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Sample records for high damage-threshold sol-gel

  1. Development of photonic crystals using sol-gel process for high power laser applications

    International Nuclear Information System (INIS)

    Benoit, Florence

    2015-01-01

    Three-dimensional photonic crystals (PCs) are periodic materials with a modulated refractive index on a length scale close to the light wavelength. This optical property allows the preparation of specific optical components like highly reflective mirrors. Moreover, these structured materials might have a high laser-induced damage threshold (LIDT) in the sub-nanosecond range compared to multilayered dielectric mirrors. This property is obtained because only one high LIDT material (silica) is used. In this work, we present the development of 3D PCs with narrow-sized colloidal silica particles, prepared by sol-gel process and deposited with Langmuir-Blodgett technique. Different syntheses routes have been investigated and compared regarding the optical properties of the PCs. A numerical model based on an ideal opal network including defect influence is used to explain these experimental results. (author) [fr

  2. Highly efficient solid-state neutron scintillators based on hybrid sol-gel nanocomposite materials

    International Nuclear Information System (INIS)

    Kesanli, Banu; Hong, Kunlun; Meyer, Kent; Im, Hee-Jung; Dai, Sheng

    2006-01-01

    This research highlights opportunities in the formulation of neutron scintillators that not only have high scintillation efficiencies but also can be readily cast into two-dimensional detectors. Series of transparent, crack-free monoliths were prepared from hybrid polystyrene-silica nanocomposites in the presence of arene-containing alkoxide precursor through room temperature sol-gel processing. The monoliths also contain lithium-6 salicylate as a target material for neutron-capture reactions and amphiphilic scintillator solution as a fluorescent sensitizer. Polystyrene was functionalized by trimethoxysilyl group in order to enable the covalent incorporation of aromatic functional groups into the inorganic sol-gel matrices for minimizing macroscopic phase segregation and facilitating lithium-6 doping in the sol-gel samples. Neutron and alpha responses of these hybrid polystyrene-silica monoliths were explored

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

    Science.gov (United States)

    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.

  4. High-power microcavity lasers based on highly erbium-doped sol-gel aluminosilicate glasses

    International Nuclear Information System (INIS)

    Le Ngoc Chung; Chu Thi Thu Ha; Nguyen Thu Trang; Pham Thu Nga; Pham Van Hoi; Bui Van Thien

    2006-01-01

    High-power whispering-gallery-mode (WGM) lasing from highly erbium-doped sol-gel aluminosilicate microsphere cavity coupled to a half-tapered optical fiber is presented. The lasing output power as high as 0.45 mW (-3.5 dBm) was obtained from sol-gel glass microsphere cavity with diameters in the range of 40-150 μm. The sol-gel method for making highly concentration Er-doped aluminosilicate glasses with Er-ion concentrations from 0.125 to 0.65 mol% of Er 3+ is described. Controlling collected lasing wavelength at each WGM is possible by adjusting the distance between the half-taper fiber and the microcavity and by diameter of the waist of half-taper fiber. Using the analytic formulas we calculated the TE and TM lasing modes and it is shown that the experimental results are in good agreement with the calculation prediction

  5. Radiation hardness of Ce-doped sol-gel silica fibers for high energy physics applications.

    Science.gov (United States)

    Cova, Francesca; Moretti, Federico; Fasoli, Mauro; Chiodini, Norberto; Pauwels, Kristof; Auffray, Etiennette; Lucchini, Marco Toliman; Baccaro, Stefania; Cemmi, Alessia; Bártová, Hana; Vedda, Anna

    2018-02-15

    The results of irradiation tests on Ce-doped sol-gel silica using x- and γ-rays up to 10 kGy are reported in order to investigate the radiation hardness of this material for high-energy physics applications. Sol-gel silica fibers with Ce concentrations of 0.0125 and 0.05 mol. % are characterized by means of optical absorption and attenuation length measurements before and after irradiation. The two different techniques give comparable results, evidencing the formation of a main broad radiation-induced absorption band, peaking at about 2.2 eV, related to radiation-induced color centers. The results are compared with those obtained on bulk silica. This study reveals that an improvement of the radiation hardness of Ce-doped silica fibers can be achieved by reducing Ce content inside the fiber core, paving the way for further material development.

  6. Tantala-based sol-gel coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Tran, MinhPhuong; Turner, Erica B; Segro, Scott S; Fang, Li; Seyyal, Emre; Malik, Abdul

    2017-11-03

    A sol-gel organic-inorganic hybrid sorbent, consisting of chemically integrated tantalum (V) ethoxide (TaEO) and polypropylene glycol methacrylate (PPGM), was developed for capillary microextraction (CME). The sol-gel sorbent was synthesized within a fused silica capillary through hydrolytic polycondensation of TaEO and chemical incorporation of PPGM into the evolving sol-gel tantala network. A part of the organic-inorganic hybrid sol-gel network evolving in the vicinity of the capillary walls had favorable conditions to get chemically bonded to the silanol groups on the capillary surface forming a surface-bonded coating. The newly developed sol-gel sorbent was employed to isolate and enrich a variety of analytes from aqueous samples for on-line analysis by high-performance liquid chromatography (HPLC) equipped with a UV detector. CME was performed on aqueous samples containing trace concentrations of analytes representing polycyclic aromatic hydrocarbons, ketones, alcohols, amines, nucleosides, and nucleotides. This sol-gel hybrid coating provided efficient extraction with CME-HPLC detection limits ranging from 4.41pM to 28.19 pM. Due to direct chemical bonding between the sol-gel sorbent coating and the fused silica capillary inner surface, this sol-gel sorbent exhibited enhanced solvent stability. The sol-gel tantala-based sorbent also exhibited excellent pH stability over a wide pH range (pH 0-pH 14). Furthermore, it displayed great performance reproducibility in CME-HPLC providing run-to-run HPLC peak area relative standard deviation (RSD) values between 0.23% and 3.83%. The capillary-to-capillary RSD (n=3), characterizing capillary preparation method reproducibility, ranged from 0.24% to 4.11%. The results show great performance consistency and application potential for the sol-gel tantala-PPGM sorbent in various fields including biomedical, pharmaceutical, and environmental areas. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Sol-gel preparation of Ag-silica nanocomposite with high electrical conductivity

    Science.gov (United States)

    Ma, Zhijun; Jiang, Yuwei; Xiao, Huisi; Jiang, Bofan; Zhang, Hao; Peng, Mingying; Dong, Guoping; Yu, Xiang; Yang, Jian

    2018-04-01

    Sol-gel derived noble-metal-silica nanocomposites are very useful in many applications. Due to relatively low price, higher conductivity, and higher chemical stability of silver (Ag) compared with copper (Cu), Ag-silica has gained much more research interest. However, it remains a significant challenge to realize high loading of Ag content in sol-gel Ag-silica composite with high structural controllability and nanoparticles' dispersity. Different from previous works by using multifunctional silicon alkoxide to anchor metal ions, here we report the synthesis of Ag-silica nanocomposite with high loading of Ag nanoparticles by employing acetonitrile bi-functionally as solvent and metal ions stabilizer. The electrical conductivity of the Ag-silica nanocomposite reached higher than 6800 S/cm. In addition, the Ag-silica nanocomposite could simultaneously possess high electrical conductivity and positive conductivity-temperature coefficient by properly controlling the loading content of Ag. Such behavior is potentially advantageous for high-temperature devices (like phosphoric acid fuel cells) and inhibiting the thermal-induced increase of devices' internal resistance. The strategy proposed here is also compatible with block-copolymer directed self-assembly of mesoporous material, spin-coating of film and electrospinning of nanofiber, making it more charming in various practical applications.

  8. High-Damage-Threshold Pinhole for Glass Fusion Laser Applications

    International Nuclear Information System (INIS)

    Kumit, N.A.; Letzring, S.A.; Johnson, R.P.

    1998-01-01

    We are investigating methods to fabricate high-damage-threshold spatial-filter pinholes that might not be susceptible to plasma closure for relatively high energies and long pulses. These are based on the observation that grazing-incidence reflection from glass can withstand in excess of 5 kJ/cm 2 (normal to the beam) without plasma formation. The high damage threshold results from both the cos q spreading of the energy across the surface and the reflection of a large fraction of the energy from the surface, thereby greatly reducing the field strength within the medium

  9. Low- and high-index sol-gel films for planar and channel-doped waveguides

    Science.gov (United States)

    Canva, Michael; Chaput, Frederic; Lahlil, Khalid; Rachet, Vincent; Goudket, Helene; Boilot, Jean-Pierre; Levy, Yves

    2001-11-01

    In view of realizing integrated optic components based on effects such as electro-optic, chi(2):chi(2) cascading, stimulated emission,... one has to first synthesize materials with the proper functionality; this may be achieved by doping solid state matrices by the appropriate organic chromophores. Second, and as important, these materials have to be properly structured into the final optical guiding structures. We shall report on issues related to the realization of chromophore-doped planar waveguides as well as channel waveguides. These structures were realized by either photo-transformation such as photo- chromism and photo-bleaching or reactive ion etching technique, starting with chromophore doped sol-gel materials at high loading contents for which optical index may be controlled via the local dopant concentration. With these materials and techniques, waveguides and components characterized by propagation losses of the order of a cm-1, measured off the edge of the absorption band of the doping species, were fabricated. In order to be also able to study and use waveguide functionalized with low concentration of chromophore species, we developed new sol-gel materials of high optical index, yet low temperature processed. These new films are under study to evaluate their potential as host for organic doped waveguides devices.

  10. Sol-gel preparation of high surface area potassium tetratitanate for the immobilization of nuclear waste metal ions

    International Nuclear Information System (INIS)

    Jung, K.T.; Shul, Y.G.; Moon, J.K.; Oh, W.J.

    1997-01-01

    Potassium tetratinates(K 2 Ti 4 O 9 ) were synthesized by using the sol-gel method to produce ion-exchangeable materials with high surface area. The effects of mole ratios of K/Ti and H 2 O/Ti were examined. K 2 Ti 4 O 9 was obtained at 740 deg. C by the sol-gel method, which uses a lower temperature than the melting method. After calcination at 800 deg. C, K 2 Ti 4 O exhibits a needle shape which is quite different from the shape of K 2 Ti 6 O 13 powder. The surface areas of K 2 Ti 4 O 9 was 15 m 2 /g by the sol-gel method after calcining at 800 C. The enhancement of BET area to 25 m 2 /g was obtained after supercritical drying using EtOH as solvent. By using the sodium alginate method, needle type potassium titanate 10μm in length, the longest aspect ratio of 1,3 x 10 3 could be obtained. There are variations in the Sr 2+ ion exchange rate and capacity according to the preparation method. Larger BET surface area provides fast ion exchange and larger capacity for Sr 2+ ion in the order; sol-gel process with supercritical drying > sol-gel process > melting process. (author). 17 refs, 21 figs, 1 tab

  11. Development of highly-ordered, ferroelectric inverse opal films using sol gel infiltration

    Science.gov (United States)

    Matsuura, N.; Yang, S.; Sun, P.; Ruda, H. E.

    2005-07-01

    Highly-ordered, ferroelectric, Pb-doped Ba0.7Sr0.3TiO3, inverse opal films were fabricated by spin-coating a sol gel precursor into a polystyrene artificial opal template followed by heat treatment. Thin films of the ferroelectric were independently studied and were shown to exhibit good dielectric properties and high refractive indices. The excellent quality of the final inverse opal film using this spin-coating infiltration method was confirmed by scanning electron microscopy images and the good correspondence between optical reflection data and theoretical simulations. Using this method, the structural and material parameters of the final ferroelectric inverse opal film were easily adjusted by template heating and through repeated infiltrations, without changes in the initial template or precursor. Also, crack-free inverse opal thin films were fabricated over areas comparable to that of the initial crack-free polystyrene template (˜100 by 100 μm2).

  12. A novel tantalum-based sol-gel packed microextraction syringe for highly specific enrichment of phosphopeptides in MALDI-MS applications.

    Science.gov (United States)

    Çelikbıçak, Ömür; Atakay, Mehmet; Güler, Ülkü; Salih, Bekir

    2013-08-07

    A new tantalum-based sol-gel material was synthesized using a unique sol-gel synthesis pathway by PEG incorporation into the sol-gel structure without performing a calcination step. This improved its chemical and physical properties for the high capacity and selective enrichment of phosphopeptides from protein digests in complex biological media. The specificity of the tantalum-based sol-gel material for phosphopeptides was evaluated and compared with tantalum(V) oxide (Ta2O5) in different phosphopeptide enrichment applications. The tantalum-based sol-gel and tantalum(V) oxide were characterized in detail using FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM), and also using a surface area and pore size analyzer. In the characterization studies, the surface morphology, pore volume, crystallinity of the materials and PEG incorporation into the sol-gel structure to produce a more hydrophilic material were successfully demonstrated. The X-ray diffractograms of the two different materials were compared and it was noted that the broad signals of the tantalum-based sol-gel clearly represented the amorphous structure of the sol-gel material, which was more likely to create enough surface area and to provide more accessible tantalum atoms for phosphopeptides to be easily adsorbed when compared with the neat and more crystalline structure of Ta2O5. Therefore, the phosphopeptide enrichment performance of the tantalum-based sol-gels was found to be remarkably higher than the more crystalline Ta2O5 in our studies. Phosphopeptides at femtomole levels could be selectively enriched using the tantalum-based sol-gel and detected with a higher signal-to-noise ratio by matrix-assisted laser desorption/ionization-mass spectrometer (MALDI-MS). Moreover, phosphopeptides in a tryptic digest of non-fat bovine milk as a complex real-world biological sample were retained with higher yield using a tantalum-based sol-gel. Additionally, the sol-gel material

  13. High dose thermoluminescence dosimetry performance of Sol-gel synthesized TiO{sub 2} phosphors

    Energy Technology Data Exchange (ETDEWEB)

    Salas J, Ch. J.; Cruz V, C. [Universidad de Sonora, Departamento de Investigacion en Polimeros y Materiales, Apdo. Postal 130, 83000 Hermosillo, Sonora (Mexico); Castillo U, D. M.; Flores M, K. [Universidad de Sonora, Departamento de Ciencias Quimico Biologicas, Apdo. Postal 130, 83000 Hermosillo, Sonora (Mexico); Bernal, R. [Universidad de Sonora, Departamento de Investigacion en Fisica, Apdo. Postal 5-088, 83190 Hermosillo, Sonora (Mexico); Castano, V. M., E-mail: castillouzeta@gmail.com [UNAM, Instituto de Fisica, Centro de Fisica Aplicada y Tecnologia Avanzada, Apdo. Postal 1-1010, Queretaro, Qro. (Mexico)

    2015-10-15

    Full text: TiO{sub 2} is a ceramic material with many applications due to their different crystalline phases (rutile, anatase and brookite). It has attracted attention in several fields because their high mechanical strength, chemical stability and ion-conducting properties. Moreover, in recent years, some research groups gained interest in the thermoluminescence features of TiO{sub 2} concerning their potential use as thermoluminescence dosimeter. In this work, we present experimental results obtained in the first stage of a long-term research project focused in the synthesis of TiO{sub 2} phosphors for dosimetric applications. The thermoluminescent characterization of samples was carried out after being exposed to beta particle irradiation. TiO{sub 2} was prepared by alkoxide sol-gel route using titanium tetrabutoxide as precursor, ethanol, water and ammonia as catalyst. Pellet-shaped samples were annealed at 700 degrees C for 6 h in air atmosphere followed by slow cooling, and then were exposed to radiation doses from 25 to 400 Gy. The glow curves display maxima located at 103 and 238 degrees C when a 5 C/s heating rate is used. From the experimental results here presented, we conclude that TiO{sub 2} is a promising material to develop high dose Tl dosimeters. (Author)

  14. Synthesis and studies of Y-Ba-Cu-O high temperature superconductor prepared by sol-gel method

    International Nuclear Information System (INIS)

    Grigoryan, S.G.; Manukyan, A.L.; Hayrapetyan, A.G.; Arzumanyan, A.M.; Rashidyan, L.H.; Mkrtichyan, N.Y.; Mkrtchyan, A.A.; Kurginyan, K.A.; Trozyan, A.H.; Vardanyan, R.S.

    2004-01-01

    The method of preparation of Y-Ba-Cu-O high temperature superconducting materials by sol-gel processing technique both for powders and thin films are described. All these methods are based on using yttrium alkoxides as precursors, which are not ready available reagents, besides the majority of these methods use copper alkoxides, which show low solubility in organic solvents, moreover they are very sensitive to hydrolysis in air. The new method of preparation of Y-Ba-Cu-O ceramic materials by sol-gel processing technique based on new and convenient precursors stable in air, having high compatibility with each other is offered. Basic scientific and technological issues related to the synthesis of bulk materials, their structure and electrical conductivity are discussed

  15. Highly stable and imperceptible electronics utilizing photoactivated heterogeneous sol-gel metal-oxide dielectrics and semiconductors.

    Science.gov (United States)

    Jo, Jeong-Wan; Kim, Jaekyun; Kim, Kyung-Tae; Kang, Jin-Gu; Kim, Myung-Gil; Kim, Kwang-Ho; Ko, Hyungduk; Kim, Jiwan; Kim, Yong-Hoon; Park, Sung Kyu

    2015-02-18

    Incorporation of Zr into an AlOx matrix generates an intrinsically activated ZAO surface enabling the formation of a stable semiconducting IGZO film and good interfacial properties. Photochemically annealed metal-oxide devices and circuits with the optimized sol-gel ZAO dielectric and IGZO semiconductor layers demonstrate the high performance and electrically/mechanically stable operation of flexible electronics fabricated via a low-temperature solution process. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Sol-gel technology applied to alternative high-level waste forms development

    International Nuclear Information System (INIS)

    Angelini, P.; Stinton, D.P.; Vavruska, J.S.; Caputo, A.J.; Lackey, W.J.

    1981-01-01

    Sol-gel technology appears applicable to waste solidification. It is attractive for remote operation, and a variety of waste compositions and forms can be produced. Spheres and pellets of gel-derived Synroc waste forms were produced. Spheres of the Synroc-B type were coated with pyrolytic carbon and silicon carbide. Partitioning of actinides in Synroc-B was experimentally determined

  17. Fluorescent silica hybrid materials containing benzimidazole dyes obtained by sol-gel method and high pressure processing

    International Nuclear Information System (INIS)

    Hoffmann, Helena Sofia; Stefani, Valter; Benvenutti, Edilson Valmir; Costa, Tania Maria Haas; Gallas, Marcia Russman

    2011-01-01

    Research highlights: → Sol-gel technique was used to obtain silica based hybrid materials containing benzimidazole dyes. → The sol-gel catalysts, HF and NaF, produce xerogels with different optical and textural characteristics. → High pressure technique (6.0 GPa) was used to produce fluorescent and transparent silica compacts with the dyes entrapped in closed pores, maintaining their optical properties. → The excited state intramolecular proton transfer (ESIPT) mechanism of benzimidazole dyes was studied by steady-state fluorescence spectroscopy for the monoliths, powders, and compacts. - Abstract: New silica hybrid materials were obtained by incorporation of two benzimidazole dyes in the silica network by sol-gel technique, using tetraethylorthosilicate (TEOS) as inorganic precursor. Several syntheses were performed with two catalysts (HF and NaF) producing powders and monoliths with different characteristics. The dye 2-(2'-hydroxy-5'-aminophenyl)benzimidazole was dispersed and physically adsorbed in the matrix, and the dye 2'(5'-N-(3-triethoxysilyl)propylurea-2'-hydroxyphenyl)benzimidazole was silylated, becoming chemically bonded to the silica network. High pressure technique was used to produce fluorescent and transparent silica compacts with the silylated and incorporated dye, at 6.0 GPa and room temperature. The excited state intramolecular proton transfer (ESIPT) mechanism of benzimidazole dyes was studied by steady-state fluorescence spectroscopy for the monoliths, powders, and compacts. The influence of the syntheses conditions was investigated by textural analysis using nitrogen adsorption isotherms.

  18. Fast Processing of Sol-Gel TCO

    NARCIS (Netherlands)

    Deelen, J. van; Rem, M.; Arfsten, N.; Buskens, P.P.

    2016-01-01

    TCOs are usually deposited using sputtering or chemical vapor deposition, which have a yield of typically 50-75%. The sol gel method does not need low pressure and can be done with a high precursor yield in the range of 90 – 100%. Sol gel enables also the TCO function as a planarization or

  19. Highly sensitive determination of hydroxylamine using fused gold nanoparticles immobilized on sol-gel film modified gold electrode

    Energy Technology Data Exchange (ETDEWEB)

    Kannan, P. [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul, Tamilnadu (India); John, S. Abraham, E-mail: abrajohn@yahoo.co.in [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul, Tamilnadu (India)

    2010-03-24

    We are reporting the highly sensitive determination of hydroxylamine (HA) using 2-mercapto-4-methyl-5-thiazoleacetic acid (TAA) capped fused spherical gold nanoparticles (AuNPs) modified Au electrode. The fused TAA-AuNPs were immobilized on (3-mercaptopropyl)-trimethoxysilane (MPTS) sol-gel film, which was pre-assembled on Au electrode. The immobilization of fused TAA-AuNPs on MPTS sol-gel film was confirmed by UV-vis absorption spectroscopy and atomic force microscopy (AFM). The AFM image showed that the AuNPs retained the fused spherical morphology after immobilized on sol-gel film. The fused TAA-AuNPs on MPTS modified Au electrode were used for the determination of HA in phosphate buffer (PB) solution (pH = 7.2). When compared to bare Au electrode, the fused AuNPs modified electrode not only shifted the oxidation potential of HA towards less positive potential but also enhanced its oxidation peak current. Further, the oxidation of HA was highly stable at fused AuNPs modified electrode. Using amperometric method, determination of 17.5 nM HA was achieved for the first time. Further, the current response of HA increases linearly while increasing its concentration from 17.5 nM to 22 mM and a detection limit was found to be 0.39 nM (S/N = 3). The present modified electrode was also successfully used for the determination of 17.5 nM HA in the presence of 200-fold excess of common interferents such as urea, NO{sub 2}{sup -}, NH{sub 4}{sup +}, oxalate, Mn{sup 2+}, Na{sup +}, K{sup +}, Mg{sup 2+}, Ca{sup 2+}, Ba{sup 2+} and Cu{sup 2+}. The practical application of the present modified electrode was demonstrated by measuring the concentration of HA in ground water samples.

  20. Applications of sol gel ceramic coatings

    International Nuclear Information System (INIS)

    Barrow, D.

    1996-01-01

    The sol gel method is a chemical technique in which polycrystalline ceramic films are fabricated from a solution of organometallic precursors. The technique is attractive for many industrial applications because it is a simple (films are processed in air), flexible (can be used to coat complex geometries) and cost effective (does not require expensive equipment) process. In addition, dense, high quality coatings can be achieved at much lower temperatures than is generally required for sintering bulk ceramics. In this paper the conventional sol gel method and the new datec process are reviewed and potential applications of sol gel coatings in automotive, aerospace, petrochemical, nuclear and electronic industries are discussed. (orig.)

  1. Optical Fiber Chemical Sensor with Sol-Gel Derived Refractive Material as Transducer for High Temperature Gas Sensing in Clean Coal Technology

    Energy Technology Data Exchange (ETDEWEB)

    Shiquan Tao

    2006-12-31

    The chemistry of sol-gel derived silica and refractive metal oxide has been systematically studied. Sol-gel processes have been developed for preparing porous silica and semiconductor metal oxide materials. Micelle/reversed micelle techniques have been developed for preparing nanometer sized semiconductor metal oxides and noble metal particles. Techniques for doping metal ions, metal oxides and nanosized metal particles into porous sol-gel material have also been developed. Optical properties of sol-gel derived materials in ambient and high temperature gases have been studied by using fiber optic spectroscopic techniques, such as fiber optic ultraviolet/visible absorption spectrometry, fiber optic near infrared absorption spectrometry and fiber optic fluorescence spectrometry. Fiber optic spectrometric techniques have been developed for investigating the optical properties of these sol-gel derived materials prepared as porous optical fibers or as coatings on the surface of silica optical fibers. Optical and electron microscopic techniques have been used to observe the microstructure, such as pore size, pore shape, sensing agent distribution, of sol-gel derived material, as well as the size and morphology of nanometer metal particle doped in sol-gel derived porous silica, the nature of coating of sol-gel derived materials on silica optical fiber surface. In addition, the chemical reactions of metal ion, nanostructured semiconductor metal oxides and nanometer sized metal particles with gas components at room temperature and high temperatures have also been investigated with fiber optic spectrometric methods. Three classes of fiber optic sensors have been developed based on the thorough investigation of sol-gel chemistry and sol-gel derived materials. The first group of fiber optic sensors uses porous silica optical fibers doped with metal ions or metal oxide as transducers for sensing trace NH{sub 3} and H{sub 2}S in high temperature gas samples. The second group of

  2. High Refractive Organic–Inorganic Hybrid Films Prepared by Low Water Sol-Gel and UV-Irradiation Processes

    Directory of Open Access Journals (Sweden)

    Hsiao-Yuan Ma

    2016-03-01

    Full Text Available Organic-inorganic hybrid sols (Ti–O–Si precursor were first synthesized by the sol-gel method at low addition of water, and were then employed to prepare a highly refractive hybrid optical film. This film was obtained by blending the Ti–O–Si precursor with 2-phenylphenoxyethyl acrylate (OPPEA to perform photo-polymerization by ultraviolet (UV irradiation. Results show that the film transparency of poly(Ti–O–Si precursor-co-OPPEA film is higher than that of a pure poly(Ti–O–Si precursor film, and that this poly(Ti–O–Si precursor-co-OPPEA hybrid film exhibits a high transparency of ~93.7% coupled with a high refractive index (n of 1.83 corresponding to a thickness of 2.59 μm.

  3. Optimizing sol-gel infiltration for the fabrication of high-quality titania inverse opal and its photocatalytic activity

    International Nuclear Information System (INIS)

    Liu Weijie; Zou Bo; Zhao Jing; Cui Haining

    2010-01-01

    This article reports an optimized sol-gel opal infiltration technique for the fabrication of high-quality titania inverse opal. Different from previous reports, the presently proposed method is facile, efficient and suitable for other inorganic oxide. We have compared two different infiltration strategies and their influences on the structure, photonic properties and photocatalytic activity. The obtained titania inverse opal displays excellent photonic properties with photonic band gap at 320 nm and better photocatalytic effect, which is attributed to its high-quality inverse opal nanostructure. Reproducibility tests prove that the photocatalytic activity of the resultant titania inverse opal remains intact even after five repeated photocatalytic reactions under the same procedure and experimental conditions.

  4. Large-aperture, high-damage-threshold optics for beamlet

    International Nuclear Information System (INIS)

    Campbell, J.H.; Atherton, L.J.; DeYoreo, J.J.; Kozlowski, M.R.; Maney, R.T.; Montesanti, R.C.; Sheehan, L.M.; Barker, C.E.

    1995-01-01

    Beamlet serves as a test bed for the proposed NIF laser design and components. Therefore, its optics are similar in size and quality to those proposed for the NIF. In general, the optics in the main laser cavity and transport section of Beamlet are larger and have higher damage thresholds than the optics manufactured for any of our previous laser systems. In addition, the quality of the Beamlet optical materials is higher, leading to better wavefront quality, higher optical transmission, and lower-intensity modulation of the output laser beam than, for example, that typically achieved on Nova. In this article, we discuss the properties and characteristics of the large-aperture optics used on Beamlet

  5. Robust optimization of the laser induced damage threshold of dielectric mirrors for high power lasers.

    Science.gov (United States)

    Chorel, Marine; Lanternier, Thomas; Lavastre, Éric; Bonod, Nicolas; Bousquet, Bruno; Néauport, Jérôme

    2018-04-30

    We report on a numerical optimization of the laser induced damage threshold of multi-dielectric high reflection mirrors in the sub-picosecond regime. We highlight the interplay between the electric field distribution, refractive index and intrinsic laser induced damage threshold of the materials on the overall laser induced damage threshold (LIDT) of the multilayer. We describe an optimization method of the multilayer that minimizes the field enhancement in high refractive index materials while preserving a near perfect reflectivity. This method yields a significant improvement of the damage resistance since a maximum increase of 40% can be achieved on the overall LIDT of the multilayer.

  6. A copper ion-selective electrode with high selectivity prepared by sol-gel and coated wire techniques.

    Science.gov (United States)

    Mazloum Ardakani, M; Salavati-Niasari, M; Khayat Kashani, M; Ghoreishi, S M

    2004-03-01

    A sol-gel electrode and a coated wire ion-selective poly(vinyl chloride) membrane, based on thiosemicarbazone as a neutral carrier, were successfully developed for the detection of Cu (II) in aqueous solutions. The sol-gel electrode and coated electrode exhibited linear response with Nernstian slopes of 29.2 and 28.1 mV per decade respectively, within the copper ion concentration ranges 1.0 x 10(-5) - 1.0 x 10(-1) M and 6.0 x 10(-6) - 1.0 x 10(-1) M for coated and sol-gel sensors. The coated and sol-gel electrodes show detection limits of 3.0 x 10(-6) and 6.0 x 10(-6) M respectively. The electrodes exhibited good selectivities for a number of alkali, alkaline earth, transition and heavy metal ions. The proposed electrodes have response times ranging from 10-50 s to achieve a 95% steady potential for Cu2+ concentration. The electrodes are suitable for use in aqueous solutions over a wide pH range (4-7.5). Applications of these electrodes for the determination of copper in real samples, and as an indicator electrode for potentiometric titration of Cu2+ ion using EDTA, are reported. The lifetimes of the electrodes were tested over a period of six months to investigate their stability. No significant change in the performance of the sol-gel electrode was observed over this period, but after two months the coated wire copper-selective electrode exhibited a gradual decrease in the slope. The selectivity of the sol-gel electrode was found to be better than that of the coated wire copper-selective electrode. Based on these results, a novel sol-gel copper-selective electrode is proposed for the determination of copper, and applied to real sample assays.

  7. Effect of UV-irradiation on sol-gel optical films

    International Nuclear Information System (INIS)

    Yang Fan; Shen Jun; Zhou Bin; Wu Guangming; Luo Aiyun; Sun Qi

    2005-01-01

    Sol-gel optical films were deposited on K9 glass and silicon wafer substrates by spin-coating method and a high-pressure mercury lamp was used to perform ultraviolet treating to solidify these films and improve their performance. SEM, AFM, IR and ellipsometer were used to characterize the structure and optical properties of the films. Mechanical property of films was measured by pencil hardness-testing device. Laser damage threshold of films was measured by a Q-switched Nd:YAG high power laser with the wave length of 1064 nm and the pulse width of 15 ns. The results show that UV-irradiation can improve the mechanical property and increase the refractive index of the films. Besides, the nodules on the surface of the films can be changed into pits by UV-irradiation process, so the laser damage threshold of sol-gel thin films will be increased. After UV-irradiation the laser damage threshold of single-layer ZrO 2 film reached 50.6 J/cm 2 (1064 nm, 1 ns). It is found that UV-irradiation is an effective method to avoid the infiltrating between the layers, and the degree of homogeneity of the multilayer films can be improved by this way. (authors)

  8. Thoria sol-gel processes

    International Nuclear Information System (INIS)

    Matthews, R.B.

    1978-10-01

    Alternate fuel fabrication techniques are being developed at WNRE as part of the thorium fuel cycle program. The sol-gel techniques are attractive and this report assembles and summarizes information relating to thoria sol-gel fuels. Some background information on the behaviour and advantages of sol-gel fuel forms is presented, followed by a review of relevant colloid chemistry and an explanation of the fundamental steps of sol-gel processes. Finally, several variants to the basic process are reviewed and evaluated. (author)

  9. Highly transparent ITO thin films on photosensitive glass: sol-gel synthesis, structure, morphology and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Koroesi, Laszlo; Papp, Szilvia; Dekany, Imre [University of Szeged, Supramolecular and Nanostructured Materials Research Group of the Hungarian Academy of Sciences, Szeged (Hungary); Beke, Szabolcs [Italian Institute of Technology, Department of Nanophysics, Genova (Italy); Pecz, Bela; Horvath, Robert; Petrik, Peter; Agocs, Emil [Research Institute for Technical Physics and Materials Science, Budapest (Hungary)

    2012-05-15

    Conductive and highly transparent indium tin oxide (ITO) thin films were prepared on photosensitive glass substrates by the combination of sol-gel and spin-coating techniques. First, the substrates were coated with amorphous Sn-doped indium hydroxide, and these amorphous films were then calcined at 550 {sup circle} C to produce crystalline and electrically conductive ITO layers. The resulting thin films were characterized by means of scanning electron microscopy, UV-Vis spectroscopy, X-ray photoelectron spectroscopy and spectroscopic ellipsometry. The measurements revealed that the ITO films were composed of spherical crystallites around 20 nm in size with mainly cubic crystal structure. The ITO films acted as antireflection coatings increasing the transparency of the coated substrates compared to that of the bare supports. The developed ITO films with a thickness of {proportional_to}170-330 nm were highly transparent in the visible spectrum with sheet resistances of 4.0-13.7 k{omega}/sq. By coating photosensitive glass with ITO films, our results open up new perspectives in micro- and nano-technology, for example in fabricating conductive and highly transparent 3D microreactors. (orig.)

  10. Preparation of highly hydrophobic cotton fabrics by modification with bifunctional silsesquioxanes in the sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Przybylak, Marcin, E-mail: marcin.przybylak@ppnt.poznan.pl [Poznań Science and Technology Park, Adam Mickiewicz University Foundation, Rubież 46, 61-612 Poznań (Poland); Maciejewski, Hieronim, E-mail: maciejm@amu.edu.pl [Poznań Science and Technology Park, Adam Mickiewicz University Foundation, Rubież 46, 61-612 Poznań (Poland); Faculty of Chemistry, Adam Mickiewicz University, Umultowska 89b, 61-614 Poznań (Poland); Dutkiewicz, Agnieszka, E-mail: agdut@interia.pl [Poznań Science and Technology Park, Adam Mickiewicz University Foundation, Rubież 46, 61-612 Poznań (Poland)

    2016-11-30

    Highlights: • Fabric hydrophobization process using bifunctional silsesquioxanes was studied. • Superhydrophobic fabric was produced using fluorofunctional silsesquioxanes. • Surface of modified fabrics was analyzed using different techniques. - Abstract: The surface modification of cotton fabrics was carried out using two types of bifunctional fluorinated silsesquioxanes with different ratios of functional groups. The modification was performed either by one- or two-step process. Two methods, the sol-gel and the dip coating method were used in different configurations. The heat treatment and the washing process were applied after modification. The wettability of cotton fabric was evaluated by measuring water contact angles (WCA). Changes in the surface morphology were examined by scanning electron microscopy (SEM, SEM-LFD) and atomic force microscopy (AFM). Moreover, the modified fabrics were subjected to analysis of elemental composition of the applied coatings using SEM-EDS techniques. Highly hydrophobic textiles were obtained in all cases studied and one of the modifications resulted in imparting superhydrophobic properties. Most of impregnated textiles remained hydrophobic even after multiple washing process which shows that the studied modification is durable.

  11. Influence of calcination temperature on sol-gel synthesized single-phase bismuth titanate for high dielectric capacitor applications

    Energy Technology Data Exchange (ETDEWEB)

    Thiruramanathan, Pandirengan; Marikani, Arumugam [Mepco Schlenk Engineering College, Tamil Nadu (India). Dept. of Physics; Madhavan, Durairaj [Mepco Schlenk Engineering College, Tamil Nadu (India). Dept. of Chemistry; Bharadwaj, Suresh; Awasthi, Anand Mohan [UGC-DAE Consortium for Scientific Research, Indore (India). Thermodynamics Lab.

    2016-05-15

    An inexpensive sol-gel combustion method using citric acid as fuel has been used to synthesize bismuth titanate, Bi{sub 4}Ti{sub 3}O{sub 12} nanopowders. Thermogravimetric analysis proved that a calcination temperature of 900 C is sufficient for the preparation of single-phase bismuth titanate. X-ray diffraction and Fourier transform infrared spectroscopy are used to examine the influence of calcination temperature on the structural growth of the Bi{sub 4}Ti{sub 3}O{sub 12} nanopowder. The average crystallite size estimated by using the Scherrer method and the Williamson-Hall method was found to increase with calcination temperature. Photoluminescence behavior as a function of calcination temperature was observed at two different excitation wavelengths of 300 nm and 420 nm. The morphology of the particles analyzed using images obtained from field emission scanning electron microscopy displayed irregular, random sized, and spherical-shaped structures. The stoichiometry and purity of the nanopowder are confirmed by energy-dispersive spectroscopy. The broadband dielectric results established the highest dielectric constant (ε{sub r} = 450) for a frequency of 100 Hz achieved with a potential capacitance of 138 pF m{sup -2}. This establishes Bi{sub 4}Ti{sub 3}O{sub 12} as a promising dielectric material for achieving high energy density capacitors for the next-generation passive devices.

  12. Effect of ionizing radiation on nanocomposites of high density polyethylene with pseudoboehmite obtained by sol-gel process

    International Nuclear Information System (INIS)

    Miranda, Leila F.; Munhoz Junior, Antonio H.; Terence, Mauro C.; Alves, Alexandre P.

    2009-01-01

    Nanocomposites are polymeric hybrid materials where inorganic substances of nanometric dimensions are dispersed in a polymeric matrix. The fillers present area of raised surface, promoting better dispersion in the polymeric matrix and therefore an improvement of the physical properties of the composite that depends on the homogeneity of the material. The nanocomposites preparation with polymeric matrix allows in many cases to find a relation enters a low cost, due to the use of minor amount of filler, and a raised performance level. Nanocomposites were obtained with pseudoboehmite synthesized by sol-gel process and high density polyethylene with different concentrations of pseudoboehmite. The aim of this work was to study the effects of ionizing radiation on the properties of the nanocomposites obtained. The nanocomposites were prepared by melt intercalation technique and subsequently, the samples were molded by injection, irradiated and submitted to thermal and mechanical tests. The mechanical properties (impact strength and tensile strength), temperature of thermal distortion (HDT) and Vicat softening temperature of the non irradiated and irradiated nanocomposites were determined. The irradiation doses were of 30, 50 and 100kGy in a gamma cell. The results showed an increase in the values of tensile strength; a decrease in the impact strength and an increase in the temperature of thermal distortion (HDT) evidencing the interaction of nanofiller with the polymeric matrix. (author)

  13. High Cycling Performance Cathode Material: Interconnected LiFePO4/Carbon Nanoparticles Fabricated by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Zhigao Yang

    2014-01-01

    Full Text Available Interconnected LiFePO4/carbon nanoparticles for Li-ion battery cathode have been fabricated by sol-gel method followed by a carbon coating process involving redox reactions. The carbon layers coated on the LiFePO4 nanoparticles not only served as a protection layer but also supplied fast electrons by building a 3D conductive network. As a cooperation, LiFePO4 nanoparticles encapsulated in interconnected conductive carbon layers provided the electrode reactions with fast lithium ions by offering the lithium ions shortening and unobstructed pathways. Field emission scanning electron microscopy (FESEM and X-ray diffraction (XRD tests showed optimized morphology. Electrochemical characterizations including galvanostatic charge/discharge, cyclic voltammetry (CV, and electrochemical impedance spectroscopy (EIS tests, together with impedance parameters calculated, all indicated better electrochemical performance and excellent cycling performance at high rate (with less than 9.5% discharge capacity loss over 2000 cycles, the coulombic efficiency maintained about 100%.

  14. Barium zirconate-titanate/barium calcium-titanate ceramics via sol-gel process: novel high-energy-density capacitors

    International Nuclear Information System (INIS)

    Puli, Venkata Sreenivas; Kumar, Ashok; Scott, J F; Katiyar, Ram S; Chrisey, Douglas B; Tomozawa, M

    2011-01-01

    Lead-free barium zirconate-titanate/barium calcium-titanate, [(BaZr 0.2 Ti 0.80 )O 3 ] 1-x -[(Ba 0.70 Ca 0.30 )TiO 3 ] x (x = 0.10, 0.15, 0.20) (BZT-BCT) ceramics with high dielectric constant, low dielectric loss and moderate electric breakdown field were prepared by the sol-gel synthesis technique. X-ray diffraction patterns revealed tetragonal crystal structure and this was further confirmed by Raman spectra. Well-behaved ferroelectric hysteresis loops and moderate polarizations (spontaneous polarization, P s ∼ 3-6 μC cm -2 ) were obtained in these BZT-BCT ceramics. Frequency-dependent dielectric spectra confirmed that ferroelectric diffuse phase transition (DPT) exists near room temperature. Scanning electron microscope images revealed monolithic grain growth in samples sintered at 1280 deg. C. 1000/ε versus (T) plots revealed ferroelectric DPT behaviour with estimated γ values of ∼1.52, 1.51 and 1.88, respectively, for the studied BZT-BCT compositions. All three compositions showed packing-limited breakdown fields of ∼47-73 kV cm -1 with an energy density of 0.05-0.6 J cm -3 for thick ceramics (>1 mm). Therefore these compositions might be useful in Y5V-type capacitor applications.

  15. Barium zirconate-titanate/barium calcium-titanate ceramics via sol-gel process: novel high-energy-density capacitors

    Energy Technology Data Exchange (ETDEWEB)

    Puli, Venkata Sreenivas; Kumar, Ashok; Scott, J F; Katiyar, Ram S [SPECLAB, Department of Physics, University of Puerto Rico, San Juan, PR 00936 (Puerto Rico); Chrisey, Douglas B; Tomozawa, M, E-mail: rkatiyar@uprrp.edu [Department of Materials Science and Engineering, Rensselaer Polytechnic Institute, Troy, NY 12180-3590 (United States)

    2011-10-05

    Lead-free barium zirconate-titanate/barium calcium-titanate, [(BaZr{sub 0.2}Ti{sub 0.80})O{sub 3}]{sub 1-x}-[(Ba{sub 0.70}Ca{sub 0.30})TiO{sub 3}]{sub x} (x = 0.10, 0.15, 0.20) (BZT-BCT) ceramics with high dielectric constant, low dielectric loss and moderate electric breakdown field were prepared by the sol-gel synthesis technique. X-ray diffraction patterns revealed tetragonal crystal structure and this was further confirmed by Raman spectra. Well-behaved ferroelectric hysteresis loops and moderate polarizations (spontaneous polarization, P{sub s} {approx} 3-6 {mu}C cm{sup -2}) were obtained in these BZT-BCT ceramics. Frequency-dependent dielectric spectra confirmed that ferroelectric diffuse phase transition (DPT) exists near room temperature. Scanning electron microscope images revealed monolithic grain growth in samples sintered at 1280 deg. C. 1000/{epsilon} versus (T) plots revealed ferroelectric DPT behaviour with estimated {gamma} values of {approx}1.52, 1.51 and 1.88, respectively, for the studied BZT-BCT compositions. All three compositions showed packing-limited breakdown fields of {approx}47-73 kV cm{sup -1} with an energy density of 0.05-0.6 J cm{sup -3} for thick ceramics (>1 mm). Therefore these compositions might be useful in Y5V-type capacitor applications.

  16. Urea functionalized surface-bonded sol-gel coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

    Science.gov (United States)

    Jillani, Shehzada Muhammad Sajid; Alhooshani, Khalid

    2018-03-30

    Sol-gel urea functionalized-[bis(hydroxyethyl)amine] terminated polydimethylsiloxane coating was developed for capillary microextraction-high performance liquid chromatographic analysis from aqueous samples. A fused silica capillary is coated from the inside with surface bonded coating material and is created through in-situ sol-gel reaction. The urea-functionalized coating was immobilized to the inner surface of the capillary by the condensation reaction of silanol groups of capillary and sol-solution. The characterization of the coating material was successfully done by using X-ray photoelectron spectroscopy, thermogravimetric analysis, field emission scanning electron microscope, and energy dispersive X-ray spectrometer. To make a setup of online capillary microextraction-high performance liquid chromatography, the urea functionalized capillary was installed in the HPLC manual injection port. The analytes of interest were pre-concentrated in the coated sampling loop, desorbed by the mobile phase, chromatographically separated on C-18 column, and analyzed by UV detector. Sol-gel coated capillaries were used for online extraction and high-performance liquid chromatographic analysis of phenols, ketones, aldehydes, and polyaromatic hydrocarbons. This newly developed coating showed excellent extraction for a variety of analytes ranging from highly polar to non-polar in nature. The analysis using sol-gel coating showed excellent overall sensitivity in terms of lower detection limits (S/N = 3) for the analytes (0.10 ng mL -1 -14.29 ng mL -1 ) with acceptable reproducibility that is less than 12.0%RSD (n = 3). Moreover, the capillary to capillary reproducibility of the analysis was also tested by changing the capillary of the same size. This provided excellent%RSD of less than 10.0% (n = 3). Copyright © 2018 Elsevier B.V. All rights reserved.

  17. A highly active PtCu3 intermetallic core-shell, multilayered Pt-skin, carbon embedded electrocatalyst produced by a scale-up sol-gel synthesis.

    Science.gov (United States)

    Bele, M; Jovanovič, P; Pavlišič, A; Jozinović, B; Zorko, M; Rečnik, A; Chernyshova, E; Hočevar, S; Hodnik, N; Gaberšček, M

    2014-11-07

    We present a novel, scaled-up sol-gel synthesis which enables one to produce 20 g batches of highly active and stable carbon supported PtCu3 nanoparticles as cathode materials for low temperature fuel cell application. We confirm the presence of an ordered intermetallic phase underneath a multilayered Pt-skin together with firm embedment of nanoparticles in the carbon matrix.

  18. Neutron detector using sol-gel absorber

    Science.gov (United States)

    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.

  19. Hybrid sol-gel optical materials

    Science.gov (United States)

    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.

  20. Nanocrystal/sol-gel nanocomposites

    Science.gov (United States)

    Petruska, Melissa A [Los Alamos, NM; Klimov, Victor L [Los Alamos, NM

    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.

  1. Fabrication of highly conductive graphene/ITO transparent bi-film through CVD and organic additives-free sol-gel techniques.

    Science.gov (United States)

    Hemasiri, Bastian Waduge Naveen Harindu; Kim, Jae-Kwan; Lee, Ji-Myon

    2017-12-19

    Indium tin oxide (ITO) still remains as the main candidate for high-performance optoelectronic devices, but there is a vital requirement in the development of sol-gel based synthesizing techniques with regards to green environment and higher conductivity. Graphene/ITO transparent bi-film was synthesized by a two-step process: 10 wt. % tin-doped ITO thin films were produced by an environmentally friendly aqueous sol-gel spin coating technique with economical salts of In(NO 3 ) 3 .H 2 O and SnCl 4 , without using organic additives, on surface free energy enhanced (from 53.826 to 97.698 mJm -2 ) glass substrate by oxygen plasma treatment, which facilitated void-free continuous ITO film due to high surface wetting. The chemical vapor deposited monolayer graphene was transferred onto the synthesized ITO to enhance its electrical properties and it was capable of reducing sheet resistance over 12% while preserving the bi-film surface smoother. The ITO films contain the In 2 O 3 phase only and exhibit the polycrystalline nature of cubic structure with 14.35 ± 0.5 nm crystallite size. The graphene/ITO bi-film exhibits reproducible optical transparency with 88.66% transmittance at 550 nm wavelength, and electrical conductivity with sheet resistance of 117 Ω/sq which is much lower than that of individual sol-gel derived ITO film.

  2. Damage thresholds of thin film materials and high reflectors at 248 nm

    International Nuclear Information System (INIS)

    Rainer, F.; Lowdermilk, W.H.; Milam, D.; Carniglia, C.K.; Hart, T.T.; Lichtenstein, T.L.

    1982-01-01

    Twenty-ns, 248-nm KrF laser pulses were used to measure laser damage thresholds for halfwave-thick layers of 15 oxide and fluoride coating materials, and for high reflectance coatings made with 13 combinations of these materials. The damage thresholds of the reflectors and single-layer films were compared to measurements of several properties of the halfwave-thick films to determine whether measurements of these properties of single-layer films to determine whether measurements of these properties of single-layer films were useful for identifying materials for fabrication of damage resistant coatings

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

    Science.gov (United States)

    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.

  4. Inexpensive sol-gel synthesis of multiwalled carbon nanotube-TiO{sub 2} hybrids for high performance antibacterial materials

    Energy Technology Data Exchange (ETDEWEB)

    Abbas, Nadir; Shao, Godlisten N. [Department of Fusion Chemical Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of); Haider, M. Salman [Department of Civil and Environmental System Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of); Imran, Syed Muhammad; Park, Sung Soo; Jeon, Sun-Jeong [Department of Fusion Chemical Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of); Kim, Hee Taik, E-mail: khtaik@hanyang.ac.kr [Department of Fusion Chemical Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of)

    2016-11-01

    This study reports an inexpensive sol-gel method to synthesize TiO{sub 2}-CNT hybrid materials. Synthesized TiO{sub 2}-CNT materials show strong antibacterial activity in the absence of light. Cheap TiO{sub 2} source TiOCl{sub 2} is used during synthesis in the absence of high temperatures, high pressures and organic solvents. TiO{sub 2}-CNT materials with 0, 2, 5, 10, 15 and 20 wt% of CNT were synthesized and compared for antibacterial activity, surface area, porosity, crystalline structure, chemical state, and HaCaT cell proliferation. The antibacterial strength of hybrid materials increased significantly with the increase in CNT loading amount, and the TiO{sub 2}-CNT samples with a CNT loading of 10 wt% or more nearly removed all of the E.coli bacteria. HaCaT cell proliferation studies of synthesized hybrid materials illustrated that prepared TiO{sub 2}-CNT systems exhibit minimum cytotoxicity. The characteristics of prepared materials were analyzed by means of XRD, FTIR, Raman spectroscopy, XPS, TEM, and nitrogen gas physisorption studies, compared and discussed. - Highlights: • An inexpensive scheme of preparing TiO{sub 2}-CNT hybrids is presented. • Significant increase in the antibacterial properties of TiO{sub 2} in absence of light • Effects of CNT addition on the physicochemical properties of hybrids are studied. • Antibacterial activity increases with increase in CNT content. • Hybrids show no toxicity towards HaCaT skin cell line.

  5. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    Science.gov (United States)

    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.

  6. Sol-Gel Derived Hafnia Coatings

    Science.gov (United States)

    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.

  7. Synthesis and characterization of high surface area nanosilica from rice husk ash by surfactant-free sol-gel method

    Czech Academy of Sciences Publication Activity Database

    Hassan, A F.; Abdelghny, A.M.; Elhadidy, Hassan; Youssef, A.M.

    2014-01-01

    Roč. 69, č. 3 (2014), 465-472 ISSN 0928-0707 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0068; GA MŠk(CZ) EE2.3.20.0214 Institutional support: RVO:68081723 Keywords : Nanosilica * Rice husk * Sol-gel method * N-2 adsorption Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.532, year: 2014

  8. Synthesis and stabilization of oxide-based colloidal suspensions in organic media: application in the preparation of hybrids organic-inorganic materials for very high laser damage threshold coatings

    International Nuclear Information System (INIS)

    Marchet, N.

    2008-02-01

    Multilayer coatings are widely used in optic and particular in the field of high power laser on the components of laser chains. The development of a highly reflective coating with a laser damage resistance requires the fine-tuning of a multilayer stack constituted by a succession alternated by materials with low and high refractive index. In order to limit the number of layers in the stack, refractive indexes must be optimized. To do it, an original approach consists in synthesizing new organic-inorganic hybrid materials satisfying the criteria of laser damage resistance and optimized refractive index. These hybrid materials are constituted by nano-particles of metal oxides synthesized by sol-gel process and dispersed in an organic polymer with high laser damage threshold. Nevertheless, this composite system requires returning both compatible phases between them by chemical grafting of alc-oxy-silanes or carboxylic acids. We showed that it was so possible to disperse in a homogeneous way these functionalized nano-particles in non-polar, aprotic solvent containing solubilized organic polymers, to obtain time-stable nano-composite solutions. From these organic-inorganic hybrid solutions, thin films with optical quality and high laser damage threshold were obtained. These promising results have permitted to realize highly reflective stacks, constituted by 7 pairs with optical properties in agreement with the theoretical models and high laser damage threshold. (author)

  9. Molecularly imprinted sol-gel nanofibers based solid phase microextraction coupled on-line with high performance liquid chromatography for selective determination of acesulfame.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-Adergani, Behrouz

    2015-03-01

    Sol-gel based molecularly imprinted polymer (MIP) nanofiber was successfully fabricated by electrospinning technique on the surface of a stainless steel bar. The manufactured tool was applied for on-line selective solid phase microextraction (SPME) and determination of acesulfame (ACF) as an artificial sweetener with high performance liquid chromatography (HPLC). The selective ability of method for the extraction of ACF was investigated in the presence of some selected sweeteners such as saccharine (SCH), aspartame (ASP) and caffeine (CAF). Electrospinning of MIP sol-gel solution on the stainless steel bar provided an unbreakable sorbent with high thermal, mechanical, and chemical stability. Moreover, application of the MIP-SPME tool revealed a unique approach for the selective microextraction of the analyte in beverage samples. In this work, 3-(triethoxysilyl)-propylamine (TMSPA) was chosen as a precursor due to its ability to imprint the analyte by hydrogen bonding, Van der Walls, and dipole-dipole interactions. Nylon 6 was also added as a backbone and support for the precursor in which sol could greatly growth during the sol-gel process and makes the solution electrospinable. Various effective parameters in the extraction efficiency of the MIP-SPME tool such as loading time, flow rate, desorption time, selectivity, and the sample volume were evaluated. The linearity for the ACF in beverage sample was in the range of 0.78-100.5 ng mL(-1). Limit of detection (LOD) and quantification (LOQ) were 0.23 and 0.78 ng mL(-1) respectively. The RSD values (n=5) were all below 3.5%at the 20 ng mL(-1) level. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Fast sol-gel synthesis of LiFePO{sub 4}/C for high power lithium-ion batteries for hybrid electric vehicle application

    Energy Technology Data Exchange (ETDEWEB)

    Beninati, Sabina; Damen, Libero; Mastragostino, Marina [University of Bologna, Department of Metal Science, Electrochemistry and Chemical Techniques, Via San Donato 15, 40127 Bologna (Italy)

    2009-12-01

    LiFePO{sub 4}/C of high purity grade was successfully synthesized by microwave accelerated sol-gel synthesis and showed excellent electrochemical performance in terms of specific capacity and stability. This cathode material was characterized in battery configuration with a graphite counter electrode by USABC-DOE tests for power-assist hybrid electric vehicle. It yielded a non-conventional Ragone plot that represents complexity of battery functioning in power-assist HEV and shows that the pulse power capability and available energy of such a battery surpasses the DOE goal for such an application. (author)

  11. Improvement of the damage threshold of high reflectivity multidielectric coatings 1.06 μM

    International Nuclear Information System (INIS)

    Geenen, B.; Malherbes, A.; Guerain, J.; Boisgard, D.

    1985-01-01

    Development of new high power laser for laser-matter interaction in C.E.A. Limeil requires the realization of H.R. coatings with damage thresholds above 8 J/cm/sup 2/. MATRA's laboratory ''couches minces optiques'' (thin optical layers) production commercial mirrors was around 3.5 J/cm/sup 2/ in 1982. In order to obtain better results the authors decided to improve the control of evaporation parameters such as: vacuum and regulation of oxygen pressure by means of a mass spectrometer; better measurements of evaporation temperature and regulation of evaporation rate; measurement and control of substrate temperature by pyrometric observation; and to automatize the process. These different measurements and controls enable them to establish new processing operations giving better evaporation conditions. The result was an increase of damage threshold from 3.5 J/cm/sup 2/ to 8 J/cm/sup 2/

  12. High-damage-threshold static laser beam shaping using optically patterned liquid-crystal devices.

    Science.gov (United States)

    Dorrer, C; Wei, S K-H; Leung, P; Vargas, M; Wegman, K; Boulé, J; Zhao, Z; Marshall, K L; Chen, S H

    2011-10-15

    Beam shaping of coherent laser beams is demonstrated using liquid crystal (LC) cells with optically patterned pixels. The twist angle of a nematic LC is locally set to either 0 or 90° by an alignment layer prepared via exposure to polarized UV light. The two distinct pixel types induce either no polarization rotation or a 90° polarization rotation, respectively, on a linearly polarized optical field. An LC device placed between polarizers functions as a binary transmission beam shaper with a highly improved damage threshold compared to metal beam shapers. Using a coumarin-based photoalignment layer, various devices have been fabricated and tested, with a measured single-shot nanosecond damage threshold higher than 30 J/cm2.

  13. Safe and Environmentally Acceptable Sol-Gel-Derived Pyrophoric Pyrotechnics

    National Research Council Canada - National Science Library

    Simpson, Randall L; Hubble, William; Stevenson, Bradley; Gash, Alexander; Satcher, Joe; Metcalf, Patricia

    2004-01-01

    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...

  14. Sol-gel derived sorbents

    Science.gov (United States)

    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.

  15. Low-Temperature Sol-Gel Synthesis of Nitrogen-Doped Anatase/Brookite Biphasic Nanoparticles with High Surface Area and Visible-Light Performance

    Directory of Open Access Journals (Sweden)

    Liang Jiang

    2017-12-01

    Full Text Available Nitrogen doping in combination with the brookite phase or a mixture of TiO2 polymorphs nanomaterials can enhance photocatalytic activity under visible light. Generally, nitrogen-dopedanatase/brookite mixed phases TiO2 nanoparticles obtained by hydrothermal or solvothermal method need to be at high temperature and with long time heating treatment. Furthermore, the surface areas of them are low (<125 m2/g. There is hardly a report on the simple and direct preparation of N-doped anatase/brookite mixed phase TiO2 nanostructures using sol-gel method at low heating temperature. In this paper, the nitrogen-doped anatase/brookite biphasic nanoparticles with large surface area (240 m2/g were successfully prepared using sol-gel method at low temperature (165 °C, and with short heating time (4 h under autogenous pressure. The obtained sample without subsequent annealing at elevated temperatures showed enhanced photocatalytic efficiency for the degradation of methyl orange (MO with 4.2-, 9.6-, and 7.5-fold visible light activities compared to P25 and the amorphous samples heated in muffle furnace with air or in tube furnace with a flow of nitrogen at 165 °C, respectively. This result was attributed to the synergistic effects of nitrogen doping, mixed crystalline phases, and high surface area.

  16. Sol-gel optical coatings for lasers: Part 1

    International Nuclear Information System (INIS)

    Floch, H.G.; Belleville, P.F.; Priotton, J.J.

    1995-01-01

    Many manufacturers and users claim that optical coatings are best prepared by physical vapor deposition technology. Others believe that sol-gel technology is an effective and competitive alternative. This article, the first of three, emphasizes sol-gel thin-film history and relates it to high-power laser technology, chemistry of the sol-gel process, production of optical coatings and deposition techniques. The second and third articles describe the preparation and performance of antireflective and highly reflective sol-gel optical coatings, respectively, that have been developed for the 1.8-MJ/500-TW (351-nm) pulsed neodymium-glass laser. This powerful laser is to be used in France's Inertial Confinement Fusion (ICF) program. It will demonstrate, at the laboratory scale, ignition of deuterium-tritium fusion fuel

  17. Sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) electrogenerated chemiluminescence sensor for high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Choi, Han Nim; Cho, Sung-Hee; Park, Yu-Jin; Lee, Dai Woon; Lee, Won-Yong

    2005-01-01

    The sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy) 3 2+ ] electrogenerated chemiluminescence (ECL) sensor was applied to the reversed-phase high-performance liquid chromatography (HPLC) determination of phenothiazine derivatives (promazine, chlorpromazine, triflupromazine, thioridazine, and trifluoperazine) and erythromycin in human urine samples. In this method, Ru(bpy) 3 2+ was immobilized in sol-gel-derived titania (TiO 2 )-Nafion nanocomposite films coated on a dual platinum electrode. This method eliminates an extra pump needed for the delivery of Ru(bpy) 3 2+ reagent into a reaction/observation zone in front of photomultiplier tube because the immobilized-Ru(bpy) 3 2+ is recycled on the electrode surface by an applied potential at +1.3 V versus Ag/AgCl (3 M NaCl) reference electrode. The resulting analytical performances such as detection limit, working range, sensitivity, and measurement precision were slightly worse than those obtained with the conventional post-column Ru(bpy) 3 2+ addition approach. The lack of significant interferences and the low detection limits for phenothiazine derivatives and erythromycin indicate that the proposed HPLC-Ru(bpy) 3 2+ ECL detection method is suitable for the determination of those compounds in biological fluids

  18. Influence of sol-gel parameters on the properties of chemical optodes. Application to on-line analysis of high acidities

    International Nuclear Information System (INIS)

    Bouzon, C.

    2000-01-01

    An optical chemical sensor (optode) has been optimized to control high acidity levels (ranging from 1 to 10 N) of solutions from nuclear fuel reprocessing. The sol-gel process has been used successfully to prepare a porous silica layer doped with an indicator called Chromoxane Cyanine R (CCR). The sensor response represents changes in the absorption properties of the dye according to the acidity. In a first step, the leaching of the dye has been studied according to the sol-gel parameters. An experimental Hadamard matrix has been used to find the most influent parameters. The influent parameters resulting from the first step have been studied using a parametrical optimization based on a Doelhert experimental design. This optimization highlights a quantitative correlation between sensor response and the chemical parameters. Results indicate that the most suitable microporous xerogel films are those prepared using tetramethoxysilane at a pH set below the isoelectric point (lEP) of silica. The two other influent parameters are: water / alkoxide ratio (R) and aging temperature (T a ). The optimized values are R = 4 and T a = 55 C. The lifetime of the sensor tested in a permanent circulation has been increased from several days to over 6 months in a 8 N nitric acid solution. Furthermore, this sensor can be used with hydrochloric and perchloric acids. (author) [fr

  19. Sol-Gel Manufactured Energetic Materials

    Science.gov (United States)

    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. Production of continuous mullite fiber via sol-gel processing

    Science.gov (United States)

    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.

  1. Sol-Gel Chemistry for Carbon Dots.

    Science.gov (United States)

    Malfatti, Luca; Innocenzi, Plinio

    2018-03-14

    Carbon dots are an emerging class of carbon-based nanostructures produced by low-cost raw materials which exhibit a widely-tunable photoluminescence and a high quantum yield. The potential of these nanomaterials as a substitute of semiconductor quantum dots in optoelectronics and biomedicine is very high, however they need a customized chemistry to be integrated in host-guest systems or functionalized in core-shell structures. This review is focused on recent advances of the sol-gel chemistry applied to the C-dots technology. The surface modification, the fine tailoring of the chemical composition and the embedding into a complex nanostructured material are the main targets of combining sol-gel processing with C-dots chemistry. In addition, the synergistic effect of the sol-gel precursor combined with the C-dots contribute to modify the intrinsic chemo-physical properties of the dots, empowering the emission efficiency or enabling the tuning of the photoluminescence over a wide range of the visible spectrum. © 2018 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Design and fabrication of a high-damage threshold infrared Smattt interferometer

    International Nuclear Information System (INIS)

    Hammond, R.B.; Gibbs, A.J.

    1981-01-01

    It has been shown that a Smartt interferometer may be used as a very precise alignment tool for infrared lasers. This interferometer may also be used effectively to investigate the phase front of a laser pulse. To use this tool for applications to high-power, fast-pulse laser systems such as Helios and Antares; however, it has been necessary to fabricate a structure with the unique optical characteristics of the Smartt interferometer combined with a very high optical-damage threshold. We have been successful in this effort by utilizing the high technology, process control, and unique properties of semiconductor-grade, single-crystal Si

  3. Ionogel Electrolytes through Sol-Gel Processing

    Science.gov (United States)

    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. Preparation of high density (Th, U)O2 pellets by sol-gel microsphere pelletization and 1300 C air sintering

    International Nuclear Information System (INIS)

    Yamagishi, Shigeru; Takahashi, Yoshihisa

    1994-01-01

    The fabrication of high density (Th, U)O 2 pellets by the sol-gel microsphere pelletization (SGMP) process was studied. To prepare source ThO 2 -UO 3 microspheres, isopropyl alcohol was substituted for the water in gel and thereafter removed by evacuating and subsequently by heating at 200 C in air. After humidifying the microspheres up to the moisture content ranging 10-21%, they were compacted into a pellet under 150-500 MPa and sintered in air at 1300 C. Even at the relatively low temperature, the maximum density reached 98% TD or higher for the U/(Th+U) ratios of 5-20 mol%. Such high density products survived as firm pellets with a similarly high density of 99% TD during the reduction into (Th, U)O 2 in Ar-4% H 2 at 1300 C. ((orig.))

  5. Design of a high pulse repitition frequency carbon dioxide laser for processing high damage threshold materials

    Science.gov (United States)

    Chatwin, Christopher R.; McDonald, Donald W.; Scott, Brian F.

    1989-07-01

    The absence of an applications led design philosophy has compromised both the development of laser source technology and its effective implementation into manufacturing technology in particular. For example, CO2 lasers are still incapable of processing classes of refractory and non-ferrous metals. Whilst the scope of this paper is restricted to high power CO2 lasers; the design methodology reported herein is applicable to source technology in general, which when exploited, will effect an expansion of applications. The CO2 laser operational envelope should not only be expanded to incorporate high damage threshold materials but also offer a greater degree of controllability. By a combination of modelling and experimentation the requisite beam characteristics, at the workpiece, were determined then utilised to design the Laser Manufacturing System. The design of sub-system elements was achieved by a combination of experimentation and simulation which benefited from a comprehensive set of software tools. By linking these tools the physical processes in the laser - electron processes in the plasma, the history of photons in the resonator, etc. - can be related, in a detailed model, to the heating mechanisms in the workpiece.

  6. Metal-silica sol-gel materials

    Science.gov (United States)

    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.

  7. Sol-Gel Glasses

    Science.gov (United States)

    Mukherjee, S. P.

    1985-01-01

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

  8. Functional coatings: the sol-gel approach

    International Nuclear Information System (INIS)

    Belleville, Ph.

    2010-01-01

    CEA's sol-gel laboratory is specialized in the development of innovative sol-gel optical coatings and has extended its application field to membrane materials and coatings for energy conversion, to electric coatings for microelectronics devices and to thin films for gas sensing. This article describes, by way of examples, the laboratory's research on sol-gel functional coatings, including nano-material synthesis, organic-inorganic hybrid-based solution preparation as well as deposition process development and prototyping. (author)

  9. Highly efficient visible light TiO{sub 2} photocatalyst prepared by sol-gel method at temperatures lower than 300 {sup o}C

    Energy Technology Data Exchange (ETDEWEB)

    Wang Desong, E-mail: dswang06@126.com [School of Sciences, Hebei University of Science and Technology, Shijiazhuang, Hebei 050018 (China); Xiao Libin; Luo Qingzhi; Li Xueyan; An Jing [School of Sciences, Hebei University of Science and Technology, Shijiazhuang, Hebei 050018 (China); Duan Yandong [College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang, Hebei 050018 (China)

    2011-08-15

    Graphical abstract: Display Omitted Highlights: {yields} Mesoporous anatase nano-TiO{sub 2} photocatalyst was synthesized by sol-gel method at lower temperature ({<=}300 {sup o}C). {yields} Its visible light photocatalytic activity is greatly higher than that of TiO{sub 2} (P-25) and its photocatalytic stability is excellent. {yields} Carbon self-doping and visible photosensitive organic groups result in the improvement of the visible light photocatalytic activity. -- Abstract: Highly efficient visible light TiO{sub 2} photocatalyst was prepared by the sol-gel method at lower temperature ({<=}300 {sup o}C), and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and differential scanning calorimetry-thermogravimetric analysis (DSC-TGA). The effects of the heat treatment temperature and time of the as-prepared TiO{sub 2} on its visible light photocatalytic activity were investigated by monitoring the degradation of methyl orange solution under visible light irradiation (wavelength {>=} 400 nm). Results show that the as-prepared TiO{sub 2} nanoparticles possess an anatase phase and mesoporous structure with carbon self-doping and visible photosensitive organic groups. The visible light photocatalytic activity of the as-prepared TiO{sub 2} is greatly higher than those of the commercial TiO{sub 2} (P-25) and other visible photocatalysts reported in literature (such as PPy/TiO{sub 2}, P3HT/TiO{sub 2}, PANI/TiO{sub 2}, N-TiO{sub 2} and Fe{sup 3+}-TiO{sub 2}) and its photocatalytic stability is excellent. The reasons for improving the visible light photocatalytic activity of the as-prepared TiO{sub 2} can be explained by carbon self-doping and a large amount of visible photosensitive groups existing in the as-prepared TiO{sub 2}. The apparent optical thickness ({tau}{sub app}), local

  10. Laser Direct Writing Process for Making Electrodes and High-k Sol-Gel ZrO2 for Boosting Performances of MoS2 Transistors.

    Science.gov (United States)

    Kwon, Hyuk-Jun; Jang, Jaewon; Grigoropoulos, Costas P

    2016-04-13

    A series of two-dimensional (2D) transition metal dichalcogenides (TMDCs), including molybdenum disulfide (MoS2), can be attractive materials for photonic and electronic applications due to their exceptional properties. Among these unique properties, high mobility of 2D TMDCs enables realization of high-performance nanoelectronics based on a thin film transistor (TFT) platform. In this contribution, we report highly enhanced field effect mobility (μ(eff) = 50.1 cm(2)/(V s), ∼2.5 times) of MoS2 TFTs through the sol-gel processed high-k ZrO2 (∼22.0) insulator, compared to those of typical MoS2/SiO2/Si structures (μ(eff) = 19.4 cm(2)/(V s)) because a high-k dielectric layer can suppress Coulomb electron scattering and reduce interface trap concentration. Additionally, in order to avoid costly conventional mask based photolithography and define the patterns, we employ a simple laser direct writing (LDW) process. This process allows precise and flexible control with reasonable resolution (up to ∼10 nm), depending on the system, and enables fabrication of arbitrarily patterned devices. Taking advantage of continuing developments in laser technology offers a substantial cost decrease, and LDW may emerge as a promising technology.

  11. Highly sensitive and selective spectrofluorimetric determination of metoclopramide hydrochloride in pharmaceutical tablets and serum samples using Eu3+ ion doped in sol-gel matrix.

    Science.gov (United States)

    Attia, M S; Aboaly, M M

    2010-06-30

    A simple, sensitive and selective spectrofluorimetric method for the determination of Metoclopramide hydrochloride (MCP) is developed. The MCP can remarkably enhances the luminescence intensity of the Eu(3+) ion doped in sol-gel matrix at lambda(ex)=380 nm in DMSO at pH 8.7. The intensity of the emission band of Eu(3+) ion doped in sol-gel matrix increases due to energy transfer from MCP to Eu(3+) in the excited state. The enhancement of the emission band of Eu(3+) ion doped in sol-gel matrix at 617 nm was found to be directly proportional to the concentration of MCP with a dynamic range of 5 x 10(-9) - 1.0 x 10(-6) mol L(-1) and detection limit of 2.2 x10(-11) mol L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

  12. Sol-gel processing with inorganic metal salt precursors

    Science.gov (United States)

    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.

  13. Effect of nano-particulate sol-gel coatings on the oxidation resistance of high-strength steel alloys during the press-hardening process

    Energy Technology Data Exchange (ETDEWEB)

    Yekehtaz, M.; Benfer, S.; Fuerbeth, W. [DECHEMA-Forschungsinstitut, Theodor-Heuss-Allee 25, D-60486 Frankfurt am Main (Germany); Klesen, C.; Bleck, W. [Institut fuer Eisenhuettenkunde der RWTH Aachen, Intzestrasse 1, D-52072 Aachen (Germany)

    2012-10-15

    The need for lighter constructional materials in automotive industries has increased the use of high-strength steel alloys. To enhance passenger's safety press hardening may be applied to steel parts. However, as the steel parts are heated up to 950 C during this process they have to be protected by some kind of coating against the intense oxide formation usually taking place. As the coating systems used so far all have certain disadvantages in this work the ability of nano-particulate thin coatings obtained by the sol-gel process to improve the oxidation resistance of 22MnB5 steel is investigated. The coatings obtained from three sols containing lithium aluminum silicate and potassium aluminum silicate showed the best performance against oxidation. The structural properties of the coating materials were characterized using different methods like XRD and differential thermal analysis. Comparison of the oxidation rate constants proved the ability of the coatings to protect against oxidation at temperatures up to 800 C. Press-hardening experiments in combination with investigations on the thermal shock resistance of the coated samples also showed the ability of the coatings to stay intact during press hardening with only slight spalling of the coatings in the bending areas. The absence of any secondary intermetallic phases and layer residues during laser beam welding experiments on coated samples proves the suitability of the nano-particulate coatings for further industrial processing. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  14. Sol-gel technology for biomedical engineering

    International Nuclear Information System (INIS)

    Podbielska, H.; Ulatowska-Jarza, A.

    2005-01-01

    Sol-gel derived silica possess many promising features, including low-temperature preparation procedure, porosity, chemical and physical stability. Applications exploiting porous materials to encapsulate sensor molecules, enzymes and many other compounds, are developing rapidly. In this paper some potential applications, with emphasis on biomedical and environmental ones, are reviewed. The material preparation procedure is described and practical remarks on silica-based sol-gels are included. It is reported that sol-gels with entrapped various molecules may be used in construction of implants and coatings with bioactive properties. It is shown how to exploit the sol-gel production route for construction of sol-gel coated fiberoptic applicators for laser therapy. The applications of bioactive materials are discussed, as well. It is demonstrated that it is possible to immobilize photosensitive compounds in sol-gel matrix without loosing their photoactivity. Some examples of sol-gel based biosensors are demonstrated, as well, showing their potential for detecting various gases, toxic substances, acidity, humidity, enzymes and biologically active agents. (authors)

  15. Sol-gel bonding of silicon wafers

    International Nuclear Information System (INIS)

    Barbe, C.J.; Cassidy, D.J.; Triani, G.; Latella, B.A.; Mitchell, D.R.G.; Finnie, K.S.; Short, K.; Bartlett, J.R.; Woolfrey, J.L.; Collins, G.A.

    2005-01-01

    Sol-gel bonds have been produced between smooth, clean silicon substrates by spin-coating solutions containing partially hydrolysed silicon alkoxides. The two coated substrates were assembled and the resulting sandwich fired at temperatures ranging from 60 to 600 deg. C. The sol-gel coatings were characterised using attenuated total reflectance Fourier transform infrared spectroscopy, ellipsometry, and atomic force microscopy, while the corresponding bonded specimens were investigated using scanning electron microscopy and cross-sectional transmission electron microscopy. Mechanical properties were characterised using both microindentation and tensile testing. Bonding of silicon wafers has been successfully achieved at temperatures as low as 60 deg. C. At 300 deg. C, the interfacial fracture energy was 1.55 J/m 2 . At 600 deg. C, sol-gel bonding provided superior interfacial fracture energy over classical hydrophilic bonding (3.4 J/m 2 vs. 1.5 J/m 2 ). The increase in the interfacial fracture energy is related to the increase in film density due to the sintering of the sol-gel interface with increasing temperature. The superior interfacial fracture energy obtained by sol-gel bonding at low temperature is due to the formation of an interfacial layer, which chemically bonds the two sol-gel coatings on each wafer. Application of a tensile stress on the resulting bond leads to fracture of the samples at the silicon/sol-gel interface

  16. Development of high damage threshold optics for petawatt-class short-pulse lasers

    International Nuclear Information System (INIS)

    Stuart, B.C.; Perry, M.D.; Boyd, R.D.

    1995-01-01

    The authors report laser-induced damage threshold measurements on pure and multilayer dielectrics and gold-coated optics at 1053 and 526 nm for pulse durations, τ, ranging from 140 fs to 1 ns. Damage thresholds of gold coatings are limited to 500 mJ/cm 2 in the subpicosecond range for 1053-nm pulses. In dielectrics, qualitative differences in the morphology of damage and a departure from the diffusion-dominated τ1/2 scaling indicate that damage results from plasma formation and ablation for τ≤10 ps and from conventional melting and boiling for τ>50 ps. A theoretical model based on electron production via multiphoton ionization, Joule heating, and collisional (avalanche) ionization is in quantitative agreement with both the pulsewidth and wavelength scaling of experimental results

  17. Preparation of high-purity ZrSiO4 powder using sol-gel processing and mechanical properties of the sintered body

    International Nuclear Information System (INIS)

    Mori, T.; Yamamura, H.; Kobayashi, H.; Mitamura, T.

    1992-01-01

    This paper reports that effects of the concentration of ZrOCl 2 , calcination temperature, heating rate, and the size of secondary particles after hydrolysis on the preparation of high-purity ZrSiO 4 fine powders from ZrOCl 2 :8H 2 O (0.2M to 1.7M) and equimolar colloidal SiO 2 using Sol--gel processing have been studied. Mechanical properties of the sintered ZrSiO 4 from the high-purity ZrSiO 4 powders have been also investigated. Single-phase ZrSiO 4 fine powders were synthesized at 1300 degrees C by forming ZrSiO 4 precursors having a Zr---O---Si bond, which was found in all the hydrolysis solutions, and by controlling a secondary particle size after hydrolysis. The conversion rate of ZrSiO 4 precursor gels to ZrSiO 4 powders from concentrations other than 0.4M ZrOCl 2 ·8H 2 O increased when the heating rate was high, whereupon the crystallization of unreacted ZrO 2 and SiO 2 was depressed and the propagation and increase of ZrSiO 4 nuclei in the gels were accelerated. The density of the ZrSiO 4 sintered bodies, manufactured by firing the ZrSiO 4 compacts at 1600 degrees to 1700 degrees C, was more than 95% of the theoretical density, and the grain size ranged around 2 to 4 μm. The mechanical strength was 320 MPa (room temperature to 1400 degrees C), and the thermal shock resistance was superior to that of mullite and alumina, with fairly high stability at higher temperatures

  18. Neutron detector based on lithiated sol-gel glass

    CERN Document Server

    Wallace, S; Miller, L F; Dai, S

    2002-01-01

    A neutron detector technology is demonstrated based on sup 6 Li/ sup 1 sup 0 B doped sol-gel glass. The detector is a sol-gel glass film coated silicon surface barrier detector (SBD). The ionized charged particles from (n, alpha) reactions in the sol-gel film enter the SBD and are counted. Data showing that gamma-ray pulse amplitudes interfere with identifying charged particles that exit the film layer with energies below the gamma-ray energy is presented. Experiments were performed showing the effect of sup 1 sup 3 sup 7 Cs and sup 6 sup 0 Co gamma rays on the SBD detector. The reaction product energies of the triton and alpha particles from sup 6 Li are significantly greater than the energies of the Compton electrons from high-energy gamma rays, allowing the measurement of neutrons in a high gamma background. The sol-gel radiation detection technology may be applicable to the characterization of transuranic waste, spent nuclear fuel and to the monitoring of stored plutonium.

  19. AuNPs Hybrid Black ZnO Nanorods Made by a Sol-Gel Method for Highly Sensitive Humidity Sensing

    Directory of Open Access Journals (Sweden)

    Hongyan Zhang

    2018-01-01

    Full Text Available A highly sensitive self-powered humidity sensor has been realized from AuNPs hybrid black zinc oxide (ZnO nanorods prepared through a sol-gel method. XRD pattern reveals that both ZnO and ZnO/AuNPs exhibit a wurtzite structure. ZnO/AuNPs nanorods grow in a vertical alignment, which possesses high uniformity and forms dense arrays with a smaller diameter than that of ZnO nanoparticles. All ZnO/AuNPs and pure black ZnO show lower band gap energy than the typically reported 3.34 eV of pure ZnO. Furthermore, the band gap of ZnO/AuNPs nanocomposites is effectively influenced by the amount of AuNPs. The humidity sensing tests clearly prove that all the ZnO/AuNPs humidity sensors exhibit much higher response than that of ZnO sensors, and the sensitivity of such ZnO/AuNPs nanorods (6 mL AuNPs display a change three orders higher than that of pure ZnO with relative humidity (RH ranging from 11% to 95% at room temperature. The response and recovery time of the ZnO/AuNPs are 5.6 s and 32.4 s, respectively. This study of the construction of semiconductor/noble metal sensors provides a rational way to control the morphology of semiconductor nanomaterials and to design a humidity sensor with high performance.

  20. Vapor-Liquid Sol-Gel Approach to Fabricating Highly Durable and Robust Superhydrophobic Polydimethylsiloxane@Silica Surface on Polyester Textile for Oil-Water Separation.

    Science.gov (United States)

    Su, Xiaojing; Li, Hongqiang; Lai, Xuejun; Zhang, Lin; Wang, Jing; Liao, Xiaofeng; Zeng, Xingrong

    2017-08-23

    Large-scale fabrication of superhydrophobic surfaces with excellent durability by simple techniques has been of considerable interest for its urgent practical application in oil-water separation in recent years. Herein, we proposed a facile vapor-liquid sol-gel approach to fabricating highly durable and robust superhydrophobic polydimethylsiloxane@silica surfaces on the cross-structure polyester textiles. Scanning electron microscopy and Fourier transform infrared spectroscopy demonstrated that the silica generated from the hydrolysis-condensation of tetraethyl orthosilicate (TEOS) gradually aggregated at microscale driven by the extreme nonpolar dihydroxyl-terminated polydimethylsiloxane (PDMS(OH)). This led to construction of hierarchical roughness and micronano structures of the superhydrophobic textile surface. The as-fabricated superhydrophobic textile possessed outstanding durability in deionized water, various solvents, strong acid/base solutions, and boiling/ice water. Remarkably, the polyester textile still retained great water repellency and even after ultrasonic treatment for 18 h, 96 laundering cycles, and 600 abrasion cycles, exhibiting excellent mechanical robustness. Importantly, the superhydrophobic polyester textile was further applied for oil-water separation as absorption materials and/or filter pipes, presenting high separation efficiency and great reusability. Our method to construct superhydrophobic textiles is simple but highly efficient; no special equipment, chemicals, or atmosphere is required. Additionally, no fluorinated slianes and organic solvents are involved, which is very beneficial for environment safety and protection. Our findings conceivably stand out as a new tool to fabricate organic-inorganic superhydrophobic surfaces with strong durability and robustness for practical applications in oil spill accidents and industrial sewage emission.

  1. Highly Sensitive Ethanol Chemical Sensor Based on Novel Ag-Doped Mesoporous α-Fe2O3 Prepared by Modified Sol-Gel Process

    Science.gov (United States)

    Alqahtani, Moteb M.; Ali, Atif M.; Harraz, Farid A.; Faisal, M.; Ismail, Adel A.; Sayed, Mahmoud A.; Al-Assiri, M. S.

    2018-05-01

    Mesoporous α-Fe2O3 has been synthesized via a simple sol-gel procedure in the presence of Pluronic (F-127) triblock copolymer as structure directing agent. Silver (Ag) nanoparticles were deposited onto α-Fe2O3 matrix by the photochemical reduction approach. Morphological analysis revealed the formation of Ag nanoparticles with small sizes < 20 nm onto the mesoporous structure of α-Fe2O3 possessing < 50 nm semi-spherical shape. The XRD, FTIR, Raman, UV-vis, PL, and N2 sorption isotherm studies confirmed the high crystallinity, mesoporosity, and optical characteristics of the synthesized product. The electrochemical sensing toward liquid ethanol has been performed using the current devolved Ag/α-Fe2O3-modified glassy carbon electrode (GCE) by cyclic voltammetry ( CV) and current potential ( I-V) techniques, and the obtained results were compared with bare GCE or pure α-Fe2O3. Mesoporous Ag/α-Fe2O3 was found to largely enhance the sensor sensitivity and it exhibited excellent sensing characteristics during the precision detection of low concentrations of ethanol. High and reproducible sensitivity of 41.27 μAmM- 1 cm- 2 at lower ethanol concentration region (0.05 to 0.8 mM) and 2.93 μAmM- 1 cm- 2 at higher concentration zone (0.8 to 15 mM), with a limit of detection (LOD) of 15.4 μM have been achieved. Investigation on reaction kinetics revealed a characteristic behavior of mixed surface and diffusion-controlled processes. Detailed sensing studies revealed also that the sensitivity toward ethanol was higher than that of methanol or isopropanol. With further effort in developing the synthesis and fabrication approaches, a proper utility for the current proposed protocol for fabricating a better sensor device performance is possible.

  2. Kramers-Kronig method for determination of optical properties of PZT nanotubes fabricated by sol-gel method and porous anodic alumina with high aspect ratio

    Science.gov (United States)

    Pakizeh, Esmaeil; Moradi, Mahmood

    2018-03-01

    Ferroelectric Pb(ZrTi)O3 (PZT) nanotubes were prepared by sol-gel method and porous anodic alumina (PAA) membrane using spin-coating technique. This method is based on filling-pyrolysis-filling process and the use of one-stage alumina membranes. One of the advantages of this method is its rapidity, which takes only 1 h time before the calcination step. The effect of repeated pores filling was investigated to get the required size of nanotubes. The field emission scanning electron microscope (FE-SEM) images were shown that the PZT nanotubes have inner diameters in the range of 65-90 nm and length of about 50-60 μm. This means that the samples have a significant aspect ratio (700-800). Also the FE-SEM image confirmed that the highly ordered, hexagonally distributed PAA membranes with the pore diameter about 140-150 nm were formed. The X-ray diffraction (XRD) results showed that the PZT nanotubes have a tetragonal structure. The metal oxide bands like ZrO6 and TiO6 of the final PZT nanotubes were detected by Fourier transform infrared (FT-IR) analysis and confirmed the formation of perovskite structure. By using FT-IR spectroscopy and Kramers-Kronig transformation method, the optical constants like real 𝜀1(ω) and imaginary 𝜀2(ω) parts of dielectric function, extinction coefficient k(ω) and refractive index n(ω) were determined. It was shown that the optical constants of PZT nanotubes are different from PZT nanoparticles.

  3. Sol-gel antireflective coating on plastics

    Science.gov (United States)

    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.

  4. Characterisation of a new alkoxide sol-gel hydroxyapatite

    International Nuclear Information System (INIS)

    Green, D.D.; Kannangara, G.S.K.; Milev, A.; Ben-Nissan, B.

    1999-01-01

    Hydroxyapatite (HAp) coatings have been used to promote bone growth and fixation towards implant surfaces to encourage faster recovery times for the recipient. Current coating processing techniques, capable of producing thin HAp layers are pulsed-laser deposition and sputtering (high-temperature processing). Other technologies are in vitro methods, electrodeposition and sol-gel, due to the fact that these techniques utilise lower processing temperatures they avoid structural instabilities of HAp at elevated temperatures. The term sol-gel encompasses any process of producing ceramic materials (single and mixed oxides, as well as non-oxides e.g. nitrides) from solutions. The sol-gel process was first identified by Ebelman, and has been used to produce ceramic powders, coatings, and bulk materials including glasses. The implementation of a sol-gel methodology enables increased stoichiometry and homogeneity, while having the ability to coat complex shapes. Sol-gel hydroxyapatite reported by Chai et al. employed tri ethyl phosphite [ P(OEt) 3 ] as the staring phosphorus alkoxide precursor, whereby it was established that in order to obtain monophasic hydroxyapatite upon firing there must be a 24 hour ripening period. The ripening period was determined to be an equilibrium step whereby the equilibrium intermediate phase lied in favour of a diethyl phosphite arrangement (species) within the sol. Therefore, the work here under taken was to produce hydroxyapatite using diethyl phosphite [HOP(OEt) 2 ] as a starting alkoxide precursor with a final aim to reduce or eliminate the ageing period as observed by Chai et al in P(OEt) 3 solutions

  5. Sol-gel silica-based nanocomposites containing a high PEG amount: Chemical characterization and study of biological properties

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, Michelina; Bollino, Flavia [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29, 81031 Aversa (CE) (Italy); Gloria, Antonio [Institute of Polymers, Composites and Biomaterials - National Research Council of Italy, V.le J. F. Kennedy 54 - Mostra d’Oltremare Pad. 20, 80125 Naples (Italy)

    2016-05-18

    The objective of the present study was to synthesize and to characterize Silica/polyethylene glycol (SiO{sub 2}/PEG) organic-inorganic hybrid materials containing a high polymer amount (60 and 70 wt%) for biomedical applications. Scanning electron microscopy (SEM) showed that the samples are homogeneous on the nanometer scale, confirming that they are nanocomposites. Fourier transform infrared spectroscopy (FT-IR) proved that the materials are class I hybrids because the two phases (SiO{sub 2} and PEG) interact by hydrogen bonds. To evaluate the possibility of using them in the biomedical field, the bioactivity and biocompatibility of the synthesized hybrids have been ascertained. The formation of a hydroxyapatite layer was observed on the hybrid surface by SEM/EDX and FTIR after soaking in simulated body fluid (SBF). Moreover, their biocompatibility was assessed by performing WST-8 cytotoxicity assay in vitro.

  6. Sol-gel silica-based nanocomposites containing a high PEG amount: Chemical characterization and study of biological properties

    Science.gov (United States)

    Catauro, Michelina; Bollino, Flavia; Gloria, Antonio

    2016-05-01

    The objective of the present study was to synthesize and to characterize Silica/polyethylene glycol (SiO2/PEG) organic-inorganic hybrid materials containing a high polymer amount (60 and 70 wt%) for biomedical applications. Scanning electron microscopy (SEM) showed that the samples are homogeneous on the nanometer scale, confirming that they are nanocomposites. Fourier transform infrared spectroscopy (FT-IR) proved that the materials are class I hybrids because the two phases (SiO2 and PEG) interact by hydrogen bonds. To evaluate the possibility of using them in the biomedical field, the bioactivity and biocompatibility of the synthesized hybrids have been ascertained. The formation of a hydroxyapatite layer was observed on the hybrid surface by SEM/EDX and FTIR after soaking in simulated body fluid (SBF). Moreover, their biocompatibility was assessed by performing WST-8 cytotoxicity assay in vitro.

  7. Phase transformation in sol-gel prepared zirconia using in-situ high temperature X-ray diffraction

    International Nuclear Information System (INIS)

    Srinivasan, R.; Davis, B.H.; Hubbard, C.R.; Cavin, O.B.; Porter, W.D.

    1991-01-01

    Zirconia was precipitated at a pH of 10.5 by admixing a solution of ZrCl 4 and NH 4 OH both rapidly (∼ 1 min) and slowly (∼ 8 hr). The precipitate was calcined at 500C for 5 hours and then furnace cooled. The former exhibited monoclinic phase while the latter yielded tetragonal phase. The pathway from amorphous to crystalline form was followed by in-situ high temperature X-ray diffraction in flowing air and in He. The data showed the evolution of the tetragonal crystalline phase on heating. On rapid cooling the tetragonal phase is retained at R.T., and on slow cooling the transformation to monoclinic phase occurs in air

  8. Sol-gel silica-based nanocomposites containing a high PEG amount: Chemical characterization and study of biological properties

    International Nuclear Information System (INIS)

    Catauro, Michelina; Bollino, Flavia; Gloria, Antonio

    2016-01-01

    The objective of the present study was to synthesize and to characterize Silica/polyethylene glycol (SiO 2 /PEG) organic-inorganic hybrid materials containing a high polymer amount (60 and 70 wt%) for biomedical applications. Scanning electron microscopy (SEM) showed that the samples are homogeneous on the nanometer scale, confirming that they are nanocomposites. Fourier transform infrared spectroscopy (FT-IR) proved that the materials are class I hybrids because the two phases (SiO 2 and PEG) interact by hydrogen bonds. To evaluate the possibility of using them in the biomedical field, the bioactivity and biocompatibility of the synthesized hybrids have been ascertained. The formation of a hydroxyapatite layer was observed on the hybrid surface by SEM/EDX and FTIR after soaking in simulated body fluid (SBF). Moreover, their biocompatibility was assessed by performing WST-8 cytotoxicity assay in vitro.

  9. Efficient Phase Locking of Fiber Amplifiers Using a Low-Cost and High-Damage-Threshold Phase Control System

    International Nuclear Information System (INIS)

    Pu, Zhou; Yan-Xing, Ma; Xiao-Lin, Wang; Hao-Tong, Ma; Xiao-Jun, Xu; Ze-Jin, Liu

    2010-01-01

    We propose a low-cost and high-damage-threshold phase control system that employs a piezoelectric ceramic transducer modulator controlled by a stochastic parallel gradient descent algorithm. Efficient phase locking of two fiber amplifiers is demonstrated. Experimental results show that energy encircled in the target pinhole is increased by a factor of 1.76 and the visibility of the fringe pattern is as high as 90% when the system is in close-loop. The phase control system has potential in phase locking of large-number and high-power fiber laser endeavors. (fundamental areas of phenomenology (including applications))

  10. Sol-gel synthesis of hydroxyapatite

    International Nuclear Information System (INIS)

    Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P.

    2010-01-01

    Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

  11. Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process.

    Science.gov (United States)

    Li, Fa-Liang; Zhang, Hai-Jun

    2017-08-25

    The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  14. Porous alumina scaffold produced by sol-gel combined polymeric sponge method

    Science.gov (United States)

    Hasmaliza, M.; Fazliah, M. N.; Shafinaz, R. J.

    2012-09-01

    Sol gel is a novel method used to produce high purity alumina with nanometric scale. In this study, three-dimensional porous alumina scaffold was produced using sol-gel polymeric sponge method. Briefly, sol gel alumina was prepared by evaporation and polymeric sponge cut to designated sizes were immersed in the sol gel followed by sintering at 1250 and 1550°C. In order to study the cell interaction, the porous alumina scaffold was sterilized using autoclave prior to Human Mesenchymal Stem Cells (HMSCs) seeding on the scaffold and the cell proliferation was assessed by alamarBlue® assay. SEM results showed that during the 21 day period, HMSCs were able to attach on the scaffold surface and the interconnecting pores while maintaining its proliferation. These findings suggested the potential use of the porous alumina produced as a scaffold for implantation procedure.

  15. Dip coating of sol-gels

    Science.gov (United States)

    Schunk, P. R.; Hurd, A. J.; Brinker, C. J.

    Dip coating is the primary means of depositing sol-gel films for precision optical coatings. Sols are typically multicomponent systems consisting of an inorganic phase dispersed in a solvent mixture, with each component differing in volatility and surface tension. This, together with slow coating speeds (less than 1cm/s), makes analysis of the coating process complicated; unlike most high-speed coating methods, solvent evaporation, evolving rheology, and surface tension gradients alter significantly the fluid mechanics of the deposition stage. These phenomena were studied with computer-aided predictions of the flow and species transport fields. The underlying theory involves mass, momentum, and species transport on a domain of unknown shape, with models and constitutive equations for vapor-liquid equilibria and surface tension. Due accounting is made for the unknown position of the free surface, which locates according to the capillary hydrodynamic forces and solvent loss by evaporation. Predictions of the effects of mass transfer, hydrodynamics, and surface tension gradients on final film thickness are compared with ellipsometry measurements of film thickness on a laboratory pilot coater. Although quantitative agreement is still lacking, both experiment and theory reveal that the film profile near the drying line takes on a parabolic shape.

  16. Synthesis of cadmium tungstate films via sol-gel processing

    Energy Technology Data Exchange (ETDEWEB)

    Lennstrom, Kirk; Limmer, Steven J.; Cao Guozhong

    2003-06-23

    Cadmium tungstate is a scintillator material with excellent intrinsic photoluminescent properties. It is highly resistant to gamma radiation, has an almost non-existent afterglow and is highly efficient. Cadmium tungstate is also non-hydroscopic, unlike the more prevalent thallium-doped alkali halide scintillators. In order to create thin films of cadmium tungstate with precise stoichiometric control, a sol-gel processing technique has been applied to produce this material for the first time. In addition to lower processing temperatures, sol-gel-derived cadmium tungstate is cheaper and easier than other technologies, particularly for thin films. Furthermore, it has the potential to produce nanostructured materials with good optical quality. X-Ray diffraction results of sol-gel-derived materials fired at various temperatures imply crystallization of cadmium tungstate without the intermediate formation of either tungsten oxide or cadmium oxide. Scanning electron microscopy analysis shows the formation of nano-sized particles prior to heat treatment, which form meso-sized particles after the heat treatment. Photoluminesce analysis indicates emission of derived films at 480 nm, which agrees with other published data. Finally, the efficiency of derived films was approximately 6%{+-}1.8%.

  17. Sol-gel processing of bioactive glass nanoparticles: A review.

    Science.gov (United States)

    Zheng, Kai; Boccaccini, Aldo R

    2017-11-01

    Silicate-based bioactive glass nanoparticles (BGN) are gaining increasing attention in various biomedical applications due to their unique properties. Controlled synthesis of BGN is critical to their effective use in biomedical applications since BGN characteristics, such as morphology and composition, determining the properties of BGN, are highly related to the synthesis process. In the last decade, numerous investigations focusing on BGN synthesis have been reported. BGN can mainly be produced through the conventional melt-quench approach or by sol-gel methods. The latter approaches are drawing widespread attention, considering the convenience and versatility they offer to tune the properties of BGN. In this paper, we review the strategies of sol-gel processing of BGN, including those adopting different catalysts for initiating the hydrolysis and condensation of silicate precursors as well as those combining sol-gel chemistry with other techniques. The processes and mechanism of different synthesis approaches are introduced and discussed in detail. Considering the importance of the BGN morphology and composition to their biomedical applications, strategies put forward to control the size, shape, pore structure and composition of BGN are discussed. BGN are particularly interesting biomaterials for bone-related applications, however, they also have potential for other biomedical applications, e.g. in soft tissue regeneration/repair. Therefore, in the last part of this review, recently reported applications of BGN in soft tissue repair and wound healing are presented. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  19. Fluorescence metrology of silica sol-gels

    Indian Academy of Sciences (India)

    We have developed a new method for measuring in-situ the growth of the nanometre-size silica particles which lead to the formation of sol-gel glasses. This technique is based on the decay of fluorescence polarisation anisotropy due to Brownian rotation of dye molecules bound to the particles. Results to date give near ...

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

    Science.gov (United States)

    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.

  1. Synthesis of phthalocyanine doped sol-gel materials

    Science.gov (United States)

    Dunn, Bruce

    1993-01-01

    section ratio, 4, however, the tetrasulfonate groups make the dye soluble in water which greatly facilitates its incorporation into the sol-gel matrix. The nonlinear transmission of CuPc4S in a pH 2 buffer solution and in a silica xerogel were compared. It is evident that the CuPc4S preserves its optical limiting behavior in the sol-gel matrix, indicating that the fundamental excited state absorption process is essentially the same for a molecule in solution or in the solid state. Although the spectroscopic details of energy level lifetimes are unknown, the significance is that passive optical limiting has been achieved in the solid state via incorporation of a dye into an inorganic host. The only compromise occurs at the extremely high energy regime where photobleaching is observed. This is a result of the limited mobility of the dye molecules in the solid silica host relative to a liquid host. The effects of photodegradation in the xerogel are additive, whereas the solution provides a supply of fresh molecules that are free to enter the active volume between pulses.

  2. Sol-gel additive for systems with inorganic binders

    International Nuclear Information System (INIS)

    Akstinat, M.; Antenen, D.; Suter, W.

    1996-01-01

    A sol-gel additive for inorganic binder systems and sol-gel process for producing air-placed concrete and mortar by using such sol-gel additives are disclosed. Sol-gel additives for gel-derived inorganic binder systems (for example plaster, cement, lime, special slags, etc.) marked improve the consistency of such binder systems during processing or allow their consistency to be regulated. In addition, these sol-gel additives regulate setting times and substantially improve durability (chemical resistance, reduced permeability) and the mechanical properties of the set binder system. (author)

  3. Effects of deposition rates on laser damage threshold of TiO2/SiO2 high reflectors

    International Nuclear Information System (INIS)

    Yao Jianke; Xu Cheng; Ma Jianyong; Fang Ming; Fan Zhengxiu; Jin Yunxia; Zhao Yuanan; He Hongbo; Shao Jianda

    2009-01-01

    TiO 2 single layers and TiO 2 /SiO 2 high reflectors (HR) are prepared by electron beam evaporation at different TiO 2 deposition rates. It is found that the changes of properties of TiO 2 films with the increase of rate, such as the increase of refractive index and extinction coefficient and the decrease of physical thickness, lead to the spectrum shift and reflectivity bandwidth broadening of HR together with the increase of absorption and decrease of laser-induced damage threshold. The damages are found of different morphologies: a shallow pit to a seriously delaminated and deep crater, and the different amorphous-to-anatase-to-rutile phase transition processes detected by Raman study. The frequency shift of Raman vibration mode correlates with the strain in film. Energy dispersive X-ray analysis reveals that impurities and non-stoichiometric defects are two absorption initiations resulting to the laser-induced transformation.

  4. Ring-Resonator/Sol-Gel Interferometric Immunosensor

    Science.gov (United States)

    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.

  5. Transparent Hydrophobic Coating by Sol Gel Method

    International Nuclear Information System (INIS)

    Mohd Hamzah Harun; Nik Ghazali Nik Salleh; Mahathir Mohamed; Mohd Sofian Alias

    2016-01-01

    Transparent hydrophobic coating of inorganic based tetra orthosilicate (TEOS) was prepared by sol gel method by varying fluoroalkylsilane (FAS) content which works as hydrophobic agent. Surface contact angle, transmittance degree and surface morphology were characterized for each sample. All samples show good transparency which was confirmed by UV visible spectroscopy. The hydrophobicity obtained increases with FAS content indicates that FAS is best candidate to induce hydrophobicity for inorganic coating. (author)

  6. Sol-gel bonding of silicon wafers

    International Nuclear Information System (INIS)

    Barbe, C.J.; Cassidy, D.J.; Triani, G.; Latella, B.A.; Mitchell, D.R.G.; Finnie, K.S.; Bartlett, J.R.; Woolfrey, J.L.; Collins, G.A.

    2005-01-01

    Low temperature bonding of silicon wafers was achieved using sol-gel technology. The initial sol-gel chemistry of the coating solution was found to influence the mechanical properties of the resulting bonds. More precisely, the influence of parameters such as the alkoxide concentration, water-to-alkoxide molar ratio, pH, and solution aging on the final bond morphologies and interfacial fracture energy was studied. The thickness and density of the sol-gel coating were characterised using ellipsometry. The corresponding bonded specimens were investigated using attenuated total reflectance Fourier transformed infrared spectroscopy to monitor their chemical composition, infrared imaging to control bond integrity, and cross-sectional transmission electron microscopy to study their microstructure. Their interfacial fracture energy was measured using microindentation. An optimum water-to-alkoxide molar ratio of 10 and hydrolysis water at pH = 2 were found. Such conditions led to relatively dense films (> 90%), resulting in bonds with a fracture energy of 3.5 J/m 2 , significantly higher than those obtained using classical hydrophilic bonding (typically 1.5-2.5 J/m 2 ). Ageing of the coating solution was found to decrease the bond strength

  7. Sol-gel growth of vanadium dioxide

    International Nuclear Information System (INIS)

    Speck, K.R.

    1990-01-01

    This thesis examines the chemical reactivity of vanadium (IV) tetrakis(t-butoxide) as a precursor for the sol-gel synthesis of vanadium dioxide. Hydrolysis and condensation of the alkoxide was studied by FTIR spectroscopy. Chemical modification of the vanadium tetraalkoxide by alcohol interchange was studied using 51 V NMR and FTIR. Vanadium dioxide thin films and powders were made from vanadium tetrakis(t-butoxide) by standard sol-gel techniques. Post-deposition heating under nitrogen was necessary to transform amorphous gels into vanadium dioxide. Crystallization of films and powders was studied by FTIR, DSC, TGA, and XRD. Gel-derived vanadium dioxide films undergo a reversible semiconductor-to-metal phase transition near 68C, exhibiting characteristic resistive and spectral changes. The electrical resistance decreased by two to three orders of magnitude and the infrared transmission sharply dropped as the material was cycled through this thermally induced phase transition. The sol-gel method was also used to make doped vanadium dioxide films. Films were doped with tungsten and molybdenum ions to effectively lower the temperature at which the transition occurs

  8. A novel method for the elaboration of hydroxyapatite with high purity by sol-gel using the albumin and comparison with the classical methods

    Science.gov (United States)

    Mohammed, Eddya; Bouazza, Tbib; Khalil, El-Hami

    2018-02-01

    In this paper, we report the first synthesis of hydroxyapatite (Hap) by sol-gel using the albumin (egg white) compared with the four classical elaboration methods such as co-precipitation, solid state, and solid-liquid samples of hydroxyapatite. We use a reference sample of hydroxyapatite bought from Fluka Chemika company (Lot and Filling code 385330/1 14599). All samples are characterized by X-ray diffraction (XRD), Uv-visible spectroscopy (Uv-Vis), and Fourier transforms infrared spectroscopy (FT-IR). The XRD study showed the existence of a Hexagonal phase for all our samples prepared in our laboratory and an orthorhombic phase for the Fulka Chemika sample of Hap (Lot and Filling code 385330/1 14599). The study by Uv-visible spectroscopy was performed to determine and compare the optical gap and the disorder of each sample of Hap. The FT-IR spectroscopy demonstrated that all our Hap samples had a similar mode of vibration of the chemical bonds (OH-) and (PO4)3-.

  9. SOL-Gel microspheres and nanospheres for controlled release applications

    International Nuclear Information System (INIS)

    Barbe, C.; Beyer, R.; Kong, L.; Blackford, M.; Trautman, R.; Bartlett, J.

    2002-01-01

    one hour. The particles thus produced were washed with cyclohexane and carefully dried. Release Kinetics. The release of the encapsulated species from the particles was monitored by placing a fixed quantity of the sample in water or physiological saline, and monitoring the concentration of the released species using UV/Vis spectroscopy. The fraction released was normalised to the total mass initially encapsulated. The influence of the emulsion chemistry on the size of the microspheres obtained at pH 2 is illustrated in Figure 1 for microspheres containing encapsulated Orange II Using essentially identical sol-gel chemistries, particles with dimensions ranging from 50 nm to 50 μm can be readily obtained. The size of the particles is controlled by the size of the emulsion droplets, which act as micro-reactors for the sol-gel reactions. In turn, the size of the droplets is determined predominantly by the hydrophile/lipophile balance of the surfactant/ solvent couple and by processing parameters such as the water to surfactant ratio and the concentration of surfactant. The effect of sol-gel processing parameters on the morphology and associated release kinetics is illustrated in Figure 2. Although both samples have essentially identical particle sizes (not shown), their morphologies are significantly different. Processing under acidic conditions leads to the formation of nanosized linear silicate 'building block' which are woven tightly together in the final gel matrix, to produce a microporous material (pore diameters 2 nm). The different morphologies are clearly reflected in the release rate of the encapsulated species from the respective matrices; rapid release kinetics are evident for the mesoporous material (high pH), while significantly slower release rates are obtained for the microporous material (low pH). A combined sol-gel/emulsion processing method has been developed to produce inorganic matrices with tailored nanostructures containing encapsulated organic and

  10. Sol-gel synthesis of hydroxyapatite; Sintese de hidroxiapatita via sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P., E-mail: michelledunin@yahoo.com.b [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil)

    2010-07-01

    Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

  11. Highly dispersed spherical Bi3.25La0.75Ti3O12 nanocrystals via topotactic crystallization of aggregation-free gel particles from an effective inverse miniemulsion sol-gel approach

    Science.gov (United States)

    Wang, Aijun; Zeng, Yanwei; Han, Longxiang; Ding, Chuan; Cao, Liangliang; Li, Rongjie

    2015-09-01

    Aggregation-free spherical lanthanum-doped bismuth titanate (Bi3.25La0.75Ti3O12, BLT) gel particles with an average size of about 150 nm were successfully obtained from an inverse miniemulsion sol-gel process, with Span-80 acting as surfactant, n-butanol as co-surfactant, cyclohexane as continuous phase, and submicro-droplets of aqueous solution containing Bi3+, La3+ and Ti4+ ions as dispersed phase, and then topotactically transformed into highly dispersed spherical BLT nanocrystals after an in situ crystallization at 600 °C for 8 h. It has been found that the BLT gel particles can be obtained via a moderate sol-gel reaction inside the miniemulsion droplets at 65 °C, but their morphology and aggregation degree are strongly affected by the relative amounts of Span-80 and n-butanol. The perfect spherical BLT gel particles with no aggregation can be achieved only under the condition of 3 wt% n-butanol relative to the mass of cyclohexane, with excessive amount of n-butanol leading to the formation of ill-gelled particles with irregular shapes, while insufficient addition of n-butanol resulting in terrible aggregation of gel particles. To understand the formation of aggregation-free spherical BLT gel particles, a tentative mechanism is proposed and discussed, which reveals that a well-coordinated oil-water interfacial film made up of Span-80 and n-butanol molecules and the appropriately enhanced evaporation of water from such interfaces should be responsible for the formation of aggregation-free spherical BLT gel particles.

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

    Science.gov (United States)

    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.

  13. Preparation of high laser-induced damage threshold Ta{sub 2}O{sub 5} films

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Cheng, E-mail: xucheng@cumt.edu.cn [School of Materials Science and Engineering, China University of Mining and Technology, Xuzhou 221116 (China); Yi, Peng; Fan, Heliang; Qi, Jianwei; Yang, Shuai; Qiang, Yinghuai; Liu, Jiongtian [School of Materials Science and Engineering, China University of Mining and Technology, Xuzhou 221116 (China); Li, Dawei [Key Laboratory of High Power Laser Materials, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China)

    2014-08-01

    High laser-induced damage threshold (LIDT) Ta{sub 2}O{sub 5} films were prepared by the sol–gel method using TaCl{sub 5} as a new precursor. The optical properties, surface morphologies, chemical composition, absorption and LIDT of the films were investigated. The results showed that the transparent and homogenous Ta{sub 2}O{sub 5} films had small surface roughness, low absorption and high LIDT even with large number of layers. The maximum LIDT at 1064 nm and 12 ns of the films was 24.8 J/cm{sup 2}. The ion chromatograph and Fourier transform infrared spectrum were used to reveal the functions of the addition of H{sub 2}O{sub 2} in the sol formation. It was shown that H{sub 2}O{sub 2} had two important functions, which were the decrease of Cl element content and the rapid generation of tantalum oxide. The high LIDT achieved was mainly due to the nearly free of defects in the films.

  14. Bioactive materials for biomedical applications using sol-gel technology

    International Nuclear Information System (INIS)

    Gupta, Radha; Kumar, Ashok

    2008-01-01

    This review paper focuses on the sol-gel technology that has been applied in many of the potential research areas and highlights the importance of sol-gel technology for preparing bioactive materials for biomedical applications. The versatility of sol-gel chemistry enables us to manipulate the characteristics of material required for particular applications. Sol-gel derived materials have proved to be good biomaterials for coating films and for the construction of super-paramagnetic nanoparticles, bioactive glasses and fiberoptic applicators for various biomedical applications. The introduction of the sol-gel route in a conventional method of preparing implants improves the mechanical strength, biocompatibility and bioactivity of scaffolds and prevents corrosion of metallic implants. The use of organically modified silanes (ORMOSILS) yields flexible and bioactive materials for soft and hard tissue replacement. A novel approach of nitric-oxide-releasing sol-gels as antibacterial coatings for reducing the infection around orthopedic implants has also been discussed

  15. Recubrimientos de hidroxiapatita preparados mediante un proceso sol-gel

    Directory of Open Access Journals (Sweden)

    Peón, E.

    2005-12-01

    Full Text Available Hydroxyapatite coatings (HAp have been obtained starting from precursors of sol-gel type. The coatings previously oxidized were deposited on metal surfaces of a based on iron alloy so-called MA956. The alloys were at high temperatures, in order to improve the adhesion with the hydroxyapatite coatings. The sol-gel coating was obtained applying an aqueous route, using triethyl phosphite and aqueous calcium nitrate, as precursors of phosphorous and calcium, respectively. Different sintering thermal treatments were applied on the resulting gels in order to obtain a homogeneous, adherent and crystalline hydroxyapatite coating. The characterization techniques used for this study were optical microscopy, SEM/EDX, XDR and FTIR. Moreover, the adhesion between the hydroxylapatite coating and the substrate was assessed according to the ASTM D 3359-02 standard test method. The results of this study showed that the best thermal treatment is obtained for a sintering temperature of 550 °C during a time of 72 h.

    Se han preparado nuevos recubrimientos de hidroxiapatita (HAp obtenidos a partir de precursores de tipo sol-gel, depositados sobre sustratos metálicos de una aleación de base hierro denominada MA956, previamente oxidados a elevadas temperaturas, para mejorar la adherencia con los recubrimientos de hidroxiapatita. El recubrimiento sol-gel se obtuvo aplicando una ruta acuosa, utilizando como precursores del fósforo y del calcio trietilfosfito y nitrato cálcico tetrahidratado, respectivamente. Sobre los geles resultantes se aplicaron distintos tratamientos térmicos de sinterización, hasta la obtención de recubrimientos de hidroxiapatita homogéneos, adherentes y cristalinos. Las técnicas de caracterización utilizadas para realizar este estudio han sido microscopía óptica, MBE/EDX, DRX y FTIR. Así mismo, se ha determinado la adherencia entre el substrato y el recubrimiento de hidroxiapatita según la norma ASTM D 3359-02. Los resultados

  16. Efficacy of a new tan doped sol-gel sorbent for uptake of zinc

    International Nuclear Information System (INIS)

    Khan, A.; Ahmed, S.; Riaz, M.; Mahmood, F.; Younas Khokhar, M.

    2003-01-01

    A TAN (1-(2-Thiazolylazo)-2-naphthol) doped sol gel silica sorbent (reddish colour, porous, stable, hard, non-swelling) were prepared and investigated for the removal of Zn (II) from aqueous solutions. The kinetics, adsorption isotherm, equilibration time and pH effect on the removal were studied from non competitive aqueous solution to optimize the conditions to be utilized on a large scale. Fast equilibration was observed and adsorption equilibria were reached within 30 minutes. Adsorption of zinc ions on the blank (un-doped) sol gel was found negligible. The maximum adsorption of Zn (II) ions onto the TAN doped sol-gel from single solutions were 2.33 mg/g (0.035 mmol/g). TAN doped sol gel can be regenerated through washing with a solution of 0.1 M HCl solution. The maximum regeneration value was as high as 99.0%. The TAN-doped sol gel silica is suitable at least for four adsorption-desorption cycles without experiencing considerable loss of adsorption capacity. The uptake route and the nature of the Zn-TAN complex have been discussed. (orig.)

  17. Screen-printable sol-gel enzyme-containing carbon inks.

    Science.gov (United States)

    Wang, J; Pamidi, P V; Park, D S

    1996-08-01

    Enzymes usually cannot withstand the high-temperature curing associated with the thick-film fabrication process and require a separate immobilization step in connection with the production of single-use biosensors. We report on the development of sol-gel-derived enzyme-containing carbon inks that display compatibility with the screen-printing process. Such coupling of sol-gel and thick-film technologies offers a one-step fabrication of disposable enzyme electrodes, as it obviates the need for thermal curing. The enzyme-containing sol-gel carbon ink, prepared by dispersing the biocatalyst, along with the graphite powder and a binder, within the sol-gel precursors, is cured very rapidly (10 min) at low temperature (4 °C). The influence of the ink preparation conditions is explored, and the sensor performance is evaluated in connection with the incorporation of glucose oxidase or horseradish peroxidase. The resulting strips are stable for at least 3 months. Such sol-gel-derived carbon inks should serve as hosts for other heat-sensitive biomaterials in connection with the microfabrication of various thick-film biosensors.

  18. Abstracts of International Conference on Sol-Gel Materials' 04

    International Nuclear Information System (INIS)

    2004-01-01

    International Conference on Sol-Gel Materials '04 was an important forum for discussion on problems related to sol-gel processes applied for preparation materials with special physical properties and assignment. The application of sol-gel materials as phosphors, surface coatings, sensors, waveguides, medical implants, joints etc. has been presented. Preparation conditions, methods of physical characterization as well as optimal chemical composition of such materials have been also discussed in detail

  19. Current and future possibilities of sol-gel process

    International Nuclear Information System (INIS)

    Sakka, Sumio

    2004-01-01

    The sol-gel method is characterized by the low temperature processing. Since this method starts from solutions, the product is essentially nanomaterials. So far, various kinds of microstructures, including dense, porous, hybrid, amorphous and crystalline microstructures have been realized. Accordingly, sol-gel materials cover a wide range of functions, such as optical, electronic, mechanical, chemical and bio-functions. Future perspectives of the sol-gel method are described in the article. (author)

  20. Industrial applications of sol-gel technology

    International Nuclear Information System (INIS)

    Tuloch, S.M.; Tulloch, G.E.

    1995-01-01

    The purpose of this paper has been to provide a broad, rather than comprehensive view. We have presented a range of applications and only a selection of involved companies and researchers and have relied to a large extent on published information. Nevertheless, we are sure that our view of the importance of Sol-gel technology as an emerging technology, with enormous impact across a wide range of manufacturing, is demonstrated. Applications which are either in production or have been foreshadowed include four broad categories: coatings, fibres, powders and monoliths

  1. Modelling single shot damage thresholds of multilayer optics for high-intensity short-wavelength radiation sources

    NARCIS (Netherlands)

    Loch, R.A.; Sobierajski, R.; Louis, Eric; Bosgra, J.; Bosgra, J.; Bijkerk, Frederik

    2012-01-01

    The single shot damage thresholds of multilayer optics for highintensity short-wavelength radiation sources are theoretically investigated, using a model developed on the basis of experimental data obtained at the FLASH and LCLS free electron lasers. We compare the radiation hardness of commonly

  2. Nanostructured energetic materials derived from sol-gel chemistry

    International Nuclear Information System (INIS)

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

    2000-01-01

    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

  3. Effect of concentrations of plasticizers on the sol-gel properties developed from alkoxides precursors

    Energy Technology Data Exchange (ETDEWEB)

    Kunst, Sandra Raquel; Longhi, Marielen; Zini, Lucas Pandolphi [Universidade de Caxias do Sul (CCET/UCS), Caxias do Sul, RS (Brazil). Centro de Ciências Exatas e Tecnologia; Beltrami, Lilian Vanessa Rossa; Boniatti, Rosiana; Cardoso, Henrique Ribeiro Piaggio; Vega, Maria Rita Ortega; Malfatti, Célia de Fraga, E-mail: lvrossa@yahoo.com.br [Universidade Federal do Rio Grande do Sul (LAPEC/UFRGS), Porto Alegre, RS (Brazil). Laboratorio de Pesquisa em Corrosão

    2017-07-01

    Coatings developed through sol-gel method is presented as an interesting replacement to chromium coating. Sol-gel method present advantages as high purity and excellent distribution of the components. The objective of this work is to synthesize and characterize a film obtained by sol-gel route. The film was prepared with 3-(trimethoxysilylpropyl) methacrylate (TMSPMA), tetraethoxysilane (TEOS) and cerium nitrate, using water and ethanol as solvents. Polyethyleneglycol (PEG) plasticizer was added at four different concentrations. The sol was characterized by techniques of viscosity, thermogravimetric analysis (TGA), X-ray diffraction (XRD) nuclear magnetic resonance spectroscopy (NMR) and Fourier transform infrared spectroscopy (FT-IR). The results showed that tetrafunctional alkoxides condensation was retarded by the plasticizer, forming a compact film. The film with 20 g.L-1 of PEG showed the best electrochemical behavior. (author)

  4. Effect of concentrations of plasticizers on the sol-gel properties developed from alkoxides precursors

    Directory of Open Access Journals (Sweden)

    Sandra Raquel Kunst

    Full Text Available Abstract Coatings developed through sol-gel method is presented as an interesting replacement to chromium coating. Sol-gel method present advantages as high purity and excellent distribution of the components. The objective of this work is to synthesize and characterize a film obtained by sol-gel route. The film was prepared with 3-(trimethoxysilylpropyl methacrylate (TMSPMA, tetraethoxysilane (TEOS and cerium nitrate, using water and ethanol as solvents. Polyethyleneglycol (PEG plasticizer was added at four different concentrations. The sol was characterized by techniques of viscosity, thermogravimetric analysis (TGA, X-ray diffraction (XRD nuclear magnetic resonance spectroscopy (NMR and Fourier transform infrared spectroscopy (FT-IR. The results showed that tetrafunctional alkoxides condensation was retarded by the plasticizer, forming a compact film. The film with 20 g.L-1 of PEG showed the best electrochemical behavior.

  5. Thermal stability of octadecylsilane hybrid silicas prepared by grafting and sol-gel methods

    International Nuclear Information System (INIS)

    Brambilla, Rodrigo; Santos, Joao H.Z. dos; Miranda, Marcia S.L.; Frost, Ray L.

    2008-01-01

    Hybrid silicas bearing octadecylsilane groups were prepared by grafting and sol-gel (SG) methods. The effect of the preparative route on the thermal stability was evaluated by means of thermal gravimetric analysis (TGA), infrared emission spectroscopy (IRES) and, complementary, by 13 C solid-state nuclear magnetic resonance ( 13 C NMR) and matrix assisted laser deionization time of flight mass spectroscopy (MALDI-TOF-MS). Silicas prepared by the grafting route seem to be slightly more stable than those produced by the sol-gel method. This behavior seems to be associated to the preparative route, since grafting affords a liquid-like conformation, while in the case of sol-gel a highly organized crystalline chain conformation was observed

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

    Science.gov (United States)

    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.

  7. Sol-gel precursors and products thereof

    Science.gov (United States)

    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##

  8. Sol-gel method for encapsulating molecules

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    McClure, Zachary D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Padilla Cintron, Cristina [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    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.

  10. Study of silica sol-gel materials for sensor development

    Science.gov (United States)

    Lei, Qiong

    Silica sol-gel is a transparent, highly porous silicon oxide glass made at room temperature by sol-gel process. The name of silica sol-gel comes from the observable physical phase transition from liquid sol to solid gel during its preparation. Silica sol-gel is chemically inert, thermally stable, and photostable, it can be fabricated into different desired shapes during or after gelation, and its porous structure allows encapsulation of guest molecules either before or after gelation while still retaining their functions and sensitivities to surrounding environments. All those distinctive features make silica sol-gel ideal for sensor development. Study of guest-host interactions in silica sol-gel is important for silica-based sensor development, because it helps to tailor local environments inside sol-gel matrix so that higher guest loading, longer shelf-life, higher sensitivity and faster response of silica gel based sensors could be achieved. We focused on pore surface modification of two different types of silica sol-gel by post-grafting method, and construction of stable silica hydrogel-like thin films for sensor development. By monitoring the mobility and photostability of rhodamine 6G (R6G) molecules in silica alcogel thin films through single molecule spectroscopy (SMS), the guest-host interactions altered by post-synthesis grafting were examined. While physical confinement remains the major factor that controls mobility in modified alcogels, both R6G mobility and photostability register discernable changes after surface charges are respectively reversed and neutralized by aminopropyltriethoxysilane (APTS) and methyltriethoxysilane (MTES) grafting. The change in R6G photostability was found to be more sensitive to surface grafting than that of mobility. In addition, silica film modification by 0.4% APTS is as efficient as that by pure MTES in lowering R6G photostability, which suggests that surface charge reversal is more effective than charge neutralization

  11. Fabrication of superhydrophobic sol-gel composite films using hydrophobically modified colloidal zinc hydroxide.

    Science.gov (United States)

    Lakshmi, R V; Basu, Bharathibai J

    2009-11-15

    A superhydrophobic sol-gel composite film was fabricated by incorporating hydrophobically modified colloidal zinc hydroxide (CZH) in sol-gel matrix. CZH was prepared by controlled precipitation and modified by treatment with stearic acid. The concentration of stearic acid and stirring time were optimized to obtain modified CZH with very high water contact angle (WCA) of 165 degrees and sliding angle (SA)superhydrophobic surfaces. FTIR spectrum also confirmed the presence of zinc stearate in the composite film. The method is simple and cost-effective and does not involve any expensive chemicals or equipments.

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

    Science.gov (United States)

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

    2012-12-18

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

  13. All-silica nanofluidic devices for DNA-analysis fabricated by imprint of sol-gel silica with silicon stamp

    DEFF Research Database (Denmark)

    Mikkelsen, Morten Bo Lindholm; Letailleur, Alban A; Søndergård, Elin

    2011-01-01

    We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination of the imprin......We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination...... of the imprinted hybrid sol-gel material produces purely inorganic silica, which has very low autofluorescence and can be fusion bonded to a glass lid. Compared to top-down processing of fused silica or silicon substrates, imprint of sol-gel silica enables fabrication of high-quality nanofluidic devices without...

  14. Brilliant molecular nanocrystals emerging from sol-gel thin films: towards a new generation of fluorescent biochips

    International Nuclear Information System (INIS)

    Dubuisson, E; Monnier, V; Sanz-Menez, N; Ibanez, A; Boury, B; Usson, Y; Pansu, R B

    2009-01-01

    To develop highly sensitive biosensors, we made directly available to biological aqueous solutions organic nanocrystals previously grown in the pores of sol-gel films. Through the controlled dissolution of the sol-gel surface, we obtained emerging nanocrystals that remained strongly anchored to the sol-gel coating for good mechanical stability of the final sensing device. We demonstrated that in the presence of a solution of DNA functionalized with a molecular probe, the nanocrystal fluorescence is strongly quenched by Foerster resonance energy transfer thus opening the way towards very sensitive fluorescent biosensors through biomolecules grafted onto fluorescent nanocrystals. Finally, this controlled dissolution, involving weak concentrated NaOH solution, is a generic process that can be used for the thinning of any kind of sol-gel layer.

  15. Study of Different Sol-Gel Coatings to Enhance the Lifetime of PDMS Devices: Evaluation of Their Biocompatibility.

    Science.gov (United States)

    Aymerich, María; Gómez-Varela, Ana I; Álvarez, Ezequiel; Flores-Arias, María T

    2016-08-25

    A study of PDMS (polydimethylsiloxane) sol-gel-coated channels fabricated using soft lithography and a laser direct writing technique is presented. PDMS is a biocompatible material that presents a high versatility to reproduce several structures. It is widely employed in the fabrication of preclinical devices due to its advantages but it presents a rapid chemical deterioration to organic solvents. The use of sol-gel layers to cover the PDMS overcomes this problem since it provides the robustness of glass for the structures made with PDMS, decreasing its deterioration and changing the biocompatibility of the surface. In this work, PDMS channels are coated with three different kinds of sol-gel compositions (60MTES/40TEOS, 70MTES/30TISP and 80MTES/20TISP). The endothelial cell adhesion to the different coated devices is evaluated in order to determine the most suitable sol-gel preparation conditions to enhance cellular adhesion.

  16. Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

    Science.gov (United States)

    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…

  17. Reversible sol-gel-sol medium for enzymatic optical biosensors

    NARCIS (Netherlands)

    Safaryan, S.; Yakovlev, A.; Pidko, E.A.; Vinogradov, A.; Vinogradov, V.

    2017-01-01

    In this paper we for the first time report a reversible sol-gel-sol approach to obtain optical enzymatic biosensors with improved enzyme stability and good sensitivity by using desktop inkjet printing. The developed technique is based on the bio-inorganic inks allowing for a sol-gel-sol transition

  18. Self-Healing Corrosion Protective Sol-Gel Coatings

    NARCIS (Netherlands)

    Abdolah Zadeh, M.

    2016-01-01

    Inspired by the state of the art and the recent advances in the field of self-healing corrosion protective coatings, the thesis entitled “Self-healing corrosion protective sol-gel coatings” addresses novel routes to self-healing corrosion protective sol-gel coatings via extrinsic and intrinsic

  19. Matrix molecularly imprinted mesoporous sol-gel sorbent for efficient solid-phase extraction of chloramphenicol from milk.

    Science.gov (United States)

    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

  20. Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method. Optimisation, characterisation and rheology.

    Science.gov (United States)

    Tredwin, Christopher J; Young, Anne M; Georgiou, George; Shin, Song-Hee; Kim, Hae-Won; Knowles, Jonathan C

    2013-02-01

    Currently, most titanium implant coatings are made using hydroxyapatite and a plasma spraying technique. There are however limitations associated with plasma spraying processes including poor adherence, high porosity and cost. An alternative method utilising the sol-gel technique offers many potential advantages but is currently lacking research data for this application. It was the objective of this study to characterise and optimise the production of Hydroxyapatite (HA), fluorhydroxyapatite (FHA) and fluorapatite (FA) using a sol-gel technique and assess the rheological properties of these materials. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethylphosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the sol-gel derived FHA and FA. Optimisation of the chemistry and subsequent characterisation of the sol-gel derived materials was carried out using X-ray Diffraction (XRD) and Differential Thermal Analysis (DTA). Rheology of the sol-gels was investigated using a viscometer and contact angle measurement. A protocol was established that allowed synthesis of HA, FHA and FA that were at least 99% phase pure. The more fluoride incorporated into the apatite structure; the lower the crystallisation temperature, the smaller the unit cell size (changes in the a-axis), the higher the viscosity and contact angle of the sol-gel derived apatite. A technique has been developed for the production of HA, FHA and FA by the sol-gel technique. Increasing fluoride substitution in the apatite structure alters the potential coating properties. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

  1. Superconductive ceramics obtained with sol gel method

    International Nuclear Information System (INIS)

    Arcangeli, A.; Mosci, A.; Nardi, A.; Vatteroni, R.; Zondini, C.

    1988-01-01

    Several sol gel routes have been considered, studied and developed to produce large quantities of granulates which can be processed to obtain ceramics having good superconducting characteristics. In the considered process a mixture of commercial nitrates is atomized, at room temperature, in a solution 1:1 of Primene JMT and Benzene and a pale blue gel of the starting elements is suddently formed. The granulates obtained are free flowing, very reactive and well suited for pressing. For their intrinsic characteristics they could be very good precursors for the production of large quantities of superconductive ceramics in different forms. The precipitated gel is dried, calcinated, pressed in the form of cylindrical pellets which are sintered up to 960 degrees C. No griding or different thermal treatments are needed. The sintered material has low electric resistence, shows a clear Meissner effect and has a transition temperature of between 91 and 95 K

  2. Processing, adhesion and electrical properties of silicon steel having non-oriented grains coated with silica and alumina sol-gel

    International Nuclear Information System (INIS)

    Vasconcelos, D.C.L.; Orefice, R.L.; Vasconcelos, W.L.

    2007-01-01

    Silicon steels having non-oriented grains are usually coated with a series of inorganic or organic films to be used in electrical applications. However, the commercially available coatings have several disadvantages that include poor adhesion to the substrates, low values of electrical resistance and degradation at higher temperatures. In this work, silica and alumina sol-gel films were deposited onto silicon steel in order to evaluate the possibility of replacing the commercially available coatings by these sol-gel derived materials. Silica and alumina sol-gel coatings were prepared by dipping silicon steel samples into hydrolyzed silicon or aluminum alkoxides. Samples coated with sol-gel films were studied by scanning electron microscopy, energy dispersive spectroscopy and infrared spectroscopy. Adhesion between silicon steel and sol-gel films was measured by using several standard adhesion tests. Electrical properties were evaluated by the Franklin method. Results showed that homogeneous sol-gel films can be deposited onto silicon steel. Thicknesses of the films could be easily managed by altering the speed of deposition. The structure of the films could also be tailored by introducing additives, such as nitric acid and N,N-dimethyl formamide. Adhesion tests revealed a high level of adhesion between coatings and metal. The Franklin test showed that sol-gel films can produce coated samples with electrical resistances suitable for electrical applications. Electrical properties of the coated samples could also be manipulated by altering the structure of the sol-gel films or by changing the thickness of them

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

    Science.gov (United States)

    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

  4. Study of the luminescence of tris(2-thenoyltrifluoroacetonato)lanthanide(III) complexes covalently linked to 1,10-phenanthroline-functionalized hybrid sol-gel glasses

    International Nuclear Information System (INIS)

    Lenaerts, Philip; Ryckebosch, Eline; Driesen, Kris; Deun, Rik van; Nockemann, Peter; Goerller-Walrand, Christiane; Binnemans, Koen

    2005-01-01

    The solubility and uniform distribution of lanthanide complexes in sol-gel glasses can be improved by covalently linking the complexes to the sol-gel matrix. In this study, several lanthanide β-diketonate complexes (Ln=Nd, Sm, Eu, Tb, Er, Yb) were immobilized on a 1,10-phenanthroline functionalized sol-gel glass. For the europium(III) complex, a sol-gel material of diethoxydimethylsilane (DEDMS) with polymer-like properties was derived. For the other lanthanide complexes, the sol-gel glass was prepared by using a matrix of tetramethoxysilane (TMOS) and DEDMS. Both systems were prepared under neutral reaction conditions. High-resolution emission and excitation spectra were recorded. The luminescence lifetimes were measured

  5. Sol-Gel-Hydrothermal Synthesis of the Heterostructured TiO2/N-Bi2WO6 Composite with High-Visible-Light- and Ultraviolet-Light-Induced Photocatalytic Performances

    Directory of Open Access Journals (Sweden)

    Jiang Zhang

    2012-01-01

    Full Text Available The heterostructured TiO2/N-Bi2WO6 composites were prepared by a facile sol-gel-hydrothermal method. The phase structures, morphologies, and optical properties of the samples were characterized by using X-ray powder diffraction (XRD, scanning electron microscopy (SEM, high-resolution transmission electron microscopy (HRTEM, energy dispersive spectroscopy (EDS, and UV-vis diffuse reflectance spectroscopy. The photocatalytic activities for rhodamine B of the as-prepared products were measured under visible and ultraviolet light irradiation at room temperature. The TiO2/N-Bi2WO6 composites exhibited much higher photocatalytic performances than TiO2 as well as Bi2WO6. The enhancement in the visible light photocatalytic performance of the TiO2/N-Bi2WO6 composites could be attributed to the effective electron-hole separations at the interfaces of the two semiconductors, which facilitate the transfer of the photoinduced carriers.

  6. Structure and properties of carbon nanotubes/sol-gel nanocomposites

    International Nuclear Information System (INIS)

    Pokrass, Mariana

    2013-08-01

    Carbon Nanotubes (CNTs) are promising filler materials owing to their exceptional mechanical, electrical, thermal and optical properties. Since their discovery in 1991, a major effort has been made in developing CNT-polymer nanocomposites, whereas CNT/ceramic based nanocomposites, in particularly, CNT/silica nanocomposites, have been very little studied. This thesis focuses on preparation and characterization of novel CNT/silica nanocomposite glasses synthesized by the Sol-Gel technology. A comprehensive analysis of their morphological, optical, and electrical properties was conducted, and analyzed according to existing theoretical models. The nanocomposites hosting matrix is a hybrid organic/inorganic glass prepared by the Fast-Sol-Gel (FSG) route. Using specific conditions in the FSG procedure, the resultant glasses are nonporous, exhibiting no contraction upon drying. Their analogous Classical-Sol-Gel (CSG) glasses, however, are porous, and do exhibit contraction upon drying. The FSG glasses are relatively new materials, and their physical and optical properties were only meagerly studied. In our present work we have conducted a comprehensive experimental research on some previously ignored characteristics such as: UV-vis-IR optical absorption and transmission, and the organic content effect on the refraction index n, density ρ, thermal expansion coefficient β, and thermo-optic coefficient dn/dT. We found that organic residues within the glass decrease the refractive index, density, and thermo-optic coefficient. The thermal expansion coefficient, however, increases with the organic content. A negative linear dependence of the thermo-optic coefficient on the thermal expansion coefficient was obtained. CNT/FSG nanocomposites were prepared by using a solution mixing method, while CNT/CSG nanocomposites were prepared by means of an in situ polymerization technique. Nanocomposites based on FSG hybrid glasses were characterized for their nonlinear optical and

  7. Sol-Gel Glass Holographic Light-Shaping Diffusers

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-04-15

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

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

    International Nuclear Information System (INIS)

    Kim, Dae-Sung; Ryu, Bong-ki

    2017-01-01

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

  10. Sol-gel preparation of uranium oxide spheres

    International Nuclear Information System (INIS)

    Dolezal, J.; Urbanek, V.

    1978-01-01

    Information is presented on problems of preparing nuclear fuel by the sol-gel method. Basic data on different process types are given. A more detailed description of the method of preparation of spherical particles of uranium oxide gel developed and used at the Nuclear Research Institute at Rez is given. Advantages and disadvantages of sol-gel materials are discussed in comparison with fuel materials prepared by classical precipitation methods. The feasibility of the sol-gel methods for preparing other materials is shortly mentioned and their application outlined. (author)

  11. Spatially resolved speckle-correlometry of sol-gel transition

    Science.gov (United States)

    Isaeva, A. A.; Isaeva, E. A.; Pantyukov, A. V.; Zimnyakov, D. A.

    2018-04-01

    Sol-gel transition was studied using the speckle correlometry method with a localized light source and spatial filtering of backscattered radiation. Water solutions of technical or food gelatin with added TiO2 nanoparticles were used as studied objects. Structural transformation of "sol-gel" system was studied at various temperatures from 25°C to 50°C using analysis of the correlation and structure functions of speckle intensity fluctuations. The characteristic temperatures of "sol - gel" transition were evaluated for studied systems. Obtained results can be used for various applications in biomedicine and food industry.

  12. Amperometric biosensor for hydrogen peroxide based on hemoglobin entrapped in titania sol-gel film

    International Nuclear Information System (INIS)

    Yu Jiuhong; Ju Huangxian

    2003-01-01

    Hemoglobin (Hb) was entrapped in a titania sol-gel matrix and used as a mimetic peroxidase to construct a novel amperometric biosensor for hydrogen peroxide. The Hb entrapped titania sol-gel film was obtained with a vapor deposition method, which simplified the traditional sol-gel process for protein immobilization. The morphologies of both titania sol-gel and the Hb films were characterized using scanning electron microscopy (SEM) and proved to be chemically clean, porous, homogeneous. This matrix provided a biocompatible microenvironment for retaining the native structure and activity of the entrapped Hb and a very low mass transport barrier to the substrates. H 2 O 2 could be reduced by the catalysis of the entrapped hemoglobin at -300 mV without any mediator. The reagentless H 2 O 2 sensor exhibited a fast response (less than 5 s) and sensitivity as high as 1.29 mA mM -1 cm -2 . The linear range for H 2 O 2 determination was from 5.0x10 -7 to 5.4x10 -5 M with a detection limit of 1.2x10 -7 M. The apparent Michaelis-Menten constant of the encapsulated hemoglobin was calculated to be 0.18±0.02 mM. The stability of the biosensor was also evaluated

  13. Foldable and Cytocompatible Sol-gel TiO2 Photonics.

    Science.gov (United States)

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

    2015-09-07

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

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

    Science.gov (United States)

    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

  15. Development of novel biocompatible hybrid nanocomposites based on polyurethane-silica prepared by sol gel process

    Energy Technology Data Exchange (ETDEWEB)

    Rashti, Ali [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Yahyaei, Hossein [Department of Polymer Engineering and Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Firoozi, Saman [Department of Tissue Engineering & Regenerative Medicine, Faculty of Advanced Technologies in Medicine, Iran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Ramezani, Sara [Department of Neuroscience, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Rahiminejad, Ali [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Karimi, Roya [Department of Tissue Engineering and Applied Cell Science, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Farzaneh, Khadijeh [Tehran Heart Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Mohseni, Mohsen [Department of Polymer Engineering and Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Ghanbari, Hossein, E-mail: hghanbari@tums.ac.ir [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Tehran Heart Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Medical Biomaterials Research Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of)

    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. - Highlights: • Nanocomposites based on polyurethane and nanosilica prepared by sol-gel method fabricated • Addition of inorganic phase improved mechanical properties. • Nanosilica prepared by sol-gel method increased hydrophilicity. • By adding nanosilica to polyurethane biocompatibility increased significantly.

  16. Variables of synthesis in obtaining nanosilicas with sol-gel

    International Nuclear Information System (INIS)

    Elia, A; Martin-Aispuro, P; Musante, L; Martin-Martinez, J.M; Vazquez, P

    2008-01-01

    Amorphous silica materials and polycrystalline are now being developed for different applications as optic components, superconductors, nano-particles used as charges in adhesives and paints, among others. Some methods of obtaining these materials involve complex techniques and high costs. Generally, the materials constituents are fused, for example, using the pyrogenic silica technique, widely used industrially. Meanwhile, the sol-gel meted is based on a mixture of liquid reagents at the molecular level, to easily obtain amorphous and polycrystalline materials, even at room temperature. Therefore, the sol-gel way is a promising option for producing new materials, due to its cost advantages compared to the traditional methods. The sol-gel technique consists of the simultaneous reaction of the hydrolysis and the condensation. In this process the precursor solution, the TEOS in our case, becomes a polymeric gel network polymer. The partial hydrolysis of the orthosilicate takes place when it is mixed with water and ethanol (EtOH), the reaction that occurs is: S i(OEt) 4 + H 2 O S i(OEt) 3 (OH) + EtOH. The condensation takes place between two OH groups or between an OH group and an ethoxy to form an oxygen bridge plus water or ethanol. S i(OEt) 4 + H 2 O + S i(OEt) 3 (OH)(EtO) 3 Si-O-Si(OEt) 3 (OH) + H 2 O S i-OH + HO-Si S i-O-Si + H 2 O. The addition of a base or of an acid catalyzes the process and changes the pH of the solution influencing the condensation process and size of the final particle. This work focuses on finding different conditions by varying the pH, using HCI, with and without agitation during the addition of the HCI, and washing the solid obtained with ethanol in order to study its effect. The nanosilicas were characterized by TEM-EDX, DTA-TGA, S BET , FT-IR, DRX, DRS, SEM and pH measurements. The morphology of the nanosilicas was characterized with SEM and TEM. Using these techniques a partial conclusion showed that the samples synthesized with HCI

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

    Science.gov (United States)

    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. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Electrophoretic Porosimetry of Sol-Gels

    Science.gov (United States)

    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.

  19. Safe and Environmentally Acceptable Sol-Gel-Derived Pyrophoric Pyrotechnics

    National Research Council Canada - National Science Library

    Simpson, Randall L; Hubble, William; Stevenson, Bradley; Gash, Alexander; Satcher, Joe; Metcalf, Patricia

    2004-01-01

    ...% H2 in Ar, N2, CO2, 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...

  20. Sol-Gel Derived, Nanostructured Oxide Lubricant Coatings

    National Research Council Canada - National Science Library

    Taylor, Douglas

    2000-01-01

    In this program, we deposited oxide coatings of titanium and nickel by wet-chemical deposition methods, also referred to as sol-gel, which showed excellent tribological properties in previous investigations...

  1. Sol-gel materials for optofluidics - process and applications

    DEFF Research Database (Denmark)

    Mikkelsen, Morten Bo Lindholm

    2011-01-01

    This Ph.D. thesis is concerned with the use of sol-gel materials in optofluidic applications and the physics of DNA molecules in nanoconfinement. The bottom-up formation of solid material, which is provided by the sol-gel process, enables control of the chemical composition and porosity...... of the material. At early stages of gelation, thin gel coatings can be structured by nanoimprint lithography, and purely inorganic silica materials can be obtained by subsequent thermal annealing. The sol-gel process thus constitutes a unique method for nanofabrication of silica materials of special properties....... In this work, sol-gel silica is introduced as a new material class for the fabrication of lab-on-a-chip devices for DNA analysis. An imprint process with a rigid, non-permeable stamp was developed, which enabled fabrication of micro- and nanofluidic silica channels in a single process step without use of any...

  2. Very high laser-damage threshold of polymer-derived Si(B)CN-carbon nanotube composite coatings.

    Science.gov (United States)

    Bhandavat, R; Feldman, A; Cromer, C; Lehman, J; Singh, G

    2013-04-10

    We study the laser irradiance behavior and resulting structural evolution of polymer-derived silicon-boron-carbonitride (Si(B)CN) functionalized multiwall carbon nanotube (MWCNT) composite spray coatings on copper substrate. We report a damage threshold value of 15 kWcm(-2) and an optical absorbance of 0.97 after irradiation. This is an order of magnitude improvement over MWCNT (1.4 kWcm(-2), 0.76), SWCNT (0.8 kWcm(-2), 0.65) and carbon paint (0.1 kWcm(-2), 0.87) coatings previously tested at 10.6 μm (2.5 kW CO2 laser) exposure. Electron microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy suggests partial oxidation of Si(B)CN forming a stable protective SiO2 phase upon irradiation.

  3. Sol-gel process for thermal reactor fuel fabrication

    International Nuclear Information System (INIS)

    Mukerjee, S.K.

    2008-01-01

    Full text: Sol-gel processes have revolutionized conventional ceramic technology by providing extremely fine and uniform powders for the fabrication of ceramics. The use of this technology for nuclear fuel fabrication has also been explored in many countries. Unlike the conventional sol-gel process, sol-gel process for nuclear fuels tries to eliminate the preparation of powders in view of the toxic nature of the powders particularly those of plutonium and 233 U. The elimination of powder handling thus makes this process more readily amenable for use in glove boxes or for remote handling. In this process, the first step is the preparation of microspheres of the fuel material from a solution which is then followed by vibro-compaction of these microspheres of different sizes to obtain the required smear density of fuel inside a pin. The maximum achievable packing density of 92 % makes it suitable for fast reactors only. With a view to extend the applicability of sol-gel process for thermal reactor fuel fabrication the concept of converting the gel microspheres derived from sol-gel process, to the pellets, has been under investigation for several years. The unique feature of this process is that it combines the advantages of sol-gel process for the preparation of fuel oxide gel microspheres of reproducible quality with proven irradiation behavior of the pellet fuel. One of the important pre-requisite for the success of this process is the preparation of soft oxide gel microspheres suitable for conversion to dense pellets free from berry structure. Studies on the internal gelation process, one of the many variants of sol-gel process, for obtaining soft oxide gel microspheres suitable for gel pelletisation is now under investigation at BARC. Some of the recent findings related to Sol-Gel Microsphere Pelletisation (SGMP) in urania-plutonia and thoria-urania systems will be presented

  4. Optical Studies on Sol-Gel Derived Lead Chloride Crystals

    OpenAIRE

    Rejeena, I; Lillibai, B; Nithyaja, B; Nampoori, P.N V; Radhakrishnan, P

    2013-01-01

    Optical characterization of lead chloride crystals prepared by sol-gel method is reported. The relevant sol-gel technique is used for the preparation of PbCl2 samples with five different types. In this paper, we report the absorption and fluorescence behaviour of pure, UV& IR irradiated and electric & magnetic field applied lead chloride crystal samples in solution phase at two different concentrations. Optical bandgap and emission studies of these crystals are also done.

  5. Sol-gel derived C-SiC composites and protective coatings for sustained durability in the space environment

    Science.gov (United States)

    Haruvy, Yair; Liedtke, Volker

    2003-09-01

    Composites and coatings were produced via the fast sol-gel process of a mixture of alkoxysilane precursors. The composites were comprised of carbon fibers, fabrics, or their precursors as reinforcement, and sol-gel-derived silicon carbide as matrix, aiming at high-temperature stable ceramics that can be utilized for re-entry structures. The protective coatings were comprised of fluorine-rich sol-gel derived resins, which exhibit high flexibility and coherence to provide sustained ATOX protection necessary for LEO space-exposed elements. For producing the composites, the sol-gel-derived resin is cast onto the reinforcement fibers/fabrics mat (carbon or its precursors) to produce a 'green' composite that is being cured. The 'green' composite is converted into a C-SiC composite via a gradual heat-pressure process under inert atmosphere, during which the organic substituents on the silicon atoms undergo internal oxidative pyrolysis via the schematic reaction: (SiRO3/2)n -> SiC + CO2 + H2O. The composition of the resultant silicon-oxi-carbide is tailorable via modifying the composition of the sol-gel reactants. The reinforcement, when made of carbon precursors, is converted into carbon during the heat-and-pressure processing as well. The C-SiC composites thus derived exhibit superior thermal stability and comparable thermal conductivity, combined with good mechanical strength features and failure resistance, which render them greatly applicable for re-entry shielding, heat-exchange pipes, and the like. Fluorine rich sol-gel derived coatings were developed as well, via the use of HF rich sol-gel process. These coatings provide oxidation-protection via the silica formation process, together with flexibility that allows 18,000 repetitive folding of the coating without cracking.

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

    Science.gov (United States)

    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.

  7. Silica Sol-Gel Entrapment of the Enzyme Chloro peroxidase

    International Nuclear Information System (INIS)

    Le, T.; Chan, S.; Ebaid, B.; Sommerhalter, M.

    2015-01-01

    The enzyme chloro peroxidase (CPO) was immobilized in silica sol-gel beads prepared from tetramethoxysilane. The average pore diameter of the silica host structure (∼3 nm) was smaller than the globular CPO diameter (∼6 nm) and the enzyme remained entrapped after sol-gel maturation. The catalytic performance of the entrapped enzyme was assessed via the pyrogallol peroxidation reaction. Sol-gel beads loaded with 4 μg CPO per mL sol solution reached 9-12% relative activity compared to free CPO in solution. Enzyme kinetic analysis revealed a decrease in K_cat but no changes in K_M or K_I . Product release or enzyme damage might thus limit catalytic performance. Yet circular dichroism and visible absorption spectra of transparent CPO sol-gel sheets did not indicate enzyme damage. Activity decline due to methanol exposure was shown to be reversible in solution. To improve catalytic performance the sol-gel protocol was modified. The incorporation of 5, 20, or 40% methyltrimethoxysilane resulted in more brittle sol-gel beads but the catalytic performance increased to 14% relative to free CPO in solution. The use of more acidic casting buffers (ph 4.5 or 5.5 instead of 6.5) resulted in a more porous silica host reaching up to 18% relative activity

  8. Synthesis, growth and characterization of o-phenylinediaminium benzilate: An SHG material with high laser damage threshold for NLO applications

    Science.gov (United States)

    Rajkumar, M.; Chandramohan, A.

    2017-02-01

    An organic molecular charge transfer complex salt, o-phenylenediaminium benzilate was synthesized and single crystals grown by slow solvent evaporation solution growth technique in methanol at ambient temperature. The grown crystal was subjected to Single crystal XRD analysis to establish the molecular structure. The molecular structure was further confirmed by 1H and 13C NMR spectral studies. The formation of the charge transfer complex salt was confirmed by UV-VIS spectroscopic technique. To identify the optical transmittance window and lower wavelength cut-off, the crystal was subjected to UV-Vis-NIR transmission spectral studies. The presence of various functional groups in the salt crystal was confirmed by FT-IR spectroscopic technique. Photoluminescence study was carried out to explore its efficiency towards device fabrications. The TG and DTA thermal analyses were simultaneously carried out to establish the thermal stability of the crystal. The dielectric studies of the grown crystal were executed at different temperatures as a function of frequency to investigate its electrical properties. The SHG efficiency of the crystal was determined using the modified Kurtz and Perry powder technique and its value was found to be 1.98 times that of the KDP crystal. Laser damage threshold value was measured using Nd:YAG laser. The mechanical stability of the title crystal was established employing Vickers micro hardness tester.

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

    Science.gov (United States)

    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. © 2014 Entomological Society of America.

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

    Science.gov (United States)

    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.

  11. Sol-gel optical thin films for an advanced megajoule-class Nd:glass laser ICF-driver

    International Nuclear Information System (INIS)

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

    1995-01-01

    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 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

  12. Preparation of highly oriented Al:ZnO and Cu/Al:ZnO thin films by sol-gel method and their characterization

    Energy Technology Data Exchange (ETDEWEB)

    Vijayaprasath, G.; Murugan, R. [School of Physics, Alagappa University, Karaikudi 630 004, Tamil Nadu (India); Mahalingam, T. [Department of Electrical and Computer Engineering, Ajou University, Suwon 443-749 (Korea, Republic of); Hayakawa, Y. [Research Institute of Electronics, Shizuoka University, Hamamatsu 432-8011 (Japan); Ravi, G., E-mail: gravicrc@gmail.com [School of Physics, Alagappa University, Karaikudi 630 004, Tamil Nadu (India)

    2015-11-15

    Highly oriented thin films of Al doped ZnO (Al:ZnO) and Cu co-doped Al:ZnO (Cu/Al:ZnO) thin films were successfully deposited by sol–gel spin coating on glass substrates. The deposited films were characterized using X-ray diffraction analysis and found to exhibit hexagonal wurtzite structure with c-axis orientation. SEM images revealed that hexagonal rod shaped morphologies were grown perpendicular to the substrate surface due to repeated deposition process. High transmittance values were observed for pure ZnO compared to Al:ZnO and Cu/Al:ZnO thin films. The band gap widening is caused by the increase of carrier concentration, which is believed to be due to Burstein-Moss effect due to Al and Cu doping. PL spectra of Cu/Al:ZnO thin films indicate that the UV emission peaks slightly shifted towards lower energy side. XPS study was carried out for Zn{sub 0.80}Al{sub 0.10}Cu{sub 0.10}O thin films to analyze the binding energy of Al, Cu, Zn and O. Magnetic measurement studies exhibited ferromagnetic behavior at room temperature, which may be due to the increase in copper concentration in the doped films. The ferromagnetic behavior can be understood from the exchange coupling between localized ‘d’ spin of Cu ion mediated by free delocalized carriers. - Highlights: • High quality of Al:ZnO and Cu co-doped Al:ZnO thin films were fabricated by sol–gel method. • The XRD analyses revealed that the deposited thin films have hexagonal wurtzite structure. • XPS was carried out for Zn{sub 0.80}Al{sub 0.10}Cu{sub 0.10}O films to analyze the binding energy of Al, Cu, Zn and O. • SEM studies were made for Al:ZnO and Cu/Al:ZnO thin films. • RTFM was observed in Cu co-doped Al:ZnO thin films.

  13. Surfactant-assisted sol gel preparation of high-surface area mesoporous TiO2 nanocrystalline Li-ion battery anodes

    International Nuclear Information System (INIS)

    Casino, S.; Di Lupo, F.; Francia, C.; Tuel, A.; Bodoardo, S.; Gerbaldi, C.

    2014-01-01

    Highlights: • Mesoporous TiO 2 nanocrystalline lithium battery anodes with tunable morphology. • Simple sol–gel technique using different cationic surfactants is adopted. • Textural/morphological characteristics define the electrochemical behaviour. • TiO 2 anatase using C16TAB exhibits stable performance after 200 cycles. • It shows promising prospects as high-voltage safe Li-ion battery anode. - Abstract: We here investigate the physico-chemical/morphological characteristics and cycling behaviour of several kinds of nanocrystalline TiO 2 Li-ion battery anodes selectively prepared through a simple sol–gel strategy based on a low-cost titanium oxysulfate precursor, by mediation of different cationic surfactants having different features (e.g., chain lengths, counter ion, etc.): i.e., cetyl-trimethylammonium bromide (CTAB), cetyl-trimethylammonium chloride (CTAC), benzalkonium chloride (BC) or octadecyl-trimethyl ammonium bromide (C 18 TAB). X-ray diffraction profiles reveal single phase anatase having good correspondence with the reference pattern when using short chain CTAB, while in the other cases the presence of chloride and/or an increased chain length affect the purity of the samples. FESEM analysis reveal nanosized particles forming cauliflower-like aggregates. TiO 2 materials demonstrate mesoporous characteristics and large specific surface area ranging from 250 to 30 m 2 g −1 . Remarkably stable electrode performance are achieved by appropriately selecting the cationic surfactant and the surfactant/precursor ratio. Detailed analysis is provided on the effect of the reaction conditions upon the formation of mesoporous crystalline titania enlightening new directions for the development of high performing lithium storage electrodes by a simple and low cost sol–gel strategy

  14. Surfactant-assisted sol gel preparation of high-surface area mesoporous TiO{sub 2} nanocrystalline Li-ion battery anodes

    Energy Technology Data Exchange (ETDEWEB)

    Casino, S. [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Di Lupo, F., E-mail: francesca.dilupo@polito.it [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Francia, C. [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Tuel, A. [IRCELYON, Institut de Recherches sur la Catalyse et l’environnement de Lyon, UMR 5256, CNRS-Université de Lyon 1, 2 Avenue Albert Einstein, 69626 Villeurbanne Cedex (France); Bodoardo, S. [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Gerbaldi, C., E-mail: claudio.gerbaldi@polito.it [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy)

    2014-05-01

    Highlights: • Mesoporous TiO{sub 2} nanocrystalline lithium battery anodes with tunable morphology. • Simple sol–gel technique using different cationic surfactants is adopted. • Textural/morphological characteristics define the electrochemical behaviour. • TiO{sub 2} anatase using C16TAB exhibits stable performance after 200 cycles. • It shows promising prospects as high-voltage safe Li-ion battery anode. - Abstract: We here investigate the physico-chemical/morphological characteristics and cycling behaviour of several kinds of nanocrystalline TiO{sub 2} Li-ion battery anodes selectively prepared through a simple sol–gel strategy based on a low-cost titanium oxysulfate precursor, by mediation of different cationic surfactants having different features (e.g., chain lengths, counter ion, etc.): i.e., cetyl-trimethylammonium bromide (CTAB), cetyl-trimethylammonium chloride (CTAC), benzalkonium chloride (BC) or octadecyl-trimethyl ammonium bromide (C{sub 18}TAB). X-ray diffraction profiles reveal single phase anatase having good correspondence with the reference pattern when using short chain CTAB, while in the other cases the presence of chloride and/or an increased chain length affect the purity of the samples. FESEM analysis reveal nanosized particles forming cauliflower-like aggregates. TiO{sub 2} materials demonstrate mesoporous characteristics and large specific surface area ranging from 250 to 30 m{sup 2} g{sup −1}. Remarkably stable electrode performance are achieved by appropriately selecting the cationic surfactant and the surfactant/precursor ratio. Detailed analysis is provided on the effect of the reaction conditions upon the formation of mesoporous crystalline titania enlightening new directions for the development of high performing lithium storage electrodes by a simple and low cost sol–gel strategy.

  15. Osteoconducting bioglass synthesis via sol-gel process; Biovidro osteocondutor sintetizado pelo processo sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, R.V.; Aragones, A.; Barra, G.O.M.; Salmoria, G.V.; Fredel, M.C., E-mail: rafaelavpereira@gmail.com [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil)

    2012-07-01

    The presence of bioglasses in scaffolds has been studied as they promote the osteoconduction in bones. The scaffolds are developed in order to induce the repair and regeneration in bone tissue. An absorbable bioglass from SiO2-CaO-P2O5 system was synthesized by sol-gel process with the intent of producing these scaffolds. Bioglass 58S was define for these work once it presents ions (Ca and P) which assist at the carbonated apatite layer formation when released. The apatite layer presents an important role at the bone regeneration and metabolism, being involved at grow and mineralization of bones. FTIR was realized to characterize the synthesized bioglass on its chemical composition, XRD to analyze the crystalline structure, solubility test to observe the weight variance and SEM to observe the particles morphology. The obtained results confirmed the production of a bioglass with the desired composition to produce osteoconducting scaffolds. (author)

  16. Structural Evolution and Stability of Sol-Gel Biocatalysts

    International Nuclear Information System (INIS)

    Rodgers, L.E.; Foster, L.J.R.; Holden, P.J.; Knott, R.B.; Bartlett, J.B.

    2005-01-01

    Full text: Immobilisation strategies for catalytic enzymes are important as they allow reuse of the biocatalysts. Sol-gel materials have been used to immobilise Candida antarctica lipase B (CALB), a commonly used industrial enzyme with a known crystal structure. The sol-gel bioencapsulate is produced through the condensation of suitable metal alkoxides in the presence of CALB, yielding materials with controlled pore sizes, volume and surface chemistry. Sol-gel matrices have been shown to prolong the catalytic life and enhance the activity of CALB, although the molecular basis for this effect has yet to be elucidated due to the limitations of analysis techniques applied to date. Small angle neutron scattering (SANS) allows such multicomponent systems to be characterised through contrast matching. In the sol-gel bioencapsulate system, at the contrast match point for silica, residual scattering intensity is due to the CALB and density fluctuations in the matrix. A SANS contrast variation series found the match point for the silica matrix, both with and without enzyme present, to be around 35 percent. The model presented here proposes a mechanism for the interaction between CALB and the surrounding sol-gel matrix, and the observed improvement in enzyme activity and matrix strength. The SANS protocol developed here may be applied more generally to bioencapsulates. (authors)

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

    International Nuclear Information System (INIS)

    King, C.M.; Thompson, M.C.; Buchanan, B.R.; King, R.B.; Garber, A.R.

    1990-01-01

    Nuclear Magnetic Resonance (NMR) investigations on the Oak Ridge National Laboratory process for sol-gel synthesis of microspherical nuclear fuel (UO 2 ), has been extremely useful in sorting out the chemical mechanism in the sol-gel steps. 13 C, 15 N, and 1 H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C 6 H 12 N 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. 17 O NMR of uranyl (UO 2 ++ ) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, [(UO 2 ) 3 (μ 3 -O)(μ 2 -OH) 3 ] + , 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 + 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 4 ) 2 [(UO 2 ) 8 O 4 (OH) 10 ] · 8H 2 O. This compound is the precursor to sintered UO 2 ceramic fuel. 23 refs., 10 figs

  18. Influence of post-deposition treatment by UV light and oxygen (ozone) on 350 nm damage thresholds of SiO2 films deposited from sols

    International Nuclear Information System (INIS)

    Thomas, I.; Wilder, J.; Lee, A.; George, D.

    1988-01-01

    Certain multilayer porous silica AR coatings on fused silica substrates prepared by the sol-gel process have been found to have a much lower laser damage threshold than single layer coatings prepared by the same method. Treatment with UV light in the presence of oxygen (which gives ozone) at low temperature was found to restore damage thresholds to the levels found in single layers. Damage thresholds were measured at 350 nm with a 25 ns pulse for 1000 shots at 25 Hz. The effect of exposure time and other factors such as replacement of oxygen with nitrogen and vacuum are described

  19. Electrochemical impedimetric sensor based on molecularly imprinted polymers/sol-gel chemistry for methidathion organophosphorous insecticide recognition.

    Science.gov (United States)

    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. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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

  1. Sol-gel derived electrode materials for supercapacitor applications

    Science.gov (United States)

    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.

  2. The role sol-gel process for nuclear fuels - an overview

    International Nuclear Information System (INIS)

    Sood, D.D.

    2009-01-01

    The paper reviews the sol-gel methods used for the preparation of fuel materials in the form of microspheres. It also discusses how these microspheres can be fabricated into nuclear fuels for reactors like High Temperature Gas Cooled Reactors and Fast Reactors. Performance of these microsphere based fuels is reviewed. More recent applications, like transmutation of minor actinides, (Np, Am and Cm) and hydrogen production, are also briefly covered. (author)

  3. Hydrogen permeation through steel coated with erbium oxide by sol-gel method

    International Nuclear Information System (INIS)

    Yao Zhenyu; Suzuki, Akihiro; Levchuk, Denis; Chikada, Takumi; Tanaka, Teruya; Muroga, Takeo; Terai, Takayuki

    2009-01-01

    Er 2 O 3 coating is formed on austenitic stainless steel 316ss by sol-gel method. The results showed good crystallization of coating by baking in high purity flowing-argon at 973 K, and indicated that a little oxygen in baking atmosphere is necessary to crystallization of coating. The best baking temperature could be thought as 973 K, to get good crystallization of coating and avoid strong oxidation of steel substrate. The deuterium permeation test was performed for coated and bare 316ss, to evaluate the property of Er 2 O 3 sol-gel coating as a potential tritium permeation barrier. In this study, the deuterium permeability of coated 316ss is about 1-2 orders of magnitude lower than that of bare 316ss, and is about 2-3 orders of magnitude than the referred data of bare Eurofer97 and F82H martensitic steel.

  4. Moisture sensor based on evanescent wave light scattering by porous sol-gel silica coating

    Science.gov (United States)

    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.

  5. Sol-gel-state of hydrated zirconium dioxide

    International Nuclear Information System (INIS)

    Karakchiev, L.G.; Lyakhov, N.Z.

    1995-01-01

    The change in viscosity and density of a system in the course of sol-gel-xerogel has been traced. The size and molecular mass of particles in sol have been determined. Initial sol is practically a monodisperse system. Gel is a spatial net of similar particles. Reversible character of sol-gel transition with a change in water content in the system suggests instability of the bond between the particles in the structure of the solid state body formed. 11 refs.; 4 figs

  6. Silica scintillating materials prepared by sol-gel methods

    International Nuclear Information System (INIS)

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

    1993-01-01

    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

  7. Functionalization of sol-gel zirconia composites with europium complexes

    International Nuclear Information System (INIS)

    Danchova, Nina; Gutzov, Stoyan

    2014-01-01

    Different sol-gel strategies based on functionalization of ZrO 2 :Eu microparticles with 1,10-phenanthroline (phen) and incorporation of colloidal Eu(phen) 2 (NO 3 ) 3 into zirconia have been used to obtain hybrid sol-gel composites with controlled optical properties. The process leads to materials with quantum yields of about 48 % monitoring the 615 nm emission line at 350 nm excitation. Excitation/luminescence spectroscopy, diffuse reflectance spectroscopy and X-ray diffraction have been used to characterize the hybrid zirconia composites. (orig.)

  8. Ceramic protective coatings applied by sol-gel or electrophoresis

    International Nuclear Information System (INIS)

    Stoch, A.

    1993-01-01

    Sol-gel and electrophoresis are the complementary techniques which may be used for obtaining the ceramic coatings. The composition of such a coatings depends on the composition of electrophoresis bath or sol solution. Thermal treatment is used for densifying the coating and promoting the adherence of coating to the substrate. In presented work silica, silica-alumina or alumina coatings are applied by sol-gel dip coating procedure on steel, aluminium or ceramic substrates. Electrophoresis is employed for obtaining zirconia, alumina or hydroxyapatite coatings on stainless steel. (author). 7 refs

  9. Exploring encapsulation mechanism of DNA and mononucleotides in sol-gel derived silica.

    Science.gov (United States)

    Kapusuz, Derya; Durucan, Caner

    2017-07-01

    The encapsulation mechanism of DNA in sol-gel derived silica has been explored in order to elucidate the effect of DNA conformation on encapsulation and to identify the nature of chemical/physical interaction of DNA with silica during and after sol-gel transition. In this respect, double stranded DNA and dAMP (2'-deoxyadenosine 5'-monophosphate) were encapsulated in silica using an alkoxide-based sol-gel route. Biomolecule-encapsulating gels have been characterized using UV-Vis, 29 Si NMR, FTIR spectroscopy and gas adsorption (BET) to investigate chemical interactions of biomolecules with the porous silica network and to examine the extent of sol-gel reactions upon encapsulation. Ethidium bromide intercalation and leach out tests showed that helix conformation of DNA was preserved after encapsulation. For both biomolecules, high water-to-alkoxide ratio promoted water-producing condensation and prevented alcoholic denaturation. NMR and FTIR analyses confirmed high hydraulic reactivity (water adsorption) for more silanol groups-containing DNA and dAMP encapsulated gels than plain silica gel. No chemical binding/interaction occurred between biomolecules and silica network. DNA and dAMP encapsulated silica gelled faster than plain silica due to basic nature of DNA or dAMP containing buffer solutions. DNA was not released from silica gels to aqueous environment up to 9 days. The chemical association between DNA/dAMP and silica host was through phosphate groups and molecular water attached to silanols, acting as a barrier around biomolecules. The helix morphology was found not to be essential for such interaction. BET analyses showed that interconnected, inkbottle-shaped mesoporous silica network was condensed around DNA and dAMP molecules.

  10. Crystal structures of sol-gel deposited zirconia thin films

    International Nuclear Information System (INIS)

    Bell, J.M.; Cheary, R.W.; Rice, M.; Ben-Nissan, B.; Cocking, J.L.; Johnstone, G.R.

    1992-01-01

    The authors reports on the crystal structure of zirconia thin films by high temperature x-ray diffraction. The films were deposited by sol-gel processing onto polished stainless steel substrates, and dried at 200 deg C. X-ray diffraction at temperatures between 400 deg C and 800 deg C was carried out using an APEX diffractometer with a position sensitive detector. Previous results indicated that there was a transformation between the tetragonal phase and the monoclinic phase at approximately 770 deg C. Two experiments have been carried out: temperature runs, where the structure evolution is studied as a function of temperature; and time evolution of the structure at fixed temperatures. The results for both experiments, including structural analysis of the different phases found in the thin zirconia films and an analysis of the kinetics of the phase transformation(s) from the time evolution work are presented. This will include a comparison with theories of nucleation and crystallisation in single element films. Impurity phases introduced by interaction of the zirconia with the substrate have been observed, and the effect of increasing annealing time on the substrate-film interaction will also be discussed. 17 refs., 1 tab., 3 figs

  11. Preparation of silica by sol-gel method using formamide

    Directory of Open Access Journals (Sweden)

    R.F.S. Lenza

    2001-07-01

    Full Text Available In this work we obtained microporous and mesoporous silica gels by sol-gel processing. Tetraethylortosilicate (TEOS was used as precursor. Nitric acid and hydrofluoric acid were used as catalysts. In order to study the affect of formamide as drying additive, we used a molar ratio alkoxide/formamide of 1/1. The performance of formamide in obtaining crack-free gels was evaluated through monolithicity measurements. The structural evolution occurring in the interconnected network of the gels during thermal treatment was monitored by Fourier transform infrared spectroscopy (FTIR, shrinkage and density measurements and nitrogen gas sorption. We noted that in the presence of formamide, the Si-O-Si bonds are stronger and belong to a more cross-linked structure. The samples obtained in the presence of formamide have larger pore volume and its pore structure is in the range of mesoporosity. The samples obtained without additive are microporous. Formamide allowed the preparation of crack-free silica gels stabilized at high temperatures.

  12. Mesoscopic objects, porous layers and nanocomposites-Possibilities of sol-gel chemistry

    International Nuclear Information System (INIS)

    Piwonski, Ireneusz

    2009-01-01

    The goal of this study was to prepare mesoscopic objects, thin porous films and nanocomposite coatings with the use of sol-gel technique. Silica nanotubes, titania nanoparticles, porous titania and zirconia coatings as well as titania nanocomposites were successfully synthesized by changing the type of sol-gel precursor, sol composition and applying dip-coating deposition procedure in order to obtain thin films or coatings. All materials were visualized and characterized by the Atomic Force Microcscopy (AFM) technique. Moreover, characterization of titania nanocomposites was extended to the tribological tests performed by means of microtribometer operating in normal loads range of 30-100 mN. The AFM analysis of mesoscopic objects and nanoparticles showed that the diameter of synthesized silica nanotubes was 60-70 nm and the size of titania nanoparticles was 43 nm. In case of porous layers the pore size in titania and zirconia coatings oscillated between 100 and 240 nm, however their shape and distribution were irregular. Microtribological studies of nanocomposites revealed the moderate decrease of the coefficient of friction for samples containing 5, 15 and 5 wt.% of zirconia nanoparticles in titania coatings annealed at 100, 500 and 1000 deg. C respectively. An enhancement of antiwear properties was already observed for 1 wt.% of nanophase content, except the sample annealed at 500 deg. C. It was also found that the annealing at high temperatures is a primary factor which affects the reduction of friction and wear of titania coatings while the presence of nanoparticles has secondary effect. Investigations in this study carried out with the use of the AFM technique highlighted the potential and flexibility of sol-gel approach in designing of various types of advanced materials in a form of mesoscopic objects, porous coatings and composite layers. Results collected in this study clearly demonstrated that sol-gel technique can be applied effectively in preparation of

  13. Sol - gel inorganic ion exchangers for conditioning of medium level radioactive waste

    International Nuclear Information System (INIS)

    Arcangeli, G.; Traverso, D.M.; Gerontopoulos, P.; Fava, R.

    1988-01-01

    Decontamination of high-level liquid wastes and medium activity wastes streams by inorganic ion exchange combined with the conversion of the spent inorganic ion exchange material to waste ceramics presents a considerable potential for utilisation in waste conditioning. Ceramic waste forms are found superior to other candidate waste immobilisation forms but practical implementation is hampered because of the complexity of the related fabrication technology. This report shows the possibility of improving this situation by resorting to sol gel techniques earlier developed for preparation of nuclear fuel ceramics. The principal findings are: - superior quality ion exchange xerogel titanates in the form of mechanically resistant, size controlled microspheres can be prepared using a simple sol-gel technique; - the titanate particles can be also used as precursors in Evaporative Deposition on Xerogel Particles (EDXP) a new waste solidification process based on physical impregnation of the xerogel material with the waste liquid followed by evaporation; - waste loaded ion exchange microspheres can be converted to leach resistant ceramics by firing and/or cold pressing and sintering at 900 0 -1100 0 C; - sol-gel inorganic ion exchange and EDXP may find useful application in conditioning MAW streams. 44 figs., 43 refs

  14. Dielectric and piezoelectric properties of sol-gel derived Ca doped PbTiO3

    International Nuclear Information System (INIS)

    Chauhan, Arun Kumar Singh; Gupta, Vinay; Sreenivas, K.

    2006-01-01

    Synthesis of Ca doped PbTiO 3 powder by a chemically derived sol-gel process is described. Crystallization characteristics of different compositions Pb 1-x Ca x TiO 3 (PCT) with varying calcium (Ca) content in the range x = 0-0.45 has been investigated by DTA/TGA, X-ray diffraction and scanning electron microscopy. The crystallization temperature is found to decrease with increasing calcium content. X-ray diffraction reveals a tetragonal structure for PCT compositions with x ≤ 0.35, and a cubic structure for x = 0.45. Dielectric properties on sintered ceramics prepared with fine sol-gel derived powders have been measured. The dielectric constant is found to increase with increasing Ca content, and the dielectric loss decreases continuously. Sol-gel derived Pb 1-x Ca x TiO 3 ceramics with x = 0.45 after poling exhibit infinite electromechanical anisotropy (k t /k p ) with a high d 33 = 80 pC/N, ε' = 298 and low dielectric loss (tan δ = 0.0041)

  15. One-step immobilization of tris(2,2'-bipyridyl)ruthenium(II) via vapor-surface sol-gel deposition towards solid-state electrochemiluminescence detection

    International Nuclear Information System (INIS)

    Qian Lei; Yang Xiurong

    2008-01-01

    A novel method for immobilization of tris(2,2'-bipyridyl)ruthenium(II) (Ru(bpy) 3 Cl 2 ) on electrode surfaces based on the vapor-surface sol-gel deposition strategy is first demonstrated in this paper. Ru(bpy) 3 Cl 2 immobilized sol-gel (Ru(bpy) 3 Cl 2 /sol-gel) films were characterized by UV-vis spectroscopy and field-emitted scanning electron microscopy (FE-SEM). These results showed that Ru(bpy) 3 Cl 2 was successfully incorporated into the silica sol-gel film. It was found that many irregular Ru(bpy) 3 Cl 2 /sol-gel clusters were formed on surfaces through one deposition and thick sol-gel films were observed after further deposition. Electrochemical properties and electrochemiluminescence (ECL) behaviors of Ru(bpy) 3 Cl 2 /sol-gel films could be easily adjusted by deposition numbers and time. At last, the Ru(bpy) 3 Cl 2 /sol-gel film modified electrode was used for solid-state ECL detection of tripropylamine. The linear range was from 5.8 x 10 -8 to 2.4 x 10 -4 M with the detection limit of 5 nM, which was three orders of magnitude lower than that from pure Nafion-modified electrodes. The ECL sensor also exhibited high stability, and still remained 92% response after being stored in air for 35 days. This method for immobilization of Ru(bpy) 3 Cl 2 is simple, convenient and low-cost relative to others, so it shows promising applications in solid-state ECL detection

  16. Hydrogen Production by Steam Reforming of Ethanol over Nickel Catalysts Supported on Sol Gel Made Alumina: Influence of Calcination Temperature on Supports.

    Science.gov (United States)

    Yaakob, Zahira; Bshish, Ahmed; Ebshish, Ali; Tasirin, Siti Masrinda; Alhasan, Fatah H

    2013-05-30

    Selecting a proper support in the catalyst system plays an important role in hydrogen production via ethanol steam reforming. In this study, sol gel made alumina supports prepared for nickel (Ni) catalysts were calcined at different temperatures. A series of (Ni/Al S.G. ) catalysts were synthesized by an impregnation procedure. The influence of varying the calcination temperature of the sol gel made supports on catalyst activity was tested in ethanol reforming reaction. The characteristics of the sol gel alumina supports and Ni catalysts were affected by the calcination temperature of the supports. The structure of the sol gel made alumina supports was transformed in the order of γ → (γ + θ) → θ-alumina as the calcination temperature of the supports increased from 600 °C to 1000 °C. Both hydrogen yield and ethanol conversion presented a volcano-shaped behavior with maximum values of 4.3 mol/mol ethanol fed and 99.5%, respectively. The optimum values were exhibited over Ni/Al S.G800 (Ni catalyst supported on sol gel made alumina calcined at 800 °C). The high performance of the Ni/Al S.G800 catalyst may be attributed to the strong interaction of Ni species and sol gel made alumina which lead to high nickel dispersion and small particle size.

  17. Sol-gel coatings on carbon/carbon composites

    International Nuclear Information System (INIS)

    Sim, S.M.; Krabill, R.M.; Dalzell, W.J. Jr.; Chu, P.Y.; Clark, D.E.

    1986-01-01

    The need for structural materials that can withstand severe environments up to 4000 0 F has promulgated the investigation of sol-gel derived ceramic and composite coatings on carbon/carbon composite materials. Alumina and zirconia sols have been deposited via thermophoresis on carbon/carbon substrates

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

    Science.gov (United States)

    Congdon, James W [Aiken, SC

    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.

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

    Science.gov (United States)

    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...

  20. Stoichiometric hydroxyapatite obtained by precipitation and sol gel processes

    Energy Technology Data Exchange (ETDEWEB)

    Guzman V, C.; Pina B, C.; Munguia, N. [IIM-UNAM, A.P. 70-360, 04510 Mexico D.F. (Mexico)]. e-mail: caroguz@servidor.unam.mx

    2005-07-01

    Three methods for obtaining hydroxyapatite (HA) are described. HA is a very interesting ceramic because of its many medical applications. The first two precipitation methods start from calcium and phosphorous compounds, whereas the third method is a sol-gel process that uses alkoxides. The products were characterized and compared. The observed differences are important for practical applications. (Author)

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

    Science.gov (United States)

    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.

  2. Analyses of laser and furnace treated sol-gel coatings

    NARCIS (Netherlands)

    De Hosson, JT; De Haas, M; Sudarshan, TS; Jeandin, M; Khor, KA

    1998-01-01

    Here we explore a new method that allows thin films to be made with almost any composition and degree of porosity by means of a combination of sol-gel and laser technology. Results are presented for furnace and laser treated TEOTI-(tetraethylorthotitanate as sol precursor) coated silicon samples.

  3. Athermal silicon optical add-drop multiplexers based on thermo-optic coefficient tuning of sol-gel material.

    Science.gov (United States)

    Namnabat, Soha; Kim, Kyung-Jo; Jones, Adam; Himmelhuber, Roland; DeRose, Christopher T; Trotter, Douglas C; Starbuck, Andrew L; Pomerene, Andrew; Lentine, Anthony L; Norwood, Robert A

    2017-09-04

    Silicon photonics has gained interest for its potential to provide higher efficiency, bandwidth and reduced power consumption compared to electrical interconnects in datacenters and high performance computing environments. However, it is well known that silicon photonic devices suffer from temperature fluctuations due to silicon's high thermo-optic coefficient and therefore, temperature control in many applications is required. Here we present an athermal optical add-drop multiplexer fabricated from ring resonators. We used a sol-gel inorganic-organic hybrid material as an alternative to previously used materials such as polymers and titanium dioxide. In this work we studied the thermal curing parameters of the sol-gel and their effect on thermal wavelength shift of the rings. With this method, we were able to demonstrate a thermal shift down to -6.8 pm/°C for transverse electric (TE) polarization in ring resonators with waveguide widths of 325 nm when the sol-gel was cured at 130°C for 10.5 hours. We also achieved thermal shifts below 1 pm/°C for transverse magnetic (TM) polarization in the C band under different curing conditions. Curing time compared to curing temperature shows to be the most important factor to control sol-gel's thermo-optic value in order to obtain an athermal device in a wide temperature range.

  4. A Sol-gel Integrated Dual-readout Microarray Platform for Quantification and Identification of Prostate-specific Antigen.

    Science.gov (United States)

    Lee, SangWook; Lee, Jong Hyun; Kwon, Hyuck Gi; Laurell, Thomas; Jeong, Ok Chan; Kim, Soyoun

    2018-01-01

    Here, we report a sol-gel integrated affinity microarray for on-chip matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) that enables capture and identification of prostate?specific antigen (PSA) in samples. An anti-PSA antibody (H117) was mixed with a sol?gel, and the mixture was spotted onto a porous silicon (pSi) surface without additional surface modifications. The antibody easily penetrates the sol-gel macropore fluidic network structure, making possible high affinities. To assess the capture affinity of the platform, we performed a direct assay using fluorescein isothiocyanate-labeled PSA. Pure PSA was subjected to on-chip MALDI-TOF-MS analysis, yielding three clear mass peptide peaks (m/z = 1272, 1407, and 1872). The sol-gel microarray platform enables dual readout of PSA both fluorometric and MALDI-TOF MS analysis in biological samples. Here we report a useful method for a means for discovery of biomarkers in complex body fluids.

  5. The application of silicon sol-gel technology to forensic blood substitute development: Mimicking aspects of whole human blood rheology.

    Science.gov (United States)

    Stotesbury, Theresa; Illes, Mike; Wilson, Paul; Vreugdenhil, Andrew J

    2017-01-01

    Solution-gelation chemistry has promising applications in forensic synthetic blood substitute development. This research offers a silicon-based sol-gel approach to creating stable materials that share similar rheological properties to that of whole human blood samples. Room temperature, high water content, silicon sol-gels were created using the organosilane precursors 3-glycidoxypropyltrimethoxysilane and tetraethylorthosilicate along with various concentrations of filler and pigment. Shear-thinning non-Newtonian properties were observed within most formulations of the presented materials. The effects of colloidal concentration, temperature, age and filler addition on the viscosity of the sol-gels were investigated. SEM-EDS analysis was used to identify the behavior of the fillers within the film and support their inclusion for basic bloodstain pattern simulation. A final proposed candidate sol-gel was assessed using a previously reported passive drip simulation test on a hard, dry surface and passed. This works represents encouraging development in providing safe material alternatives to using whole human blood for forensic training and research. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  6. Analysis of the damage threshold of the GaAs pseudomorphic high electron mobility transistor induced by the electromagnetic pulse

    International Nuclear Information System (INIS)

    Xi Xiao-Wen; Chai Chang-Chun; Liu Yang; Yang Yin-Tang; Fan Qing-Yang; Shi Chun-Lei

    2016-01-01

    An electromagnetic pulse (EMP)-induced damage model based on the internal damage mechanism of the GaAs pseudomorphic high electron mobility transistor (PHEMT) is established in this paper. With this model, the relationships among the damage power, damage energy, pulse width and signal amplitude are investigated. Simulation results show that the pulse width index from the damage power formula obtained here is higher than that from the empirical formula due to the hotspot transferring in the damage process of the device. It is observed that the damage energy is not a constant, which decreases with the signal amplitude increasing, and then changes little when the signal amplitude reaches up to a certain level. (paper)

  7. Luminescent hybrid porphyrinosilica obtained by sol gel chemistry

    Directory of Open Access Journals (Sweden)

    Neri Cláudio Roberto

    2003-01-01

    Full Text Available The sol-gel process is a methodology used to obtain organic-inorganic hybrid solids, which open new possibilities in the field of material science. The sol-gel technique offers a low temperature attractive approach for introducing organic molecules into amorphous materials. In order to introduce tetrakis (2-hydroxy-5-nitrophenylporphyrin covalently bounded to a silicate matrix, the inorganic precursor 3-isocyanatopropyltriethoxysilane was added (molar ratio 2:1 to the porphyrin solution in anhydrous dimethylformamide and triethylamine. The isolated porphyrin and the hybrid porphyrinosilica have excitation maximum centred at 400 nm and 424 nm, respectively and the emission spectra for both materials has bands centred at 650 nm and 713 nm. The formation of hybrid matrix was investigated by FTIR.

  8. Tough ceramic coatings: Carbon nanotube reinforced silica sol-gel

    Science.gov (United States)

    López, A. J.; Rico, A.; Rodríguez, J.; Rams, J.

    2010-08-01

    Silica coatings reinforced with carbon nanotubes were produced via sol-gel route using two mixing techniques of the sol-gel precursors, mechanical and ultrasonic mixing, and dip-coating as deposition process on magnesium alloy substrates. Effective incorporation and distribution of 0.1 wt.% of carbon nanotubes in the amorphous silica matrix of the coatings were achieved using both techniques. Fabrication procedure determines the morphological aspects of the coating. Only mechanical mixing process produced coatings dense and free of defects. Nanoindentation technique was used to examine the influence of the fabrication process in the mechanical features of the final coatings, i.e. indentation fracture toughness, Young's modulus and hardness. A maximum toughening effect of about 24% was achieved in silica coatings reinforced with carbon nanotubes produced by the mechanical mixing route. Scanning electron microscopy investigation revealed that the toughening of these reinforced coatings was mainly due to bridging effect of the reinforcement.

  9. Electrophoretic deposition of sol-gel-derived ceramic coatings

    International Nuclear Information System (INIS)

    Zhang, Y.; Crooks, R.M.

    1992-01-01

    In this paper the physical, optical, and chemical characteristics of electrophoretically and dip-coated sol-gel ceramic films are compared. The results indicate that electrophoresis may allow a higher level of control over the chemistry and structure of ceramic coatings than dip-coating techniques. For example, controlled-thickness sol-gel coatings can be prepared by adjusting the deposition time or voltage. Additionally, electrophoretic coatings can be prepared in a four-component alumino-borosilicate sol display interesting optical characteristics. For example, the ellipsometrically-measured refractive indices of electrophoretic coatings are higher than the refractive indices of dip-coated films cast from identical sols, and they are also higher than any of the individual sol components. This result suggests that there are physical and/or chemical differences between films prepared by dip-coating and electrophoresis

  10. Sol-gel based optical sensor for determination of Fe (II): a novel probe for iron speciation.

    Science.gov (United States)

    Samadi-Maybodi, Abdolraouf; Rezaei, Vida; Rastegarzadeh, Saadat

    2015-02-05

    A highly selective optical sensor for Fe (II) ions was developed based on entrapment of a sensitive reagent, 2,4,6-tri(2-pyridyl)-s-triazine (TPTZ), in a silica sol-gel thin film coated on a glass substrate. The thin films fabricated based on tetraethoxysilane (TEOS) as precursor, sol-gel pH∼3, water:alkoxyde ratio of 4:1 and TPTZ concentration of 0.112 mol L(-1). The influence of sol-gel parameters on sensing behavior of the fabricated sensor was also investigated. The fabricated sensor can be used for determination of Fe (II) ion with an outstanding high selectivity over a dynamic range of 5-115 ng mL(-1) and a detection limit of 1.68 ng mL(-1). It also showed reproducible results with relative standard deviation of 3.5% and 1.27% for 10 and 90 ng mL(-1) of Fe (II), respectively, along with a fast response time of ∼120 s. Total iron also was determined after reduction of Fe (III) to Fe (II) using ascorbic acid as reducing agent. Then, the concentration of Fe (III) was calculated by subtracting the concentration of Fe (II) from the total iron concentration. Interference studies showed a good selectivity for Fe (II) with trapping TPTZ into sol-gel matrix and appropriately adjusting the structure of doped sol-gel. The sensor was compared with other sensors and was applied to determine iron in different water samples with good results. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Epoxy-silica hybrids by nonaqueous sol-gel process

    Czech Academy of Sciences Publication Activity Database

    Ponyrko, Sergii; Kobera, Libor; Brus, Jiří; Matějka, Libor

    2013-01-01

    Roč. 54, č. 23 (2013), s. 6271-6282 ISSN 0032-3861 R&D Projects: GA ČR GAP108/12/1459 Grant - others:AV ČR(CZ) M200500903 Institutional support: RVO:61389013 Keywords : epoxy-silica hybrid * nonaqueous sol-gel process * gelation Subject RIV: CD - Macromolecular Chemistry Impact factor: 3.766, year: 2013

  12. Sol-Gel Thin Films for Plasmonic Gas Sensors

    Science.gov (United States)

    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

  13. Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

    Science.gov (United States)

    Gąsiorek, Jolanta; Babiarczuk, Bartosz; Kaleta, Jerzy; Jones, Walis; Krzak, Justyna

    2018-01-01

    Corrosion is constantly a major problem of the world economy in the field of metal products, metal processing and other areas that utilise metals. Previously used compounds utilizing hexavalent chromium were amongst the most effective materials for corrosion protection but regulations have been recently introduced that forbid their use. Consequently, there is a huge drive by engineers, technologists and scientists from different disciplines focused on searching a new, more effective and environmentally-friendly means of corrosion protection. One novel group of materials with the potential to solve metal protection problems are sol-gel thin films, which are increasingly interesting as mitigation corrosion barriers. These environmentally-friendly and easy-to-obtain coatings have the promise to be an effective alternative to hexavalent chromium compounds using for anti-corrosion industrial coatings. In this review the authors present a range of different solutions for slow down the corrosion processes of metallic substrates by using the oxides and doped oxides obtained by the sol-gel method. Examples of techniques used to the sol-gel coating examinations, in terms of anti-corrosion protection, are also presented. PMID:29373540

  14. Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

    Directory of Open Access Journals (Sweden)

    Jolanta Gąsiorek

    2018-01-01

    Full Text Available Corrosion is constantly a major problem of the world economy in the field of metal products, metal processing and other areas that utilise metals. Previously used compounds utilizing hexavalent chromium were amongst the most effective materials for corrosion protection but regulations have been recently introduced that forbid their use. Consequently, there is a huge drive by engineers, technologists and scientists from different disciplines focused on searching a new, more effective and environmentally-friendly means of corrosion protection. One novel group of materials with the potential to solve metal protection problems are sol-gel thin films, which are increasingly interesting as mitigation corrosion barriers. These environmentally-friendly and easy-to-obtain coatings have the promise to be an effective alternative to hexavalent chromium compounds using for anti-corrosion industrial coatings. In this review the authors present a range of different solutions for slow down the corrosion processes of metallic substrates by using the oxides and doped oxides obtained by the sol-gel method. Examples of techniques used to the sol-gel coating examinations, in terms of anti-corrosion protection, are also presented.

  15. Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation.

    Science.gov (United States)

    Gąsiorek, Jolanta; Szczurek, Anna; Babiarczuk, Bartosz; Kaleta, Jerzy; Jones, Walis; Krzak, Justyna

    2018-01-26

    Corrosion is constantly a major problem of the world economy in the field of metal products, metal processing and other areas that utilise metals. Previously used compounds utilizing hexavalent chromium were amongst the most effective materials for corrosion protection but regulations have been recently introduced that forbid their use. Consequently, there is a huge drive by engineers, technologists and scientists from different disciplines focused on searching a new, more effective and environmentally-friendly means of corrosion protection. One novel group of materials with the potential to solve metal protection problems are sol-gel thin films, which are increasingly interesting as mitigation corrosion barriers. These environmentally-friendly and easy-to-obtain coatings have the promise to be an effective alternative to hexavalent chromium compounds using for anti-corrosion industrial coatings. In this review the authors present a range of different solutions for slow down the corrosion processes of metallic substrates by using the oxides and doped oxides obtained by the sol-gel method. Examples of techniques used to the sol-gel coating examinations, in terms of anti-corrosion protection, are also presented.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Shankhwar, Nisha; Srinivasan, A

    2016-05-01

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

  18. Sol-gel processes. January 1970-September 1989 (Citations from the NTIS data base). Report for January 1970-September 1989

    International Nuclear Information System (INIS)

    1989-09-01

    This bibliography contains citations concerning the development and utilization of sol-gel processes and techniques. Topics include antireflective coatings, studies of sol-gel transitions, sol-gel synthesis and polymerization, sol-gel derived thin films and glasses, and sol-gel production of microspheres. Applications in nuclear waste management, nuclear-fuel manufacturing, glass optical waveguide development, and solar-energy collection are presented. (This updated bibliography contains 179 citations, 39 of which are new entries to the previous edition.)

  19. Evolution of heterogeneity accompanying sol-gel transitions in a supramolecular hydrogel.

    Science.gov (United States)

    Matsumoto, Yuji; Shundo, Atsuomi; Ohno, Masashi; Tsuruzoe, Nobutomo; Goto, Masahiro; Tanaka, Keiji

    2017-10-18

    When a peptide amphiphile is dispersed in water, it self-assembles into a fibrous network, leading to a supramolecular hydrogel. When the gel is physically disrupted by shaking, it transforms into a sol state. After aging at room temperature for a while, it spontaneously returns to the gel state, called sol-gel transition. However, repeating the sol-gel transition often causes a change in the rheological properties of the gel. To gain a better understanding of the sol-gel transition and its reversibility, we herein examined the thermal motion of probe particles at different locations in a supramolecular hydrogel. The sol obtained by shaking the gel was heterogeneous in terms of the rheological properties and the extent decreased with increasing aging time. This time course of heterogeneity, or homogeneity, which corresponded to the sol-to-gel transition, was observed for the 1st cycle. However, this was not the case for the 2nd and 3rd cycles; the heterogeneity was preserved even after aging. Fourier-transform infrared spectroscopy, small-angle X-ray scattering, and atomic force and confocal laser scanning microscopies revealed that, although the molecular aggregation states of amphiphiles both in the gel and sol remained unchanged with the cycles, the fibril density diversified to high and low density regions even after aging. The tracking of particles with different sizes indicated that the partial mesh size in the high density region and the characteristic length scale of the density fluctuation were smaller than 50 nm and 6 μm, respectively.

  20. Gamma ray irradiation induced optical band gap variations in silica sol-gel doped sucrose

    International Nuclear Information System (INIS)

    Marzouki, F.; Farah, K.; Hamzaoui, A.H; Ben Ouada, H

    2015-01-01

    The silica xerogels doped sucrose was prepared via sol-gel process and exposed at room temperature to different doses of high energy ("6"0Co) gamma irradiation. Changes in the UV-visible and FTIR spectra of pristine and irradiated xerogels with varying of gamma doses rays show variation in the gap energy. It was found that energy gap of the investigated silica xerogels decreases with increasing the gamma irradiation doses. Thereby the irradiated samples reveal behaviour changes, from an insulator (Eg ∼5,8 eV) towards a semiconductor with (Eg ∼ 3.5 eV).

  1. Low-temperature sol-gel synthesis of NaZr2P3O12

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  2. Elaboration and characterisation of yttrium oxide and hafnium oxide powders by the sol-gel process

    International Nuclear Information System (INIS)

    Hours, T.

    1988-01-01

    The two classical sol-gel processes, colloidal and polymeric are studied for the preparation of yttrium oxide and hafnium oxide high performance powders. In the colloidal process, controlled and reproducible conditions for the preparation of yttrium oxide and hafnium oxide sols from salts or alkoxides are developed and the hydrothermal synthesis monodisperse hafnium oxide colloids is studied. The polymeric process is studied with hafnium ethyl-hexylate, hydrolysis kinetics for controlled preparation of sols and gels is investigated. Each step of preparation is detailed and powders obtained are characterized [fr

  3. Investigation of sol-gel antireflective coatings

    International Nuclear Information System (INIS)

    Schmid, A.; Guardalben, M.; Chipp, T.

    1984-03-01

    Very high power laser systems present material design challenges which often approach the inherent optical survival strength of components. Optical coatings in the UV region suffer from anomalously high absorption and scattering in the deposited layers. The losses caused by these effects are often unacceptable or, in the case of absorption, usually fatal to the absorbing coatings. Unfortunately, no metals exist that have high enough reflectivities in the UV to serve as uncoated mirrors as they normally do in the CO 2 region of the infrared. Adequate multilayer dielectric coatings are therefore critically important for the development and utilization of UV lasers. The same could be said for relfection suppressing antireflective coatings in that wavelength range. Antireflective properties of gradientindex designs have been rediscovered and their potential for resolving UV laser design difficulties has been vigorously tested. These antireflective properties have been attained on glass or fused silica surfaces by chemical surface treatments

  4. Influence of Experimental Parameters Using the Dip-Coating Method on the Barrier Performance of Hybrid Sol-Gel Coatings in Strong Alkaline Environments

    Directory of Open Access Journals (Sweden)

    Rita B. Figueira

    2015-04-01

    Full Text Available Previous studies have shown that the barrier effect and the performance of organic-inorganic hybrid (OIH sol-gel coatings are highly dependent on the coating deposition method as well as on the processing conditions. However, studies on how the coating deposition method influences the barrier properties in alkaline environments are scarce. The aim of this experimental research was to study the influence of experimental parameters using the dip-coating method on the barrier performance of an OIH sol-gel coating in contact with simulated concrete pore solutions (SCPS. The influence of residence time (Rt, a curing step between each dip step and the number of layers of sol-gel OIH films deposited on hot-dip galvanized steel to prevent corrosion in highly alkaline environments was studied. The barrier performance of these OIH sol-gel coatings, named U(400, was assessed in the first instants of contact with SCPS, using electrochemical impedance spectroscopy and potentiodynamic methods. The durability and stability of the OIH coatings in SCPS was monitored during eight days by macrocell current density. The morphological characterization of the surface was performed by Scanning Electronic Microscopy before and after exposure to SCPS. Glow Discharge Optical Emission Spectroscopy was used to investigate the thickness of the U(400 sol-gel coatings as a function of the number of layers deposited with and without Rt in the coatings thickness.

  5. The development and characterization of sol-gel substrates for chemical and optical applications

    Science.gov (United States)

    Powers, Kevin William

    1998-12-01

    The sol gel process can be used to make monolithic porous glass for various scientific and engineering uses. The porosity of the material imparts a large surface area which is advantageous in applications such as catalyst supports or in the study of surface mediated chemical reactions. The chemical stability and transparency of the porous glass also make it suitable for use in the emerging field of optical sensors. In this study fluoride catalysis is used to produce sol gel monoliths with pore radii of up to 400 Angstroms, four times larger than any previously reported using conventional drying techniques. Gel monoliths with pore radii of 200 Angstroms were found to have the best combination of surface area, pore volume and optical transparency. Typical monoliths have surface areas of 150 m2/g and pore volumes of 1.60 cm3/g with good transparency. The monoliths are chemically stable, have good mechanical strength and can be easily rehydrated without cracking. The substrates are also suitable for sintering into dense high purity silica glass with little tendency towards foaming. An in-depth study of the catalytic effect of fluoride on the sol gel process is also included. It has been theorized that fluoride serves to expand the coordination sphere of the silicon center making it more subject to nucleophilic attack. In this work an ion-specific fluoride electrode is used to monitor free fluoride concentrations in HF catalyzed sols while silicic acid is added in the form of tetramethoxysilane (TMOS). It is found that fluoride is rapidly bound by the silicic acid in a ratio of four to one, indicating the formation of silicon tetrafluoride. A concurrent decrease in pH suggests that a pentacoordinate species is formed that is more stable than previously thought. A polymerization mechanism is proposed that explains the hydrophobicity of fluoride catalyzed gels and the difficulty in retaining structural fluoride in fluoride catalyzed sol gel glasses. Finally, several

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  7. Iron porphyrins doped sol-gel glasses: a chemometric study

    International Nuclear Information System (INIS)

    Sacco, Herica C.; Vidoto, Ednalva A.; Nascimento, Otaciro R.

    2000-01-01

    This paper describes the optimized conditions for preparation of iron porphyrin-template doped silica Fe PDS-template) obtained by the sol-gel process. The following porphyrins (Fe P) were used: Fe TFPP Cl, Fe TDCSPP(Na) 4 Cl and Fe TCPP(Na) 4 Cl. Pyridine or 4-phenylimidazole was used as template. The variables that present significant influence on iron porphyrin loading on xerogel were identified and the values that maximize the iron porphyrin loading on xerogel were established . The variables (Solvent volume, fractional factorial design in two levels, 2 5-1 type, generating 16 total experiments for each Fe P studied. (author)

  8. Iron porphyrins doped sol-gel glasses: a chemometric study

    Energy Technology Data Exchange (ETDEWEB)

    Sacco, Herica C.; Vidoto, Ednalva A.; Nascimento, Otaciro R. [Soap Paulo Univ (USP), Sao Carlos (Brazil). Inst. de Fisica; Biazzotto, Juliana C.; Serra, Osvaldo A.; Iamamoto, Yassuko [Sao Paulo Univ. (USP), Ribeirao Preto, SP (Brazil). Faculdade de Filosofia, Ciencias e Letras; Ciuffi, Katia J.; Mello, Cesar A.; Oliveira, Daniela C. de [Universidade de Franca , SP (Brazil)

    2000-07-01

    This paper describes the optimized conditions for preparation of iron porphyrin-template doped silica Fe (PDS-template) obtained by the sol-gel process. The following porphyrins (Fe P) were used: Fe TFPP Cl, Fe TDCSPP(Na){sub 4}Cl and Fe TCPP(Na){sub 4} Cl. Pyridine or 4-phenylimidazole was used as template. The variables that present significant influence on iron porphyrin loading on xerogel were identified and the values that maximize the iron porphyrin loading on xerogel were established. The variables Solvent volume, fractional factorial design in two levels, 2{sup 5-1} type, generating 16 total experiments for each Fe P studied. (author)

  9. Electrochemical redox reactions in solvated silica sol-gel glass

    International Nuclear Information System (INIS)

    Opallo, M.

    2002-01-01

    The studies of electrochemical redox reactions in solvated silica sol-gel glass were reviewed. The methodology of the experiments with emphasis on the direct preparation of the solid electrolyte and the application ultra microelectrodes was described. Generally, the level of the electrochemical signal is not much below that observed in liquid electrolyte. The current depends on time elapsed after gelation, namely the longer time, the smaller current. The differences between electrochemical behaviour of the redox couples in monoliths and thin layers were described. (author)

  10. Synthesis of lithium doped zinc oxide by sol gel

    International Nuclear Information System (INIS)

    Meziane, K; Elhichou, A; Elhamidi, A; Almaggoussi, A; CHHIBA, M

    2016-01-01

    Li-doped ZnO thin films were prepared by sol-gel method and deposed on glass substrate using spin coating technique. The effects of Li on structural and optical properties were investigated. The X-ray diffraction (XRD) analysis reveals that Li incorporation leads to the great improvement of the crystalline quality of ZnO thin films. Scanning electron microscopy (SEM) images showed that nanowires are aligned nearly perpendicular to the substrate plane and are affected significantly by Li incorporation. The optical transmission of the films was higher than 80% in the visible region. It is found that the optical gap and the refractive index remain practically constant. (paper)

  11. Characterization of a sol-gel-entrapped artificial receptor

    Science.gov (United States)

    Dunbar, Richard A.; Narang, Upvan; Prasad, Paras N.; Bright, Frank V.

    1993-04-01

    We report on the development, characterization, and photophysics of a new fiber-optic-based sensor which uses a sol-gel entrapped recognition element. The recognition element is modified (beta) -cyclodextrin to which we have added a short tether (glycine) and a fluorophore (dansyl). This recognition element forms an intramolecular complex, and the dansyl group can include within the cyclodextrin cavity. Non-fluorescent analytes, that bind to the cyclodextrin cavity, can effectively displace the included dansyl group and result in a measurable change in signal. We report on the detection limits, dynamic range, and photophysics (i.e., transduction mechanism) of this new sensor.

  12. Sol-gel synthesis and characterization of lithiummolybdosilicate glass

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  13. Moment scaling at the sol-gel transition

    International Nuclear Information System (INIS)

    Botet, R.

    1998-01-01

    Two standard models of sol-gel transition are revisited here from the point of view of their fluctuations in various moments of both the mass-distribution and the gel-mass. Bond-percolation model is an at-equilibrium system and undergoes a static second-order phase transition, while Monte-Carlo Smoluchowski model is an off-equilibrium one and shows a dynamical critical phenomenon. It is shown that the macroscopic quantities can be splitted into the three classes with different scaling properties of their fluctuations, depending on whether they correspond to: (i) non-critical quantities, (ii) critical quantities or to (iii) an order parameter. (author)

  14. Equipment for production of hydrogel by sol-gel method

    International Nuclear Information System (INIS)

    Urbanek, V.

    1975-01-01

    The method of uranyl gel preparation is described by the sol-gel process of the internal gelation type. A laboratory-scale equipment with an output of 1.5 kg of gel per hour was built at the Nuclear Research Institute, Rez; the diameter of the microspheres produced may vary between 0.5 and 4.0 mm. The reliability of the equipment was verified by producing several tens of kilograms of uranyl gels and of gels based on other non-nuclear materials. (author)

  15. Modified sol-gel coatings for biotechnological applications

    Energy Technology Data Exchange (ETDEWEB)

    Beganskiene, A [Department of General and Inorganic Chemistry, Vilnius University, Vilnius LT-03225 (Lithuania); Raudonis, R [Department of General and Inorganic Chemistry, Vilnius University, Vilnius LT-03225 (Lithuania); Jokhadar, S Zemljic [Faculty of Medicine, Institute of Biophysics, Lipiceva 2, Ljubljana SI-1000 (Slovenia); Batista, U [Faculty of Medicine, Institute of Biophysics, Lipiceva 2, Ljubljana SI-1000 (Slovenia); Kareiva, A [Department of General and Inorganic Chemistry, Vilnius University, Vilnius LT-03225 (Lithuania)

    2007-12-15

    The modified sol-gel derived silica coatings were prepared and characterized. The amino and methyl groups were introduced onto the colloidal silica. The silica coatings with different wettability properties: coloidal silica (water contact angle 17 deg.), polysiloxane (61 deg.), methyl-modified (158 deg. and 46 deg.) coatings samples were tested for CaCo-2 cells proliferation. Methyl-modified coating (46 deg.) proved to be the best substrate for cell proliferation. CaCo-2 cell proliferation two days post seeding was significantly faster on almost laminine, fibronectin and collagen-1 coated samples compared to corresponding controls.

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

    Science.gov (United States)

    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. Persistent superhydrophilicity of sol-gel derived nanoporous silica thin films

    International Nuclear Information System (INIS)

    Ganjoo, S; Azimirad, R; Akhavan, O; Moshfegh, A Z

    2009-01-01

    In this investigation, sol-gel synthesized nanoporous silica thin films, annealed at different temperatures, with long time superhydrophilic property have been studied. Two kinds of sol-gel silica thin films were fabricated by dip-coating of glass substrates in two different solutions; with low and high water. The transparent coated films were dried at 100 deg. C and then annealed in a temperature range of 200-500 deg. C. The average water contact angle of the silica films prepared with low water content and annealed at 300 deg. C measured about 5 deg. for a long time (6 months) without any UV irradiation. Instead, adding water into the sol resulted in silica films with an average water contact angle greater than 60 deg. Atomic force microscopic analysis revealed that the silica films prepared with low water had a rough surface (∼30 nm), while the films prepared with high water had a smoother surface (∼2 nm). Using x-ray photoelectron spectroscopy, we have shown that with a decrease in the surface water on the film, its hydrophilicity increases logarithmically.

  18. Sol-gel auto-combustion synthesis of hydroxyapatite nanotubes array in porous alumina template

    International Nuclear Information System (INIS)

    Yuan Yuan; Liu Changsheng; Zhang Yuan; Shan Xiaoqian

    2008-01-01

    In this paper, an array of highly ordered hydroxyapatite (HAP) nanotubes was synthesized by sol-gel auto-combustion method with porous anodic aluminum oxide (AAO) template for the first time. Based on thermogravimetry (DTA/TG), Fourier transform infrared (FTIR) and X-ray diffraction (XRD), the dried gel, derived from the sol solution with Ca(NO 3 ) 2 .4H 2 O and PO(CH 3 O) 3 as precursors and ethylene glycol as the polymeric matrix, exhibited a typical self-propagating combustion behavior at low temperature, directly resulting in hexagonal crystalline HAP materials. The resultant HAP arrays fabricated from the above sol-gel in the AAO template were uniformly distributed, highly ordered nanotubes with uniform length and diameter according to the observations of scanning electron microscopy (SEM) and transmission electron microscope (TEM). The electron diffraction (ED), XRD and X-ray photoelectron spectroscopy (XPS) survey proved the formation of HAP phase with polycrystalline structure in the AAO template. Based on these results, a potential mechanism of 'an auto-combustion from dried gel to nanoparticles and a subsequent in situ reaction from nanoparticles to nanotubes' was proposed

  19. Graphene oxide-enhanced sol-gel transition sensitivity and drug release performance of an amphiphilic copolymer-based nanocomposite

    Science.gov (United States)

    Hu, Huawen; Wang, Xiaowen; Lee, Ka I; Ma, Kaikai; Hu, Hong; Xin, John H.

    2016-01-01

    We report the fabrication of a highly sensitive amphiphilic copolymer-based nanocomposite incorporating with graphene oxide (GO), which exhibited a low-intensity UV light-triggered sol-gel transition. Non-cytotoxicity was observed for the composite gels after the GO incorporation. Of particular interest were the microchannels that were formed spontaneously within the GO-incorporated UV-gel, which expedited sustained drug release. Therefore, the present highly UV-sensitive, non-cytotoxic amphiphilic copolymer-based composites is expected to provide enhanced photothermal therapy and chemotherapy by means of GO’s unique photothermal properties, as well as through efficient passive targeting resulting from the sol-gel transition characteristic of the copolymer-based system with improved sensitivity, which thus promises the enhanced treatment of patients with cancer and other diseases. PMID:27539298

  20. Sol-gel derived antireflective coatings for silicon

    Energy Technology Data Exchange (ETDEWEB)

    Brinker, C J; Harrington, M S

    1981-08-01

    The preparation of TiO2-SiO2 AR coatings, containing from 30 to 95 mol % TiO2, from alkoxide precursor solutions (titanium tetraethoxide and silicon tetraethoxide) by a sol-gel process is presented. The preparation of the solutions is described, which involves the separate partial hydrolysis of one or both alkoxides prior to their mixing (Yoldas, 1980). The solutions are applied to polished, circular (1 and 2 in. diameter) silicon wafers by a spinning process. The coated wafers are successively heated in air at each of the following temperatures: 200, 300, 350, 400, and 450 C, and optical measurements are performed on them after each heat treatment. The durability of 90 and 95% TiO2 coatings is evaluated in both acidic and basic environments, and reflectivity, film thickness, and refractive index are measured as a function of exposure time. It is shown that sol-gel films applied at 400 C reveal broad regions of antireflectance compared to other titanium-based films.

  1. Sol-gel based sensor for selective formaldehyde determination

    Energy Technology Data Exchange (ETDEWEB)

    Bunkoed, Opas [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Davis, Frank [Cranfield Health, Cranfield University, Bedford MK43 0AL (United Kingdom); Kanatharana, Proespichaya, E-mail: proespichaya.K@psu.ac.th [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Thavarungkul, Panote [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Physics, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Higson, Seamus P.J., E-mail: s.p.j.higson@cranfield.ac.uk [Cranfield Health, Cranfield University, Bedford MK43 0AL (United Kingdom)

    2010-02-05

    We report the development of transparent sol-gels with entrapped sensitive and selective reagents for the detection of formaldehyde. The sampling method is based on the adsorption of formaldehyde from the air and reaction with {beta}-diketones (for example acetylacetone) in a sol-gel matrix to produce a yellow product, lutidine, which was detected directly. The proposed method does not require preparation of samples prior to analysis and allows both screening by visual detection and quantitative measurement by simple spectrophotometry. The detection limit of 0.03 ppmv formaldehyde is reported which is lower than the maximum exposure concentrations recommended by both the World Health Organisation (WHO) and the Occupational Safety and Health Administration (OSHA). This sampling method was found to give good reproducibility, the relative standard deviation at 0.2 and 1 ppmv being 6.3% and 4.6%, respectively. Other carbonyl compounds i.e. acetaldehyde, benzaldehyde, acetone and butanone do not interfere with this analytical approach. Results are provided for the determination of formaldehyde in indoor air.

  2. Sol-gel based sensor for selective formaldehyde determination

    International Nuclear Information System (INIS)

    Bunkoed, Opas; Davis, Frank; Kanatharana, Proespichaya; Thavarungkul, Panote; Higson, Seamus P.J.

    2010-01-01

    We report the development of transparent sol-gels with entrapped sensitive and selective reagents for the detection of formaldehyde. The sampling method is based on the adsorption of formaldehyde from the air and reaction with β-diketones (for example acetylacetone) in a sol-gel matrix to produce a yellow product, lutidine, which was detected directly. The proposed method does not require preparation of samples prior to analysis and allows both screening by visual detection and quantitative measurement by simple spectrophotometry. The detection limit of 0.03 ppmv formaldehyde is reported which is lower than the maximum exposure concentrations recommended by both the World Health Organisation (WHO) and the Occupational Safety and Health Administration (OSHA). This sampling method was found to give good reproducibility, the relative standard deviation at 0.2 and 1 ppmv being 6.3% and 4.6%, respectively. Other carbonyl compounds i.e. acetaldehyde, benzaldehyde, acetone and butanone do not interfere with this analytical approach. Results are provided for the determination of formaldehyde in indoor air.

  3. Sol-gel applications for ceramic membrane preparation

    Science.gov (United States)

    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.

  4. Sol-gel derived zinc oxide films alloyed with cobalt and aluminium

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Mamta [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India); Mehra, R.M., E-mail: rammehra2003@yahoo.co [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India)

    2010-05-03

    ZnO films codoped with 5 at.% Co and 1 at.% Al were prepared by sol-gel technique on corning glass and silicon substrates with precursor sols of different pH values. The pH was varied from 5.4 to 11 by adding varying amounts of monoethanolamine to the sol. Since pH plays an important role in controlling the properties of films, we discuss in detail the effect of pH value on the structural, morphological and optical properties of the grown films. X-ray diffraction and atomic force microscopy images reveal that the size of crystallites increases with pH of the sol. The variation of pH in the reaction system influences the density of homogeneous nucleation and the crystal growth along the c-axis. High quality Co and Al codoped ZnO films annealed at 600 {sup o}C have been obtained using a sol with pH = 9. These sol-gel derived films find their suitability to be used as dilute magnetic semiconductors.

  5. Coating of the orthopaedic titanium alloys with sol-gel derived hydroxyapatite

    International Nuclear Information System (INIS)

    Milev, A.; Green, D.; Chai, C.S.; Ben-Nissan, B.

    1999-01-01

    Hydroxyapatite (HAp) is known to be both biocompatible and bioactive material, however, due to its poor mechanical properties and design limitations is not suitable for applying as a load bearing implant. This could be overcome by using appropriate metallic substrates covered with HAp, derived via different techniques. These coatings allow improved adhesion strength of the load bearing substrate to the bone, resulting in shorter healing periods as well as predictable behaviour of the implant for longer periods of time. There are different techniques of producing HAp appropriate for coating purposes. Due to the small particle size of the grains derived, sol-gel route is preferable where lower sintering temperatures are of primary importance. For better adhesion between substrate and hydroxyapatite coating, the surface of titanium substrate, in this study, was converted to titanium nitride and/or oxynitride. Sintering temperatures of 900 deg C have been used for producing crystalline HAp coatings. The control of sol-gel solutions and the analysis of the coatings were carried out using XRD, SEM and DTA techniques. Results obtained indicate high quality HAp coatings can be produced on titanium substrates especially with complex shapes that benefits over the other coating methods

  6. Sol-gel derived zinc oxide films alloyed with cobalt and aluminium

    International Nuclear Information System (INIS)

    Sharma, Mamta; Mehra, R.M.

    2010-01-01

    ZnO films codoped with 5 at.% Co and 1 at.% Al were prepared by sol-gel technique on corning glass and silicon substrates with precursor sols of different pH values. The pH was varied from 5.4 to 11 by adding varying amounts of monoethanolamine to the sol. Since pH plays an important role in controlling the properties of films, we discuss in detail the effect of pH value on the structural, morphological and optical properties of the grown films. X-ray diffraction and atomic force microscopy images reveal that the size of crystallites increases with pH of the sol. The variation of pH in the reaction system influences the density of homogeneous nucleation and the crystal growth along the c-axis. High quality Co and Al codoped ZnO films annealed at 600 o C have been obtained using a sol with pH = 9. These sol-gel derived films find their suitability to be used as dilute magnetic semiconductors.

  7. Synthesis of ZnO-CuO Nanocomposite Aerogels by the Sol-Gel Route

    Directory of Open Access Journals (Sweden)

    Rula M. Allaf

    2014-01-01

    Full Text Available The epoxide addition sol-gel method has been utilized to synthesize porous zinc-copper composite aerogels in the zinc-to-copper molar ratios of 50 : 50 to 90 : 10. A two-step mixing approach has been employed to produce aerogels composed of nano- to micrometer sized particles. The aerogels were characterized by ultrahigh resolution scanning electron microscopy, transmission electron microscopy, and powder X-ray diffraction. The as-synthesized aerogels had a thin flake- or petal-like microstructure comprised of clustered flakes on two size scales; they were identified as being crystalline with the crystalline species identified as copper nitrate hydroxide, zinc hydroxide chloride hydrate, and zinc hydroxide nitrate hydrate. Annealing of the aerogel materials at a relatively low temperature (400°C resulted in a complete phase transition of the material to give highly crystalline ZnO-CuO aerogels; the aerogels consisted of networked nanoparticles in the ~25–550 nm size range with an average crystallite size of ~3 nm and average crystallinity of 98%. ZnO-CuO aerogels are of particular interest due to their particular catalytic and sensing properties. This work emphasizes the versatility of this sol-gel route in synthesizing aerogels; this method offers a possible route for the fabrication of aerogels of different metal oxides and their composites.

  8. Preparation and characterization of ZnO transparent semiconductor thin films by sol-gel method

    International Nuclear Information System (INIS)

    Tsay, Chien-Yie; Fan, Kai-Shiung; Chen, Sih-Han; Tsai, Chia-Hao

    2010-01-01

    Transparent semiconductor thin films of zinc oxide (ZnO) were deposited onto alkali-free glass substrates by the sol-gel method and spin-coating technique. In this study, authors investigate the influence of the heating rate of the preheating process (4 or 10 o C/min) on the crystallization, surface morphology, and optical properties of sol-gel derived ZnO thin films. The ZnO sol was synthesized by dissolving zinc acetate dehydrate in ethanol, and then adding monoethanolamine. The as-coated films were preheated at 300 o C for 10 min and annealed at 500 o C for 1 h in air ambiance. Experimental results indicate that the heating rate of the preheating process strongly affected the surface morphology and transparency of ZnO thin film. Specifically, a heating rate of 10 o C/min for the preheating process produces a preferred orientation along the (0 0 2) plane and a high transmittance of 92% at a wavelength of 550 nm. Furthermore, this study reports the fabrication of thin-film transistors (TFTs) with a transparent ZnO active channel layer and evaluates their electrical performance.

  9. Holographic sol-gel monoliths: optical properties and application for humidity sensing

    Science.gov (United States)

    Ilatovskii, Daniil A.; Milichko, Valentin; Vinogradov, Alexander V.; Vinogradov, Vladimir V.

    2018-05-01

    Sol-gel monoliths based on SiO2, TiO2 and ZrO2 with holographic colourful diffraction on their surfaces were obtained via a sol-gel synthesis and soft lithography combined method. The production was carried out without any additional equipment at near room temperature and atmospheric pressure. The accurately replicated wavy structure with nanoscale size of material particles yields holographic effect and its visibility strongly depends on refractive index (RI) of materials. Addition of multi-walled carbon nanotubes (MWCNTs) in systems increases their RI and lends absorbing properties due to extremely high light absorption constant. Further prospective and intriguing applications based on the most successful samples, MWCNTs-doped titania, were investigated as reversible optical humidity sensor. Owing to such property as reversible resuspension of TiO2 nanoparticles while interacting with water, it was proved that holographic xerogels can repeatedly act as humidity sensors. Materials which can be applied as humidity sensors in dependence on holographic response were discovered for the first time.

  10. Adhesion strength of lead zirconate titanate sol-gel thin films

    Energy Technology Data Exchange (ETDEWEB)

    Berfield, Thomas A., E-mail: tom.berfield@louisville.edu [Department of Mechanical Engineering, University of Louisville, Louisville, KY 40292 (United States); Kitey, Rajesh [Department of Aerospace Engineering, Indian Institute of Technology Kanpur, Kanpur (India); Kandula, Soma S. [Intel Corporation, Portland, OR (United States)

    2016-01-01

    The adhesion strength between a thin film and substrate is often the critical parameter that controls the initiation as well as the mode of film failure. In this work, a laser-based spallation method is used to determine the adhesion strength of “as deposited” lead zirconate titanate (PZT) sol-gel thin films on the two functionally different substrates. For the first case, PZT sol-gel film is deposited onto bare Si/SiO{sub 2} substrates via spin casting. The extremely high adhesion strength between the film and the substrate necessitated an additional platinum mass superlayer to be deposited on top of the PZT film in order to induce interfacial failure. For the superlayer film system, a hybrid experimental/numerical method is employed for determining the substrate/film interfacial strength, quantified to be in the range of 460–480 MPa. A second substrate variation with lower adhesion strength is also prepared by applying a self-assembled octadecyltrichlorosilane (ODS) monolayer to the Si/SiO{sub 2} substrate prior to the film deposition. For the monolayer-coated substrate case, the adhesion strength is observed to be significantly lower (54.7 MPa) when compared to the earlier case. - Highlights: • A non-contact laser spallation method is used to determine PZT film adhesion. • A mediated self-assembled monolayer is shown to greatly reduce interface strength. • Adhesion strength for even well-bonded thin films was found using a superlayer.

  11. Improvement of Adhesion Properties and Corrosion Resistance of Sol-Gel Coating on Zinc.

    Science.gov (United States)

    Savignac, Pauline; Menu, Marie-Joëlle; Gressier, Marie; Denat, Bastien; Khadir, Yacine El; Manov, Stephan; Ansart, Florence

    2018-05-03

    Corrosion is a major problem for durability of many metals and alloys. Among the efficient classical surface treatments, chromate-based treatments must be banished from industrial use due to their toxicity. At the same time, sol-gel routes have demonstrated high potential to develop an efficient barrier effect against aggressive environments. By this process, the anti-corrosion property can be also associated to others in the case of the development of multi-functional hybrid coatings. In this paper, the main goal is precisely to improve both the corrosion resistance and the adhesion properties of phosphated zinc substrates by the deposition of a hybrid (organic-inorganic) sol-gel layer. To reach this double objective, a choice between two formulations 3-glycidoxypropyltrimethoxysilane (GPTMS)/aluminum-tri-sec-butoxide (ASB) and 3-(trimethoxysilyl)propylmethacrylate (MAP)/tetraethylorthosilicate (TEOS) was firstly made based on the results obtained by microstructural characterizations using SEM, optical analysis, and mechanical characterization such as shock and/or scratch tests (coupled to climatic chamber and salt spray exposure). Several investigations were performed in this study, and the best formulation and performances of the system were obtained by adding a new precursor (1-[3-(trimethoxysilyl)propyl]ureido-UPS) under controlled conditions, as detailed in this paper.

  12. Sol-Gel Derived Hydroxyapatite Coating on Mg-3Zn Alloy for Orthopedic Application

    Science.gov (United States)

    Singh, Sanjay; Manoj Kumar, R.; Kuntal, Kishor Kumar; Gupta, Pallavi; Das, Snehashish; Jayaganthan, R.; Roy, Partha; Lahiri, Debrupa

    2015-04-01

    In recent years, magnesium and its alloys have gained a lot of interest as orthopedic implant constituents because their biodegradability and mechanical properties are closer to that of human bone. However, one major concern with Mg in orthopedics is its high corrosion rate that results in the reduction of mechanical integrity before healing the bone tissue. The current study evaluates the sol-gel-derived hydroxyapatite (HA) coating on a selected Mg alloy (Mg-3Zn) for decreasing the corrosion rate and increasing the bioactivity of the Mg surface. The mechanical integrity of the coating is established as a function of the surface roughness of the substrate and the sintering temperature of the coating. Coating on a substrate roughness of 15-20 nm and sintering at 400°C shows the mechanical properties in similar range of bone, thus making it suitable to avoid the stress-shielding effect. The hydroxyapatite coating on the Mg alloy surface also increases corrosion resistance very significantly by 40 times. Bone cells are also found proliferating better in the HA-coated surface. All these benefits together establish the candidature of sol-gel HA-coated Mg-3Zn alloy in orthopedic application.

  13. Sol-gel niobia sorbent with a positively charged octadecyl ligand providing enhanced enrichment of nucleotides and organophosphorus pesticides in capillary microextraction for online HPLC analysis.

    Science.gov (United States)

    Kesani, Sheshanka; Malik, Abdul

    2018-04-01

    A niobia-based sol-gel organic-inorganic hybrid sorbent carrying a positively charged C 18 ligand (Nb 2 O 5 -C 18 (+ve)) was synthesized to achieve enhanced enrichment capability in capillary microextraction of organophosphorus compounds (which include organophosphorus pesticides and nucleotides) before their online analysis by high-performance liquid chromatography. The sorbent was designed to simultaneously provide three different types of molecular level interactions: electrostatic, Lewis acid-base, and van der Waals interactions. To understand relative contributions of various molecular level analyte-sorbent interactions in the extraction process, two other sol-gel niobia sorbents were also created: (a) a purely inorganic sol-gel niobia sorbent (Nb 2 O 5 ) and (b) an organic-inorganic hybrid sol-gel niobia sorbent carrying an electrically neutral-bonded octadecyl ligand (Nb 2 O 5 -C 18 ). The extraction efficiency of the created sol-gel niobia sorbent (Nb 2 O 5 -C 18 (+ve)) was compared with that of analogously designed and synthesized titania-based sol-gel sorbent (TiO 2 -C 18 (+ve)), taking into consideration that titania-based sorbents present state-of-the-art extraction media for organophosphorus compounds. In capillary microextraction with high-performance liquid chromatography analysis, Nb 2 O 5 -C 18 (+ve) had shown 40-50% higher specific extraction values (a measure of extraction efficiency) over that of TiO 2 -C 18 (+ve). Compared to TiO 2 -C 18 (+ve), Nb 2 O 5 -C 18 (+ve) also provided superior analyte desorption efficiency (96 vs. 90%) during the online release of the extracted organophosphorus pesticides from the sorbent coating in the capillary microextraction capillary to the chromatographic column using reversed-phase high-performance liquid chromatography mobile phase. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

    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 (ZrO 2 -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 ZrCl 4 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 ZrO 2 -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. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

    International Nuclear Information System (INIS)

    Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve; Berthier, Serge

    2008-01-01

    An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C

  16. Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

    Energy Technology Data Exchange (ETDEWEB)

    Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve [Unite mixte CNRS/Saint Gobain Saint Gobain Recherche, BP135, 93303 Aubervilliers (France); Berthier, Serge [Institut des Nanosciences de Paris, UMR 7588, CNRS, Universite Pierre et Marie Curie-Paris 6, 140 rue Lourmel, 75015 Paris (France)], E-mail: cperoz@lbl.gov

    2008-12-01

    An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C.

  17. Preparation and studies of Co(II) and Co(III)-substituted barium ferrite prepared by sol-gel method

    International Nuclear Information System (INIS)

    Teh, Geok Bee; Nagalingam, Saravanan; Jefferson, David A.

    2007-01-01

    The sol-gel preparative method was employed to synthesise Co(II) and Co(III)-substituted barium ferrite. This method was attempted to achieve higher homogeneity of the final product. Samples of substituted ferrites were characterised by various experimental techniques including high resolution transmission electron microscopy, X-ray diffraction analysis, magnetometry and thermal gravimetric analysis. The microstructural changes induced by such substitution are also discussed

  18. Preparation and studies of Co(II) and Co(III)-substituted barium ferrite prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Teh, Geok Bee [Department of Bioscience and Chemistry, Faculty of Engineering and Science, Universiti Tunku Abdul Rahman, 53300 Kuala Lumpur (Malaysia)]. E-mail: tehgb@mail.utar.edu.my; Nagalingam, Saravanan [Department of Bioscience and Chemistry, Faculty of Engineering and Science, Universiti Tunku Abdul Rahman, 53300 Kuala Lumpur (Malaysia); Jefferson, David A. [Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW (United Kingdom)

    2007-01-15

    The sol-gel preparative method was employed to synthesise Co(II) and Co(III)-substituted barium ferrite. This method was attempted to achieve higher homogeneity of the final product. Samples of substituted ferrites were characterised by various experimental techniques including high resolution transmission electron microscopy, X-ray diffraction analysis, magnetometry and thermal gravimetric analysis. The microstructural changes induced by such substitution are also discussed.

  19. Fabrication of YBa2Cu3O7-δ superconducting fibers by the sol-gel method

    International Nuclear Information System (INIS)

    Umeda, Tetsu; Kozuka, Hiromitsu; Sakka, Sumio

    1988-01-01

    High-T c superconducting oxide fibers were fabricated by the sol-gel method. An aqueous solution of metal acetates was concentrated to form a viscous sol, from which gel fibers were spun. The gel fibers, 5 to 1,000 μm in diameter, were converted to ceramic fibers by heating to 900 degree C. The fired fibers (T c (onset) of 94 K and T c (end) of 62.2 K) were rough and had porous microstructures

  20. Mechanical and thermal expansion properties of β-eucryptite prepared by sol-gel methods and hot pressing

    International Nuclear Information System (INIS)

    Xia, L.; Wen, G.W.; Qin, C.L.; Wang, X.Y.; Song, L.

    2011-01-01

    Research highlights: → Dense LAS glass-ceramics were fabricated by sol-gel and hot pressing technique. → The LAS glass-ceramics have relative good mechanical properties. → The negative thermal expansion behavior of LAS glass-ceramics was investigated. -- Abstract: The microstructures, mechanical properties and thermal expansion behavior of monolithic lithium aluminosilicate glass-ceramics, prepared by sol-gel method and hot pressing, were investigated by using X-ray diffraction, scanning and transmission electron microscopies, three-point bend tests and dilatometry. β-eucryptite appeared as main phase in the monolithic lithium aluminosilicate glass-ceramics. The glass ceramics exhibited high relative densities and the average flexural strength and fracture toughness values were 154 MPa and 2.46 MPa m 1/2 , respectively. The lithium aluminosilicate glass-ceramics hot pressed 1300 and 1350 o C demonstrated negative coefficient of thermal expansion, which was affected by amount and type of crystalline phases.

  1. Development and application of a sol-gel immunosorbent-based method for the determination of isoproturon in surface water.

    Science.gov (United States)

    Zhang, Xiuli; Martens, Dieter; Krämer, Petra M; Kettrup, Antonius A; Liang, Xinmiao

    2006-01-13

    An immunosorbent was fabricated by encapsulation of monoclonal anti-isoproturon antibodies in sol-gel matrix. The immunosorbent-based loading, rinsing and eluting processes were optimized. Based on these optimizations, the sol-gel immunosorbent (SG-IS) selectively extracted isoproturon from an artificial mixture of 68 pesticides. In addition to this high selectivity, the SG-IS proved to be reusable. The SG-IS was combined with liquid chromatography-tandem mass spectrometry (LC-MS-MS) to determine isoproturon in surface water, and the linear range was up to 2.2 microg/l with correlation coefficient higher than 0.99 and relative standard deviation (RSD) lower than 5% (n=8). The limit of quantitation (LOQ) for 25-ml surface water sample was 5 ng/l.

  2. Dielectric Properties of Sol-Gel Derived Barium Strontium Titanate and Microwave Sintering of Ceramics

    Science.gov (United States)

    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

  3. Effects of parameters of sol-gel process on the phase evolution of sol-gel-derived hydroxyapatite

    International Nuclear Information System (INIS)

    Eshtiagh-Hosseini, Hossein; Housaindokht, Mohammad Reza; Chahkandi, Mohammad

    2007-01-01

    It has been established that hydroxyapatite powders can be produced using an alkoxide-based sol-gel technique. Nanocrystalline powders of hydroxyapatite (HA) were prepared from Ca(NO 3 ) 2 .4H 2 O and PO(OC 2 H 5 ) 3 as calcium and phosphorus precursors, respectively, using a sol-gel route. For a number of samples, sol of phosphorus was first hydrolyzed for 24 h with distilled water. The sol temperature, aging time and heat treatment temperature on apatite formation were systematically studied. Increasing the aging time affected the reducing of CaO. Also, increasing the mixed sol solution temperature up to 80 deg. C had a positive effect on the disappearance of impurity phases. With the increase of the calcination temperature >600 deg. C, calcium phosphate impurity phases disappeared. Structural evolution during the synthesis of hydroxyapatite is investigated by using infrared (IR) analysis, X-ray diffraction (XRD), thermal behavior (DTA), and elemental analysis of electron microscopy examination (SEM). X-ray diffraction with the aid of Scherrer and Williamson-Hall equations has been used to characterize the distributions of crystallite size and micro-strain of HA powders .The results indicated that mean crystallite size increased and micro-strain decreased significantly with the rise in firing temperature

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

    Science.gov (United States)

    Watkins, Anthony N. (Inventor); Leighty, Bradley D. (Inventor); Oglesby, Donald M. (Inventor); Patry, 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.

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

    Science.gov (United States)

    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. Reprint & Copyright © 2014 Association of Military Surgeons of the U.S.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  7. Photocatalytic degradation of methylene blue dye by zinc oxide nanoparticles obtained from precipitation and sol-gel methods.

    Science.gov (United States)

    Balcha, Abebe; Yadav, Om Prakash; Dey, Tania

    2016-12-01

    Zinc oxide (ZnO) nanoparticles were synthesized by precipitation and sol-gel methods. The aim of this study was to understand how different synthetic methods can affect the photocatalytic activity of ZnO nanoparticles. As-synthesized ZnO nanoparticles were characterized by X-ray diffraction (XRD) and UV-Visible spectroscopic techniques. XRD patterns of ZnO powders synthesized by precipitation and sol-gel methods revealed their hexagonal wurtzite structure with crystallite sizes of 30 and 28 nm, respectively. Their photocatalytic activities were evaluated by photocatalytic degradation of methylene blue, a common water pollutant, under UV radiation. The effects of operational parameters such as photocatalyst load and initial concentration of the dye on photocatalytic degradation of methylene blue were investigated. While the degradation of dye decreased over the studied dye concentration range of 20 to 100 mg/L, an optimum photocatalyst load of 250 mg/L was needed to achieve dye degradation as high as 81 and 92.5 % for ZnO prepared by precipitation and sol-gel methods, respectively. Assuming pseudo first-order reaction kinetics, this corresponded to rate constants of 8.4 × 10 -3 and 12.4 × 10 -3  min -1 , respectively. Hence, sol-gel method is preferred over precipitation method in order to achieve higher photocatalytic activity of ZnO nanostructures. Photocatalytic activity is further augmented by better choice of capping ligand for colloidal stabilization, starch being more effective than polyethylene glycol (PEG).

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

    Science.gov (United States)

    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.

  9. Anion embedded sol-gel films on Al for corrosion protection

    International Nuclear Information System (INIS)

    Sheffer, Mari; Groysman, Alec; Starosvetsky, David; Savchenko, Natali; Mandler, Daniel

    2004-01-01

    We report here on the successful incorporation of organic anions into a sol-gel film on Al as a means of enhancing the protection against corrosion. Following our previous study where we showed that hydrophobic sol-gel films provided pronounced corrosion inhibition, we studied the corrosion inhibition that phenylphosphonic acid (PPA) has when embedded inside a thin sol-gel coating on Al. The anion of this organic anion tends to stay inside a phenyltrimethoxysilane (PTMOS) based sol-gel film due to π-interactions. Our findings, which are derived primarily from potentiodynamic polarization measurements, electrochemical noise, scanning electron microscopy measurements and Auger electron spectroscopy (AES), clearly show that the organic phosphonate adds to the protection efficiency of the sol-gel film

  10. Sol-gel titania-coated needles for solid phase dynamic extraction-GC/MS analysis of desomorphine and desocodeine.

    Science.gov (United States)

    Su, Chi-Ju; Srimurugan, Sankarewaran; Chen, Chinpiao; Shu, Hun-Chi

    2011-01-01

    Novel sol-gel titania film coated needles for solid-phase dynamic extraction (SPDE)-GC/MS analysis of desomorphine and desocodeine are described. The high thermal stability of titania film permits efficient extraction and analysis of poorly volatile opiate drugs. The influences of sol-gel reaction time, coating layer, extraction and desorption time and temperature on the SPDE needle performance were investigated. The deuterium labeled internal standard was introduced either during the extraction of analyte or directly injected to GC after the extraction process. The latter method was shown to be more sensitive for the analysis of water and urine samples containing opiate drugs. The proposed conditions provided a wide linear range (from 5-5000 ppb), and satisfactory linearity, with R(2) values from 0.9958 to 0.9999, and prominent sensitivity, LOQs (1.0-5.0 ng/g). The sol-gel titania film coated needle with SPDE-GC/MS will be a promising technique for desomorphine and desocodeine analysis in urine.

  11. Dielectric and piezoelectric properties of sol-gel derived Ca doped PbTiO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Chauhan, Arun Kumar Singh [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India); Gupta, Vinay [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India)]. E-mail: drvin_gupta@rediffmail.com; Sreenivas, K. [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India)

    2006-06-15

    Synthesis of Ca doped PbTiO{sub 3} powder by a chemically derived sol-gel process is described. Crystallization characteristics of different compositions Pb{sub 1-x}Ca {sub x}TiO{sub 3} (PCT) with varying calcium (Ca) content in the range x = 0-0.45 has been investigated by DTA/TGA, X-ray diffraction and scanning electron microscopy. The crystallization temperature is found to decrease with increasing calcium content. X-ray diffraction reveals a tetragonal structure for PCT compositions with x {<=} 0.35, and a cubic structure for x = 0.45. Dielectric properties on sintered ceramics prepared with fine sol-gel derived powders have been measured. The dielectric constant is found to increase with increasing Ca content, and the dielectric loss decreases continuously. Sol-gel derived Pb{sub 1-x}Ca {sub x}TiO{sub 3} ceramics with x = 0.45 after poling exhibit infinite electromechanical anisotropy (k {sub t}/k {sub p}) with a high d {sub 33} = 80 pC/N, {epsilon}' = 298 and low dielectric loss (tan {delta} = 0.0041)

  12. A review of hydroxyapatite-based coating techniques: Sol-gel and electrochemical depositions on biocompatible metals.

    Science.gov (United States)

    Asri, R I M; Harun, W S W; Hassan, M A; Ghani, S A C; Buyong, Z

    2016-04-01

    New promising techniques for depositing biocompatible hydroxyapatite-based coatings on biocompatible metal substrates for biomedical applications have continuously been exploited for more than two decades. Currently, various experimental deposition processes have been employed. In this review, the two most frequently used deposition processes will be discussed: a sol-gel dip coating and an electrochemical deposition. This study deliberates the surface morphologies and chemical composition, mechanical performance and biological responses of sol-gel dip coating as well as the electrochemical deposition for two different sample conditions, with and without coating. The review shows that sol-gel dip coatings and electrochemical deposition were able to obtain the uniform and homogeneous coating thickness and high adherent biocompatible coatings even in complex shapes. It has been accepted that both coating techniques improve bone strength and initial osseointegration rate. The main advantages and limitations of those techniques of hydroxyapatite-based coatings are presented. Furthermore, the most significant challenges and critical issues are also highlighted. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Solid-phase microextraction Ni-Ti fibers coated with functionalised silica particles immobilized in a sol-gel matrix.

    Science.gov (United States)

    Azenha, Manuel; Ornelas, Mariana; Fernando Silva, A

    2009-03-20

    One of the possible approaches for the development of novel solid-phase microextraction (SPME) fibers is the physical deposition of porous materials onto a support using high-temperature epoxy glue. However, a major drawback arises from decomposition of epoxy glue at temperatures below 300 degrees C and instability in some organic solvents. This limitation motivated us to explore the possibility of replacing the epoxy glue with a sol-gel film, thermally more stable and resistant to organic solvents. We found that functionalised silica particles could be successfully attached to a robust Ni-Ti wire by using a UV-curable sol-gel film. The particles were found to be more important than the sol-gel layer during the microextraction process, as shown by competitive extraction trials and by the different extraction profiles observed with differently functionalised particles. If a quality control microscopic-check aiming at the rejection of fibers exhibiting unacceptably low particle load was conducted, acceptable (6-14%) reproducibility of preparation of C(18)-silica fibers was observed, and a strong indication of the durability of the fibers was also obtained. A cyclohexyldiol-silica fiber was used, as a simple example of applicability, for the successful determination of benzaldehyde, acetophenone and dimethylphenol at trace level in spiked tap water. Recoveries: 95-109%; limits of detection: 2-7 microg/L; no competition effects within the studied range (

  14. Sol-gel open tubular ODS columns with reversed electroosmotic flow for capillary electrochromatography.

    Science.gov (United States)

    Hayes, J D; Malik, A

    2001-03-01

    Sol-gel chemistry was successfully used for the fabrication of open tubular columns with surface-bonded octadecylsilane (ODS) stationary-phase coating for capillary electrochromatography (OT-CEC). Following column preparations, a series of experiments were performed to investigate the performance of the sol-gel coated ODS columns in OT-CEC. The incorporation of N-octadecyldimethyl[3-(trimethoxysilyl)propyl]ammonium chloride as one of the sol-gel precursors played an important role in the electrochromatographic performance of the prepared columns. This chemical reagent possesses a chromatographically favorable, bonded ODS moiety, in conjunction with three methoxy groups allowing for sol-gel reactivity. In addition, a positively charged nitrogen atom is present in the molecular structure of this reagent and provides a positively charged capillary surface responsible for the reversed electroosmotic flow (EOF) in the columns during CEC operation. Comparative studies involving the EOF within such sol-gel ODS coated and uncoated capillaries were performed using acetonitrile and methanol as the organic modifiers in the mobile phase. The use of a deactivating reagent, phenyldimethylsilane, in the sol-gel solution was evaluated. Efficiency values of over 400,000 theoretical plates per meter were achieved in CEC on a 64 cm x 25 microm i.d. sol-gel ODS open tubular column. Test mixtures of polycyclic aromatic hydrocarbons, benzene derivatives, and aromatic aldehydes and ketones were used to evaluate the CEC performances of both nondeactivated and deactivated open tubular sol-gel columns. The effects of mobile-phase organic modifier contents and pH on EOF in such columns were evaluated. The prepared sol-gel ODS columns are characterized by switchable electroosmotic flow. A pH value of approximately 8.5 was found correspond to the isoelectric point for the prepared sol-gel ODS coatings.

  15. Synthesis of ZNO nanoparticles by Sol-Gel processing

    International Nuclear Information System (INIS)

    Savi, B.M.; Rodrigues, L.; Uggioni, E.; Bernardin, A.M.

    2011-01-01

    The aim of this study was to obtain and characterize ZnO nanoparticles by Sol-Gel technique. ZnCl 2 , Zn(NO 3 ) 2 , NaOH were used as precursors for the synthesis. NaOH was dissolved in distilled water at a concentration of 1.0 M with agitation to the desired reaction temperature (50°C and 90°C). 0.5 M ZnCl 2 and 0.5 M Zn(NO3)2 were added by dripping (60 and 30 min). The powder was characterized by XRD (Cu Kα), UV-Vis, and HR-TEM. Nano ZnO particles were obtained with crystallite size between 20 and 40 nm (HR-TEM and XRD). The results of UV-Vis spectrometry show that the band gap energy, given by the absorbance at 300 nm depends on the precursor used. (author)

  16. Bioorganically doped sol-gel materials containing amyloglucosidase activity

    Directory of Open Access Journals (Sweden)

    Vlad-Oros Beatrice

    2006-01-01

    Full Text Available Amyloglucosidase (AMG from Aspergillus niger was encapsulated in various matrices derived from tetraethoxysilane, methyltriethoxysilane, phenyltriethoxysilane and vinyltriacetoxysilane by different methods of immobilization. The immobilized enzyme was prepared by entrapment in two steps, in one-step and entrapment/deposition, respectively. The activities of the immobilized AMG were assayed and compared with that of the native enzyme. The effects of the organosilaneprecursors and their molar ratios, the immobilization method, the inorganic support (white ceramic, red ceramic, purolite, alumina, TiO2, celite, zeolite and enzyme loading upon the immobilized enzyme activity were tested. The efficiency of the sol-gel biocomposites can be improved through combination of the fundamental immobilization techniques and selection of the precursors.

  17. Polymer sol-gel composite inverse opal structures.

    Science.gov (United States)

    Zhang, Xiaoran; Blanchard, G J

    2015-03-25

    We report on the formation of composite inverse opal structures where the matrix used to form the inverse opal contains both silica, formed using sol-gel chemistry, and poly(ethylene glycol), PEG. We find that the morphology of the inverse opal structure depends on both the amount of PEG incorporated into the matrix and its molecular weight. The extent of organization in the inverse opal structure, which is characterized by scanning electron microscopy and optical reflectance data, is mediated by the chemical bonding interactions between the silica and PEG constituents in the hybrid matrix. Both polymer chain terminus Si-O-C bonding and hydrogen bonding between the polymer backbone oxygens and silanol functionalities can contribute, with the polymer mediating the extent to which Si-O-Si bonds can form within the silica regions of the matrix due to hydrogen-bonding interactions.

  18. Uranium Dioxide Powder Flow ability Improvement Using Sol-Gel

    International Nuclear Information System (INIS)

    Juanda, D.; Sambodo Daru, G.

    1998-01-01

    The improvement of flow ability characteristics of uranium dioxide powder has been done using sol-gel process. To anticipate a pellet mass production with uniform pellet dimension, the uranium dioxide powder must be have a spherical form. Uranium dioxide spherical powder has been diluted in acid transformed into sol colloidal solution. To obtain uranium dioxide spherical form, the uranium sol-colloidal solution has been dropped in a hot paraffin ( at the temperature of 90 0 C) to form gelatinous colloid and then dried at 800 0 C, and sintered at the temperature of 1700 0 C. The flow ability of spherical uranium dioxide powder has been examined by using Flowmeter Hall (ASTM. B. 213-46T). The measurement result reveals that the spherical uranium dioxide powder has a flow ability twice than that of unprocessed uranium dioxide powder

  19. Manufacture of Regularly Shaped Sol-Gel Pellets

    Science.gov (United States)

    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.

  20. Application of Sol-Gel Method as a Protective Layer on a Specular Reflective Surface for Secondary Reflector in a Solar Receiver

    Energy Technology Data Exchange (ETDEWEB)

    Afrin, Samia; Dagdelen, John; Ma, Zhiwen; Kumar, Vinod

    2017-01-01

    Highly-specular reflective surfaces that can withstand elevated-temperatures are desirable for many applications including reflective heat shielding in solar receivers and secondary reflectors, which can be used between primary concentrators and heat collectors. A high-efficiency, high-temperature solar receiver design based on arrays of cavities needs a highly-specular reflective surface on its front section to help sunlight penetrate into the absorber tubes for effective flux spreading. Since this application is for high-temperature solar receivers, this surface needs to be durable and to maintain its optical properties through the usable life. Degradation mechanisms associated with elevated temperatures and thermal cycling, which include cracking, delamination, corrosion/oxidation, and environmental effects, could cause the optical properties of surfaces to degrade rapidly in these conditions. Protected mirror surfaces for these applications have been tested by depositing a thin layer of SiO2 on top of electrodeposited silver by means of the sol-gel method. To obtain an effective thin film structure, this sol-gel procedure has been investigated extensively by varying process parameters that affect film porosity and thickness. Endurance tests have been performed in a furnace at 150 degrees C for thousands of hours. This paper presents the sol-gel process for intermediate-temperature specular reflective coatings and provides the long-term reliability test results of sol-gel protected silver-coated surfaces.

  1. Characterization of selenium doped silica glasses synthesized by sol-gel method

    International Nuclear Information System (INIS)

    Kobayashi, R.A.; Toffoli, S.M.

    2012-01-01

    Selenium is a rare element in nature. It is used in the food, pharmaceutical, and glass industries. In commercial glasses, selenium is the element responsible for most of the pink or light red color, but its effect is primarily dependent on the oxidation state of the element in the glassy matrix. Besides, selenium is highly volatile, and as high as 80 wt% may be lost in the furnace during the industrial glass elaboration. The sol– gel method yields synthesized materials of high purity and homogeneity, and uses low processing temperatures. Samples of silica glass were obtained by sol-gel method, incorporating precursors of selenium, with the main objective of reducing selenium losses during its heating. The results of optical absorption, XRD and thermal analysis (TGA, DSC) of the glasses are presented and discussed. (author)

  2. A utilização de materiais obtidos pelo processo de sol-gel na construção de biossensores The utilization of materials obtained by the sol-gel process in biosensors construction

    Directory of Open Access Journals (Sweden)

    Antonio A. S. Alfaya

    2002-09-01

    Full Text Available The use of sol-gel materials to develop new biosensors has received great attention due to its characteristics and versatility of sol-gel process. An overview is presented of the state-of-the-art of electrochemical biosensors employing sol-gel materials. Low-temperature, porous sol-gel ceramics represent a new class for the immobilization of biomolecules. The rational design of sol-gel sensing materials, based on the judicious choice of the starting alkoxide, encapsulated reagents, and preparation conditions, allows tailoring of material properties in a wide range, and offers great potential for the development of electrochemical biosensors.

  3. Formulation and evaluation of antimicrobial activity of Morus alba sol-gel against periodontal pathogens

    Directory of Open Access Journals (Sweden)

    Shilpa Gunjal

    2015-01-01

    Full Text Available Background: Periodontitis has a multifactorial etiology, with primary etiologic agents being pathogenic bacteria that reside in the subgingival area. Recent advances in the field of alternative medicine introduced various herbal products for the treatment of periodontitis. Aim: To assess and compare the antimicrobial activity of Morus alba sol-gel with chlorhexidine sol-gel against ATCC standard strains of Aggregatibacter actinomycetemcomitans, Porphyromonas gingivalis, and Tannerella forsythia. Materials and Methods: Crude extract of Morus alba leaves was prepared by Soxhlet method by using ethanol as a solvent. Phytochemical screening of the crude extract of M. alba was performed to check the various chemical constituents. M. alba sol-gel and chlorhexidine sol-gel were formulated using Pluronic f127 and Pluronic f108 and compared for their antimicrobial activity. The minimum inhibitory concentration of both the gels was performed using agar well diffusion technique. Results: The minimum inhibitory concentration of M. alba sol-gel and chlorhexidine sol-gel against A. actinomycetemcomitans is 19 and 17 mm, T. forsythia is 12 and 21 mm, and P. gingivalis is 16 and 18 mm, respectively. Conclusion: Both M. alba and chlorhexidine sol-gel exhibited potent antimicrobial activity against periodontal pathogens.

  4. Organic carbon aerogels from the sol-gel polymerization of phenolic-furfural mixtures

    Science.gov (United States)

    Pekala, R.W.

    1998-04-28

    The sol-gel polymerization of a phenolic-furfural mixture in dilute solution leads to a highly cross-linked network that can be supercritically dried to form a high surface area foam. These porous materials have cell/pore sizes {<=}1000 {angstrom}, and although they are dark brown in color, they can be classified as a new type of aerogel. The phenolic-furfural aerogel can be pyrolyzed in an inert atmosphere at 1050 C to produce carbon aerogels. This new aerogel may be used for thermal insulation, chromatographic packing, water filtration, ion-exchange, and carbon electrodes for energy storage devices, such as batteries and double-layer capacitors. 8 figs.

  5. Organic aerogels from the sol-gel polymerization of phenolic-furfural mixtures

    Science.gov (United States)

    Pekala, R.W.

    1995-12-19

    The sol-gel polymerization of a phenolic-furfural mixture in dilute solution leads to a highly cross-linked network that can be supercritically dried to form a high surface area foam. These porous materials have cell/pore sizes{<=}1000{angstrom}, and although they are dark brown in color, they can be classified as a new type of aerogel. The phenolic-furfural aerogel can be pyrolyzed in an inert atmosphere at 1050 C to produce carbon aerogels. This new aerogel may be used for thermal insulation, chromatographic packing, water filtration, ion-exchange, and carbon electrodes for energy storage devices, such as batteries and double-layer capacitors. 8 figs.

  6. Template-directed formation of functional complex metal-oxide nanostructures by combination of sol-gel processing and spin coating

    International Nuclear Information System (INIS)

    Choi, Y.C.; Kim, J.; Bu, S.D.

    2006-01-01

    We report the template-based formation of functional complex metal-oxide nanostructures by a combination of sol-gel processing and spin coating. This method employs the spin-coating of a sol-gel solution into an anodic aluminum oxide membrane (SSAM). Various metal-oxide nanowires and nanotubes with a high aspect-ratio were prepared. The aspect-ratios of the PbO 2 nanowires and Pb(Zr 0.52 Ti 0.48 )O 3 nanowires were about 300 and 400, respectively, and their diameters were about 50 nm. The fabricated PbTiO 3 nanotubes have a relatively constant wall thickness of about 20 nm with an outer diameter of about 60 nm. The deposition time for all of the fabricated metal-oxide nanowires and nanotubes is less than 120 s, which is far shorter than those required in both the sol-gel dipping and sol-gel electrophoretic methods. These results indicate that the SSAM method can be a versatile pathway to prepare functional complex metal-oxide nanowires and nanotubes with a high aspect-ratio. The possible formation process for the one-dimensional nanostructures by SSAM is discussed

  7. Minimally Adhesive, Advanced Non-toxic Coatings of Dendrimeric Catalysts in Sol-Gel Matrices

    Science.gov (United States)

    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...Technical Report for ONR N00014-09-1-0217 Minimally Adhesive, Advanced Non-toxic Coatings of Dendrimeric Catalysts in Sol -Gel Matrices Michael R. Detty, PI...Environmentally benign sol -gel antifouling and foul-releasing coatings. Ace. Chem. Res. 2014, 47, 678-687. 11) Alberto, E. E.; Müller, L. M

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

    Science.gov (United States)

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

    2017-03-01

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

  9. A novel green nonaqueous sol-gel process for preparation of partially stabilized zirconia nanopowder

    Directory of Open Access Journals (Sweden)

    Guo Feng

    2017-09-01

    Full Text Available A novel green nonaqueous sol-gel process was developed to prepare 3 mol% Y2O3-doped ZrO2 nanopowder from zirconium oxychloride and without need for washing of the obtained particles. It was shown that highly dispersive nanometer-scale zirconia powder with the particle size of 15–25 nm and BET surface area of 41.2 m2/g can be prepared. The sintering behaviour was also investigated. Density of the translucent body sintered at 1400 °C is 98.7 ± 0.3% of its theoretical density and the surface and cross section areas are dense without holes or other defects. The bending strength of the sintered sample is 928 ± 64 MPa.

  10. Use of hydroxyapatite prepared by sol-gel method for gamma ray and electron beam dosimetry

    International Nuclear Information System (INIS)

    Hajiloo, N.; Ziaie, F.; Hesami, M.

    2011-01-01

    In this research, radiation dosimetry was made through measuring free radicals induced in synthetic hydroxyapatite using EPR spectroscopy. At the first step, the hydroxyapatite nano-powders were synthesized via sol-gel method. The produced powders were passed through a thermal treatment, weighted and packed. Then, the samples were irradiated at different dose rates using 60 Co γ-ray and 10 MeV electron beam radiation at a high dose range. The hydroxyapatite signal intensity of hydroxyapatite samples were measured at room temperature in the air. Subsequently, the variations of the EPR signal intensities were constructed as peak-to-peak signal amplitude and were compared with alanine and bone powder samples. The results showed that the EPR signal intensity of the hydroxyapatite samples are several times higher than alanine and bone powder and are saturated at the higher dose rates in comparison with other species.

  11. Enhanced emission of nile red fluorescent nanoparticles embedded in hybrid sol-gel glasses.

    Science.gov (United States)

    Ferrer, Maria L; del Monte, Francisco

    2005-01-13

    Highly fluorescent Nile Red (NR) nanoparticles embedded in a hybrid sol-gel glass are reported. The crystallite growth within the confined system created by the porous hybrid matrix results in NR nanoparticles of averaged dimensions below 36 nm. The preparation process allows for the control of both the conformation adopted by single NR molecules prior to aggregation (e.g., near planar) and the configuration of the aggregates (e.g., oblique with phi architecture which ultimately forms the nanoparticles. The full preservation of the fluorescent configuration of the aggregates in the nanoparticles is confirmed through the application of the exciton theory, and it is responsible for the significant increase of the fluorescence emission intensity (e.g., up to 525- and 70-fold as compared to that obtained for single NR molecules embedded in pure and hybrid silica glasses, respectively).

  12. Effect of templates on inverse opals fabricated through annular self-assembly/sol-gel method

    International Nuclear Information System (INIS)

    Ge Dengteng; Yang Lili; Fan Zeng; Zhao Jiupeng; Li Yao

    2011-01-01

    Highlights: → Flexible inverse opals could be facilely prepared through annular growth method. → The infiltrated materials are highly densified due to the existence of templates. → The crystalline grains are refined due to the the existence of templates. - Abstract: There is a strong interest in simple preparation of flexible inverse opals for applications. In this article, indium tin oxides (ITO) flexible inverse opals were prepared through annular growth of templates and sol-gel process. It is shown that this method provides a facile route for large scale flexible inverse opals with excellent ordered structures. ITO materials are found much denser in inverse opals, which is due to the increased capillary force during drying process and enhanced shrinkage during annealing process. It is also found that the crystalline grains are refined and the photoluminescence performance is strengthened in low frequency.

  13. Sol-gel synthesis and densification of aluminoborosilicate powders. Part 1: Synthesis

    Science.gov (United States)

    Bull, Jeffrey; Selvaduray, Guna; Leiser, Daniel

    1992-01-01

    Aluminoborosilicate powders high in alumina content were synthesized by the sol-gel process utilizing various methods of preparation. Properties and microstructural effects related to these syntheses were examined. After heating to 600 C for 2 h in flowing air, the powders were amorphous with the metal oxides comprising 87 percent of the weight and uncombusted organics the remainder. DTA of dried powders revealed a T(sub g) at approximately 835 C and an exotherm near 900 C due to crystallization. Powders derived from aluminum secbutoxide consisted of particles with a mean diameter 5 microns less than those from aluminum isopropoxide. Powders synthesized with aluminum isopropoxide produced agglomerates comprised of rod shaped particulates while powders made with the secbutoxide precursor produced irregular glassy shards. Compacts formed from these powders required different loadings for equivalent densities according to the method of synthesis.

  14. Morphological, Structural, and Electrical Characterization of Sol-Gel-Synthesized ZnO Nano rods

    International Nuclear Information System (INIS)

    Kashif, M.; Hashim, U.; Foo, K.L.; Ali, M.E.; Ali, M.E.; Ali, S.M.U.

    2013-01-01

    ZnO nano rods were grown on thermally oxidized p-type silicon substrate using sol-gel method. The SEM image revealed high-density, well-aligned, and perpendicular ZnO nano rods on the oxidized silicon substrate. The XRD profile confirmed the c-axis orientation of the nano rods. PL measurements showed the synthesized ZnO nano rods have strong ultraviolet (UV) emission. The electrical characterization was performed using interdigitated silver electrodes to investigate the stability in the current flow of the fabricated device under different ultraviolet (UV) exposure times. It was notified that a stable current flow was observed after 60 min of UV exposure. The determination of stable current flow after UV exposure is necessary for UV-based gas sensing and optoelectronic devices.

  15. Sol gel coatings doped with Ce ions deposited on industrial applications metals

    International Nuclear Information System (INIS)

    Pepe, A; Aparicio, M; Duran, A; Cere, S

    2004-01-01

    Compounds that contain chromates as corrosion inhibitors are widely used. Since these compounds are highly toxic, enormous efforts are being made to replace them. The lanthanides, especially cerium, have the right properties for this substitution. Different substrates can be protected by a variety of coatings. The sol-gel derived films can be deposited on different metals or alloys to increase their resistance to corrosion or to modify their surface properties by doped with different substances that can increase their protective strength, by combining the barrier capacity of the hybrid coating with the inhibitory properties of the cerium. This work presents the conditions for obtaining soles doped with cerium III and IV salts at room temperature and humidity. The parameters are also described for obtaining coatings by free immersion-extraction of fissures and pores on metallic substrates (stainless steel AISI 304). The behavior with corrosion of the coated samples was characterized with electrochemical tests (CW)

  16. Synthesis, Consolidation and Characterization of Sol-gel Derived Tantalum-Tungsten Oxide Thermite Composites

    Energy Technology Data Exchange (ETDEWEB)

    Cervantes, O [Univ. of California, Davis, CA (United States)

    2010-06-01

    Energetic composite powders consisting of sol-gel (SG) 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 SG derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The SG derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta - WO3) energetic composite was consolidated to a density of 9.17 g·cm-3 or 93% relative density. In addition, those samples were consolidated without significant pre-reaction of the constituents, thus retaining their stored chemical energy.

  17. A needle extraction utilizing a molecularly imprinted-sol-gel xerogel for on-line microextraction of the lung cancer biomarker bilirubin from plasma and urine samples.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Jabbar, Dunia; Colmsjö, Anders; Abdel-Rehim, Mohamed

    2014-10-31

    In the present work, a needle trap utilizing a molecularly imprinted sol-gel xerogel was prepared for the on-line microextraction of bilirubin from plasma and urine samples. Each prepared needle could be used for approximately one hundred extractions before it was discarded. Imprinted and non-imprinted sol-gel xerogel were applied for the extraction of bilirubin from plasma and urine samples. The produced molecularly imprinted sol-gel xerogel polymer showed high binding capacity and fast adsorption/desorption kinetics for bilirubin in plasma and urine samples. The adsorption capacity of molecularly imprinted sol-gel xerogel polymer was approximately 60% higher than that of non-imprinted polymer. The effect of the conditioning, washing and elution solvents, pH, extraction time, adsorption capacity and imprinting factor were investigated. The limit of detection and the lower limit of quantification were set to 1.6 and 5nmolL(-1), respectively using plasma or urine samples. The standard calibration curves were obtained within the concentration range of 5-1000nmolL(-1) in both plasma and urine samples. The coefficients of determination values (R(2)) were ≥0.998 for all runs. The extraction recovery was approximately 80% for BR in the human plasma and urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Low Concentration Fe-Doped Alumina Catalysts Using Sol-Gel and Impregnation Methods: The Synthesis, Characterization and Catalytic Performance during the Combustion of Trichloroethylene

    Directory of Open Access Journals (Sweden)

    Carolina Solis Maldonado

    2014-03-01

    Full Text Available The role of iron in two modes of integration into alumina catalysts was studied at 0.39 wt% Fe and tested in trichloroethylene combustion. One modified alumina was synthesized using the sol-gel method with Fe added in situ during hydrolysis; another modification was performed using calcined alumina, prepared using the sol-gel method and impregnated with Fe. Several characterization techniques were used to study the level of Fe modification in the γ-Al2O3 phase formed and to correlate the catalytic properties during trichloroethylene (TCE combustion. The introduction of Fe in situ during the sol-gel process influenced the crystallite size, and three iron species were generated, namely, magnetite, maghemite and hematite. The impregnated Fe-alumina formed hematite and maghemite, which were highly dispersed on the γ-Al2O3 surface. The X-ray photoelectron spectra (XPS, FT-IR and Mössbauer spectroscopy analyses revealed how Fe interacted with the γ-Al2O3 lattice in both catalysts. The impregnated Fe-catalyst showed the best catalytic performance compared to the catalyst that was Fe-doped in situ by the sol-gel method; both had better catalytic activity than pure alumina. This difference in activity was correlated with the accessibility of the reactants to the hematite iron species on the surface. The chlorine poisoning for all three catalysts was less than 1.8%.

  19. Low Concentration Fe-Doped Alumina Catalysts Using Sol-Gel and Impregnation Methods: The Synthesis, Characterization and Catalytic Performance during the Combustion of Trichloroethylene.

    Science.gov (United States)

    Maldonado, Carolina Solis; De la Rosa, Javier Rivera; Lucio-Ortiz, Carlos J; Hernández-Ramírez, Aracely; Barraza, Felipe F Castillón; Valente, Jaime S

    2014-03-12

    The role of iron in two modes of integration into alumina catalysts was studied at 0.39 wt% Fe and tested in trichloroethylene combustion. One modified alumina was synthesized using the sol-gel method with Fe added in situ during hydrolysis; another modification was performed using calcined alumina, prepared using the sol-gel method and impregnated with Fe. Several characterization techniques were used to study the level of Fe modification in the γ-Al₂O₃ phase formed and to correlate the catalytic properties during trichloroethylene (TCE) combustion. The introduction of Fe in situ during the sol-gel process influenced the crystallite size, and three iron species were generated, namely, magnetite, maghemite and hematite. The impregnated Fe-alumina formed hematite and maghemite, which were highly dispersed on the γ-Al₂O 3 surface. The X-ray photoelectron spectra (XPS), FT-IR and Mössbauer spectroscopy analyses revealed how Fe interacted with the γ-Al₂O₃ lattice in both catalysts. The impregnated Fe-catalyst showed the best catalytic performance compared to the catalyst that was Fe-doped in situ by the sol-gel method; both had better catalytic activity than pure alumina. This difference in activity was correlated with the accessibility of the reactants to the hematite iron species on the surface. The chlorine poisoning for all three catalysts was less than 1.8%.

  20. Lithium containing MgAl mixed oxides obtained from sol-gel hydrotalcite for transesterification

    Directory of Open Access Journals (Sweden)

    Renata A. B. Lima-Corrêa

    Full Text Available Abstract The innumerous advantages of heterogeneous catalysts employed in biodiesel production have stimulated the search for a solid catalyst capable of replacing the industrially used homogeneous catalysts. This paper investigates the effect of the sol-gel method in the catalytic activity and stability of Li-MgAl mixed oxides prepared by the “in situ” lithium addition to a MgAl hydrotalcite. The analyses based on N2 physisorption, thermogravimetric analysis, X-ray diffractometry, scanning electron microscopy and temperature-programmed desorption of CO2 were carried out to elucidate the properties of the catalysts. Considerable differences in the physico-chemical properties of the catalysts were observed with the Li addition. Li reduced the surface area and increased the crystallite size of the oxides. Furthermore, Li-MgAl mixed oxides prepared by the calcination of the sol-gel MgAl hydrotalcites presented substantial morphological differences when compared to the same oxides obtained by heat treatment of hydrotalcites synthesized via the conventional co-precipitation route. Furthermore, Li increased the number and strength of the base sites which resulted in the increase of the oxide reactivities towards the transesterification reaction between methyl acetate and ethanol. The activity was dependent on the Li loading on the catalysts. The catalyst containing only 5 wt.% Li turned out to be highly active (( 85% conversion at 50°C, ethanol/methyl acetate molar ratio = 6/1, 4 wt.% of catalyst and 30 min of reaction. Stability tests showed that the Li-MgAl catalysts lose activity after 3 reuse cycles.

  1. Sol-gel synthesis and characterisation of nano-scale hydroxyapatite

    International Nuclear Information System (INIS)

    Bilton, M; Brown, A P; Milne, S J

    2010-01-01

    Hydroxyapatite (HAp) forms the main mineral component of bone and teeth. This naturally occurring HAp is in the form of nano-metre sized crystallites of Ca 10 (PO 4 ) 6 (OH) 2 that contain a number of cation and anion impurities, for example CO 3 2- , F - , Na + , Mg 2+ and Sr 2+ . Synthetic nano-sized HAp particles exhibit favourable biocompatibility and bioactivity and in order to better match the composition to natural HAp there is great interest in producing a range of chemically modified powders. In this study, two HAp powders have been synthesised via a water-based low-temperature sol-gel method and a third, commercial powder from Sigma-Aldrich have been analysed. Subsequent powder calcination has been carried out within the temperature range of 500-700 0 C and the products characterised by bulk chemical analysis, X-ray diffraction and electron microscopy. Energy dispersive X-ray spectroscopy (EDX) in the TEM has been used to assess the composition of individual HAp particles. In order to do this accurately it is first necessary to account for the sensitivity of the HAp structure and composition to irradiation by the high energy electron beam of the TEM. This was done by monitoring the estimated Ca/P ratio derived from TEM-EDX of stoichiometric HAp under increasing levels of electron fluence. A fluence threshold (at a given beam energy) was established below which the measured Ca/P ratio can be considered to be stable. Subsequent elemental analysis at or below this threshold has enabled the variation in composition between particles both within and between synthesis batches to be accurately assessed. Compositional variability between particles is also evident, even in the commercial powder, but is far greater in the powders prepared by the sol-gel method.

  2. Magnetic properties of sol-gel synthesized C-doped ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Dung, Nguyen Duc, E-mail: dung.nguyenduc@hust.edu.vn [Advanced Institute of Science and Technology (AIST), Hanoi University of Science and Technology, No.1 Dai Co Viet, Hanoi (Viet Nam); Son, Cao Thai; Loc, Pham Vu; Cuong, Nguyen Huu; Kien, Pham The; Huy, Pham Thanh [Advanced Institute of Science and Technology (AIST), Hanoi University of Science and Technology, No.1 Dai Co Viet, Hanoi (Viet Nam); Ha, Ngo Ngoc [International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology, No.1 Dai Co Viet, Hanoi (Viet Nam)

    2016-05-25

    ZnO doping with Carbon (C-doped ZnO) materials were prepared by sol-gel technique following with a heat treatment process. Single phase of Wurtzite crystal structure of ZnO was concluded via x-ray diffraction (XRD) with a large amount of excess C tracking by energy dispersive X-ray spectroscopy (EDX) analysis. Two types of ZnO crystals (twinning particles) with different grain sizes and shapes were identified via scanning electron microscopy (FE-SEM). The first type has a smaller grain size of about 20 nm and hexagonal shape. And the second type has a larger grain size of about 80–120 nm and round shape. C substitutions of both Zn and O sites to form C–O and C–Zn bonds were conclusively confirmed via x-ray photoelectron spectroscope (XPS). Experimental evidences for the co-existence of different ferromagnetic phases in the materials are reported and discussed. Two Curie points at high temperatures (>500 °C) are presented. A metamagnetic transition was observed at magnetic field H = 19.2 kOe which was related to the co-existence of ferromagnetic phases. These involve in the formation of twinning C-doped ZnO nanoparticles. - Highlights: • Formation of sol-gel prepared single phase wurtzite ZnO nanoparticles. • Two morphological C-doped ZnO nanoparticles of different grain sizes. • The room temperature ferromagnetism. • An abnormal metamagnetic transition at magnetic field H = 19.2 kOe. • Two different Curie points (T{sub C}) at 500–600 °C.

  3. Sol-Gel Deposition of Iridium Oxide for Biomedical Micro-Devices

    Directory of Open Access Journals (Sweden)

    Cuong M. Nguyen

    2015-02-01

    Full Text Available Flexible iridium oxide (IrOx-based micro-electrodes were fabricated on flexible polyimide substrates using a sol-gel deposition process for utilization as integrated pseudo-reference electrodes for bio-electrochemical sensing applications. The fabrication method yields reliable miniature on-probe IrOx electrodes with long lifetime, high stability and repeatability. Such sensors can be used for long-term measurements. Various dimensions of sol-gel iridium oxide electrodes including 1 mm × 1 mm, 500 µm × 500 µm, and 100 µm × 100 µm were fabricated. Sensor longevity and pH dependence were investigated by immersing the electrodes in hydrochloric acid, fetal bovine serum (FBS, and sodium hydroxide solutions for 30 days. Less pH dependent responses, compared to IrOx electrodes fabricated by electrochemical deposition processes, were measured at 58.8 ± 0.4 mV/pH, 53.8 ± 1.3 mV/pH and 48 ± 0.6 mV/pH, respectively. The on-probe IrOx pseudo-reference electrodes were utilized for dopamine sensing. The baseline responses of the sensors were higher than the one using an external Ag/AgCl reference electrode. Using IrOx reference electrodes integrated on the same probe with working electrodes eliminated the use of cytotoxic Ag/AgCl reference electrode without loss in sensitivity. This enables employing such sensors in long-term recording of concentrations of neurotransmitters in central nervous systems of animals and humans.

  4. Sol-Gel Deposition of Iridium Oxide for Biomedical Micro-Devices

    Science.gov (United States)

    Nguyen, Cuong M.; Rao, Smitha; Yang, Xuesong; Dubey, Souvik; Mays, Jeffrey; Cao, Hung; Chiao, Jung-Chih

    2015-01-01

    Flexible iridium oxide (IrOx)-based micro-electrodes were fabricated on flexible polyimide substrates using a sol-gel deposition process for utilization as integrated pseudo-reference electrodes for bio-electrochemical sensing applications. The fabrication method yields reliable miniature on-probe IrOx electrodes with long lifetime, high stability and repeatability. Such sensors can be used for long-term measurements. Various dimensions of sol-gel iridium oxide electrodes including 1 mm × 1 mm, 500 μm × 500 μm, and 100 μm × 100 μm were fabricated. Sensor longevity and pH dependence were investigated by immersing the electrodes in hydrochloric acid, fetal bovine serum (FBS), and sodium hydroxide solutions for 30 days. Less pH dependent responses, compared to IrOx electrodes fabricated by electrochemical deposition processes, were measured at 58.8 ± 0.4 mV/pH, 53.8 ± 1.3 mV/pH and 48 ± 0.6 mV/pH, respectively. The on-probe IrOx pseudo-reference electrodes were utilized for dopamine sensing. The baseline responses of the sensors were higher than the one using an external Ag/AgCl reference electrode. Using IrOx reference electrodes integrated on the same probe with working electrodes eliminated the use of cytotoxic Ag/AgCl reference electrode without loss in sensitivity. This enables employing such sensors in long-term recording of concentrations of neurotransmitters in central nervous systems of animals and humans. PMID:25686309

  5. Electrochemical corrosion behavior of composite MAO/sol-gel coatings on magnesium alloy AZ91D using combined micro-arc oxidation and sol-gel technique

    International Nuclear Information System (INIS)

    Shang Wei; Chen Baizhen; Shi Xichang; Chen Ya; Xiao Xiang

    2009-01-01

    Protective composite coatings were obtained on a magnesium alloy by micro-arc oxidation (MAO) and sol-gel technique. The coatings consisted of a MAO layer and a sol-gel layer. The microstructure and composition of the MAO coating and the composite coatings were analyzed by scanning electron microscopy (SEM) and energy dispersive X-rays (EDX). Potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and total immersion tests were used to evaluate the corrosion behavior of these coatings in a 3.5 wt.% NaCl solution. The results show that the sol-gel layer provides corrosion protection by physically sealing the pores in the MAO coating and acting as a barrier. The composite coatings can suppress the corrosion process by preventing the corrosive ions from transferring or diffusing to the magnesium alloy substrate. This enhances the corrosion resistance of the magnesium alloy AZ91D significantly

  6. Synthesis of uranium and thorium dioxides by Complex Sol-Gel Processes (CSGP). Synthesis of uranium oxides by Complex Sol-Gel Processes (CSGP)

    International Nuclear Information System (INIS)

    Deptula, A.; Brykala, M.; Lada, W.; Olczak, T.; Wawszczak, D.; Chmielewski, A.G.; Modolo, G.; Daniels, H.

    2010-01-01

    In the Institute of Nuclear Chemistry and Technology (INCT), a new method of synthesis of uranium and thorium dioxides by original variant of sol-gel method - Complex Sol-Gel Process (CSGP), has been elaborated. The main modification step is the formation of nitrate-ascorbate sols from components alkalized by aqueous ammonia. Those sols were gelled into: - irregularly agglomerates by evaporation of water; - medium sized microspheres (diameter <150) by IChTJ variant of sol-gel processes by water extraction from drops of emulsion sols in 2-ethylhexanol-1 by this solvent. Uranium dioxide was obtained by a reduction of gels with hydrogen at temperatures >700 deg. C, while thorium dioxide by a simple calcination in the air atmosphere. (authors)

  7. Tertiary-amine-containing thermo- and pH-sensitive hydrophilic ABA triblock copolymers: effect of different tertiary amines on thermally induced sol-gel transitions.

    Science.gov (United States)

    Henn, Daniel M; Wright, Roger A E; Woodcock, Jeremiah W; Hu, Bin; Zhao, Bin

    2014-03-11

    This Article reports on the synthesis of a series of well-defined, tertiary-amine-containing ABA triblock copolymers, composed of a poly(ethylene oxide) (PEO) central block and thermo- and pH-sensitive outer blocks, and the study of the effect of different tertiary amines on thermally induced sol-gel transition temperatures (T(sol-gel)) of their 10 wt % aqueous solutions. The doubly responsive ABA triblock copolymers were prepared from a difunctional PEO macroinitiator by atom transfer radical polymerization of methoxydi(ethylene glycol) methacrylate and ethoxydi(ethylene glycol) methacrylate at a feed molar ratio of 30:70 with ∼5 mol % of either N,N-diethylaminoethyl methacrylate (DEAEMA), N,N-diisopropylaminoethyl methacrylate, or N,N-di(n-butyl)aminoethyl methacrylate. The chain lengths of thermosensitive outer blocks and the molar contents of tertiary amines were very similar for all copolymers. Using rheological measurements, we determined the pH dependences of T(sol-gel) of 10 wt % aqueous solutions of these copolymers in a phosphate buffer. The T(sol-gel) versus pH curves of all polymers exhibited a sigmoidal shape. The T(sol-gel) increased with decreasing pH; the changes were small on both high and low pH sides. At a specific pH, the T(sol-gel) decreased with increasing the hydrophobicity of the tertiary amine, and upon decreasing pH the onset pH value for the T(sol-gel) to begin to increase noticeably was lower for the more hydrophobic tertiary amine-containing copolymer. In addition, we studied the effect of different tertiary amines on the release behavior of FITC-dextran from 10 wt % micellar gels in an acidic medium at 37 and 27 °C. The release profiles for three studied hydrogels at 37 °C were essentially the same, suggesting that the release was dominated by the diffusion of FITC-dextran. At 27 °C, the release was significantly faster for the DEAEMA-containing copolymer, indicating that both diffusion and gel dissolution contributed to the

  8. Synthesis and physicochemical properties of bis(L-asparaginato) zinc(II): A promising new semiorganic crystal with high laser damage threshold for shorter wavelength generation

    Science.gov (United States)

    Subhashini, R.; Arjunan, S.

    2018-05-01

    An exceedingly apparent nonlinear semiorganic optical crystals of bis(L-asparaginato)zinc(II) [BLAZ], was synthesized by a traditional slow evaporation solution growth technique. The cell parameters were estimated from single crystal X-ray diffraction analysis. Spectroscopic study substantiates the presence of functional groups. The UV spectrum shows the sustenance of wide transparency window and several optical constants, such as extinction coefficient (K), refractive index, optical conductivity and electric susceptibility with real and imaginary parts of dielectric constant were calculated using the transmittance data. The fluorescence emission spectrum of the crystal pronounces red emission. The laser induced surface damage threshold of the crystal was measured using Nd:YAG laser. The output intensity of second harmonic generation was estimated using the Kurtz and Perry powder method. The hardness stability was investigated by Vickers microhardness test. The decomposition and thermal stability of the compound were scrutinized by TGA-DSC studies. Dielectric studies were carried out to anatomize the electrical properties of the crystal. SEM analysis reveals the existence of minute crystallites on the growth surface.

  9. Control size of silver nanoparticles in sol-gel glasses

    Science.gov (United States)

    Renteria, Victor M.; Celis, Antonio C.; Garcia-Macedo, Jorge A.

    2000-10-01

    By the sol-gel processing, silver ions in presence of stabilizing function (3-thiocyanatopropyl)triethoxysilane are reduced by heating gels at 180 C for several times in air atmosphere. The spectroscopic Uv-Vis observations, confirm silver nanoparticles presence with peak maximum around 350 nm. The optical properties of the metallic particles are observed at room temperature as function of time, and the absorption spectra practically do not change, which indicated they are trapped and stabilized within the fine porous silica cage. Mie theory calculations, considering the mean free path effect of the conduction electrons, are compatible with experimental spectra, indicating homogeneity in size and form of the metallic nanoparticles. Smithard correlation curve, between half width height (W1/2) of the optical absorption and the particle diameter 2r, predict silver particles size between 4 and 10 nm, during composite heating. Activation energy was measured and compared with previous data on similar systems and the probable reduction process are discussed.

  10. Synthesis of Titania-Silica Materials by Sol-Gel

    Directory of Open Access Journals (Sweden)

    Rubia F. S. Lenza

    2002-10-01

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

  11. Porous olivine composites synthesized by sol-gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Dominko, R.; Bele, M.; Gaberscek, M.; Jamnik, J. [National Institute of Chemistry, P.O. Box 660, SI-1001 Ljubljana (Slovenia); Remskar, M.; Hanzel, D. [Jozef Stefan Institute, Jamova 39, SI-1000 Ljubljana (Slovenia); Goupil, J.M. [ENSICAEN, UMR CNRS 6506, Catalyse and Spectrochimie Lab, F-14050 Caen (France); Pejovnik, S. [Faculty of Chemistry and Chemical Technology, University of Ljubljana, Askerceva 5, SI-1000 Ljubljana (Slovenia)

    2006-02-28

    Porous LiMPO{sub 4}/C composites (where M stands for Fe and/or Mn) with micro-sized particles were synthesised by sol-gel technique. Particles porosity is discussed in terms of qualitative results obtained from SEM micrographs and in terms of quantitative results obtained from N{sub 2} adsorption isotherms. Porous particles could be described as an inverse picture of nanoparticulate arrangement, where the pores serve as channels for lithium supply and the distance between the pores determines the materials kinetics. Tests show that the electrochemical behaviour of porous LiMPO{sub 4}/C composite is comparable with the results from the literature. The best electrochemical results were obtained with a LiFePO{sub 4}/C composite (over 140mAhg{sup -1} at C/2 rate during continuous cycling). The capacity obtained with LiMnPO{sub 4}/C composite is much lower (40mAhg{sup -1} at C/20 rate), although the textural properties are similar to those observed in the LiFePO{sub 4}/C composite. (author)

  12. The chemistry of plutonium in sol-gel processes

    International Nuclear Information System (INIS)

    Lloyd, M.H.; Haire, R.G.

    1978-01-01

    Studies of plutonium chemical behavior conducted in conjunction with plutonia sol-gel process development at ORNL are described. The colloidal solutions produced consist of 'Pu(IV) polymer,' and this is therefore the study of polymeric plutonium behavior. Spectrophotometric, electron diffraction, and electron microscopy studies, in addition to specific studies that were concerned with the colloidal behavior of Pu(IV) polymer, indicate several characteristics of polymer that are not generally recognized. The particle nature of Pu(IV) polymer indicated by electron microscopy, the amorphous-crystalline characteristics of primary polymer particles demonstrated by electron diffraction, and the reversible and irreversible aggregation of the primary particles shown by spectrophotometric techniques present a useful view of the nature of Pu(IV) polymer that has been helpful in solving or understanding various types of processing problems involving plutonium hydrolytic behavior. The colloidal characteristics of Pu(IV) polymer and crystallite growth of primary polymer particles by thermal denitration are also described. (orig.) [de

  13. Sol-gel-cum-hydrothermal synthesis of mesoporous Co-Fe@Al2O3 ...

    Indian Academy of Sciences (India)

    Oxides; sol-gel; adsorption; surface properties; composite materials. 1. Introduction. Industrial dyes ... acid green 25, Congo red, N719), phenolic compounds. (bromophenol blue .... microscopy (TEM) images were obtained using Philips CM.

  14. The role of crosslinkers in epoxy-amine crosslinked silicon sol-gel barrier protection coatings

    International Nuclear Information System (INIS)

    Vreugdenhil, A.J.; Gelling, V.J.; Woods, M.E.; Schmelz, J.R.; Enderson, B.P.

    2008-01-01

    The search for chromate replacements in corrosion prevention materials has identified the use of hybrid sol-gel coatings as one, very promising approach. Appropriately functionalized hybrid sol-gel materials can be crosslinked to enhance their chemical durability and mechanical strength. In this work, we evaluate three crosslinkers used in a tetramethoxysilane-glycidoxypropyltrimethoxysilane binary sol-gel system in order to identify the role of the crosslinkers in corrosion protection. The crosslinkers examined were ethylenediamine, N-aminethylepiperazine, and diethylenetriamine. The sol-gel coatings were examined by contact angle, atomic force microscopy, and electrochemical impedance spectroscopy (EIS). Circuit modeling of the EIS results yielded valuable insights into the significant differences between the durabilities of the variously crosslinked coatings. Crosslinker hydrophobicity was identified as not playing a significant role whereas the number of reactive sites per crosslinker and the resulting morphology of the material may be an important parameter

  15. Waveguide fabrication in UV-photocurable sol-gel materials: Influence of the photoinitiating system

    International Nuclear Information System (INIS)

    Versace, D.L.; Oubaha, M.; Copperwhite, R.; Croutxe-Barghorn, C.; MacCraith, B.D.

    2008-01-01

    In this paper we identify and explain the different chemical interactions involved between a sol-gel matrix and photoinitiators used in the fabrication of optical waveguides. A well-established sol-gel matrix composed of 3-methacryloxypropyltrimethoxysilane, zirconium n-propoxide and methacrylic acid was developed, and two different photoinitiators (Irgacure (registered) 819 and 1800) were added to the host matrix. Optical microscopy was used to characterise the structure of the waveguides as a function of the photoinitiator nature and concentration, and aging of the hybrid sol-gel material. It is clearly demonstrated that the width of the waveguides is strongly influenced by the sol aging. Furthermore, it is shown that degradation of photoinitiators occurs during the sol-gel process. Oxidation of the phosphonyl groups by the zirconium complex accounts for this results

  16. Amoeba-like self-oscillating polymeric fluids with autonomous sol-gel transition.

    Science.gov (United States)

    Onoda, Michika; Ueki, Takeshi; Tamate, Ryota; Shibayama, Mitsuhiro; Yoshida, Ryo

    2017-07-13

    In the field of polymer science, many kinds of polymeric material systems that show a sol-gel transition have been created. However, most systems are unidirectional stimuli-responsive systems that require physical signals such as a change in temperature. Here, we report on the design of a block copolymer solution that undergoes autonomous and periodic sol-gel transition under constant conditions without any on-off switching through external stimuli. The amplitude of this self-oscillation of the viscosity is about 2,000 mPa s. We also demonstrate an intermittent forward motion of a droplet of the polymer solution synchronized with the autonomous sol-gel transition. This polymer solution bears the potential to become the base for a type of slime-like soft robot that can transform its shape kaleidoscopically and move autonomously, which is associated with the living amoeba that moves forward by a repeated sol-gel transition.

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

    Science.gov (United States)

    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.

  18. Environmentally Benign Sol-Gel Surface Treatment for Aluminum Bonding Applications

    National Research Council Canada - National Science Library

    Osborne, Joseph

    1996-01-01

    A surface treatment process for aluminum using sol-gel chemistry has been developed that produces strong adhesive bonds without the rinse water requirements of traditional anodizing or etching processes...

  19. Extraction of Silica from Cassava Periderm using Modified Sol-Gel ...

    African Journals Online (AJOL)

    Akorede

    6School of Chemical and Metallurgical Engineering, Faculty of Engineering and the Built ... glycol as capping agent in modified sol-gel method for ..... Effect of Organic Acid Treatment on the Properties of ... Journal of Analytical and Applied.

  20. Synthesis of yttrium silicate luminescent materials by sol-gel method

    International Nuclear Information System (INIS)

    Arkhipov, D.V.; Vasina, O.Yu.; Popovich, N.V.; Galaktionov, S.S.; Soshchin, N.P.

    1996-01-01

    Several yttrium-silicate composition with Y 2 O 3 content within 44-56% have been synthesized. it is ascertained that employment of sol-gel technique permits preparation of luminescent materials on yttrium silicate basis, which compare favourably with bath-produced specimens. The influence of phase composition of sol-gel phosphors on basic performance indices: intensity and luminescence spectrum, has been analyzed

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Bansal, Narottam P.

    1989-01-01

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

  3. Morphology, structure and optical properties of sol-gel ITO thin films

    Energy Technology Data Exchange (ETDEWEB)

    Stoica, T.F.; Teodorescu, V.S.; Blanchin, M.G.; Stoica, T.A.; Gartner, M.; Losurdo, M.; Zaharescu, M

    2003-08-15

    The alkoxidic route and the spinning deposition were used to prepare monolayer sol-gel indium tin oxide (ITO) films. The morphology and crystalline structure were investigated by cross-section transmission electron microscopy (XTEM) and atomic force microscopy (AFM). The ITO sol-gel mono-layer contains three regions of different porosities. The basic crystalline structure is that of the In{sub 2}O{sub 3} lattice. The optical properties have been studied by optical transmission and spectroscopic ellipsometry.

  4. Novel hybrid sol-gel coatings for corrosion protection of AZ31B magnesium alloy

    International Nuclear Information System (INIS)

    Lamaka, S.V.; Montemor, M.F.; Galio, A.F.; Zheludkevich, M.L.; Trindade, C.; Dick, L.F.; Ferreira, M.G.S.

    2008-01-01

    This work aims to develop and study new anticorrosion films for AZ31B magnesium alloy based on the sol-gel coating approach. Hybrid organic-inorganic sols were synthesized by copolymerization of epoxy-siloxane and titanium or zirconium alkoxides. Tris(trimethylsilyl) phosphate was also used as additive to confer additional corrosion protection to magnesium-based alloy. A sol-gel coating, about 5-μm thick, shows good adhesion to the metal substrate and prevents corrosion attack in 0.005 M NaCl solution for 2 weeks. The sol-gel coating system doped with tris(trimethylsilyl)-phosphate revealed improved corrosion protection of the magnesium alloy due to formation of hydrolytically stable Mg-O-P chemical bonds. The structure and the thickness of the sol-gel film were characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The corrosion behaviour of AZ31B substrates pre-treated with the sol-gel derived hybrid coatings was tested by electrochemical impedance spectroscopy (EIS). The chemical composition of the silylphosphate-containing sol-gel film at different depths was investigated by X-ray photoelectron spectroscopy (XPS) with depth profiling

  5. Controlled release of vancomycin from thin sol-gel films on implant surfaces successfully controls osteomyelitis.

    Science.gov (United States)

    Adams, Christopher S; Antoci, Valentin; Harrison, Gerald; Patal, Payal; Freeman, Terry A; Shapiro, Irving M; Parvizi, Javad; Hickok, Noreen J; Radin, Shula; Ducheyne, Paul

    2009-06-01

    Peri-prosthetic infection remains a serious complication of joint replacement surgery. Herein, we demonstrate that a vancomycin-containing sol-gel film on Ti alloy rods can successfully treat bacterial infections in an animal model. The vancomycin-containing sol-gel films exhibited predictable release kinetics, while significantly inhibiting S. aureus adhesion. When evaluated in a rat osteomyelitis model, microbiological analysis indicated that the vancomycin-containing sol-gel film caused a profound decrease in S. aureus number. Radiologically, while the control side showed extensive bone degradation, including abscesses and an extensive periosteal reaction, rods coated with the vancomycin-containing sol-gel film resulted in minimal signs of infection. MicroCT analysis confirmed the radiological results, while demonstrating that the vancomycin-containing sol-gel film significantly protected dense bone from resorption and minimized remodeling. These results clearly demonstrate that this novel thin sol-gel technology can be used for the targeted delivery of antibiotics for the treatment of periprosthetic as well as other bone infections. Copyright 2008 Orthopaedic Research Society

  6. Sol-gel processes and materials. January 1970-August 1988 (Citations from the US Patent data base). Report for January 1970-August 1988

    International Nuclear Information System (INIS)

    1988-08-01

    This bibliography contains citations of selected patents concerning Sol-Gel processes and Sol-Gel derived materials and products. Selected patents include Sol-Gel compositions, ceramic and refractory materials, fabrication of silica glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, Sol-Gel production of microspheres, Sol-Gel thin films and coatings, photographic materials, and dental materials. (Contains 71 citations fully indexed and including a title list.)

  7. High-power optical coatings for a mega-joule class ICF laser

    International Nuclear Information System (INIS)

    Kozlowski, M.R.; Thomas, I.M.; Campbell, J.H.; Rainer, F.

    1992-11-01

    As a consequence of advancements in Inertial Confinement Fusion research, LLNL is developing plans for a new 1.5 to 2 mega-joule solid-state Nd:glass laser designed to achieve fusion ignition. The new design is possible in part due to advances in optical coatings suitable for high power laser systems. High damage threshold mirrors and polarizers are comprised of electron beam deposited dielectric multilayers. Subthreshold illumination, or laser conditioning, of the multilayer coatings results in an increase in the damage thresholds by factors of 2 to 3 at 1.06μm, thus meeting the fluence requirements of the advanced architecture. For anti-reflective coatings, protective organic coatings for non-linear crystals and phase plates for beam smoothing, sol-gel films provide high damage thresholds coatings at low cost

  8. Applicability of Sol-Gel Derived Adsorbent for the Production of (n,f) 99Mo Generator

    International Nuclear Information System (INIS)

    Lee, Jun-Sig; Lee, Jong-Sup; Park, Ul-Jae; Son, Kwang-Jae; Han, Hyon-Soo; Kim, Myung Sic; Koo, Sung Chan; Chung, Young-Ju

    2007-01-01

    High performance adsorbents as the column material for (n,γ) 99 Mo/ 99 mTc and 188 W/ 188 Re generators have been developed at KAERI. These adsorbents should have enough loading capacities to produce such generators with high activities as the loading isotopes are not carrier-free. In this regard, the adsorbents are synthesized by sol-gel processing in which the ligand density can easily be adjusted and maximized. The marginal capacity of such adsorbents should be higher than 200 mg/g for molybdenum. From the previous works, the sol-gel processing techniques are adequately applied to meet the criteria. Further studies are being undertaken to employ the adsorbents for the production of high capacity (n,f) 99 Mo/ 99 mTc. Domestically, a private company has lined up the production facility of the molybdenum generator in the activity range of 300 ∼ 1,000 mCi/ea. The column elements are composed of manganese oxide doped on silica and alumina at the backup layer. In this column, the manganese oxide is the main reactive layer to retain (n,f) 99 Mo. The sol-gel derived adsorbent, in this study, is employed as the replacement of the manganese oxide doped silica in the column and tested for the loading efficiency of (n,f) 99 Mo, elution of 99 mTc, labeling property of the eluted 99 mTc. The same loading and elution procedures as the commercial production are applied for the tests and quality controls

  9. Low temperature sol-gel process for optical coatings based on magnesium fluoride and titanium dioxide; Niedertemperatur Sol-Gel Verfahren fuer optische Schichtsysteme auf Basis von Magnesiumfluorid und Titandioxid

    Energy Technology Data Exchange (ETDEWEB)

    Krueger, Hannes

    2009-09-24

    This work deals with the development of a low temperature sol-gel spincoating process for thin films with thicknesses in the nanometer range based on metal oxides and metal fluorides. Optical films such as anti-reflective (AR) or high reflective coatings are of much interest and consist of alternating dielectric layers of low and high refractive index materials. Regarding the general procedure for the metal fluorides a novel nonaqueous sol-gel synthesis starting from metal alkoxides and alcohol-dissolved HF was used. The coatings were dried and calcined at 100 C. The morphology of these films was characterised with REM, TEM and AFM. EDX and XPS were used to identify the chemical composition and ellipsometry and UV-vis spectroscopy to determine the optical properties of the films. This new process allows the preparation of homogeneous magnesium fluoride and titanium dioxide layers with low roughness (R{sub a} {<=} 1,9 nm) on silicon and quartz substrates. The magnesium fluoride layers are partially amorphous or microcrystalline with crystallite sizes from 2 nm to 10 nm. The titanium dioxide layers are predominantly amorphous. The thicknesses of the magnesium fluoride and titanium dioxide single layers were adjustable between 25 nm and 500 nm depending on the number of coating steps and on the concentration of the used sols. The magnesium fluoride layers had a refractive index of n{sub 500} = 1,36 and the titanium dioxide layers a refraction index of n{sub 500} = 2,05. For the first time, an alternating metal fluoride and oxide multilayer system was produced with a low temperature sol-gel method (consisting of magnesium fluoride and titanium dioxide). Based on the determined optical constants of the magnesium fluoride and titanium dioxide single layers, AR and HR multilayer systems were calculated and fabricated. The transmission spectra of the designs and the corresponding multilayer were in good agreement. Similar results were obtained with the reflection spectra

  10. COMPARISON OF SOL-GEL SILICATE COATINGS ON Ti SUBSTRATE

    Directory of Open Access Journals (Sweden)

    DIANA HORKAVCOVÁ

    2012-12-01

    Full Text Available The objective of the submitted work was to prepare and to characterize two types of silicate coatings prepared by the sol-gel method using the dip-coating technique on a titanium substrate. Efforts have been made to use mechanical properties of bio-inert titanium and bioactive properties of a silicate layer enriched with an admixture of compounds identified below. The first group consisted of silicate coatings containing silver, brushite and monetite. The other group of silicate coatings contained calcium nitrate and triethyl phosphate. Mechanically and chemically treated titanium substrates were dipped into sols and dried and fired. Silicate coatings from the first group were also chemically treated in 10 mol.l-1 solution of sodium hydroxide. All coatings were measured to determine their adhesive and bioactive properties and furthermore the antibacterial properties were tested in the case of first group. Surfaces of the coated substrates were investigated after the firing and after the individual tests with optical and electron microscopy and X-ray microdiffraction. A tape test demonstrated excellent adhesive property of all coatings to the substrate, classified with degree 5. A static in vitro test demonstrated bioactivity of nearly all the coatings. The basic silicate coating from the first group and one type of coating from the second group were identified as inert. Antibacterial properties of silicate coatings containing silver showed to be different when tested against Escherichia coli bacteria. A complete inhibition of the growth of bacteria under our experimental conditions was observed for the coating containing silver and monetite and a partial inhibition of the growth of bacteria for coatings containing silver and silver in combination with brushite.

  11. Lithium ceramics: sol-gel preparation and tritium release

    International Nuclear Information System (INIS)

    Renoult, O.

    1994-04-01

    Ceramics based on lithium aluminate (LiA1O 2 ), lithium zirconate (Li 2 ZrO 3 ) and lithium titanate (Li 2 TiO 3 ) are candidates as tritium breeder blanket materials for forthcoming nuclear fusion reactors. Lithium silico-aluminate Li 4+x A1 4-3x Si 2x O 8 (0 ≤ x ≤ 0,25) powders were synthetized from alkoxyde-hydroxyde sol-gel route. By direct sintering at 850-1100 deg C (without prior calcination), ceramics with controlled stoichiometry and homogenous microstructure were obtained. We have also prepared, using a comparable method, Li 2 Zr 1-x Ti x O 3 (x = 0, x = 0,1 et x = 1) materials. All these ceramics, with different microstructures and compositions, have been tested in out-of-reactor experiments. Concerning lithium aluminate microporous ceramics, the silicon substitution leads to a significant improvement of the tritrium release. Classical models taking into account independent surface mechanisms are not able to describe correctly the observed tritium release kinetics. We show, using a simple model, that the release kinetics is in fact limited by an intergranular diffusion followed by a desorption. The delay in tritium release, which occurs when the ceramic compacity increases, is explained in terms of an enhancement of the ionic T + diffusion path length. The energy required for desorption includes a leading term independent of hydrogen contained in the sweep gas. This term is attributed to the limiting recombination step of T + in molecular species HTO. For similar microstructures, the facility of tritium release for the different studied materials is explained by three properties: the crystal structure of the ceramic, the acidity of oxides and finally the presence of electronic non-stoichiometric defects. (author). 89 refs., 50 figs., 2 tabs., 1 annexe

  12. Progress of studies on preparation of TiO2 photocatalysts with sol-gel auto igniting synthesis

    Science.gov (United States)

    Wu, Di; Shi, Zaifeng; Zhang, Xiaopeng; Xinghui, Wu

    2017-11-01

    In this article, influencing factors on the kinetics of the process of Sol-gel Auto igniting Synthesis (SAS) which is an advanced technology for preparing nanometer particles of inorganic materials were reviewed. The studies on preparing of nanometer TiO2 photocatalysts with SAS were focused. It was concluded that SAS will play an important role in practical preparing of high-pure nanometer TiO2 powder, and as a technical support, preparation of titania TiO2 from titanic iron ore with SAS is feasible and practicable.

  13. Nitrate ions as cathodic alkalization promoters for the electro-assisted deposition of sol-gel thin films

    Energy Technology Data Exchange (ETDEWEB)

    Ding Shangzhi; Liu Liang [Department of Chemistry, Yuquan Campus, Zhejiang University, Hangzhou, Zhejiang 310027 (China); Hu Jiming [Department of Chemistry, Yuquan Campus, Zhejiang University, Hangzhou, Zhejiang 310027 (China)], E-mail: kejmhu@zju.edu.cn; Zhang Jianqing; Cao Chunan [Department of Chemistry, Yuquan Campus, Zhejiang University, Hangzhou, Zhejiang 310027 (China); State Key Laboratory for Corrosion and Protection, Shenyang 110016 (China)

    2008-08-15

    Nitrate was used as a promoter to prepare dodecyltrimethoxysilane thin films on aluminum substrates. With the addition of nitrate into silane sol-gel precursors, the electro-assisted formation of silane films was facilitated, as indicated by electrochemical impedance spectroscopy, scanning electron microscopy and secondary-ion mass spectroscopy, due to the promotion in cathodic alkalization. However, an extra-high concentration of nitrate would be harmful because of the salting-out effect in precursors and the soluble nitrate remaining in silane films.

  14. Li3PO4 surface coating on Ni-rich LiNi0.6Co0.2Mn0.2O2 by a citric acid assisted sol-gel method: Improved thermal stability and high-voltage performance

    Science.gov (United States)

    Lee, Suk-Woo; Kim, Myeong-Seong; Jeong, Jun Hui; Kim, Dong-Hyun; Chung, Kyung Yoon; Roh, Kwang Chul; Kim, Kwang-Bum

    2017-08-01

    A surface coating of Li3PO4 was applied to a Ni-rich LiNi0.6Co0.2Mn0.2O2 (NCM) material to improve its thermal stability and electrochemical properties via a citric acid assisted sol-gel method. The addition of citric acid effectively suppressed the instant formation of Li3PO4 in solution, resulting in successful coating of the NCM surface. The improved thermal stability of NCM after Li3PO4 surface coating was demonstrated by differential scanning calorimetry (DSC) analysis and in situ time-resolved X-ray diffraction (TR-XRD). In particular, the TR-XRD results showed that the improved thermal stability after Li3PO4 surface coating originates from suppression of the phase transition of charged NCM at high temperatures. Furthermore, the charge-discharge tests demonstrated that Li3PO4-coated LiNi0.6Co0.2Mn0.2O2 (LP-NCM) has excellent electrochemical properties. LP-NCM exhibited a specific capacity of 192.7 mAh g-1, a capacity retention of 44.1% at 10 C, and a capacity retention of 79.7% after 100 cycles at a high cut-off voltage of 4.7 V; these values represent remarkably improved electrochemical properties compared with those of bare NCM. These improved thermal and electrochemical properties were mainly attributed to the improvement of the structural stability of the material and the suppression of the interface reaction between the cathode and the electrolyte owing to the Li3PO4 coating.

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

    Science.gov (United States)

    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.

  16. Lithium ceramics: sol-gel preparation and tritium release; Ceramiques lithiees: elaboration sol-gel et relachement du tritium

    Energy Technology Data Exchange (ETDEWEB)

    Renoult, O

    1994-04-01

    Ceramics based on lithium aluminate (LiA1O{sub 2}), lithium zirconate (Li{sub 2}ZrO{sub 3}) and lithium titanate (Li{sub 2}TiO{sub 3}) are candidates as tritium breeder blanket materials for forthcoming nuclear fusion reactors. Lithium silico-aluminate Li{sub 4+x}A1{sub 4-3x}Si{sub 2x}O{sub 8} (0 {<=} x {<=} 0,25) powders were synthetized from alkoxyde-hydroxyde sol-gel route. By direct sintering at 850-1100 deg C (without prior calcination), ceramics with controlled stoichiometry and homogenous microstructure were obtained. We have also prepared, using a comparable method, Li{sub 2}Zr{sub 1-x}Ti{sub x}O{sub 3} (x = 0, x = 0,1 et x = 1) materials. All these ceramics, with different microstructures and compositions, have been tested in out-of-reactor experiments. Concerning lithium aluminate microporous ceramics, the silicon substitution leads to a significant improvement of the tritrium release. Classical models taking into account independent surface mechanisms are not able to describe correctly the observed tritium release kinetics. We show, using a simple model, that the release kinetics is in fact limited by an intergranular diffusion followed by a desorption. The delay in tritium release, which occurs when the ceramic compacity increases, is explained in terms of an enhancement of the ionic T{sup +} diffusion path length. The energy required for desorption includes a leading term independent of hydrogen contained in the sweep gas. This term is attributed to the limiting recombination step of T{sup +} in molecular species HTO. For similar microstructures, the facility of tritium release for the different studied materials is explained by three properties: the crystal structure of the ceramic, the acidity of oxides and finally the presence of electronic non-stoichiometric defects. (author). 89 refs., 50 figs., 2 tabs., 1 annexe.

  17. Database of average-power damage thresholds at 1064 nm

    International Nuclear Information System (INIS)

    Rainer, F.; Hildum, E.A.; Milam, D.

    1987-01-01

    We have completed a database of average-power, laser-induced, damage thresholds at 1064 nm on a variety of materials. Measurements were made with a newly constructed laser to provide design input for moderate and high average-power laser projects. The measurements were conducted with 16-ns pulses at pulse-repetition frequencies ranging from 6 to 120 Hz. Samples were typically irradiated for time ranging from a fraction of a second up to 5 minutes (36,000 shots). We tested seven categories of samples which included antireflective coatings, high reflectors, polarizers, single and multiple layers of the same material, bare and overcoated metal surfaces, bare polished surfaces, and bulk materials. The measured damage threshold ranged from 2 for some metals to > 46 J/cm 2 for a bare polished glass substrate. 4 refs., 7 figs., 1 tab

  18. Sol-Gel Process for Making Pt-Ru Fuel-Cell Catalysts

    Science.gov (United States)

    Narayanan, Sekharipuram; Valdez, Thomas; Kumta, Prashant; Kim, Y.

    2005-01-01

    A sol-gel process has been developed as a superior alternative to a prior process for making platinum-ruthenium alloy catalysts for electro-oxidation of methanol in fuel cells. The starting materials in the prior process are chloride salts of platinum and ruthenium. The process involves multiple steps, is time-consuming, and yields a Pt-Ru product that has relatively low specific surface area and contains some chloride residue. Low specific surface area translates to incomplete utilization of the catalytic activity that might otherwise be available, while chloride residue further reduces catalytic activity ("poisons" the catalyst). In contrast, the sol-gel process involves fewer steps and less time, does not leave chloride residue, and yields a product of greater specific area and, hence, greater catalytic activity. In this sol-gel process (see figure), the starting materials are platinum(II) acetylacetonate [Pt(C5H7O2)2, also denoted Pt-acac] and ruthenium(III) acetylacetonate [Ru(C5H7O2)3, also denoted Ru-acac]. First, Pt-acac and Ru-acac are dissolved in acetone at the desired concentrations (typically, 0.00338 moles of each salt per 100 mL of acetone) at a temperature of 50 C. A solution of 25 percent tetramethylammonium hydroxide [(CH3)4NOH, also denoted TMAH] in methanol is added to the Pt-acac/Ruacac/ acetone solution to act as a high-molecular-weight hydrolyzing agent. The addition of the TMAH counteracts the undesired tendency of Pt-acac and Ru-acac to precipitate as separate phases during the subsequent evaporation of the solvent, thereby helping to yield a desired homogeneous amorphous gel. The solution is stirred for 10 minutes, then the solvent is evaporated until the solution becomes viscous, eventually transforming into a gel. The viscous gel is dried in air at a temperature of 170 C for about 10 hours. The dried gel is crushed to make a powder that is the immediate precursor of the final catalytic product. The precursor powder is converted to the

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

    Science.gov (United States)

    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.

  20. Magnetic resonance as a structural probe of a uranium (VI) sol-gel process

    International Nuclear Information System (INIS)

    King, C.M.; Thompson, M.C.; Buchanan, B.R.; King, R.B.; Garber, A.R.

    1989-01-01

    NMR investigations on the ORNL process for sol-gel synthesis of microspherical nuclear fuel (UO 2 ), has been useful in sorting out the chemical mechanism in the sol-gel steps. 13 C, 15 N, and 1 H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C 6 H l2 N 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. 17 0 NMR of uranyl (UO 2 ++ ) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, [(UO 2 ) 3 (μ 3 -O)(μ 2 -OH) 3 ] + , 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 + 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 4 ) 2 [(UO 2 ) 8 O 4 (OH) 10 ] · 8H 2 0. This compound is the precursor to sintered U0 2 ceramic fuel

  1. Salt-assisted and salt-suppressed sol-gel transitions of methylcellulose in water.

    Science.gov (United States)

    Xu, Y; Wang, C; Tam, K C; Li, L

    2004-02-03

    The effects of various salts on the sol-gel transition of aqueous methylcellulose (MC) solutions have been studied systematically by means of a micro differential scanning calorimeter. It was found that the heating process was endothermic while the cooling process was exothermic for both MC solutions with and without salts. The addition of salts did not change the patterns of gelation and degelation of MC. However, the salts could shift the sol-gel transition and the gel-sol transition to lower or higher temperatures from a pure MC solution, depending on the salt type. These opposite effects were termed the salt-assisted and salt-suppressed sol-gel transitions. Either the salt-assisted transition or the salt-suppressed sol-gel transition was a function of salt concentration. In addition, each salt was found to have its own concentration limit for producing a stable aqueous solution of MC at a given concentration of MC, which was related to the anionic charge density of the salt. Cations were proved to have weaker effects than anions. The "salt-out strength", defined as the salt effect per mole of anion, was obtained for each anion studied. The thermodynamic mechanisms involved in the salt-assisted and salt-suppressed sol-gel transitions are discussed.

  2. Optical sensing of HCl with phenol red doped sol-gels

    International Nuclear Information System (INIS)

    Wang Enju; Chow, Kwok-Fan; Wang Wenqun; Wong, Crystal; Yee, Cynthia; Persad, Alvin; Mann, Jonathan; Bocarsly, Andrew

    2005-01-01

    A dye doped sol-gel for the sensing of hydrochloric acid in solution and/or gaseous phase is described. The sol-gel is obtained by acidic hydrolysis of tetraethoxysilane (TEOS) and phenyltriethoxysilane (Ph-TriEOS) in the presence of phenol red (PR) and further spin-coating onto glass slides. The sensitive response is based on an increase of the absorption band at 510 nm of phenol red entrapped in the sol-gel casting when exposed to HCl solution or gas, due to protonation of the dye. The detection limit of the sol-gel response to moisturized gaseous HCl is below 12 ppm, and its response to HCl in solution falls in the range of 0.01-6 M. The sol-gel coating has a response time of less than 40 s in steady-state, and life-time of more than a year. Weak acids such as acetic acid, benzoic acid, salicylate acid, citrate acid, and carbonic acid do not interfere the response. The responses in acid solutions are completely reversible. In the gaseous phase, response of HCl appears to be moisture sensitive

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

    Science.gov (United States)

    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.

  4. Spectroscopic and electrochemical characterization of cytochrome c encapsulated in a bio sol-gel matrix.

    Science.gov (United States)

    Deriu, Daniela; Pagnotta, Sara Emanuela; Santucci, Roberto; Rosato, Nicola

    2008-08-01

    Sol-gel technique represents a remarkably versatile method for protein encapsulation. To enhance sol-gel biocompatibility, systems envisaging the presence of calcium and phosphates in the sol-gel composition were recently prepared and investigated. Unfortunately, the low pH at which solutions were prepared (pH proteins, because the acidic environment induces protein denaturation. In this paper we apply a new protocol based on the introduction of calcium nitrate to the inorganic phase, with formation of a binary bioactive system. In this case protein encapsulation results versatile and secure, being achieved at a pH close to neutrality (pH 6.0); also, the presence of calcium is expected to enhance system biocompatibility. To determine the properties of the salt-doped sol-gel and the influence exerted on entrapped biosystems, the structural and functional properties of embedded cytochrome c have been investigated. Data obtained indicate that the salt-doped sol-gel induces no significant change in the structure and the redox properties of the embedded protein; also, the matrix increases protein stability. Interestingly, the presence of calcium nitrate appears determinant for refolding of the acid-denatured protein. This is of interest in the perspective of future applications in biosensoristic area.

  5. Optical sensing of HCl with phenol red doped sol-gels

    Energy Technology Data Exchange (ETDEWEB)

    Wang Enju [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States)]. E-mail: wange@stjohns.edu; Chow, Kwok-Fan [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Wang Wenqun [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Wong, Crystal [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Yee, Cynthia [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Persad, Alvin [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Mann, Jonathan [Department of Chemistry, Princeton University, Princeton, NJ 08540 (United States); Bocarsly, Andrew [Department of Chemistry, Princeton University, Princeton, NJ 08540 (United States)

    2005-04-08

    A dye doped sol-gel for the sensing of hydrochloric acid in solution and/or gaseous phase is described. The sol-gel is obtained by acidic hydrolysis of tetraethoxysilane (TEOS) and phenyltriethoxysilane (Ph-TriEOS) in the presence of phenol red (PR) and further spin-coating onto glass slides. The sensitive response is based on an increase of the absorption band at 510 nm of phenol red entrapped in the sol-gel casting when exposed to HCl solution or gas, due to protonation of the dye. The detection limit of the sol-gel response to moisturized gaseous HCl is below 12 ppm, and its response to HCl in solution falls in the range of 0.01-6 M. The sol-gel coating has a response time of less than 40 s in steady-state, and life-time of more than a year. Weak acids such as acetic acid, benzoic acid, salicylate acid, citrate acid, and carbonic acid do not interfere the response. The responses in acid solutions are completely reversible. In the gaseous phase, response of HCl appears to be moisture sensitive.

  6. Submicrometric gratings fabrication from photosensitive organo-silica-hafnia thin films elaborated by sol-gel processing

    Energy Technology Data Exchange (ETDEWEB)

    Franc, Janyce [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Barnier, Vincent, E-mail: barnier@emse.fr [Ecole Nationale Superieure des Mines, SMS-EMSE, CNRS:UMR 5146, LCG, F-42023 Saint-Etienne (France); Vocanson, Francis, E-mail: francis.vocanson@univ-st-etienne.fr [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Gamet, Emilie; Lesage, Maryline [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Jamon, Damien [Universite de Lyon, F-42023 Saint-Etienne (France); Laboratoire Claude Chappe, Telecom Saint-Etienne, 42000 Saint-Etienne Cedex 2 (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Jourlin, Yves [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France)

    2012-07-31

    The aim of this study is the elaboration of a high index sol-gel material in order to prepare submicrometric grating. The gratings were obtained after few seconds of UV exposure in one step using an organically modified silica-hafnia matrix. The chemical composition of thin films after UV and annealing treatments were studied using Fourier Transform Infrared Spectroscopy and X-Ray Photoelectron Spectroscopy. The study of optical properties revealed that the annealed films are transparent from 200 to 1000 nm and have a refractive index from 1.550 to 1.701 depending on the hafnium concentration. - Highlights: Black-Right-Pointing-Pointer Silica-hafnia matrix with high refractive index was prepared using sol-gel process. Black-Right-Pointing-Pointer Organic and inorganic networks formation of thin films was investigated. Black-Right-Pointing-Pointer Optical properties are influenced by annealing treatment and initial hafnium amount. Black-Right-Pointing-Pointer The use of high Si:Hf molar ratio can lead to a loss transmittance below 300 nm. Black-Right-Pointing-Pointer Submicrometric grating period can be prepared using a holographic method.

  7. 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.

    Science.gov (United States)

    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-C 12 ) and phenethyl (PhE) ligands. Here, the ability of the PF-C 12 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-C 12 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

  8. Sol-gel synthesis of Bi3.25La0.75Ti3O12 nanotubes

    International Nuclear Information System (INIS)

    Wang Wen; Ke Hua; Rao Jiancun; Feng Jinbiao; Feng Ming; Jia Dechang; Zhou Yu

    2011-01-01

    Research highlights: → One-dimensional (1D) ferroelectrics have been successfully synthesized. The sol-gel template synthesis is a versatile and inexpensive technique for producing nanostructures, and particularly facilitates the fabrication of complex oxide nanotubes or nanowires. Compared with the synthesis of the general nanotubes such as carbon nanotubes with simple crystal structure, the synthesis of ferroelectric compound is difficult due to the multielement and the complex crystal structures of these ferroelectrics. Herein, we report the synthesis of one-dimensional BLT nanotubes on anodic alumina (AAO) templates by immersing a template membrane in sol without polymeric additive. - Abstract: Ferroelectric Bi 3.25 La 0.75 Ti 3 O 12 (BLT) nanotubes were synthesized by sol-gel technique using nanochannel porous anodic aluminum oxide (AAO) templates, and were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). BLT nanotubes with diameter of around 240 nm and the wall thickness of about 25 nm exhibited a single orthorhombic perovskite structure and highly preferential crystal growth along the [1 1 7] orientation, which have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. The formation mechanism of BLT nanotubes was discussed.

  9. Electrical stability of Al-doped ZnO transparent electrode prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Tabassum, Samia, E-mail: shawon14@gmail.com; Yamasue, Eiji; Okumura, Hideyuki; Ishihara, Keiichi N.

    2016-07-30

    Highlights: • Al-doped ZnO thin film was deposited by sol-gel method in different annealing temperature and duration. • We examined the environmental stability in ambient and damp heat condition. • We investigated chemical state of thin film. • Better stability was observed in the film annealed at high temperature (600 °C) along with longer duration (120 min). • An ultrathin aluminum oxide layer formation was predicted by XPS measurement which protects further oxidation and improves stability. - Abstract: Al-doped zinc oxide (AZO) thin films have been considered as a promising alternative to tin doped indium oxide (ITO), which is currently used in various optoelectronic applications. However, the environmental stability of AZO film is not satisfactory, in that the resistivity is significantly increases in air. Here, we investigate the resistivity stability of AZO thin films prepared by sol-gel method using various annealing temperatures and durations. The degradation of resistivity property was observed for AZO films stored in ambient or damp heat environment, where the degradation rate was influenced by annealing temperature. A significant improvement of electrical stability was attained in AZO films that were prepared at high annealing temperature. The films, which showed the highest and the lowest increasing rate of resistivity, were further characterized in detail to shed light on the possible mechanisms explaining the improved stability through crystallinity, surface morphology and elemental state of the thin film.

  10. Electrical stability of Al-doped ZnO transparent electrode prepared by sol-gel method

    International Nuclear Information System (INIS)

    Tabassum, Samia; Yamasue, Eiji; Okumura, Hideyuki; Ishihara, Keiichi N.

    2016-01-01

    Highlights: • Al-doped ZnO thin film was deposited by sol-gel method in different annealing temperature and duration. • We examined the environmental stability in ambient and damp heat condition. • We investigated chemical state of thin film. • Better stability was observed in the film annealed at high temperature (600 °C) along with longer duration (120 min). • An ultrathin aluminum oxide layer formation was predicted by XPS measurement which protects further oxidation and improves stability. - Abstract: Al-doped zinc oxide (AZO) thin films have been considered as a promising alternative to tin doped indium oxide (ITO), which is currently used in various optoelectronic applications. However, the environmental stability of AZO film is not satisfactory, in that the resistivity is significantly increases in air. Here, we investigate the resistivity stability of AZO thin films prepared by sol-gel method using various annealing temperatures and durations. The degradation of resistivity property was observed for AZO films stored in ambient or damp heat environment, where the degradation rate was influenced by annealing temperature. A significant improvement of electrical stability was attained in AZO films that were prepared at high annealing temperature. The films, which showed the highest and the lowest increasing rate of resistivity, were further characterized in detail to shed light on the possible mechanisms explaining the improved stability through crystallinity, surface morphology and elemental state of the thin film.

  11. Investigation of the visible light photocatalytic activity of BiVO4 prepared by sol gel method assisted by ultrasonication.

    Science.gov (United States)

    Deebasree, J P; Maheskumar, V; Vidhya, B

    2018-07-01

    Visible light induced photocatalyst BiVO 4 with monoclinic scheelite structure has been synthesised via sol gel method assisted by ultrasonication. The prepared samples were characterised using X-ray diffraction (XRD), scanning electron microscope (SEM), UV-Vis diffused reflectance spectroscopy (DRS) techniques. The photocatalytic efficiency was evaluated by decolourisation of MB under visible light irradiation. The effect of ultrasound output power on the properties of BiVO 4 during and after preparation by sol-gel method has been compared with normal agitated sample (As prepared). The power of ultrasonic vibration has been varied and an ideal output power which yields better catalytic efficiency is determined. BiVO 4 sonicated with 80 W during preparation 80 W (D) exhibited relatively high surface area, better surface morphology and better catalytic efficiency compared to other samples which were sonicated with 100, 160 and 200 W. The results signify that the photodegradation rate of BiVO 4 80 W (D) sample is high up to 96% in 90 min compared to other samples. Change in morphology leading to better catalytic efficiency was obtained just by exposing the sample to ultrasonic radiation without addition of any surfactant. The recovery test showed that the sample was stable for four consecutive cycles. Using radical test, a reasonable mechanism for photodegradation has been proposed. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Quantum dot based on tin/titanium mixed oxide doped with europium synthesized by protein sol-gel method

    International Nuclear Information System (INIS)

    Paganini, Paula P.; Felinto, Maria Claudia F.C.; Brito, Hermi F.

    2011-01-01

    Special luminescence biomarkers have been developed to find more sensitive fluoroimmunoassay methods. A new generation of these biomarkers is the semiconductors nanocrystals, known as quantum dots, doped with lanthanides. The use of lanthanides ions as luminescent markers has many advantages, for example a security method, low cost, high specificity and also the luminescence can be promptly measured with high sensibility and accuracy. The protein sol-gel is a modification of conventional method, in which the coconut water replacing the alkoxides normally used. The advantage is that, the proteins present in coconut water bind chemically with metal salts forming a polymer chain. This work presents nanoparticles based on tin/titanium mixed oxide doped with 3% of europium synthesized by protein sol-gel method. The nanoparticles were burned at 300 deg C, 500 deg C, 800 deg C and 1100 deg C. The samples were analyzed and characterized by thermal analysis, X-ray powder diffraction (XRD), infrared spectroscopy (IR) and scanning electron microscopy (SEM). The synthesis was effective and the nanoparticles showed nanometric size and structural differences with the annealing. To be used in the fluoroimmunoassays tests, these particles need to be functionalized before be connect with biological molecules and after this process, these nanoparticles going to be submitted at gamma radiation for sterilization. (author)

  13. Quantum dot based on tin/titanium mixed oxide doped with europium synthesized by protein sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Paganini, Paula P.; Felinto, Maria Claudia F.C., E-mail: paulapaganini@usp.b, E-mail: mfelinto@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Brito, Hermi F., E-mail: hefbrito@iq.usp.b [Universidade de Sao Paulo (IQ/USP), Sao Paulo, SP (Brazil). Inst. de Quimica. Lab. de Elementos do Bloco f

    2011-07-01

    Special luminescence biomarkers have been developed to find more sensitive fluoroimmunoassay methods. A new generation of these biomarkers is the semiconductors nanocrystals, known as quantum dots, doped with lanthanides. The use of lanthanides ions as luminescent markers has many advantages, for example a security method, low cost, high specificity and also the luminescence can be promptly measured with high sensibility and accuracy. The protein sol-gel is a modification of conventional method, in which the coconut water replacing the alkoxides normally used. The advantage is that, the proteins present in coconut water bind chemically with metal salts forming a polymer chain. This work presents nanoparticles based on tin/titanium mixed oxide doped with 3% of europium synthesized by protein sol-gel method. The nanoparticles were burned at 300 deg C, 500 deg C, 800 deg C and 1100 deg C. The samples were analyzed and characterized by thermal analysis, X-ray powder diffraction (XRD), infrared spectroscopy (IR) and scanning electron microscopy (SEM). The synthesis was effective and the nanoparticles showed nanometric size and structural differences with the annealing. To be used in the fluoroimmunoassays tests, these particles need to be functionalized before be connect with biological molecules and after this process, these nanoparticles going to be submitted at gamma radiation for sterilization. (author)

  14. Bulk and thick films of the superconducting phase YBa2Cu3O7/sub -//sub y/ made by controlled precipitation and sol-gel processes

    International Nuclear Information System (INIS)

    Barboux, P.; Tarascon, J.M.; Greene, L.H.; Hull, G.W.; Bagley, B.G.

    1988-01-01

    The synthesis of high-temperature superconducting oxides using solution chemistry has been investigated and physical properties are compared to ceramics obtained by conventional solid-state reactions. We report on controlled precipitation and sol-gel processes, both of which produce materials with particle sizes smaller than 5 μm. We find that the superconducting properties of the high T/sub c/ ceramics are affected by their manner of preparation, such that the transitions are slightly lower in temperature, but sharper, for samples made by solution rather than solid-state chemistry. The ability to prepare stable viscous gels provides an opportunity for obtaining large areas of superconducting coatings. For thick films on alumina or silicon substrates, contamination from the substrate is shown to be a problem. Finally, we observe that the sol-gel process lowers the synthesis temperature by 100 0 C.ing,

  15. Preparation and characterization of bismuth ruthenate pyrochlore via solid state reaction and sol-gel methods

    Directory of Open Access Journals (Sweden)

    Mayuree Sansernnivet

    2010-01-01

    Full Text Available Bismuth ruthenate pyrochlores, potential cathode materials for intermediate temperature solid oxide fuel cells(ITSOFCs, were prepared via solid-state and sol-gel method. Effects of the preparation routes and conditions on the phase and microstructures of the materials were investigated in this study using XRD and SEM. The study showed that the preparation method and the adding sequence of the starting meterials have a significant effect on the crystal phase and the particle size obtained. Sol-gel synthesis could yield a material with only pyrochlore structure, i.e. Bi2Ru2O7, while the solid state method yielded powder with a small amount of the secondary RuO2 phase. The sol-gel synthesis resulted in materialswith a finer particle size (~0.3-1.0 μm compared to powder synthesized via the solid state reaction method.

  16. Nanostructured Mesoporous Titanium Dioxide Thin Film Prepared by Sol-Gel Method for Dye-Sensitized Solar Cell

    Directory of Open Access Journals (Sweden)

    Yu-Chang Liu

    2011-01-01

    Full Text Available Titanium dioxide (TiO2 paste was prepared by sol-gel and hydrothermal method with various precursors. Nanostructured mesoporous TiO2 thin-film back electrode was fabricated from the nanoparticle colloidal paste, and its performance was compared with that made of commercial P25 TiO2. The best performance was demonstrated by the DSSC having a 16 μm-thick TTIP-TiO2 back electrode, which gave a solar energy conversion efficiency of 6.03%. The ability of stong adhesion on ITO conducting glass substrate and the high surface area are considered important characteristics of TiO2 thin film. The results show that a thin film with good adhesion can be made from the prepared colloidal paste as a result of alleviating the possibility of electron transfer loss. One can control the colloidal particle size from sol-gel method. Therefore, by optimizing the preparation conditions, TiO2 paste with nanoparticle and narrow diameter distribution was obtained.

  17. Evaluation of the photocatalytic ability of a sol-gel-derived MgO-ZrO2 oxide material

    Directory of Open Access Journals (Sweden)

    Ciesielczyk Filip

    2017-02-01

    Full Text Available This paper deals with the synthesis and characterization of a novel group of potential photocatalysts, based on sol-gel-derived MgO-ZrO2 oxide material. The material was synthesized in a typical sol-gel system using organic precursors of magnesia and zirconia, ammonia as a promoter of hydrolysis and methanol as a solvent. All materials were thoroughly analyzed, including morphology and particle sizes, chemical composition, identification of characteristic functional groups, porous structure parameters and crystalline structure. The proposed methodology of synthesis resulted in obtaining pure MgO-ZrO2 oxide material with micrometric-sized particles and a relatively high surface area. The samples underwent an additional calcination process which led to the crystalline phase of zirconia being formed. The key element of the study was the evaluation of the effectiveness of decomposition of C.I. Basic Blue 9 dye. It was shown that the calcined materials exhibit both satisfactory adsorption and photocatalytic activity with respect to the decomposition of a selected model organic impurity. Total dye removal varied in the range of 50-70%, and was strongly dependent on process parameters such as quantity of photocatalyst, time of irradiation, and the addition of promoters.

  18. Fabrication of silica ceramic membrane via sol-gel dip-coating method at different nitric acid amount

    Science.gov (United States)

    Kahlib, N. A. Z.; Daud, F. D. M.; Mel, M.; Hairin, A. L. N.; Azhar, A. Z. A.; Hassan, N. A.

    2018-01-01

    Fabrication of silica ceramics via the sol-gel method has offered more advantages over other methods in the fabrication of ceramic membrane, such as simple operation, high purity homogeneous, well defined-structure and complex shapes of end products. This work presents the fabrication of silica ceramic membrane via sol-gel dip-coating methods by varying nitric acid amount. The nitric acid plays an important role as catalyst in fabrication reaction which involved hydrolysis and condensation process. The tubular ceramic support, used as the substrate, was dipped into the sol of Tetrethylorthosilicate (TEOS), distilled water and ethanol with the addition of nitric acid. The fabricated silica membrane was then characterized by (Field Emission Scanning Electron Microscope) FESEM and (Fourier transform infrared spectroscopy) FTIR to determine structural and chemical properties at different amount of acids. From the XRD analysis, the fabricated silica ceramic membrane showed the existence of silicate hydrate in the final product. FESEM images indicated that the silica ceramic membrane has been deposited on the tubular ceramic support as a substrate and penetrate into the pore walls. The intensity peak of FTIR decreased with increasing of amount of acids. Hence, the 8 ml of acid has demonstrated the appropriate amount of catalyst in fabricating good physical and chemical characteristic of silica ceramic membrane.

  19. Fabrication of high quality Cu2SnS3 thin film solar cell with 1.12% power conversion efficiency obtain by low cost environment friendly sol-gel technique

    Science.gov (United States)

    Chaudhari, J. J.; Joshi, U. S.

    2018-03-01

    Cu2SnS3 (CTS) is an emerging ternery chalcogenide material with great potential application in thin film solar cells. We present here high quality Cu2SnS3 thin films using a facile spin coating method. The as deposited films of CTS were sulphurized in a graphite box using tubular furnace at 520 °C for 60 min at the rate of 2.83 °C min-1 in argon atmosphere. X-ray diffraction (XRD) and Raman spectroscopy studies confirm tetragonal phase and absence of any secondary phase in sulphurized CTS thin films. X-ray photoelectron spectroscopy (XPS) demonstrates that Cu and Sn are in +1 and +4 oxidation state respectively. Surface morphology of CTS films were analyzed by field emission scanning electron microscope and atomic force microscope (AFM), which revealed a smooth surface with roughness (RMS) of 6.32 nm for sulphurized CTS film. Hall measurements confirmed p-type conductivity with hole concentartion of sulphurized CTS thin film is of 6.5348 × 1020 cm-3. UV-vis spectra revealed a direct energy band gap varies from 1.45 eV to 1.01 eV for as-deposited and sulphurized CTS thin film respectively. Such band gap values are optimum for semiconductor material as an absorber layer of thin film solar cell. The CTS thin film solar cell had following structure: SLG/FTO/ZnO/CTS/Al with short circuit current density of (Jsc) of 11.6 mA cm-2, open circuit voltage (Voc) of 0.276 V, active area of 0.16 cm2, fill factor (FF) of 35% and power conversion efficiency of 1.12% under AM 1.5 (100 mW cm-2) illumination in simulated standard test conditions.

  20. Sol-gel technology applied to crystalline ceramic nuclear waste forms

    International Nuclear Information System (INIS)

    Angelini, P.; Bond, W.D.; Caputo, A.J.; Mack, J.E.; Lackey, W.J.; Lee, D.A.; Stinton, D.P.

    1980-01-01

    The sol-gel process is being developed for the solidification and isolation of high-level nuclear fuel waste. Three gelation methods are being developed for producing alternative waste forms. These include internal gelation for producing spheres of up to 1 mm diam suitable for coating, external gelation, and water extraction methods for producing material suitable for alternate ceramic processing. In this study internal gelation has been used to produce ceramic spheres of various alternative nuclear waste compositions. A gelation system capable of producing 100-g batches has been assembled and used for development. Waste forms containing up to 70 wt % simulated Savannah River Plant waste have been produced. Dopants such as Cs, Sr, Nd, Ru, and Mo were used in some experiments to observe side waste streams and sintering effects. Synroc microspheres were coated with both low-density carbon, high-density impermeable carbon, high-temperature dense SiC, and SiC deposited at temperatures near 900 0 C. Other gelation methods and other alternative waste forms are being developed

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

    Science.gov (United States)

    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. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    1992-01-01

    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

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

    National Research Council Canada - National Science Library

    Schmidt, Helmut

    1998-01-01

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

  4. Influence of New Sol-gel Refractory Coating on the Casting Properties of Cold Box and Furan Cores for Grey Cast iron

    DEFF Research Database (Denmark)

    Nwaogu, Ugochukwu Chibuzoh; Poulsen, T.; Bischoff, C

    2010-01-01

    New Sol-Gel coated sand cores made from coldbox and furan binder systems were investigated. The idea of the coating was to improve the surface quality of castings. Grey iron was cast on the cores in a sand casting process. The effect of the high temperature of the melt on the cores was assessed...... by measuring the heating curves. The viscosity of the coating, moisture content and the permeability of the cores were evaluated. The surface quality of the castings was investigated using SEM and OM. The results show that the moisture content of the cores affected the permeability. In furan cores the vapour...... transport zone (VTZ) when in contact with the melt is larger than it is in a coldbox which means the furan cores have higher moisture content. The new sol-gel coating has the potential for improving the surface quality of castings without negative effects on the graphite distribution. The surface...

  5. Encapsulation of Polymer Colloids in a Sol-Gel Matrix. Direct-Writing of Coassembling Organic-Inorganic Hybrid Photonic Crystals.

    Science.gov (United States)

    Mikosch, Annabel; Kuehne, Alexander J C

    2016-03-22

    The spontaneous self-assembly of polymer colloids into ordered arrangements provides a facile strategy for the creation of photonic crystals. However, these structures often suffer from defects and insufficient cohesion, which result in flaking and delamination from the substrate. A coassembly process has been developed for convective assembly, resulting in large-area encapsulated colloidal crystals. However, to generate patterns or discrete deposits in designated places, convective assembly is not suitable. Here we experimentally develop conditions for direct-writing of coassembling monodisperse dye-doped polystyrene particles with a sol-gel precursor to form solid encapsulated photonic crystals. In a simple procedure the colloids are formulated in a sol-gel precursor solution, drop-cast on a flat substrate, and dried. We here establish the optimal parameters to form reproducible highly ordered photonic crystals with good optical performance. The obtained photonic crystals interact with light in the visible spectrum with a narrow optical stop-gap.

  6. Sol-gel synthesis of lanthanum-gallate-based ceramic coatings

    International Nuclear Information System (INIS)

    Golubko, N.V.; Kaleva, G.M.; Roginskaya, Yu.E.; Politova, E.D.

    2007-01-01

    Phase-pure (La 0.9 Sr 0.1 )(Ga 0.7 Fe 0.3 )O 3-y and (Sr 1.8 La 0.2 )(GaFe)O 5.1 solid solutions with the perovskite and brownmillerite structures have been prepared from salt solutions by sol-gel processing at temperatures from 570 to 870 K. Ceramic coatings up to 100 μm in thickness have been produced by applying suspensions of the sol-gel powders to various substrates. The structure and microstructure of the ceramic coatings have been studied by X-ray diffraction and scanning electron microscopy [ru

  7. Fundamental electrochemiluminescence characteristics of fluorine-doped tin oxides synthesized by sol-gel combustion.

    Science.gov (United States)

    Moon, B H; Chaoumead, A; Sung, Y M

    2013-10-01

    Fluorine-doped tin oxide (FTO) materials synthesized by sol-gel combustion method were investigated for electrochemical luminescence (ECL) application. Effects of sol-gel combustion conditions on the structures and morphology of the porous FTO (p-FTO) materials were studied. ECL efficiency of p-FTO-based cell was about 251 cd/m2 at 4 V bias, which is higher than the sell using only FTO electrodes (102.8 cd/m2). The highest intensity of the emitting light was obtained at the wavelength of about 610 nm. The porous FTO layer was effective for increasing ECL intensities.

  8. Application of sol-gel process on the elaboration of SnO2 based ceramics

    International Nuclear Information System (INIS)

    Prescatan, R.T.; Silva, D.V. da; Hiratsuka, R.S.; Santilli, C.V.; Pulcinelli, S.H.

    1990-01-01

    The electrical, optical and chemical peculiar properties of SnO 2 confers it-self some potential application. The densification difficulty during sintering of SnO 2 compromises its elaboration by ceramic conventional process. In this work the preparation of SnO 2 ceramics by sol-gel process was investigated. Some parameters envolved on the colloidal stability, sol-gel transition and drying process were analysed. The obtained materials were characterized by rheological, X-ray diffraction, infra-red spectroscopy and pores size distribution measurements. The results show that a considerable densification during sintering at 400 and 600 0 C was obtained. (author) [pt

  9. Micro- and nanostructured sol-gel-based materials for optical chemical sensing (2005–2015)

    International Nuclear Information System (INIS)

    Barczak, Mariusz; McDonagh, Colette; Wencel, Dorota

    2016-01-01

    This review (with 172 references) highlights the progress made in the past 10 years in silica sol-gel-based materials for use in optical chemical sensing. Following an introduction, the processes leading to the sol-gel-based and ormosil materials, their printability and methods for characterisation are discussed. Then various classes of optical sensors, with a focus on sensors for pH values, oxygen, carbon dioxide, ammonia (also in dissolved form), and heavy metal ions are described. A further section covers nanoparticle-based optical sensors mainly for use in intracellular sensing of the above species. Recent developments in this area are also emphasised and future trends discussed. (author)

  10. Deposition of sol-gel sensor spots by nanoimprint lithography and hemi-wicking

    DEFF Research Database (Denmark)

    Mikkelsen, Morten Bo Lindholm; Marie, Rodolphe; Hansen, Jan H.

    2011-01-01

    We present a method for homogeneous deposition of sol-gel sensor materials, which enable fabrication of sensor spots for optical pH and oxygen measurements inside plastic containers. A periodic pattern of posts is imprinted into a polycarbonate substrate and, using the principle of hemi-wicking, ......We present a method for homogeneous deposition of sol-gel sensor materials, which enable fabrication of sensor spots for optical pH and oxygen measurements inside plastic containers. A periodic pattern of posts is imprinted into a polycarbonate substrate and, using the principle of hemi...

  11. Positron annihilation lifetime studies of sol-gel transition of carrageenan gels

    International Nuclear Information System (INIS)

    Wakabayashi, Y.; Ito, K.; Li, H.L.; Ujihara, Y.

    1996-01-01

    Positron annihilation lifetime measurement was applied to study the sol-gel transition of anionic polysaccharide aqueous solutions in terms of free-volume parameters the size, intensity, and size distribution of free volumes of the gelation of K-form κ-carrageenan solutions as a function of temperature. Slight variations of free volume size and intensity against temperature were observed near 295 K. The correlation of free-volume data with other physical properties vibrational spectra (IR and Raman), conductivity, SAXS, elastic measurement, differential scanning calorimetry were investigated to understand the mechanism of sol-gel transition of carrageenan. (author)

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

    Science.gov (United States)

    Stiegman, Albert E.

    1995-01-01

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

  13. Site selective generation of sol-gel deposits in layered bimetallic macroporous electrode architectures.

    Science.gov (United States)

    Lalo, Hélène; Bon-Saint-Côme, Yémima; Plano, Bernard; Etienne, Mathieu; Walcarius, Alain; Kuhn, Alexander

    2012-02-07

    The elaboration of an original composite bimetallic macroporous electrode containing a site-selective sol-gel deposit is reported. Regular colloidal crystals, obtained by a modified Langmuir-Blodgett approach, are used as templates for the electrogeneration of the desired metals in the form of a well-defined layered bimetallic porous electrode. This porous matrix shows a spatially modulated electroactivity which is subsequently used as a strategy for targeted electrogeneration of a sol-gel deposit, exclusively in one predefined part of the porous electrode.

  14. Comparative microstructure and electrical property studies of lead scandium tantalate thin films as prepared by LDCVD, sol-gel and sputtering techniques

    International Nuclear Information System (INIS)

    Huang, Z; Donohue, P P; Zhang, Q; Williams, D J; Anthony, C J; Whatmore, R W; Todd, M A

    2003-01-01

    Lead scandium tantalate (PST) thin films for uncooled infrared (IR) detector applications have been deposited by liquid delivery chemical vapour deposition (LDCVD), sputtering and sol-gel techniques. The sol-gel and sputtered films were deposited at low temperature into a non-ferroelectric phase with the required perovskite structure being formed using a high temperature rapid thermal anneal (RTA). In contrast to this, the LDCVD films were deposited at high temperature directly into the perovskite phase but were found to still require a high temperature RTA step to optimize their merit for IR detection. Detailed structural and electrical characterization of the PST films deposited by these different methods have revealed that there is no simple relationship between microstructure and electrical properties. The sol-gel and LDCVD techniques produce thin films with excellent microstructures, as determined by x-ray diffraction analysis and transmission electron microscopy, but inferior electrical properties and relatively low merit figures. By contrast, the sputtered and then rapid thermal annealed films have inferior microstructures, characterized by extensive voiding, but excellent electrical properties and high merit figures

  15. Crystallization of sol-gel derived lead zirconate titanate thin films in argon and oxygen atmospheres

    International Nuclear Information System (INIS)

    Bursill, L.A.

    1994-01-01

    Electron diffraction and high-resolution electron microscopic techniques are applied to reveal the mechanisms of crystallization of 75 nm thin films of ferroelectric lead-zirconate-titanate (PZT). Sol-gel methods, followed by pyrolysis at 350 deg C, were used to provide a common starting point after which a variety of rapid-thermal annealing (RTA) experiments in the temperature range 400-700 deg C were made in argon, oxygen and nitrogen/hydrogen atmospheres. The results are interpreted in terms of the crystal chemical analysis, which points out that partial pressure of oxygen and heating rate are important experimental parameters which must be controlled if ferroelectric perovskite-type Pb 2 ZrTiO 6 , rather than pyrochlore-type Pb 2 ZrTiO 6+x , where O < X < 1 or -1 < X < O, is to be obtained after the RTA step. Thus significant improvements in the crystallization of perovskite-type PZT were clearly demonstrated by using argon atmospheres for the RTA step. The results have significance for the production of high-quality ferroelectric thin films, with improved switching and fatigue characteristics, since even small amounts of the pyrochlore phase prove detrimental for these properties. 18 refs., 1 tab., 10 figs

  16. Crystallization of sol-gel derived lead zirconate titanate thin films in argon and oxygen atmospheres

    Energy Technology Data Exchange (ETDEWEB)

    Bursill, L A [Melbourne Univ., Parkville, VIC (Australia). School of Physics; Brooks, K G [Ecole Polytechnique Federale, Lausanne (Switzerland)

    1994-12-31

    Electron diffraction and high-resolution electron microscopic techniques are applied to reveal the mechanisms of crystallization of 75 nm thin films of ferroelectric lead-zirconate-titanate (PZT). Sol-gel methods, followed by pyrolysis at 350 deg C, were used to provide a common starting point after which a variety of rapid-thermal annealing (RTA) experiments in the temperature range 400-700 deg C were made in argon, oxygen and nitrogen/hydrogen atmospheres. The results are interpreted in terms of the crystal chemical analysis, which points out that partial pressure of oxygen and heating rate are important experimental parameters which must be controlled if ferroelectric perovskite-type Pb{sub 2}ZrTiO{sub 6}, rather than pyrochlore-type Pb{sub 2}ZrTiO{sub 6+x}, where O < X < 1 or -1 < X < O, is to be obtained after the RTA step. Thus significant improvements in the crystallization of perovskite-type PZT were clearly demonstrated by using argon atmospheres for the RTA step. The results have significance for the production of high-quality ferroelectric thin films, with improved switching and fatigue characteristics, since even small amounts of the pyrochlore phase prove detrimental for these properties. 18 refs., 1 tab., 10 figs.

  17. Zinc oxide films impurified with Ti and prepared by the Sol-gel method

    International Nuclear Information System (INIS)

    Tirado G, S.; Cazares R, J.M.; Maldonado, A.

    2006-01-01

    Titanium-doped zinc oxide thin films have been prepared on silicon substrate using the Sol-Gel technique. The structural, morphology, electrical and optical properties of such thin films were studied as a function of titanium concentration (0.5, 1 and 1.5 %) and the thin films thickness. Zinc acetate dihydrate and titanium (VI)-oxy acetylacetonate were used as precursor materials, using 2-methoxyethanol and monoethanolamine as via. The X-ray diffraction spectra show polycrystalline films in all the cases. It can see for all the thin films a preferential growth along the (002) planes where the titanium concentration and also the thin films thickness play an important rule. No structural changes are observed at all. The surface morphology studied shows as the grain size decreases when thin thickness is increases. For titanium concentration of 0.5, 1 and 1.5 % values the grains size increase also. The thin films thickness for titanium concentration of 1.5 % was 500 nm (4v), 400 nm (3v), 180 nm (2v) and 130 nm (1v), values obtained from cross-section micrographs. Highly resistive samples are obtained for substrate soda-lime even showing high transmittance. Better physical properties are required for gas sensors or semitransparent electrodes and other possible applications. (Author)

  18. In situ observation of sol-gel transition of agarose aqueous solution by fluorescence measurement.

    Science.gov (United States)

    Wang, Zheng; Yang, Kun; Li, Haining; Yuan, Chaosheng; Zhu, Xiang; Huang, Haijun; Wang, Yongqiang; Su, Lei; Fang, Yapeng

    2018-06-01

    Sol-gel transition behavior of agarose aqueous solution was investigated by using rheology and fluorescence measurement. On heating, the storage modulus G' decreased gradually, then deviated abruptly at the temperature of about 65°C, and finally decreased slowly again. For fluorescence measurement, the phase transition point kept almost at the temperature of 65°C, which was consistent with that in rheology measurement. Upon compression, it was indicated that the fluorescence lifetime for the probe in the agarose aqueous solution showed a dramatic change in the vicinity of the phase transition point. T vs. P phase diagram of agarose aqueous solution was constructed, which showed that the melting point was an increasing function of pressure. Based on the phase diagram, the agarose gels were prepared by cooling under atmospheric pressure and the pressure of 300MPa, respectively. From the result of the recovered samples studied by optical rheometry, it was found that agarose gel prepared under high pressure had a higher elasticity and lower viscosity index, compared with that under atmospheric pressure. It could be speculated that such kinds of properties might be attributed to the smaller pore size during gelation under high pressure. Copyright © 2018. Published by Elsevier B.V.

  19. Spray drying of silica microparticles for sustained release application with a new sol-gel precursor.

    Science.gov (United States)

    Wang, Bifeng; Friess, Wolfgang

    2017-10-30

    A new precursor, tetrakis(2-methoxyethyl) orthosilicate (TMEOS) was used to fabricate microparticles for sustained release application, specifically for biopharmaceuticals, by spray drying. The advantages of TMEOS over the currently applied precursors are its water solubility and hydrolysis at moderate pH without the need of organic solvents or catalyzers. Thus a detrimental effect on biomolecular drug is avoided. By generating spray-dried silica particles encapsulating the high molecular weight model compound FITC-dextran 150 via the nano spray dryer Büchi-90, we demonstrated how formulation parameters affect and enable control of drug release properties. The implemented strategies to regulate release included incorporating different quantities of dextrans with varying molecular weight as well as adjusting the pH of the precursor solution to modify the internal microstructures. The addition of dextran significantly altered the released amount, while the release became faster with increasing dextran molecular weight. A sustained release over 35days could be achieved with addition of 60 kD dextran. The rate of FITC-Dextran 150 release from the dextran 60 containing particles decreased with higher precursor solution pH. In conclusion, the new precursor TMEOS presents a promising alternative sol-gel technology based carrier material for sustained release application of high molecular weight biopharmaceutical drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Wafer scale lead zirconate titanate film preparation by sol-gel method using stress balance layer

    International Nuclear Information System (INIS)

    Lu Jian; Kobayashi, Takeshi; Yi Zhang; Maeda, Ryutaro; Mihara, Takashi

    2006-01-01

    In this paper, platinum/titanium (Pt/Ti) film was introduced as a residual stress balance layer into wafer scale thick lead zirconate titanate (PZT) film fabrication by sol-gel method. The stress developing in PZT film's bottom electrode as well as in PZT film itself during deposition were analyzed; the wafer curvatures, PZT crystallizations and PZT electric properties before and after using Pt/Ti stress balance layer were studied and compared. It was found that this layer is effective to balance the residual stress in PZT film's bottom electrode induced by thermal expansion coefficient mismatch and Ti diffusion, thus can notably reduce the curvature of 4-in. wafer from - 40.5 μm to - 12.9 μm after PZT film deposition. This stress balance layer was also found effective to avoid the PZT film cracking even when annealed by rapid thermal annealing with heating-rate up to 10.5 deg. C/s. According to X-ray diffraction analysis and electric properties characterization, crack-free uniform 1-μm-thick PZT film with preferred pervoskite (001) orientation, excellent dielectric constant, as high as 1310, and excellent remanent polarization, as high as 39.8 μC/cm 2 , can be obtained on 4-in. wafer

  1. Microfabrication and Integration of a Sol-Gel PZT Folded Spring Energy Harvester

    Directory of Open Access Journals (Sweden)

    Jonathan Lueke

    2015-05-01

    Full Text Available This paper presents the methodology and challenges experienced in the microfabrication, packaging, and integration of a fixed-fixed folded spring piezoelectric energy harvester. A variety of challenges were overcome in the fabrication of the energy harvesters, such as the diagnosis and rectification of sol-gel PZT film quality and adhesion issues. A packaging and integration methodology was developed to allow for the characterizing the harvesters under a base vibration. The conditioning circuitry developed allowed for a complete energy harvesting system, consisting a harvester, a voltage doubler, a voltage regulator and a NiMH battery. A feasibility study was undertaken with the designed conditioning circuitry to determine the effect of the input parameters on the overall performance of the circuit. It was found that the maximum efficiency does not correlate to the maximum charging current supplied to the battery. The efficiency and charging current must be balanced to achieve a high output and a reasonable output current. The development of the complete energy harvesting system allows for the direct integration of the energy harvesting technology into existing power management schemes for wireless sensing.

  2. Optical Constants of Crystallized TiO2 Coatings Prepared by Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Jun Shen

    2013-07-01

    Full Text Available Titanium oxide coatings have been deposited by the sol-gel dip-coating method. Crystallization of titanium oxide coatings was then achieved through thermal annealing at temperatures above 400 °C. The structural properties and surface morphology of the crystallized coatings were studied by micro-Raman spectroscopy and atomic force microscopy, respectively. Characterization technique, based on least-square fitting to the measured reflectance and transmittance spectra, is used to determine the refractive indices of the crystallized TiO2 coatings. The stability of the synthesized sol was also investigated by dynamic light scattering particle size analyzer. The influence of the thermal annealing on the optical properties was then discussed. The increase in refractive index with high temperature thermal annealing process was observed, obtaining refractive index values from 1.98 to 2.57 at He-Ne laser wavelength of 633 nm. The Raman spectroscopy and atomic force microscopy studies indicate that the index variation is due to the changes in crystalline phase, density, and morphology during thermal annealing.

  3. Afterglow luminescence in sol-gel/Pechini grown oxide materials: persistence or phosphorescence process? (Conference Presentation)

    Science.gov (United States)

    Sontakke, Atul; Ferrier, Alban; Viana, Bruno

    2017-03-01

    Persistent luminescence and phosphorescence, both yields afterglow luminescence, but are completely different mechanisms. Persistent luminescence involves a slow thermal release of trapped electrons stored in defect states, whereas the phosphorescence is caused due to triplet to singlet transition [1,2]. Many persistent luminescence phosphors are based on oxide inorganic hosts, and exhibit long afterglow luminescence after ceasing the excitation. We observed intense and long afterglow luminescence in sol-gel/pechini grown inorganic oxides, and as a first interpretation thought to be due to persistence mechanism. However, some of these materials do not exhibit defect trap centers, and a detailed investigation suggested it is due to phosphorescence, but not the persistence. Phosphorescence is not common in inorganic solids, and that too at room temperature, and therefore usually misinterpreted as persistence luminescence [3]. Here we present a detailed methodology to distinguish phosphorescence from persistence luminescence in inorganic solids, and the process to harvest highly efficient long phosphorescence afterglow at room temperature. 1. Jian Xu, Setsuhisa Tanabe, Atul D. Sontakke, Jumpei Ueda, Appl. Phys. Lett. 107, 081903 (2015) 2. Sebastian Reineke, Marc A. Baldo, Scientific Reports, 4, 3797 (2014) 3. Pengchong Xue, Panpan Wang, Peng Chen, Boqi Yao, Peng Gong, Jiabao Sun, Zhenqi Zhang, Ran Lu, Chem. Sci. (2016) DOI: 10.1039/C5SC03739E

  4. Sol-Gel TiO2 thin films sensitized with the mulberry pigment cyanidin

    Directory of Open Access Journals (Sweden)

    Emerson Henrique de Faria

    2007-12-01

    Full Text Available TiO2 films have various applications, among them solar cells and photodegradation of pollutants. In this study, we investigated TiO2 films functionalized with the organic dye cyanidin extracted from black mulberry (Morus nigra. The TiO2 was functionalized by the sol-gel method and the film was deposited on glass substrates by dip-coating. Our aim was to investigate the interaction between the semiconductor and the dye, as well as the influence of the velocity and number of deposits on the characteristics of the film. Using ultraviolet-visible spectroscopy, we observed a shift from the maximum absorption band at 545 nm for the dye’s ethanol solution to 595 nm for the film, indicating interaction of the cyanidin with the TiO2. The absorption spectra in the infrared region of the functionalized TiO2 particles showed bands characteristic of the oxide and indicated their interaction with the dye. Using profilometry and m-line techniques, we found that the films presented thicknesses in the order of 100 nm. A SEM analysis confirmed the high density of the films.

  5. Low temperature synthesis of hydroxyapatite nano-rods by a modified sol-gel technique

    International Nuclear Information System (INIS)

    Jadalannagari, Sushma; More, Sandeep; Kowshik, Meenal; Ramanan, Sutapa Roy

    2011-01-01

    Hydroxyapatite (HAp) nano-rods were successfully synthesized by a modified sol-gel method using a solution of CaCl 2 .2H 2 O in water, along with a solution of H 3 PO 4 in triethylamine and NH 4 OH as starting materials. The Ca/P molar ratio was maintained at 1.67. The sol obtained was dried in an oven for 2 days at 100 deg. C after being dialyzed for 12 h. Pellets were made from the crystalline powders and immersed in simulated body fluid (SBF) to check its biocompatibility after 15, 45 and 180 days of immersion. The HAp powders and pellets were characterized by X-Ray Diffraction crystallography (XRD), Fourier transform Infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The HAp nano-rods had an average diameter of 25 nm and length 110-120 nm. Immersion of the HAp pellets in SBF led to the formation of a highly porous interconnecting HAp layer on the surface. The porosity increased with increase in immersion time. Highlights: → Low temperature synthesis of hydroxyapatite nanorods using Ca and P sources and triethylamine. → The synthesis time was only 0.5 hours. → Crystalline material was obtained after drying at 100oC only in air. → SBF studies showed the HAP bodies to be biocompatible.

  6. Sol-gel synthesis of lithium metatitanate as tritium breeding material under different sintering conditions

    Science.gov (United States)

    Lu, Wei; Wang, Jing; Pu, Wenjing; Li, Kaiping; Ma, Shubing; Wang, Weihua

    2018-04-01

    Lithium metatitanate (Li2TiO3) is a promising tritium breeding material candidate for solid blanket of D-T fusion reactors, due to its high mechanical strength, chemical stability, and tritium release rate. In this paper, Li2TiO3 powder with homogeneous crystal structure is synthesized by sol-gel method. The chemical reactions in gel thermal cracking and sintering process are studied by thermo gravimetric/differential scanning calorimetry (TG-DSC). The relationship between the sintering condition and the particle/grain size is characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Results show that below 673 K the gel precursor is completely decomposed and Li2TiO3 phase initially forms. The LiTiO2 by-product formed under the reductive atmosphere in muffle furnace, could be oxidized continually to Li2TiO3 at higher sintering temperature (≥1273 K) for longer sintering time (≥10 h). Both grain and particle sizes rely on a linear growth with the increase of sintering time at 1273 K. Over 1473 K, significant agglomerations exist among particles. The optimal sintering condition is selected as 1273 K for 10 h, for the purer Li2TiO3 phase (>99%), smaller grain and particle size.

  7. Luminescence from Ce in sol-gel SiO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Kroon, R.E., E-mail: KroonRE@ufs.ac.za [Department of Physics, University of the Free State, IB51, Box 339, Bloemfontein 9300 (South Africa); Seed Ahmed, H.A.A.; Ntwaeaborwa, O.M. [Department of Physics, University of the Free State, IB51, Box 339, Bloemfontein 9300 (South Africa); Koao, L.F. [Department of Physics, University of the Free State (Qwaqwa Campus), Private Bag X13, Phuthaditjhaba 9866 (South Africa); Nagpure, I.M.; Gusowski, M.A. [Department of Physics, University of the Free State, IB51, Box 339, Bloemfontein 9300 (South Africa); Botha, J.R. [Department of Physics, Nelson Mandela Metropolitan University, Box 77000, Port Elizabeth 6031 (South Africa); Swart, H.C. [Department of Physics, University of the Free State, IB51, Box 339, Bloemfontein 9300 (South Africa)

    2012-05-15

    The sol-gel process provides an attractive low temperature alternative to the melt process for producing Ce-doped silica, but reports of the emission wavelength have not been consistent. In this paper, luminescence measurements using a variety of excitation methods, including cathodoluminescence not yet reported by other researchers, are compared and evaluated in the light of previously published data. Several papers report luminescence around 350 nm but emission near this wavelength was not found from our samples. This luminescence originates from Ce that has not yet been incorporated in the silica and is found in samples that have not undergone high temperature annealing. Our photoluminescence results from samples annealed in a reducing atmosphere suggest that emission from Ce incorporated in the silica lattice occurs near 455 nm, and some indication of the emission from Ce in amorphous clusters at 400 nm is also found. However, our results also confirm earlier indications that intrinsic defects in silica can create photoluminescence near both these wavelengths, which can make identification of the luminescence due to Ce difficult. Finally, it has been found that samples which have been annealed in air, and therefore display poor photoluminescence because most of the Ce occurs in the tetravalent form, are luminescent under electron beam excitation. It is suggested that during cathodoluminescence measurements Ce{sup 4+} ions capture electrons to form excited Ce{sup 3+} ions from which the luminescence originates.

  8. Synthesis and characterization of CdO nano particles by the sol-gel method

    Science.gov (United States)

    Vadgama, V. S.; Vyas, R. P.; Jogiya, B. V.; Joshi, M. J.

    2017-05-01

    Cadmium Oxide (CdO) is an inorganic compound and one of the main precursors to other cadmium compounds. It finds applications in cadmium plating, storage batteries, in transparent conducting film, etc. Here, an attempt is made to synthesize CdO nano particles by sol-gel technique. The gel was prepared using cadmium nitrate tetra hydrate (Cd(NO3)2.4H2O) and aqueous ammonium hydroxide (NH4OH) as a precursor. The synthesized powder is further characterized by techniques like Powder X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Thermal gravimetric analysis (TGA). Powder XRD analysis suggested the nano-crystalline nature of the sample with the cubic crystal system. Nano scaled particles of spherical morphology with the size ranging from 50-100 nm are observed from TEM images. While, FT-IR study is used to confirm the presence of different functional groups. Thermo-gravimetric analysis suggests the highly thermally stable nature of the samples. The results are discussed.

  9. Partial Oxidation of n-Butane over a Sol-Gel Prepared Vanadium Phosphorous Oxide

    Directory of Open Access Journals (Sweden)

    Juan M. Salazar

    2013-01-01

    Full Text Available Vanadium phosphorous oxide (VPO is traditionally manufactured from solid vanadium oxides by synthesizing VOHPO4∙0.5H2O (the precursor followed by in situ activation to produce (VO2P2O7 (the active phase. This paper discusses an alternative synthesis method based on sol-gel techniques. Vanadium (V triisopropoxide oxide was reacted with ortho-phosphoric acid in an aprotic solvent. The products were dried at high pressure in an autoclave with a controlled excess of solvent. This procedure produced a gel of VOPO4 with interlayer entrapped molecules. The surface area of the obtained materials was between 50 and 120 m2/g. Alcohol produced by the alkoxide hydrolysis reduced the vanadium during the drying step, thus VOPO4 was converted to the precursor. This procedure yielded non-agglomerated platelets, which were dehydrated and evaluated in a butane-air mixture. Catalysts were significantly more selective than the traditionally prepared materials with similar intrinsic activity. It is suggested that the small crystallite size obtained increased their selectivity towards maleic anhydride.

  10. Porous MnO2 prepared by sol-gel method for electrochemical supercapacitor

    Science.gov (United States)

    Bazzi, K.; Kumar, A.; Jayakumar, O. D.; Nazri, G. A.; Naik, V. M.; Naik, R.

    2015-03-01

    MnO2 has attracted great attention as material for electrochemical pseudocapacitor due to its high theoretical specific faradic capacitance (~ 1370 F .g-1) , environmental friendliness and wide potential window in both aqueous and nonaqueous electrolytes. However, the MnO2 has a low surface area which depresses its electrochemical performance. The amorphous α-MnO2 composite was synthesized by sol gel method in the presence of the tri-block copolymer P123. Our aim is to investigate the role of P123 on the electrochemical performance of MnO2. The samples with and without P123 were prepared and characterized by x-ray diffraction (XRD), SEM, TEM and Brunauer-Emmett-Teller (BET) method. The electrochemical performances of the amorphous MnO2 composites as the electrode materials for supercapacitors were evaluated by cyclic voltammetry and AC impedance measurements in a 1M Na2SO4 solution. The results show that the sample prepared without P123 exhibited a relatively low specific capacitance of 28F .g-1, whereas the porous MnO2 prepared with P123 exhibited 117 F .g-1at 5 mV/s. The results of crystalline MnO2 composites will also be presented. The authors acknowledge the support from the Richard J. Barber Foundation for Interdisciplinary Research.

  11. Enhanced fatigue characteristics of sol-gel derived PZT thin films

    International Nuclear Information System (INIS)

    Shim, Donghyun; Pak, Jaemoon; Nam, Kuangwoo; Park, Gwangweo

    2008-01-01

    Pb(Zr,Ti)O 3 (PZT) thin films with Zr/Ti ratio of 52:48 were deposited on Pt/Ti/SiO 2 /Si substrates using the sol-gel method. Since the conditions of heat-treatment play a great role in film growth, post-annealing processes were conducted under different environments. After standard processing, films were annealed at 600 deg. C in three different atmosphere-air, O 2 and a two-step process conducted in air for 30 min and then in O 2 ambient, all done for 10 min. Through electron microscopy and X-ray diffraction, we found that all films were crack-free and highly (1 1 1) oriented. Hysteresis measurements showed a generally large polarization value. The fatigue properties differ drastically for all processes, showing an abnormal behaviour near the end of the measurement. The hysteresis loops before and after 1 x 10 10 switching cycles have been slightly changed in both shape and magnitude. Such abnormality and fatigue-free property is an unusual result for PZT films prepared on conventional Pt/Ti/SiO 2 /Si substrates

  12. Microfabrication and integration of a sol-gel PZT folded spring energy harvester.

    Science.gov (United States)

    Lueke, Jonathan; Badr, Ahmed; Lou, Edmond; Moussa, Walied A

    2015-05-26

    This paper presents the methodology and challenges experienced in the microfabrication, packaging, and integration of a fixed-fixed folded spring piezoelectric energy harvester. A variety of challenges were overcome in the fabrication of the energy harvesters, such as the diagnosis and rectification of sol-gel PZT film quality and adhesion issues. A packaging and integration methodology was developed to allow for the characterizing the harvesters under a base vibration. The conditioning circuitry developed allowed for a complete energy harvesting system, consisting a harvester, a voltage doubler, a voltage regulator and a NiMH battery. A feasibility study was undertaken with the designed conditioning circuitry to determine the effect of the input parameters on the overall performance of the circuit. It was found that the maximum efficiency does not correlate to the maximum charging current supplied to the battery. The efficiency and charging current must be balanced to achieve a high output and a reasonable output current. The development of the complete energy harvesting system allows for the direct integration of the energy harvesting technology into existing power management schemes for wireless sensing.

  13. Au Nanoparticle Sub-Monolayers Sandwiched between Sol-Gel Oxide Thin Films

    Science.gov (United States)

    Della Gaspera, Enrico; Menin, Enrico; Sada, Cinzia

    2018-01-01

    Sub-monolayers of monodisperse Au colloids with different surface coverage have been embedded in between two different metal oxide thin films, combining sol-gel depositions and proper substrates functionalization processes. The synthetized films were TiO2, ZnO, and NiO. X-ray diffraction shows the crystallinity of all the oxides and verifies the nominal surface coverage of Au colloids. The surface plasmon resonance (SPR) of the metal nanoparticles is affected by both bottom and top oxides: in fact, the SPR peak of Au that is sandwiched between two different oxides is centered between the SPR frequencies of Au sub-monolayers covered with only one oxide, suggesting that Au colloids effectively lay in between the two oxide layers. The desired organization of Au nanoparticles and the morphological structure of the prepared multi-layered structures has been confirmed by Rutherford backscattering spectrometry (RBS), Secondary Ion Mass Spectrometry (SIMS), and Scanning Electron Microscopy (SEM) analyses that show a high quality sandwich structure. The multi-layered structures have been also tested as optical gas sensors. PMID:29538338

  14. Sol-gel synthesis and densification of aluminoborosilicate powders. Part 2: Densification

    Science.gov (United States)

    Bull, Jeffrey; Selvaduray, Guna; Leiser, Daniel

    1992-01-01

    Aluminoborosilicate (ABS) powders, high in alumina content, were synthesized by the sol-gel process utilizing four different methods of synthesis. The effect of these methods on the densification behavior of ABS powder compacts was studied. Five regions of shrinkage in the temperature range 25-1184 C were identified. In these regions, the greatest shrinkage occurred between the gel-to-glass transition temperature (T sub g approximately equal to 835 C) and the crystallization transformation temperature (T sub t approximately equal 900 C). The dominant mechanism of densification in this range was found to be viscous sintering. ABS powders were amorphous to x-rays up to T sub t at which a multiphasic structure crystallized. No 2Al2O3.B2O3 was found in these powders as predicted in the phase diagram. Above T sub t, densification was the result of competing mechanisms including grain growth and boria fluxed viscous sintering. Apparent activation energies for densification in each region varied according to the method of synthesis.

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

    Directory of Open Access Journals (Sweden)

    Francesco Baino

    2018-01-01

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

  16. Obtaining of Sol-Gel Ketorolac-Silica Nanoparticles: Characterization and Drug Release Kinetics

    International Nuclear Information System (INIS)

    Goerne, T.M.L.; Garcia, M.G.L.; Grada, G.R.; Perez, I.O.; Goerne, T.M.L.; Garcia, M.G.L.; Grada, G.R.; Perez, I.O.; Lemus, M.A.A.; Goerne, T.M.L.; Loez, E.G.

    2013-01-01

    Nonsteroidal anti-inflammatory drugs (NSAIDs) are among most commonly prescribed medications worldwide. NSAIDs play an important role due to their pronounced analgesic potency, anti-inflammatory effects, and lesser side effects compared to opioids. However, adverse effects including gastrointestinal and cardiovascular effects seriously complicate their prolonged use. In the present work we prepare SiO 2 -based nanoparticles with ketorolac, for controlled release proposes. The nano materials were prepared by the sol-gel technology at acidic conditions and two different water/alcoxide ratios were used. FTIR spectroscopy was performed in order to characterize the solids and drug-SiO 2 interactions. Thermal analysis and nitrogen adsorption isotherms showed thermal stability of the drug and confirmed the presence of particles with high surface area. Transmission electron micrographs of the samples showed the nano size particles (20 nm) forming aggregates. Drug release profiles were collected by means of UV-Vis spectroscopy and kinetic analysis was developed. Release data were fitted and 1:8 sample showed a sustained release over ten hours; 90% of the drug was delivered at the end of the time.

  17. Microstructure, optical, and electrochromic properties of sol-gel nanoporous tungsten oxide films

    Science.gov (United States)

    Djaoued, Yahia; Ashrit, P. V.; Badilescu, S.; Bruning, R.

    2003-08-01

    Porous tungsten oxide films have been prepared by a nonhydrolitic sol-gel method using poly(ethylene glycol) (PEG) as a structure directing agent. The method entails the hydrolysis of an ethanolic solution of tungsten ethoxide (formed by the reaction of WCl6 with ethanol) followed by condensation and polymerization at the PEG-tungsten oxide oligometers interface. A highly porous WO3 framework was obtained after PEG was burned off by calcination at a relativley low temperature. AFM images of the films treated thermally show an ordered material rather than microscopic particulates. Both fibrilar nanostructures and striped phase can be obtained via this approach, depending on the concentration of PEG in the coating solution. XRD data from the fibrils indicate that they are crystalline with very small crystals, whereas the striped phases obtained with 20% PEG correspond to two crystalline phases, one, the stoichiometric WO3 and the other one an oxygen deficient phase, containing larger crystals (~28 nm). The results show that PEG promotes the formation of oxygen deficient phases and delays crystallization. Compared to WO3 with no PEG, the optical and electrochromic properties of the macroporous tungsten oxide films appear to be significantly improved. The formation of organized nanostructures is tentatively accounted for by the strong hydrogen bonding interactions between PEG and the tungsten oxide oligomers.

  18. Doped indium nitride thin film by sol-gel spin coating method

    Science.gov (United States)

    Lee, Hui San; Ng, Sha Shiong; Yam, Fong Kwong

    2017-12-01

    In this study, magnesium doped indium nitride (InN:Mg) thin films grown on silicon (100) substrate were prepared via sol-gel spin coating method followed by nitridation process. A custom-made tube furnace was used to perform the nitridation process. Through this method, the low dissociation temperature issue of InN:Mg thin films can be solved. The deposited InN:Mg thin films were investigated using various techniques. The X-rays diffraction results revealed that two intense diffraction peaks correspond to wurtzite structure InN (100), and InN (101) were observed at 29° and 33.1° respectively. Field emission scanning electron microscopy images showed that the surface of the films exhibits densely packed grains. The elemental composition of the deposited thin films was analyzed using energy dispersive X-rays spectroscopy. The detected atomic percentages for In, N, and Mg were 43.22 %, 3.28 %, and 0.61 % respectively. The Raman spectra showed two Raman- and infrared-active modes of E2 (High) and A1 (LO) of the wurtzite InN. The band gap obtained from the Tauc plot showed around 1.74 eV. Lastly, the average surface roughness measured by AFM was around 0.133 µm.

  19. AZO Thin Films by Sol-Gel Process for Integrated Optics

    Directory of Open Access Journals (Sweden)

    Azzedine Boudrioua

    2013-07-01

    Full Text Available Undoped and aluminum-doped zinc oxide (AZO thin films are prepared by the sol-gel process. Zinc acetate dihydrate, ethanol, and monoethanolamine are used as precursor, solvent, and stabilizer, respectively. In the case of AZO, aluminum nitrate nonahydrate is added to the precursor solution with an atomic percentage equal to 1 and 2 at.% Al. The multi thin layers are deposited by spin-coating onto glass substrates, and are transformed into ZnO upon annealing at 550 °C. Films display a strong preferential orientation, with high values for the Texture Coefficients (TC of the (002 direction (TC(002 ≈ 3. The structural, morphological, and optical properties of the thin films as a function of aluminum content have been investigated using X-Ray Diffraction (XRD, Atomic Force Microscopy (AFM, and Scanning Electronic Microscopy (SEM. Waveguiding properties of the thin films have been also studied using m-lines spectroscopy. The results indicate that the films are monomodes at 632.8 nm with optical propagation optical losses estimated around 1.6 decibel per cm (dB/cm.

  20. Synthesis of palladium-doped silica nanofibers by sol-gel reaction and electrospinning process

    Energy Technology Data Exchange (ETDEWEB)

    San, Thiam Hui; Daud, Wan Ramli Wan; Kadhum, Abdul Amir Hassan; Mohamad, Abu Bakar; Kamarudin, Siti Kartom; Shyuan, Loh Kee; Majlan, Edy Herianto [Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia and Department of Chemical and Process Engineering, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia)

    2012-06-29

    Nanofiber is drawing great attention nowadays with their high surface area per volume and flexibility in surface functionalities that make them favorable as a proton exchange membrane in fuel cell application. In this study, incorporation of palladium nanoparticles in silica nanofibers was prepared by combination of a tetraorthosilane (TEOS) sol-gel reaction with electrospinning process. This method can prevent the nanoparticles from aggregation by direct mixing of palladium nanoparticles in silica sol. The as-produced electrospun fibers were thermally treated to remove poly(vinyl pyrrolidone) (PVP) and condensation of silanol in silica framework. PVP is chosen as fiber shaping agent because of its insulting and capping properties for various metal nanoparticles. Scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the silica fibers and Pd nanoparticles on the fibers. Spun fibers with average diameter ranged from 100nm to 400nm were obtained at optimum operating condition and distribution of Pd nanoparticles on silica fibers was investigated.

  1. Studies of (3-mercaptopropyl)trimethoxylsilane and bis(trimethoxysilyl)ethane sol-gel coating on copper and aluminum.

    Science.gov (United States)

    Li, Ying-Sing; Lu, Weijie; Wang, Yu; Tran, Tuan

    2009-09-01

    Bis(trimethoxysilyl)ethane (BTMSE) and (3-mercaptopropyl)trimethoxysilane (MPTMS) have been used as precursors to prepare sol-gels and hybrid sol-gel under acidic condition. From the X-ray photoelectron spectroscopy data on MPTMS sol-gel coated aluminum and copper, it has been shown that the silane film is covalently bonded to Al surface through the interfacial condensation. There is no evidence of bonding interaction between the thiol group and the Cu. The recorded reflection adsorption IR (RAIR) spectrum has provided evidence that the coating BTMSE film covalently interacts with Al. Vibrational assignments have been suggested for pure BTMSE, BTMSE sol-gel, BTMSE xerogel, and BTMSE coated Al panel based on the group frequencies and the variation of frequencies with the sample treatment conditions. The progression of condensation reaction has been observed from the IR spectra of the BTMSE sol-gel and the sol-gel coated film after the treatments at different temperatures with different lengths of time. The corrosion protection of the sol-gel coated Al and Cu has been characterized in NaCl solutions by cyclic voltammetric, potentiodynamic polarization and impedance spectroscopy methods. All these electrochemical measurements indicate that the sol-gel coated metals have better corrosion protection than the corresponding uncoated metals.

  2. Improving the scratch resistance of sol-gel metal oxide coatings cured at 250 C through use of thermogenerated amines

    NARCIS (Netherlands)

    Langanke, J.; Arfsten, N.; Buskens, P.; Habets, R.; Klankermayer, J.; Leitner, W.

    2013-01-01

    Scratch resistant sol-gel metal oxide coatings typically require a thermal post-treatment step (curing process) at temperatures between 400 and 700 C. In this report, we demonstrate that the in situ generation of amines within sol-gel films facilitates the preparation of scratch resistant metal

  3. On the healing mechanism of sol-gel derived hybrid materials containing dynamic di-sulfide bonds

    NARCIS (Netherlands)

    AbdolahZadeh, M.; Esteves, A.C.C.; Van der Zwaag, S.; Garcia Espallargas, S.J.

    2013-01-01

    Sol-gel technology is increasingly being used in coatings for corrosion protection and adhesion improvement. So far, the self-healing concept in sol-gel coatings has only been approached from extrinsic healing perspective (i.e. use of nano and micro carriers of corrosion inhibitors) [1]. Despite the

  4. Nanostructured sol-gel coatings doped with cerium nitrate as pre-treatments for AA2024-T3

    International Nuclear Information System (INIS)

    Zheludkevich, M.L.; Serra, R.; Montemor, M.F.; Yasakau, K.A.; Salvado, I.M. Miranda; Ferreira, M.G.S.

    2005-01-01

    Nanostructured hybrid sol-gel coatings doped with cerium ions were investigated in the present work as pre-treatments for the AA2024-T3 alloy. The sol-gel films have been synthesized from tetraethylorthosilicate (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTMS) precursors. Additionally the hybrid sol was doped with zirconia nanoparticles prepared from hydrolyzed tetra-n-propoxyzirconium (TPOZ). Cerium nitrate, as corrosion inhibitor, was added into the hybrid matrix or into the oxide nanoparticles. The chemical composition and the structure of the hybrid sol-gel films were studied by XPS (X-ray photoelectron spectroscopy) and AFM (atomic force microscopy), respectively. The evolution of the corrosion protection properties of the sol-gel films was studied by EIS (electrochemical impedance spectroscopy), which can provide quantitative information on the role of the different pre-treatments. Different equivalent circuits, for different stages of the corrosion processes, were used in order to model the coating degradation. The models were supported by SEM (scanning electron microscopy) measurements. The results show that the sol-gel films containing zirconia nanoparticles present improved barrier properties. Doping the hybrid nanostructured sol-gel coatings with cerium nitrate leads to additional improvement of the corrosion protection. The zirconia particles present in the sol-gel matrix seem to act as nanoreservoirs providing a prolonged release of cerium ions. The nanostructured sol-gel films doped with cerium nitrate can be proposed as a potential candidate for substitution of the chromate pre-treatments for AA2024-T3

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

    Science.gov (United States)

    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. Sol-gel encapsulation of pullulanase in the presence of hybrid magnetic (Fe3O4-chitosan) nanoparticles improves thermal and operational stability.

    Science.gov (United States)

    Long, Jie; Li, Xingfei; Zhan, Xiaobei; Xu, Xueming; Tian, Yaoqi; Xie, Zhengjun; Jin, Zhengyu

    2017-06-01

    Pullulanase was sol-gel encapsulated in the presence of magnetic chitosan/Fe 3 O 4 nanoparticles. The resulting immobilized pullulanase was characterized by scanning electron microscopy, vibrating sample magnetometry, Fourier transform infrared spectroscopy and thermogravimetric analysis. The results showed that the addition of pullulanase created a more regular surface on the sol-gel matrix and an enhanced magnetic response to an applied magnetic field. The maximal activity retention (83.9%) and specific activity (291.7 U/mg) of the immobilized pullulanase were observed under optimized conditions including an octyltriethoxysilane:tetraethoxysilane (OTES:TEOS) ratio of 1:2 and enzyme concentration of 0.484 mg/mL sol. The immobilized enzyme exhibited good thermal stability. When the temperature was above 60 °C, the immobilized pullulanase showed significantly higher activity than the free enzyme (p sol-gel encapsulation and co-immobilized by crosslinking-encapsulation retained 52 and 69% of their initial activity after 5 h at 62 °C, respectively, compared to 11% for the free enzyme. Moreover, the stability of the pullulanase was improved by crosslinking-encapsulation, as the enzyme retained more than 85 and 81% of its original activity after 5 and 6 consecutive reuses, respectively, compared to 80 and 72% of its original activity for simple sol-gel encapsulated enzymes. This indicated the leakage of enzyme molecules through the pores of the gel was substantially abated by cross-linking. Such immobilized pullulanase provides high stability and ease of enzyme recovery, characteristics that are advantageous for applications in the food industry that involve continuous starch processing.

  7. Acoustic emission sensor radiation damage threshold experiment

    International Nuclear Information System (INIS)

    Beeson, K.M.; Pepper, C.E.

    1994-01-01

    Determination of the threshold for damage to acoustic emission sensors exposed to radiation is important in their application to leak detection in radioactive waste transport and storage. Proper response to system leaks is necessary to ensure the safe operation of these systems. A radiation impaired sensor could provide ''false negative or false positive'' indication of acoustic signals from leaks within the system. Research was carried out in the Radiochemical Technology Division at Oak Ridge National Laboratory to determine the beta/gamma radiation damage threshold for acoustic emission sensor systems. The individual system consisted of an acoustic sensor mounted with a two part epoxy onto a stainless steel waveguide. The systems were placed in an irradiation fixture and exposed to a Cobalt-60 source. After each irradiation, the sensors were recalibrated by Physical Acoustics Corporation. The results were compared to the initial calibrations performed prior to irradiation and a control group, not exposed to radiation, was used to validate the results. This experiment determines the radiation damage threshold of each acoustic sensor system and verifies its life expectancy, usefulness and reliability for many applications in radioactive environments

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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

  10. Relationship between sol-gel conditions and enzyme stability: a case study with β-galactosidase/silica biocatalyst for whey hydrolysis.

    Science.gov (United States)

    Escobar, Sindy; Bernal, Claudia; Mesa, Monica

    2015-01-01

    The sol-gel process has been very useful for preparing active and stable biocatalysts, with the possibility of being reused. Especially those based on silica are well known. However, the study of the enzyme behavior during this process is not well understood until now and more, if the surfactant is involved in the synthesis mixture. This work is devoted to the encapsulation of β-galactosidase from Bacillus circulans in silica by sol-gel process, assisted by non-ionic Triton X-100 surfactant. The correlation between enzyme activity results for the β-galactosidase in three different environments (soluble in buffered aqueous reference solution, in the silica sol, and entrapment on the silica matrix) explains the enzyme behavior under stress conditions offered by the silica sol composition and gelation conditions. A stable β-galactosidase/silica biocatalyst is obtained using sodium silicate, which is a cheap source of silica, in the presence of non-ionic Triton X-100, which avoids the enzyme deactivation, even at 40 °C. The obtained biocatalyst is used in the whey hydrolysis for obtaining high value products from this waste. The preservation of the enzyme stability, which is one of the most important challenges on the enzyme immobilization through the silica sol-gel, is achieved in this study.

  11. Architectural optimization of an epoxy-based hybrid sol-gel coating for the corrosion protection of a cast Elektron21 magnesium alloy

    Science.gov (United States)

    Murillo-Gutiérrez, N. V.; Ansart, F.; Bonino, J.-P.; Kunst, S. R.; Malfatti, C. F.

    2014-08-01

    An epoxy-based hybrid sol-gel coating was prepared in various architectural configurations has been studied for the corrosion protection of a cast Elektron21 magnesium alloy. The creation of a single layer of this coating presents defects consisting of macro-pores and protuberances, which opens access for corrosive species to reach the metallic substrate. These defects are suspected to result from the high reactivity of the substrate, as well as to the irregular topography of the substrate disrupted by the microstructure of the own magnesium alloy. Hence, a sol-gel coating in bilayer architecture is proposed, where the first layer would “inert” the surface of the magnesium substrate, and the second layer would cover the defects of the first layer and also thickening the coating. The morphological characteristics of the sol-gel coatings were analyzed by scanning electron microscopy (SEM), and their corrosion behavior was evaluated by OCP (open circuit potential) monitoring and electrochemical impedance spectroscopy (EIS) in chloride media. It is shown that both the architectural arrangement and the individual thickness of the first and second layers have an important influence on the anticorrosion performances of the protective system, just as much as its global thickness.

  12. In vitro toxicity assessment of extracts derived from sol-gel coatings on polycarbonate intended to be used in food contact applications.

    Science.gov (United States)

    Séverin, Isabelle; Lionti, Krystelle; Dahbi, Laurence; Loriot, Catherine; Toury, Bérangère; Chagnon, Marie-Christine

    2016-07-01

    Polycarbonate is a widely used polymer in food contact applications all around the world. However, due to the potential release of Bisphenol A (BPA) during repeated washing cycles, its use becomes compromised as BPA is known for being an endocrine disruptor for rodents. In order to tackle this issue, sol-gel coatings based on organoalkoxysiloxane were developed on PC, to act as a physical barrier. To this end, two sol-gel systems based on tetraethylorthosilicate (TEOS), methyltriethoxysilane (MTES) and 3-glycidyloxypropyltriethoxysilane (GPTES), three common sol-gel precursors, were prepared. The coatings derived from the latter two systems were then studied with regards to their potential toxicity in vitro. Migration tests were performed in food simulants, and the maximal migration was obtained in ethanol 10% (v/v) for one system and in isooctane for the other one. In vitro genotoxicity was assessed with the Ames test (OECD 471) and the micronucleus assay (OECD 487), and no genotoxic effect was observed. Moreover, the estrogenic activity of the extracts was studied with a transcriptional activation assay using transient transfection in human cells; none of the extracts was found estrogenic. These negative in vitro results are highly promising for the future use of these new barrier coating formulations onto food contact materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Infrared and Raman spectroscopic studies of tris-[3-(trimethoxysilyl)propyl] isocyanurate, its sol-gel process, and coating on aluminum and copper.

    Science.gov (United States)

    Li, Ying-Sing; Church, Jeffrey S; Woodhead, Andrea L; Vecchio, Nicolas E; Yang, Johnny

    2014-11-11

    Tris-[3-(trimethoxysilyl)propyl] isocyanurate (TTPI) has been used as a precursor to prepare a sol using ethanol as the solvent under acidic conditions. The sol-gel was applied for the surface treatment of aluminum and copper. Infrared and Raman spectra have been recorded for pure TTPI and the TTPI sol, xerogel and TTPI sol-gel coated metals. From the vibrational spectra, TTPI is likely to have the C1 point group. Vibrational assignments are suggested based on group frequencies, the expected reactions in the sol-gel process and the vibrational studies of some related molecules. From the experimental infrared spectra of xerogels annealed at different temperatures and from the thermal-gravimetric analysis, it is found that the TTPI xerogel decomposes at around 450°C with silica being the major decomposition product. A cyclic voltammetric study of the metal electrodes coated with different concentrations of TTPI ranging from 5% to 42% (v/v) has shown that the films with high concentrations of sol would provide better corrosion protection for aluminum and copper. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Organization in sol-gel polymerization of methacrylate co-oligomers containing trimethoxysilylpropyl methacrylate

    Czech Academy of Sciences Publication Activity Database

    Vraštil, J.; Matějka, Libor; Špaček, V.; Večeřa, M.; Prokůpek, L.

    2005-01-01

    Roč. 46, č. 25 (2005), s. 11232-11240 ISSN 0032-3861 Institutional research plan: CEZ:AV0Z40500505 Keywords : organic-inorganic hybrid * sol-gel process * oligomers Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.849, year: 2005

  15. Analysis and theory of gas transport in microporous sol-gel derived ceramic membranes

    NARCIS (Netherlands)

    de Lange, R.S.A.; de Lange, Rob; Keizer, Klaas; Burggraaf, Anthonie; Burggraaf, A.J.

    1995-01-01

    Sol-gel modification of mesoporous alumina membranes is a very successful technique to improve gas separation performance. Due to the formed microporous top layer, the membranes show activated transport and molecular sieve-like separation factors. This paper concentrates on the mechanism of

  16. Study of positron lifetime spectrum for Zn O varistor ceramics fabricated by Sol-gel route

    International Nuclear Information System (INIS)

    Li Xigui; Wei Shutao; Zhang Ruiying; Cheng Guosheng; Dai Xianqi; Zhang Jincang; Xing Huaimin

    2000-01-01

    An investigation of positron lifetime spectrum for ZnO varistor ceramics fabricated by Sol-gel route was carried out. The relationship between lifetime parameters and the densification and nonlinear coefficient α was given. The dependence of electrical properties on sintering temperature and duration was discussed

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

    Science.gov (United States)

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

    2018-06-16

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

  18. Silica-Based Sol-Gel Coating on Magnesium Alloy with Green Inhibitors

    Directory of Open Access Journals (Sweden)

    Vinod Upadhyay

    2017-06-01

    Full Text Available In this work, the performances of several natural organic inhibitors were investigated in a sol-gel system (applied on the magnesium alloy Mg AZ31B substrate. The inhibitors were quinaldic acid (QDA, betaine (BET, dopamine hydrochloride (DOP, and diazolidinyl urea (DZU. Thin, uniform, and defect-free sol-gel coatings were prepared with and without organic inhibitors, and applied on the Mg AZ31B substrate. SEM and EDX were performed to analyze the coating surface properties, the adhesion to the substrate, and the thickness. Electrochemical measurements, including electrochemical impedance spectroscopy (EIS and anodic potentiodynamic polarization scan (PDS, were performed on the coated samples to characterize the coatings’ protective properties. Also, hydrogen evolution measurement—an easy method to measure magnesium corrosion—was performed in order to characterize the efficiency of coating protection on the magnesium substrate. Moreover, scanning vibrating electrode technique (SVET measurements were performed to examine the efficiency of the coatings loaded with inhibitors in preventing and containing corrosion events in defect areas. From the testing results it was observed that the formulated sol-gel coatings provided a good barrier to the substrate, affording some protection even without the presence of inhibitors. Finally, when the inhibitors’ performances were compared, the QDA-doped sol-gel was able to contain the corrosion event at the defect.

  19. Tin dioxide sol-gel derived films doped with platinum and antimony deposited on porous silicon

    NARCIS (Netherlands)

    Savaniu, C.; Arnautu, A.; Cobianu, C.; Craciun, G.; Flueraru, C.; Zaharescu, M.; Parlog, C.; Paszti, F.; van den Berg, Albert

    1999-01-01

    SnO2 sol-gel derived thin films doped simultaneously with Pt and Sb are obtained and reported for the first time. The Sn sources were tin(IV) ethoxide or tin(II) ethylhexanoate, while hexachloroplatinic acid (H2PtCl6) and antimony chloride (SbCl3) were used as platinum and antimony sources,

  20. Sol-gel/hydrothermal synthesis of mixed metal oxide of Titanium and ...

    African Journals Online (AJOL)

    Mixed metal oxides of titanium and zinc nanocomposites were prepared through sol-gel method under hydrothermal condition using titanium oxy-(1, 2 - pentadione) and zinc acetate without hazardous additives. The resulting composites were characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscope ...

  1. Influence of p H on optical properties of nano structure sol-gel-derived silica films

    International Nuclear Information System (INIS)

    Heshmatpuor, F.; Adelkhani, H.; Nahavandi, M.; Noorbakhsh Shourabadi, M.

    2006-01-01

    Sol-gel derived silica films were fabricated by dip-coating onto glass microscope substrates. Film properties such as transmission and surface morphology were monitored as function of dip speed and sol p H. Film transmission was increased with increasing of p H in visible range. The surface morphology of films were investigated with scanning electron microscopy.

  2. Hydrogen permeation through sol-gel-coated iron during galvanostatic charging

    International Nuclear Information System (INIS)

    Zakorchemna, I.; Carmona, N.; Zakroczymski, T.

    2008-01-01

    One-layer sol-gel silica-zirconia and two-layer silica-zirconia and zirconia coatings were deposited on one side of iron membranes by spin-coating, densified in air and annealed up to 800 deg. C in vacuum. Hydrogen permeation through the membranes, coated and uncoated, polarised cathodically under galvanostatic control in 0.1 M NaOH solution was studied using the electrochemical permeation technique. During the initial period, the effect of the sol-gel coatings was insignificant. However, the coatings quite efficiently prevented the iron surface become more active to hydrogen entry during a long-lasting cathodic polarisation. In addition, the electrochemical-corrosion behaviour of the coated iron and the effect of the sol-gel coatings on the effective diffusivity of hydrogen in the coated membranes were studied. On the basis of the polarisation curves and the hydrogen permeation data it was proved that the sol-gel coatings blocked the iron surface for the hydrogen evolution reaction and, consequently, for the hydrogen entry into iron. The effective coating coverage was determined by comparison of the hydrogen fluxes permeating the coated and uncoated membranes. Finally the real concentration of hydrogen beneath the uncoated iron sites and the amount of hydrogen stored in a membrane were evaluated

  3. Patterned transparent zinc oxide films produced by sol-gel embossing

    Energy Technology Data Exchange (ETDEWEB)

    Rao, J.; Koh, L.H.K.; Crean, G.M. [Tyndall National Institute, Lee Maltings, Prospect Row, Cork (Ireland); Department of Microelectronic Engineering, University College Cork, Cork (Ireland); O' Brien, S. [Tyndall National Institute, Lee Maltings, Prospect Row, Cork (Ireland); Winfield, R.J.

    2008-08-15

    A low cost zinc oxide embossing technique is reported as a method of fabricating structures relevant to a variety of applications. A zinc based sol-gel material was prepared from zinc acetate[Zn(C{sub 2}H{sub 3}O{sub 2}){sub 2}], monoethanolamine[H{sub 2}NC{sub 2}H{sub 4}OH] and isopropanol. The sol-gel was cast into a polydimethylsiloxane (PDMS) mould a track design, placed in contact with the substrate and dried under vacuum at 70 C for 3 hours. The formed track pattern was further densified to provide a stable conductor film that retained the embossed shape. An optimum Zn sol-gel content of 0.6 M was identified. The embossed films had a transparency of greater than 83% in the visible region. The optical bandgap energy was evaluated to be 3.306 eV. The influence of ZnO sol-gel film synthesis and embossing parameters on the microstructure, morphology and optical transparency of fabricated structures is described. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  4. Analysis of coupled mass transfer and sol-gel reaction in a two-phase system

    NARCIS (Netherlands)

    Castelijns, H.J.; Huinink, H.P.; Pel, L.; Zitha, P.L.J.

    2006-01-01

    The coupled mass transfer and chemical reactions of a gel-forming compound in a two-phase system were studied in detail. Tetra-methyl-ortho-silicate (TMOS) is often used as a precursor in sol-gel chemistry to produce silica gels in aqueous systems. TMOS can also be mixed with many hydrocarbons

  5. Nanocrystalline Ni-Zn ferrites prepared by sol-gel method

    Czech Academy of Sciences Publication Activity Database

    Popovici, M.; Savii, C.; Nižňanský, Daniel; Šubrt, Jan; Boháček, Jaroslav; Becherescu, D.; Caizer, C.; Enache, C.; Ionescu, C.

    2003-01-01

    Roč. 5, č. 1 (2003), s. 251-256 ISSN 1454-4164 R&D Projects: GA MŠk LN00A028 Institutional research plan: CEZ:AV0Z4032918 Keywords : nanostructures * sol-gel processing * XRD Subject RIV: CA - Inorganic Chemistry Impact factor: 0.996, year: 2003

  6. Sol-gel immobilization of serine proteases for application in organic solvents

    NARCIS (Netherlands)

    van Unen, D.J.; Engbersen, Johannes F.J.; Reinhoudt, David

    2001-01-01

    The serine proteases α-chymotrypsin, trypsin, and subtilisin Carlsberg were immobilized in a sol-gel matrix and the effects on the enzyme activity in organic media are evaluated. The percentage of immobilized enzyme is 90% in the case of α-chymotrypsin and the resulting specific enzyme activity in

  7. Sol-gel coatings of ceramic fibres for composites with ceramic matrix

    International Nuclear Information System (INIS)

    Maier, B.; Grathwohl, G.; Spallek, M.; Pannhorst, W.

    1992-01-01

    The aim of this work was to show the feasibility in principle of sol-gel coating of ceramic reinforcement components for composites from technical aspects as well. The complexity of the coating task rises with the transition from individual fibres to bundles of fibres of different thickness to weaves, and finally to composites. (orig.) [de

  8. The increase in pH during aging of porous sol-gel silica spheres

    NARCIS (Netherlands)

    Titulaer, M.K.; Kegel, W.K.; Jansen, J.B.H.; Geus, John W.

    1994-01-01

    The increase in pH in the hydrothermal fluid is studied after hydrothermal aging of porous silica gel spheres of 1–3 mm diameter. The porous silica spheres are formed by the sol-gel process from a supersaturated silica solution. The increase of the pH of the hydrothermal solution affects the silica

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  11. Sol-gel coatings on large area glass sheets for electrochromic devices

    NARCIS (Netherlands)

    Vroon, Z.A.E.P.; Spee, C.I.M.A.

    1997-01-01

    The preparation of vanadium and tungsten oxide coatings is described using vanadium oxide tri-2-propoxide/2-propanol and tungsten penta-ethoxide/2-propanol solutions. These solutions are dip coated onto K-glass substrates and cured. For vanadium oxide coatings it is shown that sol-gel/dip coat

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

    Science.gov (United States)

    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. Gel stabilization in chelate sol-gel preparation of Bi-2223 superconductors

    Czech Academy of Sciences Publication Activity Database

    Rubešová, K.; Jakeš, V.; Hlásek, T.; Vašek, Petr; Matějka, P.

    2012-01-01

    Roč. 73, č. 3 (2012), s. 448-453 ISSN 0022-3697 Institutional research plan: CEZ:AV0Z10100521 Keywords : superconductors * sol-gel growth * infrared spectroscopy * thermogravimetric analysis (TGA) * X-ray diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.527, year: 2012

  14. Epoxy-based organic-inorganic nanocomposite coatings and films prepared by sol-gel process

    Czech Academy of Sciences Publication Activity Database

    Špírková, Milena; Brus, Jiří; Matějka, Libor

    2004-01-01

    Roč. 6, 3-4 (2004), s. 7-15 R&D Projects: GA ČR GA203/01/0735; GA AV ČR IAA4050008; GA AV ČR KSK4050111 Institutional research plan: CEZ:AV0Z4050913 Keywords : sol-gel process * nanocomposite s * solid-state NMR Subject RIV: CD - Macromolecular Chemistry

  15. A sol-gel-modified poly(methyl methacrylate) electrophoresis microchip with a hydrophilic channel wall.

    Science.gov (United States)

    Chen, Gang; Xu, Xuejiao; Lin, Yuehe; Wang, Joseph

    2007-01-01

    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 approximately 27.4 degrees compared with approximately 66.3 degrees for the pure PMMA. In addition, the electro-osmotic flow increased from 2.13x10(-4) cm2 V(-1) s(-1) for the native-PMMA channel to 4.86x10(-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. Supercritical fluid extraction of silicone oil from uranate microspheres prepared by sol-gel process

    International Nuclear Information System (INIS)

    Kumar, R.; Venkatakrishnan, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

    2005-01-01

    Supercritical fluid extraction of silicone oil from urania microspheres prepared through sol-gel route was investigated. The influence of pressure, temperature, and flow rate on the extraction efficiency was studied. Experimental conditions were optimised for the complete removal of silicone oil from urania microspheres. (author)

  17. Active corrosion protection of AA2024 by sol-gel coatings with corrosion inhibitors =

    Science.gov (United States)

    Yasakau, Kiryl

    A industria aeronautica utiliza ligas de aluminio de alta resistencia para o fabrico dos elementos estruturais dos avioes. As ligas usadas possuem excelentes propriedades mecanicas mas apresentam simultaneamente uma grande tendencia para a corrosao. Por esta razao essas ligas necessitam de proteccao anticorrosiva eficaz para poderem ser utilizadas com seguranca. Ate a data, os sistemas anticorrosivos mais eficazes para ligas de aluminio contem cromio hexavalente na sua composicao, sejam pre-tratamentos, camadas de conversao ou pigmentos anticorrosivos. O reconhecimento dos efeitos carcinogenicos do cromio hexavalente levou ao aparecimento de legislacao banindo o uso desta forma de cromio pela industria. Esta decisao trouxe a necessidade de encontrar alternativas ambientalmente inocuas mas igualmente eficazes. O principal objectivo do presente trabalho e o desenvolvimento de pretratamentos anticorrosivos activos para a liga de aluminio 2024, baseados em revestimentos hibridos produzidos pelo metodo sol-gel. Estes revestimentos deverao possuir boa aderencia ao substrato metalico, boas propriedades barreira e capacidade anticorrosiva activa. A proteccao activa pode ser alcancada atraves da incorporacao de inibidores anticorrosivos no pretratamento. O objectivo foi atingido atraves de uma sucessao de etapas. Primeiro investigou-se em detalhe a corrosao localizada (por picada) da liga de aluminio 2024. Os resultados obtidos permitiram uma melhor compreensao da susceptibilidade desta liga a processos de corrosao localizada. Estudaram-se tambem varios possiveis inibidores de corrosao usando tecnicas electroquimicas e microestruturais. Numa segunda etapa desenvolveram-se revestimentos anticorrosivos hibridos organico-inorganico baseados no metodo sol-gel. Compostos derivados de titania e zirconia foram combinados com siloxanos organofuncionais a fim de obter-se boa aderencia entre o revestimento e o substrato metalico assim como boas propriedades barreira. Testes

  18. Iron specificity of a biosensor based on fluorescent pyoverdin immobilized in sol-gel glass

    Science.gov (United States)

    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. rhEGF-containing thermosensitive and mucoadhesive polymeric sol-gel for endoscopic treatment of gastric ulcer and bleeding.

    Science.gov (United States)

    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.

  20. Sol-gel processes and materials. November 1971-October 1989 (Citations from the US Patent data base). Report for November 1971-October 1989

    International Nuclear Information System (INIS)

    1990-01-01

    This bibliography contains citations of selected patents concerning sol-gel processes and sol-gel derived materials and products. Selected patents include sol-gel compositions, ceramic and refractory materials, fabrication of silica glass, sol-gel thin films and coatings, transparent inorganic oxide glass, luminescent quartz glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, sol-gel production of microspheres, alumina composites, photographic materials, and dental materials. (This updated bibliography contains 120 citations, 12 of which are new entries to the previous edition.)

  1. Sol-gel processes and materials. January 1970-August 1989 (Citations from the US Patent data base). Report for January 1970-August 1989

    International Nuclear Information System (INIS)

    1989-09-01

    This bibliography contains citations of selected patents concerning Sol-Gel processes and Sol-Gel derived materials and products. Selected patents include Sol-Gel compositions, ceramic and refractory materials, fabrication of silica glass, Sol-Gel thin films and coatings, transparent inorganic oxide glass, luminescent quartz glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, Sol-Gel production of microspheres, alumina composites, photographic materials, and dental materials. (This updated bibliography contains 108 citations, 37 of which are new entries to the previous edition.)

  2. A Urea Biosensor from Stacked Sol-Gel Films with Immobilized Nile Blue Chromoionophore and Urease Enzyme

    OpenAIRE

    Alqasaimeh, Muawia Salameh; Heng, Lee Yook; Ahmad, Musa

    2007-01-01

    An optical urea biosensor was fabricated by stacking several layers of sol-gel films. The stacking of the sol-gel films allowed the immobilization of a Nile Blue chromoionophore (ETH 5294) and urease enzyme separately without the need of any chemical attachment procedure. The absorbance response of the biosensor was monitored at 550 nm, i.e. the deprotonation of the chromoionophore. This multi-layer sol-gel film format enabled higher enzyme loading in the biosensor to be achieved. The urea op...

  3. The chemical and catalytic properties of nanocrystalline metal oxides prepared through modified sol-gel synthesis

    Science.gov (United States)

    Carnes, Corrie Leigh

    The goal of this research was to synthesize, characterize and study the chemical properties of nanocrystalline metal oxides. Nanocrystalline (NC) ZnO, CuO, NiO, Al2O3, and the binary Al2O 3/MgO and ZnO/CuO were prepared through modified sol gel methods. These NC metal oxides were studied in comparison to the commercial (CM) metal oxides. The samples were characterized by XRD, TGA, FTIR, BET, and TEM. The NC samples were all accompanied by a significant increase in surface area and decrease in crystallite size. Several chemical reactions were studied to compare the NC samples to the CM samples. One of the reactions involved a high temperature reaction between carbon tetrachloride and the oxide to form carbon dioxide and the corresponding metal chloride. A similar high temperature reaction was conducted between the metal oxide and hydrogen sulfide to form water and the corresponding metal sulfide. A room temperature gas phase adsorption was studied where SO2 was adsorbed onto the oxide. A liquid phase adsorption conducted at room temperature was the destructive adsorption of paraoxon (a toxic insecticide). In all reactions the NC samples exhibited greater activity, destroying or adsorbing a larger amount of the toxins compared to the CM samples. To better study surface area effects catalytic reactions were also studied. The catalysis of methanol was studied over the nanocrystalline ZnO, CuO, NiO, and ZnO/CuO samples in comparison to their commercial counterparts. In most cases the NC samples proved to be more active catalysts, having higher percent conversions and turnover numbers. A second catalytic reaction was also studied, this reaction was investigated to look at the support effects. The catalysis of cyclopropane to propane was studied over Pt and Co catalysts. These catalysts were supported onto NC and CM alumina by impregnation. By observing differences in the catalytic behavior, support effects have become apparent.

  4. Crystallization and magnetic characterizations of DyIG and HoIG nanopowders fabricated using citrate sol-gel

    Directory of Open Access Journals (Sweden)

    Dao Thi Thuy Nguyet

    2016-06-01

    Full Text Available Dy and Ho iron garnets in form of nanoparticles were synthesized by citrate sol-gel method. Phase formation, lattice constant and average crystallite sizes of the samples were determined via XRD measurements. Morphology and particle size distribution were studied by TEM and chemical composition was checked by EDX. Magnetic measurements in temperature range 5–600 K and in the maximum applied field of 50 kOe were carried out by using SQUID and VSM. Their magnetic parameters, including Curie temperature, magnetization compensation temperature, spontaneous magnetization, high-field susceptibility, magnetic coercivity were discussed in the framework of three interacting magnetic sublattices, magnetocrystalline anisotropy, core-shell model and compared to those of the bulk materials. Based on these analyses further evaluation on the crystallinity and homogeneity of the samples has been made.

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

    Directory of Open Access Journals (Sweden)

    Xiaodong Wang

    2012-12-01

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

  6. Electrical, dielectric and photocatalytic properties of Fe-doped ZnO nanomaterials synthesized by sol gel method

    Directory of Open Access Journals (Sweden)

    Yacine Cherif

    2016-09-01

    Full Text Available Fe-doped ZnO nanoparticles were synthesized by sol gel technique. Fine-scale and single phase hexagonal wurtzite structure in all samples were confirmed by SEM and XRD, respectively. The band gap energy depends on the amount of Fe and was found to be in the range of 3.11–2.53 eV. The electric and dielectric properties were investigated using complex impedance spectroscopy. AC conductivity data were correlated with the barrier hopping (CBH model to evaluate the binding energy (Wm, the minimum hopping distance (Rmin and the density of states at Fermi level, N(EF. Fe doping in ZnO also improved the photocatalytic activity. Thus, the sample Zn0.95Fe0.05O showed high degradation potential towards methylene blue (MB, i.e. it degrades 90% of BM in 90 min under UV light.

  7. Effect of sol-age on the surface and optical properties of sol-gel derived mesoporous zirconia thin films

    Directory of Open Access Journals (Sweden)

    Manish Kumar

    2011-06-01

    Full Text Available Mesoporous ZrO2 thin films have been deposited by a modified sol-gel dip coating technique using HCl as catalyst. Effects of sol-age on the surface and on the optical properties are studied. Transmission electron micrographs of the films reveal the pore dimensions in mesoporous regime. A strong correlation in surface topography with sol-age has been observed where increase in sol-age induces a systematic enhancement in the value of root mean square roughness of the films. Optical study shows that deposited films have high transmittance and an enhancement of 5.6 times in porosity in films prepared with sol-age of 10 days with respect to that of 1 day. Band gap estimation by Tauc's plots of films is observed to 5.74 eV, which shows invariance with the sol-age.

  8. Sol-gel synthesis of YBa2Cu3O7-x superconductor by mixed organic-inorganic polymerization

    International Nuclear Information System (INIS)

    Valente, I.; Sanchez, C.; Henry, M.; Livage, J.

    1989-01-01

    Sol-gel processes are quite attractive methods to produce films or fibers of high Tc superconducting materials. The gel step allows a good chemical homogeneity and generally provides a rather low processing temperature. Blue sols or monolithic gels can be easily produced using mixed organic-inorganic polymerisation of molecular precursors. An aqueous solution of copper, barium acetates and yttrium nitrate is mixed with an acrylic acid solution where a radical organic polymerisation process has been initiated. After pH adjustments, the viscosity of the resulting solution can be adjusted by heating. After drying at 150 0 C and calcination above 700 0 C, the YBaCuO network is formed and superconducting properties appears above 850 0 C. Fine particles (0.1-1 μm) are obtained which can be sintered to produce a ceramic material with a particularly narrow resistive transition [fr

  9. A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

    Science.gov (United States)

    Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

    2010-01-01

    A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

  10. Dependence of electrical and optical properties of sol-gel prepared undoped cadmium oxide thin films on annealing temperature

    International Nuclear Information System (INIS)

    Santos-Cruz, J.; Torres-Delgado, G.; Castanedo-Perez, R.; Jimenez-Sandoval, S.; Jimenez-Sandoval, O.; Zuniga-Romero, C.I.; Marquez Marin, J.; Zelaya-Angel, O.

    2005-01-01

    The effect of the annealing temperature (T a ) on the optical, electrical and structural properties of the undoped cadmium oxide (CdO) thin films obtained by the sol-gel method, using a simple precursor solution, was studied. All the CdO films annealed in the range from 200 to 450 deg. C are polycrystalline with (111) preferential orientation and present high optical transmission > 85% for wavelengths above 500 nm. The resistivity decreases as T a increases until it reaches a value of 6 x 10 -4 Ω cm for T a 350 deg. C. For higher temperatures the resistivity experiences a slight increase. Images obtained by atomic force microscopy show an evident incremental change of the aggregate size (clusters of grains) as T a increases. The grain size also increases when T a increases as observed in data calculated from X-ray measurements

  11. Sol-gel auto-combustion synthesis and properties of Co2Z-type hexagonal ferrite ultrafine powders

    Science.gov (United States)

    Liu, Junliang; Yang, Min; Wang, Shengyun; Lv, Jingqing; Li, Yuqing; Zhang, Ming

    2018-05-01

    Z-type hexagonal ferrite ultrafine powders with chemical formulations of (BaxSr1-x)3Co2Fe24O41 (x varied from 0.0 to 1.0) have been synthesized by a sol-gel auto-combustion technique. The average particle sizes of the synthesized powders ranged from 2 to 5 μm. The partial substitution of Ba2+ by Sr2+ led to the shrinkage of the crystal lattices and resulted in changes in the magnetic sub-lattices, which tailored the static and dynamic magnetic properties of the as-synthesized powders. As the substitution ratio of Ba2+ by Sr2+, the saturation magnetization of the synthesized powders almost consistently increased from 43.3 to 56.1 emu/g, while the real part of permeability approached to a relatively high value about 2.2 owing to the balance of the saturation magnetization and magnetic anisotropy field.

  12. Laser sintering of doped strontium aluminate via modified sol-gel for use as a ceramic pigment; Sinterizacao a laser do aluminato de estroncio dopado via sol-gel modificado para aplicacao como pigmento ceramico

    Energy Technology Data Exchange (ETDEWEB)

    Soares, F.M. dos S.; Valerio, M.E.G. [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil)

    2017-01-15

    Powder of Dy{sup 3+} co-doped SrAl{sub 2}O{sub 4} :Eu{sup 3+} was produced via proteic sol-gel method, a modified sol-gel route which allows the formation of oxides at lower temperatures than other methods. CO{sub 2} laser sintering was used as a method for heat treatment, effective in reducing trivalent europium ions in doped samples. Thermal analysis of the precursors, performed by TG and DTA, revealed that the crystallization of SrAl{sub 2}O{sub 4} phase occurred at approximately 1060 °C. X-ray diffraction showed that the samples, before and after sintering, had monoclinic and hexagonal phases formation. DLS technique revealed the presence of nanosized and micrometric particles, and particle agglomerates, confirmed by SEM images. Micrographs of the fracture surface of a sintered pellet revealed a high degree of densification caused by heat treatment. Photoluminescence measurements showed that the samples after synthesis and before heat treatment with laser had reddish emission, composed of characteristic narrow emission lines from Eu{sup 3+} and more intense emission when the samples were excited at 265 nm. The laser treatment promoted the reduction of Eu{sup 3+} to Eu{sup 2+} and this effect was confirmed by the presence of a wide emission band in the green region of the spectrum with a maximum emission obtained after excitation at 350 nm. The luminescent decay time of the thermally treated sample was approximately 100 min. Via XRF measurements of acquired frit and DTA and TG of the frit, pigment and mixtures of both, it was noticed good compatibility in terms of thermal processes, that indicated that the pigment has a potential to be used in ceramic tiles. (author)

  13. Molecularly Imprinted Sol-Gel-Based QCM Sensor Arrays for the Detection and Recognition of Volatile Aldehydes

    Directory of Open Access Journals (Sweden)

    Chuanjun Liu

    2017-02-01

    Full Text Available The detection and recognition of metabolically derived aldehydes, which have been identified as important products of oxidative stress and biomarkers of cancers; are considered as an effective approach for early cancer detection as well as health status monitoring. Quartz crystal microbalance (QCM sensor arrays based on molecularly imprinted sol-gel (MISG materials were developed in this work for highly sensitive detection and highly selective recognition of typical aldehyde vapors including hexanal (HAL; nonanal (NAL and bezaldehyde (BAL. The MISGs were prepared by a sol-gel procedure using two matrix precursors: tetraethyl orthosilicate (TEOS and tetrabutoxytitanium (TBOT. Aminopropyltriethoxysilane (APT; diethylaminopropyltrimethoxysilane (EAP and trimethoxy-phenylsilane (TMP were added as functional monomers to adjust the imprinting effect of the matrix. Hexanoic acid (HA; nonanoic acid (NA and benzoic acid (BA were used as psuedotemplates in view of their analogous structure to the target molecules as well as the strong hydrogen-bonding interaction with the matrix. Totally 13 types of MISGs with different components were prepared and coated on QCM electrodes by spin coating. Their sensing characters towards the three aldehyde vapors with different concentrations were investigated qualitatively. The results demonstrated that the response of individual sensors to each target strongly depended on the matrix precursors; functional monomers and template molecules. An optimization of the 13 MISG materials was carried out based on statistical analysis such as principle component analysis (PCA; multivariate analysis of covariance (MANCOVA and hierarchical cluster analysis (HCA. The optimized sensor array consisting of five channels showed a high discrimination ability on the aldehyde vapors; which was confirmed by quantitative comparison with a randomly selected array. It was suggested that both the molecularly imprinting (MIP effect and the matrix

  14. Uniform Thin Films of CdSe and CdSe(ZnS) Core(shell) Quantum Dots by Sol-Gel Assembly: Enabling Photoelectrochemical Characterization and Electronic Applications

    Science.gov (United States)

    Korala, Lasantha; Wang, Zhijie; Liu, Yi; Maldonado, Stephen; Brock, Stephanie L.

    2013-01-01

    Optoelectronic properties of quantum dot (QD) films are limited by (1) poor interfacial chemistry and (2) non-radiative recombination due to surface traps. To address these performance issues, sol-gel methods are applied to fabricate thin films of CdSe and core(shell) CdSe(ZnS) QDs. High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) imaging with chemical analysis confirms that the surface of the QDs in the sol-gel thin films are chalcogen-rich, consistent with an oxidative-induced gelation mechanism in which connectivity is achieved by formation of dichalcogenide covalent linkages between particles. The ligand removal and assembly process is probed by thermogravimetric, spectroscopic and microscopic studies. Further enhancement of inter-particle coupling via mild thermal annealing, which removes residual ligands and reinforces QD connectivity, results in QD sol-gel thin films with superior charge transport properties, as shown by a dramatic enhancement of electrochemical photocurrent under white light illumination relative to thin films composed of ligand-capped QDs. A more than 2-fold enhancement in photocurrent, and a further increase in photovoltage can be achieved by passivation of surface defects via overcoating with a thin ZnS shell. The ability to tune interfacial and surface characteristics for the optimization of photophysical properties suggests that the sol-gel approach may enable formation of QD thin films suitable for a range of optoelectronic applications. PMID:23350924

  15. Investigations on electrical conductivity and dielectric properties of Na doped ZnO synthesized from sol gel method

    Energy Technology Data Exchange (ETDEWEB)

    Tabib, Asma; Sdiri, Nasr [Laboratoire de Physico-Chimie des Matériaux Minéraux et leurs Applications, Centre National de Recherches en Sciences des Matériaux, B.P. 95 Hammam-Lif, 2050 (Tunisia); Elhouichet, Habib, E-mail: habib.elhouichet@fst.rnu.tn [Laboratoire de Physico-Chimie des Matériaux Minéraux et leurs Applications, Centre National de Recherches en Sciences des Matériaux, B.P. 95 Hammam-Lif, 2050 (Tunisia); Département de Physique, Faculté des Sciences de Tunis, University Tunis El Manar, Tunis 2092 (Tunisia); Férid, Mokhtar [Laboratoire de Physico-Chimie des Matériaux Minéraux et leurs Applications, Centre National de Recherches en Sciences des Matériaux, B.P. 95 Hammam-Lif, 2050 (Tunisia)

    2015-02-15

    Highlights: • ZnO nanoparticles doped with Na were prepared from sol-gel method. • Electric conductivity and dielectric properties were investigated. • The ZnO conductivity is estimated to be of p-type for critical Na doping of 1.5% at. - Abstract: Na doped ZnO nanoparticles (NPs) were elaborated by sol gel technique. The X-ray diffraction patterns show that the peaks are indexed to the hexagonal structure without any trace of an extra phase. Electric and dielectric properties were investigated using complex impedance spectroscopy. The impedance spectra were analyzed in terms of equivalent circuits involving resistors, capacitors and constant phase elements (CPE). The contribution of grain boundary resistance to the total resistance of the system is remarkable. The AC conductivity increases with temperature following the Arrhenius law, with single apparent activation energy for conduction process. The frequency dependence of the electric conductivity follows a simple power law behavior, in according to relation σ{sub AC}(ω) = σ(0) + A ω{sup s}, where s is smaller than 1. The analysis of dc conductivity indicates that the conduction is ionic in nature. The study of its variation, at fixed temperature, with Na content shows sharp decrease which is explained by the formation of Na{sub Zn} acceptor. It was found that the dc conductivity reaches its minimum value for critical Na concentration of 1.5% at which the conductivity is estimated to be of p-type. Impedance and modulus study reveals the temperature dependent non-Debye type relaxation phenomenon. Dielectric studies revealed a promising dielectric properties (relatively high ε′ at low frequencies and low loss at high frequencies). In the low-frequency region, the values of M′ tends to zero suggesting negligible or absent electrode polarization phenomenon. The frequency dependent maxima in the imaginary modulus are found to obey to Arrhenius law.

  16. Modeling of optical absorption of silver prolate nanoparticles embedded in sol-gel glasses

    International Nuclear Information System (INIS)

    Renteria, V.M.; Garcia-Macedo, J.

    2005-01-01

    Silver prolate nanoparticles were obtained in silica gels prepared by the sol-gel process. Heating them at 900 deg. C for few minutes, the samples showed a yellow-orange color. A strong optical absorption with an asymmetric peak centred at 425 nm due to surface plasmon resonance of silver nanoparticles was observed. High-resolution transmission electron microscopy images showed silver prolate particles (average axial ratio AR = 0.76) randomly oriented with broad size distribution. The size changed from 9 to 3 nm and the prolate form changed to almost spherical (AR = 0.92) when the samples were heated longer time at 900 deg. C. In these samples, the absorption peak was shifted from 425 up to 460 nm. After heat treatment, the absorption spectrum did not change any more in some months, indicating that the particles obtained through this method are stable at room temperature. The Gans theory was used to fit the experimental spectra. The fit was not good until we assumed in the calculations all the physical features come from the system such as the volume fraction, shape and size of the metallic particles, and refractive index of the silica matrix. It was necessary to consider also a refractive index that come from oxidation on the surface of the metallic particles. With these considerations the fit with the Gans theory was good enough, and the difference between the calculated and experimental spectra was very small, factor 20 better than when oxidation is ignored. So then, the oxidation from the metallic particles must be taken in account to explain the experimental absorption spectra. These results are discussed

  17. Modeling of optical absorption of silver prolate nanoparticles embedded in sol-gel glasses

    Energy Technology Data Exchange (ETDEWEB)

    Renteria, V.M. [Departamento de Estado Solido, Instituto de Fisica, UNAM, P.O. Box 20-364, 01000 Mexico, Distrito Federal (Mexico); Garcia-Macedo, J. [Departamento de Estado Solido, Instituto de Fisica, UNAM, P.O. Box 20-364, 01000 Mexico, Distrito Federal (Mexico)]. E-mail: gamaj@fisica.unam.mx

    2005-05-15

    Silver prolate nanoparticles were obtained in silica gels prepared by the sol-gel process. Heating them at 900 deg. C for few minutes, the samples showed a yellow-orange color. A strong optical absorption with an asymmetric peak centred at 425 nm due to surface plasmon resonance of silver nanoparticles was observed. High-resolution transmission electron microscopy images showed silver prolate particles (average axial ratio AR = 0.76) randomly oriented with broad size distribution. The size changed from 9 to 3 nm and the prolate form changed to almost spherical (AR = 0.92) when the samples were heated longer time at 900 deg. C. In these samples, the absorption peak was shifted from 425 up to 460 nm. After heat treatment, the absorption spectrum did not change any more in some months, indicating that the particles obtained through this method are stable at room temperature. The Gans theory was used to fit the experimental spectra. The fit was not good until we assumed in the calculations all the physical features come from the system such as the volume fraction, shape and size of the metallic particles, and refractive index of the silica matrix. It was necessary to consider also a refractive index that come from oxidation on the surface of the metallic particles. With these considerations the fit with the Gans theory was good enough, and the difference between the calculated and experimental spectra was very small, factor 20 better than when oxidation is ignored. So then, the oxidation from the metallic particles must be taken in account to explain the experimental absorption spectra. These results are discussed.

  18. Novel cobalt releasing sol-gel derived bioactive glass for bone tissue engineering

    International Nuclear Information System (INIS)

    Oliveira, Ana Celeste Ximenes; Barrioni, Breno Rocha; Leite, Maria de Fatima; Pereira, Marivalda Magalhaes

    2016-01-01

    Full text: Bone defects are caused by traumas, congenital disorders or infections, and bone grafts are the usual treatment. However, limitations of this therapy have lead to the advance of tissue engineering approaches. Bioactive glasses (BG) are an attractive bioactive ceramic for bone repair [1], due to its osteogenic properties and capability of releasing different ions, inducing specific biological responses. Tissue repair depends also on blood vessels formation. Among angiogenic agents, cobalt ion has been regarded as strategic component to incorporate into ion releasing materials. In this study, 5% (molar) cobalt releasing BG was synthesized by sol-gel method. To characterize the material, powder samples were evaluated by FTIR and DRX. To access the cytotoxic effects, MTT and LIVE/DEAD tests were performed on osteoblasts exposed to the ionic product of the material (100 μg/mL) for 72h. FTIR analysis reveals typical absorption bands of present groups in BG. X-ray diffractogram of DRX confirmed the amorphous character of BG, without the occurrence of recrystallization of cobalt precursor, suggesting that cobalt incorporation was well succeeded. MTT test showed that cells exposed to ionic product presented high levels of metabolic activity. LIVE/DEAD assay evidenced that cell membrane integrity and intracellular esterases activity were preserved. Both cytotoxic tests proved that cobalt-BG material generated a cell friendly environment. This work shows that BG with cobalt agent presented proper structural features and a non-cytotoxic behaviour. Reference: [1] Hench LL, J Mater Sci Mater Med 17(11), 967-78 (2006). (author)

  19. Sol-Gel Derived Adsorbents with Enzymatic and Complexonate Functions for Complex Water Remediation

    Directory of Open Access Journals (Sweden)

    Roman P. Pogorilyi

    2017-09-01

    Full Text Available Sol-gel technology is a versatile tool for preparation of complex silica-based materials with targeting functions for use as adsorbents in water purification. Most efficient removal of organic pollutants is achieved by using enzymatic reagents grafted on nano-carriers. However, enzymes are easily deactivated in the presence of heavy metal cations. In this work, we avoided inactivation of immobilized urease by Cu (II and Cd (II ions using magnetic nanoparticles provided with additional complexonate (diethylene triamine pentaacetic acid or DTPA functions. Obtained nanomaterials were characterized by Fourier transform infrared spectroscopy (FTIR, thermogravimetric analysis (TGA, and scanning electron microscopy (SEM. According to TGA, the obtained Fe3O4/SiO2-NH2-DTPA nanoadsorbents contained up to 0.401 mmol/g of DTPA groups. In the concentration range Ceq = 0–50 mmol/L, maximum adsorption capacities towards Cu (II and Cd (II ions were 1.1 mmol/g and 1.7 mmol/g, respectively. Langmuir adsorption model fits experimental data in concentration range Ceq = 0–10 mmol/L. The adsorption mechanisms have been evaluated for both of cations. Crosslinking of 5 wt % of immobilized urease with glutaraldehyde prevented the loss of the enzyme in repeated use of the adsorbent and improved the stability of the enzymatic function leading to unchanged activity in at least 18 cycles. Crosslinking of 10 wt % urease on the surface of the particles allowed a decrease in urea concentration in 20 mmol/L model solutions to 2 mmol/L in up to 10 consequent decomposition cycles. Due to the presence of DTPA groups, Cu2+ ions in concentration 1 µmol/L did not significantly affect the urease activity. Obtained magnetic Fe3O4/SiO2-NH2-DTPA-Urease nanocomposite sorbents revealed a high potential for urease decomposition, even in presence of heavy metal ions.

  20. Laser sintering of doped strontium aluminate via modified sol-gel for use as a ceramic pigment

    International Nuclear Information System (INIS)

    Soares, F.M. dos S.; Valerio, M.E.G.

    2017-01-01

    Powder of Dy"3"+ co-doped SrAl_2O_4 :Eu"3"+ was produced via proteic sol-gel method, a modified sol-gel route which allows the formation of oxides at lower temperatures than other methods. CO_2 laser sintering was used as a method for heat treatment, effective in reducing trivalent europium ions in doped samples. Thermal analysis of the precursors, performed by TG and DTA, revealed that the crystallization of SrAl_2O_4 phase occurred at approximately 1060 °C. X-ray diffraction showed that the samples, before and after sintering, had monoclinic and hexagonal phases formation. DLS technique revealed the presence of nanosized and micrometric particles, and particle agglomerates, confirmed by SEM images. Micrographs of the fracture surface of a sintered pellet revealed a high degree of densification caused by heat treatment. Photoluminescence measurements showed that the samples after synthesis and before heat treatment with laser had reddish emission, composed of characteristic narrow emission lines from Eu"3"+ and more intense emission when the samples were excited at 265 nm. The laser treatment promoted the reduction of Eu"3"+ to Eu"2"+ and this effect was confirmed by the presence of a wide emission band in the green region of the spectrum with a maximum emission obtained after excitation at 350 nm. The luminescent decay time of the thermally treated sample was approximately 100 min. Via XRF measurements of acquired frit and DTA and TG of the frit, pigment and mixtures of both, it was noticed good compatibility in terms of thermal processes, that indicated that the pigment has a potential to be used in ceramic tiles. (author)

  1. Compacting and crystallisation of transparent conductive oxidic sol-gel layers as illustrated by the example of zinc oxide; Verdichtung und Kristallisation von transparenten leitfaehigen oxidischen Sol-gel-Schichten am Beispiel des Zinkoxids

    Energy Technology Data Exchange (ETDEWEB)

    Schuler, T.

    2003-07-01

    It is shown that doped zinc oxide films on glass can be obtained by a low-cost sol-gel dip coating process. The lowest possible specific resistance is 1.1x10{sup -3}ohmcm for multiple layers of aluminium-doped zinc oxide. It was shown that for thick layers the crystallite size depends on the doping of the sol, the temperature and the sintering time while the film thickness is largely defined by the concentration (viscosity) of the solution and the drawing time. On this basis, a model of the observed structures was obtained which is also applicable to other sol-gel layers. Using the process parameter p of the equation ESD = p x IKG, the morphology of multiple layers can thus be defined. The structural change from a grain structure to a layered structure was at p = 2.4 to 3 and the transition from layer structure to columnar structure at p = 1. A comparison with spray pyrolysis showed that the suggested model is also suitable as a prototype model for film growth and may possibly applied to physical coating technologies as well. The observed morphology affects the electric and optical properties of the layers, as a result of grain boundaries and compacting. With increasing compacting, the specific resistance of the layer will get lower. It was demonstrated that the coating temperature can be reduced from 550 deg C to 450 deg C without impairing conductivity by reducing the thickness of individual films. Further, possibilities were shown of improving film characteristics or reducing process time by means of other sinter technologies, e.g. pyrolytic gas flame sintering and laser sintering. The biggest problem of sol-gel coating was the segregation of dopands. For all systems, it is assumed that the dopands not converted into (optical) charge carriers will segregate on the surfaces of the crystallites and may even agglomerate into X-ray amorphous oxidic phases if dopand concentrations are high enough. In any case, potential barriers will result which slow down current

  2. Manufacture of amorphous and poly-crystalline materials with the sol-gel process; Fabricacion de materiales amorfos y policristalinos con la ruta sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Castaneda-Contreras, J. [Centro Universitario de Los Lagos, Universidad de Guadalajara, Guadalajara, Jalisco (Mexico)

    2006-01-15

    The sun-gel process is a chemical route that allows the manufacture of amorphous and poly-crystalline materials in a relatively simple way. New materials can be obtained, materials that through the traditional manufacture methods, are very difficult to obtain, such as oxide combinations (SiO{sub 2}, TiO{sub 2}, ZrO{sub 2}, etc.), and that, when being produced by traditional methods, they run the risk of being contaminated with rare earth ions or organic dyes. The unique structures, micro- structures and compounds that can be made with the sun-gel process open many possibilities for practical applications, to name a few: the manufacture of optical components, preforms for optical fibers, dielectric coatings, superconductors, waveguides, nanoparticles, solar cells, etc. [Spanish] El proceso sol-gel es una ruta quimica que permite fabricar materiales amorfos y policristalinos de forma relativamente sencilla. Se pueden obtener nuevos materiales que a traves de los metodos tradicionales de fabricacion son muy dificiles de obtener, tales como combinaciones de oxidos (SiO{sub 2}, TiO{sub 2}, ZrO{sub 2}, etc.), y que, de ser producidos por metodos tradicionales corren el riesgo de contaminarse con iones de tierras raras o colorantes organicos. Las estructuras unicas, micro estructuras y compuestos que pueden hacerse con el proceso sol-gel abren muchas posibilidades para aplicaciones practicas, por nombrar algunas, la fabricacion de componentes opticos, preformas para fibras opticas, recubrimientos dielectricos, superconductores, guias de onda, nanoparticulas, celdas solares, etc.

  3. A Review of Photocatalysts Prepared by Sol-Gel Method for VOCs Removal

    Directory of Open Access Journals (Sweden)

    Ting Ke Tseng

    2010-05-01

    Full Text Available 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.

  4. Porphyrinosilica and metalloporphyrinosilica: hybrid organic-inorganic materials prepared by sol-gel processing

    Science.gov (United States)

    Iamamoto; Sacco; Biazzotto; Ciuffi; Serra

    2000-01-01

    New materials porphyrinosilica and metalloporphyrinosilica template have been obtained by a sol-gel processing where functionalyzed porphyrins and metalloporphyrins "building blocks" were assembled into a three-dimensional silicate network. The optimized conditions for preparation of these materials are revised. The monomer precursors porphyrinopropylsilyl and metalloporphyrinopropylsilyl preparation reactions and subsequent one pot sol-gel processing with tetraethoxysilane are discussed. In the case of metalloporphyrins the nitrogen base coordinates to the central metal and acts as a template in the molecular imprinting technique. UV-visible absorption spectroscopy, thermogravimetric analysis, electron paramagnetic resonance, nuclear magnetic spectra, infrared spectra, luminescence spectra, surface area and electron spectroscopy imaging of the materials are used to characterize the prepared materials. The catalytic activities of these metalloporphyrinosilica-template are compared.

  5. Innovative Formulation Combining Al, Zr and Si Precursors to Obtain Anticorrosion Hybrid Sol-Gel Coating

    Directory of Open Access Journals (Sweden)

    Clément Genet

    2018-05-01

    Full Text Available The aim of our study is to improve the aluminium alloy corrosion resistance with Organic-Inorganic Hybrid (OIH sol-gel coating. Coatings are obtained from unusual formulation with precursors mixing: glycidoxypropyltrimethoxysilane (GPTMS, zirconium (IV propoxide (TPOZ and aluminium tri-sec-butoxide (ASB. This formulation was characterized and compared with sol formulations GPTMS/TPOZ and GPTMS/ASB. In each formulation, a corrosion inhibitor, cerium (III nitrate hexahydrate, is employed to improve the corrosion performance. Coatings obtained from sol based on GPTMS/TPOZ/ASB have good anti-corrosion performances with Natural Salt Spray (NSS resistance of 500 h for a thickness lower than 4 µm. Contact angle measurement showed a coating hydrophobic behaviour. To understand these performances, nuclear magnetic resonance (NMR analyses were performed, results make sol-gel coating condensation evident and are in very good agreement with previous results.

  6. Innovative Formulation Combining Al, Zr and Si Precursors to Obtain Anticorrosion Hybrid Sol-Gel Coating.

    Science.gov (United States)

    Genet, Clément; Menu, Marie-Joëlle; Gavard, Olivier; Ansart, Florence; Gressier, Marie; Montpellaz, Robin

    2018-05-10

    The aim of our study is to improve the aluminium alloy corrosion resistance with Organic-Inorganic Hybrid (OIH) sol-gel coating. Coatings are obtained from unusual formulation with precursors mixing: glycidoxypropyltrimethoxysilane (GPTMS), zirconium (IV) propoxide (TPOZ) and aluminium tri-sec-butoxide (ASB). This formulation was characterized and compared with sol formulations GPTMS/TPOZ and GPTMS/ASB. In each formulation, a corrosion inhibitor, cerium (III) nitrate hexahydrate, is employed to improve the corrosion performance. Coatings obtained from sol based on GPTMS/TPOZ/ASB have good anti-corrosion performances with Natural Salt Spray (NSS) resistance of 500 h for a thickness lower than 4 µm. Contact angle measurement showed a coating hydrophobic behaviour. To understand these performances, nuclear magnetic resonance (NMR) analyses were performed, results make sol-gel coating condensation evident and are in very good agreement with previous results.

  7. Enhanced optical band-gap of ZnO thin films by sol-gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Raghu, P., E-mail: dpr3270@gmail.com; Naveen, C. S.; Shailaja, J.; Mahesh, H. M., E-mail: hm-mahesh@rediffmail.com [Thin Film and Solar Cell Laboratory, Department of Electronic Science, Bangalore University, Jnanabharathi, Bangalore -560056 (India)

    2016-05-06

    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.

  8. Synthesis and Characterization of Oxide Dispersion Strengthened Ferritic Steel via a Sol-Gel Route

    International Nuclear Information System (INIS)

    Sun Qinxing; Zhang Tao; Wang Xianping; Fang Qianfeng; Hu Jing; Liu Changsong

    2012-01-01

    Nanocrystalline oxide dispersion strengthened (ODS) ferritic steel powders with nominal composition of Fe-14Cr-3W-0.3Ti-0.4Y 2 O 3 are synthesized using sol-gel method and hydrogen reduction. At low reduction temperature the impurity phase of CrO is detected. At higher reduction temperature the impurity phase is Cr 2 O 3 which eventually disappears with increasing reduction time. A pure ODS ferritic steel phase is obtained after reducing the sol-gel resultant products at 1200°C for 3 h. The HRTEM and EDS mapping indicate that the Y 2 O 3 particles with a size of about 15 nm are homogenously dispersed in the alloy matrix. The bulk ODS ferritic steel samples prepared from such powders exhibit good mechanical performance with an ultimate tensile stress of 960 MPa.

  9. Incorporation of europium III complex into nanoparticles and films obtained by the Sol-Gel methodology

    Directory of Open Access Journals (Sweden)

    Faley Jean de Sousa

    2010-03-01

    Full Text Available The sol-gel process is very effective for the preparation of new materials with potential applications in optics, sensors, catalyst supports, coatings, and specialty inorganic polymers that can be used as hosts for the accommodation of organic molecules. The low temperature employed in the process is the main advantage of this methodology. In this work, the europium (III complex with 1,10-phenantroline was prepared, and this luminescent complex was incorporated into silica nanoparticles and films by the sol-gel process. The nanoparticles were obtained by the modified Stöber methodology. The films were obtained by the dip-coating technique, at different deposition rates and numbers of layers. The nanoparticles and films were characterized by photoluminescence, thermal analysis, and Raman and infrared spectroscopies. Characterization revealed that the europium (III complex was not affected upon incorporation into the nanoparticles and films, opening a new field for the application of these materials.

  10. Sol gel based fiber optic sensor for blook pH measurement

    International Nuclear Information System (INIS)

    Grant, S. A.; Glass, R. S.

    1996-01-01

    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

  11. Porphyrinosilica and metalloporphyrinosilica: hybrid organic-inorganic materials prepared by sol-gel processing

    Directory of Open Access Journals (Sweden)

    YASSUKO IAMAMOTO

    2000-03-01

    Full Text Available New materials porphyrinosilica and metalloporphyrinosilica template have been obtained by a sol-gel processing where functionalyzed porphyrins and metalloporphyrins "building blocks" were assembled into a three-dimensional silicate network. The optimized conditions for preparation of these materials are revised. The monomer precursors porphyrinopropylsilyl and metalloporphyrinopropylsilyl preparation reactions and subsequent one pot sol-gel processing with tetraethoxysilane are discussed. In the case of metalloporphyrins the nitrogen base coordinates to the central metal and acts as a template in the molecular imprinting technique. UV-visible absorption spectroscopy, thermogravimetric analysis, electron paramagnetic resonance, nuclear magnetic spectra, infrared spectra, luminescence spectra, surface area and electron spectroscopy imaging of the materials are used to characterize the prepared materials. The catalytic activities of these metalloporphyrinosilica- template are compared.

  12. Zr alkoxide chain effect on the sol-gel synthesis of lithium metazirconate

    International Nuclear Information System (INIS)

    Pfeiffer, Heriberto; Bosch, Pedro; Bulbulian, Silvia

    2003-01-01

    Lithium metazirconate (Li 2 ZrO 3 ) was synthesized by the sol-gel method, using four different Zr alkoxides: zirconium ethoxide, zirconium iso-propoxide, zirconium propoxide and zirconium butoxide. The syntheses were made under two different catalytic regimes, acid and basic. The resulting powders were mixtures of Li 2 ZrO 3 and ZrO 2 . The best yield of Li 2 ZrO 3 (100%) was obtained when the sol-gel reaction was developed with lithium methoxide and zirconium ethoxide under acid catalysis regime. This study establishes that, for base-catalyzed reactions the ZrO 2 formation decreases when the alkyl-chain increases in the alkoxides. By contrast, for acid-catalyzed reactions the ZrO 2 formation increases as the alkyl-chain increases. Finally, when Zr propoxide and Zr iso-propoxide were used, the Li 2 ZrO 3 amounts were different due to steric effects

  13. Melting Behavior of Organic Nanocrystals Grown in Sol-gel Matrices

    International Nuclear Information System (INIS)

    Sanz, N.; Boudet, A.; Ibanez, A.

    2002-01-01

    We have characterized the thermal stability of organic nanocrystals grown in the pores of sol-gel matrices. The structure has been measured with transmission electron microscopy (TEM) analysis. Depending on the nature of organic molecules and sol-gel matrices, we have modified the dye-matrix interactions and the interfacial structure between nanocrystals and gel-glasses. When the dye-matrix interactions are weak (Van der Waals' bonds), the corresponding interfacial structure observed by TEM is sharp and the nanocrystals melt below the bulk melting point. On the other hand, when the dye-matrix interactions are strong (hydrogen bonds), the interfacial structure is fuzzy and a great superheating of organic nanocrystals is observed in comparison to the bulk melting point of the dye

  14. A sol-gel method to synthesize indium tin oxide nanoparticles

    Institute of Scientific and Technical Information of China (English)

    Xiuhua Li; Xiujuan xu; Xin Yin; Chunzhong Li; Jianrong Zhang

    2011-01-01

    Transparent conductive indium tin oxide (ITO) nanoparticles were synthesized by a novel sol-gel method.Granulated indium and tin were dissolved in HNO3 and partially complexed with citric acid.A sol-gel process was induced when tertiary butyl alcohol was added dropwise to the above solution.ITO nanoparticles with an average crystallite size of 18.5 nm and surface area of 32.6 m2/g were obtained after the gel was heat-treated at 700 C.The ITO nanoparticles showed good sinterability,the starting sintering temperature decreased sharply to 900 C,and the 1400 C sintered pellet had a density of 98.1 % of theoretical density (TD).

  15. Dissolution testing of intermediary products in uranium dioxide production by the sol-gel method

    International Nuclear Information System (INIS)

    Melichar, F.; Landspersky, H.; Urbanek, V.

    1979-01-01

    A method was developed of dissolving polyuranates and uranium dioxides in sulphuric acid and in carbonate solutions for testing intermediate products in the sol-gel process preparation of uranium dioxide. A detailed granulometric analysis of spherical particle dispersion was included as part of the tests. Two different production methods were used for the two types of studied materials. The test results show that the test method is suitable for determining temperature sensitivity of the materials to dissolution reaction. The geometrical distribution of impurities in the spherical particles can be determined from the dissolution kinetics. The method allows the determination of the effect of carbon from impurities on the process of uranium dioxide leaching and is thus applicable for testing materials prepared by the sol-gel method. (Z.M.)

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

    Science.gov (United States)

    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.

  17. Optical characterization of Er-implanted ZnO films formed by sol-gel method

    International Nuclear Information System (INIS)

    Fukudome, T.; Kaminaka, A.; Isshiki, H.; Saito, R.; Yugo, S.; Kimura, T.

    2003-01-01

    In this paper, we report on the 1.54 μm photoluminescence (PL) of Er-implanted ZnO thin films formed by a sol-gel method on Si substrates. In spite of the polycrystalline structure of the sol-gel ZnO thin films, they showed strong PL emissions due to the near band edge recombination at 375 nm as well as the Er-related luminescence at 1.54 μm. The Er-related luminescence showed no decrease (quench) in the intensity up to the Er concentration of 1.5 x 10 21 cm -3 . The PL intensity of Er-implanted ZnO at 1.54 μm was found to be as strong as Er-doped PS (porous Si) at 20 K, and the intensity reduced to 1/3 at room temperature

  18. Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

    Energy Technology Data Exchange (ETDEWEB)

    Hou Aiqin, E-mail: aiqinhou@dhu.edu.c [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China); Chen Huawei [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China)

    2010-03-15

    The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

  19. Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

    International Nuclear Information System (INIS)

    Hou Aiqin; Chen Huawei

    2010-01-01

    The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

  20. Comparative study of ZnO thin films prepared by different sol-gel route

    Directory of Open Access Journals (Sweden)

    F Esmaieli Ghodsi

    2012-03-01

    Full Text Available   Retraction Notice    The paper "Comparative study of ZnO thin films prepared by different sol-gel route" by H. Absalan and F. E. Ghodsi, which appeared in Iranian Journal of Physics Research, Vol. 11, No. 4, 423-428 (in Farsi is translation of the paper "Comparative Study of ZnO Thin Films Prepared by Different Sol-Gel Route" by F. E. Ghodsi and H. Absalan, which appeared in ACTA PHYSICA POLONICA A, Vol 118 (2010 (in English and for this reason is retracted from this journal.The corresponding author  (and also the first author is the only responsible person for this action.   

  1. Exploratory experiments on the feasibility of Th and Pu sol-gel particles

    International Nuclear Information System (INIS)

    Vanhellemont, G.; Beullens, J.; Bairiot, H.

    1965-05-01

    The sol-gel process as developed by the O.E.C.D. Dragon Project has been applied by the Plutonium Project at Mol to determine the feasibility of producing spherical particles containing Th02, Pu02 and C, in the proportions necessary to fabricate thorium-plutonium carbide kernels for irradiation specimens and for fuel cartridges for the Dragon Reactor Experiment. The process has been extended successfully to the preparation of thorium and plutonium gels, having a significant excess of carbon, with the object of evaluating the feasibility of the sol-gel process for the production of Th, C-10 type kernels. Other experiments have been performed to test the feasibility of incorporating U02 powder into the gel spheres. By using this technique, U to Th ratios of up to 9:1 have been obtained. (author)

  2. Microcontroller based instrumentation for the fuel pin preparation facility by sol-gel method

    International Nuclear Information System (INIS)

    Suhasini, B.; Prabhakar Rao, J.; Srinivas, K.C.

    2009-01-01

    The fuel pin preparation facility by Sol-Gel route has been set up at Chemistry Group at Indira Gandhi Centre for Atomic Research, Kalpakkam. Sol-Gel, a solution-gelation process involves conversion of solutions of nitrates of uranium-plutonium (at 0 deg C) into gel microspheres. To measure the exact quantities of the above solutions and to ensure their temperatures, a variety of sensors have been used at various stages in the plant. To monitor and acquire the data of process parameters used in the production and for an automated operation of the plant, a PC (master)-microcontroller (slave) based instrumentation has been developed along with acquisition software and a GU interface developed in Visual Basic. (author)

  3. Generation of amorphous ceramic capacitor coatings on titanium using a continuous sol-gel process

    International Nuclear Information System (INIS)

    Dixon, B.G.; Walsh, M.A. III; Phillips, P.G.; Morris, R.S.

    1995-01-01

    Thin amorphous films of ceramic capacitor materials were successfully deposited using sol-gel chemistry onto titanium wire using a continuous, computer controlled process. By repeatedly depositing and calcining very thin layers of material, smooth and even coats can be produced. Surface analyses revealed the layered nature of these thin coats, as well as the amorphous nature of the ceramic. The electrical properties of the better coatings, all composed of niobium, bismuth, zinc oxides, were then evaluated. copyright 1995 Materials Research Society

  4. Sol-gel derived bioactive coating on zirconia: Effect on flexural strength and cell proliferation.

    Science.gov (United States)

    Shahramian, Khalil; Leminen, Heidi; Meretoja, Ville; Linderbäck, Paula; Kangasniemi, Ilkka; Lassila, Lippo; Abdulmajeed, Aous; Närhi, Timo

    2017-11-01

    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 (TiO 2 ) coating, zirconia with sol-gel derived zirconia (ZrO 2 ) 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 TiO 2 coated and ZrO 2 coated groups (5.7 and 5.4, respectively) were lower than the control (8.0). Specimens coated with ZrO 2 showed significantly lower fibroblast proliferation compared to other groups (p sol-gel derived coatings have no influence on the flexural strength of zirconia. ZrO 2 coated specimens showed significantly lower cell proliferation after 12 days than TiO 2 coated or non-coated control. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 2401-2407, 2017. © 2016 Wiley Periodicals, Inc.

  5. Processing of non-oxide ceramics from sol-gel methods

    Science.gov (United States)

    Landingham, Richard; Reibold, Robert A.; Satcher, Joe

    2014-12-12

    A general procedure applied to a variety of sol-gel precursors and solvent systems for preparing and controlling homogeneous dispersions of very small particles within each other. Fine homogenous dispersions processed at elevated temperatures and controlled atmospheres make a ceramic powder to be consolidated into a component by standard commercial means: sinter, hot press, hot isostatic pressing (HIP), hot/cold extrusion, spark plasma sinter (SPS), etc.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-01

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

  7. In situ ion-beam analysis and modification of sol-gel zirconia thin films

    International Nuclear Information System (INIS)

    Levine, T.E.; Mayer, J.W.

    1995-01-01

    We report the investigation of ion-beam-induced densification of sol-gel zirconia thin films via in situ ion backscattering spectrometry. We have irradiated three regions of a sample with neon, argon, and krypton ions. For each ion species, a series of irradiation and analysis steps were performed using an interconnected 3 MV tandem accelerator. The technique offers the advantages of minimizing the variation of experimental parameters and sequentially monitoring the densification phenomenon with increasing ion dose

  8. Vapor phase modification of sol-gel derived titania (TiO{sub 2}) surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Piwonski, Ireneusz [University of Lodz, Department of Chemical Technology and Environmental Protection, Pomorska 163, 90-236 Lodz (Poland)]. E-mail: irek@uni.lodz.pl; Ilik, Aneta [University of Lodz, Department of Chemical Technology and Environmental Protection, Pomorska 163, 90-236 Lodz (Poland)

    2006-12-30

    Chemical vapor deposition (CVD) method was used in titania surface modification. Titania layers were obtained in sol-gel process and prepared as thin films on silicon wafers in dip-coating method. In order to define the influence of modification on titania surface properties (e.g., friction), various types of fluoroalkylsilanes were used. The effectiveness of the modification was monitored by FT-IR spectroscopy. The topography and frictional measurements were investigated with the use of atomic force microscopy (AFM)

  9. Performance of the sol-gel method for the preparation of optical fibers

    Czech Academy of Sciences Publication Activity Database

    Matějec, Vlastimil; Hayer, Miloš; Mrázek, Jan; Kašík, Ivan; Podrazký, Ondřej; Pospíšilová, Marie

    2007-01-01

    Roč. 52, č. 10 (2007), s. 991-998 ISSN 0035-3930. [Physical Chemistry Conference ROMPHYSCHEM /12./. Bucharest, 06.09.2006-08.09.2006] R&D Projects: GA ČR GA102/05/0956 Institutional research plan: CEZ:AV0Z20670512 Keywords : sol-gel processing * optical fibres * chemical sensors Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 0.262, year: 2007

  10. Fabrications and properties of doped porous polysiloxane sol-gel layers on optical fibers

    Czech Academy of Sciences Publication Activity Database

    Berková, Daniela; Sedlář, Miroslav; Matějec, Vlastimil; Kašík, Ivan; Chomát, Miroslav; Abdelghani, A.; Jaffrezic-Renault, N.; Lacroix, M.

    1998-01-01

    Roč. 13, 1/3 (1998), s. 569-573 ISSN 0928-0707. [Glasses, Ceramics, Hybrids and Nanocomposites from Gels - SOL-GEL'97 /9./. Sheffield, 31.08.1997-05.09.1997] R&D Projects: GA ČR GA102/95/0871; GA ČR GA102/96/0939 Keywords : nonelectric sensing devices * optical fibres Subject RIV: JB - Sensors, Measurment, Regulation Impact factor: 1.526, year: 1997

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

    Science.gov (United States)

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

    2009-10-01

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

  12. Sol-gel synthesis of 45S5 bioglass – Prosthetic coating by electrophoretic deposition

    Directory of Open Access Journals (Sweden)

    Faure Joel

    2013-11-01

    Full Text Available In this work, the 45S5 bioactive glass has been prepared by the sol-gel process using an organic acid catalyst instead of nitric acid usually used. The physico-chemical and structural characterizations confirmed and validated the elemental composition of the resulting glass. In addition, the 45S5 bioactive glass powder thus obtained was successfully used to elaborate by electrophoretic deposition a prosthetic coating on titanium alloy Ti6Al4V.

  13. Microstructure of Zirconia-Based Sol-Gel Glasses Studied by SANS

    Czech Academy of Sciences Publication Activity Database

    Ryukhtin, Vasyl; Strunz, Pavel; Kopitsa, G. P.; Ezdakova, K. V.; Gubanova, N. N.; Ivanov, V. K.; Baranchikov, A. Y.; Angelov, Borislav; Feoktistov, A.; Pipich, V.; Levinský, P.

    2015-01-01

    Roč. 128, č. 4 (2015), s. 582-584 ISSN 0587-4246. [ISPMA 13 - 13th INTERNATIONAL SYMPOSIUM ON PHYSICS OF MATERIALS. Praha, 31.08.2014 - 04.09.2014] R&D Projects: GA ČR GB14-36566G; GA MŠk LM2011019 Institutional support: RVO:61389013 ; RVO:61389005 Keywords : sol-gel method * SANS * USANS Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.525, year: 2015

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

    Science.gov (United States)

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

    1983-01-01

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

  15. Development of novel sol-gel indicators (SGI's) for in-situ environmental measurements

    International Nuclear Information System (INIS)

    Livingston, R.R.; Wicks, G.G.; Baylor, L.C.; Whitaker, M.J.

    1993-01-01

    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

  16. Sol-gel-derived mesoporous silica films with low dielectric constants

    Energy Technology Data Exchange (ETDEWEB)

    Seraji, S.; Wu, Yun; Forbess, M.; Limmer, S.J.; Chou, T.; Cao, Guozhong [Washington Univ., Seattle, WA (United States). Dept. of Materials Science and Engineering

    2000-11-16

    Mesoporous silica films with low dielectric constants and possibly closed pores have been achieved with a multiple step sol-gel processing technique. Crack-free films with approximately 50% porosity and 0.9 {mu}m thicknesses were obtained, a tape-test revealing good adhesion between films and substrates or metal electrodes. Dielectric constants remained virtually unchanged after aging at room temperature at 56% humidity over 6 days. (orig.)

  17. Diffusion structural analysis study of titania films deposited by sol-gel technique on silica glass

    Czech Academy of Sciences Publication Activity Database

    Balek, V.; Mitsuhashi, T.; Bountseva, I.M.; Haneda, H.; Málek, Z.; Šubrt, Jan

    2003-01-01

    Roč. 26, 1-3 (2003), s. 185-189 ISSN 0928-0707. [International Workshop on Glasses, Ceramics, Hybrids and Nanocomposites from Gels /11./. Abano Terme, 16.09.2001-21.09.2001] Institutional research plan: CEZ:AV0Z4032918 Keywords : titania film * diffusion structural analysis * sol-gel Subject RIV: CA - Inorganic Chemistry Impact factor: 1.546, year: 2003

  18. Electrochemical behaviour of ceramic yttria stabilized zirconia on carbon steel synthesized via sol-gel process

    International Nuclear Information System (INIS)

    Crespo, M.A. Dominguez; Murillo, A. Garcia; Torres-Huerta, A.M.; Yanez-Zamora, C.; Carrillo-Romo, F. de J

    2009-01-01

    Chromate conversion coatings have been widely applied for the corrosion of different metallic substrates. However, the waste containing Cr 6+ has many limitations due to the environmental consideration and health hazards. An interesting alternative seems to be the deposition on metallic surface of thin layers of yttria or zirconia or both by the sol-gel process. In this study, Ytttria and Yttria stabilized zirconia (YSZ, 8% Y 2 O 3 ) thin films were used for coating commercial carbon steel substrates by sol-gel method and the dip-coating process. The evolution of organic compounds up to crystallization process as a function of heat treatments was study by FT-IR spectroscopy. The structure and morphology of the coatings were analysed using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The anticorrosion performance of the coatings has been evaluated by using electrochemical techniques in an aggressive media (3.5 wt.% NaCl). The corrosion behaviour of sol-gel method was compared with traditional chromate conversion coatings. Differences in the electrochemical behaviour of YSZ coatings are related to the development of microcracks during the sintering process and to the presence of organic compounds during growth film. Electrochemical results showed that sol-gel YSZ and Y 2 O 3 coatings can act as protective barriers against wet corrosion; however yttria films displayed low adhesion to substrate. The corrosion parameters provide an explanation of the role of each film and show a considerable increase in the corrosion resistance for coated samples in comparison to the bare steel samples.

  19. Electrochemical behaviour of ceramic yttria stabilized zirconia on carbon steel synthesized via sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Crespo, M.A. Dominguez, E-mail: mdominguezc@ipn.m [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Murillo, A. Garcia; Torres-Huerta, A.M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Yanez-Zamora, C. [Estudiante del postgrado en Tecnologia Avanzada del CICATA-IPN, Unidad Altamira, km 14.5, Carr. Tampico-Puerto Industrial. C.P. 89600, Altamira, Tamaulipas (Mexico); Carrillo-Romo, F. de J [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico)

    2009-08-26

    Chromate conversion coatings have been widely applied for the corrosion of different metallic substrates. However, the waste containing Cr{sup 6+} has many limitations due to the environmental consideration and health hazards. An interesting alternative seems to be the deposition on metallic surface of thin layers of yttria or zirconia or both by the sol-gel process. In this study, Ytttria and Yttria stabilized zirconia (YSZ, 8% Y{sub 2}O{sub 3}) thin films were used for coating commercial carbon steel substrates by sol-gel method and the dip-coating process. The evolution of organic compounds up to crystallization process as a function of heat treatments was study by FT-IR spectroscopy. The structure and morphology of the coatings were analysed using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The anticorrosion performance of the coatings has been evaluated by using electrochemical techniques in an aggressive media (3.5 wt.% NaCl). The corrosion behaviour of sol-gel method was compared with traditional chromate conversion coatings. Differences in the electrochemical behaviour of YSZ coatings are related to the development of microcracks during the sintering process and to the presence of organic compounds during growth film. Electrochemical results showed that sol-gel YSZ and Y{sub 2}O{sub 3} coatings can act as protective barriers against wet corrosion; however yttria films displayed low adhesion to substrate. The corrosion parameters provide an explanation of the role of each film and show a considerable increase in the corrosion resistance for coated samples in comparison to the bare steel samples.

  20. Acquisition of a Scanning Ultrasound Analyzer for Gelation and Drying Studies in Sol-Gel Ceramic Coatings and Monoliths

    National Research Council Canada - National Science Library

    Archer, Lynden

    1997-01-01

    The overall goal of this research project was to develop a fundamental understanding of how colloid chemistry influences structure and properties of ceramic monoliths fabricated by sol-gel synthesis...