high-current-density devices, could benefit from the precise meso- to macroscopic structure control afforded by the silica sol-gel process. The porous materials made by silica sol-gel chemistry are typically insulators, however, which has restricted their application. Here we present a simple, yet highly versatile silica sol-gel process built around a multifunctional sol-gel precursor that is derived from the following: amino acids, hydroxy acids or peptides; a silicon alkoxide; and a metal acetate. This approach allows a wide range of biological functionalities and metals--including noble metals--to be combined into a library of sol-gel materials with a high degree of control over composition and structure. We demonstrate that the sol-gel process based on these precursors is compatible with block-copolymer self-assembly, colloidal crystal templating and the Stöber process. As a result of the exceptionally high metal content, these materials can be thermally processed to make porous nanocomposites with metallic percolation networks that have an electrical conductivity of over 1,000 S cm(-1). This improves the electrical conductivity of porous silica sol-gel nanocomposites by three orders of magnitude over existing approaches, opening applications to high-current-density devices.

  20. Review and the state of the art: Sol-gel and melt quenched bioactive glasses for tissue engineering.

    PubMed

    Kaur, Gurbinder; Pickrell, Gary; Sriranganathan, Nammalwar; Kumar, Vishal; Homa, Daniel

    2016-08-01

    Biomaterial development is currently the most active research area in the field of biomedical engineering. The bioglasses possess immense potential for being the ideal biomaterials due to their high adaptiveness to the biological environment as well as tunable properties. Bioglasses like 45S5 has shown great clinical success over the past 10 years. The bioglasses like 45S5 were prepared using melt-quenching techniques but recently porous bioactive glasses have been derived through sol-gel process. The synthesis route exhibits marked effect on the specific surface area, as well as degradability of the material. This article is an attempt to provide state of the art of the sol-gel and melt quenched bioactive bioglasses for tissue regeneration. Fabrication routes for bioglasses suitable for bone tissue engineering are highlighted and the effect of these fabrication techniques on the porosity, pore-volume, mechanical properties, cytocompatibilty and especially apatite layer formation on the surface of bioglasses is analyzed in detail. Drug delivery capability of bioglasses is addressed shortly along with the bioactivity of mesoporous glasses. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 1248-1275, 2016.

  1. Structural, textural and morphological characteristics of tannins from Acacia mearnsii encapsulated using sol-gel methods: Applications as antimicrobial agents.

    PubMed

    Dos Santos, Cristiane; Vargas, Álvaro; Fronza, Ney; Dos Santos, João Henrique Zimnoch

    2017-03-01

    Tannins from Acacia mearnsii were encapsulated using four different sol-gel methods acid (SGAR), basic (SGBR), silicate (SGSR) and non-hydrolytic (SGNHR) routes. The hybrid materials were analyzed using a set of techniques to characterize their structure, texture and morphology. The antimicrobial performance of the encapsulated materials was evaluated against different microorganisms (Staphylococcus aureus, Escherichia coli, Aspergillus niger and Candida sp.). The data showed that the encapsulation route significantly affects the characteristics of the resulting hybrid materials. Better functional performances were obtained using the silicate route, which produced mesoporous materials with a small surface area (0.96m(2)g(-1)) and small particle size (<1nm). These characteristics promoted the gradual release of tannins in an aqueous medium and improved their interactions with microorganisms. Furthermore, the process demonstrated the preservation of tannins after synthesis and increased antimicrobial activity (via a controlled tannin release), as demonstrated by the moderate activity against filamentous fungi and yeast.

  2. Ultrasound-assisted sol-gel synthesis of ZrO2.

    PubMed

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

    2017-03-01

    Synthesis of tetragonal ZrO2 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 ZrO2 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.

  3. Mediated patterning of sol-gel thin layers: Shrinkage, decohesion, and lift-off

    NASA Astrophysics Data System (ADS)

    Mikalsen, Erik Arthur

    This thesis explores the unique de-cohesion and lift-off processes that occur during mediated patterning of integrated sol-gel thin films of functional materials. Mediated deposition, an additive patterning approach, was introduced by Jeon et al. (J. Mater. Res., 10[12]: 2996--9 (1995)), where microcontact printing (mu-CP) facilitated the selective transfer of a molecular 'ink' (e.g., octadecyltrichlorosilane, ODTS) to the substrate, and de-cohesion of sol-gel films occurred exclusively above the printed ink regions after heat treatment (<150°C). Patterned sol-gel films of uniform thickness were revealed after facile lift-off of cracked fragments, without the use of etchants. In this thesis, the origin and mechanics of de-cohesion and lift-off were determined through direct observations and measurements. The disparate mechanical behaviors of sol-gel films on functionalized and unmodified surfaces were determined, with emphasis on interfacial strength, in-plane biaxial stress, thin film mechanics, and crack propagation for sol-gel layers on silicon, glass and fused silica substrates. In addition, direct patterning of sol-gel layers was demonstrated for the first time on curved glassy surfaces using mu-CP and mediated patterning methods. The shrinkage and densification of sol-gel layers were determined by in-situ and ex-situ measurements, where a ˜30% decrease in thickness (t) was typical during drying of sol-gel layers (T < 300°C). Constrained shrinkage, resulting from adhesion to the supporting silicon substrate, led to a coherent (crack-free) film with biaxial stresses of ˜200 MPa (t ˜ 50 nm). For ODTS-mediated sol-gel films, however, precise in-situ wafer curvature measurements determined that film stresses never exceeded 75 MPa. Additionally, interfacial adhesive strength between the substrate and the sol-gel film were evaluated for the first time using a unique pulsed-laser stress-wave technique. An adhesive strength threshold of 15 MPa was determined for

  4. Examination of light distribution from sol-gel based applicators for interstitial laser therapy

    NASA Astrophysics Data System (ADS)

    Hołowacz, I.; Ulatowska-Jarża, A.; Podbielska, H.; Garbaczewska, I.

    2006-02-01

    We describe here the construction of sol-gel based applicators for interstitial thermotheraphy. The silica sol-gel coatings were prepared from silicate precursor TEOS (tetraethylorthosilicate) mixed with ethyl alcohol in acid catalyzed hydrolysis. The matrices were produced with various ratios R=5, 10, 20, 32, 50, whereas R denotes the number of solvent molds (here ethanol) to the number of TEOS moles. The spatial light intensity distribution was examined in order to find out the influence of R factor on the light distribution shape. It was shows that the most homogeneous patterns are observed for sol-gel coatings with R factors equal 10 and 20.

  5. Solventless sol-gel chemistry through ring-opening polymerization of bridged disilaoxacyclopentanes

    SciTech Connect

    RAHIMIAN,KAMYAR; LOY,DOUGLAS A.

    2000-05-01

    Ring-opening polymerization (ROP) of disilaoxacyclopentanes has proven to be an excellent approach to sol-gel type hybrid organic-inorganic materials. These materials have shown promise as precursors for encapsulation and microelectronics applications. The polymers are highly crosslinked and are structurally similar to traditional sol-gels, but unlike typical sol-gels they are prepared by an organic base or Bronsted acid (formic or triflic acid), without the use of solvents and water, they have low VOC's and show little shrinkage during processing.

  6. Sol-gel-derived biomaterials of silica and carrageenans.

    PubMed

    Shchipunov, Yurii A

    2003-12-01

    A new precursor, tetrakis(2-hydroxyethyl) orthosilicate (THEOS), introduced by Hoffmann et al. (J. Phys. Chem. B 106 (2002) 1528-1533), was used to synthesize monolithic hybrid biomaterials on the basis of silica and three main types of carrageenans, kappa-, iota-, and lambda-carrageenans. The advantage of THEOS over the currently applied TEOS and TMOS is in its complete solubility in water. This negated the need to add organic solvents, thus excluding a denaturating effect on biopolymers. In their turn, carrageenans introduced into the precursor solution made use of common catalysts unneeded to trigger the sol-gel transition. It was found that they promoted the mineralization, acting as a template for the inorganic component. The kinetics of sol-gel processes, mechanical properties, phase behavior, and structure of novel hybrid biomaterials were studied by dynamic rheology, differential scanning calorimetry, and scanning electron microscopy. The material properties were regulated by both the precursor and carrageenan. The increase of silicate concentration led to a rise in the stiffness and brittleness of the material, whereas the polysaccharide addition made it softer and more elastic. It was shown that the formation and properties of mixed gels were determined by the nature of carrageenan. kappa-Carrageenans brought about shrinkage of hybrid materials that led to water separation, while iota- and lambda-carrageenans did not induce the syneresis. This is in line with the difference in polysaccharide properties when they are in aqueous solutions without silicate. Furthermore, kappa- and iota-carrageenans experienced a thermoreversible phase transition in the hybrid materials owing to the helix-coil transition. This resulted in a step like change in the mechanical properties of mixed systems in the corresponding temperature range. lambda-Carrageenan is a nongelling polysaccharide, which is why the rheological parameters of its hybrid gel were unchanged with the

  7. Optical properties of sol-gel-derived PZT thin films

    NASA Astrophysics Data System (ADS)

    Teowee, Gimtong T.; Boulton, J. M.; Motakef, Sharnaz; Uhlmann, Donald R.; Zelinski, Brian J.; Zanoni, Raymond; Moon, M.

    1992-12-01

    A series of sol-gel derived PT-based films, including PT, PZ, PZT, PLT, PLZ and PLZT, was prepared on platinized Si, fused SiO2 and Corning 7059 substrates. These films were fired at 400 - 700 C for 30 mins. The phase assembly and development were dependent on the precursor chemistries, processing and choice of substrates. The presence of Zr impacted significantly on the crystallization behavior, PbO loss and cracking behavior of the films. Crystallization was severely retarded, especially in Zr-containing PZT films when deposited on amorphous substrates compared to crystalline Pt substrates. Amorphous and crystalline PZT films can be utilized for passive and active optical applications. Waveguiding was achieved in an amorphous PZT 53/47 and a crystalline PLT 28 films and gave attenuation losses of 1.0 and 1.4 dB/cm respectively which represent the lowest values reported to date. The optical properties of the films were investigated using ellipsometry, UV-VIS transmission spectroscopy and waveguide loss measurements. Depending on composition and processing conditions, PZT films (2500 A thick) with refractive indices of 1.60 to 2.33 and absorption edges of 2900 - 3100 A can be obtained. It was ascertained that the resulting interfacial reaction layers between the films and substrates affected considerably the optical properties of thinner films (< 2000 A).

  8. /dopamine films prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Valverde-Aguilar, G.; Prado-Prone, G.; Vergara-Aragón, P.; Garcia-Macedo, J.; Santiago, Patricia; Rendón, Luis

    2014-09-01

    Dopamine was encapsulated into nanoporous amorphous TiO2 matrix by sol-gel method under atmospheric conditions. A second sample was obtained by the addition of the crown-ether 15C5 in this previous sample. Thin films were spin-coated on glass wafers. No heat treatment was employed in both films. All films were characterized using infrared spectroscopy, high resolution transmission electronic microscopy, X-ray diffraction, optical absorption and scanning electronic microscopy. Despite the films prepared with 15C5 were no calcined, a partial crystallization was identified. Anatase and rutile nanoparticles with sizes of 4-5 nm were obtained. Photoconductivity technique was used to determine the charge transport mechanism on these films. Experimental data were fitted with straight lines at darkness and under illumination wavelengths at 320, 400, and 515 nm. It indicates an ohmic behavior. Photovoltaic and photoconductivity parameters were determined from the current density vs. the applied-electrical-field results. Amorphous film has bigger photovoltaic and photoconductive parameters than the partially crystalline film. Results observed in the present investigation prove that the nanoporous TiO2 matrix can protect the dopamine inhibiting its chemical instability. This fact modifies the optical, physical and electrical properties of the film, and is intensified when 15C5 is added.

  9. Sol-gel template synthesis of semiconductor nanostructures

    SciTech Connect

    Lakshmi, B.B.; Dorhout, P.K.; Martin, C.R.

    1997-03-01

    The template method for preparing nanostructures entails synthesis of the desired material within the pores of a nanoporous membrane or other solid. A nonofibril or tubule of the desired material is obtained within each pore. Methods used previously to deposit materials within the pores of such membranes include electrochemical and electroless deposition and in situ polymerization. This paper describes the first use of sol-gel chemistry to prepare semiconductor nanofibrils and tubules within the pores of an alumina template membrane. TiO{sub 2}, WO{sub 3}, and ZnO nanostructures have been prepared. TiO{sub 2} nanofibrils with diameters of 22 nm were found to be single crystals of anatase with the c-axis oriented along the fibril axis. Bundles of these fibrils were also found to be single crystalline, suggesting that the individual fibrils are arranged in a highly organized fashion within the bundle. Finally, 200 nm diameter TiO{sub 2} fibrils were used as photocatalysts for the decomposition of salicylic acid. 30 refs., 8 figs.

  10. Enantioselective, chirally templated sol-gel thin films.

    PubMed

    Fireman-Shoresh, Sharon; Popov, Inna; Avnir, David; Marx, Sharon

    2005-03-02

    Enantioselective surfactant-templated thin films were fabricated through the sol-gel (SG) process. The enantioselectivity is general in the sense that it discriminates between pairs of enantiomers not used for the imprinting process. The chiral cationic surfactant (-)-N-dodecyl-N-methylephedrinium bromide (1) was used as the surfactant template, and after its extraction chiral domains were created. The chiral discriminative feature of these films was examined by challenging with pure enantiomer solutions for rebinding. Selective adsorption was shown using (R)- and (S)-propranolol, (R)-2 and (S)-2, respectively, and (R)- and (S)-2,2,2-trifluoro-1-(9-anthryl)ethanol, (R)-3 and (S)-3, respectively, as the chiral probes. The selective adsorption was measured by fluorescence analysis, and the chiral selectivity factors were found to be 1.6 for 2 and 2.25 for 3. In both cases, (R)-enantiomer was adsorbed preferably. The resulting material was characterized by transmission electron microscopy, by diffraction, and by surface area measurements, and was found to be semicrystalline with short-range ordered domains (50 A) of hexagonal symmetry.

  11. "Non-hydrolytic" sol-gel synthesis of molybdenum sulfides

    NASA Astrophysics Data System (ADS)

    Leidich, Saskia; Buechele, Dominique; Lauenstein, Raphael; Kluenker, Martin; Lind, Cora

    2016-10-01

    Non-hydrolytic sol-gel reactions provide a low temperature solution based synthetic approach to solid-state materials. In this paper, reactions between molybdenum chloride and hexamethyldisilthiane in chloroform were explored, which gave access to both MoS2 and Mo2S3 after heat treatment of as-recovered amorphous samples to 600-1000 °C. Interesting morphologies were obtained for MoS2, ranging from fused spherical particles to well-defined nanoplatelets and nanoflakes. Both 2H- and 3R-MoS2 were observed, which formed thin hexagonal and triangular platelets, respectively. The platelets exhibited thicknesses of 10-30 nm, which corresponds to 15-50 MoS2 layers. No attempts to prevent agglomeration were made, however, well separated platelets were observed for many samples. Heating at 1000 °C led to formation of Mo2S3 for samples that showed well-defined MoS2 at lower temperatures, while less crystalline samples had a tendency to retain the MoS2 structure.

  12. Sol-gel derived electrode materials for supercapacitor applications

    NASA Astrophysics Data System (ADS)

    Lin, Chuan

    1998-12-01

    Electrochemical capacitors have been receiving increasing interest in recent years for use in energy storage systems because of their high energy and power density and long cycle lifes. Possible applications of electrochemical capacitors include high power pulsed lasers, hybrid power system for electric vehicles, etc. In this dissertation, the preparation of electrode materials for use as electrochemical capacitors has been studied using the sol-gel process. The high surface area electrode materials explored in this work include a synthetic carbon xerogel for use in a double-layer capacitor, a cobalt oxide xerogel for use in a pseudocapacitor, and a carbon-ruthenium xerogel composite, which utilizes both double-layer and faradaic capacitances. The preparation conditions of these materials were investigated in detail to maximize the surface area and optimize the pore size so that more energy could be stored while minimizing mass transfer limitations. The microstructures of the materials were also correlated with their performance as electrochemical capacitors to improve their energy and power densities. Finally, an idealistic mathematical model, including both double-layer and faradaic processes, was developed and solved numerically. This model can be used to perform the parametric studies of an electrochemical capacitor so as to gain a better understanding of how the capacitor works and also how to improve cell operations and electrode materials design.

  13. Mesoporous nanocomposite coatings for photonic devices: sol-gel approach

    NASA Astrophysics Data System (ADS)

    Islam, Shumaila; Bidin, Noriah; Riaz, Saira; Suan, Lau Pik; Naseem, Shahzad; Sanagi, Mohd. Marsin

    2016-10-01

    Thermally stable, optically active inorganic nanocomposites, i.e., aluminum-silicate (AS) and silica-titania (ST), are synthesized via acid-catalyzed low-temperature sol-gel method in order to get stable, crack-free coating material for photonic devices. The samples are characterized by atomic force microscope, field emission scanning electron microscope (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett--Teller (BET) surface area, Barrett-Joyner-Halenda (BJH) pore size distribution surface analysis and UV-Vis spectroscopy. Microscopic results show good incorporation of ST and AS particles as composites with grain size within range of 12-17 and 62-109 nm, respectively. EDX analysis substantiated the stoichiometric formation of homogeneous nanocomposites. XRD of the films reveals primary polycrystalline anatase titania phase and mullite phase of ST and AS nanocomposites. FTIR confirms the heterogeneous bond linkage between titania, silica and alumina species. Furthermore, the fabricated samples have mesoporous nature with high surface area, large pore volume and diameter. The tunable refractive index of 1.33-1.35 with high transparency is obtained for synthesized nanocomposites. The experimental findings show that these physically modified and thermally stable alumina- and titania-doped silica-based composite coatings are promising for photonic devices modification.

  14. Processing, properties, and applications of sol-gel silica optics

    NASA Astrophysics Data System (ADS)

    Nogues, Jean-Luc R.; LaPaglia, Anthony J.

    1989-12-01

    For many years the market share maintained by U.S. optics manufacturers has been declining continuously caused in part by intense competition principally from countries in the Far East, and in part by the lack of a highly trained cadre of opticians to replace the current generation. This fact could place in jeopardy the defense system of the United States in case of international war. For example, in 1987, optical glass component imports accounted for approximately 50 percent of the Department of Defense (DOD) consumption. GELTECH's sol-gel technology is a new process for making a high quality optical glass and components for commercial and military uses. This technology offers in addition to being a local source of optics, the possibility to create new materials for high-tech optical applications, and the elimination of the major part of grinding and polishing for which the skill moved off-shore. This paper presents a summary of the solgel technology for the manufacture of high quality optical glass and components. Properties of pure silica glass made by solgel process (Type V and Type VI silicas) are given and include: ultraviolet, visible and near infrared spectrophotometry, optical homogeneity and thermal expansion. Many applications such as near net shape casting or Fresnel lens surface replication are discussed. Several potential new applications offered by the solgel technology such as organic-inorganic composites for non linear optics or scintillation detection are also reported in this paper.

  15. Thin Film Deposition Using SOL-GEL Technology

    NASA Astrophysics Data System (ADS)

    Puyane, R.; Gonzalez-Oliver, C. J. R.

    1983-11-01

    Sol-Gel technology can be used to deposit a wide variety of oxide coatings on substrates such as glass, ceramics or metals. This presentation outlines the fundamentals of the process and the possibilities offered by this technique. Several oxide layers have been prepared in our laboratories including single oxides like SiO2, TiO2, ZrO2, VO2+x, V205, as well as multicomponent systems such as SiO2-Ge02, SiO2-TiO2, SiO2-Y203 and SiO2-TiO2-Al203. The coatings are deposited by dipping the substrate into a solution containing the appropriate organometallic compound with control of the surrounding atmosphere. Subsequent thermal treatments are required to eliminate the volatile solvents, which are physically and chemically absorbed into the oxide layer and to densify the layers. The first thermal treatments are carried out at temperatures up to 150°C. Further treatments up to about 600°C (depending on oxide composition) are necessary to eliminate organic traces and residual moisture as well as to harden further the oxide coating.

  16. Cobalt silicon mixed oxide nanocomposites by modified sol gel method

    NASA Astrophysics Data System (ADS)

    Esposito, Serena; Turco, Maria; Ramis, Gianguido; Bagnasco, Giovanni; Pernice, Pasquale; Pagliuca, Concetta; Bevilacqua, Maria; Aronne, Antonio

    2007-12-01

    Cobalt-silicon mixed oxide materials (Co/Si=0.111, 0.250 and 0.428) were synthesised starting from Co(NO 3) 2·6H 2O and Si(OC 2H 5) 4 using a modified sol-gel method. Structural, textural and surface chemical properties were investigated by thermogravimetric/differential thermal analyses (TG/DTA), XRD, UV-vis, FT-IR spectroscopy and N 2 adsorption at -196 °C. The nature of cobalt species and their interactions with the siloxane matrix were strongly depending on both the cobalt loading and the heat treatment. All dried gels were amorphous and contained Co 2+ ions forming both tetrahedral and octahedral complexes with the siloxane matrix. After treatment at 400 °C, the sample with lowest Co content appeared amorphous and contained only Co 2+ tetrahedral complexes, while at higher cobalt loading Co 3O 4 was present as the only crystalline phase, besides Co 2+ ions strongly interacting with siloxane matrix. At 850 °C, in all samples crystalline Co 2SiO 4 was formed and was the only crystallising phase for the nanocomposite with the lowest cobalt content. All materials retained high surface areas also after treatments at 600 °C and exhibited surface Lewis acidity, due to cationic sites. The presence of cobalt affected the textural properties of the siloxane matrix decreasing microporosity and increasing mesoporosity.

  17. Sol-gel synthesis and catalytic properties of sulfated zirconia

    SciTech Connect

    Li, Binghui; Gonzalez, R.D.

    1996-10-01

    Sulfate zirconia catalysts were prepared using a two-step sol-gel method with zirconium n-propoxide as the alcoxide precursor and a water/alcoxide ratio of 40. The resulting xerogel was pretreated prior to sulfation in flowing He at 385{degrees}C for 3 hours. The sulfation step was performed by immersing the dried xerogel in 15 ml of H{sub 2}SO{sub 4} solution per gram of sample for 15 min followed by drying in an oven at 130{degrees}C for 16 hours. The sulfated zirconia was activated in flowing oxygen at 600{degrees}C for 1 hour. A thermal desorption study of the deactivated catalyst showed two SO{sub 2} (m/e=64) peaks at 600{degrees}C and 900{degrees}C. The SO{sub 2} desorption peak at 600{degrees}C was coincidental with a CO{sub 2} (m/e=44) peak at the same temperature. These results are interpreted in terms of an organo-sulfur complex on the surface of the deactivated catalyst.

  18. Preparation of oxide glasses from metal alkoxides by sol-gel method

    NASA Technical Reports Server (NTRS)

    Kamiya, K.; Yoko, T.; Sakka, S.

    1987-01-01

    An investigation is carried out on the types of siloxane polymers produced in the course of the hydrolysis of silicon tetraethoxide, as well as the preparation of oxide glasses from metal alkoxides by the sol-gel method.

  19. Enhanced piezoelectric performance of composite sol-gel thick films evaluated using piezoresponse force microscopy.

    PubMed

    Liu, Yuanming; Lam, Kwok Ho; Kirk Shung, K; Li, Jiangyu; Zhou, Qifa

    2013-05-14

    Conventional composite sol-gel method has been modified to enhance the piezoelectric performance of ceramic thick films. Lead zirconate titanate (PZT) and lead magnesium niobate-lead titanate (PMN-PT) thick films were fabricated using the modified sol-gel method for ultrasonic transducer applications. In this work, piezoresponse force microscopy was employed to evaluate the piezoelectric characteristics of PZT and PMN-PT composite sol-gel thick films. The images of the piezoelectric response and the strain-electric field hysteresis loop behavior were measured. The effective piezoelectric coefficient (d33,eff) of the films was determined from the measured loop data. It was found that the effective local piezoelectric coefficient of both PZT and PMN-PT composite films is comparable to that of their bulk ceramics. The promising results suggest that the modified composite sol-gel method is a promising way to prepare the high-quality, crack-free ceramic thick films.

  20. Molecular receptors in metal oxide sol-gel materials prepared via molecular imprinting

    DOEpatents

    Sasaki, Darryl Y.; Brinker, C. Jeffrey; Ashley, Carol S.; Daitch, Charles E.; Shea, Kenneth J.; Rush, Daniel J.

    2000-01-01

    A method is provided for molecularly imprinting the surface of a sol-gel material, by forming a solution comprised of a sol-gel material, a solvent, an imprinting molecule, and a functionalizing siloxane monomer of the form Si(OR).sub.3-n X.sub.n, wherein n is an integer between zero and three and X is a functional group capable of reacting with the imprinting molecule, evaporating the solvent, and removing the imprinting molecule to form the molecularly imprinted metal oxide sol-gel material. The use of metal oxide sol-gels allows the material porosity, pore size, density, surface area, hardness, electrostatic charge, polarity, optical density, and surface hydrophobicity to be tailored and be employed as sensors and in catalytic and separations operations.

  1. Dye-doped sol-gel materials for two-photon absorption induced fluorescence

    NASA Astrophysics Data System (ADS)

    Canva, Michael; Roger, Gisèle; Cassagne, Florence; Lévy, Yves; Brun, Alain; Chaput, Frédéric; Boilot, Jean-Pierre; Rapaport, Alexandra; Heerdt, Céline; Bass, Michael

    2002-01-01

    Two-photon absorption (TPA) and subsequent fluorescence properties of laser dyes are retained when doped into solid state sol-gel materials. These properties were demonstrated to be applicable in true 3D displays.

  2. Optical pH detector based on LTCC and sol-gel technologies

    NASA Astrophysics Data System (ADS)

    Tadaszak, R. J.; Łukowiak, A.; Golonka, L. J.

    2013-01-01

    This paper presents an investigation on using sol-gel thin film as a material for sensors application in LTCC (Low Temperature Co-fired Ceramics) technology. This material gives the opportunity to make new, low-cost highly integrated optoelectronic devices. Sensors with optical detection are a significant part of these applications. They can be used for quick and safe diagnostics of some parameters. Authors present a pH detector with the optical detection system made of the LTCC material. The main part of the device is a flow channel with the chamber and sol-gel active material. The silica sol-gel with bromocresol green indicator was used. As the absorbance of sol-gel layer changes with the pH value of a measured medium, the transmitted light power was measured. The pH detector was integrated with the electronic components on the LTCC substrate.

  3. Silica and silica-titania sol-gel materials: synthesis and analytical application.

    PubMed

    Morosanova, Elena I

    2012-12-15

    This review describes last decade progress in the synthesis of sol-gel materials with analytically relevant properties and their application for the determination of metal ions, non-metal and organic compounds. The following types of materials are discussed: silica sol-gel materials doped with various analytical reagents, organofunctional silica sol-gel materials, and silica titania sol-gel materials. The variety of obtained materials allows their application for a wide range of analytical systems: electrochemical sensors, solid phase spectrophotometrical and SIA determination, and also for test determination including the employment of "length-of-stain" indicator tubes. This review surveys the results of studies on mentioned above subjects and summarizes the works accomplished in the field by author's team in Moscow State University.

  4. Application of polyaniline/sol-gel derived tetraethylorthosilicate films to an amperometric lactate biosensor.

    PubMed

    Chaubey, Asha; Pande, K K; Malhotra, B D

    2003-11-01

    The electrochemical entrapment of polyaniline (PANI) onto sol-gel derived tetraethylorthosilicate (TEOS) films deposited onto indium-tin-oxide (ITO) coated glass has been utilized for immobilization of lactate dehydrogenase (LDH). The performance of these sol-gel/PANI/LDH electrodes has been investigated as a function of the lactate concentration, applied potential, pH of the medium and interferents. The amperometric response of the electrodes under optimum conditions exhibited a linear relationship from 1 mM to 4 mM. An attempt has been made to extend the linearity up to 10 mM for lactate by coating an external layer of polyvinyl chloride (PVC) over the sol-gel/PANI/LDH electrodes with a correlation coefficient of 0.89. These sol-gel/PANI/LDH electrodes have a response time of about 60 s, a shelf life of about 8 weeks at 0-4 degrees C and have implications in a lactate biosensor.

  5. Sol-gel coatings for high pressure polarized ^3He nuclear targets

    NASA Astrophysics Data System (ADS)

    Deur, Alexandre; Cates, Gordon D.; Chaput, Julien; Singh, Jaideep; Tobias, William A.

    2001-11-01

    Sol-gel coated glass cells have been shown to exhibit longitudinal lifetimes T1 in excess of 350 hours for ^3He that is polarized by spin-exchange optical pumping.( Ming F. Hsu shape et al, Appl. Phys. Lett.) series 77 (2000) 2069. The sol-gel technique was designed to minimize spin-relaxation due to wall collisions so that only dipole-dipole interactions between colliding ^3He atoms dominate in the relaxation process. Until now, sol-gel technology has not been applied to high pressure ^3He gas targets used in nuclear scattering experiments. Latest developments on incorporating the sol-gel technique in the production of these ^3He targets will be presented.

  6. Application of Sol-Gel Technology to High Pressure Polarized 3HE Nuclear Targets

    NASA Astrophysics Data System (ADS)

    Tobias, W. A.; Cates, G. D.; Chaput, J.; Deur, A.; Rohrbaugh, S.; Singh, J.

    2003-01-01

    High-purity sol-gel solutions have been developed to coat the interior surface of glass vessels used for polarizing 3He by spin-exchange optical pumping. Such cells have been shown to exhibit 3He longitudinal lifetimes T1 in excess of 350 hours1. The sol-gel technique was designed to minimize spin-relaxation due to wall collisions so that only dipole-dipole interactions between colliding 3He atoms dominate in the relaxation process. Until now, sol-gel technology had not been applied to high pressure 3He gas targets used in nuclear scattering experiments. A description of the sol-gel technique and recent developments on its integration into the production of 3He targets will be presented.

  7. Strength of interactions between immobilized dye molecules and sol-gel matrices.

    PubMed

    Ismail, Fanya; Schoenleber, Monika; Mansour, Rolan; Bastani, Behnam; Fielden, Peter; Goddard, Nicholas J

    2011-02-21

    In this paper we present a new theory to re-examine the immobilization technique of dye doped sol-gel films, define the strength and types of possible bonds between the immobilized molecule and sol-gel glass, and show that the immobilized molecule is not free inside the pores as was previously thought. Immobilizing three different pH sensitive dyes with different size and functional groups inside the same sol-gel films revealed important information about the nature of the interaction between the doped molecule and the sol-gel matrix. The samples were characterized by means of ultraviolet-visible spectrophotometer (UV-VIS), thermal gravimetric analysis (TGA), mercury porosimetry (MP), nuclear magnetic resonance spectroscopy ((29)Si NMR) and field-emission environmental scanning electron microscopy (ESEM-FEG). It was found that the doped molecule itself has a great effect on the strength and types of the bonds. A number of factors were identified, such as number and types of the functional groups, overall charge, size, pK(a) and number of the silanol groups which surround the immobilized molecule. These results were confirmed by the successful immobilization of bromocresol green (BCG) after a completely polymerized sol-gel was made. The sol-gel consisted of 50% tetraethoxysilane (TEOS) and 50% methyltriethoxysilane (MTEOS) (w/w). Moreover, the effect of the immobilized molecule on the structure of the sol-gel was studied by means of a leaky waveguide (LW) mode for doped films made before and after polymerization of the sol-gel.

  8. Making MgO/SiO2 Glasses By The Sol-Gel Process

    NASA Technical Reports Server (NTRS)

    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.

  9. Sol-gel hybrid materials for aerospace applications: Chemical characterization and comparative investigation of the magnetic properties

    NASA Astrophysics Data System (ADS)

    Catauro, Michelina; Mozzati, Maria Cristina; Bollino, Flavia

    2015-12-01

    In the material science field, weightless conditions can be successfully used to understand the relationship between manufacturing process, structure and properties of the obtained materials. Aerogels with controlled microstructure could be obtained by sol-gel methods in microgravity environment, simulated using magnetic levitation if they are diamagnetic. In the present work, a sol-gel route was used to synthesize class I, organic-inorganic nanocomposite materials. Two different formulations were prepared: the former consisted in a SiO2 matrix in which different percentages of polyethylene glycol (PEG) were incorporated, the latter was a ZrO2 matrix entrapping different amounts of poly (ε-caprolactone) (PCL). Fourier Transform Infrared Spectroscopy (FT-IR) detected that the organic and the inorganic components in both the formulation interact by means of hydrogen bonds. X-ray diffraction (XRD) analysis highlighted the amorphous nature of the synthesized materials and Scanning Electron Microscope (SEM) showed that they have homogeneous morphology and are nanocomposites. Superconducting Quantum Interference Device (SQUID) magnetometry confirmed the expected diamagnetic character of those hybrid systems. The obtained results were compared to those achieved in previous studies regarding the influence of the polymer amount on the magnetic properties of SiO2/PCL and ZiO2/PEG hybrids, in order to understand how the diamagnetic susceptibility is influenced by variation of both the inorganic matrix and organic component.

  10. Synthesis of sol-gel derived glass powder and in vitro bioactivity property tested in simulated body fluid

    NASA Astrophysics Data System (ADS)

    Fadzli, S. A. Syed Nuzul; Roslinda, S.; Zainuddin, Firuz; Ismail, Hamisah

    2016-11-01

    The objective of this study is to determine the apatite forming ability of sol-gel derived glass based on chemical composition 50%(SiO2)-40%(CaO)-10%(PO4) by examine the reacted sample surface after soaking in simulated body fluid (SBF). The glass was synthesized via an acid catalyzed low temperature sol-gel route, dried, crushed and uniaxial pressed into pellets before finally heated at 600°C to maintain the amorphous nature and to obtain stabilized glass pellets. The bioactivity test of the glass was carried out in vitro by soaking the pellets into simulated body fluid (SBF) for various times up to 14 days. It was revealed that apatite-like structures were rapidly formed on the surface of the glass showed by the glass surface was totally covered with these crystallized apatite within the first 24 hours of immersion. The formation of crystallized carbonated apatite (HCA) was proved within the first 24 hours of immersion via XRD, FTIR and FE-SEM analysis method. Increased in immersion time period to 14 days was significantly effects in enlargement of the apatite particle sizes and transformation these apatite into a typical coral-like apatite structures.

  11. Synthesis and characterization of 8YSZ/5GDC composite and dissimiliar-bulk by sonochemistry assisted sol-gel method

    NASA Astrophysics Data System (ADS)

    Rivai, A. K.; Shabrina, N.; Setiawan, A. R.

    2017-03-01

    Synthesis and characterization of 8YSZ (8%mol Y2O3 – ZrO2) and 5GDC (5%mol Gd2O3–CeO2) combination in the form of composite and dissimilar bulk using sonochemistry assisted sol-gel method have been done. 8YSZ and 5GDC powders were produced from sol-gel route method. Each of the powder was then ultrasonicated for 30 hours with 25kHz±50Hz of frequency and 39% of amplitude. Toluene was used as a solution for the ultrasonication process. 8YSZ/5GDC composite was made by mixing the powders of 50%:50% in weight, and afterward compacted become a pellet. 8YSZ/5GDC dissimilar bulk was made by connected between 8YSZ pellet and 5GDC pellet at a flat part, and afterward re-compacted become a single pellet. Then, the pellets were sintered at 1400°C of temperature for 3 hours. The results showed that the ionic conductivity of the composite is higher than the dissimilar bulk.

  12. Robust aptamer sol-gel solid phase microextraction of very polar adenosine from human plasma.

    PubMed

    Mu, Li; Hu, Xiangang; Wen, Jianping; Zhou, Qixing

    2013-03-01

    Conventional solid phase microextraction (SPME) has a limited capacity to extract very polar analytes, such as adenosine. To solve this problem, aptamer conjugating sol-gel methodology was coupled with an SPME fiber. According to the authors' knowledge, this is the first reported use of aptamer SPME. The fiber of aptamer sol-gel SPME with a mesoporous structure has high porosity, large surface area, and small water contact angle. Rather than employing direct entrapment, covalent immobilization was the dominant method of aptamer loading in sol-gel. Aptamer sol-gel fiber captured a specified analyte from among the analog molecules, thereby, exhibiting an excellent selective property. Compared with commercial SPME fibers, this aptamer fiber was suitable for extracting adenosine, presenting an extraction efficiency higher than 20-fold. The values of repeatability and reproducibility expressed by relative standard deviation were low (9.4%). Interestingly, the sol-gel network enhanced the resistance of aptamer SPME to both nuclease and nonspecific proteins. Furthermore, the aptamer sol-gel fiber was applied in human plasma with LOQ 1.5 μg/L, which is an acceptable level. This fiber also demonstrates durability and regeneration over 20-cycles without significant loss of efficiency. Given the various targets (from metal ions to biomacromolecules and cells) of aptamers, this methodology will extend the multi-domain applications of SPME.

  13. Preparation and antioxidant capacity of element selenium nanoparticles sol-gel compounds.

    PubMed

    Bai, Yan; Qin, Biyin; Zhou, Yanhui; Wang, Yudong; Wang, Zi; Zheng, Wenjie

    2011-06-01

    This paper reported the preparation and antioxidant capacities of element selenium nanoparticles (nanoSe(0))-ascorbic acid (Vc) sol and nanSe(0)/Vc/selenocystine (SeCys) sol-gel compounds. NanoSe(0)-Vc sol was prepared by reduction of selenious dioxide (SeO2) with Vc. In the nanoSe(0)-Vc sol, highly concentrated Vc was also used as a modifier to modulate the diameter of Se(0) nanoparticles in the liquid phase. Then excellent nanoSe(0) sol-gel compounds were obtained by adding SeCys into the nanoSe(0)-Vc sol. The structure of the nanoSe(0)/Vc/SeCys sol-gel compounds was defined, which was constructed via C-Se, Se-H and O=C-Se valences and by interaction between SeCys and Vc via peptide bonds, esterification and dehydration. The antioxidant capacities of the nanoSe(0)-Vc sol and the nanoSe(0)Vc/SeCys sol-gel compounds were estimated by oxygen radical absorption capacity (ORAC) assay. The nanoSe(0)/Vc/SeCys sol-gel compounds possessed a strong antioxidant capacity due to forming the perfect three-dimensional (3D) frameworks structure. The results suggested that the nanoSe(0)-Vc sol and the nanoSe(0)Vc/SeCys sol-gel compounds might be potential medicine, especially antioxidant.

  14. One-step sol-gel imprint lithography for guided-mode resonance structures.

    PubMed

    Huang, Yin; Liu, Longju; Johnson, Michael; C Hillier, Andrew; Lu, Meng

    2016-03-04

    Guided-mode resonance (GMR) structures consisting of sub-wavelength periodic gratings are capable of producing narrow-linewidth optical resonances. This paper describes a sol-gel-based imprint lithography method for the fabrication of submicron 1D and 2D GMR structures. This method utilizes a patterned polydimethylsiloxane (PDMS) mold to fabricate the grating coupler and waveguide for a GMR device using a sol-gel thin film in a single step. An organic-inorganic hybrid sol-gel film was selected as the imprint material because of its relatively high refractive index. The optical responses of several sol-gel GMR devices were characterized, and the experimental results were in good agreement with the results of electromagnetic simulations. The influence of processing parameters was investigated in order to determine how finely the spectral response and resonant wavelength of the GMR devices could be tuned. As an example potential application, refractometric sensing experiments were performed using a 1D sol-gel device. The results demonstrated a refractive index sensitivity of 50 nm/refractive index unit. This one-step fabrication process offers a simple, rapid, and low-cost means of fabricating GMR structures. We anticipate that this method can be valuable in the development of various GMR-based devices as it can readily enable the fabrication of complex shapes and allow the doping of optically active materials into sol-gel thin film.

  15. Preparation and characterization of conductive and transparent ruthenium dioxide sol-gel films.

    PubMed

    Allhusen, John S; Conboy, John C

    2013-11-27

    RuO2 conductive thin films were synthesized using the sol-gel method and deposited onto transparent insulating substrates. The optical transmission, film thickness, surface morphology and composition, resistivity, and spectroelectrochemical performance have been characterized. The optical transmission values of these films ranged from 70 to 89% in the visible region and from 56 to 88% in the infrared region. Resistivity values of the RuO2 sol-gel films varied from 1.02 × 10(-3) to 1.13 Ω cm and are highly dependent on the initial solution concentration of RuO2 in the sol-gel. The RuO2 sol-gel films were used as electrodes for the electrochemical oxidation and reduction of ferrocenemethanol. The electrochemical behavior of our novel RuO2 sol-gel films was compared to that of a standard platinum disk electrode and showed no appreciable differences in the half-wave potential (E1/2). The mechanical and chemical stability of the coatings was tested by physical abrasion and exposure to highly acidic, oxidizing Piranha solution. Repeated exposure to these extreme conditions did not result in any appreciable decline in electrochemical performance. Finally, the use of the novel RuO2 sol-gel conductive and transparent films was demonstrated in a spectroelectrochemistry experiment in which the oxidation and reduction of ferrocenemethanol was monitored via UV-vis spectroscopy as the applied potential was cycled.

  16. One-step sol-gel imprint lithography for guided-mode resonance structures

    NASA Astrophysics Data System (ADS)

    Huang, Yin; Liu, Longju; Johnson, Michael; Hillier, Andrew C.; Lu, Meng

    2016-03-01

    Guided-mode resonance (GMR) structures consisting of sub-wavelength periodic gratings are capable of producing narrow-linewidth optical resonances. This paper describes a sol-gel-based imprint lithography method for the fabrication of submicron 1D and 2D GMR structures. This method utilizes a patterned polydimethylsiloxane (PDMS) mold to fabricate the grating coupler and waveguide for a GMR device using a sol-gel thin film in a single step. An organic-inorganic hybrid sol-gel film was selected as the imprint material because of its relatively high refractive index. The optical responses of several sol-gel GMR devices were characterized, and the experimental results were in good agreement with the results of electromagnetic simulations. The influence of processing parameters was investigated in order to determine how finely the spectral response and resonant wavelength of the GMR devices could be tuned. As an example potential application, refractometric sensing experiments were performed using a 1D sol-gel device. The results demonstrated a refractive index sensitivity of 50 nm/refractive index unit. This one-step fabrication process offers a simple, rapid, and low-cost means of fabricating GMR structures. We anticipate that this method can be valuable in the development of various GMR-based devices as it can readily enable the fabrication of complex shapes and allow the doping of optically active materials into sol-gel thin film.

  17. Structural Modification of Sol-Gel Materials through Retro Diels-Alder Reaction

    SciTech Connect

    SHALTOUT,RAAFAT M.; LOY,DOUGLAS A.; MCCLAIN,MARK D.; PRABAKAR,SHESHASAYANA; GREAVES,JOHN; SHEA,KENNETH J.

    1999-12-08

    Hydrolysis and condensation of organically bridged bis-triethoxysilanes, (EtO){sub 3}Si-R-Si(OEt){sub 3}, results in the formation of three dimensional organic/inorganic hybrid networks (Equation 1). Properties of these materials, including porosity, are dependent on the nature of the bridging group, R. Flexible groups (akylene-spacers longer than five carbons in length) polymerize under acidic conditions to give non-porous materials. Rigid groups (such as arylene-, alkynylene-, or alkenylene) form non-porous, microporous, and macroporous gels. In many cases the pore size distributions are quite narrow. One of the motivations for preparing hybrid organic-inorganic materials is to extend the range of properties available with sol-gel systems by incorporating organic groups into the inorganic network. For example, organically modified silica gels arc either prepared by co-polymerizing an organoalkoxysilane with a silica precursor or surface silylating the inorganic gel. This can serve to increase hydrophobicity or to introduce some reactive organic functionality. However, the type and orientation of these organic functionalities is difficult to control. Furthermore, many organoalkoxysilanes can act to inhibitor even prevent gelation, limiting the final density of organic functionalities. We have devised a new route for preparing highly functionalized pores in hybrid materials using bridging groups that are thermally converted into the desired functionalities after the gel has been obtained. In this paper, we present the preparation and characterization of bridged polysilsesquioxanes with Diels-Alder adducts as the bridging groups from the sol-gel polymerization of monomers 2 and 4. The bridging groups are constructed such that the retro Diela-Alder reaction releases the dienes and leaves the dienophiles as integral parts of the network polymers. In the rigid architecture of a xerogel, this loss of organic functionality should liberate sufficient space to modify the

  18. Novel sol-gel synthesis of acidic MgF(2-x)(OH)(x) materials.

    PubMed

    Wuttke, Stefan; Coman, Simona M; Scholz, Gudrun; Kirmse, Holm; Vimont, Alexandré; Daturi, Maro; Schroeder, Sven L M; Kemnitz, Erhard

    2008-01-01

    Novel magnesium fluorides have been prepared by a new fluorolytic sol-gel synthesis for fluoride materials based on aqueous HF. By changing the amount of water at constant stoichiometric amount of HF, it is possible to tune the surface acidity of the resulting partly hydroxylated magnesium fluorides. These materials possess medium-strength Lewis acid sites and, by increasing the amount of water, Brønsted acid sites as well. Magnesium hydroxyl groups normally have a basic nature and only with this new synthetic route is it possible to create Brønsted acidic magnesium hydroxyl groups. XRD, MAS NMR, TEM, thermal analysis, and elemental analysis have been applied to study the structure, composition, and thermal behaviour of the bulk materials. XPS measurements, FTIR with probe molecules, and the determination of N(2)/Ar adsorption-desorption isotherms have been carried out to investigate the surface properties. Furthermore, activity data have indicated that the tuning of the acidic properties makes these materials versatile catalysts for different classes of reactions, such as the synthesis of (all-rac)-[alpha]-tocopherol through the condensation of 2,3,6-trimethylhydroquinone (TMHQ) with isophytol (IP).

  19. Water-based sol-gel synthesis of hydroxyapatite: process development.

    PubMed

    Liu, D M; Troczynski, T; Tseng, W J

    2001-07-01

    Hydroxyapatite (HA) ceramics were synthesized using a sol-gel route with triethyl phosphite and calcium nitrate as phosphorus and calcium precursors, respectively. Two solvents, water and anhydrous ethanol, were used as diluting media for HA sol preparation. The sols were stable and no gelling occurred in ambient environment for over 5 days. The sols became a white gel only after removal of the solvents at 60 degrees C. X-ray diffraction showed that apatitic structure first appeared at a temperature as low as 350 degrees C. The crystal size and the HA content in both gels increase with increasing calcination temperature. The type of initial diluting media (i.e., water vs. anhydrous ethanol) did not affect the microstructural evolution and crystallinity of the resulting HA ceramic. The ethanol-based sol dip-coated onto a Ti substrate, followed by calcination at 450 degrees C, was found to be porous with pore size ranging from 0.3 to 1 microm. This morphology is beneficial to the circulation of physiological fluid when the coating is used for biomedical applications. The satisfactory adhesion between the coating and substrate suggests its suitability for load-bearing uses.

  20. Low density lipoprotein adsorption on sol-gel derived alumina for blood purification therapy.

    PubMed

    Asano, Takuji; Tsuru, Kanji; Hayakawa, Satoshi; Osaka, Akiyoshi

    2008-01-01

    Among the clinical treatments of Familial Hyper cholesterolemia patients to reduce the concentration of low density lipoprotein (LDL), blood purification therapy is most suitable in which a blood-compatible adsorbent is employed. In the present study, alumina powders were prepared via a sol-gel route to develop a LDL-adsorbent Aluminum tri2-propoxide was hydrolyzed and subsequently calcined up to 1200 degrees C. Surface charge density and pore size distribution were measured, and the phases were identified. The alumina calcined above 400 degrees C had excellent blood compatibility in terms of endogenous clotting parameters, i.e., partial thromboplastin time: (PTT), prothrombin time: (PT), and the amount of fibrinogen: (Fib). The amount of LDL-adsorption (DeltaW(LDL)) increased with the calcining temperature, showing a good linear correlation to surface charge density. The 1200 degrees C sample consisted only of alpha-alumina, and was greatest in DeltaW(LDL). All samples involved pores smaller than 20 nm but not the pores large enough to accommodate LDL molecules (20-25 nm). From those results, it was concluded for the present alumina particles that the surface charge density was the primary factor and that the chemical activity of alpha-alumina also contributed to the excellent LDL-adsorption for the 1200 degrees C sample, while entrapping LDL in the pores was not an active mechanism.

  1. Synthesis and Characterization of Sol-Gel Prepared Silver Nanoparticles

    NASA Astrophysics Data System (ADS)

    Ahlawat, Dharamvir Singh; Kumari, Rekha; Rachna; Yadav, Indu

    2014-03-01

    Silver nanoparticles (SNPs) have been successfully prepared using sol-gel method by annealing the sample at 550°C for 30 min. The SNPs were not confirmed by X-ray diffraction (XRD) analysis when the annealing temperature was considered at 450°C. They were also not confirmed without calcination of the sample. The physical mechanism of silver clusters formation in the densified silica matrix with respect to thermal treatment has been understood. The presence of silver metal in the silica matrix was confirmed by XRD analysis and TEM image of the samples. The average size of nanoparticles dispersed in silica matrix was determined as 10.2 nm by the XRD technique. The synthesized nanocomposites were also characterized by UV-Visible spectroscopy with a peak in the absorption spectra at around 375 nm. The distribution of particle size has been reported here in the range from 8 nm to 25 nm by TEM observations of the sample prepared at 550°C. The spherically smaller size (≈10 nm) SNPs have reported the surface plasmons resonance (SPR) peak less than or near to 400 nm due to blue-shifting and effect of local refractive index. Without annealing the silica samples the absorption spectra does not show any peak around 375 nm. The FTIR spectroscopy of the three types of samples prepared at different temperatures (room temperature, 450°C and 550°C) has also been reported. This spectra have provided the identification of different chemical groups in the prepared samples. It has been predicted that the size of SNPs by XRD, UV-Visible and TEM results have agreed well with each other. It may be concluded that formation of SNPs is a function of annealing temperature.

  2. Development of electrochromic smart windows by sol-gel techniques

    NASA Astrophysics Data System (ADS)

    Munro, Brian; Kraemer, S.; Zapp, P.; Krug, Herbert; Schmidt, Helmut K.

    1997-10-01

    A novel nanocomposite lithium ion-conducting electrolyte has been developed, based on organically modified silanes, which is suitable for application in a sol-gel electrochromic system. The system developed consists of FTO-coated (fluorine doped tin oxide) glass coated with tungsten oxide, WO3, at one side of the device as the electrochromic layer, with a cerium oxide-titanium oxide layer, CeO2-TiO2, acting as ion-storage layer or counter electrode. The adhesive properties of the electrolyte enabled the manufacture of electrochromic devices in a laminated structure: glassFTOWO3nanocomp.elect.CeO2-TiO2FTOglass. The conductivity of the nanocomposite electrolyte system varies between 10-4 and 10-5 Scm-1 at 25 degrees Celsius depending on the exact composition. The temperature dependence of the conductivity exhibits typical Vogel-Tamman-Fulcher (VTF) behavior. The thickness of the electrolyte between the two halves of the device could be adjusted by the use of a spacer technique in the range 10 - 150 micrometer. Optoelectrochemical measurements were conducted on electrochromic devices to study the kinetics of coloration and bleaching as a function of the number of switching cycles. At present, cells are constructed in two formats: 10 multiplied by 15 cm2 and 35 multiplied by 35 cm2. Switching times under one minute were achieved for the smaller format with a corresponding optical modulation between 75% to 20% (at lambda equals 0.633 micrometer). In the case of the larger format the switching time increases to several minutes due to the increase in geometric area.

  3. Sol-gel SiO2 film contained Au/SiO2/quantum dot core/shell/shell nanostructures with plasmonic enhanced photoluminescence.

    PubMed

    Yang, Ping; Zhang, Lipeng; Wang, Yingzi

    2012-12-01

    A sol-gel method has been developed to fabricate functional silica film with Au/SiO2/quantum dot (QD) core/shell/shell nanostructures which exhibited plasmonic enhanced photoluminescence (PL). Au nanoparticles (NPs) were homogeneously coated with a SiO2 shell by an optimal Stöber synthesis. Hydrophobic CdSe/ZnS QDs was transferred into water phase via a ligand exchange by a thin functional SiO2 layer consisted of partially hydrolyzed 3-aminopropyltrimethoxysilane (APS) sol. The Au/SiO2/QD core/shell/shell nanostructure was created by assembling the functional SiO2-coated QDs to the SiO2-coated Au NPs while QDs transferred into water phase. Those partially hydrolyzed APS molecules play an important role for the connection between the QDs and SiO2-coated Au NPs. The Au/SiO2/QD core/shell/shell nanostructures were embedded in functional sol-gel SiO2 films fabricated via spinning and dipping coating, in which the film revealed strong surface plasmon scattering and enhanced PL. Because of the dual functionality, the film is utilizable for various applications including biological and medical sensors, optical devices, and solar cells. This technique can serve as a general route for encapsulating a variety of nanomaterials in sol-gel films.

  4. Antibacterial modification of an injectable, biodegradable, non-cytotoxic block copolymer-based physical gel with body temperature-stimulated sol-gel transition and controlled drug release.

    PubMed

    Wang, Xiaowen; Hu, Huawen; Wang, Wenyi; Lee, Ka I; Gao, Chang; He, Liang; Wang, Yuanfeng; Lai, Chuilin; Fei, Bin; Xin, John H

    2016-07-01

    Biomaterials are being extensively used in various biomedical fields; however, they are readily infected with microorganisms, thus posing a serious threat to the public health care. We herein presented a facile route to the antibacterial modification of an important A-B-A type biomaterial using poly (ethylene glycol) methyl ether (mPEG)- poly(ε-caprolactone) (PCL)-mPEG as a typical model. Inexpensive, commercial bis(2-hydroxyethyl) methylammonium chloride (DMA) was adopted as an antibacterial unit. The effective synthesis of the antibacterial copolymer mPEG-PCL-∼∼∼-PCL-mPEG (where ∼∼∼ denotes the segment with DMA units) was well confirmed by FTIR and (1)H NMR spectra. At an appropriate modification extent, the DMA unit could render the copolymer mPEG-PCL-∼∼∼-PCL-mPEG highly antibacterial, but did not largely alter its fascinating intrinsic properties including the thermosensitivity (e.g., the body temperature-induced sol-gel transition), non-cytotoxicity, and controlled drug release. A detailed study on the sol-gel-sol transition behavior of different copolymers showed that an appropriate extent of modification with DMA retained a sol-gel-sol transition, despite the fact that a too high extent caused a loss of sol-gel-sol transition. The hydrophilic and hydrophobic balance between mPEG and PCL was most likely broken upon a high extent of quaternization due to a large disturbance effect of DMA units at a large quantity (as evidenced by the heavily depressed PCL segment crystallinity), and thus the micelle aggregation mechanism for the gel formation could not work anymore, along with the loss of the thermosensitivity. The work presented here is highly expected to be generalized for synthesis of various block copolymers with immunity to microorganisms. Light may also be shed on understanding the phase transition behavior of various multiblock copolymers.

  5. Entrapment of subtilisin in ceramic sol-gel coating for antifouling applications.

    PubMed

    Regina, Viduthalai Rasheedkhan; Søhoel, Helmer; Lokanathan, Arcot Raghupathi; Bischoff, Claus; Kingshott, Peter; Revsbech, Niels Peter; Meyer, Rikke Louise

    2012-11-01

    Enzymes with antifouling properties are of great interest in developing nontoxic antifouling coatings. A bottleneck in developing enzyme-based antifouling coatings is to immobilize the enzyme in a suitable coating matrix without compromising its activity and stability. Entrapment of enzymes in ceramics using the sol-gel method is known to have several advantages over other immobilization methods. The sol-gel method can be used to make robust coatings, and the aim of this study was to explore if sol-gel technology can be used to develop robust coatings harboring active enzymes for antifouling applications. We successfully entrapped a protease, subtilisin (Savinase, Novozymes), in a ceramic coating using a sol-gel method. The sol-gel formulation, when coated on a stainless steel surface, adhered strongly and cured at room temperature in less than 8 h. The resultant coating was smoother and less hydrophobic than stainless steel. Changes in the coating's surface structure, thickness and chemistry indicate that the coating undergoes gradual erosion in aqueous medium, which results in release of subtilisin. Subtilisin activity in the coating increased initially, and then gradually decreased. After 9 months, 13% of the initial enzyme activity remained. Compared to stainless steel, the sol-gel-coated surfaces with active subtilisin were able to reduce bacterial attachment of both Gram positive and Gram negative bacteria by 2 orders of magnitude. Together, our results demonstrate that the sol-gel method is a promising coating technology for entrapping active enzymes, presenting an interesting avenue for enzyme-based antifouling solutions.

  6. Quasi-one-dimensional nanostructured cobalt (Co) intercalated vanadium oxide (V{sub 2}O{sub 5}): Peroxovanadate sol gel synthesis and structural study

    SciTech Connect

    Langie da Silva, Douglas; Moreira, Eduardo Ceretta; Dias, Fábio Teixeira; Neves Vieira, Valdemar das; Brandt, Iuri Stefani; Cas Viegas, Alexandre da; Pasa, André Avelino

    2015-01-15

    Nanostructured cobalt vanadium oxide (V{sub 2}O{sub 5}) xerogels spread onto crystalline Si substrates were synthesized via peroxovanadate sol gel route. The resulting products were characterized by distinct experimental techniques. The surface morphology and the nanostructure of xerogels correlate with Co concentration. The decrease of the structural coherence length is followed by the formation of a loose network of nanopores when the concentration of intercalated species was greater than 4 at% of Co. The efficiency of the synthesis route also drops with the increase of Co concentration. The interaction between the Co(OH{sub 2}){sub 6}{sup 2+} cations and the (H{sub 2}V{sub 10}O{sub 28}){sup 4−} anions during the synthesis was suggested as a possible explanation for the incomplete condensation of the V{sub 2}O{sub 5} gel. Finally the experimental results points for the intercalation of Co between the bilayers of the V{sub 2}O{sub 5}. In this scenario two possible preferential occupation sites for the metallic atoms in the framework of the xerogel were proposed. - Graphical abstract: Quasi-one-dimensional nanostructured cobalt (Co) intercalated vanadium oxide (V{sub 2}O{sub 5}) nanoribbons synthesized by peroxovanadate sol gel route. - Highlights: • Nanostructured cobalt V{sub 2}O{sub 5} gel spread onto c{sub S}i were synthesized via peroxovanadate sol gel route. • The micro and nanostructure correlates with the cobalt content. • The efficiency of the synthesis route shows to be also dependent of Co content. • The experimental results points for the intercalation of Co between the bilayers of the V{sub 2}O{sub 5} xerogel.

  7. Sol-Gel Technology for Low-VOC, Nonchromated Adhesive Bonding Applications SERDP; Project PP-1113, Task 1

    DTIC Science & Technology

    2006-05-31

    4 6 8 10 Wet Time (WT Abrasive Type (AT) Sol-Gel App. (SG) Paper Grade (PG) A-DT A- AB Dry Time (DT) Abrade Time ( AB ) A-SM Sanding Method (SM) Alloy...Addition of a surfactant to the aqueous-based sol-gel can improve the wettability of the sol-gel solution on titanium and result in a more uniform

  8. Ionic conductivity of Bi{sub 2}Ni{sub x}V{sub 1−x}O{sub 5.5−3x/2} (0.1 ≤ x ≤ 0.2) oxides prepared by a low temperature sol-gel route

    SciTech Connect

    Rusli, Rolan; Patah, Aep Prijamboedi, Bambang Ismunandar; Abrahams, Isaac

    2014-03-24

    Solid oxides fuel cells (SOFCs) is one technology that could contribute toward future sustainable energy. One of the most important components of an SOFC is the electrolyte, which must have high ionic conductivity. Cation substitution of vanadium in Bi{sub 4}V{sub 2}O{sub 11} yields a family of fast oxide ion conducting solids known collectively as the BIMEVOXes (bismuth metal vanadium oxide), which have the potential to be applied as electrolytes in SOFCs. The purpose of this work is to study the effect of Ni concentration, when used as a dopant, on the ionic conductivity of Bi{sub 2}Ni{sub x}V{sub 1−x}O{sub 5.5−3x/2} (BINIVOX) oxides (0.1 ≤ x ≤ 0.2) when prepared by a sol gel method. The gels were calcined at 600 °C for 24 h to produce pure BINIVOX. These oxides were found to exhibit the γ-phase structure with tetragonal symmetry in space group I4/mmm. Ionic conductivity of BINIVOX at 300 °C were 6.9 × 10{sup −3} S cm{sup −1}, 1.2 × 10{sup −3} S cm{sup −1}, and 8.2 × 10{sup −4} S cm{sup −1}, for x = 0.1; 0.15; and 0.2; respectively; and at 600 °C were 1.1 × 10{sup −1} S cm{sup −1}, 5.3 × 10{sup −2} S cm{sup −1}, and 2.8 ×10{sup −2} S cm{sup −1}, for x = 0.1; 0.15; and 0.2; respectively.

  9. Synthesis of nanocrystalline NiCuZn ferrite powders by sol-gel auto-combustion method

    NASA Astrophysics Data System (ADS)

    Yue, Zhenxing; Zhou, Ji; Li, Longtu; Zhang, Hongguo; Gui, Zhilun

    2000-01-01

    A nitrate-citrate gel was prepared from metal nitrates and citric acid by sol-gel process, in order to synthesize Ni 0.25Cu 0.25Zn 0.50Fe 2O 4 ferrite. The thermal decomposition process was investigated by DTA-TG, IR and XRD techniques. The results revealed that the nitrate-citrate gel exhibits self-propagating combustion behavior. After combustion, the gel directly transformed into single-phase, nano-sized NiCuZn ferrite particles with spinel crystal structure. The synthesized powder can be densified at a temperature lower than 900°C. The sintered body possesses fine-grained microstructure, good frequency stability and high-quality factor compared to the sample prepared by conventional ceramic route.

  10. Origin of the high tunability of BaTiSnO3 thin films deposited by sol-gel

    NASA Astrophysics Data System (ADS)

    Mascot, Manuel; Carru, Jean-Claude; Fasquelle, Didier

    2015-10-01

    Ba(Sn0.02Ti0.98)O3 thin films (BTS) were prepared by sol-gel route and deposited by spin-coating on commercial Pt/Ti/SiO2/Si substrates. By modifying the annealing conditions from 750°C at 1 h to 950°C at 15 min, the relative tunability nr at 100°C in the paraelectric state increased from 45 to 70% while the DC dielectric permittivity ɛ‧(0) increased as well. The evolutions of ɛ‧(E) and nr(E) are explained from Devonshire thermodynamic formalism. The very high value of tunability of 70% is explained by the grain size increase of our BTS thin films and the decrease of the dead layer effect when the annealing conditions are optimized.

  11. Recycling of chemicals from alkaline waste generated during preparation of UO 3 microspheres by sol-gel process

    NASA Astrophysics Data System (ADS)

    Kumar, Ashok; Vittal Rao, T. V.; Mukerjee, S. K.; Vaidya, V. N.

    2006-05-01

    Internal gelation process, one of the sol-gel processes for nuclear fuel fabrication, offers many advantages over conventional powder pellet route. However, one of the limitation of the process is generation of large volume of alkaline liquid waste containing hexamethylenetetramine, urea, ammonium nitrate, ammonium hydroxide etc. Presence of ammonium nitrate with hexamethylenetetramine and urea presents a fire hazard which prevents direct disposal of the waste as well as its recycle by evaporation. The paper describes the studies carried out to suitably process the waste. Nitrate was removed from the waste by passing through Dowex 1 × 4 anion exchange resin in OH - form. 1.0 M NaOH was used to regenerate the resin. The nitrate-free waste was further treated to recover and recycle hexamethylenetetramine, urea and ammonium hydroxide for preparation of UO 3 microspheres. The quality of the microspheres obtained was satisfactory. An optimized flow sheet for processing of the waste solution has been suggested.

  12. Preparation and rapid analysis of antibacterial silver, copper and zinc doped sol-gel surfaces.

    PubMed

    Jaiswal, Swarna; McHale, Patrick; Duffy, Brendan

    2012-06-01

    The colonisation of clinical and industrial surfaces with microorganisms, including antibiotic-resistant strains, has promoted increased research into the development of effective antibacterial and antifouling coatings. This study describes the preparation of metal nitrate (Ag, Cu, Zn) doped methyltriethoxysilane (MTEOS) coatings and the rapid assessment of their antibacterial activity using polyproylene microtitre plates. Microtitre plate wells were coated with different volumes of liquid sol-gel and cured under various conditions. Curing parameters were analysed by thermogravimetric analysis (TGA) and visual examination. The optimum curing conditions were determined to be 50-70°C using a volume of 200 μl. The coated wells were challenged with Gram-positive and Gram-negative bacterial cultures, including biofilm-forming and antibiotic-resistant strains. The antibacterial activities of the metal doped sol-gel, at equivalent concentrations, were found to have the following order: silver>zinc>copper. The order is due to several factors, including the increased presence of silver nanoparticles at the sol-gel coating surface, as determined by X-ray photoelectron spectroscopy, leading to higher elution rates as measured by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The use of microtitre plates enabled a variety of sol-gel coatings to be screened for their antibacterial activity against a wide range of bacteria in a relatively short time. The broad-spectrum antibacterial activity of the silver doped sol-gel showed its potential for use as a coating for biomaterials.

  13. Mechanical compatibility of sol-gel annealing with titanium for orthopaedic prostheses.

    PubMed

    Greer, Andrew I M; Lim, Teoh S; Brydone, Alistair S; Gadegaard, Nikolaj

    2016-01-01

    Sol-gel processing is an attractive method for large-scale surface coating due to its facile and inexpensive preparation, even with the inclusion of precision nanotopographies. These are desirable traits for metal orthopaedic prostheses where ceramic coatings are known to be osteoinductive and the effects may be amplified through nanotexturing. However there are a few concerns associated with the application of sol-gel technology to orthopaedics. Primarily, the annealing stage required to transform the sol-gel into a ceramic may compromise the physical integrity of the underlying metal. Secondly, loose particles on medical implants can be carcinogenic and cause inflammation so the coating needs to be strongly bonded to the implant. These concerns are addressed in this paper. Titanium, the dominant material for orthopaedics at present, is examined before and after sol-gel processing for changes in hardness and flexural modulus. Wear resistance, bending and pull tests are also performed to evaluate the ceramic coating. The findings suggest that sol-gel coatings will be compatible with titanium implants for an optimum temperature of 500 °C.

  14. Radiation hardening of sol gel-derived silica fiber preforms through fictive temperature reduction.

    PubMed

    Hari Babu, B; Lancry, Matthieu; Ollier, Nadege; El Hamzaoui, Hicham; Bouazaoui, Mohamed; Poumellec, Bertrand

    2016-09-20

    The impact of fictive temperature (Tf) on the evolution of point defects and optical attenuation in non-doped and Er3+-doped sol-gel silica glasses was studied and compared to Suprasil F300 and Infrasil 301 glasses before and after γ-irradiation. To this aim, sol-gel optical fiber preforms have been fabricated by the densification of erbium salt-soaked nanoporous silica xerogels through the polymeric sol-gel technique. These γ-irradiated fiber preforms have been characterized by FTIR, UV-vis-NIR absorption spectroscopy, electron paramagnetic resonance, and photoluminescence measurements. We showed that a decrease in the glass fictive temperature leads to a decrease in the glass disorder and strained bonds. This mainly results in a lower defect generation rate and thus less radiation-induced attenuation in the UV-vis range. Furthermore, it was found that γ-radiation "hardness" is higher in Er3+-doped sol-gel silica compared to un-doped sol-gel silica and standard synthetic silica glasses. The present work demonstrates an effective strategy to improve the radiation resistance of optical fiber preforms and glasses through glass fictive temperature reduction.

  15. Carbon nanotube-coated solid-phase microextraction metal fiber based on sol-gel technique.

    PubMed

    Jiang, Ruifen; Zhu, Fang; Luan, Tiangang; Tong, Yexiang; Liu, Hong; Ouyang, Gangfeng; Pawliszyn, Janusz

    2009-05-29

    A novel carbon nanotube (CNT)-coated solid-phase microextraction fiber was prepared based on sol-gel technique. Commonly used fragile fused silica fiber was replaced with stainless steel wire, which made the fiber unbreakable. An approach was also proposed for batch producing, and good reproducibilities for fiber to fiber and between fibers were achieved. Experiments showed that the sol-gel-CNT fiber exhibited high thermal stability to resist 350 degrees C and excellent solvent durability in methanol and acetonitrile. Compared to commercial polydimethylsiloxane (PDMS) fiber, the sol-gel-CNT fiber represented significantly improved extraction efficiencies for both polar (phenols) and non-polar (benzene, toluene, ethylbenzene, and o-xylene) compounds. Meanwhile, no replacement effect, low carry-over and wide linear range demonstrated that the newly prepared sol-gel-CNT coating has liquid properties, which allow a relatively easy quantification procedure. Moreover, the characterization of the sol-gel-CNT coating was also evaluated with McReynold probe solutes. The results showed that the coating has better affinity for all the five types of solutes compared to commercial 7microm PDMS fiber, which suggested that the coating has the potential to be developed as GC stationary phase.

  16. Flexible metal-oxide devices made by room-temperature photochemical activation of sol-gel films.

    PubMed

    Kim, Yong-Hoon; Heo, Jae-Sang; Kim, Tae-Hyeong; Park, Sungjun; Yoon, Myung-Han; Kim, Jiwan; Oh, Min Suk; Yi, Gi-Ra; Noh, Yong-Young; Park, Sung Kyu

    2012-09-06

    Amorphous metal-oxide semiconductors have emerged as potential replacements for organic and silicon materials in thin-film electronics. The high carrier mobility in the amorphous state, and excellent large-area uniformity, have extended their applications to active-matrix electronics, including displays, sensor arrays and X-ray detectors. Moreover, their solution processability and optical transparency have opened new horizons for low-cost printable and transparent electronics on plastic substrates. But metal-oxide formation by the sol-gel route requires an annealing step at relatively high temperature, which has prevented the incorporation of these materials with the polymer substrates used in high-performance flexible electronics. Here we report a general method for forming high-performance and operationally stable metal-oxide semiconductors at room temperature, by deep-ultraviolet photochemical activation of sol-gel films. Deep-ultraviolet irradiation induces efficient condensation and densification of oxide semiconducting films by photochemical activation at low temperature. This photochemical activation is applicable to numerous metal-oxide semiconductors, and the performance (in terms of transistor mobility and operational stability) of thin-film transistors fabricated by this route compares favourably with that of thin-film transistors based on thermally annealed materials. The field-effect mobilities of the photo-activated metal-oxide semiconductors are as high as 14 and 7 cm(2) V(-1) s(-1) (with an Al(2)O(3) gate insulator) on glass and polymer substrates, respectively; and seven-stage ring oscillators fabricated on polymer substrates operate with an oscillation frequency of more than 340 kHz, corresponding to a propagation delay of less than 210 nanoseconds per stage.

  17. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    PubMed

    Seyyal, Emre; Malik, Abdul

    2017-04-29

    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C12) and phenethyl (PhE) ligands. Here, the ability of the PF-C12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L(-1) limit of detections (LOD

  18. Sol-gel transition accelerated by the co-assembly of two components in supramolecular hydrogels.

    PubMed

    Matsumoto, Keigo; Shundo, Atsuomi; Ohno, Masashi; Saruhashi, Kowichiro; Miyachi, Nobuhide; Tsuruzoe, Nobutomo; Tanaka, Keiji

    2015-10-28

    N-Palmitoyl-Gly-His (PalGH) and glycerol 1-monopalmitate (GMP) in water co-assembled into fibrils with twisted ribbon structures and formed a homogeneous network, resulting in gel formation. Shaking the gel easily broke the fibril network leading to a sol in which high and low fibril density regions exist. After a period at room temperature, the higher density regions became interconnected. The spontaneous sol-gel transition did not take place for a gel made from only PalGH. Also, during the transition, the aggregation state of the co-assembly remained unchanged at a molecular level, unlike the fibril network. Thus, it can be claimed that the sol-gel transition is not associated with the assembled molecular configuration, but with the change in the fibril network. This knowledge might be useful for understanding and controlling sol-gel transition, thereby leading to the design and functionalization of hydrogels.

  19. High-energy-density sol-gel thin film based on neat 2-cyanoethyltrimethoxysilane.

    PubMed

    Kim, Yunsang; Kathaperumal, Mohanalingam; Smith, O'Neil L; Pan, Ming-Jen; Cai, Ye; Sandhage, Kenneth H; Perry, Joseph W

    2013-03-13

    Hybrid organic-inorganic sol-gel dielectric thin films from a neat 2-cyanoethyltrimethoxysilane (CNETMS) precursor have been fabricated and their permittivity, dielectric strength, and energy density characterized. CNETMS sol-gel films possess compact, polar cyanoethyl groups and exhibit a relative permittivity of 20 at 1 kHz and breakdown strengths ranging from 650 V/μm to 250 V/μm for film thicknesses of 1.3 to 3.5 μm. Capacitors based on CNETMS films exhibit extractable energy densities of 7 J/cm(3) at 300 V/μm, as determined by charge-discharge and polarization-electric field measurements, as well as an energy extraction efficiency of ~91%. The large extractable energy resulting from the linear dielectric polarization behavior suggests that CNETMS films are promising sol-gel materials for pulsed power applications.

  20. Ultrapure glass optical waveguide development in microgravity by the sol-gel process

    NASA Technical Reports Server (NTRS)

    Mukherjee, S. P.; Holman, R. A.

    1981-01-01

    Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process referred to here is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation. The use of gels offers several advantages such as high purity and lower melting times and temperatures. The sol-gel process is studied for utilization in the preparation of multicomponent ultrapure glass batches for subsequent containerless melting of the batches in space to prepare glass blanks for optical waveguides.

  1. Photochromic organic-inorganic composite materials prepared by sol-gel processing: properties and potentials

    NASA Astrophysics Data System (ADS)

    Hou, Lisong; Mennig, Martin; Schmidt, Helmut K.

    1994-09-01

    The sol-gel method which features a low-temperature wet-chemical process opens vast possibilities to incorporating organic dyes into solid matrices for various optical applications. In this paper we present our experimental results on the sol-gel derived photochromic organic- inorganic composite (Ormocer) materials following an introductory description of the sol-gel process and a brief review on the state of the art of the photochromic solids prepared using this method. Our photochromic spirooxazine-Ormocer gels and coatings possess better photochromic response and color-change speed than the corresponding photochromic polymer coatings and similar photochemical stability to the latter. Further developments are proposed as to tackle the temperature dependence problem and further tap the potentialities of the photochromic dye-Ormocer material for practical applications.

  2. Tantalum-Tungsten Oxide Thermite Composite Prepared by Sol-Gel Synthesis and Spark Plasma Sintering

    SciTech Connect

    Cervantes, O; Kuntz, J; Gash, A; Munir, Z

    2009-02-13

    Energetic composite powders consisting of sol-gel derived nanostructured tungsten oxide were produced with various amounts of micrometer-scale tantalum fuel metal. Such energetic composite powders were ignition tested and results show that the powders are not sensitive to friction, spark and/or impact ignition. Initial consolidation experiments, using the High Pressure Spark Plasma Sintering (HPSPS) technique, on the sol-gel derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The sol-gel derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta - WO{sub 3}) energetic composite was consolidated to a density of 9.17 g.cm{sup -3} or 93% relative density. In addition those parts were consolidated without significant pre-reaction of the constituents, thus the sample retained its stored chemical energy.

  3. Optical pH sensor based on sol-gel-doped new luminescent dye

    NASA Astrophysics Data System (ADS)

    Lobnik, Aleksandra; Niederreiter, Karlheinz; Uray, Georg

    1999-11-01

    The sol-gel process is an exciting new technology that enables the production of gel glasses and ceramic materials at room temperature. Sol-gel technology offers simple methods for manipulation of the structure, configuration, composition and chemical characteristics of organic matrices. A novel longwave luminescent dye based on the europium luminescence initiated by a covalently bonded antenna fluorophore was designed, synthesized and characterized. The dye was successfully entrapped into various sol-gel and ormosil matrices and consequent optical- , leaching- and light fastness-properties were tested. Finally, sensor layer based on TMOS doped with Eu3+- complex and bromothymol blue was found to be most appropriate for purposes of sensing pH over the range 5-10.

  4. Examination of the structure of sol-gel derived matrices for optoelectronic sensors

    NASA Astrophysics Data System (ADS)

    Ulatowska, Agnieszka; Podbielska, Halina; Lechna, Monika; Grzegorzewski, Bronisław

    2001-06-01

    Sol-gel technology was used to produce glass-like materials doped with different compounds. The sol-gel matrices were prepared on the way of acid hydrolysis. Two types of materials in the form of thin layers were examined: sol-gel bulk type (type I) and thin film type (type II). The structure was visualized by means of a light microscope. The microscopic images were digitized and their luminances were calculated. The thin film type (type II) matrices were investigated also by means of small-angle light scattering. The material properties with dopants such as albumin, ruthenium complex and osmium tetraoxide were examined. The type II matrices showed more homogeneous structure. Lower scattering in doped materials than in the pure matrices was observed.

  5. Impressing technology of optical Bragg's gratings on planar optical sol-gel waveguides

    NASA Astrophysics Data System (ADS)

    Pustelny, T.; Zielonka, I.; Tyszkiewicz, C.; Karasiński, P.; Pustelny, B.

    2006-06-01

    The aim of the presented investigations was to develop a technique of producing Bragg's grating couplers on planar waveguides. Waveguides are obtained by means of the sol-gel technology. The introduction of a light beam into the structure of the waveguide is in the case of planar or strip optical systems always an essential technical problem, requiring simple and reproducible solutions without extending excessively the waveguide structure. The paper presents a technology of producing grating couplers by impressing the pattern of the network while forming the planar waveguide structure applying the sol-gel method. Some remarks concerning the sol-gel technology are also presented. The results of investigations on grating couplers obtained in such a way have been discussed, too. Attention has been drawn to the possibility of using such structures in optoelectronic sensors, particularly gas sensors, including sensors of water vapour as well as toxic gases.

  6. Preparation and characterization of indium tin oxide films by sol-gel method

    NASA Astrophysics Data System (ADS)

    Ciuciumis, Alina; Cernica, Ileana

    2007-05-01

    Sol-gel technology is a relatively simple and cheap process to deposit oxides under thin film form out of a sol. The experiments were developed in order to obtain nanomaterials by sol-gel method; nanomaterials that mixed with resin and additives can be deposited in thin and uniform films by spraying on different lignocellulosic composite surfaces. This method assures a functional finishing of the nanomaterials. These films are transparent and the surfaces are flat with no cracks. The influence of substrate type, morphology of the films and of the substrates before and after deposition was studied by means of optical microscopy, scanning electron microscopy (SEM) and atomic force microscopy (AFM). The sol-gel deposit on the lignocellulosic composite substrates lowered the sorption rates of water and water vapours.

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

    PubMed

    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.

  8. Sol-gel deposited electrochromic films for electrochromic smart window glass

    SciTech Connect

    Oezer, N.; Lampert, C.M.; Rubin, M.

    1996-08-01

    Electrochromic windows offer the ability to dynamically change the transmittance of a glazing. With the appropriate sensor and controls, this smart window can be used for energy regulation and glare control for a variety of glazing applications. The most promising are building and automotive applications. This work covers the use of sol-gel deposition processes to make active films for these windows. The sol-gel process offers a low-capital investment for the deposition of these active films. Sol-gel serves as an alternative to more expensive vacuum deposition processes. The sol-gel process utilizes solution coating followed by a hydrolysis and condensation. In this investigation the authors report on tungsten oxide and nickel oxide films made by the sol-gel process for electrochromic windows. The properties of the sol-gel films compare favorably to those of films made by other techniques. A typical laminated electrochromic window consists of two glass sheets coated with transparent conductors, which are coated with the active films. The two sheets are laminated together with an ionically conductive polymer. The range of visible transmission modulation of the tungsten oxide was 60% and for the nickel oxide was 20%. The authors used the device configuration of glass/SnO{sub 2}:F/W0{sub 3}/polymer/Li{sub Z}NiO{sub x}H{sub y}/SnO{sub 2}:F glass to test the films. The nickel oxide layer had a low level of lithiation and possibly contained a small amount of water. Lithiated oxymethylene-linked poly(ethylene oxide) was used as the laminating polymer. Commercially available SnO{sub 2}:F/glass (LOF-Tec glass) was used as the transparent conducting glass. The authors found reasonable device switching characteristics which could be used for devices.

  9. Development of novel Sol-Gel Indicators (SGI's) for in-situ environmental measurements: Part 1, Program and a new pH Sol-Gel Indicator

    SciTech Connect

    Livingston, R.R.; Baylor, L.; Wicks, G.G.

    1992-11-03

    The feasibility of incorporating analytical indicators into a sol-gel glassy matrix and then coating substrates with this composite material has bee demonstrated. Substrates coated include paper, wood, glass, and the lens of an analytical probe. The first SRTC sol-gel indicator, comprising bromophenol blue dispersed in a silica matrix, was fabricated and successfully used to measure solution pH in the range of pH 3.0 to 7.5. material exhibited a quick response time, as measured by color changes both qualitatively and quantitatively, and the measuring device was reversible or reusable. Additional indicators with responses over other ranges as well as indicators sensitive to the presence of elements of interest, are also under development. The new SGI composites possess promising properties and an excellent potential for performing a variety important in-situ environmental measurements and area discussed in this report.

  10. Sol-gel process for the manufacture of high power switches

    DOEpatents

    Landingham, Richard L.; Satcher, Jr, Joe; Reibold, Robert

    2016-09-27

    According to one embodiment, a photoconductive semiconductor switch includes a structure of nanopowder of a high band gap material, where the nanopowder is optically transparent, and where the nanopowder has a physical characteristic of formation from a sol-gel process. According to another embodiment, a method includes mixing a sol-gel precursor compound, a hydroxy benzene and an aldehyde in a solvent thereby creating a mixture, causing the mixture to gel thereby forming a wet gel, drying the wet gel to form a nanopowder, and applying a thermal treatment to form a SiC nanopowder.

  11. Novel Sol-Gel Based Pt Nanocluster Catalysts for Propane Dehydrogenation

    SciTech Connect

    Boespflug, Elaine; Kawola, Jeffrey S.; Martino, Anthony; Sault, Allen G.

    1999-08-09

    We report propane dehydrogenation behavior of catalysts prepared using two novel synthesis strategies that combine inverse micelle Pt nanocluster technology with silica and alumina sol-gel processing. Unlike some other sol-gel catalyst preparations. Pt particles in these catalysts are not encapsulated in the support structure and the entire Pt particle surface is accessible for reaction. Turnover frequencies (TOF) for these catalysts are comparable to those obtained over Pt catalysts prepared by traditional techniques such as impregnation, yet the resistance to deactivation by carbon poisoning is much greater in our catalysts. The deactivation behavior is more typical of traditionally prepared PtSn catalysts than of pure Pt catalysts.

  12. Transparent poly(vinyl acetate)-silica gels by a sol-gel process

    NASA Astrophysics Data System (ADS)

    Wojcik, Anna B.; Klein, Lisa C.

    1993-12-01

    Rod shaped silica-poly(vinyl acetate) (PVAc) gels have been prepared by a sol gel process. In situ polymerization of tetraethoxysilane (TEOS) was accomplished in the presence of low molecular weight PVAc by dissolving various amounts of PVAc in a mixture of TEOS, ethanol, water and hydrochloric acid (HCl). Gelation of this mixture was carried out between room temperature and slightly above. Silica-PVAc rods recovered from cylindrical molds were homogeneous and transparent. Gels with weight percents of PVAc ranging from 2% to 50% were prepared. Silica-PVAc gels have higher flexure strengths, less brittle character and improved water durability in comparison with pure sol- gel silica.

  13. Fabrication of SWNT/silica composites by the sol-gel process.

    PubMed

    Babooram, Keshwaree; Narain, Ravin

    2009-01-01

    Single-walled carbon nanotubes (SWNTs) have successfully been incorporated into a silica matrix using the sol-gel process. The SWNTs were first functionalized with 3-aminopropyltriethoxysilane (APTES) through an amide linkage formed between the carboxylic acid groups already present on their surface and the amino group on APTES. The silane moieties were then used to form silica with and without the presence of tetramethylorthosilicate (TMOS) in a sol-gel reaction. The addition of TMOS was found to influence the molecular arrangement of the SWNT in the silica matrix and also to retard the degradation of the silica-SWNT composite.

  14. Porous Silica Sol-Gel Glasses Containing Reactive V2O5 Groups

    NASA Technical Reports Server (NTRS)

    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.

  15. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    NASA Astrophysics Data System (ADS)

    Figus, Cristiana; Quochi, Francesco; Artizzu, Flavia; Piana, Giacomo; Saba, Michele; Mercuri, Maria Laura; Serpe, Angela; Deplano, Paola; Mura, Andrea; Bongiovanni, Giovanni

    2014-10-01

    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ4) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ4 are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution.

  16. Synthesis of superhydrophobic alumina membrane: Effects of sol-gel coating, steam impingement and water treatment

    NASA Astrophysics Data System (ADS)

    Ahmad, N. A.; Leo, C. P.; Ahmad, A. L.

    2013-11-01

    Ceramic membranes possess natural hydrophilicity thus tending to absorb water droplets. The absorption of water molecules on membrane surface reduces their application in filtration, membrane distillation, osmotic evaporation and membrane gas absorption. Fluoroalkylsilane (FAS) grafting allows the conversion of hydrophilic ceramic membranes into superhydrophobic thin layer, but it usually introduces a great increment of mass transfer resistance. In this study, superhydrophobic alumina membranes were synthesized by dip coating alumina support into sol-gel and grafted with the fluoroalkylsilane (FAS) named (heptadecafluoro-1,1,2,2-tetra hydrodecyl) triethoxysilane. Steam impingement and water treatment acted as additional steps to generate surface roughness on sol-gel and most importantly to reduce mass transfer resistance. Superhydrophobic alumina membrane with high water contact angle (158.4°) and low resistance (139.5 ± 24.9 G m-1) was successfully formed when the alumina membrane was dip coated into sol-gel for 7 s, treated with steam impingement for 1 min and immersed in hot water at 100 °C. However, the mass transfer resistance was greatly induced to 535.6 ± 23.5 G m-1 when the dip coating time was increased to 60 s. Long dip coating time contributes more on the blockage of porous structure rather than creates a thin film on the top of membrane surface. Reducing the pore size and porosity significantly due to increase of coating molecules deposited on the membrane. Steam impingement for 1 min promoted the formation of cones and valleys on the sol-gel, but the macro-roughness was destroyed when the steam impingement duration was extended to more than 3 min. The immersions of membranes into hot water at temperatures higher than 60 °C encouraged the formation of boehmite which enhances the formation of additional roughness and enlarges pore size greatly. Thus, this work showed that the formation of superhydrophobic alumina membrane with low resistance is

  17. Sol-gel processed alumina based materials in microcalorimeter sensor device fabrication for automotive applications

    SciTech Connect

    Nakouzi, S.R.; McBride, J.R.; Nietering, K.E.; Narula, C.K.

    1996-12-31

    The application of sol-gel processed materials in a variety of sensors has been proposed. The authors describe microcalorimeter sensor devices employing sol-gel processed alumina based materials which can be used to monitor pollutants in automotive exhaust. These sensors operate by measuring changes in resistance upon catalysis and are economically acceptable for automotive applications. It is important to point out that automobiles will be required to have a means of monitoring exhaust gases by on-board sensors as mandated by the EPA and the California Air Resources Board (OBD-II).

  18. Microwave sintering of sol-gel composite films using a domestic microwave oven

    NASA Astrophysics Data System (ADS)

    Kobayashi, Makiko; Matsumoto, Makoto

    2016-07-01

    Feasibility study of sol-gel composite microwave sintering using a domestic microwave oven was carried out. Two kinds of lead zirconate titanate (PZT) powders were mixed with PZT sol-gel solution and the mixture was sprayed onto 3-mm-thick titanium substrate. The films were sintered by 700 W domestic oven for 10 min. Ultrasonic measurement was carried out in pulse-echo mode and clear multiple echoes were confirmed. It would be suitable method to fabricate high frequency broadband focused ultrasonic transducers. Further research is required to improve sintering degree.

  19. Development of high efficiency q-switched glass laser via sol-gel processing

    NASA Astrophysics Data System (ADS)

    Moreshead, William V.

    1988-02-01

    The sol-gel process is a logical choice for silica-based laser glasses, since it requires lower processing temperatures than traditional melt glass techniques, and allows good control of purity. This report describes attempts to prepare silica glasses containing neodymium or neodymium and erbium using sol-gel technology. A description of two different doping procedures is given, along with results. The materials produced were characterized and the spectral, thermal, and physical properties are reported. Fluorescence spectra and fluorescence lifetimes are given for three different materials prepared.

  20. Scintillators based on aromatic dye molecules doped in a sol-gel glass host

    NASA Astrophysics Data System (ADS)

    Nikl, M.; Solovieva, N.; Apperson, K.; Birch, D. J. S.; Voloshinovskii, A.

    2005-03-01

    Ultraviolet and x-ray excited luminescence of fluorescein and rhodamine-6G doped sol-gel glasses were studied at room temperature with the aim of characterizing and understanding the scintillation performance of such materials. Fast energy transfer from the glass host to the dye luminescent centers was found. While the overall radioluminescence efficiency was rather low due to nonradiative losses in the glass host, our results demonstrate the potential of sol-gel technology as a versatile tool in controlling the spectral and time response of such unusual organic-inorganic scintillators.

  1. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    SciTech Connect

    Figus, Cristiana Quochi, Francesco Piana, Giacomo; Saba, Michele; Mura, Andrea; Bongiovanni, Giovanni; Artizzu, Flavia; Mercuri, Maria Laura; Serpe, Angela; Deplano, Paola

    2014-10-21

    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ{sub 4}) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ{sub 4} are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution.

  2. A comparative synthesis and physicochemical characterizations of Ni/Al2O3-MgO nanocatalyst via sequential impregnation and sol-gel methods used for CO2 reforming of methane.

    PubMed

    Aghamohammadi, Sogand; Haghighi, Mohammad; Karimipour, Samira

    2013-07-01

    Carbon dioxide reforming of methane is an interesting route for synthesis gas production especially over nano-sized catalysts. The present research deals with catalyst development for dry reforming of methane with the aim of reaching the most stable catalyst. Effect of preparation method, one of the most significant variables, on the properties of the catalysts was taken in to account. The Ni/Al2O3-MgO catalysts were prepared via sol-gel and sequential impregnation methods and characterized with XRD, FESEM, EDAX, BET and FTIR techniques. The reforming reactions were carried out using different feed ratios, gas hourly space velocities (GHSV) and reaction temperatures to identify the influence of operational variables. FESEM images indicate uniform particle size distribution for the sample synthesized with sol-gel method. It has been found that the sol-gel method has the potential to improve catalyst desired properties especially metal surface enrichment resulting in catalytic performance enhancement. The highest yield of products was obtained at 850 degrees C for both of the catalysts. During the 10 h stability test, CH4 and CO2 conversions gained higher values in the case of sol-gel made catalyst compared to impregnated one.

  3. Silica/quercetin sol-gel hybrids as antioxidant dental implant materials

    NASA Astrophysics Data System (ADS)

    Catauro, Michelina; Papale, Ferdinando; Bollino, Flavia; Piccolella, Simona; Marciano, Sabina; Nocera, Paola; Pacifico, Severina

    2015-06-01

    The development of biomaterials with intrinsic antioxidant properties could represent a valuable strategy for preventing the onset of peri-implant diseases. In this context, quercetin, a naturally occurring flavonoid, has been entrapped at different weight percentages in a silica-based inorganic material by a sol-gel route. The establishment of hydrogen bond interactions between the flavonol and the solid matrix was ascertained by Fourier transform infrared spectroscopy. This technique also evidenced changes in the stretching frequencies of the quercetin dienonic moiety, suggesting that the formation of a secondary product occurs. Scanning electron microscopy was applied to detect the morphology of the synthesized materials. Their bioactivity was shown by the formation of a hydroxyapatite layer on sample surface soaked in a fluid that simulates the composition of human blood plasma. When the potential release of flavonol was determined by liquid chromatography coupled with ultraviolet and electrospray ionization tandem mass spectrometry techniques, the eluates displayed a retention time that was 0.5 min less than quercetin. Collision-activated dissociation mass spectrometry and untraviolet-visible spectroscopy were in accordance with the release of a quercetin derivative. The antiradical properties of the investigated systems were evaluated by DPPH and ABTS methods, whereas the 2,7-dichlorofluorescein diacetate assay highlighted their ability to inhibit the H2O2-induced intracellular production of reactive oxygen species in NIH-3T3 mouse fibroblast cells. Data obtained, along with data gathered from the MTT cytotoxicity test, revealed that the materials that entrapped the highest amount of quercetin showed notable antioxidant effectiveness.

  4. Environmentally benign sol-gel antifouling and foul-releasing coatings.

    PubMed

    Detty, Michael R; Ciriminna, Rosaria; Bright, Frank V; Pagliaro, Mario

    2014-02-18

    Biofouling on ships and boats, characterized by aquatic bacteria and small organisms attaching to the hull, is an important global issue, since over 80000 tons of antifouling paint is used annually. This biofilm, which can form in as little as 48 hours depending on water temperature, increases drag on watercraft, which greatly reduces their fuel efficiency. In addition, biofouling can lead to microbially induced corrosion (MIC) due to H2S formed by the bacteria, especially sulfate-reducing bacteria. When the International Maritime Organization (IMO) international convention banned the use of effective but environmentally damaging coatings containing tributyl tin in 2008, the development of clean and effective antifouling systems became more important than ever. New nonbiocidal coatings are now in high demand. Scientists have developed new polymers, materials, and biocides, including new elastomeric coatings that they have obtained by improving the original silicone (polydimethylsiloxane) formulation patented in 1975. However, the high cost of silicones, especially of fluoropolymer-modified silicones, has generally prevented their large-scale diffusion. In 2009, traditional antifouling coatings using cuprous oxide formulated in copolymer paints still represented 95% of the global market volume of anti-fouling paints. The sol-gel nanochemistry approach to functional materials has emerged as an attractive candidate for creating low fouling surfaces due to the unique structure and properties of silica-based coatings and of hybrid inorganic-organic silicas in particular. Sol-gel formulations easily bind to all types of surfaces, such as steel, fiberglass, aluminum, and wood. In addition, they can cure at room temperature and form thin glassy coatings that are markedly different from thick silicone elastomeric foul-releasing coatings. Good to excellent performance against biofouling, low cure temperatures, enhanced and prolonged chemical and physical stability, ease of

  5. THERMALLY STABLE NANOCRYSTALLINE TIO2 PHOTOCATALYSTS SYNTHESIZED VIA SOL-GEL METHODS MODIFIED WITH IONIC LIQUID AND SURFACTANT MOLECULES

    EPA Science Inventory

    Recently, sol-gel methods employing ionic liquids (ILs) have shown significant implications for the synthesis of well-defined nanostructured inorganic materials. Herein, we synthesized nanocrystalline TiO2 particles via an alkoxide sol-gel method employing a water-immi...

  6. Electrochemical and In Vitro Behavior of Nanostructure Sol-Gel Coated 316L Stainless Steel Incorporated with Rosemary Extract

    NASA Astrophysics Data System (ADS)

    Motalebi, Abolfazl; Nasr-Esfahani, Mojtaba

    2013-06-01

    The corrosion resistance of AISI 316L stainless steel for biomedical applications, was significantly enhanced by means of hybrid organic-inorganic sol-gel thin films deposited by spin-coating. Thin films of less than 100 nm with different hybrid characters were obtained by incorporating rosemary extract as green corrosion inhibitor. The morphology, composition, and adhesion of hybrid sol-gel coatings have been examined by SEM, EDX, and pull-off test, respectively. Addition of high additive concentrations (0.1%) did not disorganize the sol-gel network. Direct pull-off test recorded a mean coating-substrate bonding strength larger than 21.2 MPa for the hybrid sol-gel coating. The effect of rosemary extract, with various added concentrations from 0.012 to 0.1%, on the anticorrosion properties of sol-gel films have been characterized by electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization tests in simulated body fluid (SBF) solution and has been compared to the bare metal. Rosemary extract additions (0.05%) have significantly increased the corrosion protection of the sol-gel thin film to higher than 90%. The in vitro bioactivity of prepared films indicates that hydroxyapatite nuclei can form and grow on the surface of the doped sol-gel thin films. The present study shows that due to their excellent anticorrosion properties, bioactivity and bonding strength to substrate, doped sol-gel thin films are practical hybrid films in biomedical applications.

  7. Increasing the activity and enantioselectivity of lipases by sol-gel immobilization: further advancements of practical interest.

    PubMed

    Tielmann, Patrick; Kierkels, Hans; Zonta, Albin; Ilie, Adriana; Reetz, Manfred T

    2014-06-21

    The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of the sol-gel approach.

  8. Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment

    PubMed Central

    Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha

    2015-01-01

    Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol-gel SiO2 is non-toxic and safe, whereas the sol-gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped active agents, thereby broadening the practical utilization of chemically unstable essential oils (EOs). Reviewing progress in the fabrication of diverse odorant and flavored sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits. PMID:26322304

  9. Effectiveness of silica based Sol-gel microencapsulation Method for odorants and flavours leading to sustainable Environment

    NASA Astrophysics Data System (ADS)

    Ashraf, Muhammad Aqeel; Khan, Ayesha Masood; Sarfraz, Maliha; Ahmad, Mushtaq

    2015-08-01

    Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol-gel SiO2 is non-toxic and safe, whereas the sol-gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped actives, thereby broadening the practical utilization of chemically unstable essential oils. Reviewing progress in the fabrication of diverse odorant and flavoured sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

  10. Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment.

    PubMed

    Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha

    2015-01-01

    Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol-gel SiO2 is non-toxic and safe, whereas the sol-gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped active agents, thereby broadening the practical utilization of chemically unstable essential oils (EOs). Reviewing progress in the fabrication of diverse odorant and flavored sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

  11. Foldable and Cytocompatible Sol-gel TiO2 Photonics

    NASA Astrophysics Data System (ADS)

    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

    2015-09-01

    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.

  12. Improving the temperature performance of low-density ceramic heatshields through sol-gel processing

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey; Leiser, Daniel; Sommers, Jeneen; Esfahani, Lili

    1991-01-01

    The performance of rigid insulations for use as thermal protection materials on reentry vehicles can be characterized by their resistance to dimensional and morphological change when exposed to an isothermal environment equivalent to that generated in entry. Improvements in these material characteristics for alumina-enhanced thermal barrier insulation by compositional modification through sol-gel processing are reported.

  13. Ternary Phase-Separation Investigation of Sol-Gel Derived Silica from Ethyl Silicate 40.

    PubMed

    Wang, Shengnan; Wang, David K; Smart, Simon; da Costa, João C Diniz

    2015-09-28

    A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification.

  14. Non-cytotoxic antibacterial silver-coumarin complex doped sol-gel coatings.

    PubMed

    Jaiswal, Swarna; Bhattacharya, Kunal; Sullivan, Maeve; Walsh, Maureen; Creaven, Bernadette S; Laffir, Fathima; Duffy, Brendan; McHale, Patrick

    2013-02-01

    Microbial colonisation on clinical and industrial surfaces is currently of global concern and silane based sol-gel coatings are being proposed as potential solutions. Sol-gels are chemically inert, stable and homogeneous and can be designed to act as a reservoir for releasing antimicrobial agents over extended time periods. In the present study, silver nitrate (AgN) and a series of silver coumarin complexes based on coumarin-3-carboxylatosilver (AgC) and it is 6, 7 and 8 hydroxylated analogues (Ag6, Ag7, Ag8) were incorporated into sol-gel coatings. The comparative antibacterial activity of the coatings was determined against meticillin resistant Staphylococcus aureus (MRSA) and multidrug resistance Enterobacter cloacae WT6. The percentage growth inhibitions were found in the range of 9.2 (±2.7)-66.0 (±1.2)% at low silver loadings of 0.3% (w/w) with E. cloacae being the more susceptible. Results showed that among the Ag coumarin complexes, the Ag8 doped coating had the highest antibiofilm property. XPS confirmed the presence of silver in the nanoparticulate state (Ag(0)) at the coating surface where it remained after 4 days of exposure to bacterial culture. Comparative cytotoxicity studies revealed that the Ag-complex coatings were less toxic than the AgN coating. Thus, it can be concluded that a sol-gel matrix with Ag-coumarin complexes may provide non-toxic surfaces with antibacterial properties.

  15. Sol-gel deposition of buffer layers on biaxially textured metal substances

    DOEpatents

    Shoup, Shara S.; Paranthamam, Mariappan; Beach, David B.; Kroeger, Donald M.; Goyal, Amit

    2000-01-01

    A method is disclosed for forming a biaxially textured buffer layer on a biaxially oriented metal substrate by using a sol-gel coating technique followed by pyrolyzing/annealing in a reducing atmosphere. This method is advantageous for providing substrates for depositing electronically active materials thereon.

  16. Hybrid Thin Film Organosilica Sol-Gel Coatings To Support Neuronal Growth and Limit Astrocyte Growth.

    PubMed

    Capeletti, Larissa Brentano; Cardoso, Mateus Borba; Dos Santos, João Henrique Zimnoch; He, Wei

    2016-10-07

    Thin films of silica prepared by a sol-gel process are becoming a feasible coating option for surface modification of implantable neural sensors without imposing adverse effects on the devices' electrical properties. In order to advance the application of such silica-based coatings in the context of neural interfacing, the characteristics of silica sol-gel are further tailored to gain active control of interactions between cells and the coating materials. By incorporating various readily available organotrialkoxysilanes carrying distinct organic functional groups during the sol-gel process, a library of hybrid organosilica coatings is developed and investigated. In vitro neural cultures using PC12 cells and primary cortical neurons both reveal that, among these different types of hybrid organosilica, the introduction of aminopropyl groups drastically transforms the silica into robust neural permissive substrate, supporting neuron adhesion and neurite outgrowth. Moreover, when this organosilica is cultured with astrocytes, a key type of glial cells responsible for glial scar response toward neural implants, such cell growth promoting effect is not observed. These findings highlight the potential of organo-group-bearing silica sol-gel to function as advanced coating materials to selectively modulate cell response and promote neural integration with implantable sensing devices.

  17. Influence of Calcium on the Initial Stages of the Sol-Gel Synthesis of Bioactive Glasses.

    PubMed

    Côté, Alexander S; Cormack, Alastair N; Tilocca, Antonio

    2016-11-17

    Understanding how calcium interacts with silica sources and influences their polycondensation in aqueous solutions is of central importance for the development of more effective biomaterials by sol-gel approaches. For this purpose, the atomic-scale evolutions of a calcium-containing precursor solution corresponding to a typical sol-gel bioactive glass and of a corresponding Ca-free solution were compared using reactive molecular dynamics simulations. The simulations highlight a significantly faster rate of condensation when calcium is present in the initial solution, resulting in the formation of large and ramified silica clusters within 5 ns, which are absent in the Ca-free system. This different behavior has been analyzed and interpreted in terms of the Ca-induced nanosegregation in calcium-rich and silica-rich regions, which promotes the condensation reactions within the latter. By identifying a possible mechanism behind the limited incorporation of calcium in the silica nanoclusters formed in the early stages of the sol-gel process, these results could guide further studies aimed at identifying favorable experimental conditions to enhance initial calcium incorporation and thus produce sol-gel biomaterials with improved properties.

  18. Thin-film silica sol-gel coatings for neural microelectrodes.

    PubMed

    Pierce, Andrew L; Sommakia, Salah; Rickus, Jenna L; Otto, Kevin J

    2009-05-30

    The reactive tissue response of the brain to chronically implanted materials remains a formidable obstacle to stable recording from implanted microelectrodes. One approach to mitigate this response is to apply a bioactive coating in the form of an ultra-porous silica sol-gel, which can be engineered to improve biocompatibility and to enable local drug delivery. The first step in establishing the feasibility of such a coating is to investigate the effects of the coating on electrode properties. In this paper, we describe a method to apply a thin-film silica sol-gel coating to silicon-based microelectrodes, and discuss the resultant changes in the electrode properties. Fluorescently labeled coatings were used to confirm coating adherence to the electrode. Cyclic voltammetry and impedance spectroscopy were used to evaluate electrical property changes. The silica sol-gel was found to successfully adhere to the electrodes as a thin coating. The voltammograms revealed a slight increase in charge carrying capacity of the electrodes following coating. Impedance spectrograms showed a mild increase in impedance at high frequencies but a more pronounced decrease in impedance at mid to low frequencies. These results demonstrate the feasibility of applying silica sol-gel coatings to silicon-based microelectrodes and are encouraging for the continued investigation of their use in mitigating the reactive tissue response.

  19. Synthesis and characterization of polymer-silica hybrid latexes and sol-gel-derived films

    NASA Astrophysics Data System (ADS)

    Petcu, Cristian; Purcar, Violeta; Ianchiş, Raluca; Spătaru, Cătălin-Ilie; Ghiurea, Marius; Nicolae, Cristian Andi; Stroescu, Hermine; Atanase, Leonard-Ionuţ; Frone, Adriana Nicoleta; Trică, Bogdan; Donescu, Dan

    2016-12-01

    Sol-gel derived organic-inorganic hybrid systems were obtained by applying alkaline-catalyzed co-hydrolysis and copolycondensation reactions of tetraethoxysilane (TEOS), methyltriethoxysilane (MTES), isobutyltriethoxysilane (IBTES), diethoxydimethylsilane (DMDES), and vinyltriethoxysilane (VTES), respectively, into a polymer latex functionalized with vinyltriethoxysilane (VTES). The properties of the latex hybrid materials were analyzed by FTIR, water contact angle, environmental scanning electron microscopy (ESEM), TEM and AFM analysis, respectively. FT-IR spectra confirmed that the chemical structures of the sol-gel derived organic-inorganic materials are changed as function of inorganic precursor and Sisbnd Osbnd Si networks are formed during the co-hydrolysis and copolycondensation reactions. The water contact angle on the sol-gel latex film containing TEOS + VTES increased to 135° ± 2 compared to 65° ± 5 for the blank latex, due VTES incorporation into latex material. TGA curves of hybrid sample modifies against neat polymer, the thermal stability being influenced by the presence of the inorganic partner. ESEM analysis showed that the latex hybrid films prepared with different inorganic precursors were formed and the Si-based polymers were distributed on the surface of the dried sol-gel hybrid films. TEM and AFM photos revealed that the latex emulsion morphology was modified due to the VTES incorporation into system.

  20. Foldable and Cytocompatible Sol-gel TiO2 Photonics.

    PubMed

    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.

  1. Low-density nanoporous iron foams synthesized by sol-gel autocombustion

    PubMed Central

    2012-01-01

    Nanoporous iron metal foams were synthesized by an improved sol-gel autocombustion method in this report. It has been confirmed to be pure phase iron by X-ray diffraction measurements. The nanoporous characteristics were illustrated through scanning electron microscope and transmission electron microscope images. Very low density and quite large saturation magnetization has been performed in the synthesized samples. PMID:22333555

  2. Self-Protection of Electrochemical Storage Devices via a Thermal Reversible Sol-Gel Transition.

    PubMed

    Yang, Hui; Liu, Zhiyuan; Chandran, Bevita K; Deng, Jiyang; Yu, Jiancan; Qi, Dianpeng; Li, Wenlong; Tang, Yuxin; Zhang, Chenguang; Chen, Xiaodong

    2015-10-07

    Thermal self-protected intelligent electrochemical storage devices are fabricated using a reversible sol-gel transition of the electrolyte, which can decrease the specific capacitance and increase and enable temperature-dependent charging and discharging rates in the device. This work represents proof of a simple and useful concept, which shows tremendous promise for the safe and controlled power delivery in electrochemical devices.

  3. Auto-organisation of hybrid organic-inorganic materials prepared by sol-gel process.

    PubMed

    Boury, Bruno; Corriu, Robert J P

    2002-04-21

    Silica-based hybrid organic-inorganic materials prepared by sol-gel chemistry exhibit chemical and physical properties revealing their anisotropic organisation. Besides the opportunities that this phenomenon opens for the preparation of new materials, it also provides arguments to the chemist looking for a better comprehension and control of the organisation of solids.

  4. Investigation of optical properties of anthocyanin doped into sol-gel based matrix

    NASA Astrophysics Data System (ADS)

    Hashim, Hasrina; Abdul Aziz, Nik Mohd Azmi Nik; Isnin, Aishah

    2012-06-01

    Anthocyanin dye was extracted from petal of Hibiscus rosasinensis (Bunga Raya) and doped into sol-gel based matrix to investigate an effect of pH change on its optical properties. Sol-gel matrix based on Vinyl triethoxysilene (VTES) as a precursor was prepared through Sol-gel process at pH 7. The sol was doped with 0.1% of Anthocyanin and the same amount of dye was also dissolved in ethanol as a comparative sample. Hydrochloric Acid, HCl and Tetramethylammonium Hydroxide, TMAH were used to change the pH value by adding them at various concentrations into each sample. The emission spectra and chemical structures of the samples were measured by Spectrofluorometer and Fourier Transform Infrared (FTIR) respectively. When excited at 410 nm, two emission peaks at about 492 and 574 nm were observed for Anthocyanin in acidic environment both in ethanol and VTES sol. In base environment however, only Anthocyanin dissolved in ethanol produced emission peak with a single peak at about 539 nm. The sensitivity of Anthocyanin dye toward pH changes in VTES open a possibility to use it as sensing element in which sol-gel based matrix are known to have higher mechanical strength and thermal stability.

  5. The effect of silica-coating by sol-gel process on resin-zirconia bonding.

    PubMed

    Lung, Christie Ying Kei; Kukk, Edwin; Matinlinna, Jukka Pekka

    2013-01-01

    The effect of silica-coating by sol-gel process on the bond strength of resin composite to zirconia was evaluated and compared against the sandblasting method. Four groups of zirconia samples were silica-coated by sol-gel process under varied reagent ratios of ethanol, water, ammonia and tetraethyl orthosilicate and for different deposition times. One control group of zirconia samples were treated with sandblasting. Within each of these five groups, one subgroup of samples was kept in dry storage while another subgroup was aged by thermocycling for 6,000 times. Besides shear bond testing, the surface topography and surface elemental composition of silica-coated zirconia samples were also examined using scanning electron microscopy and X-ray photoelectron spectroscopy. Comparison of silica coating methods revealed significant differences in bond strength among the Dry groups (p<0.001) and Thermocycled groups (p<0.001). Comparison of sol-gel deposition times also revealed significant differences in bond strength among the Dry groups (p<0.01) and Thermocycled groups (p<0.001). Highest bond strengths were obtained after 141-h deposition: Dry (7.97±3.72 MPa); Thermocycled (2.33±0.79 MPa). It was concluded that silica-coating of zirconia by sol-gel process resulted in weaker resin bonding than by sandblasting.

  6. Foldable and Cytocompatible Sol-gel TiO2 Photonics

    PubMed Central

    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

    2015-01-01

    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. PMID:26344823

  7. Ternary Phase-Separation Investigation of Sol-Gel Derived Silica from Ethyl Silicate 40

    NASA Astrophysics Data System (ADS)

    Wang, Shengnan; Wang, David K.; Smart, Simon; Diniz da Costa, João C.

    2015-09-01

    A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification.

  8. Ternary Phase-Separation Investigation of Sol-Gel Derived Silica from Ethyl Silicate 40

    PubMed Central

    Wang, Shengnan; Wang, David K.; Smart, Simon; Diniz da Costa, João C.

    2015-01-01

    A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification. PMID:26411484

  9. Selection and elution of aptamers using nanoporous sol-gel arrays with integrated microheaters.

    PubMed

    Park, Seung-Min; Ahn, Ji-Young; Jo, Minjoung; Lee, Dong-Ki; Lis, John T; Craighead, Harold G; Kim, Soyoun

    2009-05-07

    RNA and DNA aptamers that bind to target molecules with high specificity and affinity have been a focus of diagnostics and therapeutic research. These aptamers are obtained by SELEX (Systematic Evolution of Ligands by EXponential enrichment) often requiring more than 10 successive cycles of selection and amplification, where each cycle normally takes 2 days per cycle of SELEX. Here, we have demonstrated the use of sol-gel arrays of proteins in a microfluidic system for efficient selection of RNA aptamers against multiple target molecules. The microfluidic chip incorporates five sol-gel binding droplets, within which specific target proteins are imbedded. The droplets are patterned on top of individually addressable electrical microheaters used for selective elution of aptamers bound to target proteins in the sol-gel droplets. We demonstrate that specific aptamers bind their respective protein targets and can be selectively eluted by micro-heating. Finally, our microfluidic SELEX system greatly improved selection efficiency, reducing the number of selection cycles needed to produce high affinity aptamers. The process is readily scalable to larger arrays of sol-gel-embedded proteins. To our knowledge, this is the first demonstration of a chip-based selection of aptamers using microfluidics, thereby allowing development of a high throughput and efficient SELEX procedures.

  10. Air Vehicle Technology Integration Program (AVTIP). Delivery Order 0004: Advanced Sol-Gel Adhesion Processes

    DTIC Science & Technology

    2002-04-01

    AFRL-ML-WP-TR-2003-4173 AIR VEHICLE TECHNOLOGY INTEGRATION PROGRAM (AVTIP) Delivery Order 0004: Advanced Sol-Gel Adhesion Processes Kay Y...2001 – 03/31/2002 5a. CONTRACT NUMBER F33615-00-D-3052 5b. GRANT NUMBER 4. TITLE AND SUBTITLE AIR VEHICLE TECHNOLOGY INTEGRATION PROGRAM

  11. Nitric Oxide Sensors Obtained Through the Entrapment of Iron Complexes in Sol-Gel Matrix

    DTIC Science & Technology

    2002-04-05

    iron complexes in sol-gel matrix Juliana C. Biazzotto, Jodo F. Borin, Roberto Mendonga Faria’ and Carlos F.O Graeff Departamento de Fisica e...Matemdtica-FFCLRP-USP, Av. Bandeirantes 3900, 14040-901 Ribeirdo Preto, Brazil 1-Instituto de Fisica de S~o Carlos-USP, C.P. 369, 13560-970 Sdo Carlos, Brazil

  12. Preparation and complex characterization of silica holmium sol-gel monoliths.

    PubMed

    Cacaina, D; Areva, S; Laaksonen, H; Simon, S; Ylänen, H

    2011-01-01

    Amorphous, sol-gel derived SiO(2) are known to biocompatible and bioresorbable materials. Biodegradable and inert materials containing radioactive isotopes have potential application as delivery vehicles of the beta radiation to the cancer tumors inside the body. Incorporation of holmium in the sol-gel derived SiO(2) could lead to the formation of a biodegradable material which could be used as carrier biomaterial for the radiation of radioactive holmium to the various cancer sites. The homogeneity of the prepared sol-gel silica holmium monoliths was investigated by Back Scattered Electron Imaging of Scanning Electron Microscope equipped with Energy Dispersive X-ray Analysis, X-ray Induced Photoelectron Spectroscopy and Nuclear Magnetic Resonance Spectroscopy. The biodegradation of the monoliths was investigated in Simulated Body Fluid and TRIS (Trizma pre-set Crystals) solution. The results show that by suitable tailoring of the sol-gel processing parameters holmium can be homogeneously incorporated in the silica matrix with a controlled biodegradation rate.

  13. Sol-gel deposition of buffer layers on biaxially textured metal substances

    SciTech Connect

    Shoup, S.S.; Paranthamam, M.; Beach, D.B.; Kroeger, D.M.; Goyal, A.

    2000-06-20

    A method is disclosed for forming a biaxially textured buffer layer on a biaxially oriented metal substrate by using a sol-gel coating technique followed by pyrolyzing/annealing in a reducing atmosphere. This method is advantageous for providing substrates for depositing electronically active materials thereon.

  14. Investigation of an automated cleaning system for LMJ coating sol-gel process

    NASA Astrophysics Data System (ADS)

    Lavastre, E.; Fontaine, S.; Bergez, R.; Wender, P.; Cormont, P.; Pellegrini, C.; Beaurain, L.; Belleville, P.

    2008-09-01

    The French Commission for Atomic Energy is currently involved in a project which consists in the construction of a 2MJ/500TW (351nm) laser, so called LMJ (Megajoule-class laser) devoted to Inertial Confinement Fusion (ICF) research in France[1]. For this high power lasers, the sol-gel process[2] has been selected for 95% of laser optical coated area because of room temperature and atmospheric pressure conditions with guarantee for high optical and laser induced damage threshold (LIDT) performances at a low cost compared to conventional vacuum deposition processes. The production rate of sol-gel coatings for the LMJ optical components will require an automated cleaning surface step during sol-gel process. We are investigating a spraying system and wash cycles compatible with the two sol-gel deposition methods: dip and laminar-flow coating. The challenge is to achieve the same cleaned optical surfaces as manual process without using organic solvents. Therefore the main specifications of the cleaning quality are the following ones: a high surface energy over all optical sides (up to 400×400 mm2 area) and no degradation of polished sides (surface defects and LIDT). We present the metrologies carried out and the first results obtained from different wash cycles. These one mainly consist in measurement of contact angles, defects inspections under specific lighting conditions and LIDT tests. Several parameters of wash cycles have been investigated such as washing and rinsing temperatures, water quality, type and concentration of detergents, wettability effects...

  15. A Sol-Gel-Modified Poly(methyl methacrylate) Electrophoresis Microchip with a Hydrophilic Channel Wall

    SciTech Connect

    Chen, Gang; Xu, Xuejiao; Lin, Yuehe; Wang, Joseph

    2007-07-27

    A sol-gel method was employed to fabricate a poly(methyl methacrylate) (PMMA) electrophoresis microchip that contains a hydrophilic channel wall. To fabricate such a device, tetraethoxysilane (TEOS) was injected into the PMMA channel and was allowed to diffuse into the surface layer for 24 h. After removing the excess TEOS, the channel was filled with an acidic solution for 3 h. Subsequently, the channel was flushed with water and was pretreated in an oven to obtain a sol-gel-modified PMMA microchip. The water contact angle for the sol-gel-modified PMMA was 27.4° compared with 66.3° for the pure PMMA. In addition, the electro-osmotic flow increased from 2.13×10-4 cm2 V-1 s-1 for the native-PMMA channel to 4.86×10-4 cm2 V-1 s-1 for the modified one. The analytical performance of the sol-gel-modified PMMA microchip was demonstrated for the electrophoretic separation of several purines, coupled with amperometric detection. The separation efficiency of uric acid increased to 74 882.3 m-1 compared with 14 730.5 m-1 for native-PMMA microchips. The result of this simple modification is a significant improvement in the performance of PMMA for microchip electrophoresis and microfluidic applications.

  16. Planar optical integrated circuits based on UV-patternable sol-gel technology

    NASA Astrophysics Data System (ADS)

    Sabattie, Jean-Marc; MacCraith, Brian D.; Mongey, Karen; Charmet, Jerome; O'Dwyer, Kieran; Pez, Mathias M.; Quentel, Francois; Thierry, Dean

    2003-03-01

    Planar lightwave circuits (PLCs) made from photo-patternable sol-gel materials are attracting considerable R&D interest. This is due to the advantages they offer for applications in optical telecommunications and their compatibility with existing silicon technology process equipment. In particular, the ability to produce devices compatible with silica optical fibres using a straightforward, environmentally friendly, photolithographic process is very attractive. The approach is now well-established in the literature and typically involves the incorporation of an acrylate moiety in the sol-gel precursor mixture, thereby providing a photo-polymerisability function. In this work, we report on the fabrication of passive optical components and devices designed for datacomms applications using visible diode lasers or the 1st telecom window. Silica-based sol-gel waveguides have been integrated in an opto-electronic multichip module (OE-MCM) demonstrator for optical interconnect applications. We have fabricated an 8-channel transmitter module for parallel optical interconnects (POI) based on 2 sub-modules: (a) an optical interface sub-assembly based on photo-patterned sol-gel optical waveguides, and (b) an optoelectronic component sub-module comprising an array of VCSELs. We describe here the fabrication, characterization and performance of the optical components and a POI Transmitter chip.

  17. Sol-gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

    NASA Astrophysics Data System (ADS)

    Kareiva, Simonas; Klimavicius, Vytautas; Momot, Aleksandr; Kausteklis, Jonas; Prichodko, Aleksandra; Dagys, Laurynas; Ivanauskas, Feliksas; Sakirzanovas, Simas; Balevicius, Vytautas; Kareiva, Aivaras

    2016-09-01

    Aqueous sol-gel chemistry route based on ammonium-hydrogen phosphate as the phosphorus precursor, calcium acetate monohydrate as source of calcium ions, and 1,2-ethylendiaminetetraacetic acid (EDTA), or 1,2-diaminocyclohexanetetracetic acid (DCTA), or tartaric acid (TA), or ethylene glycol (EG), or glycerol (GL) as complexing agents have been used to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, CHAp). The phase transformations, composition, and structural changes in the polycrystalline samples were studied by infrared spectroscopy (FTIR), X-ray powder diffraction analysis (XRD), and scanning electron microscopy (SEM). The local short-range (nano- and mezo-) scale effects in CHAp were studied using solid-state NMR spectroscopy. The spatial 3D data from the SEM images of CHAp samples obtained by TA, EG and GL sol-gel routes were recovered for the first time to our knowledge.

  18. Iron specificity of a biosensor based on fluorescent pyoverdin immobilized in sol-gel glass

    PubMed Central

    2011-01-01

    Two current technologies used in biosensor development are very promising: 1. The sol-gel process of making microporous glass at room temperature, and 2. Using a fluorescent compound that undergoes fluorescence quenching in response to a specific analyte. These technologies have been combined to produce an iron biosensor. To optimize the iron (II or III) specificity of an iron biosensor, pyoverdin (a fluorescent siderophore produced by Pseudomonas spp.) was immobilized in 3 formulations of porous sol-gel glass. The formulations, A, B, and C, varied in the amount of water added, resulting in respective R values (molar ratio of water:silicon) of 5.6, 8.2, and 10.8. Pyoverdin-doped sol-gel pellets were placed in a flow cell in a fluorometer and the fluorescence quenching was measured as pellets were exposed to 0.28 - 0.56 mM iron (II or III). After 10 minutes of exposure to iron, ferrous ion caused a small fluorescence quenching (89 - 97% of the initial fluorescence, over the range of iron tested) while ferric ion caused much greater quenching (65 - 88%). The most specific and linear response was observed for pyoverdin immobilized in sol-gel C. In contrast, a solution of pyoverdin (3.0 μM) exposed to iron (II or III) for 10 minutes showed an increase in fluorescence (101 - 114%) at low ferrous concentrations (0.45 - 2.18 μM) while exposure to all ferric ion concentrations (0.45 - 3.03 μM) caused quenching. In summary, the iron specificity of pyoverdin was improved by immobilizing it in sol-gel glass C. PMID:21554740

  19. Fabrication and characterization of sol-gel derived 45S5 Bioglass®-ceramic scaffolds.

    PubMed

    Chen, Qi-Zhi; Thouas, George A

    2011-10-01

    Although Bioglass® has existed for nearly half a century its ability to trigger bone formation and tuneable degradability is vastly superior to other bioceramics, such as SiO(2)-CaO bioactive glasses. The sol-gel process of producing glass foams is well established for SiO(2)-CaO compositions, but not yet established for 45S5 composites containing Na(2)O. In this work the sol-gel derived 45S5 Bioglass® has for the first time been foamed into highly porous three-dimensional scaffolds using a surfactant, combined with vigorous mechanical stirring and subsequent sintering at 1000°C for 2 h. It was found that the mechanical strength of the sintered sol-gel derived Bioglass® scaffolds was significantly improved, attributable to the small fraction of material on the pore walls. More importantly, the compressive strength of the three-dimensional scaffolds produced by this surfactant foaming method could be predicted using Gibson and Ashby's closed cell model of porous networks. A comparative experiment revealed that ion release from the sol-gel derived Bioglass® foams was faster than that of counterparts produced by the replication technique. In vitro evaluation using osteoblast-like cells demonstrated that the sol-gel derived 45S5 Bioglass foams supported the proliferation of viable cell populations on the surface of the scaffolds, although few cells were observed to migrate into the virtually closed pores within the foams. Further work should be focused on modifications of the reaction conditions or alternative foaming techniques to improve pore interconnection.

  20. Magnetic resonance as a structural probe of a uranium (VI) sol-gel process

    SciTech Connect

    King, C.M.; Thompson, M.C.; Buchanan, B.R. ); King, R.B. . Dept. of Chemistry); Garber, A.R. . Dept. of Chemistry)

    1989-01-01

    NMR investigations on the ORNL process for sol-gel synthesis of microspherical nuclear fuel (UO{sub 2}), has been useful in sorting out the chemical mechanism in the sol-gel steps. {sup 13}C, {sup 15}N, and {sup 1}H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C{sub 6}H{sub l2}N{sub 4}) has revealed near quantitative stability of this adamantane-like compound in the sol-Gel process, contrary to its historical role as an ammonia source for gelation from the worldwide technical literature. {sub 17}0 NMR of uranyl (UO{sub 2}{sup ++}) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, ((UO{sub 2}){sub 3}({mu}{sub 3}-O)({mu}{sub 2}-OH){sub 3}){sup +}, induced by basic hydrolysis with the HMTA gelation agent. Spectroscopic results show that trimer condensation occurs during sol-gel processing leading to layered polyanionic hydrous uranium oxides in which HMTAH{sup +} is occluded as an intercalation'' cation. Subsequent sol-gel processing of microspheres by ammonia washing results in in-situ ion exchange and formation of a layered hydrous ammonium uranate with a proposed structural formula of (NH{sub 4}){sub 2}((UO{sub 2}){sub 8}O{sub 4}(OH){sub 10}) {center dot} 8H{sub 2}0. This compound is the precursor to sintered U0{sub 2} ceramic fuel.

  1. Magnetic resonance as a structural probe of a uranium (VI) sol-gel process

    SciTech Connect

    King, C.M.; Thompson, M.C.; Buchanan, B.R.; King, R.B.; Garber, A.R.

    1989-12-31

    NMR investigations on the ORNL process for sol-gel synthesis of microspherical nuclear fuel (UO{sub 2}), has been useful in sorting out the chemical mechanism in the sol-gel steps. {sup 13}C, {sup 15}N, and {sup 1}H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C{sub 6}H{sub l2}N{sub 4}) has revealed near quantitative stability of this adamantane-like compound in the sol-Gel process, contrary to its historical role as an ammonia source for gelation from the worldwide technical literature. {sub 17}0 NMR of uranyl (UO{sub 2}{sup ++}) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, [(UO{sub 2}){sub 3}({mu}{sub 3}-O)({mu}{sub 2}-OH){sub 3}]{sup +}, induced by basic hydrolysis with the HMTA gelation agent. Spectroscopic results show that trimer condensation occurs during sol-gel processing leading to layered polyanionic hydrous uranium oxides in which HMTAH{sup +} is occluded as an ``intercalation`` cation. Subsequent sol-gel processing of microspheres by ammonia washing results in in-situ ion exchange and formation of a layered hydrous ammonium uranate with a proposed structural formula of (NH{sub 4}){sub 2}[(UO{sub 2}){sub 8}O{sub 4}(OH){sub 10}] {center_dot} 8H{sub 2}0. This compound is the precursor to sintered U0{sub 2} ceramic fuel.

  2. Large-area sol-gel optical coatings for the Megajoule Laser prototype

    NASA Astrophysics Data System (ADS)

    Pegon, Philippe M.; Germain, Chantal V.; Rorato, Yannick R.; Belleville, Philippe F.; Lavastre, Eric

    2004-02-01

    In the field of thin film coatings, sol-gel (SG) process is an alternative to the conventional Physical Vapor Deposition (PVD) techniques. Sol-gel process is particularly competitive on large-area or fragile substates by taking advantage of various liquid phase deposition techniques performed at room temperature and atmospheric pressure, coupled with the versatility of organo-metallic chemistry. Developed by the French Commission for Atomic Energy (CEA) since 1985 for its former high-power lasers generation, optimized sol-gel coatings proved also very resistant to laser energy. In 1998, THALES Angenieux (TAGX) was selected by CEA to provide all the sol-gel coatings dedicated to the French Laser MegaJoule (LMJ) prototype, named Ligne d'Integration Laser (LIL). In cooperation with Saint-Etienne Pole Optique et Vision (POV), TAGX initiated the building of a sol-gel technological platform (SGPF) aimed at demonstrating the feasibility of production of optical and functional coatings on large area substrates. A technology transfer was performed by CEA (Le Ripault) to TAGX focusing on the manufacture mainly of single-layer antireflective coatings (SLAR), but also of multi-layer AR-coatings and of multi-layered highly reflective (HR)-coatings. Since beginning of 2001 and using SGPF equipments, TAGX successfully coated within specificaitons and schedule most of the 300 optics required for LIL activation. After this 2 years 1/2 production campaign in pre-industrial conditions, we can now analyse the advantages of each deposition technique used, the repeatability of the several processes, and the performance of the various coatings.

  3. Low temperature and UV curable sol-gel coatings for long lasting optical fiber biosensors

    NASA Astrophysics Data System (ADS)

    Otaduy, D.; Villar, A.; Gomez-Herrero, E.; Goitandia, A. M.; Gorritxategi, E.; Quintana, I.

    2010-04-01

    The use of optical fibers as sensing element is increasing in clinical, pharmaceutical and industrial applications. Excellent light delivery, long interaction length, low cost and ability not only to excite the target molecules but also to capture the emitted light from the targets are the hallmarks of optical fiber as biosensors. In biosensors based on fiber optics the interaction with the analyte can occur within an element of the optical fiber. One of the techniques for this kind of biosensors is to remove the fiber optic cladding and substitute it for biological coatings that will interact with the parameter to sensorize. The deposition of these layers can be made by sol-gel technology. The sol-gel technology is being increasingly used mainly due to the high versatility to tailor their optical features. Incorporation of suitable chemical and biochemical sensing agents have allowed determining pH, gases, and biochemical species, among others. Nonetheless, the relatively high processing temperatures and short lifetime values mean severe drawbacks for a successful exploitation of sol-gel based coated optical fibres. With regard to the latter, herein we present the design, preparation and characterization of novel sol-gel coated optical fibres. Low temperature and UV curable coating formulations were optimized to achieve a good adhesion and optical performance. The UV photopolymerizable formulation was comprised by glycidoxypropyltrimethoxysilane (GLYMO), Tetraethylorthosilicate (TEOS) and an initiator. While the thermoset coating was prepared by using 3-aminopropyltrimethoxysilane, GLYMO, and TEOS as main reagents. Both curable sol-gel coated fibres were analysed by FTIR, SEM and optical characterization. Furthermore, in the present work a new technique for silica cladding removal has been developed by ultra-short pulses laser processing, getting good dimensional accuracy and surface integrity.

  4. rhEGF-containing thermosensitive and mucoadhesive polymeric sol-gel for endoscopic treatment of gastric ulcer and bleeding.

    PubMed

    Maeng, Jin Hee; So, Jung Won; Kim, Jungju; Kim, In Ae; Jung, Ji Hoon; Min, Kyunghyun; Lee, Don Haeng; Yang, Su-Geun

    2014-03-01

    Gastrointestinal endoscopy is a standard diagnostic tool for gastrointestinal ulcers and cancer. In this study, we have developed recombinant human epidermal growth factor-containing ulcer-coating polymeric sol-gel for endoscopic application. Chitosan and pluronic F127 were employed for their thermoresponsive and bioadhesive properties. At temperatures below 21, polymeric sol-gel remains liquid during endoscopic application and transforms to gel at body temperature after application on ulcers. In an in vitro cellular wounding assay, recombinant human epidermal growth factor sol-gel significantly enhanced the cell migration and decreased the wounding area (68%) compared to nontreated, recombinant human epidermal growth factor solution, and sol-gel without recombinant human epidermal growth factor (42, 49, and 32 % decreased at day 1). The in vivo ulcer-healing study was performed in an acetic acid-induced gastric ulcer rat model and proved that our recombinant human epidermal growth factor endoscopic sol-gel facilitated the ulcer-healing process more efficiently than the other treatments. Ulcer sizes in the recombinant human epidermal growth factor sol-gel group were decreased 2.9- and 2.1-fold compared with those in the nontreated group on days 1 and 3 after ulceration, respectively. The mucosal thickness in the recombinant human epidermal growth factor sol-gel group was significantly increased compared to that in the nontreated group (3.2- and 6.9-fold on days 1 and 3 after ulceration, respectively). In a gastric retention study, recombinant human epidermal growth factor sol-gel stayed on the gastric mucosa more than 2 h after application. The present study suggests that recombinant human epidermal growth factor sol-gel is a prospective candidate for treating gastric ulcers via endoscopic application.

  5. Preparation and characterization of urease-encapsulated biosensors in poly(vinyl alcohol)-modified silica sol-gel materials.

    PubMed

    Tsai, Hsiao-chung; Doong, Ruey-an

    2007-08-30

    The microenvironments of the sol-gel-derived urease biosensors in terms of elemental ratio, surface morphology, specific surface area and pore size were investigated to characterize the physicochemical properties of poly(vinyl alcohol) (PVA)-modified sol-gel materials. X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and surface area analyzer were used to identify the surface species, topography and pore distribution of the organically doped sol-gel network. XPS results showed that stoichiometric ratios of oxygen-to-silicon in sol-gel materials were in the range 2.08-2.11. The sol-gel materials were partially dried and negatively charged, which retained 6-8% water content to maintain urease activity. The surface morphology of the sol-gel altered obviously when macromolecules were encapsulated, resulting in the increase in surface mean roughness from 0.207 to 2.636 nm. The specific surface area decreased dramatically after the immobilization of biomolecules and organic additives, which clearly depicts that PVA and urease were co-encapsulated into the sol-gel network. However, there still exist enough pore volumes for analytes to mass transport. The apparent Michaelis-Menten constant value (Km) of the encapsulated urease was similar to that in solution and the overall catalytic efficiency in PVA-doped sol-gel-derived glasses only decreased by a factor of 3.2 relative to the value in solution. In addition, the analytical performance of the entrapped urease in PVA-doped sol-gel materials was examined by determining the Cu(II) concentration in aqueous solution. The analytical range of Cu(II) was in the range 2x10(-6) to 2x10(-2) M with a detection limit of 1.5 microg L(-1). Results obtained in this study demonstrate a strategy for maintaining urease activity for biomedical and environmental applications.

  6. Novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as solid phase extraction sorbent for organophosphorus pesticides.

    PubMed

    Wan Ibrahim, Wan Aini; Veloo, Krishna Veni; Sanagi, Mohd Marsin

    2012-03-16

    A novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was produced and applied as sorbent for solid phase extraction (SPE). Five selected organophosphorus pesticides (OPPs) were employed as model compounds to evaluate the extraction performance of the synthesized sol-gel organic-inorganic hybrid MTMOS-TEOS. Analysis was performed using gas chromatography-mass spectrometry. Several important SPE parameters were optimized. Under the optimum extraction conditions, the method using the sol-gel organic-inorganic hybrid MTMOS-TEOS as SPE sorbent showed good linearity in the range of 0.001-1 μg L(-1), good repeatability (RSD 2.1-3.1%, n=5), low limits of detection at S/N=3 (0.5-0.9 pg mL(-1)) and limit of quantification (1-3 pg mL(-1), S/N=10). The performance of the MTMOS-TEOS SPE was compared to commercial C18 Supelclean SPE since C18 SPE is widely used for OPPs. The MTMOS-TEOS SPE method LOD was 500-600 × lower than the LOD of commercial C18 SPE. The LOD achieved with the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent allowed the detection of these OPPs in drinking water well below the level set by European Union (EU) at 0.1 μg L(-1) of each pesticides. The developed MTMOS-TEOS SPE method was successfully applied to real sample analysis of the selected OPPs from several water samples and its application extended to the analysis of several fruits samples. Excellent recoveries and RSDs of the OPPs were obtained from the various water samples (recoveries: 97-111%, RSDs 0.4-2.8%, n=3) and fruit samples (recoveries: 96-111%), RSDs 1-4%, n=5) using the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent. Recoveries and RSDs of OPPs from river water samples and fruit samples using C18 Supelclean SPE sorbent were 91-97%, RSD 0.9-2.6, n=3 and 86-96%, RSD 3-8%, n=5, respectively). The novel sol-gel hybrid MTMOS-TEOS SPE sorbent demonstrate the potential as an alternative inexpensive extraction sorbent for OPPs with higher sensitivity for

  7. Fiber-optic chemical sensors using sol-gel membranes and photocatalysts

    NASA Astrophysics Data System (ADS)

    Nivens, Delana Amber Gajdosik

    Fiber-optic sensors have been developed that incorporate multi-layer organo-silica sol-gel membranes. Multilayer sol-gel sensors have been designed to offer improved stability over other sol-gel membranes and to measure COsb2 and the unreactive analytes trichloroethylene and perchloroethylene. Single layer pH sensors were fabricated using a base-catalyzed organo-silica sol-gel containing organosilane coupling agents. A base catalyst was found to be better suited for complete incorporation of the aminopropyltriethoxysilane used to attach dye molecules. This allows the production of optically transparent gels that respond to pH in less than 15 seconds. Dual layer COsb2 sensors use the pH sol-gel layer overcoated with a hydrophobic ORganically MOdified SIlica sol-gel membrane (ORMOSIL). The ORMOSIL reduces much of the pH cross sensitivity found in gas sensors and allows fast, reversible diffusion of COsb2. The sensors respond to COsb2 gas within 10 seconds and dissolved COsb2 in 2 minutes. COsb2 sensors have been found to be stable and reproducible for 12 months when stored dry and at least 6 months when stored in buffer. Many volatile organochloride compounds (VOC's) have been difficult to measure using current fiber-optic sensor transduction schemes. The three-layer optical sensor described here incorporates a TiOsb2/SiOsb2 membrane to degrade VOC's into smaller, detectable products, Hsp+, Clsp- and COsb2. Upon exposure to UV light, TiOsb2, a semiconductor with a bandgap of 3.2 eV, produces highly reactive electron-hole pairs that photodegrade organic compounds. The products produced on the TiOsb2 surface diffuse into the nearby indicator membrane where they are detected. Carbon dioxide and protons produced are detected by the pH sensitive indicator layer described above. Preliminary data for the measurement of VOC's indicates that the detection limit for PCE is less than 1.65 ppm in the headspace (10 ppm in solution). Photocatalysis is also used to measure uranyl

  8. Synthesis and enhanced thermal stability of albumins@alumina: towards injectable sol-gel materials.

    PubMed

    Rutenberg, Avi; Vinogradov, Vladimir V; Avnir, David

    2013-06-25

    A major obstacle to the introduction of bioactively-doped sol-gel based materials for medical applications has been the fact that silica - the most widely studied sol-gel material - despite being a GRAS material, which is widely used as an additive in foods and drug formulations, is still not approved by regulatory agencies for intramuscular injections. Here we point to a potential solution to this problem by shifting the weight to alumina, which is approved for injections as the most common immunization adjuvant. Towards the achievement of this goal we describe the development of protein entrapment methods tailored to alumina, and show high thermal stability of protein-dopants, using a newly developed DSC methodology for this purpose.

  9. Sol-gel co-assembly of hollow cylindrical inverse opals and inverse opal columns.

    PubMed

    Haibin, Ni; Ming, Wang; Wei, Chen

    2011-12-19

    A facile approach of fabricating hollow cylindrical inverse opals and inverse opal columns by sol-gel co-assembly method was proposed. Polystyrene (PS) colloidal suspension added with hydrolyzed silicate precursor solution was used to self-assemble composite colloidal crystals which consist of PS colloidal crystal template and infiltrated silica gel in the interstitial of microspheres. Continuous hollow cylindrical composite colloidal crystal films have been produced on capillaries' outside and internal surface. Composite colloidal crystal columns which filling up the interior of a capillary were fabricated by pressure assisted sol-gel co-assembly method. Hollow cylindrical inverse opals and inverse opal columns were obtained after removing PS colloidal crystal from the composite colloidal crystal. Optical properties of the silica hollow cylindrical inverse opals were characterized by transmission spectrum and a stop band was observed. Structure and optical properties of the inverse opal columns were investigated.

  10. The porosity of sol-gel silica thin films for optrode applications

    SciTech Connect

    Harris, T.M.; Knobbe, E.T.

    1995-12-01

    Porous silica thin films produced by sol-gel processing are being considered for use in optical sensor (optrode) applications. In this study, thin films were produced by dip-coating onto glass slides. The porosity was then measured indirectly, by determining the amount of methylene blue adsorption on each slide. Using this technique, it has been determined that the {open_quotes}two-step{close_quotes} sol-gel process provides a greater surface area than the acid-catalyzed process. With the two-step process, increasing the amount of solvent (ethanol) and decreasing the rate of slide withdrawal from the sol provided increased surface area when normalized to the mass of the deposit.

  11. Cotton Fabric Surface Modification by Sol-Gel Deposition of ZnO Thin Films

    NASA Astrophysics Data System (ADS)

    Vihodceva, S.; Kukle, S.

    2012-08-01

    One of the main tasks of research is to impact the additional value on natural textiles by adding to them ultraviolet (UV) absorption and antimicrobial protection properties with ZnO nano-level coatings. ZnO shows high absorption in the UV region of the light spectrum, in comparison with organic absorbers conventionally used in the textile industry shows no significant degradation, is stable and classified as non-toxic material. Nanosols were prepared by using the sol-gel process. In this work comparison of samples coated by nanosols with zinc acetate (Zn (CH3COO)2-2H2O) and zinc sulphate (ZnSO4) was made. Scanning electron microscopy (SEM) was used to examine the nature of the surface modification with ZnO coating by the sol-gel technique as also after exploitation of samples; energy dispersive X-ray spectroscopy was used for the analysis of elemental composition of coated fabric samples.

  12. β-Diketones and their derivatives in sol-gel processes

    NASA Astrophysics Data System (ADS)

    Zolotareva, N. V.; Semenov, V. V.

    2013-10-01

    Published data on the use of β-diketones, metal β-diketonates and some structurally related compounds in sol-gel synthesis of new organic-inorganic hybrid materials are analyzed. Functionalization methods of β-diketones with carbofunctional organosilicon compounds are considered. Ways of insertion of a metal cation into the organic-inorganic hybrid matrix using non-functionalized β-diketonates are demonstrated. Particular attention is devoted to luminescent lanthanide derivatives, which is due to the prospects of practical application of materials obtained from them in photonics, integrated optics and medical diagnosis. The types and properties of most widely used sol-gel monomers and oligomers and the luminescence behaviour of lanthanide β-diketonates and metal-free silica matrices are considered. The bibliography includes 220 references.

  13. Nanocrystalline indium tin oxide fabricated via sol-gel combustion for electrochemical luminescence cells.

    PubMed

    Chaoumead, Accarat; Kim, Tae-Woo; Park, Min-Woo; Sung, Youl-Moon

    2012-04-01

    Nanoporous indium tin oxide (ITO) was synthesized via a sol-gel combustion hybrid method using Ketjenblack as a fuel. The effects of the sol-gel combustion conditions on the structures and morphology of the ITO particles were studied. The size of the nanoporous powder was found to be 20-30 nm in diameter. The layer of the nanoporous ITO electrode (-10 microm thickness) with large surface area (-360 m2/g) was fabricated for an electrochemical luminescence (ECL) cell. At 4 V bias, the ECL efficiency of the cell consisting of the nanoporous ITO layer was approximately 1050 cd/m2, which is significantly higher than the cell using only the FTO electrode (450 cd/m2). The nanoporous ITO layer was effective in increasing the ECL intensities.

  14. Sol-gel production of bioactive nanocoatings for medical applications. Part 1: an introduction.

    PubMed

    Ben-Nissan, Besim; Choi, Andy H

    2006-10-01

    Coatings offer the possibility of modifying the surface properties of surgical-grade materials to achieve improvements in performance, reliability and biocompatibility. Sol-gel-derived coatings demonstrate promise owing to their relative ease of production, ability to form a physically and chemically pure and uniform coating over complex geometric shapes and potential to deliver exceptional mechanical properties owing to their nanocrystalline structure. Other advantages unique to sol-gel include the production of a homogeneous material, since mixing takes place on the atomic scale, and its relatively low processing temperature avoids decomposition of the coating materials and limits the damage to metallic substrate materials as a result of exposure to elevated temperatures. A range of materials can be adapted easily for a number of biomedical and engineering applications.

  15. Fluor-hydroxyapatite sol-gel coating on titanium substrate for hard tissue implants.

    PubMed

    Kim, Hae-Won; Kim, Hyoun-Ee; Knowles, Jonathan C

    2004-08-01

    Hydroxyapatite (HA) and fluor-hydroxyapatite (FHA) films were deposited on a titanium substrate using a sol-gel technique. Different concentrations of F- were incorporated into the apatite structure during the sol preparation. Typical apatite structures were obtained for all coatings after dipping and subsequent heat treatment at 500 degrees C. The films obtained were uniform and dense, with a thickness of approximately 5 microm. The dissolution rate of the coating layer decreased with increasing F- incorporation within the apatite structure, which demonstrates the possibility of tailoring the solubility by a functional gradient coating of HA and FHA. The cell proliferation rate on the coating layer decreased slightly with increasing F- incorporation. The alkaline phosphatase (ALP) activity of the cells on all the HA and FHA coated samples showed much higher expression levels compared to pure Ti. This confirmed the improved activity of cell functions on the substrates with the sol-gel coating treatment.

  16. Sol-gel derived aluminosilicate coatings on alumina as substrate for osteoblasts.

    PubMed

    Leivo, Jarkko; Meretoja, Ville; Vippola, Minnamari; Levänen, Erkki; Vallittu, Pekka; Mäntylä, Tapio A

    2006-11-01

    Rat bone marrow stromal cell differentiation on aluminosilicate 3Al(2)O(3)-2SiO(2) coatings was investigated. Thin ceramic coatings were prepared on alpha-alumina substrates by the sol-gel process and calcined in order to establish an amorphous aluminosilicate ceramic phase with and without nanosized transitional mullite crystals. In addition, coatings of thermally sprayed aluminosilicate and diphasic gamma-alumina-silica nanosized colloids were prepared. Cell culture testing by rat osteoblasts showed good biocompatibility for aluminosilicates with sustained normal osteoblast functions. Despite mutual disparities in physical and chemical nanostructures, the culture findings suggested fairly similar osteoblast response to all tested coatings. The results suggest that topographical frequency parameters and chemical uniformity are important parameters in determining the best conditions for osteoblasts on sol-gel derived aluminosilicate materials.

  17. Surface aspects of sol-gel derived hematite films for the photoelectrochemical oxidation of water.

    PubMed

    Herrmann-Geppert, Iris; Bogdanoff, Peter; Radnik, Jörg; Fengler, Steffen; Dittrich, Thomas; Fiechter, Sebastian

    2013-02-07

    α-Fe(2)O(3) (hematite) photoanodes for the oxygen evolution reaction (OER) were prepared by a cost-efficient sol-gel procedure. Due to low active photoelectrochemical properties observed, it is assumed that the sol-gel procedure leads to hematite films with defects and surface states on which generated charge carriers are recombined or immobilized in trap processes. Electrochemical activation was proven to diminish unfavourable surface groups to some extent. More efficiently, a plasma treatment improves significantly the photoelectrochemical properties of the OER. X-ray photoelectron spectroscopy (XPS) analysis reveals an oxygen enriched surface layer with new oxygen species which may be responsible for the improved electrochemical activity. Due to surface photovoltage an increased fraction of transferred charge carriers from these newly produced surface defects are identified.

  18. Moisture sensor based on evanescent wave light scattering by porous sol-gel silica coating

    DOEpatents

    Tao, Shiquan; Singh, Jagdish P.; Winstead, Christopher B.

    2006-05-02

    An optical fiber moisture sensor that can be used to sense moisture present in gas phase in a wide range of concentrations is provided, as well techniques for making the same. The present invention includes a method that utilizes the light scattering phenomenon which occurs in a porous sol-gel silica by coating an optical fiber core with such silica. Thus, a porous sol-gel silica polymer coated on an optical fiber core forms the transducer of an optical fiber moisture sensor according to an embodiment. The resulting optical fiber sensor of the present invention can be used in various applications, including to sense moisture content in indoor/outdoor air, soil, concrete, and low/high temperature gas streams.

  19. Enhanced optical band-gap of ZnO thin films by sol-gel technique

    NASA Astrophysics Data System (ADS)

    Raghu, P.; Naveen, C. S.; Shailaja, J.; Mahesh, H. M.

    2016-05-01

    Transparent ZnO thin films were prepared using different molar concentration (0.1 M, 0.2 M & 0.8 M) of zinc acetate on soda lime glass substrates by the sol-gel spin coating technique. The optical properties revealed that the transmittance found to decrease with increase in molar concentration. Absorption edge showed that the higher concentration film has increasingly red shifted. An increased band gap energy of the thin films was found to be direct allowed transition of ˜3.9 eV exhibiting their relevance for photovoltaic applications. The extinction coefficient analysis revealed maximum transmittance with negligible absorption coefficient in the respective wavelengths. The results of ZnO thin film prepared by sol-gel technique reveal its suitability for optoelectronics and as a window layer in solar cell applications.

  20. Glucose microbiosensor based on alumina sol-gel matrix/electropolymerized composite membrane.

    PubMed

    Chen, Xiaohong; Hu, Yibai; Wilson, George S

    2002-12-01

    A procedure is described that provides co-immobilization of enzyme and bovine serum albumin (BSA) within an alumina sol-gel matrix and a polyphenol layer permselective for endogenous electroactive species. BSA has first been employed for the immobilization of glucose oxidase (GOx) on a Pt electrode in a sol-gel to produce a uniform, thin and compact film with enhanced enzyme activity. Electropolymerization of phenol was then employed to form an anti-interference and protective polyphenol film within the enzyme layer. In addition, a stability-reinforcing membrane derived from (3-aminopropyl)-trimethoxysilane was constructed by electrochemically-assisted crosslinking. This hybrid film outside the enzyme layer contributed both to the improved stability and to permselectivity. The resulting glucose sensor was characterized by a short response time (<10 s), high sensitivity (10.4 nA/mM mm(2)), low interference from endogenous electroactive species, and a working lifetime of at least 60 days.

  1. The Physics of Evaporation-Induced Assembly of Sol-Gel Materials

    SciTech Connect

    HURD,ALAN J.; STEINBERG,LEV

    2000-07-24

    Remarkable materials ordered at the nanoscale emerge when a sol-gel solution becomes co-organized with a surfactant. At sufficiently high concentration, the surfactant forms crystalline or liquid-crystalline arrays of micelles in the presence of the sol-gel, and as gelation proceeds the arrays become locked into the gel. Recent experiments demonstrate that the degree of order in the resulting mesoporous ceramic phase can be enhanced and controlled by continuous dip coating in which the solution, initially dilute, evolves through the critical micelle concentration by steady-state evaporation. The long-range order and microstructural orientation in these films suggest that the propagation of a critical-micelle-concentration transition front, with large physico-chemical gradients, promotes oriented self assembly of surfactant aggregates. This steep-gradient view is supported by results from unsteady evaporation of aerosols of similar solutions, in which internally well-ordered but complex particles are formed.

  2. Ultrapure glass optical waveguide development in microgravity by the sol-gel process

    NASA Technical Reports Server (NTRS)

    1982-01-01

    Containerless melting of glasses in space for the preparation of ultrapure homogeneous glass for optical waveguides is discussed. The homogenization of the glass using conventional raw materials is normally achieved on Earth either by the gravity induced convection currents or by the mechanical stirring of the melt. Because of the absence of gravity induced convection currents, the homogenization of glass using convectional raw materials is difficult in the space environment. Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation.

  3. Sol-gel technologies in thin film fabrication for integrated optics lasers and amplifiers

    NASA Astrophysics Data System (ADS)

    Almeida, Rui M.; Vasconcelos, H. C.

    1997-07-01

    There is a strong need for the development of cheap component technologies for optical functions such as switching, demultiplexing and amplification. Silica-on- silicon integrated optics using sol-gel processing is probably the best technology for such low cost applications. This review focuses on the sol-gel based thin film fabrication technologies for integrated optics (IO) lasers and amplifiers, using Nd3+ and Er3+ as the active species. Special emphasis is given to the work performed under the European Union sponsored projects NODES (ESPRIT) and CAPITAL (ACTS), in particular to the processing and characterization of Nd3+ and Er3+-doped silica-titania planar waveguides for IO lasers and amplifiers.

  4. Versatile technique to functionalize optical microfibers via a modified sol-gel dip-coating method.

    PubMed

    Xu, Z Y; Li, Y H; Wang, L J

    2014-01-01

    We present a convenient and versatile technique to functionalize microfibers by depositing sol-gel jackets via a modified dip-coating method. This was elucidated by gain-functionalizing microfibers with erbium-ytterbium codoped silica sol-gel jackets. For a 4.5-cm-long coated microfiber, an internal gain of 1.8 dB and a net gain of 0.8 dB for a 1550 nm signal were observed, when combing together the gain of the doped jackets and low loss of microfibers. With benefits of convenience and versatility, this technique can be used for functionalizing microfibers with jackets showing gains in other spectral ranges, high nonlinearity, high sensitivity, and many other functions.

  5. Relaxation dynamics near the sol-gel transition: From cluster approach to mode-coupling theory

    NASA Astrophysics Data System (ADS)

    Coniglio, A.; Arenzon, J. J.; Fierro, A.; Sellitto, M.

    2014-10-01

    A long standing problem in glassy dynamics is the geometrical interpretation of clusters and the role they play in the observed scaling laws. In this context, the mode-coupling theory (MCT) of type-A transition and the sol-gel transition are both characterized by a structural arrest to a disordered state in which the long-time limit of the correlator continuously approaches zero at the transition point. In this paper, we describe a cluster approach to the sol-gel transition and explore its predictions, including universal scaling laws and a new stretched relaxation regime close to criticality. We show that while MCT consistently describes gelation at mean-field level, the percolation approach elucidates the geometrical character underlying MCT scaling laws.

  6. Pulsed electric field assisted sol-gel preparation of TiO2 nanoparticles

    NASA Astrophysics Data System (ADS)

    Mani, Rajaboopathi; Han, Bing; Louhi-Kultanen, Marjatta

    2016-10-01

    This work studies the effect of a pulsed electric field (PEF) on the precipitation and properties of TiO2 nanoparticles. TiO2 nanoparticles were prepared using pulsed DC electric field assisted sol-gel method. The duration of the PEF treatment was varied to investigate its effect on the particle size of TiO2 nanoparticles. The nanoparticles were characterized by X-ray powder diffraction (XRD), Raman spectroscopy, UV diffuse reflectance spectroscopy (UV-DRS) and transmission electron microscopy (TEM). It was found that TiO2 particles prepared with pulsed electric field assisted sol-gel method had enhanced average crystallite size due to the effect of the pulsed electric field on primary nucleation. The effect of electric field on nanoparticle preparation is interesting which can be used to control the grain and crystallite size of nanoparticle.

  7. Photochemical reduction of methyl viologen in silicate xerogels obtained by the sol gel process

    NASA Astrophysics Data System (ADS)

    Maruszewski, Krzysztof; Jasiorski, Marek; Hreniak, Dariusz; Stręk, Wiesław

    2001-10-01

    Mixture of ruthenium (II) tris-bipyridine complex (Ru(bpy) 32+ — photosensitizer), methyl viologen (MV 2+ — electron acceptor) and EDTA (sacrificial electron donor) has been immobilized in silicate xerogels obtained by the sol-gel technique. Mixtures of Ru(bpy) 32+, MV 2+ and EDTA are capable of formation of the blue photoreduced MV rad + cation radical in aqueous solutions upon UV (around 280 nm) or visible (around 450 nm) excitations. However, when entrapped in silicate xerogels they do not exhibit blue coloration at all. On the other hand, UV excitation of xerogels doped only with MV 2+ results in appearance of blue color indicative of the paraquat photoreduction. It has been shown that in the case of the xerogel-entrapped methyl viologen the source of the reducing photoelectron is ethanol. The alcohol molecules are produced during the tetraethoxysilane (precursor) hydrolysis step of the silicate matrix production occurring via the sol-gel process.

  8. The role of temperature in forming sol-gel biocomposites containing polydopamine

    PubMed Central

    Dyke, Jason Christopher; Hu, Huamin; Lee, Dong Joon; Ko, Ching-Chang; You, Wei

    2014-01-01

    To further improve the physical strength and biomedical applicability of bioceramicsbuilt on hydroxyapatite-gelatin (HAp-Gel) and siloxane sol-gel reactions, we incorporated mussel adhesive inspired polydopamine (PD) into our original composite based on HAp-Gel cross-linked with siloxane. Surprisingly, with the addition of PD, we observed that the processing conditions and temperatures play an important role in the structure and performance of these materials. A systematic study to investigate this temperature dependence behavior discloses that the rate of crosslinking of silane during the sol-gel process is significantly influenced by the temperature, whereas the polymerization of the dopamine only shows minor temperature dependence. With this discovery, we report an innovative thermal process for the design and application of these biocomposites. PMID:25485111

  9. Nonlinear optical properties of sol-gel-type glasses containing oxidized Cu2Se nanoparticles

    NASA Astrophysics Data System (ADS)

    Yumashev, K. V.

    2000-03-01

    Nonlinear absorption of sol-gel-type glasses containing oxidized Cu2Se nanoparticles (25 nm in radius) is investigated with the aid of the picosecond excitation-probing technique. The oxidation of Cu2Se nanoparticles leads to the appearance of a wide absorption band, which has a maximum roughly at 1 µm and which is bleached on exposure to laser pulses. The time of relaxation of the bleached state approaches 300 psec, and the cross section for absorption at 1.06 µm is equal to about 1.3·10-16 cm2, as evaluated from the measured absorption saturation curve. The regime of Q-switching is obtained for a number of solid-state lasers with generation wavelengths 1.06, 1.34, and 1.54 µm, when sol-gel-type glasses containing oxidized Cu2Se nanoparticles were used as passive shutters.

  10. A Review of Photocatalysts Prepared by Sol-Gel Method for VOCs Removal

    PubMed Central

    Tseng, Ting Ke; Lin, Yi Shing; Chen, Yi Ju; Chu, Hsin

    2010-01-01

    The sol-gel process is a wet-chemical technique (chemical solution deposition), which has been widely used in the fields of materials science, ceramic engineering, and especially in the preparation of photocatalysts. Volatile organic compounds (VOCs) are prevalent components of indoor air pollution. Among the approaches to remove VOCs from indoor air, photocatalytic oxidation (PCO) is regarded as a promising method. This paper is a review of the status of research on the sol-gel method for photocatalyst preparation and for the PCO purification of VOCs. The review and discussion will focus on the preparation and coating of various photocatalysts, operational parameters, and will provide an overview of general PCO models described in the literature. PMID:20640156

  11. Reversible Sol-Gel Transitions in Aqueous Solutions of N-Isopropylacrylamide Ionic Copolymers

    SciTech Connect

    Krzyminski, Karol J.; Jasionowski, Marek; Gutowska, Anna

    2008-04-01

    Ionic copolymers of N-isopropylacrylamide (NIPA) exhibiting sol-gel transitions in aqueous solutions were investigated. The studies were aimed at understanding of the structure-property relationship in design of injectable, in situ forming gels for potential biomedical applications in delivery of therapeutics and tissue engineering. Aqueous solutions of NIPA ionic copolymers were found to flow freely at ambient temperatures and formed soft gels with controlled syneresis above 32°C, the lower critical solution temperature of NIPA. The sol-gel transitions and temperature dependent properties of the resulting gels were analyzed using dynamic rheometry, UV and IR spectrometry, and were found to be controlled by the molecular weight and composition of copolymers, ionization state of comonomers, and composition of aqueous solvent.

  12. Sol gel based fiber optic sensor for blook pH measurement

    SciTech Connect

    Grant, S. A.; Glass, R. S.

    1996-12-19

    This paper describes a fiber-optic pH sensor based upon sol-gel encapsulation of a self-referencing dye, seminaphthorhodamine-1 carboxylate (SNARF-1C). The simple sol-gel fabrication procedure and low coating leachability are ideal for encapsulation and immobilization of dye molecules onto the end of an optical fiber. A miniature bench-top fluorimeter system was developed for use with the optical fiber to obtain pH measurements. Linear and reproducible responses were obtained in human blood in the pH range 6.8 to 8.0, which encompasses the clinically-relevant range. Therefore, this sensor can be considered for in vivo use.

  13. Luminescent characteristics of sol-gel produced zinc sulphide display structures

    NASA Astrophysics Data System (ADS)

    Kavanagh, Yvonne M.; Cameron, David C.; Ryan, Brendan; Tobin, Ger

    2003-03-01

    Thin film electroluminescent (TFEL) display structures have been produced by sol-gel technology, with the active layer comprising doped zinc sulphide films produced by the sulphidation of sol-gel deposited zinc oxide thin films. The luminescent properties of display structures using manganese-doped zinc sulphide, which has a strong orange emission due to the Mn2+4 T1(4G) 6A1(6S) transitions have been investigated using photoluminescence (PL), cathodoluminescence (CL), and electroluminescence (EL) and the correlation between the luminescence produced by the various methods has been studied. A comparison of the spectra using PL, CL and EL has shown how these excitation methods can be used to quantify the electroluminescence produced by the zinc sulphide. The effects of the interaction between the insulating layer and the emission layer have also been studied.

  14. Synthesis and Characterization of Al doped ZnO (AZO) by Sol-gel Method

    NASA Astrophysics Data System (ADS)

    Munawaroh, H.; Wahyuningsih, S.; Ramelan, A. H.

    2017-02-01

    Al doped ZnO (AZO) nanoparticles have been successfully synthesized by the simple sol-gel method. The starting materials of Al doped ZnO were Zn(CH3COO)2·2H2O and Al(OH)(CH3COO)2. Preparation of AZO using polyethylene glycol as a surfactant. The solution of precursors was stirred at 60 °C for 2 hour in the conditions of Al contents are 0%, 2%, 3% and 4% (g/mL), respectivelly. In the last step reaction, gelation occurred from solution to sol gel. The sol gel then were dried at 60 °C following by annealing process for crystalization. By this simple sol gel method, the nanoparticles have been produced. The characterizations were conducted X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Fourrier Transform Infra-Red (FTIR) and X-Ray Fluorescence (XRF). XRD analysis reveals that all samples has crystallizes in polycrystalline nature and exhibit no other impurity phase. The variation of Al doped ZnO slighly affect the crystallinity and crystal size. Both crystallinity and crystal size decrease with increasing of Al content in AZO. Morphology of AZO shown the particle distribution more equitable with increased Al content. The synthesized AZO gaved shift peak absorption of asymetric and symetric vibrations of Zn-O-Zn around wavelengths of 680 cm-1 and 1630 cm-1 atributed of the uptake of the Al-O-Al bond instead Zn-O-Zn. XRF analysis shown that the increase ratio of Al entering into Zn influenced the Al dopant concentration.

  15. Sol-gel derived bioactive coating on zirconia: Effect on flexural strength and cell proliferation.

    PubMed

    Shahramian, Khalil; Leminen, Heidi; Meretoja, Ville; Linderbäck, Paula; Kangasniemi, Ilkka; Lassila, Lippo; Abdulmajeed, Aous; Närhi, Timo

    2016-09-07

    The purpose of this study was to evaluate the effect of sol-gel derived bioactive coatings on the biaxial flexural strength and fibroblast proliferation of zirconia, aimed to be used as an implant abutment material. Yttrium stabilized zirconia disc-shaped specimens were cut, ground, sintered, and finally cleansed ultrasonically in each of acetone and ethanol for 5 minutes. Three experimental groups (n = 15) were fabricated, zirconia with sol-gel derived titania (TiO2 ) coating, zirconia with sol-gel derived zirconia (ZrO2 ) coating, and non-coated zirconia as a control. The surfaces of the specimens were analyzed through images taken using a scanning electron microscope (SEM), and a non-contact tapping mode atomic force microscope (AFM) was used to record the surface topography and roughness of the coated specimens. Biaxial flexural strength values were determined using the piston-on-three ball technique. Human gingival fibroblast proliferation on the surface of the specimens was evaluated using AlamarBlue assay™. Data were analyzed using a one-way analysis of variance (ANOVA) followed by Tukey's post-hoc test. Additionally, the biaxial flexural strength data was also statistically analyzed with the Weibull distribution. The biaxial flexural strength of zirconia specimens was unaffected (p > 0.05). Weibull modulus of TiO2 coated and ZrO2 coated groups (5.7 and 5.4, respectively) were lower than the control (8.0). Specimens coated with ZrO2 showed significantly lower fibroblast proliferation compared to other groups (p < 0.05). In conclusion, sol-gel derived coatings have no influence on the flexural strength of zirconia. ZrO2 coated specimens showed significantly lower cell proliferation after 12 days than TiO2 coated or non-coated control. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2016.

  16. Development of novel sol-gel indicators (SGI`s) for in-situ environmental measurements

    SciTech Connect

    Livingston, R.R.; Wicks, G.G.; Baylor, L.C.; Whitaker, M.J.

    1993-10-01

    Organic indicator molecules have been incorporated in a porous sol- gel matrix coated on the end of a fiber-optic lens assembly to create sensors for in situ environmental measurements. Probes have been made that are sensitive to pH and uranyl concentration. The use of fiber optics allows the probe to be lowered into a well or bore hole, while support equipment such as a spectrophotometer and computer may be situated hundreds of meters away.

  17. The detection of hexavalent chromium by organically doped sol-gels

    SciTech Connect

    Wong, P.W.; Mackenzie, J.D.

    1994-12-31

    The sol-gel process can be used to produce porous inorganic matrices that are doped with organic molecules. These doped gels can be used as a quantitative method for the spectrophotometric determination of trace concentrations of metallic ions. For the detection of hexavalent chromium, malachite green was used as the dopant. Preliminary results indicate concentrations on the order of 5 ppb are detectable using this method.

  18. Synthetic implant surfaces. 1. The formation and characterization of sol-gel titania films.

    PubMed

    Haddow, D B; Kothari, S; James, P F; Short, R D; Hatton, P V; van Noort, R

    1996-03-01

    Sol-gel has been used to prepare thin titania films. We have investigated the effects of dip rate, sintering temperature and time on the chemical composition of the films, their physical structure and thickness, and adherence to a silica substrate. Our aim has been to produce films that mimic as closely as possible the natural oxide layer that is found on titanium. These films are to be used as substrates in an in vitro model of osseointegration.

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

    NASA Technical Reports Server (NTRS)

    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.

  20. Novel Sol-Gel Deposition for Repair of Conducting Paths in Polyceramic Systems

    DTIC Science & Technology

    1994-02-24

    and spectroelectroanalytical techniques. Based on elemental analysis results, the doping level of chemically synthesized polyaniline and poly...at 60C until the gel was formed. The resulting sol-gel composites ( polyaniline /poly(MMA-MSNA)-S0 2 ) were doped with HC1 aqueous solution to convert...MSMA (10%) was found to be soluble in m-cresol. Doped polyaniline or blends of emeraldine base and camphorsulfonic acid were dissolved in m-cresol and

  1. Minimally Adhesive, Advanced Non-toxic Coatings of Dendrimeric Catalysts in Sol-Gel Matrices

    DTIC Science & Technology

    2015-10-19

    Catalysts in Sol-Gel Matrices 5a. CONTRACT NUMBER 5b. GRANT NUMBER N00014-09-1-0217 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Detty, Michael R. 5d...SUPPLEMENTARY NOTES 14. ABSTRACT We have developed new xerogel coatings with organochalcogenide or metal oxide catalysts for the activation of...hydrogen peroxide as anti-fouling, fouling-release surfaces. The catalysts perform more efficiently when covalently attached to the xerogel framework

  2. Sensor layers and waveguide layers produced in sol-gel technology

    NASA Astrophysics Data System (ADS)

    Karasinski, Pawel; Zielonka, Iwona

    2003-04-01

    The paper presents the results of investigation studies on the application of sol-gel technology for the production of sensor layers and waveguide layers for the system of planar waveguide sensors. The sensor layers are made up by silica SiO2, which is playing the role of a matrix fixing bromocresol purpole. These layers are sensitive to ammonia. The waveguide layers are produced in a two-component system SiO2:TiO2.

  3. Secondary Crystal Growth on a Cracked Hydrotalcite-Based Film Synthesized by the Sol-Gel Method.

    PubMed

    Lee, Wooyoung; Lee, Chan Hyun; Lee, Ki Bong

    2016-05-02

    The sol-gel synthesis method is an attractive technology for the fabrication of ceramic films due to its preparation simplicity and ease of varying the metal composition. However, this technique presents some limitations in relation to the film thickness. Notably, when the film thickness exceeds the critical limit, large tensile stresses occur, resulting in a cracked morphology. In this study, a secondary crystal growth method was introduced as a post-treatment process for Mg/Al hydrotalcite-based films synthesized by the sol-gel method, which typically present a cracked morphology. The cracked hydrotalcite-based film was hydrothermally treated for the secondary growth of hydrotalcite crystals. In the resulting film, hydrotalcite grew with a vertical orientation, and the gaps formed during the sol-gel synthesis were filled with hydrotalcite after the crystal growth. The secondary crystal growth method provides a new solution for cracked ceramic films synthesized by the sol-gel method.

  4. Photoresist-Free Fully Self-Patterned Transparent Amorphous Oxide Thin-Film Transistors Obtained by Sol-Gel Process

    NASA Astrophysics Data System (ADS)

    Lim, Hyun Soo; Rim, You Seung; Kim, Hyun Jae

    2014-04-01

    We demonstrated self-patterned solution-processed amorphous oxide semiconductor thin-film transistors (TFTs) using photosensitive sol-gels. The photosensitive sol-gels were synthesized by adding β-diketone compounds, i.e., benzoylacetone and acetylacetone, to sol-gels. The chemically modified photosensitive sol-gels showed a high optical absorption at specific wavelengths due to the formation of metal chelate bonds. Photoreactions of the modified solutions enabled a photoresist-free process. Moreover, Zn-Sn-O with a high Sn ratio, which is hard to wet-etch using conventional photolithography due to its chemical durability, was easily patterned via the self-patterning process. Finally, we fabricated a solution-processed oxide TFT that included fully self-patterned electrodes and an active layer.

  5. Thermodynamic analysis of sol-gel transition of gelatin in terms of water activity in various solutions.

    PubMed

    Miyawaki, Osato; Omote, Chiaki; Matsuhira, Keiko

    2015-12-01

    Sol-gel transition of gelatin was analyzed as a multisite stoichiometric reaction of a gelatin molecule with water and solute molecules. The equilibrium sol-gel transition temperature, Tt , was estimated from the average of gelation and melting temperature measured by differential scanning calorimetry. From Tt and the melting enthalpy, ΔHsol , the equilibrium sol-to-gel ratio was estimated by the van't Hoff equation. The reciprocal form of the Wyman-Tanford equation, which describes the sol-to-gel ratio as a function of water activity, was successfully applied to obtain a good linear relationship. From this analysis, the role of water activity on the sol-gel transition of gelatin was clearly explained and the contributions of hydration and solute binding to gelatin molecules were separately discussed in sol-gel transition. The general solution for the free energy for gel-stabilization in various solutions was obtained as a simple function of solute concentration.

  6. Research of materials for porous matrices in sol-gel systems based on silicon dioxide and metallic oxides

    NASA Astrophysics Data System (ADS)

    Maraeva, E. V.; Bobkov, A. A.; Maximov, A. I.; Moshnikov, V. A.; Nalimova, S. S.

    2015-11-01

    In this study silicon dioxide - stannic oxide and silicon dioxide - zinc nanomaterials oxide were obtained through sol-gel technology. The results of nitrogen thermal desorption measurements, atomic force microscopy measurements and particle sizes measurements are discussed.

  7. Silica sol-gel matrix doped with Photolon molecules for sensing and medical therapy purposes.

    PubMed

    Podbielska, Halina; Ulatowska-Jarza, Agnieszka; Müller, Gerhard; Holowacz, Iwona; Bauer, Joanna; Bindig, Uwe

    2007-11-01

    Photolon is one of the new photosensitisers that has found application in photodynamic therapy (PDT). Its chemical structure has a partially reduced porphyrin moiety and its molecular structure is comparable to chlorin e(6), which can be isolated after hydrolysis of the 5-membered exocyclic beta-ketoester moiety of pheophorbide a. For this study, a Photolon doped sol-gel matrix was produced in the form of coatings deposited on silica fibers cores. The material was produced from sols prepared from the silicate precursor TEOS mixed with ethyl alcohol. The sol-gel films were prepared with factor R=20, where R denotes the solvent-to-precursor molar ratio. Hydrochloric acid was added as a catalyst in the correct proportion to ensure acid hydrolysis (pH approximately 2). The mixture was stirred at room temperature for 4h using a magnetic stirrer (speed 400 rpm). The coated fibers were examined in different environments, liquid and gaseous, at different pH values and with various zinc cation concentrations. The chemical reactions were studied by means of spectroscopic methods, whereby the fluorescence response was studied. It was demonstrated that Photolon immobilized in a sol-gel matrix is accessible for the environment and shows visible response to the external changes. Furthermore, it was observed that these reactions are reversible. These biomaterials are also examined as carriers for PDT. It was also proved that a toxic effect is observed an environment with microorganisms, meaning that doped coatings have photodynamic activity.

  8. Disinfection studies on TiO2 thin films prepared by a sol-gel method.

    PubMed

    Kambala, Venkata Subba Rao; Naidu, Ravi

    2009-02-01

    Transparent anatase TiO2 nanometer thin films were prepared by dip-coating on soda-lime glass plates via the sol-gel method. The un-calcined and the calcined films were characterized by X-ray diffraction (XRD), AFM, Nano-indentation (hardness and Young's modulus), UV-vis spectrometry, thickness and hydrophilicity (contact angle measurements). The photocatalytic activity of the thin films was evaluated by performing disinfection studies on the Gram-negative microorganisms like Escherichia coli, and Staphylococcus Aureus, a Gram-positive organism. The photocatalytic activity for both groups of organisms was studied in saline and nutrient broth. The leakage of potassium from the bacteria was observed parallel to cell viability. The activity of the sol-gel prepared TiO2 thin films were compared under UV lamps and natural day light (ND) lamps with Degussa P-25 TiO2 thin films prepared on soda-lime glass using a polymer support and the commercial self-cleaning glass (SC). The sol-gel prepared thin films which were annealed at 450 degrees C, show highest photocatalytic activity, the slowest conversion rate from hydrophilic to a hydrophobic state, light-induced hydrophilicity, and also higher disinfection activities compared to P-25 films and commercial self-cleaning glass. The films also show excellent activities when continuously reused for more than a month.

  9. MOS solar cells with oxides deposited by sol-gel spin-coating techniques

    SciTech Connect

    Huang, Chia-Hong; Chang, Chung-Cheng; Tsai, Jung-Hui

    2013-06-15

    The metal-oxide-semiconductor (MOS) solar cells with sol-gel derived silicon dioxides (SiO{sub 2}) deposited by spin coating are proposed in this study. The sol-gel derived SiO{sub 2} layer is prepared at low temperature of 450 Degree-Sign C. Such processes are simple and low-cost. These techniques are, therefore, useful for largescale and large-amount manufacturing in MOS solar cells. It is observed that the short-circuit current (I{sub sc}) of 2.48 mA, the open-circuit voltage (V{sub os}) of 0.44 V, the fill factor (FF) of 0.46 and the conversion efficiency ({eta}%) of 2.01% were obtained by means of the current-voltage (I-V) measurements under AM 1.5 (100 mW/cm{sup 2}) irradiance at 25 Degree-Sign C in the MOS solar cell with sol-gel derived SiO{sub 2}.

  10. Sol-Gel Material-Enabled Electro-Optic Polymer Modulators.

    PubMed

    Himmelhuber, Roland; Norwood, Robert A; Enami, Yasufumi; Peyghambarian, Nasser

    2015-07-27

    Sol-gels are an important material class, as they provide easy modification of material properties, good processability and are easy to synthesize. In general, an electro-optic (EO) modulator transforms an electrical signal into an optical signal. The incoming electrical signal is most commonly information encoded in a voltage change. This voltage change is then transformed into either a phase change or an intensity change in the light signal. The less voltage needed to drive the modulator and the lower the optical loss, the higher the link gain and, therefore, the better the performance of the modulator. In this review, we will show how sol-gels can be used to enhance the performance of electro-optic modulators by allowing for designs with low optical loss, increased poling efficiency and manipulation of the electric field used for driving the modulator. The optical loss is influenced by the propagation loss in the device, as well as the losses occurring during fiber coupling in and out of the device. In both cases, the use of sol-gel materials can be beneficial due to the wide range of available refractive indices and low optical attenuation. The influence of material properties and synthesis conditions on the device performance will be discussed.

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

    PubMed

    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.

  12. Surface modification of quartz fibres for dental composites through a sol-gel process.

    PubMed

    Wang, Yazi; Wang, Renlin; Habib, Eric; Wang, Ruili; Zhang, Qinghong; Sun, Bin; Zhu, Meifang

    2017-05-01

    In this study, quartz fibres (QFs) surface modification using a sol-gel method was proposed and dental posts reinforced with modified QFs were produced. A silica sol (SS) was prepared using tetraethoxysilane (TEOS) and 3-methacryloxypropyltrimethoxysilane (γ-MPS) as precursors. The amount of γ-MPS in the sol-gel system was varied from 0 to 24wt.% with a constant molar ratio of TEOS, ethanol, deionized water, and HCl. Thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), and contact angle (CA) measurements were used to characterize the modified QFs, which confirmed that SS had successfully coated the surface of QFs. SEM images showed good interfacial bonding between the modified QFs and the resin matrix. The results of three-point bending tests of the fibre reinforced composite (FRC) posts showed that the QFs modified by SS with 12wt.% γ-MPS presented the best mechanical properties, demonstrating improvements of 108.3% and 89.6% for the flexural strength and flexural modulus, respectively, compared with untreated QFs. Furthermore, the sorption and solubility of the prepared dental posts were also studied by immersing the posts in artificial saliva (AS) for 4weeks, and yielded favourable results. This sol-gel surface modification method promises to resolve interfacial bonding issues of fibres with the resin matrix, and produce FRC posts with excellent properties.

  13. Direct test of the critical exponents at the sol-gel transition

    NASA Astrophysics Data System (ADS)

    Kaya, Demet; Pekcan, Önder; Yılmaz, Yaşar

    2004-01-01

    The steady state fluorescence technique was used to study the sol-gel transition for the solution-free radical cross-linking polymerization of acrylamide (AAm), with N,N'-methylenebis (acrylamide) as cross linker in the presence of ammonium persulfate as an initiator. Pyranine (8-hydroxypyrene-1, 3,6-trisulfonic acid, trisodium salt) is used as a fluoroprobe for monitoring the polymerization. Pyranine molecules start to bind to acrylamide polymer chains upon the initiation of the polymerization, thus the spectra of the bonded pyranines shift to the shorter wavelengths. Fluorescence spectra from the bonded pyranines allows one to monitor the sol-gel transition, without disturbing the system mechanically, and to test the universality of the sol-gel transition as a function of some kinetic parameters such as polymer concentration, cross-linker concentration, and temperature. Observations around the critical point show that there are three regimes for AAm concentration in which the exponents differ drastically. The gel fraction exponent β and the weight average degree of polymerization exponent γ agree best with the static percolation results for higher acrylamide concentrations above 1M, but they cross over from percolation to mean-field (Flory-Stockmayer) values when the AAm concentration is lower than 2M. For very low polymer concentrations, below which the system can not form the gel, the exponents differ considerably from both the percolation and the mean-field values.

  14. Use of sol-gel-derived titania coating for direct soft tissue attachment.

    PubMed

    Areva, Sami; Paldan, Hannu; Peltola, Timo; Närhi, Timo; Jokinen, Mika; Lindén, Mika

    2004-08-01

    A firm bond between an implant and the surrounding soft tissue is important for the performance of many medical devices (e.g., stents, canyls, and dental implants). In this study, the performance of nonresorbable and reactive sol-gel-derived nano-porous titania (TiO(2)) coatings in a soft tissue environment was investigated. A direct attachment between the soft tissue and the sol-gel-derived titania coatings was found in vivo after 2 days of implantation, whereas the titanium control implants showed no evidence of soft tissue attachment. The coated implants were in immediate contact with the connective tissue, whereas the titanium controls formed a gap and a fibrous capsule on the implant-tissue interface. The good soft tissue attachment of titania coatings may result from their ability to initiate calcium phosphate nucleation and growth on their surfaces (although the formation of poorly crystalline bonelike apatite does not occur). Thus, the formation of a bonelike CaP layer is not crucial for their integration in soft tissue. The formation of bonelike apatite was hindered by the adsorption of proteins onto the initially formed amorphous calcium phosphate growth centers, thus preventing the dissolution/reprecipitation processes required for the formation of poorly crystalline bonelike apatite. These findings might open novel application areas for sol-gel-derived titania-based coatings.

  15. Thin-film silica sol-gels doped with ion-responsive fluorescent lipid bilayers

    NASA Astrophysics Data System (ADS)

    Sasaki, Darryl Y.; Shea, Lauren E.; Sinclair, Michael B.

    1999-05-01

    A metal ion sensitive, fluorescent lipid-bilayer material (5% PSIDA/DSPC) was successfully immobilized in a silica matrix using a tetramethoxysilane (TMOS) sol-gel procedure. The sol- gel immobilization method was quantitative in the entrapment of self-assembled lipid-bilayers and yielded thin films for facile configuration to optical fiber platforms. The silica matrix was compatible with the solvent sensitive lipid bilayers and provided physical stabilization as well as biological protection. Immobilization in the silica sol-gel produced an added benefit of improving the bilayer's metal ion sensitivity by up to two orders of magnitude. This enhanced performance was attributed to a preconcentrator effect from the anionic surface of the silica matrix. Thin gels (193 micron thickness) were coupled to a bifurcated fiber optic bundle to produce a metal ion sensor probe. Response times of 10 - 15 minutes to 0.1 M CuCl2 were realized with complete regeneration of the sensor using an ethylenediaminetetraacetic acid (EDTA) solution.

  16. Fabrication and characterization of sol-gel based nanoparticles for drug delivery

    NASA Astrophysics Data System (ADS)

    Yadav, Reeta

    Nanogels are cross linked polymeric sol-gel based nanoparticles that offer an interior network for incorporation and protection of biomolecules, exhibiting unique advantages for polymer based delivery systems. We have successfully synthesized stable sol-gel nanoparticles by means of [a] silicification reactions using cationic peptides like polylysine as gelating agents, and [b] lyophilization of sol-gels. Macromolecules such as Hemoglobin and Glucose Oxidase and small molecules such as Sodium Nitroprusside (SNP) and antibiotics were encapsulated within the nanogels. We have used transmission electron microscopy, dynamic light scattering, zeta potential analysis, and spectroscopy to perform a physicochemical characterization of the nanogels resulting from the two approaches. Our studies have indicated that the nanogel encapsulated proteins and small molecules remain intact, stable and functional. A Hydrogen Peroxide (H2O2) and Nitric Oxide (NO) generating drug carrier was synthesized using these nanogels and the effect of generation of H2O2 from Glucose Oxidase encapsulated nanogels and NO from SNP encapsulated nanogels was tested on E.coli. The results show that the nanoparticles exert antimicrobial activity against E.Coli, in addition NO generating nanogels potentiated H2O2 generating nanogels induced killing. These data suggest that these NO and H2O2 releasing nanogels have the potential to serve as a novel class of antimicrobials for the treatment of multidrug resistant bacteria. The unique properties of these protein/drug incorporated nanogels raise the prospect of fine tailoring to specific applications such as drug delivery and bio imaging.

  17. Aqueous sol-gel encapsulation of genetically engineered Moraxella spp. cells for the detection of organophosphates.

    PubMed

    Yu, Diana; Volponi, Joanne; Chhabra, Swapnil; Brinker, C Jeffrey; Mulchandani, Ashok; Singh, Anup K

    2005-01-15

    An all-aqueous sol-gel method for encapsulation of bacterial cells in porous silicate matrices towards the development of a biosensor is described. The sol-gel encapsulation of cells is achieved at room temperature and neutral pH. Furthermore, use of sodium silicate as precursor avoids generation of alcohol that can be detrimental to cells in contrast to the traditional alkoxide sol-gel encapsulation process. Moraxella spp. cells engineered to express recombinant organophosphorus hydrolase (OPH) on the cell surface were encapsulated and OPH enzymatic activity was measured for paraoxon hydrolysis. Kinetic parameters (Km and Vmax) as well as pH behavior of surface-expressed OPH were determined to evaluate the effect of encapsulation. Cells encapsulated by the sodium silicate method displayed higher activity retention compared to those by the traditional alkoxide process. Time-course studies over a 2-month period indicate that immobilization through the sodium silicate process led to a reduction in activity of approximately 5% as compared to approximately 30% activity reduction in case of free cells in buffer indicating that immobilization leads to stabilization, a key parameter in biosensor development.

  18. Conformal sol-gel coatings on three-dimensional nanostructured templates

    NASA Astrophysics Data System (ADS)

    Weatherspoon, Michael R.

    Sol-gel processing techniques, such as spin coating and dip coating, have successfully been utilized over the past several decades to apply conformal coatings on planar substrates; however, controlled film growth on three-dimensional (3-D) nanostructured templates using the sol-gel process remains a significant challenge. Obstacles such as, uncontrolled hydrolyzation and condensation of metal alkoxide precursors on nanostructured surfaces are a few of the obstacles which lead to coatings with undesirable thicknesses and excess inorganic particles. A little over a decade ago, a surface sol-gel process was developed which utilizes stepwise film growth of anhydrous metal alkoxide precursors with hydroxylated surfaces. The surface sol-gel process provides control over the applied coating thickness and is viewed as a wet chemical analog to atomic layer deposition (ALD). The work presented in this dissertation has focused on applying conformal sol-gel derived coatings with controlled thicknesses on 3-D nanostructured templates. The templates utilized in this work were derived from biological species, such as diatoms and butterflies, as well as a synthetic photoresist polymer (SU-8). Coatings were applied on the templates using a conventional reflux/evaporation deposition process and a custom-built computer controlled surface sol-gel pumping system. The coatings applied using the reflux/evaporation process yielded conformal coatings with uncontrolled film thicknesses whereas the coatings applied using the surface sol-gel process yielded conformal coatings with controlled thicknesses. Barium titanate and europium-doped barium titanate coatings were applied on diatom frustules using the reflux/evaporation deposition process. The silica-based diatom frustules had to first be converted into magnesia/silicon composite replicas using a gas/solid displacement reaction to render the template chemically compatible with the barium titanate-based coating. Conformal titanate

  19. Qualification of Target Chamber Vacuum Systems Cleanliness using Sol-Gel Coatings

    SciTech Connect

    Miller, P; Stowers, I F; Ertel, J R

    2006-01-03

    This document defines the procedure necessary to qualify the airborne molecular cleanliness (AMC) of vacuum systems (enclosures or large components) that are placed within the National Ignition Facility (NIF) target chamber or are attached to it and communicate with it during vacuum operation. This test is specific to the NIF target chamber because the allowable time dependent rate of rise in the pore filling of a sol-gel coated SAW sensor is based on some nominal change-out time for the disposable debris shields. These debris shields will be sol-gel coated and thus they represent a means of ''pumping'' AMCs from the target chamber. The debris shield pumping rate sets the allowable change in pore filling with time specified in the test procedure. This document describes a two-part procedure that provides both a static measurement of sol-gel pore filling at the end of a 48-hour test period and a dynamic record of pore-filling measured throughout the test period. Successful qualification of a vacuum system requires that both the static and dynamic measurements meet the criteria set forth in Section 7 of this document.

  20. Thin-film silica sol-gels doped with ion responsive fluorescent lipid bilayers

    SciTech Connect

    Sasaki, D.Y.; Shea, L.E.; Sinclair, M.B.

    1999-01-12

    A metal ion sensitive, fluorescent lipid-b i layer material (5oA PSIDA/DSPC) was successfully immobilized in a silica matrix using a tetramethoxysilane (TMOS) sol-gel procedure. The sol-gel immobilization method was quantitative in the entrapment of seif-assembled Iipid-bilayers and yielded thin films for facile configuration to optical fiber piatforms. The silica matrix was compatible with the solvent sensitive lipid bilayers and provided physical stabilization as well as biological protection. Immobilization in the silica sol-gel produced an added benefit of improving the bilayer's metal ion sensitivity by up to two orders of magnitude. This enhanced performance was attributed to a preconcentrator effect from the anionic surface of the silica matrix. Thin gels (193 micron thickness) were coupled to a bifurcated fiber optic bundle to produce a metal ion sensor probe. Response times of 10 - 15 minutes to 0.1 M CUCIZ were realized with complete regeneration of the sensor using an ethylenediarninetetraacetic acid (EDTA) solution.

  1. Sol-Gel Material-Enabled Electro-Optic Polymer Modulators

    PubMed Central

    Himmelhuber, Roland; Norwood, Robert A.; Enami, Yasufumi; Peyghambarian, Nasser

    2015-01-01

    Sol-gels are an important material class, as they provide easy modification of material properties, good processability and are easy to synthesize. In general, an electro-optic (EO) modulator transforms an electrical signal into an optical signal. The incoming electrical signal is most commonly information encoded in a voltage change. This voltage change is then transformed into either a phase change or an intensity change in the light signal. The less voltage needed to drive the modulator and the lower the optical loss, the higher the link gain and, therefore, the better the performance of the modulator. In this review, we will show how sol-gels can be used to enhance the performance of electro-optic modulators by allowing for designs with low optical loss, increased poling efficiency and manipulation of the electric field used for driving the modulator. The optical loss is influenced by the propagation loss in the device, as well as the losses occurring during fiber coupling in and out of the device. In both cases, the use of sol-gel materials can be beneficial due to the wide range of available refractive indices and low optical attenuation. The influence of material properties and synthesis conditions on the device performance will be discussed. PMID:26225971

  2. Synthesis of polymeric fluorinated sol-gel precursor for fabrication of superhydrophobic coating

    NASA Astrophysics Data System (ADS)

    Li, Qianqian; Yan, Yuheng; Yu, Miao; Song, Botao; Shi, Suqing; Gong, Yongkuan

    2016-03-01

    A fluorinated polymeric sol-gel precursor (PFT) is synthesized by copolymerization of 2,3,4,5,5,5-hexafluoro-2,4-bis(trifluorinated methyl)pentyl methacrylate (FMA) and 3-methacryloxypropyltrimethoxysilane (TSMA) to replace the expensive long chain fluorinated alkylsilanes. The fluorinated silica sol is prepared by introducing PFT as co-precursor of tetraethyl orthosilicate (TEOS) in the sol-gel process with ammonium hydroxide as catalyst, which is then used to fabricate superhydrophobic coating on glass substrate through a simple dip-coating method. The effects of PFT concentrations on the chemical structure of the formed fluorinated silica, the surface chemical composition, surface morphology, wetting and self-cleaning properties of the resultant fluorinated silica coatings were studied by using X-ray powder diffraction (XRD), Fourier transform infrared spectrometer (FTIR), X-ray photoelectron spectrophotometer (XPS), scanning electron microscopy (SEM) and water contact angle measurements (WCA). The results show that the fluorinated silica sols are successfully obtained. The size and size distribution of the fluorinated silica particles are found greatly dependent on the concentration of PFT, which play a crucial role in the surface morphology of the corresponding fluorinated silica coatings. The suitable PFT concentration added in the sol-gel stage, i.e. for F-sol-1 and F-sol-2, is helpful to achieve both the low surface energy and multi-scaled microstructures, leading to the formation of the superhydrophobic coatings with bio-mimicking self-cleaning property similar to lotus leaves.

  3. Preparation and characterisation of a sol-gel process α-Al₂O₃ polycrystalline detector.

    PubMed

    Ferreira, H R; Santos, A

    2015-02-01

    This article presents the dosimetric characteristics of α-Al2O3 detectors prepared through the sol-gel process, disc pressing and sintering in a highly reducing atmosphere. Comparative tests between the sol-gel process α-Al2O3 polycrystalline and anion-defective α-Al2O3:C single-crystal detectors indicate that the ones prepared through this approach present good dosimetric characteristics similar to those found in single-crystal detectors, such as a simple glow curve with the main peak at ∼198 °C (2 °C s(-1)), high sensitivity, a detection threshold of 1.7 µGy, linearity of response, low fading, relatively low photon energy dependence, reusability without annealing and good reproducibility. However, the undesirable feature of heating rate dependence of the thermoluminescence (TL) output in α-Al2O3:C single crystal is practically non-existent in the sol-gel process α-Al2O3 polycrystalline detector. This characteristic renders it useful for the routine processing of large numbers of personal and environmental dosemeters at higher heating rates and also when it comes to the proposal for new approaches to thermal quenching investigation.

  4. Effect of two-step sol-gel reaction on the mesoporous silica structure.

    PubMed

    Choi, Dae-Geun; Yang, Seung-Man

    2003-05-01

    In the present study, we investigated the effects of two-step sol-gel reaction by abrupt pH change on the SBA-15 and mesocellular silica foams (MCF). Mesoporous silica was fabricated by using triblock copolymer templates (poly(ethylene oxide) and poly(propylene oxide)). The prepared silica structure was characterized by X-ray diffraction, transmission electron microscopy, and N(2) sorption experiment. Specifically, we prepared SBA-15 with long-range two-dimensional hexagonal arrangement of 3 to 6-nm feature spacing and MCF with larger pores of a few tens of nanometers. The pore size and ordering were influenced by pH change in a two-step sol-gel reaction and the concentration of organic solvent. Although well-ordered hexagonal arrangement of mesopores was prevalent in acidic conditions, the materials synthesized by a single-step reaction in neutral or basic conditions possessed gel-like structure without mesopores. However, the present two-step reaction (low pH sol-gel reaction followed by high pH reaction) not only produced mesoporous materials but also provided controllability of the pore size. In particular, mesoporous structures with pore sizes as large as those of MCF were successfully fabricated by the two-step reaction without using organic swelling agents. As expected, when xylene was added as a swelling agent, the pore size increased with the xylene/copolymer weight ratio.

  5. Hybrid sol-gel technology for fast prototyping in astronomical interferometry

    NASA Astrophysics Data System (ADS)

    Ghasempour, A.; Leite, A. M. P.; Alexandre, D.; Reynaud, F.; Marques, P. V. S.; Garcia, P. J. V.

    2010-07-01

    Hybrid sol-gel technology was used for fabrication of prototypes of coaxial two, three and four telescopes beam combiners for astronomical applications. These devices were designed for the astronomical J-band and have been characterized using an optical source with emission centered at 1265 nm and with a spectral FWHM of 50 nm. Interferometric characterization of the two, three and four beam combiners, showed average contrasts respectively higher than 98%, 96% and 95%. Interferometric spectral analysis of the beam combiners revealed that the chromatic differential dispersion is the main contributor to the observed contrast decay in the latter cases. The laser direct writing technique was used for fabrication of a coaxial two beam combiner on sol-gel material; it showed a contrast of 95%. The measured high contrast fringes confirm that the procedures used lead to performant IO beam combiners. These results demonstrate the capabilities of the hybrid sol-gel technology for fast prototyping of complex chip designs for astronomical applications.

  6. Nanoscale morphology for high hydrophobicity of a hard sol gel thin film

    NASA Astrophysics Data System (ADS)

    Wu, Y. L.; Chen, Z.; Zeng, X. T.

    2008-08-01

    It is challenging to obtain a hydrophobic smooth coating with high optical and mechanical properties at the same time because the hydrophobic additives are soft in nature resulting in reduced hardness and durability. This paper reports a durable hydrophobic transparent coating on glass fabricated by sol-gel technology and a low volume medium pressure (LVMP) spray process. The sol-gel formula consists of a pre-linked hydrophobic nano-cluster from hydroxyl-terminated polydimethylsiloxane, titanium tetraisopropoxide and a silica-based sol-gel matrix with silica hard fillers. Polydimethylsiloxane (PDMS) is uniformly distributed throughout the coating layer providing durable hydrophobic property. Mechanical properties are achieved by the hard matrix and hard fillers with the nano-structures. Due to the surface nano-morphology, a high degree of hydrophobicity was maintained with only 10 vol.% PDMS, while the hardness and abrasion resistance of the coatings were not significantly compromised. Chemical analyses by FTIR confirmed the uniform distribution of the PDMS and surface morphology analyses by atomic force microscopy (AFM) displayed the nano-surface structures that enhanced the hydrophobicity. The special surface nanostructures can be quantified using surface Kurtosis and ratio between asperity peak height to distance between peaks. The LVMP process influences the spray droplet size resulting in different surface structures.

  7. Increasing the activity and enantioselectivity of lipases by sol-gel immobilization: further advancements of practical interest

    NASA Astrophysics Data System (ADS)

    Tielmann, Patrick; Kierkels, Hans; Zonta, Albin; Ilie, Adriana; Reetz, Manfred T.

    2014-05-01

    The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of the sol-gel approach.The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of

  8. Matrix molecularly imprinted mesoporous sol-gel sorbent for efficient solid-phase extraction of chloramphenicol from milk.

    PubMed

    Samanidou, Victoria; Kehagia, Maria; Kabir, Abuzar; Furton, Kenneth G

    2016-03-31

    Highly selective and efficient chloramphenicol imprinted sol-gel silica based inorganic polymeric sorbent (sol-gel MIP) was synthesized via matrix imprinting approach for the extraction of chloramphenicol in milk. Chloramphenicol was used as the template molecule, 3-aminopropyltriethoxysilane (3-APTES) and triethoxyphenylsilane (TEPS) as the functional precursors, tetramethyl orthosilicate (TMOS) as the cross-linker, isopropanol as the solvent/porogen, and HCl as the sol-gel catalyst. Non-imprinted sol-gel polymer (sol-gel NIP) was synthesized under identical conditions in absence of template molecules for comparison purpose. Both synthesized materials were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and nitrogen adsorption porosimetry, which unambiguously confirmed their significant structural and morphological differences. The synthesized MIP and NIP materials were evaluated as sorbents for molecularly imprinted solid phase extraction (MISPE) of chloramphenicol in milk. The effect of critical extraction parameters (flow rate, elution solvent, sample and eluent volume, selectivity coefficient, retention capacity) was studied in terms of retention and desorption of chloramphenicol. Competition and cross reactivity tests have proved that sol-gel MIP sorbent possesses significantly higher specific retention and enrichment capacity for chloramphenicol compared to its non-imprinted analogue. The maximum imprinting factor (IF) was found as 9.7, whereas the highest adsorption capacity of chloramphenicol by sol-gel MIP was 23 mg/g. The sol-gel MIP was found to be adequately selective towards chloramphenicol to provide the necessary minimum required performance limit (MRPL) of 0.3 μg/kg set forth by European Commission after analysis by LC-MS even without requiring time consuming solvent evaporation and sample reconstitution step, often considered as an integral part in solid phase extraction work-flow. Intra and

  9. Spectroscopic studies of trimetoxypropylsilane and bis(trimethoxysilyl)ethane sol-gel coatings on aluminum and copper

    NASA Astrophysics Data System (ADS)

    Li, Ying-Sing; Tran, Tuan; Xu, Yue; Vecchio, Nicolas E.

    2006-11-01

    Trimethoxypropylsilane (TMPS) and bis(trimethoxysilyl)ethane (BTMSE) were used as surface modifiers of metal vie the sol-gel process and dip coating. In addition to the single coating of Al, Cu and Sn, double treatments of Al were also conducted by combining coatings with these sol-gels in different sequences. Reflection and absorption infrared spectroscopy (RAIR) was employed to characterize and to trace the proceeding of the sol-gel process of the films. It was found that the silanol condensation occurs in the coating films on Al and the covalent linkage exists between the TMPS film and copper surface. From the assigned vibration modes, two conformers were identified in pure TMPS, TMPS sol-gel and coated film. A series of dip coating experiments with different concentrations of TMPS sol-gel was conducted, and the results from the collected RAIR spectra of the coated samples suggested that the coated Cu consistently has a better RAIR spectrum than that of the coated Al. The TMPS sol-gel appeared to have a better affinity to Cu than to Al. The temperature effect and the aging effect in the coating films were studied. X-ray photoelectronic spectroscopy (XPS) was employed to characterize the coated film, and the XPS data confirm the formation of the siloxane film from the silane coupling agents (SCA). Electrochemical impedance spectra (EIS) have been collected for bare Al and Cu, BTMSE sol-gel coated Al, and TMPS sol-gel coated Cu in 0.15 M NaCl solution. The corresponding electronic circuit parameters have been determined to match the experimental EIS data.

  10. Sol-gel preparation and characterization of SiO2 coated VO2 films with enhanced transmittance and high thermochromic performance

    NASA Astrophysics Data System (ADS)

    Li, Dezeng; Shan, Yongkui; Huang, Fuqiang; Ding, Shangjun

    2014-10-01

    Vanadium dioxide (VO2) films prepared at low-temperature with a low cost are considerable for energy-saving applications. Here, SiO2 coated VO2 films with clearly enhanced visible transmittance by introducing antireflection coatings (ARCs) and excellent thermochromic performance were present. The VO2 films have been prepared via a stable and low-cost sol-gel synthesis route using vanadium pentaoxide powder as precursor, and their structural, morphological, optical and electrical properties and thermochromic performance were systemically characterized. The resistance of VO2 films varies by 4 orders of magnitude and the transmittance changes from 11.8% to 69.3% at 2500 nm while no significant deviation appears in the visible region during metal-insulator transition (MIT). Nanoporous SiO2 coating with good optical transparency was coated on the surface of VO2 film via sol-gel dip-coating technique to enhance its optical transmittance, and the visible transmittance is increased by 14.6% due to the significantly decreased reflectance. The critical transition temperature (63 °C) and infrared switching properties of VO2 films are not much deteriorated by applying SiO2 layer. The synergistic effect of antireflection and thermochromism on SiO2 coated VO2 films was investigated.

  11. Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

    PubMed

    Catauro, M; Papale, F; Bollino, F

    2016-01-01

    The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0sol-gel route starting from tetraethyl orthosilicate and calcium nitrate tetrahydrate. Those materials, still in the sol phase, have been used to coat titanium substrates by means of the dip-coating technique. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) allowed the materials to be characterized and a microstructural analysis of the coatings obtained was performed using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated titanium 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. To investigate cell-material interactions, mouse embryonic fibroblast cells (3T3) were seeded onto the specimens and the cell viability was evaluated by a WST-8 assay.

  12. Sol-gel synthesis and characterization of SiO2/PCL hybrid materials containing quercetin as new materials for antioxidant implants.

    PubMed

    Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando; Piccolella, Simona; Pacifico, Severina

    2016-01-01

    The development of biomaterials with intrinsic antioxidant properties could represent a valuable strategy for preventing peri-implant disease onset. In this context quercetin, a naturally occurring flavonoid, has been entrapped, at different weight percentages in a silica/poly(ε-caprolactone)-based hybrid material by a sol-gel route. FT-IR and UV spectroscopic techniques were employed in order to characterize the hybrids. FT-IR analysis indicated changes in stretching frequencies of the quercetin dienonic moiety, suggesting that a flavonol oxidized derivative was formed during the sol-gel process. The establishment of hydrogen-bonded interactions between quercetin and silica and polymer matrices,was strongly affected by the amount of polymer. Poly(ε-caprolactone) did not interact with quercetin when it was loaded at high doses (50 wt.%). The morphology of the synthesized materials was observed by using SEM. The obtained images proved that the materials are hybrid nanocomposites. Their bioactivity was shown by the formation of a hydroxyapatite layer on samples' surface soaked in a fluid simulating the composition of the human plasma. The antiradical properties of the investigated systems were evaluated by DPPH and ABTS methods and their cytotoxicity by the MTT assay. Data obtained revealed that the synthesized materials are biocompatible and that the hybrid system,with 6 wt.% of PCL and 15 wt.% of quercetin, produced the strongest antiradical efficacy.

  13. Raman investigation of germanium- and phosphorus-doping effects on the structure of sol-gel silica-based optical fiber preforms

    NASA Astrophysics Data System (ADS)

    El Hamzaoui, Hicham; Bouazaoui, Mohamed; Capoen, Bruno

    2015-11-01

    This works reports the structural investigation of homogeneously doped sol-gel-derived silica optical fiber preforms. Crack-free germanosilicate (2.7 wt% Ge) and phosphosilicate (2.5 wt% P) glasses, suitable for optical fiber fabrication, have been prepared using the polymeric sol-gel route combined with the sol-doping technique. Space homogeneity of the doping oxide (GeO2 or P2O5) in the cylindrical preforms has been checked by chemical analysis. The structure of these glasses have been studied using Raman spectroscopy and compared to pure silica glasses. It is shown that phosphorus has a much more sensitive effect on the glassy structure than germanium, both at small and medium scales. Indeed, in the low-wavenumber region (7-100 cm-1), the phosphorus-doping was found to affect the intensity of the boson peak, suggesting an enhancement of heterogeneity at the nanometer scale. At a shorter scale, both germanium- and phosphorus-doping were found to reduce the number of three- and four-membered rings in the silica glass network.

  14. Stability High Salt Content Waste Using Sol Gel Process. Mixed Waste Focus Area. OST Reference Number 0236

    SciTech Connect

    None, None

    1999-09-01

    Mixed waste sludges, soils, and homogeneous solids containing high levels of salt ( ~ greater than 15% by weight ) have proven to be difficult to stabilize due to the soluble nature of the salts. The current stabilization technique for high salt waste, grouting with Portland cement, is limited to low waste loadings. The presence of salts interfere with the hydration and curing of the cement, cause waste form deteriorating mineral expansions, or result in an undesirable separate phase altogether. Improved technologies for the stabilization of salt waste must be able to accommodate higher salt loadings, while maintaining structural integrity, chemical durability, and leach resistance. In a joint collaboration supported by the Department of Energy’s (DOE’s) Mixed Waste Focus Area (MWFA), the Pacific Northwest National Laboratory (PNNL) and the Arizona Materials Laboratory (AML) at the University of Arizona have developed a sol-gel (wet-chemical) based, low-temperature-processing route for the stabilization of salt-containing mixed wastes. By blending and reacting liquid precursors at room temperature with salt waste, strong, impermeable “polyceram” matrices have been formed that encapsulate the environmentally hazardous waste components. As depicted by Figure 1, polycerams are hybrid organic/inorganic materials with unique properties derived from the chemical combination of polymer (organic) and ceramic (inorganic) components. For this application, the stabilizing polyceram matrices contain polybutadiene-based polymer components and silicon dioxide (SiO2) as the inorganic component. Polybutadiene (PBD) is a strong, tough, waterresistant plastic and its use in the polyceram promotes these same characteristics in the waste form. The PBD polymer component is modified to increase its reactivity with the SiO2 precursor during sol-gel processing. When combined, the polymer and SiO2 precursors react, gel, solidify, and encapsulate the

  15. Optical and transport properties of Sn-doped ZnMn2O4 prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Gherbi, R.; Bessekhouad, Y.; Trari, M.

    2016-02-01

    The paper describes the effect of ZnMn2O4 doping with different Sn ratios. Snx-ZnMn2O4 is prepared with Sol-Gel route at 700 °C. The structural, optical and electrical properties were studied. The X-ray diffraction patterns indicate the formation of pure tetragonal phase for the ratios lower than 0.03%, while for other compositions, the secondary phases were observed. The attenuated total reflectance (ATR) analysis confirmed the localization of Sn in octahedral sites. The optical properties showed not only the increase of Eg, but also the improvement of the optical characteristics such as extinction coefficient (k), optical conductivity (σopt), dissipation factor (tan δ) and the relaxation time (τ). The latter has been improved by 50%. The Hall measurements confirmed the transition of the conductivity mode, i.e, from p to n-type. The formation of SnMn1+ point defects is evidenced; however, the transport properties indicate that the charge carriers are mainly localized.

  16. Preparation of surface-modified ZnO quantum dots through an ultrasound assisted sol-gel process

    NASA Astrophysics Data System (ADS)

    Moghaddam, E.; Youzbashi, AA; Kazemzadeh, A.; Eshraghi, MJ

    2015-08-01

    A synthetic process of zinc oxide quantum dots (QDs) is presented. It is based on a sol-gel process, carried out in an ultrasonic bath. It allows the formation of the stable colloids, containing surface-modified ZnO QDs with the aid of 3-aminopropyltriethoxysilane (APTES) as a capping agent. For this purpose, alcoholic solutions of zinc acetate dihydrate and potassium hydroxide were used as the reactants. Effect of KOH concentration, ultrasonic irradiation, and also the presence of capping agent on the characteristics of the final product were investigated. The synthesized samples were characterized by various analytical techniques such as XRD, TEM, FT-IR, UV-vis and PL spectroscopy. XRD analysis revealed the direct formation of hexagonal wurtzite nanocrystals with average size of ∼3 nm confirmed by TEM and UV-vis spectroscopy. The PL spectroscopy indicated the influence of the capping agent on reducing the defects formation during the growth of the QDs. The present synthesis method was found to be a cost-effective and simple solution route for producing pure semiconductor ZnO QDs, exhibiting the quantum confinement effects, suitable for optical and optoelectronic applications.

  17. Magnetic properties of hard-soft SrFe10Al2O19/Co0.8Ni0.2Fe2O4 ferrite synthesized by one-pot sol-gel auto-combustion

    NASA Astrophysics Data System (ADS)

    Torkian, Shahab; Ghasemi, Ali; Razavi, Reza Shoja

    2016-10-01

    SrFe10Al2O19/Co0.8Ni0.2Fe2O4 hard/soft nanocomposite ferrites with different content of soft phase have been prepared by simple one-pot sol-gel auto-combustion route. X-ray diffraction (XRD), field emission scanning electron microscopy and vibrating ample magnetometer were employed to analysis of structural and magnetic features of synthesized samples. XRD patterns reflect the formation of hard/soft composites of ferrites without the existence of any kind of secondary phases. Narrow size distributions of particles were formed by sol-gel method. Single smooth hysteresis loops of nanocomposites show the presence of exchange coupling between hard and soft phases. Nanocomposite with 15 wt% of soft phase reaches the highest Mr/Ms ratio of 0.63. Compared to the physical mixing of hard/ soft nanocomposites, the one-pot sol-gel auto-combustion method could be considered as a suitable method for synthesizing exchange coupled magnet.

  18. A new sol-gel synthesis of 45S5 bioactive glass using an organic acid as catalyst.

    PubMed

    Faure, J; Drevet, R; Lemelle, A; Ben Jaber, N; Tara, A; El Btaouri, H; Benhayoune, H

    2015-02-01

    In this paper a new sol-gel approach was explored for the synthesis of the 45S5 bioactive glass. We demonstrate that citric acid can be used instead of the usual nitric acid to catalyze the sol-gel reactions. The substitution of nitric acid by citric acid allows to reduce strongly the concentration of the acid solution necessary to catalyze the hydrolysis of silicon and phosphorus alkoxides. Two sol-gel powders with chemical compositions very close to that of the 45S5 were obtained by using either a 2M nitric acid solution or either a 5mM citric acid solution. These powders were characterized and compared to the commercial Bioglass®. The surface properties of the two bioglass powders were assessed by scanning electron microscopy (SEM) and by Brunauer-Emmett-Teller method (BET). The Fourier transformed infrared spectroscopy (FTIR) and the X-ray diffraction (XRD) revealed a partial crystallization associated to the formation of crystalline phases on the two sol-gel powders. The in vitro bioactivity was then studied at the key times during the first hours of immersion into acellular Simulated Body Fluid (SBF). After 4h immersion into SBF we clearly demonstrate that the bioactivity level of the two sol-gel powders is similar and much higher than that of the commercial Bioglass®. This bioactivity improvement is associated to the increase of the porosity and the specific surface area of the powders synthesized by the sol-gel process. Moreover, the nitric acid is efficiently substituted by the citric acid to catalyze the sol-gel reactions without alteration of the bioactivity of the 45S5 bioactive glass.

  19. Synthesis of nano-bound microsphere Co3O4 by simple polymer-assisted sol-gel technique

    NASA Astrophysics Data System (ADS)

    Karthick, S. N.; Hemalatha, K. V.; Justin Raj, C.; Kim, Hee Je; Yi, Moonsuk

    2013-03-01

    Nano-bound Co3O4 microspheres and molten Co3O4 microspheres were synthesized for the first time by a simple polymer (poly-(vinylpyrrolidone))-assisted sol-gel and sol-gel technique, respectively. Thermal decomposition of the precursor samples of both polymer-assisted sol-gel and sol-gel technique were studied by thermogravimetric analysis. In both techniques, the material was calcined at different temperatures for the formation of phase pure Co3O4. X-ray diffraction confirmed the formation of phase pure cubic spinel structured Co3O4 at 400 and 500 °C for the polymer-assisted sol-gel and sol-gel technique, respectively. Fourier transform infrared spectroscopy revealed the vibrational assignments of functional groups associated with the cubic spinel structure of Co3O4. Scanning electron microscopy of all samples showed clear microsphere sizes ranging from 1 to 4 μm. Both techniques allowed the formation of spherical-shaped microspheres by a simple process. Nano-bound microspheres were observed from the polymer-assisted sol-gel technique because the decomposition of PVP at 400 °C is the main reason for the formation of nano-bound microspheres. The nanoparticle size of the nano-bound microsphere measured by transmission electron microscopy was 40 nm. Therefore, PVP is an essential compound for the formation of nano-bound microspheres. This very simple and inexpensive technique is suitable for the formation of spherical-shaped microspheres.

  20. Evaluation of hybrid sol-gel incorporated with nanoparticles as nano paint

    NASA Astrophysics Data System (ADS)

    Jameel, Zainab N.; Haider, Adawiya J.; Taha, Samar Y.; Gangopadhyay, Shubhra; Bok, Sangho

    2016-07-01

    A coating with self-cleaning characteristics has been developed using a TiO2/SiO2 hybrid sol-gel, TiO2 nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO2 nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO2 nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO2 phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO2 NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

  1. Evolution of microstructure in mixed niobia-hybrid silica thin films from sol-gel precursors.

    PubMed

    Besselink, Rogier; Stawski, Tomasz M; Castricum, Hessel L; ten Elshof, Johan E

    2013-08-15

    The evolution of structure in sol-gel derived mixed bridged silsesquioxane-niobium alkoxide sols and drying thin films was monitored in situ by small-angle X-ray scattering. Since sol-gel condensation of metal alkoxides proceeds much faster than that of silicon alkoxides, the incorporation of d-block metal dopants into silica typically leads to formation of densely packed nano-sized metal oxide clusters that we refer as metal oxide building blocks in a silica-based matrix. SAXS was used to study the process of niobia building block formation while drying the sol as a thin film at 40-80°C. The SAXS curves of mixed niobia-hybrid silica sols were dominated by the electron density contrast between sol particles and surrounding solvent. As the solvent evaporated and the sol particles approached each other, a correlation peak emerged. Since TEM microscopy revealed the absence of mesopores, the correlation peak was caused by a heterogeneous system of electron-rich regions and electron poor regions. The regions were assigned to small clusters that are rich in niobium and which are dispersed in a matrix that mainly consisted of hybrid silica. The correlation peak was associated with the typical distances between the electron dense clusters and corresponded with distances in real space of 1-3 nm. A relationship between the prehydrolysis time of the silica precursor and the size of the niobia building blocks was observed. When 1,2-bis(triethoxysilyl)ethane was first hydrolyzed for 30 min before adding niobium penta-ethoxide, the niobia building blocks reached a radius of 0.4 nm. Simultaneous hydrolysis of the two precursors resulted in somewhat larger average building block radii of 0.5-0.6 nm. This study shows that acid-catalyzed sol-gel polymerization of mixed hybrid silica niobium alkoxides can be rationalized and optimized by monitoring the structural evolution using time-resolved SAXS.

  2. Structural and optoelectronic characterization of TiO2 films prepared using the sol gel technique

    NASA Astrophysics Data System (ADS)

    Jiménez González, A. E.; Gelover Santiago, S.

    2007-07-01

    TiO2 is a versatile material that makes for fascinating study in any of its several physical forms: monocrystal, polycrystal, powder or thin film. Its enhanced photosensitivity to UV radiation and excellent chemical stability in acidic and aqueous media point to its excellent potential for use in a variety of applications, such as solar cells, electronic devices, chemical sensors and photocatalysts. Of late, thin films of TiO2 have permitted the study of physical and chemical properties that are almost impossible to examine in powders. Using the sol-gel technique, it was possible to prepare TiO2 films, and to specifically modify their characteristic properties by means of annealing treatments. Optical measurements carried out on sol-gel derived films produced results similar to those found in films prepared using the sputtering technique. The use of TiO2 films facilitates the study of the behaviour of crystalline structure, grain size, photoresponse, electrical conductivity in both darkness and light and energy band gap (Eg) as a function of treatment temperature. For the first time, it has been demonstrated that the photoconductivity of TiO2 becomes apparent at a treatment temperature of 350 °C, which means that below this temperature the material is not photosensitive. The photosensitivity (S) of TiO2 films prepared by the sol-gel technique reaches values between 100 and 104, surpassing by more than two orders of magnitude the photosensitivity of TiO2 in powder form. In addition, it was possible to study the surface crystalline structure, where TEM studies clearly revealed both the polycrystalline order and the atomic arrangements of the TiO2 films. Our findings will afford us an opportunity to better study the nature of TiO2 and to enhance its performance with respect to the above-mentioned applications.

  3. Synthesis and characterization of sol gel silica films doped with size-selected gold nanoparticles

    NASA Astrophysics Data System (ADS)

    Ferrara, M. C.; Mirenghi, L.; Mevoli, A.; Tapfer, L.

    2008-09-01

    Homogeneous nanocomposite silica films uniformly doped with size-selected gold nanoparticles (AuNPs) have been prepared by a combined use of colloidal chemistry and the sol-gel process. For this purpose, stable thiol-functionalized AuNPs (DDT-AuNPs) were first synthesized by a two-phase aqueous/organic system and, subsequently, dispersed in an acid-catalysed sol-gel silica solution. The microstructural morphology of the samples was investigated by x-ray diffraction and field emission scanning electron microscopy. X-ray photoelectron spectroscopy (XPS) and UV-vis optical spectrophotometry were instead employed to investigate the elemental chemical behaviour and the evolution of the surface plasmon resonance (SPR) band of the AuNPs from their synthesis up to the formation of the Au-doped silica films. The results show that the size, shape and crystalline domains of the AuNPs remain unchanged during the entire preparation process, indicating that their aggregation or decomposition was prevented. XPS results show that the DDT-AuNPs lose the capping shells and oxidize themselves when dispersed in acid-catalysed sol-gel solutions, and that bare AuNPs are embedded in the SiO2 films. A large broadening of the SPR band, observed for systems with DDT-AuNPs, suggests the presence of interface effects which cause a surface electron density lowering. Thiol chain detachment from the AuNPs determines an increase of the SPR peak intensity while the oxidation of the Au surfaces causes a red shift of its position. The latter is no longer observed in doped films, suggesting that no interfacial effects between bare AuNPs and the host medium are present.

  4. Electrophoretically active sol-gel processes to backfill, seal, and/or densify porous, flawed, and/or cracked coatings on electrically conductive material

    DOEpatents

    Panitz, Janda K.; Reed, Scott T.; Ashley, Carol S.; Neiser, Richard A.; Moffatt, William C.

    1999-01-01

    Electrophoretically active sol-gel processes to fill, seal, and/or density porous, flawed, and/or cracked coatings on electrically conductive substrates. Such coatings may be dielectrics, ceramics, or semiconductors and, by the present invention, may have deposited onto and into them sol-gel ceramic precursor compounds which are subsequently converted to sol-gel ceramics to yield composite materials with various tailored properties.

  5. Electrophoretically active sol-gel processes to backfill, seal, and/or densify porous, flawed, and/or cracked coatings on electrically conductive material

    DOEpatents

    Panitz, J.K.; Reed, S.T.; Ashley, C.S.; Neiser, R.A.; Moffatt, W.C.

    1999-07-20

    Electrophoretically active sol-gel processes to fill, seal, and/or density porous, flawed, and/or cracked coatings on electrically conductive substrates. Such coatings may be dielectrics, ceramics, or semiconductors and, by the present invention, may have deposited onto and into them sol-gel ceramic precursor compounds which are subsequently converted to sol-gel ceramics to yield composite materials with various tailored properties. 6 figs.

  6. YAG:Ce3+ Nanophosphor Synthesized with the Salted Sol-Gel Method

    SciTech Connect

    D. Jia; C. V. Shaffer; J. E. Weyant; A. Goonewardene; X. Guo; Y. Wang; X. Z. Guo; K. K. Li; Y. K. Zou; W. Jia

    2006-05-01

    Nano-phosphors of Y3Al5O12:Ce3+ (YAG:Ce) were synthesized with a novel salted sol-gel method, in which aqueous solution of inorganic salts (yttrium/cerium nitrates) were used along with the metal alkoxide precursor, aluminum sec-butoxide, Al(OC4H9)3. YAG single phase was formed at temperature as low as 800 C. Luminescence of YAG:Ce reached the maximum intensity when calcined above 1350C. The SEM image reveals that the grain sizes of the nano-phosphors calcined at 1100 C are in a range of 50-150 nm.

  7. Switching of lasing wavelength in a sol-gel laser with dynamic distributed feedback

    SciTech Connect

    Balenko, V G; Trufanov, A N; Umanskii, B A; Dolotov, S M; Petukhov, V A

    2011-09-30

    A scheme of switching the lasing wavelength of active centres in a sol-gel matrix excited by external laser radiation is proposed. A distributed feedback is formed during pumping by using a right-angle prism due to the interference of the direct and reflected pump beams. The lasing wavelength is determined by the period of the interference pattern, which depends on the convergence angle of interfering beams. Control is performed by a liquid-crystal cell, which changes the pump radiation polarisation, and a birefringent prism. As a result, the convergence angle of interfering beams changes, leading to a change in the interference pattern period and the excited radiation wavelength.

  8. Luminescence properties of Lu2O3: Tb film prepared by Pechini sol-gel method

    NASA Astrophysics Data System (ADS)

    Shen, Siqing; Wang, Jian; Xu, Zhibin; Xie, Jianjun; Shi, Ying

    2011-02-01

    Uniform and crack free Tb3+ doped lutetium oxide (Lu2O3:Tb) films were prepared by Pechini sol-gel method combined with the spin-coating technique. The influence of the different substrate (monocrystalline silicon (111) and silica glass) and atmosphere (N2 and Air) on the luminescence properties of films was investigated. According to the emission spectra, we found that the luminous intensity was higher on silica glass substrate. Moreover, it was found that the luminous intensity calcined in N2 was higher almost twice as that calcined in air.

  9. Luminescence properties of Lu2O3: Tb film prepared by Pechini sol-gel method

    NASA Astrophysics Data System (ADS)

    Shen, Siqing; Wang, Jian; Xu, Zhibin; Xie, Jianjun; Shi, Ying

    2010-10-01

    Uniform and crack free Tb3+ doped lutetium oxide (Lu2O3:Tb) films were prepared by Pechini sol-gel method combined with the spin-coating technique. The influence of the different substrate (monocrystalline silicon (111) and silica glass) and atmosphere (N2 and Air) on the luminescence properties of films was investigated. According to the emission spectra, we found that the luminous intensity was higher on silica glass substrate. Moreover, it was found that the luminous intensity calcined in N2 was higher almost twice as that calcined in air.

  10. Synthesis and luminescence properties of encapsulated sol-gel glass samarium complexes.

    PubMed

    Zaitoun, M A; Momani, K; Jaradat, Q; Qurashi, I M

    2013-11-01

    Luminescence efficiency of lanthanide complexes generally largely depend on the choice of the organic ligand and the host matrix in which these complexes are doped. Two Sm(III) complexes, namely: Sm(III) dithicarbamate - Sm(L1)3B [L1=(R)2NCS2B, R=C2H5 and B=1,10-phenanthroline] and Sm(III) complex with the polytonic ligand L2=N', N'(2)-bis[(1E)-1-(2-pyridyl)ethylidene]ethanedihydrazide {Sm2-L2-(CH3COO)2; L2=C16H16N6O2} are synthesized, these complexes are then trapped in sol-gel glass. Room temperature luminescence of Sm(L1)3B and {Sm2-L2-(CH3COO)2} complexes encapsulated in sol-gel glass are studied using a spectrofluorometer. Up on excitation by a UV light, ligand L1B absorbs this light and transfers it into the Sm(III) ions and emission bands were observed in the visible region and were attributed to f-f transitions of Sm(III). The observed emission indicated an efficient L1B ligand as a sensitizer, while ligand L2 shows no ability to work as a sensitizer. The branching ratio I4G5/2→6H9/2/I4G5/2→6H7/2) of electric dipole transition to magnetic dipole transition was used as an effective spectroscopic probe to predict symmetry of the site in which Sm(III) is located. The encapsulation of the Samaium complexes was performed for three reasons: (i) before rare earth (RE)-doped sol-gel glasses can be used in applications such as laser materials, several fluorescence quenching mechanisms must be overcome, we show in this work that lanthanide fluorescence is greatly enhanced by chelation and selecting a suitable host matrix (sol-gel) to accommodate the lanthanide complex, (ii) to improve the stability of the phosphor with efficient and high color-purity characteristics under ultraviolet excitation and (iii) this work provides a framework for preparing transparent composite glasses that are robust hosts to study the fundamental interactions between nano-materials and light.

  11. Effect of preparation conditions in sol-gel method on yellow phosphor with wide spectrum

    NASA Astrophysics Data System (ADS)

    Lin, Yenchen; Inoue, Shuhei; Matsumura, Yukihiko; Chen, Jyh-Chen

    2017-01-01

    Among several methods to obtain white light in light emitting diodes (LEDs), mixing blue light with yellow light excited by blue light is the most effective and economical method. However, the quality of white light achieved by this method is poor, making it essential to develop high-quality yellow phosphors. In this study, we synthesized yellow phosphors with broad spectral width by the sol-gel method and studied the effect of various synthetic conditions on their photoluminescence spectra. Consequently, we optimized synthesis conditions for a series of yellow phosphors and found that excess europium doping caused quenching and reduced the quantum yield.

  12. Synthesis and luminescence properties of encapsulated sol-gel glass samarium complexes

    NASA Astrophysics Data System (ADS)

    Zaitoun, M. A.; Momani, K.; Jaradat, Q.; Qurashi, I. M.

    2013-11-01

    Luminescence efficiency of lanthanide complexes generally largely depend on the choice of the organic ligand and the host matrix in which these complexes are doped. Two Sm(III) complexes, namely: Sm(III) dithicarbamate - Sm(L1)3B [L1 = (R)2NCS2B, R = C2H5 and B = 1,10-phenanthroline] and Sm(III) complex with the polytonic ligand L2 = N‧, N‧2-bis[(1E)-1-(2-pyridyl)ethylidene]ethanedihydrazide {Sm2-L2-(CH3COO)2; L2 = C16H16N6O2} are synthesized, these complexes are then trapped in sol-gel glass. Room temperature luminescence of Sm(L1)3B and {Sm2-L2-(CH3COO)2} complexes encapsulated in sol-gel glass are studied using a spectrofluorometer. Up on excitation by a UV light, ligand L1B absorbs this light and transfers it into the Sm(III) ions and emission bands were observed in the visible region and were attributed to f-f transitions of Sm(III). The observed emission indicated an efficient L1B ligand as a sensitizer, while ligand L2 shows no ability to work as a sensitizer. The branching ratio I4G5/2→6H9/2/I4G5/2→6H7/2) of electric dipole transition to magnetic dipole transition was used as an effective spectroscopic probe to predict symmetry of the site in which Sm(III) is located. The encapsulation of the Samaium complexes was performed for three reasons: (i) before rare earth (RE)-doped sol-gel glasses can be used in applications such as laser materials, several fluorescence quenching mechanisms must be overcome, we show in this work that lanthanide fluorescence is greatly enhanced by chelation and selecting a suitable host matrix (sol-gel) to accommodate the lanthanide complex, (ii) to improve the stability of the phosphor with efficient and high color-purity characteristics under ultraviolet excitation and (iii) this work provides a framework for preparing transparent composite glasses that are robust hosts to study the fundamental interactions between nano-materials and light.

  13. Rheology of gastric mucin exhibits a pH-dependent sol-gel transition.

    PubMed

    Celli, Jonathan P; Turner, Bradley S; Afdhal, Nezam H; Ewoldt, Randy H; McKinley, Gareth H; Bansil, Rama; Erramilli, Shyamsunder

    2007-05-01

    Gastric mucin, a high molecular weight glycoprotein, is responsible for providing the gel-forming properties and protective function of the gastric mucus layer. Bulk rheology measurements in the linear viscoelastic regime show that gastric mucin undergoes a pH-dependent sol-gel transition from a viscoelastic solution at neutral pH to a soft viscoelastic gel in acidic conditions, with the transition occurring near pH 4. In addition to pH-dependent gelation behavior in this system, further rheological studies under nonlinear deformations reveal shear thinning and an apparent yield stress in this material which are also highly influenced by pH.

  14. Structural, Optical and Electrical Properties of Sol-Gel Derived Titanium Dioxide Thin Film

    NASA Astrophysics Data System (ADS)

    Taşkin, Dilek; Dumludaǧ, Fatih; Altindal, Ahmet

    2007-04-01

    Optical, structural and electrical (dc and ac) properties of sol-gel derived TiO2 film in a wide range of temperature (290 - 652 K) were investigated. XRD analysis was used for investigation the crystallinity of the films. Optical bad gap of the film were determined from transmission spectra. With the examination of the impedance spectra clear differences could be seen in the dependence of ω on both real and imaginary part of impedance between 290 K and 652 K. The impedance response is significantly changed with the increase of temperature.

  15. Development of an efficient large-aperture high damage-threshold sol-gel diffraction grating.

    SciTech Connect

    Ashley, Carol S.; Rambo, Patrick K.; Schwarz, Jens; Dunphy, Darren Robert; Branson, Eric D.; Smith, Ian Craig; Johnson, William Arthur; Reed, Scott T.; Cook, Adam W.

    2005-03-01

    In order to develop the next generation of high peak intensity lasers, new grating technology providing higher damage thresholds and large apertures is required. The current assumption is that this technical innovation will be multilayer dielectric gratings, wherein the uppermost layer of a thin film mirror is etched to create the desired binary phase grating. A variant of this is explored with the upper grating layer being a lower density gelatin-based volume phase grating in either sol-gel or dichromated gelatin. One key benefit is the elimination of the etching step.

  16. Fabrication of inverted zinc oxide photonic crystal using sol-gel solution by spin coating method.

    PubMed

    Huang, Kuo-Min; Ho, Chong-Lung; Chang, Heng-Jui; Wu, Meng-Chyi

    2013-01-01

    Inverted zinc oxide photonic crystal structures were fabricated from polystyrene sphere (PSS) template using the sol-gel solution of ZnO by spin-coating method. It is easily able to control and fabricate the photonic crystal structures using the self-organized PSS with a size of 193 nm. The inverted ZnO photonic crystal structures observed show the (111) tendency of the hexagonal compact arrangement formation. The resulting structures possess the photonic band gaps in the near-ultraviolet range and exhibit an enhanced photoluminescence spectrum. The technology can effectively increase the light output intensity or efficiency for the applications of optoelectronic devices.

  17. Synthesis of hybrid sol-gel coatings for corrosion protection of we54-ae magnesium alloy

    NASA Astrophysics Data System (ADS)

    Hernández-Barrios, C. A.; Duarte, N. Z.; Hernández, L. M.; Peña, D. Y.; Coy, A. E.; Viejo, F.

    2013-11-01

    The present work shows some preliminary results related to the synthesis, characterization and corrosion evaluation of different hybrid sol-gel coatings applied on the WE54-AE magnesium alloy attending to the two experimental variables, i.e. the precursors ratio and the aging time, which may affect the quality and the electrochemical properties of the coatings resultant. The experimental results confirmed that, under some specific experimental conditions, it was possible to obtain homogeneous and uniform, porous coatings with good corrosion resistance that also permit to accommodate corrosion inhibitors.

  18. Flat ceramic ultrafiltration membranes and modules coated by the sol-gel technique

    SciTech Connect

    Pflanz, K.; Stroh, N.; Riedel, R.

    1994-12-31

    Sol-gel techniques are common in preparing inorganic ultrafiltration membranes. Since applicable membranes should exhibit improved chemical and thermal stability with respect to phase transition, pore size and particle growth, the authors developed a new method for preparing an inorganic ultrafiltration membrane made of magnesium aluminum spinel, MgAl{sub 2}O{sub 4}. This membrane is supported by a flat ceramic microfilter ({alpha}-Al{sub 2}O{sub 3}) produced via the tape casting process, which offers the opportunity of improved processing techniques and new module concepts compared to the widely used extruded multi channel modules. Membrane characteristics and some applications will be shown.

  19. Characterization of ZnO films prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Zhang, Jide; Sun, Xin; Qi, Tong; Ren, Ge; Shan, Yingyu; Dong, Qingya

    2017-03-01

    The ZnO thin films were prepared on an ordinary glass substrate using an optimized Sol-gel Method. X-ray diffraction patterns indicated that the grain size increased with increasing annealing temperature. The surface morphology of the films was also analyzed by atomic force microscopy get the same result. The UV-Vis absorption spectra showed that the band edge absorption at the ZnO band edge was strong, and the band gap of the film annealed at 450 °C was 3.29eV.

  20. Thin film of sol-gel deposited in photonic crystal fiber for cholesterol detection

    NASA Astrophysics Data System (ADS)

    Razo-Medina, D. A.; Alvarado-Méndez, E.; Trejo-Durán, M.

    2015-04-01

    In this work, the fabrication of thin films mixed with cholesterol enzyme as recognition component is shown, using solgel technique. The film was deposited at one end of photonic crystal fiber (optrode), which was used as carrier medium of sol-gel matrix. The concentration of cholesterol in the test sample was determined by the use of transmittance. Measuring device consists of a power source (laser diode), optrode and a light detector. The laser beam is transmitted through the optrode; the variations of intensity depending on cholesterol concentration are emitted to be detected by a photoresistor.

  1. Electroanalytical applications of screen-printable surfactant-induced sol-gel graphite composites

    SciTech Connect

    Guadalupe, Ana R.; Guo, Yizhu

    2001-05-15

    A process for preparing sol-gel graphite composite electrodes is presented. This process preferably uses the surfactant bis(2-ethylhexyl) sulfosuccinate (AOT) and eliminates the need for a cosolvent, an acidic catalyst, a cellulose binder and a thermal curing step from prior art processes. Fabrication of screen-printed electrodes by this process provides a simple approach for electroanalytical applications in aqueous and nonaqueous solvents. Examples of applications for such composite electrodes produced from this process include biochemical sensors such as disposable, single-use glucose sensors and ligand modified composite sensors for metal ion sensitive sensors.

  2. Highly sensitive detection of hexavalent chromium utilizing a sol-gel/carbon nanotube modified electrode.

    PubMed

    Rosolina, Samuel M; Bragg, Stefanie A; Ouyang, Ruizhuo; Chambers, James Q; Xue, Zi-Ling

    2016-11-15

    A pyridine-functionalized thin film has been fabricated to selectively preconcentrate Cr(VI) anions for electrochemical detection in the 5-300 μg L(-1) range. Glassy carbon electrodes were modified through physical deposition of single-walled carbon nanotubes (SWNTs) on the electrode surface, followed by electrochemical deposition of a sol-gel containing a 2-pyridine functional group. The use of SWNTs has increased sensitivity for Cr(VI) detection in aqueous solutions, providing a detection limit of 0.8 μg L(-1).

  3. Optical characterization of Sol-Gel ZnO:Al thin films

    NASA Astrophysics Data System (ADS)

    Ivanova, T.; Harizanova, A.; Koutzarova, T.; Vertruyen, B.

    2016-03-01

    This paper presents a sol-gel technological process for preparing thin films of ZnO and ZnO:Al. The effect of annealing treatments (500, 600, 700 and 800 °C) on their properties was studied. The structural evolution with the temperature was investigated by using X-Ray diffraction (XRD). Fourier Transform Infrared (FTIR) and UV-VIS spectrophotometry were applied to characterizing the films' vibrational and optical properties. The ZnO and ZnO:Al films possessed a polycrystalline structure. The films studied are highly transparent in the visible spectral range. The optical band gap values and the haze parameter were also determined.

  4. Investigation of sol-gel yttrium doped ZnO thin films: structural and optical properties

    NASA Astrophysics Data System (ADS)

    Ivanova, T.; Harizanova, A.; Koutzarova, T.; Vertruyen, B.

    2016-02-01

    Nanostructured metal oxide films are extensively studied due to their numerous applications such as optoelectronic devices, sensors. In this work, we report the Y-Zn-O nanostructured films prepared by sol-gel technology from sols with different concentration of yttrium precursor, followed by post-annealing treatment. The Y doped ZnO thin films have been deposited on Si and quartz substrates by spin coating method, then treated at temperatures ranging from 300-800oC. XRD analysis reveals modification of the film structure and phases in the doped ZnO films.

  5. Uncooled 160×120 microbolometer IR FPA based on sol-gel VOx

    NASA Astrophysics Data System (ADS)

    Dem'yanenko, Michael A.; Fomin, Boris I.; Ovsyuk, Victor N.; Marchishin, Igor V.; Parm, Igor O.; Vasil'ieva, Lyudmila L.; Shashkin, Valeri V.

    2005-09-01

    The technology of high-quality microbolometer focal plane arrays (FPA) fabrication has been developed. Simple and cheap sol-gel technology of thermosensitive vanadium oxide layers preparation is underlain in its basis. Uncooled 160×120 microbolometer sensor assemblies for 8-14 microns spectral range have been fabricated. The paper brief outlines simple techniques to measure crosstalk, precision of FPA temperature stabilization and sensor assembly response time to infrared signal change. The noise equivalent temperature difference better than 100 mK has been achieved at frame rate 60 Hz and F/1 optics.

  6. Hydrogen photochromism in V2O5 layers prepared by the sol-gel technology

    NASA Astrophysics Data System (ADS)

    Wang, Yi; Pan, Lei; Li, Yao; Gavrilyuk, A. I.

    2014-09-01

    Here we report on hydrogen photochromism in V2O5 highly disordered layers, i.e., photochromism that occurs due to hydrogen atoms; the hydrogen being detached under the action of light from organic molecules adsorbed on the oxide surface, whereas the V2O5 layers have been prepared by the sol-gel technology. The comprehensive characterization of the layers has been carried out, as well as the investigation of the parameters influencing their photochromic sensitivity. The high photochromic sensitivity of the V2O5 layers is provided by the surface Grotthuss diffusion of the injected protons.

  7. Effect of magnesia on the degradability and bioactivity of sol-gel derived SiO2-CaO-MgO-P2O5 system glasses.

    PubMed

    Ma, J; Chen, C Z; Wang, D G; Jiao, Y; Shi, J Z

    2010-11-01

    Mesoporous 58SiO(2)-(38-x)CaO-xMgO-4P(2)O(5) glasses (where x=0, 5, 10 and 20 mol%) have been prepared by the sol-gel synthesis route. The effects of the substitution of MgO for CaO on glass degradation and bioactivity were studied in tris-(hydroxymethyl)-aminomethane and hydrochloric acid buffer solution (Tris-HCl) and simulated body fluid (SBF), respectively. It is observed that the synthesized glasses with various MgO contents possess the similar textural properties. The studies of in vitro degradability and bioactivity show that the rate of glass degradation gradually decreases with the increase of MgO and the formation of apatite layer on glass surface is retarded. The influences of the composition upon glass properties are explained in terms of their internal structures.

  8. Sol-gel synthesis of magnetic sorbents based on porous iron oxides for the removal of U(VI) from aqueous solution

    NASA Astrophysics Data System (ADS)

    Papynov, E. K.; Portnyagin, A. S.; Cherednichenko, A. I.; Tkachenko, I. A.; Modin, E. B.; Dran'kov, A. N.; Kvach, A. A.; Zemchenko, I. V.; Tananaev, I. G.; Avramenko, V. A.

    2017-02-01

    An original synthetic route to nanostructured iron oxides with porous structure and to their reduced derivatives, prospective for uranium (VI) uptake from water media, is presented. The uniqueness of method includes combination of sol-gel technology, which used for generating inorganic framework, and template synthesis for porous structure formation with the help of poreforming agent (polymer latex). Method of consolidating porous iron oxides and its influence on such characteristics as porosity, magnetization, morphology, phase composition and sorption properties are described. Sorption properties of the materials based on iron oxides and their reduced derivatives with respect to uranium (VI) from water media of different acidity has been investigated. Mechanism of uranium (VI) sorption on the obtained materials has been determined. The interaction of the sorbents with uranyl-ions was shown to change depending on phase composition and structure of the solid matrix.

  9. Dielectric properties and alternating current conductivity of sol-gel made La0.8Ca0.2FeO3 compound

    NASA Astrophysics Data System (ADS)

    Benali, A.; Souissi, A.; Bejar, M.; Dhahri, E.; Graça, M. F. P.; Valente, M. A.

    2015-09-01

    In this work, single phase La0.8Ca0.2FeO3 nanomaterial has been synthesized by the sol-gel method using the citric acid route. By employing impedance spectroscopy, ac electrical properties have been measured over a temperature range from 300 to 673 K at various frequencies. With the analysis based on Debye's theory and a series of Arrhenius relations, the relaxation was argued to be associated with the hopping motions of charge carriers between Fe ions. The relaxation in the La0.8Ca0.2FeO3 compound was ascribed to be a polaronic relaxation. The ac electrical conduction was studied and associated to the non-overlapping small polaron tunneling (NSPT) model.

  10. Nanoscopic yttrium oxide fluorides: non-aqueous fluorolytic sol-gel synthesis and structural insights by 19F and 89Y MAS NMR.

    PubMed

    Scholz, G; Dreger, M; Bertram, R; Kemnitz, E

    2015-08-14

    Nanoscopic yttrium acetate fluorides Y(CH(3)COO)(3-z)F(z) and yttrium oxide fluorides YO(3-z)/(2)F(z )were prepared with tunable Y/F molar ratios via the fluorolytic sol-gel route. All samples were characterized by X-ray diffraction, elemental analysis and thermal analysis. In addition, local structures of all samples were studied by (19)F MAS, (19)F-(89)Y CP MAS and (1)H-(89)Y CP MAS NMR spectroscopy and the respective chemical shifts are given. For both classes of compounds, only the fluorination using one equivalent of F (z = 1) leads to defined, well crystalline matrices: yttrium acetate fluoride Y(CH(3)COO)(2)F and r-YOF.

  11. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    PubMed

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column.

  12. Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: dissolution behaviour and biological properties after crystallisation.

    PubMed

    Tredwin, Christopher J; Young, Anne M; Abou Neel, Ensanya A; Georgiou, George; Knowles, Jonathan C

    2014-01-01

    Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) were synthesised by the sol-gel method as possible implant coating or bone-grafting materials. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride were incorporated for the preparation of the FHA and FA sol-gels. After heating and powdering the sol-gels, dissolution behaviour was assessed using ion chromatography to measure Ca(2+) and PO4 (3-) ion release. Biological behaviour was assessed using cellular proliferation with human osteosarcoma cells and alamarBlue™ assay. Statistical analysis was performed with a two way analysis of variance and post hoc testing with a Bonferroni correction. Increasing fluoride substitution into an apatite structure decreased the dissolution rate. Increasing the firing temperature of the HA, FHA and FA sol-gels up to 1,000 °C decreased the dissolution rate. There was significantly higher cellular proliferation on highly substituted FHA and FA than on HA or Titanium. The properties of an implant coating or bone grafting material can be tailored to meet specific requirements by altering the amount of fluoride that is incorporated into the original apatite structure. The dissolution behaviour can further be altered by the temperature at which the sol-gel is fired.

  13. Sol-gel optical thin films for an advanced megajoule-class Nd:glass laser ICF-driver

    SciTech Connect

    Floch, H.G.; Belleville, P.F.; Pegon, P.M.; Dijonneau, C.S.; Guerain, J.

    1995-12-31

    It is well established by manufacturers and users that optical coatings are generally prepared by the well known Physical Vapor Deposition (PVD) technology. In the authors` opinion sol-gel technology is an effective and competitive alternative. The aim of this paper is to emphasize on the sol-gel thin film work carried out at Centre d`Etudes de Limeil-Valenton (CEL-V) and concerning the technology for high power lasers. The authors will briefly discuss the chemistry of the sol-gel process, the production of optical coatings and the related deposition techniques. Finally, the paper describes the preparation and performance of sol-gel optical coatings they have developed to fulfill the requirements of a future 2 MJ/500 TW (351 nm) pulsed Nd:glass laser so-called LMJ (Laser MegaJoules). This powerful laser is to be used for their national Inertial Confinement Fusion (ICF) program, to demonstrate at the laboratory scale, ignition of deuterium-tritium fusion fuel. Moreover, the aim of this article is, hopefully, to provide a convincing argument that coatings and particularly optical coatings, are some of the useful products available from sol-gel technology, and that exciting developments in other areas are almost certain to emerge within the coming decade.

  14. An improved bonded-polydimethylsiloxane solid-phase microextraction fiber obtained by a sol-gel/silica particle blend.

    PubMed

    Azenha, Manuel; Nogueira, Pedro; Fernando-Silva, A

    2008-03-10

    A novel procedure for solid-phase microextraction fiber preparation is presented, which combines the use of a rigid titanium alloy wire as a substrate with a blend of PDMS sol-gel mixture/silica particles, as a way of increasing both the mechanical robustness and the extracting capability of the sol-gel fibers. The approximately 30 microm average thick fibers displayed an improvement in the extraction capacity as compared to the previous sol-gel PDMS fibers, due to a greater load of stable covalently bonded sol-gel PDMS. The observed extraction capacity was comparable to that of 100 microm non-bonded PDMS fiber, having in this case the advantages of the superior robustness and stability conferred, respectively, by the unbreakable substrate and the sol-gel intrinsic characteristics. Repeatability (n=3) ranged 1-8% while fiber production reproducibility (n=3) ranged 15-25%. The presence of the silica particles was found to have no direct influence on the kinetics and mechanism of the extraction process, thus being possible to consider the new procedure as a refinement of the previous ones. The applicability potential of the devised fiber was illustrated with the analysis of gasoline under the context of arson samples.

  15. Sol-gel optical thin films for an advanced megajoule-class Nd:glass laser ICF driver

    NASA Astrophysics Data System (ADS)

    Floch, Herve G.; Belleville, Philippe F.; Pegon, Philippe M.; Dijonneau, Corinne S.; Guerain, Jacques R.

    1995-12-01

    It is well established by manufacturers and users that optical coatings are generally prepared by the well known physical vapor deposition (PVD) technology. In the authors' opinion sol-gel technology is an effective and competitive alternative. The aim of this paper is to emphasize the sol-gel thin film work carried out at Centre d'Etudes de Limeil-Valenton (CEL-V) and concerning the technology for high power lasers. We briefly discuss the chemistry of the sol- gel process, the production of optical coatings, and the related deposition techniques. Finally, the paper describes the preparation and performance of sol-gel optical coatings we have developed to fulfill the requirements of a future 2 MJ/500 TW (351 nm) pulsed Nd:glass laser so-called LMJ (Laser MegaJoules). This powerful laser is to be used for our national inertial confinement fusion (ICF) program, to demonstrate at the laboratory scale, ignition of deuterium-tritium fusion fuel. Moreover, the aim of this article is, hopefully, to provide a convincing argument that coatings and particularly optical coatings, are some of the useful products available from sol-gel technology , and that exciting developments in other areas are almost certain to emerge within the coming decade.

  16. Synthesis of Titania-supported Copper Nanoparticles via Refined Alkoxide Sol-gel Process

    NASA Astrophysics Data System (ADS)

    Wu, Jeffrey C. S.; Tseng, I.-Hsiang; Chang, Wan-Chen

    2001-06-01

    Nanoparticles of titania and copper-loaded titania were synthesized by a refined sol-gel method using titanium butoxide. Unlike the conventional sol-gel procedure of adding water directly, the esterification of anhydrous butanol and glacial acetic acid provided the hydrolyzing water. In addition, acetic acid also served as a chelating ligand to stabilize the hydrolysis-condensation process and minimize the agglomeration of titania. Following the hydrolysis, Cu/TiO2 was prepared by adding copper chloride to titania sol. The sol was dried, then calcined at 500°C to remove organics and transformed to anatase titania which was verified by XRD. Cu/TiO2 was further hydrogen-reduced at 300°C. The recovery of Ti was exceeded by an average of 95% from titanium butoxide. TEM micrographs show that the Cu/TiO2 particles are near uniform. The average crystallite sizes are 17-20 nm estimated from the peak broadening of XRD spectra. The bandgaps of TiO2 and reduced Cu/TiO2 range from 2.70 to 3.15 eV estimated from the diffusive reflective UV-Vis spectra. XPS analysis shows that Cu 2p3/2 is 933.4 eV indicating primary Cu2O form on the TiO2 supports. The binding energy of Ti does not exhibit chemical shift suggesting negligible interaction of Cu cluster and TiO2 support.

  17. Sol-gel network silica/modified montmorillonite clay hybrid nanocomposites for hydrophobic surface coatings.

    PubMed

    Meera, Kamal Mohamed Seeni; Sankar, Rajavelu Murali; Murali, Adhigan; Jaisankar, Sellamuthu N; Mandal, Asit Baran

    2012-02-01

    Sol-gel silica/nanoclay composites were prepared through sol-gel polymerization technique using tetraethylorthosilicate precursor and montmorillonite (MMT) clay in aqueous media. In this study, both montmorillonite-K(+) and organically modified MMT (OMMT) clays were used. The prepared composites were coated on glass substrate by making 1 wt% solution in ethyltrichlorosilane. The incorporation of nanoclay does not alter the intensity of characteristic Si-O-Si peak of silica network. Thermogravimetric studies show that increasing clay content increased the degradation temperature of the composites. Differential scanning calorimetry (DSC) results of organically modified MMT nanoclay incorporated composite show a shift in the melting behavior up to 38°C. From DSC thermograms, we observed that the ΔH value decreased with increasing clay loading. X-ray diffraction patterns prove the presence of nanoclay in the composite and increase in the concentration of organically modified nanoclay from 3 to 5 wt% increases the intensity of the peak at 2θ=8° corresponds to OMMT. Morphology of the control silica gel composite was greatly influenced by the incorporation of OMMT. The presence of nanoclay changed the surface of control silica gel composite into cleaved surface with brittle in nature. Contact angle measurements were done for the coatings to study their surface behavior. These hybrid coatings on glass substrate may have applications for hydrophobic coatings on leather substrate.

  18. Biocompatible Nb2O5 thin films prepared by means of the sol-gel process.

    PubMed

    Velten, D; Eisenbarth, E; Schanne, N; Breme, J

    2004-04-01

    Thin biocompatible oxide films with an optimised composition and structure on the surface of titanium and its alloys can improve the implant integration. The preparation of these thin oxide layers with the intended improvement of the surface properties can be realised by means of the sol-gel process. Nb2O5 is a promising coating material for this application because of its extremely high corrosion resistance and thermodynamic stability. In this study, thin Nb2O5 layers ( < 200 nm) were prepared by spin coating of polished discs of cp-titanium with a sol consisting of a mixture of niobium ethoxide, butanol and acetylacetone. The thickness, phase composition, corrosion resistance and the wettability of the oxide layers were determined after an optimisation of the processing parameters for deposition of oxide without any organic impurities. The purity of the oxide layer is an important aspect in order to avoid a negative response to the cell adhesion. The biocompatibility of the oxide layers which was investigated by in vitro tests (morphology, proliferation rate, WST-1, cell spreading) is improved as compared to uncoated and TiO2 sol-gel coated cp-titanium concerning the spreading of cells, collagen I synthesis and wettability.

  19. Phospholipid Fatty Acids as Physiological Indicators of Paracoccus denitrificans Encapsulated in Silica Sol-Gel Hydrogels

    PubMed Central

    Trögl, Josef; Jirková, Ivana; Kuráň, Pavel; Akhmetshina, Elmira; Brovdyová, Tat′jána; Sirotkin, Alexander; Kirilina, Tatiana

    2015-01-01

    The phospholipid fatty acid (PLFA) content was determined in samples of Paracoccus denitrificans encapsulated in silica hydrogel films prepared from prepolymerized tetramethoxysilane (TMOS). Immediately after encapsulation the total PLFA concentration was linearly proportional to the optical density (600 nm) of the input microbial suspension (R2 = 0.99). After 7 days this relationship remained linear, but with significantly decreased slope, indicating a higher extinction of bacteria in suspensions of input concentration 108 cells/mL and higher. trans-Fatty acids, indicators of cytoplasmatic membrane disturbances, were below the detection limit. The cy/pre ratio (i.e., ratio of cyclopropylated fatty acids (cy17:0 + cy19:0) to their metabolic precursors (16:1ω7 + 18:1ω7)), an indicator of the transition of the culture to a stationary growth-phase, decreased depending on co-immobilization of nutrients in the order phosphate buffer > mineral medium > Luria Broth rich medium. The ratio, too, was logarithmically proportional to cell concentration. These results confirm the applicability of total PLFA as an indicator for the determination of living biomass and cy/pre ratio for determination of nutrient limitation of microorganisms encapsulated in sol-gel matrices. This may be of interest for monitoring of sol-gel encapsulated bacteria proposed as optical recognition elements in biosensor construction, as well as other biotechnological applications. PMID:25690547

  20. Development of novel biocompatible hybrid nanocomposites based on polyurethane-silica prepared by sol gel process.

    PubMed

    Rashti, Ali; Yahyaei, Hossein; Firoozi, Saman; Ramezani, Sara; Rahiminejad, Ali; Karimi, Roya; Farzaneh, Khadijeh; Mohseni, Mohsen; Ghanbari, Hossein

    2016-12-01

    Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants.

  1. Application of fluorinated compounds to cotton fabrics via sol-gel

    NASA Astrophysics Data System (ADS)

    Ferrero, Franco; Periolatto, Monica

    2013-06-01

    The aim of this work was the study of the surface modification of cotton fibers to confer hydro and oil repellency to the fabrics. A surface treatment not involving the bulk of the fibers was chosen, so fabrics can maintain comfort properties. Moreover the study focused on an economical and environmental friendly process, in order to obtain an effective treatment with good fastness to washing. A modified silica based film was applied on fibers surface by sol-gel, comparing laboratory grade reagents with a commercial product as precursors and optimizing process parameters. From obtained results sol-gel can be indicated as a promising process to confer an effective and durable finishing to cotton fibers with low add-ons. Long impregnation times can significantly improve the treatment fastness, while ironing the washed samples can restore, at least partially, hydro and oil repellency lost after the washing. Obtained results were supported by a deep surface characterization of untreated, treated and washed samples. The best results were obtained using the commercial product as the only precursor. This is interesting for an industrial application, due to the low cost of this product if compared with the laboratory grade reagents investigated. Some applications of finished textiles can be for household use, technical garments, umbrellas or outdoor textiles.

  2. Sol-gel replicated optics made from single point diamond turned masters exhibit fractal surface roughness

    SciTech Connect

    Bernacki, B.E.; Miller, A.C. Jr.; Evans, B.M. III; Moreshead, W.V.; Nogues, J.L.R.

    1996-05-01

    Deterministic optics manufacturing, notably single point diamond turning (SPDT) has matured such that the current generation of machines is capable of producing refractive and reflective optics for the visible wavelength region that are quite acceptable for many applications. However, spiral tool marks are still produced that result in unwanted diffractive scattering from grating-like features having a spatial frequency determined by the machine feed, tool radius, and other influences such as vibration and material removal effects. Such regular artifacts are the characteristic of deterministic manufacturing methods such as SPDT. The authors present some initial findings suggesting that fractal, or non-deterministic surfaces can be produced by SPDT through sol-gel replication. The key is the large isotropic shrinkage that occurs through monolithic sol-gel replication (a factor of 2.5) that results in all features, including tooling marks, being reduced by that amount. The large shrinkage itself would be a laudable-enough feature of the replication process. However, by an as-yet-not understood manner, the replication process itself seems to alter the roughness character of the replicated surface such that it appears to be fractal when analyzed using contact profilometry and the power spectrum approach.

  3. Characterizations of maghemite thin films prepared by a sol-gel method

    SciTech Connect

    Lau, L. N. Ibrahim, N. B.

    2015-09-25

    Iron is one of the abundant elements of Mother Nature and its compound, iron oxide is an interesting material to study since its discovery in the form of magnetite. It can exist in many phases such as hematite and maghemite, this unique nature has put it as a potential candidate in various applications. The aim of this work is to study the influence of different precursor concentrations on the microstructural and magnetic properties of iron oxide thin film. All samples were prepared via the sol-gel method followed by a spin coating technique on quartz substrates. Iron oxide films were confirmed as maghemite phase from X-ray diffraction patterns. The film morphology was examined by a field emission scanning electron microscope and it showed non-systematic value of average grain size and film thickness throughout the study. Hysteresis loop further confirmed that maghemite is a magnetic material when it was characterized by a vibrating sample magnetometer. The coercivity did not show any correlation with molarity. Nevertheless, it increased as the precursor concentration of the film increased due to the domain behaviour. In conclusion, maghemite thin films were successfully synthesized by the sol-gel method with different precursor concentrations in this work.

  4. Versatile bio-ink for covalent immobilization of chimeric avidin on sol-gel substrates.

    PubMed

    Heikkinen, Jarkko J; Kivimäki, Liisa; Määttä, Juha A E; Mäkelä, Inka; Hakalahti, Leena; Takkinen, Kristiina; Kulomaa, Markku S; Hytönen, Vesa P; Hormi, Osmo E O

    2011-10-15

    A bio-ink for covalent deposition of thermostable, high affinity biotin-binding chimeric avidin onto sol-gel substrates was developed. The bio-ink was prepared from heterobifunctional crosslinker 6-maleimidohexanoic acid N-hydroxysuccinimide which was first reacted either with 3-aminopropyltriethoxysilane or 3-aminopropyldimethylethoxysilane to form silane linkers 6-maleimide-N-(3-(triethoxysilyl)propyl)hexanamide or -(ethoxydimethylsilyl)propyl)-hexanamide. C-terminal cysteine genetically engineered to chimeric avidin was reacted with the maleimide group of silane linker in methanol/PBS solution to form a suspension, which was printed on sol-gel modified PMMA film. Different concentrations of chimeric avidin and ratios between silane linkers were tested to find the best properties for the bio-ink to enable gravure or inkjet printing. Bio-ink prepared from 3-aminopropyltriethoxysilane was found to provide the highest amount of active immobilized chimeric avidin. The developed bio-ink was shown to be valuable for automated fabrication of avidin-functionalized polymer films.

  5. Microalgae fiber optic biosensors for herbicide monitoring using sol-gel technology.

    PubMed

    Peña-Vázquez, Elena; Maneiro, Emilia; Pérez-Conde, Concepción; Moreno-Bondi, Maria Cruz; Costas, Eduardo

    2009-08-15

    Three microalgal species (Dictyosphaerium chlorelloides (D.c.), Scenedesmus intermedius (S.i.) and Scenedesmus sp. (S.s.)) were encapsulated in silicate sol-gel matrices and the increase in the amount of chlorophyll fluorescence signal was used to quantify simazine. Influence of several parameters on the preparation of the sensing layers has been evaluated: effect of pH on sol-gel gelation time; effect of algae density on sensor response; influence of glycerol (%) on the membrane stability. Long term stability was also tested and the fluorescence signal from biosensors remained stable for at least 3 weeks. D.c. biosensor presented the lowest detection limits for simazine (3.6 microg L(-1)) and the broadest dynamic calibration range (19-860 microg L(-1)) with IC(50) 125+/-14 microg L(-1). Biosensor was validated by HPLC with UV/DAD detection. The biosensor showed response to those herbicides that inhibit the photosynthesis at photosystem II (triazines: simazine, atrazine, propazine, terbuthylazine; urea based herbicides: linuron). However, no significant increases of fluorescence response was obtained for similar concentrations of 2,4-D (hormonal herbicide) or Cu(II). The combined use of two biosensors that use two different genotypes, sensitive and resistant to simazine, jointly allowed improving microalgae biosensor specificity.

  6. Frequency control of sol-gel composite films fabricated by stencil printing for nondestructive testing applications

    NASA Astrophysics Data System (ADS)

    Kaneko, Tsukasa; Kibe, Taiga; Kimoto, Keisuke; Nishimura, Ryota; Kobayashi, Makiko

    2016-07-01

    Ultrasonic transducers made of sol-gel composites have been developed for nondestructive testing (NDT) applications in various industrial fields. Stencil printing of sol-gel composite films has been developed for the reduction of fabrication time and cost. However, it was necessary to develop low frequency (<10 MHz) ultrasonic transducers for inspecting industrial structures under severe high-temperature conditions, because high-frequency components suffer attenuation effect caused by high temperature. To realize this, increasing the thickness of Pb(Zr,Ti)O3 (PZT)/PZT films fabricated by stencil printing was attempted in this study. The samples were fabricated by single-layer stencil printing with a thick stencil mask and multilayer pure stencil printing with prespraying and postspraying. The film thicknesses were 150-185 µm, and the center frequencies of ultrasonic responses were 6.0-6.4 MHz. Throughout three thermal cycles of up to 370 K, the ultrasonic performance was stable, and the frequency characteristics were not markedly different from the beginning to the end of the test. Therefore, low-frequency ultrasonic transducers were successfully manufactured using a stencil-printing-based technique.

  7. Fabrication of optical chemical ammonia sensors using anodized alumina supports and sol-gel method.

    PubMed

    Markovics, Akos; Kovács, Barna

    2013-05-15

    In this comparative study, the fabrication and the sensing properties of various reflectometric optical ammonia gas sensors are described. In the first set of experiments the role of the support material was investigated on four different sensor membranes. Two of them were prepared by the adsorption of bromocresol green indicator on anodized aluminum plates. The applied anodizing voltages were 12 V and 24 V, which resulted in different dynamic ranges and response times for gaseous ammonia. The sol-gel method was used for the preparation of the other batch of sensors. These layers were coated on anodized aluminum plates (24 V) and on standard microscope cover glasses. In spite of the identical sensing chemistry, slightly different response times were measured merely because of the aluminum surface porosity. Gas molecules can remain entrapped in the pores, which results in delayed recovery time. On the other hand, the porous oxide film provides excellent adhesion, making the anodized aluminum an attractive support for the sol-gel layer.

  8. Surface acoustic wave characterization of optical sol-gel thin layers.

    PubMed

    Fall, Dame; Compoint, François; Duquennoy, Marc; Piombini, Hervé; Ouaftouh, Mohammadi; Jenot, Frédéric; Piwakowski, Bogdan; Belleville, Philippe; Ambard, Chrystel

    2016-05-01

    Controlling the thin film deposition and mechanical properties of materials is a major challenge in several fields of application. We are more particularly interested in the characterization of optical thin layers produced using sol-gel processes to reduce laser-induced damage. The mechanical properties of these coatings must be known to control and maintain optimal performance under various solicitations during their lifetime. It is therefore necessary to have means of characterization adapted to the scale and nature of the deposited materials. In this context, the dispersion of ultrasonic surface waves induced by a micrometric layer was studied on an amorphous substrate (fused silica) coated with a layer of ormosil using a sol-gel process. Our ormosil material is a silica-PDMS mixture with a variable polydimethylsiloxane (PDMS) content. The design and implementation of Surface Acoustic Wave InterDigital Transducers (SAW-IDT) have enabled quasi-monochromatic Rayleigh-type SAW to be generated and the dispersion phenomenon to be studied over a wide frequency range. Young's modulus and Poisson's ratio of coatings were estimated using an inverse method.

  9. Antimicrobial activity of thin solid films of silver doped hydroxyapatite prepared by sol-gel method.

    PubMed

    Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

    2014-01-01

    In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x(Ag) = 0.5 are effective against E. coli and S. aureus after 24 h.

  10. "Beating speckles" via electrically-induced vibrations of Au nanorods embedded in sol-gel.

    PubMed

    Ritenberg, Margarita; Beilis, Edith; Ilovitsh, Asaf; Barkai, Zehava; Shahmoon, Asaf; Richter, Shachar; Zalevsky, Zeev; Jelinek, Raz

    2014-01-13

    Generation of macroscopic phenomena through manipulating nano-scale properties of materials is among the most fundamental goals of nanotechnology research. We demonstrate cooperative "speckle beats" induced through electric-field modulation of gold (Au) nanorods embedded in a transparent sol-gel host. Specifically, we show that placing the Au nanorod/sol-gel matrix in an alternating current (AC) field gives rise to dramatic modulation of incident light scattered from the material. The speckle light patterns take form of "beats", for which the amplitude and frequency are directly correlated with the voltage and frequency, respectively, of the applied AC field. The data indicate that the speckle beats arise from localized vibrations of the gel-embedded Au nanorods, induced through the interactions between the AC field and the electrostatically-charged nanorods. This phenomenon opens the way for new means of investigating nanoparticles in constrained environments. Applications in electro-optical devices, such as optical modulators, movable lenses, and others are also envisaged.

  11. External polyacrylate-coating as alternative material for preparation of photopolymerized sol-gel monolithic column.

    PubMed

    Vaz, Fernando Antonio Simas; de Castro, Patrícia Mendonça; Molina, Celso; Ribeiro, Sidney José Lima; Polachini, Ferminio César; Messaddeq, Younes; Nunes, Adriana Palombo; de Oliveira, Marcone Augusto Leal

    2008-06-30

    Photopolymerized sol-gel monolithic columns for use in capillary electrochromatography were prepared in 125 microm i.d. polyacrylate-coated fused-silica capillaries. The polyacrylate-coating, unlike the polyimide one, is transparent to the radiation used (approximately 370 nm), and thus, no coating removal is necessary. This is a very important particularity since intrinsic capillary column characteristics, such as flexibility and mechanical resistance, are unchanged. A mixture containing metacryloxypropyltrimethoxysilane (MPTMS) as the polymeric precursor, hydrochloric acid as the catalyst, toluene as the porogen and bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide (Irgacure 819) as the photoinitiator was irradiated at 370 nm for 20 min inside the capillaries to prepare the columns through sol-gel approach. The versatility and viability of the use of polyacrilate as a new capillary external coating were shown through preparation of two columns under different conditions, which were tested in electrochromatography for separation of standard mixture containing thiourea (marker compound), propylbenzene, phenanthrene and pyrene.

  12. TiO2/PCL hybrid materials synthesized via sol-gel technique for biomedical applications.

    PubMed

    Catauro, M; Bollino, F; Papale, F; Marciano, S; Pacifico, S

    2015-02-01

    The aim of the present work has been the synthesis of organic/inorganic hybrid materials based on titanium dioxide and poly(ε-caprolactone) (PCL) to be used in the biomedical field. Several materials have been synthesized using sol-gel methods by adding different amounts of polymer to the inorganic sol. The obtained gels have been characterized using Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and atomic force microscopy (AFM). The FT-IR data allowed us to hypothesize that the structure formed was that of an interpenetrating network, realized by hydrogen bonds between TiOH groups in the sol-gel intermediate species and carbonyl groups in the polymer repeating units. SEM and AFM analyses highlighted that the obtained materials were nanostructurated hybrids. To evaluate the biological properties of the hybrids, their bioactivity and cytotoxicity were investigated as a function of the PCL amount. The bioactivity of the synthesized systems was proven by the formation of a hydroxyapatite layer on the surface of samples soaked in a fluid simulating human blood plasma (SBF). MTT cytotoxicity tests and Trypan Blue dye exclusion tests were carried out exposing NIH-3T3 mouse embryonic fibroblasts for 24 and 48h to extracts from the investigated hybrid materials. The results showed that all the hybrids had a non-cytotoxic effect on target cells.

  13. A simplified method for capillary embedment into microfluidic devices - exemplified by sol-gel-based preconcentration.

    PubMed

    Thorslund, Sara; Johannesson, Nina; Nikolajeff, Fredrik; Bergquist, Jonas

    2007-12-01

    We here describe an alternative method of embedding functionalized capillaries into microdevices fabricated in PDMS. The capillaries have square-shaped outer dimensions and fit into elastic PDMS channel networks of similar dimensions. By modifying the capillary off-chip, the technique makes it possible to integrate a new chip function without risking contamination of already existing chemically patterned areas because of new reagent solutions. Leak-free insertion of these capillaries has earlier been reported, where a thin layer of uncured PDMS bonded the capillary to the microchannel and the lid structure. In this new approach, oxygen plasma is used to bond the square capillary to the PDMS, eliminating the risk of clogging the microsystem with uncured prepolymer. The new embedding technique was exemplified and evaluated by inserting a square capillary piece containing monolithic sol-gel for sample preconcentration application. The assembled microdevice was run with mass spectrometric detection, showing that peptides were preconcentrated without leakage from either the sol-gel itself or around the inserted capillary. Repeated preconcentration runs showed migration times better than 3% for all peptides. We believe that the presented microchip assembling technique greatly simplifies the insertion of functionalized capillary pieces, e.g., an initial preconcentrator to a PDMS device containing other downstream modules.

  14. NiO-silica based nanostructured materials obtained by microemulsion assisted sol-gel procedure

    SciTech Connect

    Mihaly, M.; Comanescu, A.F.; Rogozea, A.E.; Vasile, E.; Meghea, A.

    2011-10-15

    Graphical abstract: TEM micrograph of NiO/SiO{sub 2} nanoparticles. Highlights: {yields} Microemulsion assisted sol-gel procedure for NiO silica nanomaterials synthesis. {yields} Controlling the size and shape of nanoparticles and avoiding their aggregation. {yields} Narrow band-gap semiconductors (energies <3 eV) absorbing VIS or near-UV light biologically and chemically inert semiconductors entrapping/coating in silica network. {yields} Low cost as the microemulsion is firstly used in water metallic cation extraction. -- Abstract: NiO-silica based materials have been synthesized by microemulsion assisted sol-gel procedure. The versatility of these soft nanotechnology techniques has been exploited in order to obtain different types of nanostructures, such as NiO nanoparticles, NiO silica coated nanoparticles and NiO embedded in silica matrix. These materials have been characterized by adequate structural and morphology techniques: DLS, HR-TEM/SAED, BET, AFM. Optical and semiconducting properties (band-gap values) of the synthesized materials have been quantified by means of VIS-NIR diffuse reflectance spectra, thus demonstrating their applicative potential in various electron transfer phenomena such as photocatalysis, electrochromic thin films, solid oxide fuel cells.

  15. Combining inkjet printing and sol-gel chemistry for making pH-sensitive surfaces.

    PubMed

    Orsi, Gianni; De Maria, Carmelo; Montemurro, Francesca; Chauhan, Veeren M; Aylott, Jonathan W; Vozzi, Giovanni

    2015-01-01

    Today biomedical sciences are experiencing the importance of imaging biological parameters with luminescence methods. Studying 2D pH distribution with those methods allows building knowledge about complex cellular processes. Immobilizing pH sensitive nanoparticles inside hydrogel matrixes, in order to guarantee a proper SNR, could easily make stable and biocompatible 2D sensors. Inkjet printing is also well known as tool for printing images onto porous surfaces. Recently it has been used as a free-form fabrication method for building three-dimensional parts, and now is being explored as a way of printing electrical and optical devices. Inkjet printing was used either as a rapid prototyping method for custom biosensors. Sol-gel method is naturally bound with inkjet, because the picoliter-sized ink droplets evaporate quickly, thus allowing quick sol-gel transitions on the printed surface. In this work will be shown how to merge those technologies, in order to make a nanoparticles doped printable hydrogel, which could be used for making 2D/3D smart scaffolds able to monitor cell activities. An automated image analysis system was developed in order to quickly have the pH measurements from pH nanosensors fluorescence images.

  16. Development of sol-gel bioactive glass for hard tissue regeneration

    NASA Astrophysics Data System (ADS)

    Noor, Siti Noor Fazliah Mohd; Zain, Nurul Shazwani Mohd; Wei, Poh Yong; Azizan, Nur Syazana; Mohamad, Hasmaliza

    2016-12-01

    The regeneration of hard tissues requires various contributing factors such as cells, scaffolds and growth factors. Bioactive glasses are known for its properties to stimulate hard tissue regeneration. In this study, sol-gel bioactive glasses (BG) were prepared and characterized. Sol-gel BG powders having particle size less than 25 µm were incubated with cell culture medium for 4 hours at 37°C on continuous rolling, and then the medium was filtered using 0.22 µm syringe filters. Prior to use, the SGBG-conditioned media were supplemented with 10% (v/v) fetal bovine serum and 1% (v/v) antibiotic-antimycotic, and were allowed to equilibrate overnight inside a CO2 incubator. The human dental pulp stem cells (DPSC) were incubated with the BG-conditioned media and their viability and proliferation were assessed at day 1, 2, 4 and 7 using Alamar Blue and MTT assays. The results showed that BG at various powders to liquid ratio concentrations promoted DPSC growth. The BG have potential to be used for hard tissue regeneration especially in the field of regenerative dentistry.

  17. Experimental Determination of the Formation Enthalpy of Calcium Cobaltate from Sol-Gel Precursors

    NASA Astrophysics Data System (ADS)

    Holgate, T. C.; Wu, N.; Nong, N. V.; Pryds, N.

    2017-02-01

    Calcium cobaltate (Ca3Co4O9) remains one of the most promising p-type oxide materials for high-temperature thermoelectric energy conversion. While much progress has been made in refining our understanding of the unique structure of the material, as well as optimization of the transport properties for thermoelectric efficiency, there remains a gap in the knowledge, both experimental and theoretical, of the thermodynamics of the system. Presented herein is an analysis of the heat of formation of the Ca3Co4O9 phase from sol-gel precursors using a highly sensitive differential scanning calorimeter, as well as observations of its decomposition into the Ca3Co2O6 phase. The reaction enthalpy of forming Ca3Co4O9 from CaCO3 and Co3O4 sol-gel precursors was determined to be +284 (±2%) kJ/mol, leading to a standard enthalpy of Ca3Co4O9 of -3307 (±3.5%) kJ/mol.

  18. Sol-Gel Synthesis of Layered Lithium Compounds and its Properties as Electrode for Lithium Batteries

    NASA Astrophysics Data System (ADS)

    Liu, H. X.; Hu, C.; Zhu, X. J.; Gan, X. Y.; Zhao, S. X.; Zhou, J.; Ouyang, S. X.

    Layered structural LixMnO2 was successfully synthesized by sol-gel and ion-exchange method in this study. The conditions of synthesis of layered LixMnO2 were investigated, the phase content of layered NaxMnO2 precursor and layered LixMnO2 were identified by X-ray diffractometer (XRD) with Cu Kα radiation. The microstructures of oxide powders were characterized by scanning electron microscope (SEM). The electrochemical properties of layered LixMnO2 cathode materials were tested, The effect of Co3+ and Zn2+ doped on the electrochemical properties were studied. We found that the P2 type layered structure β-Na0.7Mn1-xMxO2 (M = Co, Zn) could be obtained by heating the sol-gel precursor in air at 750°C for 1 h, layered β-Na0.7Mn1-xMxO2 could were transited into O2 type layered LiyMn1-xMxO2(y ≈ 0.67). The electrochemical properties of the layered LiyMn1-xMxO2 are high. The capacity of cathode material was increased by Co doped, the capacity of the cathode material was decreased by Zn doped.

  19. Synthesis and characterization of NiO nanopowder by sol-gel process

    SciTech Connect

    Ningsih, Sherly Kasuma Warda

    2015-09-30

    Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms were produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.

  20. Formation and microwave absorption of barium and strontium ferrite prepared by sol-gel technique

    NASA Astrophysics Data System (ADS)

    Sürig, C.; Hempel, K. A.; Bonnenberg, D.

    1993-11-01

    Ba and Sr ferrites are prepared by sol-gel technique with different Fe/Ba(Sr) ratios in the starting materials. Magnetization, coercive, and anisotropy field strength are determined depending on the heat treatment of the gel and the iron/barium(strontium) ratio in the starting material. A two-step heat treatment is used to prepare single-domain powders with high magnetization. These powders prepared by sol-gel technique show single-domain behavior with specific magnetization σS=649 A cm2/g and coercive field strength HcM=402 kA/m in the case of Ba ferrite and σS=695 A cm2/g and HcM=416 kA/m for Sr the ferrite. Al-substituted ferrites with high anisotropy field strengths are prepared additionally. Ferromagnetic resonance absorption is used to determine the anisotropy field strength and to investigate the formation process of the hexaferrite phase during the heat treatment. The beginning of hexaferrite formation occurs at annealing temperatures below 700 °C.

  1. A Guided Materials Screening Approach for Developing Quantitative Sol-gel Derived Protein Microarrays

    PubMed Central

    Helka, Blake-Joseph; Brennan, John D.

    2013-01-01

    Microarrays have found use in the development of high-throughput assays for new materials and discovery of small-molecule drug leads. Herein we describe a guided material screening approach to identify sol-gel based materials that are suitable for producing three-dimensional protein microarrays. The approach first identifies materials that can be printed as microarrays, narrows down the number of materials by identifying those that are compatible with a given enzyme assay, and then hones in on optimal materials based on retention of maximum enzyme activity. This approach is applied to develop microarrays suitable for two different enzyme assays, one using acetylcholinesterase and the other using a set of four key kinases involved in cancer. In each case, it was possible to produce microarrays that could be used for quantitative small-molecule screening assays and production of dose-dependent inhibitor response curves. Importantly, the ability to screen many materials produced information on the types of materials that best suited both microarray production and retention of enzyme activity. The materials data provide insight into basic material requirements necessary for tailoring optimal, high-density sol-gel derived microarrays. PMID:24022739

  2. Energetic Nanocomposites with Sol-gel Chemistry: Synthesis, Safety and Characterization

    SciTech Connect

    Gash, A E; Simpson, R L; Satcher, J H

    2002-05-15

    The preparation and characterization of energetic composite materials containing nanometer-sized constituents is currently a very active and exciting area of research at laboratories around the world. Some of these efforts have produced materials that have shown very unique and important properties relative to traditional energetic materials. We have previously reported on the use of sol-gel chemical methods to prepare energetic nanocomposites. Primarily we reported on the sol-gel method to synthesize nanometer-sized ferric oxide that was combined with aluminum fuel to make pyrotechnic nanocomposites. Since then we have developed a synthetic approach that allows for the preparation of hybrid inorganic/organic energetic nanocomposites. This material has been characterized by thermal methods, energy-filtered transmission electron microscopy (EFTEM), N, adsorption/desorption methods, and Fourier-Transform (FT-IR) spectroscopy, results of which will be discussed. According to these characterization methods the organic polymer phase fills the nanopores of the composite material, providing superb mixing of the component phases in the energetic nanocomposite. The EFTEM results provide a convenient and effective way to evaluate the intimacy of mixing between these component phases. The safe handling and preparation of energetic nanocomposites is of paramount importance to this research and we will report on studies performed to ensure such.

  3. Dialkylenecarbonate-Bridged Polysilsesquioxanes. Hybrid Organic Sol-Gels with a Thermally Labile Bridging Group

    SciTech Connect

    Loy, D.A.; Beach, J.V.; Baugher, B.M.; Assink, R.A.; Shea, K.J.; Tran, J.; Small, J.H.

    1999-04-21

    In this paper, we introduce a new approach for altering the properties of bridged polysilsesquioxane xerogels using post-processing modification of the polymeric network. The bridging organic group contains latent functionalities that can be liberated thermally, photochemically, or by chemical means after the gel has been processed to a xerogel. These modifications can produce changes in density, volubility, porosity, and or chemical properties of the material. Since every monomer possesses two latent functional groups, the technique allows for the introduction of high levels of functionality in hybrid organic-inorganic materials. Dialkylenecarbonate-bridged polysilsesquioxane gels were prepared by the sol-gel polymerization of bis(triethoxysilylpropyl)carbonate (1) and bis(triethoxysilylisobutyl)-carbonate (2). Thermal treatment of the resulting non-porous xerogels and aerogels at 300-350 C resulted in quantitative decarboxylation of the dialkylenecarbonate bridging groups to give new hydroxyalkyl and olefinic substituted polysilsesquioxane monolithic xerogels and aerogels that can not be directly prepared through direct sol-gel polymerization of organotrialkoxysilanes.

  4. Energetic Nanocomposites with Sol-gel Chemistry: Synthesis, Safety, and Characterization

    SciTech Connect

    Gash, A E; Simpson, R L; Satcher, J H

    2002-06-05

    The preparation and characterization of energetic composite materials containing nanometer-sized constituents is currently a very active and exciting area of research at laboratories around the world. Some of these efforts have produced materials that have shown very unique and important properties relative to traditional energetic materials. We have previously reported on the use of sol-gel chemical methods to prepare energetic nanocomposites. Primarily we reported on the sol-gel method to synthesize nanometer-sized ferric oxide that was combined with aluminum fuel to make pyrotechnic nanocomposites. Since then we have developed a synthetic approach that allows for the preparation of hybrid inorganic/organic energetic nanocomposites. This material has been characterized by thermal methods, energy-filtered transmission electron microscopy (EFTEM), N{sub 2} adsorption/description methods, and Fourier-Transform (FT-IR) spectroscopy, results of which will be discussed. According to these characterization methods the organic polymer phase fills the nanopores of the composite material, providing superb mixing of the component phases in the energetic nanocomposite. The EFTEM results provide a convenient and effective way to evaluate the intimacy of mixing between these component phases. The safe handling and preparation of energetic nanocomposites is of paramount importance to this research and we will report on studies performed to ensure such.

  5. Sol-gel processing of anti-inflammatory entrapment in silica, release kinetics, and bioactivity.

    PubMed

    Catauro, M; Melisi, D; Curcio, A; Rimoli, M G

    2008-12-15

    Controlled and local drug-delivery systems for anti-inflammatory agents are drawing increasing attention for possible pharmaceutical and biomedical applications, because of their extended therapeutic effect and reduced side effects. A single-step sol-gel process was used to precipitate silica microspheres containing Ketoprofen, Indomethacin, Ketorolac tris salt, or Triamcinolone acetonide, for controlled drug delivery applications. The amorphous nature of the gels was ascertained by X-ray diffraction analysis. Release kinetics in a simulated body fluid (SBF) has been subsequently investigated. The amount of drug released has been detected by UV-vis spectroscopy. The pure anti-inflammatory agent exhibited linear release with time, while sol-gel silica-entrapped drugs were released with a logarithmic time dependence, starting with an initial burst effect followed by a gradual decrease. Finally, SEM micrography and EDS analysis showed the formation of a hydroxyapatite layer on the surface of the samples soaked in SBF. All the materials showed good release and therefore could be used as drug-delivery systems.

  6. Use of sol-gel systems for solid/liquid separation.

    SciTech Connect

    Chaiko, D. J.; Kopasz, J. P.; Elison, A. J. G.; Chemical Engineering

    1998-01-01

    A unique approach using sol-gel technology is presented for separating and recovering particulates and colloids from caustic waste slurries. The approach involves the addition of an alkali silicate and an organic gelling agent directly to the waste stream to immobilize particulates that range from macro sizes to submicron colloids. The particulates and colloids become trapped within a silica network that remains porous during the early stages of the sol-gel process. The freshly gelled monolith undergoes a process of syneresis, whereby the water and soluble salts are ejected from the monolith as it contracts. The approach has been illustrated by removal of ultrafine particulates from a Hanford Tank Waste simulant. Initial laboratory tests have shown that it is possible to produce silica monoliths in the presence of 4 M hydroxide. Analysis of the mother liquor produced during syneresis indicated quantitative recovery of the particulates within the monolith. The partitioning of ions between the silica gel and the mother liquor during syneresis correlates directly with the lyotropic series. Salt recoveries from the mother liquor in excess of 90% can be achieved. With a capability of recovering >99.999% of all particulates, including colloids, the process is more efficient than membrane filtration. This approach produces a rock-hard silica monolith that can be used directly as a feedstock to a glass melter or can be consolidated to near theoretical density by sintering.

  7. Sol-gel method as a way of carbonyl iron powder surface modification for interaction improvement

    NASA Astrophysics Data System (ADS)

    Małecki, P.; Kolman, K.; Pigłowski, J.; Kaleta, J.; Krzak, J.

    2015-03-01

    This article presents a method for modification of carbonyl iron particles' surface (CIP), (d50=4-9 μm) by silica coatings obtained using the sol-gel method. Reaction parameters were determined to obtain dry magnetic powder with homogeneous silica coatings without further processing and without any by-product in the solid or liquid phase. This approach is new among the commonly used methods of silica coating of iron particles. No attempt has been made to cover a carbonyl iron surface by silica in a waste-free method, up to date. In the current work two different silica core/shell structures were made by the sol-gel process, based on different silica precursors: tetraethoxy-silane (TEOS) and tetramethoxy-silane (TMOS). The dependence between the synthesis procedure and thickness of silica shell covering carbonyl iron particles has been described. Surface morphology of the modified magnetic particles and the coating thickness were characterized with the use of scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Determination of the physicochemical structure of the obtained materials was performed by the energy-dispersive X-ray spectroscope (EDS), and the infrared technique (IR). The surface composition was analyzed using X-ray photoelectron spectroscopy (XPS). Additionally, distribution of particle size was measured using light microscopy. The new, efficient process of covering micro-size CIP with a nanometric silica layer was shown. Results of a performed analysis confirm the effectiveness of the presented method.

  8. Epoxide opening versus silica condensation during sol-gel hybrid biomaterial synthesis.

    PubMed

    Gabrielli, Luca; Russo, Laura; Poveda, Ana; Jones, Julian R; Nicotra, Francesco; Jiménez-Barbero, Jesús; Cipolla, Laura

    2013-06-10

    Hybrid organic-inorganic solids represent an important class of engineering materials, usually prepared by sol-gel processes by cross-reaction between organic and inorganic precursors. The choice of the two components and control of the reaction conditions (especially pH value) allow the synthesis of hybrid materials with novel properties and functionalities. 3-Glycidoxypropyltrimethoxysilane (GPTMS) is one of the most commonly used organic silanes for hybrid-material fabrication. Herein, the reactivity of GPTMS in water at different pH values (pH 2-11) was deeply investigated for the first time by solution-state multinuclear NMR spectroscopic and mass spectrometric analysis. The extent of the different and competing reactions that take place as a function of the pH value was elucidated. The NMR spectroscopic and mass spectrometric data clearly indicate that the pH value determines the kinetics of epoxide hydrolysis versus silicon condensation. Under slighly acidic conditions, the epoxy-ring hydrolysis is kinetically more favourable than the formation of the silica network. In contrast, under basic conditions, silicon condensation is the main reaction that takes place. Full characterisation of the formed intermediates was carried out by using NMR spectroscopic and mass spectrometric analysis. These results indicate that strict control of the pH values allows tuning of the reactivity of the organic and inorganic moities, thus laying the foundations for the design and synthesis of sol-gel hybrid biomaterials with tuneable properties.

  9. Entrapment of fluorescence signaling DNA enzymes in sol-gel-derived materials for metal ion sensing.

    PubMed

    Shen, Yutu; Mackey, Gillian; Rupcich, Nicholas; Gloster, Darin; Chiuman, William; Li, Yingfu; Brennan, John D

    2007-05-01

    Three fluorescence signaling DNA enzymes (deoxyribozymes or DNAzymes) were successfully immobilized within a series of sol-gel-derived matrixes and used for sensing of various metal ions. The DNAzymes are designed such that binding of appropriate metal ions induces the formation of a catalytic site that cleaves a ribonucleotide linkage within a DNA substrate. A fluorophore (fluorescein) and a quencher (DABCYL, [4-(4-dimethylaminophenylazo)benzoic acid]) were placed on the two deoxythymidines flanking the ribonucleotide to allow the generation of fluorescence upon the catalytic cleavage at the RNA linkage. In general, all DNAzymes retained at least partial catalytic function when entrapped in either hydrophilic or hydrophobic silica-based materials, but displayed slower response times and lower overall signal changes relative to solution. Interestingly, it was determined that maximum sensitivity toward metal ions was obtained when DNAzymes were entrapped into composite materials containing approximately 40% of methyltrimethoxysilane (MTMS) and approximately 60% tetramethoxysilane (TMOS). Highly polar materials derived from sodium silicate, diglycerylsilane, or TMOS had relatively low signal enhancements, while materials with very high levels of MTMS showed significant leaching and low signal enhancements. Entrapment into the hybrid silica material also reduced signal interferences that were related to metal-induced quenching; such interferences were a significant problem for solution-based assays and for polar materials. Extension of the solid-phase DNAzyme assay toward a multiplexed assay format for metal detection is demonstrated, and shows that sol-gel technology can provide new opportunities for the development of DNAzyme-based biosensors.

  10. Finite element modeling of evaporation and condensation during sol-gel film and fiber formation

    SciTech Connect

    Schunk, P.R.; Hurd, A.J.; Brinker, C.J.; Rao, R.R.

    1993-07-01

    Free surfaces, multicomponent phase change, volume expansion and compression, and surface tension gradients make for challenging application of the finite element method to sol-gel (ceramic) film and fiber formation. The microstructure of the final product is largely controlled by the competition between the drying, curing, and underlying fluid mechanics of formation. Sol-gel materials are peculiar because they often contain more than one solvent, each solvent differing in volatility and surface tension. Hence, nonuniform evaporation can produce surface tension gradients that dramatically change the meniscus shape. These processes are complicated further by a volume change that accompanies evaporation and condensation, making for shock-like discontinuities in concentration and velocity at the free surface. Computer-aided predictions of film formation by dip coating and of fiber spinning (see Figure 1) are made for alcohol-water mixtures with one non-volatile species. The Navier-Stokes system is augmented with two convective-diffusion equations to track the concentration of alcohol and water, and an energy equation to monitor temperature changes. The equations are solved in both phases by discretizing them first with the Galerkin/finite element method. The resulting non-linear algebraic equation set is solved with Newton`s method. The subdomaining technique is based on elliptic grid generation and is designed to parameterize the moving meniscus. Special treatment of the functional representations of velocity and concentration within the elements lining the free surface are made to accommodate the volume change that accompanies mass exchange between phases.

  11. New optical fiber type: microporous sol-gel-clad optical fibers

    NASA Astrophysics Data System (ADS)

    Skutnik, Bolesh J.

    1999-04-01

    A new type of optical fiber has been developed. It is made with all pure silica in both the core and cladding. This is possible because the cladding is a micro porous silica produced by a modified sol-gel technology. The formation and characteristics of this new optical fiber type are described. In particular the optical and mechanical properties are illustrated and described. The strength and fatigue of these optical fibers are very good, even without additional protective jackets. Unjacketed fibers have mean Weibull strengths in bending of 6.5 to 7.6 GPa with Weibull slopes in the 40 to 60 range. Fatigue results for fibers tested in ambient air, ambient water and boiling water are presented. The dynamic and static fatigue parameters are around 20. The micro porous structure of the sol-gel cladding provides sites for attaching different moieties which could activate biochemical reactions or be useful as sensing sites. Based on preliminary experiments, some possibilities are presented. In general this new structure can provide opportunities for as yet unidentified applications where chemicals and or light must be brought in close contact with body tissue to effect beneficial reactions there.

  12. Responsive hydrogels produced via organic sol-gel chemistry for cell culture applications.

    PubMed

    Patil, Smruti; Chaudhury, Pulkit; Clarizia, Lisa; McDonald, Melisenda; Reynaud, Emmanuelle; Gaines, Peter; Schmidt, Daniel F

    2012-08-01

    In this study, we report the synthesis of novel environmentally responsive polyurea hydrogel networks prepared via organic sol-gel chemistry and demonstrate that the networks can stabilize pH while releasing glucose both in simple aqueous media and in mammalian cell culture settings. Hydrogel formulations have been developed based on the combination of an aliphatic triisocyanate with pH-insensitive amine functional polyether and pH-sensitive poly(ethyleneimine) segments in a minimally toxic solvent suitable for the sol-gel reaction. The polyether component of the polyurea network is sufficiently hydrophilic to give rise to some level of swelling independent of environmental pH, while the poly(ethyleneimine) component contains tertiary amine groups providing pH sensitivity to the network in the form of enhanced swelling and release under acidic conditions. The reaction of these materials to form a network is rapid and requires no catalyst. The resultant material exhibits the desired pH-responsive swelling behavior and demonstrates its ability to simultaneously neutralize lactic acid and release glucose in both cell-free culture media and mammalian cell culture, with no detectable evidence of cytotoxicity or changes in cell behavior, in the case of either SA-13 human hybridomas or mouse embryonic stem cells. Furthermore, pH is observed to have a clear effect on the rate at which glucose is released from the hydrogel network. Such characteristics promise to maintain a favorable cell culture environment in the absence of human intervention.

  13. Silica Sol-Gel Optical Biosensors: Ultrahigh Enzyme Loading Capacity on Thin Films via Kinetic Doping.

    PubMed

    Crosley, Matthew S; Yip, Wai Tak

    2017-03-09

    Easy to use and easy to produce biosensors would have a huge range of applications. To reach this goal many see the incorporation of a protein into a sol-gel network as one of the most viable options. The current most prevalent technique of predoping presents inherent limits on the concentration possible for the resulting thin film. In this study we demonstrate a new process utilizing the newly developed kinetic doping method to load silica sol-gel thin films with cytochrome C (CytC) and horseradish peroxidase (HRP). Both enzymes are shown to successfully load and have a concentration increase over their original loading solution by factors of 1300× and 2600×, respectively. Furthermore, each enzyme once loaded retained the ability to act as a catalyst for the detection of hydrogen peroxide. Ultimately the CytC- and HRP-loaded thin films were found to have enzyme concentrations of 11 ± 1 mM and 6.0 ± 0.4 mM, respectively, a considerable step up from any doping method reported in the past.

  14. Fabrication of dye-sensitized solar cells using Nb2O5 blocking layer made by sol-gel method.

    PubMed

    Kim, Jaehwan; Kim, Jongsung

    2011-08-01

    In this study, nanocrystalline Nb2O5 thin film has been prepared via sol-gel process using niobium ethoxide as a precursor. Sol-gel films using various ratios of H2O/Nb have been prepared on fluorinated tin oxide (FTO) glass substrate, and used as electron-blocking layer of dye-sensitized solar cell (DSSC). The Nb2O5 film as deposited was amorphous, but became crystalline with hexagonal phase after heat treatment at 600 degrees C. With higher H2O/Nb molar ratio, denser and more uniform Nb2O5 film surface was obtained. DSSCs with the structure of FTO/Nb2O5/TiO2/Dye/EL/Pt/FTO have been prepared, and their solar-cell performance was evaluated. By introduction of Nb2O5 sol-gel film between FTO and TiO2 layer in DSSCs, energy conversion efficiency could be improved.

  15. Luminescence of Eu(3+) doped SiO2 Thin Films and Glass Prepared by Sol-gel Technology

    NASA Technical Reports Server (NTRS)

    Castro, Lymari; Jia, Weiyi; Wang, Yanyun; Santiago, Miguel; Liu, Huimin

    1998-01-01

    Trivalent europium ions are an important luminophore for lighting and display. The emission of (5)D0 to (7)F2 transition exhibits a red color at about 610 nm, which is very attractive and fulfills the requirement for most red-emitting phosphors including lamp and cathode ray phosphorescence materials. Various EU(3+) doped phosphors have been developed, and luminescence properties have been extensively studied. On the other hand, sol-gel technology has been well developed by chemists. In recent years, applications of this technology to optical materials have drawn a great attention. Sol-gel technology provides a unique way to obtain homogeneous composition distribution and uniform doping, and the processing temperature can be very low. In this work, EU(3+) doped SiO2 thin films and glasses were prepared by sol-gel technology and their spectroscopic properties were investigated.

  16. Electrochemical impedimetric sensor based on molecularly imprinted polymers/sol-gel chemistry for methidathion organophosphorous insecticide recognition.

    PubMed

    Bakas, Idriss; Hayat, Akhtar; Piletsky, Sergey; Piletska, Elena; Chehimi, Mohamed M; Noguer, Thierry; Rouillon, Régis

    2014-12-01

    We report here a novel method to detect methidathion organophosphorous insecticides. The sensing platform was architected by the combination of molecularly imprinted polymers and sol-gel technique on inexpensive, portable and disposable screen printed carbon electrodes. Electrochemical impedimetric detection technique was employed to perform the label free detection of the target analyte on the designed MIP/sol-gel integrated platform. The selection of the target specific monomer by electrochemical impedimetric methods was consistent with the results obtained by the computational modelling method. The prepared electrochemical MIP/sol-gel based sensor exhibited a high recognition capability toward methidathion, as well as a broad linear range and a low detection limit under the optimized conditions. Satisfactory results were also obtained for the methidathion determination in waste water samples.

  17. Spectrofluorimetric assessment of hydrochlorothiazide using optical sensor nano-composite terbium ion doped in sol-gel matrix.

    PubMed

    Youssef, A O

    2012-05-01

    A new, simple, sensitive and selective spectrofluorimetric method for the determination of Hydrochlorothiazide was developed in acetonitrile at pH 6.2. The Hydrochlorothiazide can remarkably enhance the luminescence intensity of the Tb(3+) ion doped in sol-gel matrix at λ(ex) = 370 nm. The intensity of the emission band of Tb(3+) ion doped in sol-gel matrix was increased due to the energy transfer from the triplet excited state of Hydrochlorothiazide to ((5)D(4)) excited energy state of Tb(3) ion. The enhancement of the emission band of Tb(3+) ion doped in sol-gel matrix at ((5)D(4)→(7)F(5)) 545 nm was directly proportion to the concentration of Hydrochlorothiazide with a dynamic ranges of 5.0 × 10(-10)-5.0 × 10(-6) mol L(-1) and detection limit of 2.2 × 10(-11) mol L(-1).

  18. Characterization of reactive ion etching of sol-gel SiO2 using Taguchi optimization method

    NASA Astrophysics Data System (ADS)

    Wee, Terence C.; Ooi, Boon Siew; Zhou, Yan; Chan, Yuen Chuen; Lam, Yee Loy

    1999-11-01

    SiO2 films prepared using sol-gel technique have found enormous potential applications in photonics, electronics and sensor devices. However, the feasibility of the devices utilizing sol-gel technology lies on the ease of the fabrication processes such as patterns transfer using wet or dry etchings. Dry etching is preferred over wet etching as it is able to produce finer features with high anisotropic etch profile. In this paper, we report the development of a dry reactive ion etching process for sol-gel SiO2 using a mixture of CF4 and O2 plasma. Parameters such as RF power, chamber pressure, CF4 and O2 flow rate, were optimized using a statistical method called Taguchi Technique. Etch rate of as high as 50nm/min, with high anisotropy etched profile, has been obtained.

  19. Dielectric Properties of Sol-Gel Derived Barium Strontium Titanate and Microwave Sintering of Ceramics

    NASA Astrophysics Data System (ADS)

    Selmi, Fathi A.

    This thesis consists of two areas of research: (1) sol-gel processing of Ba_{rm 1-x}Sr_{rm x} TiO_3 ceramics and their dielectric properties measurement; and (2) microwave versus conventional sintering of ceramics such as Al_2 O_3, Ba_{ rm 1-x}Sr_{rm x}TiO_3, Sb-doped SnO _2 and YBa_2Cu _3O_7. Sol-gel powders of BaTiO_3, SrTiO_3, and their solid solutions were synthesized by the hydrolysis of titanium isopropoxide and Ba and Sr methoxyethoxides. The loss tangent and dielectric constant of both sol-gel and conventionally prepared and sintered Ba_{rm 1-x}Sr _{rm x}TiO _3 ceramics were investigated at high frequencies. The sol-gel prepared ceramics showed higher dielectric constant and lower loss compared to those prepared conventionally. Ba _{rm 1-x}Sr _{rm x}TiO_3 ceramics were tunable with applied bias, indicating the potential use of this material for phase shifter applications. Porous Ba_{0.65}Sr _{0.35}TiO_3 was also investigated to lower the dielectric constant. Microwave sintering of alpha -Al_2O_3 and SrTiO_3 was investigated using an ordinary kitchen microwave oven (2.45 GHz; 600 Watts). The use of microwaves with good insulation of alpha -Al_2O_3 and SrTiO_3 samples resulted in their rapid sintering with good final densities of 96 and 98% of the theoretical density, respectively. A comparison of grain size for conventionally and microwave sintered SrTiO_3 samples did not show a noticeable difference. However, the grain size of microwave sintered alpha-Al_2O _3 was found to be larger than that of conventionally sintered sample. These results show that rapid sintering of ceramics can be achieved by using microwave radiation. The sintering behavior of coprecipitated Sb-doped SnO_2 was investigated using microwave power absorption. With microwave power, samples were sintered at 1450^circC for 20 minutes and showed a density as high as 99.9% of theoretical. However, samples fired in a conventional electric furnace at the same temperature for 4 hours showed only

  20. Citrate sol-gel route to high Tc superconducting YBaCuO fiber

    NASA Astrophysics Data System (ADS)

    Choy, Jin-Ho; Yoo, Jong-Seok; Park, Jung-Chul; Kang, Seong-Gu; Kim, Whan; Kang, Sang-Gu

    1991-12-01

    Drawing of the citrate gel fiber (diameter: 0.1∼2mm, length: ∞) was carried out within the pH range of 4.7∼6.1, which was theoretically estimated by considering the formation of ammine complexes in the solution. Single phase of YBa 2Cu 3O 7-δ(Tc off-set ≅ 85K) could only be obtained if the gel fiber was treated at 900°C, but the special care should be made because of the significant weight loss at 200°C and 300°C due to the decomposition of nitrates and organic constituents. Therefore, the heating rate should be lower than 1°C/min in these temperature range. From the SEM data, it was found that the fiber consisted of polycrystalline with very round graines(ø ∼ 1μm). The chemical composition was estimated as Y:Ba:Cu=1:2:3 by EPMA and the ratio of trivalent to divalent copper and the oxygen deficiency were determined as YBa 2Cu 3+0.62Cu 2+2.38O 6.81 by the redox titration.