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Sample records for sol-gel surface preparation

  1. 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

  2. Special Advanced Studies for Pollution Prevention. Delivery Order 0017: Sol-Gel Surface Preparation for Carbon Steel and Stainless Steel Bonding

    National Research Council Canada - National Science Library

    Zheng, Haixing

    1997-01-01

    The objective of this program is to study the feasibility of using sol-gel active alumina coatings for the surface preparation of carbon steel and stainless steel for adhesive bonding, and to optimize...

  3. Zirconium titanate thin film prepared by surface sol-gel process and effects of thickness on dielectric property

    CERN Document Server

    Kim, C H

    2002-01-01

    Single phase of multicomponent oxide ZrTiO sub 4 film could be prepared through surface sol-gel route simply by coating the mixture of 100mM zirconium butoxide and titanium butoxide on Pt/Ti/SiO sub 2 /Si(100) substrate, following pyrolysis at 450 .deg. C, and annealing it at 770 .deg. C. The dielectric constant of the film was reduced as the film thickness decreased due to of the interfacial effects caused by layer/electrode and a few voids inside the multilayer. However, the dielectric property was independent of applied dc bias sweeps voltage (-2 to +2 V). The dielectric constant of bulk film, 31.9, estimated using series-connected capacitor model was independent of film thickness and frequency in the measurement range, but theoretical interfacial thickness, t sub i , was dependent on the frequency. It reached a saturated t sub i value, 6.9 A, at high frequency by extraction of some capacitance component formed at low frequency range. The dielectric constant of bulk ZrTiO sub 4 pellet-shaped material was 3...

  4. 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)

  5. Fabrication and characterisation of selective solar absorber surfaces prepared by sol-gel technique

    CSIR Research Space (South Africa)

    Katumba, G

    2006-07-01

    Full Text Available characterization: The near normal spectral hemispherical reflect- ance, R, of the prepared samples was measured in the wavelength interval 0.3 to 20.0 μm1 using a Lambda 900 spec- trophotometer and a Bomem-Michel- son 110 FTIR spectrometer. Solar ab...

  6. Photocatalytic Activity in CH3CN Related to the Surface Properties of TiO2 Powders Prepared by Sol-Gel Method

    OpenAIRE

    Bettoni, Marta; Candori, Pietro; Marmottini, Fabio; Perenze, Nicoletta; Rol, Cesare; Sebastiani, Giovanni V.; Vecchiocattivi, Franco

    2009-01-01

    Some TiO2 powders, prepared from titanium(IV)tetraisopropoxide by the sol-gel method and thermally treated between 100 and 1000∘C, have been characterized by X-ray powder diffraction and by nitrogen adsorption and desorption at 77 K to calculate the BET-specific surface area, from which the micropore volume and the external surface area can be derived. The photocatalytic activity (ka) of the above powders has been evaluated considering the TiO2-sensitized photo-oxidation of 4-methoxybenzyl al...

  7. 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

  8. Photocatalytic Activity in CH3CN Related to the Surface Properties of TiO2 Powders Prepared by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Marta Bettoni

    2009-01-01

    Full Text Available Some TiO2 powders, prepared from titanium(IVtetraisopropoxide by the sol-gel method and thermally treated between 100 and 1000∘C, have been characterized by X-ray powder diffraction and by nitrogen adsorption and desorption at 77 K to calculate the BET-specific surface area, from which the micropore volume and the external surface area can be derived. The photocatalytic activity (ka of the above powders has been evaluated considering the TiO2-sensitized photo-oxidation of 4-methoxybenzyl alcohol in CH3CN as the test reaction. The decrease of ka have been related to the decrease of the BET surface area, the micropore volume, and the external surface area of the TiO2 powders, but a satisfactory linear correlation is observed only for the last superficial parameter.

  9. 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.

  10. 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.

  11. 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.

  12. Adsorption characteristics, recognition properties, and preliminary application of nordihydroguaiaretic acid molecularly imprinted polymers prepared by sol-gel surface imprinting technology

    Science.gov (United States)

    Liao, Sen; Zhang, Wen; Long, Wei; Hou, Dan; Yang, Xuechun; Tan, Ni

    2016-02-01

    In this paper, a new core-shell composite of nordihydroguaiaretic acid (NDGA) molecularly imprinted polymers layer-coated silica gel (MIP@SiO2) was prepared through sol-gel technique and applied as a material for extraction of NDGA from Ephedra. It was synthesized using NDGA as the template molecule, γ-aminopropyltriethoxysilane (APTS) and methyltriethoxysilane (MTEOS) as the functional monomers, tetraethyl orthosilicate (TEOS) as the cross-linker and ethanol as the porogenic solvent in the surface of silica. The non-imprinted polymers layer-coated silica gel (NIP@SiO2) were prepared with the same procedure, but with the absence of template molecule. In addition, the optimum adsorption affinity occurred when the molar ratio of NDGA:APTS:MTEOS:TEOS was 1:6:2:80. The prepared MIP@SiO2 and NIP@SiO2 were analyzed by scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and Fourier transform-infrared spectroscopy (FT-IR). Their affinity properties to NDGA were evaluated through dynamic adsorption, static adsorption, and selective recognition experiments, and the results showed the saturated adsorption capacity of MIP@SiO2 could reach to 5.90 mg g-1, which was two times more than that of NIP@SiO2. High performance liquid chromatography (HPLC) was used to evaluate the extraction of NDGA from the medicinal plant ephedra by the above prepared materials, and the results indicated that the MIP@SiO2 had potential application in separation of the natural active component NDGA from medicinal plants.

  13. 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

  14. 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.

  15. 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.

  16. Innovative Sol-Gel Routes for the Bottom-up Preparation of Heterogeneous Catalysts.

    Science.gov (United States)

    Debecker, Damien P

    2017-12-11

    Heterogeneous catalysts can be prepared by different methods offering various levels of control on the final properties of the solid. In this account, we exemplify bottom-up preparation routes that are based on the sol-gel chemistry and allow to tailor some decisive properties of solid catalysts. First, an emulsion templating strategy is shown to lead to macrocellular self-standing monoliths with a macroscopic 3D structure. The latter can be used as catalyst or catalyst supports in flow chemistry, without requiring any subsequent shaping step. Second, the aerosol-assisted sol-gel process allows for the one-step and continuous production of porous mixed oxides. Tailored textural properties can be obtained together with an excellent control on composition and homogeneity. Third, the application of non-hydrolytic sol-gel routes, in the absence of water, leads to mixed oxides with outstanding textural properties and with peculiar surface chemistry. In all cases, the resulting catalytic performance can be correlated with the specificities of the preparation routes presented. This is exemplified in catalytic reactions in the fields of biomass conversion, petro chemistry, enantioselective organic synthesis, and air pollution mitigation. © 2017 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. 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)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  19. 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.

  20. 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.

  1. Surface modification of quartz fibres for dental composites through a sol-gel process.

    Science.gov (United States)

    Wang, Yazi; Wang, Renlin; Habib, Eric; Wang, Ruili; Zhang, Qinghong; Sun, Bin; Zhu, Meifang

    2017-05-01

    In this study, quartz fibres (QFs) surface modification using a sol-gel method was proposed and dental posts reinforced with modified QFs were produced. A silica sol (SS) was prepared using tetraethoxysilane (TEOS) and 3-methacryloxypropyltrimethoxysilane (γ-MPS) as precursors. The amount of γ-MPS in the sol-gel system was varied from 0 to 24wt.% with a constant molar ratio of TEOS, ethanol, deionized water, and HCl. Thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), and contact angle (CA) measurements were used to characterize the modified QFs, which confirmed that SS had successfully coated the surface of QFs. SEM images showed good interfacial bonding between the modified QFs and the resin matrix. The results of three-point bending tests of the fibre reinforced composite (FRC) posts showed that the QFs modified by SS with 12wt.% γ-MPS presented the best mechanical properties, demonstrating improvements of 108.3% and 89.6% for the flexural strength and flexural modulus, respectively, compared with untreated QFs. Furthermore, the sorption and solubility of the prepared dental posts were also studied by immersing the posts in artificial saliva (AS) for 4weeks, and yielded favourable results. This sol-gel surface modification method promises to resolve interfacial bonding issues of fibres with the resin matrix, and produce FRC posts with excellent properties. Copyright © 2017. Published by Elsevier B.V.

  2. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. 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.

  4. Thermal properties and water repellency of cotton fabric prepared through sol-gel method

    Directory of Open Access Journals (Sweden)

    Gu Jia-Li

    2016-01-01

    Full Text Available Cotton fabrics were treated by one-step sol-gel method. The pure silica hydrosol and phosphorus-doped hydrosol were prepared with the addition of a hydrophobic hexadecyltrimethoxysilane to decrease the surface energy of cotton fabric. The thermal properties and water repellency of treated cotton fabric were characterized by thermo-gravimetric analysis, micro combustion, limiting oxygen index, and contact angle measurement. The results showed that cotton fabric treated by phosphorus-doped silica hydrosol had excellent flame retardance, and the water repellence was apparently improved with the addition of hexadecyltrimethoxysilane.

  5. Surface analysis and biocorrosion properties of nanostructured surface sol-gel coatings on Ti6Al4V titanium alloy implants.

    Science.gov (United States)

    Advincula, Maria C; Petersen, Don; Rahemtulla, Firoz; Advincula, Rigoberto; Lemons, Jack E

    2007-01-01

    Surfaces of biocompatible alloys used as implants play a significant role in their osseointegration. Surface sol-gel processing (SSP), a variant of the bulk sol-gel technique, is a relatively new process to prepare bioreactive nanostructured titanium oxide for thin film coatings. The surface topography, roughness, and composition of sol-gel processed Ti6Al4V titanium alloy coatings was investigated by atomic force microscopy (AFM) and X-ray electron spectroscopy (XPS). This was correlated with corrosion properties, adhesive strength, and bioreactivity in simulated body fluids (SBF). Electroimpedance spectroscopy (EIS) and polarization studies indicated similar advantageous corrosion properties between sol-gel coated and uncoated Ti6Al4V, which was attributed to the stable TiO2 composition, topography, and adhesive strength of the sol-gel coating. In addition, inductive coupled plasma (ICP) and scanning electron microscopy with energy dispersive spectrometry (SEM-EDS) analysis of substrates immersed in SBF revealed higher deposition of calcium and phosphate and low release rates of alloying elements from the sol-gel modified alloys. The equivalent corrosion behavior and the definite increase in nucleation of calcium apatite indicate the potential of the sol-gel coating for enhanced bioimplant applications. 2006 Wiley Periodicals, Inc.

  6. Influence of silane on the structure of polystyrene prepared by sol-gel coatings via UV curing

    Directory of Open Access Journals (Sweden)

    Balbay Senay

    2017-01-01

    Full Text Available Light, heat, oxygen, moisture, ozone, atmospheric pollution and biological effects are the most important effectives wreak to chemical degradation in the polymer structure. In result of chemical degradation on the polymer consist of problems such as discoloration, brittleness, surface cracks, perspiration, crumbling, smell, surface acidity. In this work, it is aimed to improve the problem of the polystyrene (PS material against chemical degradation. For this reason, PS is coated with silica sol-gel hybrid coating. Silica sol-gel was synthesized by using vinyltrimethoxysilane (VTMS as a cross-linker and tetraethylorthosilicate (TEOS as a silica source. Firstly, four different pre-treatment technique (oven, vacuum oven, lyophilizer and freezing was studied to determine the most suitable pre-treatment technique for coating on PS substrate of sol-gel prepared with initial formulation (S1. A freezing technique gave the best results for coating sample. The change of surface colour of coated PS was measured by CIE L*a*b* methods. Secondly, the most suitable curing agent (Irgacure 184, Irgacure 819, Darocur 1173 and TiO2 as crystalline anatase phase was determined to coat the sol-gel on PS. It was determined to the lowest yellowing of PS surface hybrid coated as UV curing of TEOS sol modified by VTMS and TiO2 as photo-initiators. Finally, the chemical and morphological structure of the coated PS samples was determined by FT-IR and SEM instruments, respectively.

  7. 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.

  8. 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...

  9. Preparation of Natural Rubber (NR) Based Nano-Sized Materials Using Sol-Gel Technique

    International Nuclear Information System (INIS)

    Dahlan Mohd; Mahathir Mohamed

    2011-01-01

    The objectives of this project are to prepare nano-sized natural rubber-based hybrid coating material by sol-gel technique; to explore the possibility of producing ENR-Si (epoxidized natural rubber-silica) cramer with toughening effects; and to use it in radiation curing of surface coating. Since early 1960s Malaysia has introduced various forms of value-added natural rubber such as Standard Malaysian Rubber (SMR), methylmethacrylate-grafted natural rubber (MG rubber), followed by liquid natural rubber and epoxidized natural rubber (ENR). Products such as liquid epoxidized natural rubber acrylate (LENRA) and thermoplastic natural rubber (TPNR) are still on-going research projects in Nuclear Malaysia. The former has strong possibility to be used as radiation-sensitive comparabilities in TPNR blends, besides its original purpose for example in radiation curing of surface coating. But earlier findings indicated that, to make it (as for surface coating) more effective, reinforcement system is needed to be introduced. Strong candidate is silica by sol-gel technique, since common reinforcement filler for example carbon black has drawbacks in this particular case. This technique was introduced in late 1960s to produce metal oxides such as silica and titanium oxides in solution. (author)

  10. 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

  11. 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.

  12. Fabrication of hydrophobic compressed oil palm trunk surface by sol-gel process

    Science.gov (United States)

    Muzakir, Syafiqah; Salim, Nurjannah; Huda Abu Bakar, Nurul; Roslan, Rasidi; Sin, Lim Wan; Hashim, Rokiah

    2018-04-01

    Improvement of the robustness of hydrophobic surfaces is crucial to achieving commercial applications of these surfaces in such various areas as self-cleaning, water repellency and corrosion resistance. Compressed oil palm trunk (OPT) panel is one of potential product which can be used as panelling and indoor furniture application. By adding hydrophobic properties to compressed oil palm trunk panel might increase the application of compressed oil palm trunk especially for outdoor application. In this study, fabrication is using the sol-gel technique. Sol-gel was prepared by adding ethanol with Hexadecyl Trimethyl Ammonium Bromide (CTAB) solution with Tetraethyl Orthosilicate (TEOS) with surface modification of chlorotrimethylsilane (CTMS). The surface with hydrophobic coating was undergone surface analysis with contact angle machine with the aid of software SCA 20 and the determined of the morphology of surface with scanning electron microscope (SEM). The produced compressed oil palm trunk surfaces exhibited promising hydrophobic properties with a contact angle of 104° and the relatively better mechanical robustness.

  13. 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.

  14. Preparation of ZrW{sub 2}O{sub 8} xerogel and aerogels by sol-gel chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Noailles, L.; Dunn, B.; Larson, D. [Dept. of Materials Science and Engineering, Univ. of California, Los Angeles, CA (United States); Starkovich, J.; Peng, H. [Northrop Grumman Space Technology, Redondo Beach, CA (United States)

    2004-07-01

    Xerogels and aerogels with the composition ZrW{sub 2}O{sub 8} have been synthesized using sol-gel chemistry. For the xerogel, trigonal phase is formed at 650 C and the cubic phase forms above 1100 C in less than 30 seconds. Aerogels have been prepared with an average pore diameter of 110 Aa and a surface area of 510 m{sup 2}g{sup -1}. (orig.)

  15. Comparison of the redox activities of sol-gel and conventionally prepared Bi-Mo-Ti mixed oxides

    Energy Technology Data Exchange (ETDEWEB)

    Wildberger, M.; Grundwaldt, J.D.; Mallat, T.; Baiker, A. [Lab. of Technical Chemistry, Swiss Federal Inst. of Technology, ETH-Zentrum, Zuerich (Switzerland)

    1998-12-31

    Novel sol-gel Bi-Mo-Ti oxides have been prepared and characterized by XRD, XPS, FT-Raman and HRTEM. The surface Bi{sup 3+} and Mo{sup 6+} species of some xerogels and an aerogel could be reduced and oxidized at room temperature, whereas the conventionally prepared reference materials were not reduced by H{sub 2} below 300 C. The unusual redox properties, under very mild conditions, are likely due to the unique morphology of Bi-Mo-oxides stabilized by titania. During butadiene oxidation to furan at above 400 C to sol-gel mixed oxides restructured considerably and their performance was barely better than that of titania-supported Bi-Mo oxides. (orig.)

  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. Modification of Ti6Al4V implant surfaces by biocompatible TiO{sub 2}/PCL hybrid layers prepared via sol-gel dip coating: Structural characterization, mechanical and corrosion behavior

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, Michelina, E-mail: michelina.catauro@unina2.it [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 21, 81031 Aversa (Italy); Bollino, Flavia [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 21, 81031 Aversa (Italy); Giovanardi, Roberto; Veronesi, Paolo [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Vivarelli 10, 41125 Modena (Italy)

    2017-05-01

    Surface modification of metallic implants is a promising strategy to improve tissue tolerance, osseointegration and corrosion resistance of them. In the present work, bioactive and biocompatible organic-inorganic hybrid coatings were prepared using a sol-gel dip coating route. They consist of an inorganic TiO{sub 2} matrix in which different percentages of poly(ε-caprolactone) (PCL), a biodegradable and biocompatible polymer, were incorporated. The coatings were used to modify the surface of Ti6Al4V substrates in order to improve their wear and corrosion resistance. The chemical structure of the coatings was analyzed by attenuated total reflectance (ATR) Fourier transform infrared (FTIR) spectroscopy. Coating microstructure, mechanical properties and ability to inhibit the corrosion of the substrates were evaluated as a function of the PCL amount. Scanning electron microscopy (SEM) showed that the polymer allows to obtain crack-free coatings, but when high percentages were added uncoated areas appear. Nano-indentation tests revealed that, as expected, surface hardness and elastic modulus decrease as the percentage of polymeric matrix increases, but scratch testing demonstrated that the coatings are effective in preventing scratching of the underlying metallic substrate, at least for PCL contents up to 20 wt%. The electrochemical tests (polarization curves acquired in order to evaluate the corrosion resistance) allowed to asses that the coatings have a significant effect in term of corrosion potential (E{sub corr}) but they do not significantly affect the passivation process that titanium undergoes in contact with the test solution used (modified Dulbecco's phosphate-buffered saline or DPBS). - Highlights: • Bioactive TiO{sub 2}/PCL hybrid coatings on Ti6Al4V were prepared via sol-gel dip coating. • Hybrid coatings are crack-free but when 50 wt% PCL was added, uncoated areas appear. • Coating hardness and elastic modulus decrease as the PCL percentage

  18. 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.

  19. 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

  20. Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

    Energy Technology Data Exchange (ETDEWEB)

    Abdullah, M. A. R., E-mail: ameerridhwan89@gmail.com; Mamat, M. H., E-mail: hafiz-030@yahoo.com; Ismail, A. S., E-mail: kyrin-samaxi@yahoo.com [NANO-ElecTronic Centre (NET), Faculty of Electrical Engineering, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor (Malaysia); Malek, M. F., E-mail: firz-solarzelle@yahoo.com [NANO-SciTech Centre (NST), Institute of Science (IOS), Universiti Teknologi MARA - UiTM, 40450 Shah Alam, Selangor (Malaysia); Alrokayan, Salman A. H., E-mail: dr.salman@alrokayan.com; Khan, Haseeb A., E-mail: khan-haseeb@yahoo.com [Chair of Targeting and Treatment of Cancer Using Nanoparticles, Deanship of Scientific Research, King Saud University (KSU), Riyadh 11451 (Saudi Arabia); Rusop, M., E-mail: rusop@salam.uitm.my [NANO-ElecTronic Centre (NET), Faculty of Electrical Engineering, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor (Malaysia); NANO-SciTech Centre (NST), Institute of Science (IOS), Universiti Teknologi MARA - UiTM, 40450 Shah Alam, Selangor (Malaysia)

    2016-07-06

    Preparation of NiO thin films at different annealing temperature by sol-gel method was conducted to synthesize the quality of the surface thin films. The effects of annealing temperature on the surface topology were systematically investigated. Our studies confirmed that the surface roughness of the thin films was increased whenever annealing temperature was increase. NiO thin films morphology structure analysis was confirmed by field emission scanning electron microscope. Surface roughness of the thin films was investigated by atomic force microscopy.

  1. Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

    International Nuclear Information System (INIS)

    Abdullah, M. A. R.; Mamat, M. H.; Ismail, A. S.; Malek, M. F.; Alrokayan, Salman A. H.; Khan, Haseeb A.; Rusop, M.

    2016-01-01

    Preparation of NiO thin films at different annealing temperature by sol-gel method was conducted to synthesize the quality of the surface thin films. The effects of annealing temperature on the surface topology were systematically investigated. Our studies confirmed that the surface roughness of the thin films was increased whenever annealing temperature was increase. NiO thin films morphology structure analysis was confirmed by field emission scanning electron microscope. Surface roughness of the thin films was investigated by atomic force microscopy.

  2. 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.   

  3. Excimer laser processing of ZnO thin films prepared by the sol-gel process

    International Nuclear Information System (INIS)

    Winfield, R.J.; Koh, L.H.K.; O'Brien, Shane; Crean, Gabriel M.

    2007-01-01

    ZnO thin films were prepared on soda-lime glass from a single spin-coating deposition of a sol-gel prepared with anhydrous zinc acetate [Zn(C 2 H 3 O 2 ) 2 ], monoethanolamine [H 2 NC 2 H 4 OH] and isopropanol. The deposited films were dried at 50 and 300 deg. C. X-ray analysis showed that the films were amorphous. Laser annealing was performed using an excimer laser. The laser pulse repetition rate was 25 Hz with a pulse energy of 5.9 mJ, giving a fluence of 225 mJ cm -2 on the ZnO film. Typically, five laser pulses per unit area of the film were used. After laser processing, the hexagonal wurtzite phase of zinc oxide was observed from X-ray diffraction pattern analysis. The thin films had a transparency of greater than 70% in the visible region. The optical band-gap energy was 3.454 eV. Scanning electron microscopy and profilometry analysis highlighted the change in morphology that occurred as a result of laser processing. This comparative study shows that our sol-gel processing route differs significantly from ZnO sol-gel films prepared by conventional furnace annealing which requires temperatures above 450 deg. C for the formation of crystalline ZnO

  4. 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)

  5. 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.

  6. Preparation and characterization of sol-gel derived TiO2 films

    International Nuclear Information System (INIS)

    Hong, Y.J.; Brungs, M.P.; Chaplin, R.P.; Sizgek, E.

    2001-01-01

    Crack-free transparent titania films have been prepared through a new sol-gel process combined with hydrogen peroxide treatment. Hydrogen peroxide and HCl were used to dissolve amorphous titania powder which is obtained by drying common sol-gel titania sol. The peroxo-titania sol produced a thicker film than the common sol-gel titania sol due to a higher degree of condensation. Film thickness could be further increased by controlled drying conditions of the amorphous titania powder or 'aging' the sol. Polyethylene glycol (PEG) and chemical additives were effective in controlling condensation rate by preventing rapid condensation during curing of the film. When these two components were incorporated, it was possible to create a 0.5μm transparent film and PEG could also control the porosity of the film. The cured film was analysed by XRD and Raman spectroscopy. In order to measure the reflective index and thickness of the titania film, an ellipsometer was used. Copyright (2001) The Australian Ceramic Society

  7. Sol gel synthesis for preparation of yttrium aluminium garnet

    NARCIS (Netherlands)

    Vrolijk, J.W.G.A.; Willems, J.W.M.M.; Metselaar, R.; With, de G.; Terpstra, R.A.; Metselaar, R.

    1989-01-01

    Sol-gel—synthesis for preparation of pure yttrium aluminium garnet powder with small grain size is subject of this ongoing study. Starting materials were sulfates and chlorides of yttrium and aluminium. To obtain pure YAG (Y3A1SO1Z) pH during hydrolysis as well as temperature during calcination and

  8. 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

  9. 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.

  10. 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.

  11. Chirality of Single-Handed Twisted Titania Tubular Nanoribbons Prepared Through Sol-gel Transcription.

    Science.gov (United States)

    Wang, Sibing; Zhang, Chuanyong; Li, Yi; Li, Baozong; Yang, Yonggang

    2015-08-01

    Single-handed twisted titania tubular nanoribbons were prepared through sol-gel transcription using a pair of enantiomers. Handedness was controlled by that of the template. The obtained samples were characterized using field-emission electron microscopy, transmission electron microscopy, diffuse reflectance circular dichroism (DRCD), and X-ray diffraction. The DRCD spectra indicated that the titania nanotubes exhibit optical activity. Although the tubular structure was destroyed after being calcined at 700 °C for 2.0 h, DRCD signals were still identified. However, the DRCD signals disappeared after being calcined at 1000 °C for 2.0 h. The optical activity of titania was proposed to be due to chiral defects. Previous results showed that straight titania tubes could be used as asymmetric autocatalysts, indicating that titania exhibit chirality at the angstrom level. Herein, it was found that they also exhibit DRCD signals, indicating that there are no obvious relationships between morphology at the nano level and chirality at the angstrom level. The nanotube chirality should originate from the chiral defects on the nanotube inner surface. The Fourier transform infrared spectra indicated that the chirality of the titania was transferred from the gelators through the hydrogen bonding between N-H and Ti-OH. © 2015 Wiley Periodicals, Inc.

  12. Mullite fibres preparation by aqueous sol-gel process and activation energy of mullitization

    International Nuclear Information System (INIS)

    Tan Hongbin; Ding Yaping; Yang Jianfeng

    2010-01-01

    Mullite fibres were prepared by sol-gel process using aluminum carboxylates (ACs) and silica sol. ACs was synthesized from dissolving aluminum powder in a mixture of formic acid and oxalic acid using aluminum chloride hexahydrate as catalyst. A molar ratio of 1:2:1 for aluminum, formic acid and oxalic acid was optimized to obtain clear solution and viscous ACs sol for fibres synthesis. Thermogravimetry-differential scanning calorimetry (TG-DSC), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM) analysis were used to characterize the properties of the gel and ceramic fibres. The gel fibres completely transformed to mullite at 1200 o C, with a smooth surface and uniform diameter. The activation energy for mullite formation in precursor gel fibres was determined by means of differential thermal analysis. The value obtained, E a = 741.4 kJ/mol, was lower than most data reported in the literatures, which was attributed to the silica-alumina micro-phase separation when organic acids decomposed during gel fibres heating.

  13. 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)

  14. Phase Composition of Samarium Niobate and Tantalate Thin Films Prepared by Sol-Gel Method

    Science.gov (United States)

    Bruncková, H.; Medvecký, Ľ.; Múdra, E.; Kovalčiková, A.; Ďurišin, J.; Šebek, M.; Girman, V.

    2017-12-01

    Samarium niobate SmNbO4 (SNO) and tantalate SmTaO4 (STO) thin films ( 100 nm) were prepared by sol-gel/spin-coating process on alumina substrates with PZT interlayer and annealing at 1000°C. The precursors of films were synthesized using Nb or Ta tartrate complexes. The improvement of the crystallinity of monoclinic M'-SmTaO4 phase via heating was observed through the coexistence of small amounts of tetragonal T-SmTa7O19 phase in STO precursor at 1000°C. The XRD results of SNO and STO films confirmed monoclinic M-SmNbO4 and M'-SmTaO4 phases, respectively, with traces of orthorhombic O-SmNbO4 (in SNO). In STO film, the single monoclinic M'-SmTaO4 phase was revealed. The surface morphology and topography of thin films were investigated by SEM and AFM analysis. STO film was smoother with roughness 3.2 nm in comparison with SNO (6.3 nm). In the microstructure of SNO film, small spherical ( 50 nm) and larger cuboidal particles ( 100 nm) of the SmNbO4 phase were observed. In STO, compact clusters composed of fine spherical SmTaO4 particles ( 20-50 nm) were found. Effect of samarium can contribute to the formation different polymorphs of these films for the application to environmental electrolytic thin film devices.

  15. Hybrid manganese oxide films for supercapacitor application prepared by sol-gel technique

    International Nuclear Information System (INIS)

    Chen, Chin-Yi; Wang, Sheng-Chang; Tien, Yue-Han; Tsai, Wen-Ta; Lin, Chung-Kwei

    2009-01-01

    Hybrid films were prepared by adding various concentrations of meso-carbon microbeads (MCMB) during sol-gel processing of manganese oxide films. The heat-treated films were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). In addition, electrochemical performance of the MCMB-added Mn-oxide hybrid coatings was evaluated by cyclic voltammetry (CV) and compared with its unadded counterpart. Experimental results showed that Mn-oxide films exhibited a mixture of Mn 2 O 3 and Mn 3 O 4 phases. The higher the heat-treatment temperature, the more Mn 2 O 3 can be observed. The specific capacitance of the unadded Mn-oxide electrodes is 209 F/g. Because the MCMB particles provide more interfacial surface area for electrochemical reactions, a significant improvement can be noticed by adding MCMB in Mn-oxide coatings. The 300 o C heat-treated hybrid Mn-oxide coating with a Mn/MCMB ratio of 10/1 exhibits the highest value of 350 F/g, showing a ∼ 170% increase in specific capacitance.

  16. 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.

  17. Surface functionalization of carbon nanofibers by sol-gel coating of zinc oxide

    Energy Technology Data Exchange (ETDEWEB)

    Shao Dongfeng [Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi 214122 (China); Changzhou Textile Garment Institute, Changzhou 213164 (China); Wei Qufu [Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi 214122 (China)], E-mail: qfwei@jiangnan.edu.cn; Zhang Liwei; Cai Yibing; Jiang Shudong [Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi 214122 (China)

    2008-08-15

    In this paper the functional carbon nanofibers were prepared by the carbonization of ZnO coated PAN nanofibers to expand the potential applications of carbon nanofibers. Polyacrylonitrile (PAN) nanofibers were obtained by electrospinning. The electrospun PAN nanofibers were then used as substrates for depositing the functional layer of zinc oxide (ZnO) on the PAN nanofiber surfaces by sol-gel technique. The effects of coating, pre-oxidation and carbonization on the surface morphology and structures of the nanofibers were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM), respectively. The results of SEM showed a significant increase of the size of ZnO nanograins on the surface of nanofibers after the treatments of coating, pre-oxidation and carbonization. The observations by SEM also revealed that ZnO nanoclusters were firmly and clearly distributed on the surface of the carbon nanofibers. FTIR examination also confirmed the deposition of ZnO on the surface of carbon nanofibers. The XRD analysis indicated that the crystal structure of ZnO nanograins on the surface of carbon nanofibers.

  18. Magnetic properties of Co-Ni alloy nanoparticles prepared by the sol-gel technique

    International Nuclear Information System (INIS)

    Sangregorio, C.; Fernandez, C. de Julian; Battaglin, G.; De, G.; Gatteschi, D.; Mattei, G.; Mazzoldi, P.

    2004-01-01

    The magnetic properties of Co, Ni and Co x Ni 1-x alloy nanoparticles with different composition (0 < x < 1), prepared by the sol-gel route, were investigated. ZFC and FC magnetization measurements show that the blocking temperature increases with the Co content, while a maximum in the anisotropy constant was found for x=0.7. Room temperature FMR measurements, suggest that in samples with larger Co content (x≥0.66) interparticle interactions play a relevant role in determining their magnetic properties

  19. Magnetic properties of Co-Ni alloy nanoparticles prepared by the sol-gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Sangregorio, C. E-mail: claudio.sangregorio@unifi.it; Fernandez, C. de Julian; Battaglin, G.; De, G.; Gatteschi, D.; Mattei, G.; Mazzoldi, P

    2004-05-01

    The magnetic properties of Co, Ni and Co{sub x}Ni{sub 1-x} alloy nanoparticles with different composition (0 < x < 1), prepared by the sol-gel route, were investigated. ZFC and FC magnetization measurements show that the blocking temperature increases with the Co content, while a maximum in the anisotropy constant was found for x=0.7. Room temperature FMR measurements, suggest that in samples with larger Co content (x{>=}0.66) interparticle interactions play a relevant role in determining their magnetic properties.

  20. 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.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  2. Composite coating prepared by micro-arc oxidation followed by sol-gel process and in vitro degradation properties

    International Nuclear Information System (INIS)

    Zhang Yi; Bai Kuifeng; Fu Zhenya; Zhang Caili; Zhou Huan; Wang Liguo; Zhu Shijie; Guan Shaokang; Li Dongsheng; Hu Junhua

    2012-01-01

    A Mg phosphate coating was prepared on home-developed Mg-Zn-Ca alloy to improve its anticorrosion performance in simulated body fluid (SBF, Kokubo solution). The coating was prepared by micro-arc oxidation (MAO) method at the working voltage of 120-140 V. Evident improvement of anticorrosion was obtained even through the surface was porous. To further diminish the contact with SBF, a TiO 2 layer was coated on the porous MAO layer by sol-gel dip coating followed by an annealing treatment. The coatings were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy dispersion spectroscopy (EDS). The electrochemical performance of the MAO and TiO 2 /MAO coated alloys was evaluated by anodic polarization measurements. The pores on Mg phosphate layer provided accommodation sites for the subsequent TiO 2 sol-gel coating which sealed the pores and hence significantly enhanced the anticorrosion while single MAO coating only improve anticorrosion within a limited range. The present result indicates that fabrication of composite coatings is a significant strategy to improve the corrosion resistance of Mg-Zn-Ca alloy and other alloys, thus enhancing the potential of using Mg alloys as bio-implants.

  3. 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.

  4. 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.

  5. 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.

  6. Properties of Zn O/Cr thin films prepared by Sol-Gel; Propiedades de peliculas delgadas ZnO/Cr preparadas por Sol-Gel

    Energy Technology Data Exchange (ETDEWEB)

    Tirado G, S.; Olvera A, R., E-mail: tirado@esfm.ipn.mx [IPN, Escuela Superior de Fisica y Matematicas, Edificio 9, Unidad Profesional A. L. M., San Pedro Zacatenco, 07788 Mexico D. F. (Mexico)

    2014-08-15

    Zn O films and those superficially modified with chromium were deposited on substrates of soda-lime glass, using the Sol-Gel process and the repeated immersion method. Starting from dehydrated zinc acetate was prepared a solution to 0.6 M to ambient temperature in 2-methoxyethanol and monoethanolamine (Mea) stirring magnetically. The Sol was prepared with an aging to seven days and was used to grow a films group with thickness to eight immersions. These same films were superficially modified with several depositions of a chromium nitrate Sol dissolved in ethanol to low concentration. The Zn O films were structurally characterized by X-ray diffraction, its chemical composition by energy dispersive X-ray spectroscopy and its morphology by scanning electron microscopy and atomic force microscopy, as well as their optical properties by UV-vis. Of the obtained results are proposed possible applications. (author)

  7. Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

    Science.gov (United States)

    Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

    2014-01-01

    In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x Ag = 0.5 are effective against E. coli and S. aureus after 24 h. PMID:24523630

  8. Antimicrobial activity of thin solid films of silver doped hydroxyapatite prepared by sol-gel method.

    Science.gov (United States)

    Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

    2014-01-01

    In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x(Ag) = 0.5 are effective against E. coli and S. aureus after 24 h.

  9. Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Simona Liliana Iconaru

    2014-01-01

    Full Text Available In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM with energy Dispersive X-ray attachment (X-EDS, Fourier transform infrared spectroscopy (FT-IR, and glow discharge optical emission spectroscopy (GDOES. These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with xAg=0.5 are effective against E. coli and S. aureus after 24 h.

  10. Preparation of mesoporous silica microparticles by sol-gel/emulsion route for protein release.

    Science.gov (United States)

    Vlasenkova, Mariya I; Dolinina, Ekaterina S; Parfenyuk, Elena V

    2018-04-06

    Encapsulation of therapeutic proteins into particles from appropriate material can improve both stability and delivery of the drugs, and the obtained particles can serve as a platform for development of their new oral formulations. The main goal of this work was development of sol-gel/emulsion method for preparation of silica microcapsules capable of controlled release of encapsulated protein without loss of its native structure. For this purpose, the reported in literature direct sol-gel/W/O/W emulsion method of protein encapsulation was used with some modifications, because the original method did not allow to prepare silica microcapsules capable for protein release. The particles were synthesized using sodium silicate and tetraethoxysilane as silica precursors and different compositions of oil phase. In vitro kinetics of bovine serum albumin (BSA) release in buffer (pH 7.4) was studied by Fourier transform infrared (FTIR) and fluorescence spectrometry, respectively. Structural state of encapsulated BSA and after release was evaluated. It was found that the synthesis conditions influenced substantially the porous structure of the unloaded silica particles, release properties of the BSA-loaded silica particles and structural state of the encapsulated and released protein. The modified synthesis conditions made it possible to obtain the silica particles capable of controlled release of the protein during a week without loss of the protein native structure.

  11. Preparation and characterization of strontium-fluorapatite nanopowders by sol-gel method

    Science.gov (United States)

    Kamaei, Maryam; Fathi, Mohammad Hossein

    2018-01-01

    Biomaterials based on calcium orthophosphate are especially attractive for use in medicine, for bone and teeth implants due to their biological properties, such as biocompatibility and bioactivity. Among them, hydroxyapatite (HAP; Ca10(PO4)6(OH)2) is used particularly because of its similarities to the inorganic component of bone. Hydroxyapatite has been widely used for biomedical applications. Despite desirable properties such as bioactivity, biocompatibility, solubility and adsorption, synthetic HA is limited in application due to poor thermostability and poor mechanical properties. Properties of HA can be tailored over a wide range by incorporating different ions into HA lattice. Use of the sol-gel technique is technically simple, cost effective and beneficial for fabrication biomaterials. This research aimed to prepare and characterize Sr-doped FA nanopowders (Sr-FA). Sr-FA with different Sr contents was prepared by sol-gel method. The designated degree of substitution of Ca by Sr in the mixture was determined by the x value in the general formula of (Ca10-x Srx(PO4)6F2), where x=0,0.5,1. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques were utilized to characterize the obtained nano powders. Results showed that Sr ions entered into the fluorapatite lattice and occupied Ca sites. The incorporation of Sr ions into the fluorapatite resulted in the increase of the lattice parameters.

  12. Sol-gel prepared active ternary oxide coating on titanium in cathodic protection

    Directory of Open Access Journals (Sweden)

    VLADIMIR V. PANIC

    2007-12-01

    Full Text Available The characteristics of a ternary oxide coating, on titanium, which consisted of TiO2, RuO2 and IrO2 in the molar ratio 0.6:0.3:0.1, calculated on the metal atom, were investigated for potential application for cathodic protection in a seawater environment. The oxide coatings on titanium were prepared by the sol gel procedure from a mixture of inorganic oxide sols, which were obtained by forced hydrolysis of metal chlorides. The morphology of the coating was examined by scanning electron microscopy. The electrochemical properties of activated titanium anodes were investigated by cyclic voltammetry and polarization measurements in a H2SO4- and NaCl-containing electrolyte, as well as in seawater sampled on the Adriatic coast in Tivat, Montenegro. The anode stability during operation in seawater was investigated by the galvanostatic accelerated corrosion stability test. The morphology and electrochemical characteristics of the ternary coating are compared to that of a sol-gel-prepared binary Ti0.6Ru0.4O2 coating. The activity of the ternary coating was similar to that of the binary Ti0.6Ru0.4O2 coating in the investigated solutions. However, the corrosion stability in seawater is found to be considerably greater for the ternary coating.

  13. Preparation and characterization of quercetin-loaded silica microspheres stabilized by combined multiple emulsion and sol-gel processes

    Directory of Open Access Journals (Sweden)

    Kim Young Ho

    2015-01-01

    Full Text Available Despite exhibiting a wide spectrum of cosmeceutical properties, flavonoids and related compounds have some limitations related to their stability and solubility in distilledwater. In this project, we prepared silica microspheres using a novel method that uses polyol-in-oil-in-water (P/O/W emulsion and sol-gel methods as techniques for stabilizing quercetin. A stable microsphere suspension was successfully preparedusing a mixed solvent system comprising a polyol-phase medium for performing the sol-gel processing of tetraethyl orthosilicate (TEOS as an inorganic precursor with outer water phase. The morphology of the microsphere was evaluated using a scanning electron microscope (SEM, which showed a characteristic spherical particle shape with a smooth surface. Furthermore, SEM/EDSanalysis of a representative microsphere demonstrated that the inner structure of the silica microspheres was filled with quercetin. The mean diameter of the microsphere was in the range 20.6-35.0 μm, and the encapsulation efficiency ranged from 17.8% to 27.5%. The free and encapsulated quercetin samples were incubated in separateaqueous solutions at 25 and 42°C for 28 days. The residualcontent of the quercetin encapsulated by silica microspheres was 82% at 42°C. In contrast, that of the free quercetin stored at 42°C decreased to ~24%.

  14. 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.

  15. Preparation, microstructure and properties of yttrium aluminum garnet fibers prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Li Chengshun [Key Laboratory for Liquid Structure and Heredity of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Zhang Yujun [Key Laboratory for Liquid Structure and Heredity of Materials of Ministry of Education, Shandong University, Jinan 250061 (China)], E-mail: yujunzhangcn@sdu.edu.cn; Gong Hongyu; Zhang Jingde; Nie Lifang [Key Laboratory for Liquid Structure and Heredity of Materials of Ministry of Education, Shandong University, Jinan 250061 (China)

    2009-01-15

    Yttrium aluminum garnet (YAG) fiber was prepared by sol-gel method using water as the solvent. The spinnable YAG sol was synthesized using Al powder, Y(CH{sub 3}COOH){sub 3}.4H{sub 2}O and HCl as precursors, polyethylene oxide as viscosity adjusting agent. Gel fibers with diameter of 5-10 {mu}m were prepared from the YAG sol by using centrifugal spinning technique. YAG crystalline fibers were obtained by drying gel fibers and heat-treating at selected temperature. TG/DTA analysis showed an exotherm at 906 deg. C attributed to formation of YAG phase and weight loss of 45% at 1000 deg. C. XRD and FT-IR analysis showed that phase-pure YAG can be formed at 900 deg. C, and no other intermediate was observed. The grain size of YAG fibers increased from 25 to 220 nm and tensile strength decreased rapidly from 970 to 380 MPa when the sintering temperature increased from 900 to 1550 deg. C.

  16. Characterizations of maghemite thin films prepared by a sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Lau, L. N., E-mail: lau7798@gmail.com; Ibrahim, N. B., E-mail: baayah@ukm.edu.my [School of Applied Physics, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor. Malaysia (Malaysia)

    2015-09-25

    Iron is one of the abundant elements of Mother Nature and its compound, iron oxide is an interesting material to study since its discovery in the form of magnetite. It can exist in many phases such as hematite and maghemite, this unique nature has put it as a potential candidate in various applications. The aim of this work is to study the influence of different precursor concentrations on the microstructural and magnetic properties of iron oxide thin film. All samples were prepared via the sol-gel method followed by a spin coating technique on quartz substrates. Iron oxide films were confirmed as maghemite phase from X-ray diffraction patterns. The film morphology was examined by a field emission scanning electron microscope and it showed non-systematic value of average grain size and film thickness throughout the study. Hysteresis loop further confirmed that maghemite is a magnetic material when it was characterized by a vibrating sample magnetometer. The coercivity did not show any correlation with molarity. Nevertheless, it increased as the precursor concentration of the film increased due to the domain behaviour. In conclusion, maghemite thin films were successfully synthesized by the sol-gel method with different precursor concentrations in this work.

  17. Sol-gel Process in Preparation of Organic-inorganic Hybrid Materials

    Directory of Open Access Journals (Sweden)

    Macan, J

    2008-07-01

    Full Text Available Organic-inorganic hybrid materials are a sort of nanostructured material in which the organic and inorganic phases are mixed at molecular level. The inorganic phase in hybrid materials is formed by the sol-gel process, which consists of reactions of hydrolysis and condensation of metal (usually silicon alkoxides. Flexibility of sol-gel process enables creation of hybrid materials with varying organic and inorganic phases in different ratios, and consequently fine-tuning of their properties. In order to obtain true hybrid materials, contact between the phases should be at molecular level, so phase separation between thermodynamically incompatible organic and inorganic phases has to be prevented. Phase interaction can be improved by formation of hydrogen or covalent bonds between them during preparation of hybrid materials. Covalent bond can be introduced by organically modified silicon alkoxides containing a reactive organic group (substituent capable of reacting with the organic phase. In order to obtain hybrid materials with desired structures, a detailed knowledge of hydrolysis and condensation mechanism is necessary. The choice of catalyst, whether acid or base, has the most significant influence on the structure of the inorganic phase. Other important parameters are alkoxide concentration, water: alkoxide ratio, type of alkoxide groups, solvent used, temperature, purity of chemicals used, etc. Hydrolysis and condensation of organically modified silicon alkoxides are additionally influenced by nature and size of the organic supstituent.

  18. Preparation Of Porous And Dense Bodies From Hydroxyapatite Powders Prepared Via Sol-Gel Technique

    International Nuclear Information System (INIS)

    Sopyan, Lis

    2001-01-01

    Hydroxyapatite (HA) ceramics is clinically proven and, thus, a reliable material for medical applications, that is, for use in dental and orthopedical surgery to fill cavities in bones. In this paper, we report a preliminary study on development of HA porous and dense materials manufactured using fine HA powders prepared via a sol-gel technique. In the preparation of HA porous bodies, slurries of the as-prepared powder were prepared with an adjusted loading ofHA, using Duramax of 0-3021 type as dispersant. After soaking cellulosic sponges into the slurry, the sponges were dried and then subjected to heat-treatment at 600 o C, followed by sintering at 1250 o C for I h. The apparent density of the porous bodies is 1.290 g/cm 3 , with a porosity of 59%. The sintering shrinkage is about 20% (in respect of dimension) and 44 % (in respect of volume). Morphological evaluation of the porous bodies showed that the samples contained macropores of 1-2 mm diameter and micropores of 1-2 μm diameter. The measurement of mechanical strength provided 1.31 ± 0.30 MPa. Subsequently, dense samples were prepared from the as-prepared powder. In this case, the powder was mixed with poly(vinyl alcohol) and distilled water to make a slurry. The mixture was mixed using Zirconia balls as the crusher for 2h. The suspension was then spray-dried, and well-dispersed powder was obtained. The powder was compressed uniaxially using cold pressing technique at 800 kglcm2 and the pellets obtained were sintered in air at : 250 o C for I h. The sintered dense bodies have apparent density of 2.855 g/cm 3 , with a 10% porosity. The flexural strength of the dense bodies measured on the specimens of riimension 2 mm x 2.5 mm gave rise to the considerable value of 57.7 MPa

  19. Characterization of composites prepared by sol-gel process through positrons lifetime spectroscopy

    International Nuclear Information System (INIS)

    Sousa, Edesia M.B. de; Magalhaes, Welligton F. de; Mohallem, Nelcy D.S.

    1996-01-01

    Si O 2 matrix were prepared by sol-gel method using TEOS, ethanol and H 2 O in a 1/3/10 mol ratio, with HCl and HF as catalysts. This silica gels were doped with copper and titanium adding Cu Cl and titanium tetra-iso-prop oxide in the starting solution, during agitation. The samples were prepared in monolithic shape, were dried at 110 deg C for 24 hours and thermally treated for 2 hours at 500, 900 and 1100 deg C. The structural evolution was studied y x-ray diffraction, mercury porosimetry and pycnometry. In this work, it was also used the Position Annihilation Lifetime Spectroscopy which have been used, nowadays, as a microscopic probe in order to investigate the free volume in zeolites, polymers and metallic alloy. All the samples have shown a stable pore structure until 900 deg C and a strong densification process at 1100 deg C. (author)

  20. Formation and characterization of vitreous materials prepared by the sol-gel technique

    International Nuclear Information System (INIS)

    Martinez, J.R.; Ruiz, J.F.; Cruz M, J.A. de la; Villasenor G, P.

    1999-01-01

    A full process of preparation and characterization of silica gel, which can be implemented in a experimental course for undergraduate laboratories is presented. Samples of silica gel and sol-gel derived SiO 2 films on glass substrates were fabricated and characterized using atomic force microscopy, Raman and Infrared absorption techniques. Raman and Infrared spectroscopy were used to analyze the local structure. The microstructure characteristics of the films, fabricated by dip-coating, were monitored using atomic force microscopy. The samples were prepared from alcoholic solutions of tetraethylortosilicate (TEOS) keeping the H 2 O/TEOS and Et-OH/TEOS molar ratios constant and equal to 11.66 and 4 respectively. (Author)

  1. Properties of Zn O/Cr thin films prepared by Sol-Gel

    International Nuclear Information System (INIS)

    Tirado G, S.; Olvera A, R.

    2014-08-01

    Zn O films and those superficially modified with chromium were deposited on substrates of soda-lime glass, using the Sol-Gel process and the repeated immersion method. Starting from dehydrated zinc acetate was prepared a solution to 0.6 M to ambient temperature in 2-methoxyethanol and monoethanolamine (Mea) stirring magnetically. The Sol was prepared with an aging to seven days and was used to grow a films group with thickness to eight immersions. These same films were superficially modified with several depositions of a chromium nitrate Sol dissolved in ethanol to low concentration. The Zn O films were structurally characterized by X-ray diffraction, its chemical composition by energy dispersive X-ray spectroscopy and its morphology by scanning electron microscopy and atomic force microscopy, as well as their optical properties by UV-vis. Of the obtained results are proposed possible applications. (author)

  2. Preparation of UO2 dense spherical particles by sol-gel technique

    International Nuclear Information System (INIS)

    Urbanek, V.; Dolezal, J.

    1977-01-01

    The results of the basic research and development of processes of preparation of dense UO 2 spherical particles by sol-gel technique are presented. Attention was paid to the study of chemistry of internal gelation step in the uranylnitrate-urea-hexamethylentetramine system. The existence regions of several stable gels with different properties were established in connection with variable ratio of basic gel's components and the appropriate ''Phase diagrams'' were drawn. From these diagrams, two of the most interesting types of uranyl gels were chosen for the subsequent thermal processing which included drying, reduction and sintering. The detailed studies of each step of the whole process enabled preparation of UO 2 dense spheres with well defined microstructure

  3. Luminescence of Eu(3+) doped SiO2 Thin Films and Glass Prepared by Sol-gel Technology

    Science.gov (United States)

    Castro, Lymari; Jia, Weiyi; Wang, Yanyun; Santiago, Miguel; Liu, Huimin

    1998-01-01

    Trivalent europium ions are an important luminophore for lighting and display. The emission of (5)D0 to (7)F2 transition exhibits a red color at about 610 nm, which is very attractive and fulfills the requirement for most red-emitting phosphors including lamp and cathode ray phosphorescence materials. Various EU(3+) doped phosphors have been developed, and luminescence properties have been extensively studied. On the other hand, sol-gel technology has been well developed by chemists. In recent years, applications of this technology to optical materials have drawn a great attention. Sol-gel technology provides a unique way to obtain homogeneous composition distribution and uniform doping, and the processing temperature can be very low. In this work, EU(3+) doped SiO2 thin films and glasses were prepared by sol-gel technology and their spectroscopic properties were investigated.

  4. Preparation and Optoelectrical Properties of p-CuO/n-Si Heterojunction by a Simple Sol-Gel Method

    Science.gov (United States)

    He, Bo; Xu, Jing; Ning, Huanpo; Zhao, Lei; Xing, Huaizhong; Chang, Chien-Cheng; Qin, Yuming; Zhang, Lei

    The Cuprous oxide (CuO) thin film was prepared on texturized Si wafer by a simple sol-gel method to fabricate p-CuO/n-Si heterojunction photoelectric device. The novel sol-gel method is very cheap and convenient. The structural, optical and electrical properties of the CuO film were studied by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), X-ray photoelectron spectroscopy (XPS), UV-Vis spectrophotometer and Hall effect measurement. A good nonlinear rectifying behavior is obtained for the p-CuO/n-Si heterojunction. Under reverse bias, good photoelectric behavior is obtained.

  5. Optical ph sensing material prepared from doped sol-gel film for use in acid-base titration

    Directory of Open Access Journals (Sweden)

    Musa Ahmad

    2017-11-01

    Full Text Available An optical pH sensing material has been prepared in this study by using sol-gel technique. Bromothymol blue, bromophenol blue and thymol blue were chosen in this study as acidbase indicators for strong acid-strong base, strong acid-weak base and weak acid-strong base titration, respectively. The results show that these indicators could be successfully entrapped inside the sol-gel film and still maintain its chemical behaviour as in solution. The entrapped acid-base indicators respond well to any pH changes and could be used to determine the end-point of the acid-base titration.

  6. Optical ph sensing material prepared from doped sol-gel film for use in acid-base titration

    OpenAIRE

    Musa Ahmad; T.W. Tan

    2017-01-01

    An optical pH sensing material has been prepared in this study by using sol-gel technique. Bromothymol blue, bromophenol blue and thymol blue were chosen in this study as acidbase indicators for strong acid-strong base, strong acid-weak base and weak acid-strong base titration, respectively. The results show that these indicators could be successfully entrapped inside the sol-gel film and still maintain its chemical behaviour as in solution. The entrapped acid-base indicators respond well to ...

  7. 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

  8. 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.

  9. Thermal behavior of La2O3/Nio composite prepared by sol-gel method

    International Nuclear Information System (INIS)

    Sakallioglu, M.

    2005-01-01

    The La 2 O 3 /NiO composite was prepared by sol-gel method by using transition metal oxides (La 2 O 3 /NiO). The variation of specific heat capacity Cp with temperature for La2O3/NiO composite was investigated by DSC. The heat capacity curve was taken with a heating rate of 20 degrees/min between 0-100 degrees. The variation of specific heat capacity was found by PKI Muse Standard Analysis Program. The thermal stability of the La 2 O 3 /NiO composite was investigated by thermogravimetric analysis (TG) in air atmosphere at a heating rate of 20 degrees/min. The weight loss of La 2 O 3 /NiO composite was determined by the variation of temperature

  10. Judd-Ofelt Analysis of Dy3+-Activated Aluminosilicate Glasses Prepared by Sol-Gel Method

    Science.gov (United States)

    Sengthong, Buonyavong; Van Tuyen, Ho; An, Nguyen Thi Thai; Van Do, Phan; Hai, Nguyen Thi Quy; Chau, Pham Thi Minh; Quang, Vu Xuan

    2018-04-01

    Aluminosilicate (AS) glasses doped with different Dy3+ concentrations were synthesized via sol-gel method. Absorption, photoluminescence spectra and lifetime of this material have been studied. From analytical results of absorption spectra, the Judd-Ofelt (JO) parameters of prepared samples have been determined. These JO parameters combined with photoluminescence spectra have been used to evaluate transition probabilities ( A R), branching ratios ( β) and the calculated oscillator strengths of AS:Dy3+ glasses. The radiative branching ratio of 4F9/2 → 6H13/2 transition has a minimum value at 62.2% for β R which predicts that this transition in AS:Dy3+ glasses can give rise to lasing action. JO parameters show that the Ω2 increases with the increasing of Dy3+ ion concentration due to the increased polarizability of the average coordination medium and decreased average symmetry.

  11. Preparation and characterization of ultra-thin sol-gel films

    International Nuclear Information System (INIS)

    Shapiro, Leora; Marx, Sharon; Mandler, Daniel

    2007-01-01

    The formation and characterization of nanometer thick sol-gel films are reported. The films were prepared by spin-coating of a diluted solution of a silane precursor on a number of different substrates. The effect of dilution, rotation speed and nature of substrate on the thickness and homogeneity of the films was examined. Characterization of the films was carried out by profilometry, reflectance spectroscopy, atomic force microscopy, adhesion test and electrochemistry. We find that the dilution factor has a pronounced effect on the film thickness. Moreover, the time of dilution, namely, whether dilution was carried out before or after a period of hydrolysis, has a noticeable effect on the thickness as well as on the permeability of embedded species

  12. RBS and NRA of cobalt oxide thin films prepared by the sol-gel process

    International Nuclear Information System (INIS)

    Andrade, E.; Huerta, L.; Pineda, J.C.; Zavala, E.P.; Barrera, E.; Rocha, M. F.; Vargas, C.A.

    2001-01-01

    This work presents a study of cobalt oxide thin films produced by the sol-gel process on aluminum and glass substrates. These films have been analyzed using two ion beam analysis (IBA) techniques: a) a standard RBS 4 He 2 MeV and b) nuclear reaction analysis (NRA) using a 1 MeV deuterium beam. The 12 C(d,p 0 ) 13 C nuclear reaction provides information that carbon is incorporated into the film structure, which could be associated to the sinterization film process. Other film measurements such as optical properties, XRD, and SEM were performed in order to complement the IBA analysis. The results show that cobalt oxide film coatings prepared by this technique have good optical properties as solar absorbers and potential uses in solar energy applications

  13. A sol-gel method for preparing ZnO quantum dots with strong blue emission

    International Nuclear Information System (INIS)

    Chen Zhong; Li Xiaoxia; Du Guoping; Chen Nan; Suen, Andy Y.M.

    2011-01-01

    ZnO quantum dots (QDs) with strong blue emission have been successfully synthesized by sol-gel method, and their crystal structures, sizes, and photoluminescence properties were characterized by X-ray diffractometer, scanning electron microscope, and ultraviolet-visible spectroscopy. It has been found that ZnO QDs had a hexagonal wurtzite crystal structure, and their average diameter was about 16.0-32.2 nm. Both the reaction time and temperature were found to have a strong influence on the average size and photoluminescence properties of ZnO QDs. Longer reaction time and higher reaction temperature resulted in larger average size for ZnO QDs. It has been shown that at reaction temperature 60 deg. C the emission intensity for ZnO QDs increased first with reaction time before 7 h and then decreased after 7 h. For the same reaction time 7 h, ZnO QDs synthesized at 60 deg. C showed the strongest emission intensity. It was found that annealing in nitrogen, vacuum, and air all resulted in an increase of the size of ZnO QDs and a reduction in their photoluminescence. The dependence of the size and properties of ZnO QDs on the reaction parameters as well as the annealing conditions has been discussed. - Highlights: → ZnO quantum dots (QDs) with strong blue emission were prepared by sol-gel method. → ZnO QDs had a pure spectral blue with the chromaticity coordinates (0.166, 0.215). → Optimal reaction time and temperature were 7 h and 60 deg. C, respectively.

  14. Combining inkjet printing and sol-gel chemistry for making pH-sensitive surfaces.

    Science.gov (United States)

    Orsi, Gianni; De Maria, Carmelo; Montemurro, Francesca; Chauhan, Veeren M; Aylott, Jonathan W; Vozzi, Giovanni

    2015-01-01

    Today biomedical sciences are experiencing the importance of imaging biological parameters with luminescence methods. Studying 2D pH distribution with those methods allows building knowledge about complex cellular processes. Immobilizing pH sensitive nanoparticles inside hydrogel matrixes, in order to guarantee a proper SNR, could easily make stable and biocompatible 2D sensors. Inkjet printing is also well known as tool for printing images onto porous surfaces. Recently it has been used as a free-form fabrication method for building three-dimensional parts, and now is being explored as a way of printing electrical and optical devices. Inkjet printing was used either as a rapid prototyping method for custom biosensors. Sol-gel method is naturally bound with inkjet, because the picoliter-sized ink droplets evaporate quickly, thus allowing quick sol-gel transitions on the printed surface. In this work will be shown how to merge those technologies, in order to make a nanoparticles doped printable hydrogel, which could be used for making 2D/3D smart scaffolds able to monitor cell activities. An automated image analysis system was developed in order to quickly have the pH measurements from pH nanosensors fluorescence images.

  15. 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.

  16. Characterization and hydrogen gas sensing properties of TiO{sub 2} thin films prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Haidry, Azhar Ali [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Bratislava (Slovakia); Puskelova, Jarmila [Department of Inorganic Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia); Plecenik, Tomas; Durina, Pavol; Gregus, Jan; Truchly, Martin; Roch, Tomas; Zahoran, Miroslav [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Bratislava (Slovakia); Vargova, Melinda [Department of Inorganic Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia); Kus, Peter; Plecenik, Andrej [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Bratislava (Slovakia); Plesch, Gustav, E-mail: plesch@fns.uniba.sk [Department of Inorganic Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia)

    2012-10-15

    Highlights: Black-Right-Pointing-Pointer Preparation and characterization of hydrogen sensing TiO{sub 2} thin films by sol-gel method. Black-Right-Pointing-Pointer The annealing effect on the structure, electrical, optical and sensing properties was studied. Black-Right-Pointing-Pointer The best sensitivity show the films composed of rutile with grain size of {approx}100 nm. - Abstract: Thin films of titanium dioxide with thickness of about 150 nm were deposited by spin coating method on a sapphire substrate from a sol-gel and annealed at various temperatures (from 600 Degree-Sign C to 1000 Degree-Sign C). Structural, optical and hydrogen gas sensing properties of the films were investigated. The annealing temperatures from 600 to 800 Degree-Sign C led to anatase phase with grain size in the range of 14-28 nm. Further increase of the annealing temperature resulted in transformation to rutile phase with larger grain size of about 100-120 nm. The optical band gap tended to decrease with increasing annealing temperature. The estimated values of activation energy for charge transport were in the range of 0.6-1.0 eV for films annealed at temperatures from 600 Degree-Sign C to 800 Degree-Sign C and 0.37-0.38 eV for films annealed at 900 Degree-Sign C and 1000 Degree-Sign C. The films annealed at 900 Degree-Sign C and 1000 Degree-Sign C showed better hydrogen sensitivity, what can be at least partially caused by their higher surface roughness.

  17. Synthesis of Silica Nanoparticles by Sol-Gel: Size-Dependent Properties, Surface Modification, and Applications in Silica-Polymer Nano composites-A Review

    International Nuclear Information System (INIS)

    Ismail, A.R.; Vejayakumaran, P.

    2012-01-01

    Application of silica nanoparticles as fillers in the preparation of nano composite of polymers has drawn much attention, due to the increased demand for new materials with improved thermal, mechanical, physical, and chemical properties. Recent developments in the synthesis of monodispersed, narrow-size distribution of nanoparticles by sol-gel method provide significant boost to development of silica-polymer nano composites. This paper is written by emphasizing on the synthesis of silica nanoparticles, characterization on size-dependent properties, and surface modification for the preparation of homogeneous nano composites, generally by sol-gel technique. The effect of nano silica on the properties of various types of silica-polymer composites is also summarized.

  18. Fabrication and Optical Characterization of Zinc Oxide Nanoparticles Prepared via a Simple Sol-gel Method

    Directory of Open Access Journals (Sweden)

    K. Hedayati

    2015-10-01

    Full Text Available In this research zinc oxide (ZnO nano-crystalline powders were prepared by sol-gel method using zinc acetate. The ZnO nanoparticles were characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM, ultraviolet-visible (UV-Vis, Fourier transform infra-red (FT-IR and energy dispersive X-ray (EDX spectroscopy. The structure of nanoparticles was studied using XRD pattern. The crystallite size of ZnO nanoparticles was calculated by Debye–Scherrer formula. Morphology of nano-crystals was observed and investigated using the SEM. The grain size of zinc oxide nanoparticles were in suitable agreement with the crystalline size calculated by XRD results. The optical properties of particles were studied with UV-Vis an FTIR absorption spectrum. The Raman spectrum measurements were carried out using a micro-laser Raman spectrometer forms the ZnO nanoparticles. At the end studied the effect of calcined temperature on the photoluminescence (PL emission of ZnO nanoparticles.

  19. Phase study of titanium dioxide nanoparticle prepared via sol-gel process

    Science.gov (United States)

    Oladeji Araoyinbo, Alaba; Bakri Abdullah, Mohd Mustafa Al; Salleh, Mohd Arif Anuar Mohd; Aziz, Nurul Nadia Abdul; Iskandar Azmi, Azwan

    2018-03-01

    In this study, titanium dioxide nanoparticles have been prepared via sol-gel process using titanium tetraisopropoxide as a precursor with hydrochloric acid as a catalyst, and ethanol with deionized water as solvents. The value of pH used is set to 3, 7 and 8. The sols obtained were dried at 100 °C for 1 hr and calcined at 350, 550, and 750 °C for 3 hrs to observe the phase transformation of titanium dioxide nanoparticle. The samples were characterized by x-ray diffraction and field emission scanning electron microscope. The morphology analysis is obtained from field emission scanning electron microscope. The phase transformation was investigated by x-ray diffraction. It was found that the pH of the solution affect the agglomeration of titanium dioxide particle. The x-ray diffraction pattern of titanium dioxide shows the anatase phase most abundant at temperature of 350 °C. At temperature of 550 °C the anatase and rutile phase were present. At temperature of 750 °C the rutile phase was the most abundant for pH 3, 7 and 8. It was confirmed that at higher temperature the rutile phase which is the stable phase are mostly present.

  20. 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

  1. 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.

  2. Sol-gel preparation of ion-conducting ceramics for use in thin films

    International Nuclear Information System (INIS)

    Steinhauser, M.I.

    1992-12-01

    A metal alkoxide sol-gel solution suitable for depositing a thin film of La 0.6 Sr 0.4 CoO 3 on a porous substrate has been developed; such films should be useful in fuel cell electrode and oxygen separation membrane manufacture. Crack-free films have been deposited on both dense and porous substrates by dip-coating and spin-coating techniques followed by a heat treatment in air. Fourier transform infrared spectroscopy was used to determine the chemical structure of metal alkoxide solution system. X-ray diffraction was used to determine crystalline phases formed at various temperatures, while scanning electron microscopy was used to determine physical characteristics of the films. Surface coatings have been successfully applied to porous substrates through the control of the substrate pore size, deposition parameters, and firing parameters. Conditions have been defined for which films can be deposited, and for which the physical and chemical characteristics of the film can be improved. A theoretical discussion of the chemical reactions taking place before and after hydrolysis in the mixed alkoxide solutions is presented, and the conditions necessary for successful synthesis are defined. Applicability of these films as ionic and electronic conductors is discussed

  3. 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.

  4. 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

  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. 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

  7. 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

  8. Sol-gel synthesized of nanocomposite palladium-alumina ceramic membrane for H{sub 2} permeability: Preparation and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, A.L.; Mustafa, N.N.N. [School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, Seri Ampangan, 14300 Nibong Tebal, Penang (Malaysia)

    2007-08-15

    Palladium-alumina membrane with mesopore and narrow pore size distribution was prepared by the sol-gel method. Effect of the finely dispersed metal on the microstructure and the characteristic properties of the palladium-alumina membrane were investigated. Observations were made on membrane weight loss, morphology, pore structure, pore size, surface area, pore surface fractal and membrane's crystal structure. Autosorb analysis, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform Infrared (FTIR) analysis were employed in the membrane characterization. Autosorb analysis found that, BET surface area decreased and pore size of the membrane increased with the increasing of calcinations temperature (500-1100{sup o}C) and with the increasing of palladium amount in the membrane. FTIR and TG/DTA analysis show that the suitable temperature for calcinations of palladium-alumina membrane is at 700{sup o}C. Palladium metals are highly dispersed at calcinations temperature of 700{sup o}C as observed by TEM analysis. The fine crystallinity of the palladium and {gamma}-alumina phase was obtained after calcined at 700{sup o}C. The SEM morphology shows a smooth and free crack layer of palladium-alumina membrane after repeating the process of dipping, drying and calcinations at temperature of 700{sup o}C. The membrane also successfully coated with a good adhesion on support. The thickness of the final membrane layer was estimated as 9{mu} m. (author)

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

    International Nuclear Information System (INIS)

    Zhang Wenjie; Bai Jiawei

    2012-01-01

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

  10. Effects of Calcination Temperature on Preparation of Boron-Doped TiO2 by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Wenjie Zhang

    2012-01-01

    Full Text Available Boron-doped TiO2 photocatalyst was prepared by a modified sol-gel method. Being calcinated at temperatures from 300°C to 600°C, all the 3% B-TiO2 samples presented anatase TiO2 phase, and TiO2 crystallite sizes were calculated to be 7.6, 10.3, 13.6, and 27.3 nm, respectively. The samples were composed of irregular particles with rough surfaces in the size range within 3 μm. Ti atoms were in an octahedron skeleton and existed mainly in the form of Ti4+, while the Ti-O-B structure was the main boron existing form in the 3% B-TiO2 sample. When calcination temperature increased from 300°C to 600°C, specific surface area decreased sharply from 205.6 m2/g to 31.8 m2/g. The average pore diameter was 10.53 nm with accumulative pore volume of 0.244 mL/g for the 3% B-TiO2 sample calcinated at 400°C, which performed optimal photocatalytic degradation activity. After 90 min of UV-light irradiation, degradation rate of methyl orange was 96.7% on the optimized photocatalyst.

  11. 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.

  12. Preparation and characterization of Mn-doped Li{sub 0.06}(Na{sub 0.5}K{sub 0.5}){sub 0.94}NbO{sub 3} lead-free piezoelectric ceramics with surface sol-gel coatings

    Energy Technology Data Exchange (ETDEWEB)

    Yoo, Ae Ri; Lee, Seong Eui; Lee, Hee Chul [Korea Polytechnic University, Shiheung (Korea, Republic of)

    2014-08-15

    This study investigated the effects of Mn doping and sol-gel surface coating on the structural and the electrical properties of lead-free Li{sub 0.06}(K{sub 0.5}Na{sub 0.5}){sub 0.94}NbO{sub 3}(LNKN) ceramics in disc form for use as eco-friendly piezoelectric devices. The 1-mol% Mn-doped LNKN ceramic showed a relatively high piezoelectric constant owing to its high density in the case of its being annealed at a temperature of 1010 .deg. C. A Mn-doped LNKN sol-gel solution with the same composition as that of the ceramics was spin-coated and sintered on both sides of the ceramic surfaces to acquire improved electrical properties. The sol-gel surface coating could play a decisive role in filling the pores, resulting in flat and stable interfaces between the electrodes and the piezoelectric elements. As a result, the highest piezoelectric constant, d{sub 33}, of 173 pC/N could be obtained for the Mn-doped LNKN ceramics with 420-nm-thick sol-gel surface coatings.

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

    International Nuclear Information System (INIS)

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

    1996-01-01

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

  14. Preparation and characterization of multilayer mesoporous γ-alumina membrane obtained via sol-gel using new precursors

    Directory of Open Access Journals (Sweden)

    Tafrishi R.

    2015-12-01

    Full Text Available In this paper, a mesoporous γ-alumina membrane coated on a macroporous α-alumina support via sol-gel method has been reported. A crack-free γ-alumina membrane was obtained by adding PVA to the alumina solution and optimum parameters of roughness, temperature and porosity were achieved. The support was dip-coated in different solutions using two new different solvents with different particle size distributions. Using these two solvents led to the uniform distribution of pore size in the final membrane. The alumina sols showed particle size distributions in the range of 20 to 55 nm which was measured by a DLS Zeta Sizer. X-ray diffraction technique, atomic force microscopy and scanning electron microscopy were used to characterize the membrane layer. XRD and DTA data for the γ-alumina membrane showed its thermal stability up to around 600 °C. The thickness of the mesoporous γ-alumina membrane was about 4 μm with 16 nm of surface roughness and 5 nm pore size. The resultant crack-free mesoporous membrane shows that the membrane preparation procedure was optimum. In this work, it has been investigated the performance of γ-alumina membranes for single gas permeation and separation of binary gas mixtures.

  15. Enhanced photoelectrochemical performance of Ti-doped hematite thin films prepared by the sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Lian Xiaojuan; Yang Xin; Liu Shangjun; Xu Ying; Jiang Chunping; Chen Jinwei [College of Materials Science and Engineering, Sichuan University, No.24 South Section 1, Yihuan Road, Chengdu 610065 (China); Wang Ruilin, E-mail: rlwang26@yahoo.com.cn [College of Materials Science and Engineering, Sichuan University, No.24 South Section 1, Yihuan Road, Chengdu 610065 (China)

    2012-01-15

    Ti-doped {alpha}-Fe{sub 2}O{sub 3} thin films were successfully prepared on FTO substrates by the sol-gel route. Hematite film was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy dispersive spectrometer (EDS). The XRD data showed {alpha}-Fe{sub 2}O{sub 3} had a preferred (1 1 0) orientation which belonged to the rhombohedral system. Interestingly, the grains turned into worm-like shape after annealed at high temperature. The IPCE could reach 32.6% at 400 nm without any additional potential vs. SCE. Titanium in the lattice can affect the photo electro chemical performance positively by increasing the conductivity of the thin film. So the excited electrons and holes could live longer, rather than recombining with each other rapidly as undoped hematite. And the efficient carrier density on the Ti-doped anode surface was higher than the undoped anode, which contribute to the well PEC performance.

  16. 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.

  17. 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.

  18. Photodegradation of indigo carmine and methylene blue dyes in aqueous solution by SiC-TiO{sub 2} catalysts prepared by sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Solis, Christian [Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, San Luis Potosi Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); Juarez-Ramirez, Isaias, E-mail: isajua13@yahoo.com [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Moctezuma, Edgar [Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, San Luis Potosi Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); Torres-Martinez, Leticia M. [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico)

    2012-05-30

    Highlights: Black-Right-Pointing-Pointer Photodegradation of organic dyes is possible using sol-gel SiC-TiO{sub 2} catalysts. Black-Right-Pointing-Pointer SiC-TiO{sub 2} makes a synergy effect that enhances its catalytic activity. Black-Right-Pointing-Pointer Sol-gel allows good dispersion and attachment of TiO{sub 2} particles on SiC surface. Black-Right-Pointing-Pointer SiC-TiO{sub 2} exhibits better activity than TiO{sub 2} (P25) on organic dyes degradation. Black-Right-Pointing-Pointer SiC-TiO{sub 2} catalysts are settled down and easily separated after photocatalysis. - Abstract: Indigo carmine and methylene blue dyes in aqueous solution were photodegraded using SiC-TiO{sub 2} catalysts prepared by sol-gel method. After thermal treatment at 450 Degree-Sign C, SiC-TiO{sub 2} catalysts prepared in this work showed the presence of SiC and TiO{sub 2} anatase phase. Those compounds showed specific surface area values around 22-25 m{sup 2} g{sup -1}, and energy band gap values close to 3.05 eV. In comparison with TiO{sub 2} (P25), SiC-TiO{sub 2} catalysts showed the highest activity for indigo carmine and methylene blue degradation, but this activity cannot be attributed to the properties above mentioned. Therefore, photocatalytic performance is due to the synergy effect between SiC and TiO{sub 2} particles caused by the sol-gel method used to prepare the SiC-TiO{sub 2} catalysts. TiO{sub 2} nanoparticles are well dispersed onto SiC surface allowing the transfer of electronic charges between SiC and TiO{sub 2} semiconductors, which avoid the fast recombination of the electron-hole pair during the photocatalytic process.

  19. 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

  20. Development of cobalt ferrite powder preparation employing the sol-gel technique and its structural characterization

    International Nuclear Information System (INIS)

    Sajjia, M.; Oubaha, M.; Prescott, T.; Olabi, A.G.

    2010-01-01

    Research highlights: This work focuses on the sol-gel process and the effects that the initial parameters have on the final product, which is the cobalt ferrite powder, in addition to the heat treatment. Particular interest is devoted to understand how the crosslinker and the chelating agent work and affect the final product. - Abstract: This work focuses on the development of a method to make cobalt ferrite powder using the sol-gel process. A particular emphasis is devoted to the understanding of the role of the chemical parameters involved in the sol-gel technique, and of the heat treatment on the structures and morphologies of the materials obtained. Several samples of cobalt ferrite powder were obtained by varying the initial parameters of the process in addition to the heat treatment temperature. X-ray diffraction and scanning electron microscopy were used to identify the structure and morphology of samples demonstrating the influence of the initial parameters. DTA/TGA was carried out on two standard samples to identify important reaction temperatures during the heat treatment. The average size of the nano crystallites was estimated for a sample by the full width at half maximum (FWHM) of the strongest X-ray diffraction (XRD) peak. It has been found that the chelating agent and the crosslinker have a critical influence on the resultant structure, the particle size and the particle size distribution.

  1. Preparation of Nd-doped gadolinium-gallium garnet laser ceramic powder by sol-gel method

    Institute of Scientific and Technical Information of China (English)

    YAO Yan-ping; LIU Jing-he

    2006-01-01

    Preparation of Nd3+:Gd3Ga5O12 polycrystalline material by sol-gel method was preparated in this paper.The structure and the pattern of the sample were analyzed by thermogravimetric analysis and differential thermal analysis(TG-DTA),Infrared spectrum,XRD,TEM and electron spectrum,which indicated that the powder with good characteristics of 70-100 nm can be obtained by sintering at 1 000℃.It was shown that the chemical composition of the sample was agreed with experimental requirements by electron spectrum analysis.

  2. 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.

  3. Sol-Gel SiO2-CaO-P2O5 biofilm with surface engineered for medical application

    Directory of Open Access Journals (Sweden)

    Sonia Regina Federman

    2007-06-01

    Full Text Available Sol-gel film in the SiO2-CaO-P2O5 system was prepared from TEOS, TEP, alcohol and hydrated calcium nitrate in an acidic medium. The coatings were deposited on stainless steel using the dip-coating technique. After deposition, the composite was submitted to heat treatment, at different temperatures and exposure times to investigate the influence of such parameters on the surface morphology of the composite. The coated surfaces were characterized by AFM, SEM and FTIR. The present study showed that the formation of different textures (an important parameter in implant fixation could be controlled by temperature and time of heat treatment.

  4. 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)

  5. Laser ablation inductively coupled plasma mass spectrometry analysis of agricultural soils using the sol-gel technique of pellet preparation

    International Nuclear Information System (INIS)

    Hubova, I.; Hola, M.; Vaculovic, T.; Pinkas, J.; Prokes, L.; Stefan, I.; Kanicky, V.

    2009-01-01

    Full text: Monitoring of metals in agricultural soils is gaining importance as they are accumulated by plants. A LAICPQMS method with Nd:YAG 213 nm laser has been developed for determination of Cr, Ni, Cu, Zn and Pb in soil pellets prepared by the sol-gel technique. LA-ICPMS analysis of archive samples was verified by XRF of wax-soil pellets and ICPMS with nebulization of solutions obtained by total soil decomposition and by analysis of reference materials. Sequention extraction was used for fractionation analysis. (author)

  6. Influence of temperature in TL signal induced by gamma radiation in zircon prepared by sol gel via

    International Nuclear Information System (INIS)

    Salas, P.; Castano, V.M.; Mendoza A, D.; Gonzalez M, P.R.; Rosa C, E. de la

    2000-01-01

    In this work, it was realized a study of the temperature effects in thermoluminescent signal (Tl) induced by gamma radiation in zircon, which was prepared by the sol gel method. According to the obtained results, the zircon thermically treated at 500 C or over is sensitive to radiation. This sensitivity is increased when the temperature in study is augmented, moreover, the Tl spectra form also is modified with the temperature increment. The samples thermically treated at 750 C or over present a linear response in the dose interval 27 to 165 Gy; therefore, such materials result promissories for dosimetric purposes. (Author)

  7. Characteristics of nano Ti-doped SnO2 powders prepared by sol-gel method

    International Nuclear Information System (INIS)

    Liu, X.M.; Wu, S.L.; Chu, Paul K.; Zheng, J.; Li, S.L.

    2006-01-01

    Ti 4+ -doped SnO 2 nano-powders were prepared by the sol-gel process using tin tetrachloride and titanium tetrachloride as the starting materials. The crystallinity and purity of the powders were analyzed by X-ray diffraction (XRD) and the size and distribution of Ti 4+ -doped SnO 2 grains were studied using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results show that Ti 4+ has been successfully incorporated into the SnO 2 crystal lattice and the electrical conductivity of the doped materials improves significantly

  8. 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)

  9. Comparison of sol-gel prepared catalysts for CO oxidation and N2O decomposition reactions.

    OpenAIRE

    Euesden, Claire

    2002-01-01

    This thesis comprises analysis for two types of catalysis: CO oxidation and N2O decomposition; related by their research in sol-gel catalysis. The CO oxidation work was undertaken on behalf of Servomex plc in order to understand how their catalyst-based sensor (Tfx 1750) worked and why it failed when exposed to coal power station flue streams within its two-year guarantee period. This research will show, by means of many analytical techniques and catalytic tests: 1. A comparison of the Servom...

  10. Zinc oxide films impurified with Ti and prepared by the Sol-gel method; Peliculas de oxido de zinc impurificadas con Ti y preparadas por el metodo Sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Tirado G, S. [ESFM-IPN, 07738 Mexico D.F. (Mexico); Cazares R, J.M.; Maldonado, A. [CINVESTAV-IPN, A.P. 14-740, 07000 Mexico D.F. (Mexico)

    2006-07-01

    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)

  11. 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

  12. Structural studies on iron-tellurite glasses prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Rada, S., E-mail: Simona.Rada@phys.utcluj.r [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Dehelean, A. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Stan, M. [Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Chelcea, R. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Culea, E. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania)

    2011-01-05

    Research highlights: {yields} Iron-tellurite glasses obtained using the sol-gel synthesis. - Abstract: In this study, we report structural properties of the iron-tellurite glasses obtained using the sol-gel synthesis. The samples were characterized by X-ray diffraction, FTIR, UV-vis and EPR spectroscopy. Our results indicate dominant presence of iron ions in the trivalent state and the existence some Fe{sup 2+} ions. The analysis of the IR spectra indicates a gradual transformation of iron ions from tetrahedral into octahedral sites when the concentration of Fe(NO{sub 3}){sub 3} is increased beyond 0.64 mol%. EPR studies show that the increase of Fe(NO{sub 3}){sub 3} content in the host matrix induces the growth of the number of effective g values. This can be explained considering that the orbitals of O{sup 2-} ion with a large spin-orbit interaction constant will interact with the 3d orbital of Fe{sup 3+} ion bonded to this O{sup 2-} ion, thus leading to appearance of an orbital angular momentum which contributes to the magnetic moment of Fe{sup 3+} ion. A strong dipolar interaction, which is more predominant in a glass with higher content of Fe(NO{sub 3}){sub 3}, causing a localized magnetic field along the site of the Fe{sup 3+} ions and the increase the effective g values.

  13. 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.

  14. Preparation of SDC electrolyte thin films on dense and porous substrates by modified sol-gel route

    International Nuclear Information System (INIS)

    Lin Hongfei; Ding, Changsheng; Sato, Kazuhisa; Tsutai, Yoshifumi; Ohtaki, Hiromichi; Iguchi, Mabito; Wada, Chiharu; Hashida, Toshiyuki

    2008-01-01

    Nanocrystalline fluorite type samarium doped ceria (SDC) electrolyte thin film for intermediate temperature-solid oxide fuel cells (IT-SOFCs) application were prepared on the dense and porous substrates at low temperatures of 573-1373 K using a novel citrate sol-gel route combined with a sol suspension spray coating technique. Thermogravimetric analysis showed that the decomposition of the citrate gel film and the initial crystallization of the SDC occurred at a low temperature of about 590 K. XRD examination revealed that the annealing of the green film at temperatures of 573-1373 K provided cubic nanocrystalline SDC phase. The crystallite sizes were in the range of 9-19 nm. Microscopic observations indicated that the derived film was homogeneous, dense and crack-free without pinholes. The desired thickness for preparation of thin electrolyte films from hundreds of nm to several μm should be controllable and feasible by repeating the simple and inexpensive citrate sol-gel spray coating process

  15. Some of Physical Properties of Nanostructured (Mg1-xCoxFe2O4 Ferrites Prepared by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Muhammad Abdul Ammer Alsherefi

    2018-01-01

    Full Text Available Sol-gel auto combustion technique was used to prepare nanoparticles of magnesium-cobalt ferrites with the chemical formula Mg1-xCoxFe2O4 for  (x=0, 0.2, 0.4, 0.6, 0.8, 1, where x added as weight  percentages, and sintering  at temperature (1100 oC. The X-ray patterns of prepared powder has confirmed the structure of cubic spinel structure (fcc. The prepared samples were composed of nearly spherical nano particles .An average particle size of  magnesium-cobalt ferrite  were  calculated  using  Debye Scherer’s relation is equal 53.12 nm. The surface structure of the samples was investigated by Scanning Electron Microscope(SEM. The electromagnetic properties for prepared samples were investigated using Vector Network Analyzer (VNA in X-band microwave region.

  16. 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.

  17. 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.

  18. Electroluminescence of zinc oxide thin-films prepared via polymeric precursor and via sol-gel methods

    International Nuclear Information System (INIS)

    Lima, S.A.M.; Cremona, M.; Davolos, M.R.; Legnani, C.; Quirino, W.G.

    2007-01-01

    Zinc oxide (ZnO) is an electroluminescent (EL) material that can emit light in different regions of electromagnetic spectrum when electrically excited. Since ZnO is chemically stable, inexpensive and environmentally friendly material, its EL property can be useful to construct solid-state lamps for illumination or as UV emitter. We present here two wet chemical methods to prepare ZnO thin-films: the Pechini method and the sol-gel method, with both methods resulting in crystalline and transparent films with transmittance >85% at 550 nm. These films were used to make thin-film electroluminescent devices (TFELD) using two different insulator layers: lithium fluoride (LiF) or silica (SiO 2 ). All the devices exhibit at least two wide emission bands in the visible range centered at 420 nm and at 380 nm attributed to the electronic defects in the ZnO optical band gap. Besides these two bands, the device using SiO 2 and ZnO film obtained via sol-gel exhibits an additional band in the UV range centered at 350 nm which can be attributed to excitonic emission. These emission bands of ZnO can transfer their energy when a proper dopant is present. For the devices produced the voltage-current characteristics were measured in a specific range of applied voltage

  19. A sol-gel derived pH-responsive bovine serum albumin molecularly imprinted poly(ionic liquids) on the surface of multiwall carbon nanotubes

    International Nuclear Information System (INIS)

    Liu, Mingming; Pi, Jiangyan; Wang, Xiaojie; Huang, Rong; Du, Yamei; Yu, Xiaoyang; Tan, Wenfeng; Liu, Fan; Shea, Kenneth J.

    2016-01-01

    A pH-responsive surface molecularly imprinted poly(ionic liquids) (MIPILs) was prepared on the surface of multiwall carbon nanotubes (MWCNTs) by a sol-gel technique. The material was synthesized using a 3-aminopropyl triethoxysilane modified multiwall carbon nanotube (MWCNT-APTES) as the substrate, bovine serum albumin (BSA) as the template molecule, an alkoxy-functionalized IL 1-(3-trimethoxysilyl propyl)-3-methyl imidazolium chloride ([TMSPMIM]Cl) as both the functional monomer and the sol-gel catalyst, and tetraethoxysilane (TEOS) as the crosslinking agent. The molecular interaction between BSA and [TMSPMIM]Cl was quantitatively evaluated by UV–vis spectroscopy prior to polymerization so as to identify an optimal template/monomer ratio and the most suitable pH value for the preparation of the MWCNTs@BSA-MIPILs. This strategy was found to be effective to overcome the problems of trial-and-error protocol in molecular imprinting. The optimum synthesis conditions were as follows: template/monomer ratio 7:20, crosslinking agent content 2.0–2.5 mL, temperature 4 °C and pH 8.9 Tris–HCl buffer. The influence of incubation pH on adsorption was also studied. The result showed that the imprinting effect and selectivity improved significantly with increasing incubation pH from 7.7 to 9.9. This is mainly because the non-specific binding from electrostatic and hydrogen bonding interactions decreased greatly with the increase of pH value, which made the specific binding affinity from shape selectivity strengthened instead. The polymers synthesized under the optimal conditions were then characterized by BET surface area measurement, FTIR, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The adsorption capacity, imprinting effect, selective recognition and reusability were also evaluated. The as-prepared MWCNTs@BSA-MIPILs were also found to have a number of advantages including high surface area (134.2 m"2 g"−"1), high adsorption capacity (55

  20. A sol-gel derived pH-responsive bovine serum albumin molecularly imprinted poly(ionic liquids) on the surface of multiwall carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Mingming, E-mail: liumm@mail.hzau.edu.cn [Key Laboratory of Arable Land Conservation (Middle and Lower Reaches of Yangtse River), Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Pi, Jiangyan; Wang, Xiaojie; Huang, Rong; Du, Yamei; Yu, Xiaoyang; Tan, Wenfeng; Liu, Fan [Key Laboratory of Arable Land Conservation (Middle and Lower Reaches of Yangtse River), Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Shea, Kenneth J., E-mail: kjshea@uci.edu [Department of Chemistry, University of California-Irvine, Irvine, CA 92697 (United States)

    2016-08-17

    A pH-responsive surface molecularly imprinted poly(ionic liquids) (MIPILs) was prepared on the surface of multiwall carbon nanotubes (MWCNTs) by a sol-gel technique. The material was synthesized using a 3-aminopropyl triethoxysilane modified multiwall carbon nanotube (MWCNT-APTES) as the substrate, bovine serum albumin (BSA) as the template molecule, an alkoxy-functionalized IL 1-(3-trimethoxysilyl propyl)-3-methyl imidazolium chloride ([TMSPMIM]Cl) as both the functional monomer and the sol-gel catalyst, and tetraethoxysilane (TEOS) as the crosslinking agent. The molecular interaction between BSA and [TMSPMIM]Cl was quantitatively evaluated by UV–vis spectroscopy prior to polymerization so as to identify an optimal template/monomer ratio and the most suitable pH value for the preparation of the MWCNTs@BSA-MIPILs. This strategy was found to be effective to overcome the problems of trial-and-error protocol in molecular imprinting. The optimum synthesis conditions were as follows: template/monomer ratio 7:20, crosslinking agent content 2.0–2.5 mL, temperature 4 °C and pH 8.9 Tris–HCl buffer. The influence of incubation pH on adsorption was also studied. The result showed that the imprinting effect and selectivity improved significantly with increasing incubation pH from 7.7 to 9.9. This is mainly because the non-specific binding from electrostatic and hydrogen bonding interactions decreased greatly with the increase of pH value, which made the specific binding affinity from shape selectivity strengthened instead. The polymers synthesized under the optimal conditions were then characterized by BET surface area measurement, FTIR, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The adsorption capacity, imprinting effect, selective recognition and reusability were also evaluated. The as-prepared MWCNTs@BSA-MIPILs were also found to have a number of advantages including high surface area (134.2 m{sup 2} g{sup −1}), high adsorption

  1. 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.

  2. The effect of Ni and Fe doping on YBCO powder prepared by sol gel method

    Directory of Open Access Journals (Sweden)

    F Saeb

    2009-08-01

    Full Text Available  We fabricated YBa2Cu3-xMxO7- d (M=Ni, Fe bulk samples, with stochiometric amount 0≤x≤0.045 by sol-gel method. The phase analysis and microstructure of specimens were examined by XRD and SEM. The electrical resistivity was measured using standard four probe technique for 77-300K. Investigation of XRD spectrum by MAUD shows Ni and Fe ions substitute in Cu(2 and Cu(1 site, respectively. Transition temperature decreases in 93-87K for Ni-doped samples and 93-92K for Fe-doped series. It seems that the suppression of superconductivity has no direct correlation with the magnetism of ions itself .

  3. 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.

  4. Analysis on the factors affecting the preparation of TIO2-ADUN composite sol by sol-gel method

    International Nuclear Information System (INIS)

    Wang Hui; Yin Rongcai; Liu Jinhong

    2010-01-01

    With C 2 H 2 O 5 and water as solvent and TBT as precursor and HNO 3 as the activator and valorize, the process for preparing TiO 2 -ADUN composite Sol method was studied. The influence of different reaction conditions on Sol-Gel time was analyzed in this study. The optimal reaction condition are: reaction temperature 20-25 degree C; pH value of reaction mixture 2-5; HNO 3 value of reaction mixture 0.3-0.5 ml; molar rations of alcohol to TBT 10, of water to TBT 2-3, respectively. A concentrated ADUN solution with Ti Sol , urea, water as additive is dispersed into uniform which are prepared by external mlii. (authors)

  5. Effects of sintering temperature on structural and electrical transport properties of zinc ferrites prepared by sol-gel route

    International Nuclear Information System (INIS)

    Anis-ur-Rehman, M.; Malik, M.A.; Ahmad, I.; Nasir, S.; Mubeen, M.; Abdullah, A.

    2011-01-01

    The effects of sintering temperature on the structural and electrical transport properties of nanocrystalline zinc ferrites are reported. The zinc ferrites were prepared by WOWS sol-gel synthesis route. The prepared sample was sintered at temperatures 500 deg. C, 700 deg. C and 900 deg. C respectively for 2 h. X-ray Diffraction (XRD) technique was used to describe the structural properties. The crystallite size, lattice parameters and porosity of samples were measured from the analysis of XRD data. The average crystallite size for each sample was measured using the Scherrer formula by considering the most intense (3 1 1) peak. The dielectric constant (e), dielectric loss tangent (tan theta ) and AC electrical conductivity of nanocrystalline Zn ferrites are investigated as a function of frequency and sintering temperature. All the electrical properties are explained in accordance with MaxwellWagner model and Koops phenomenological theory. (author)

  6. Annealing temperature effect on the properties of mercury-doped TiO{sub 2} films prepared by sol-gel dip-coating technique

    Energy Technology Data Exchange (ETDEWEB)

    Mechiakh, R., E-mail: raouf_mechiakh@yahoo.fr [Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar Batna, Batna (Algeria); Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia); Ben Sedrine, N. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia); Karyaoui, M. [Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar Batna, Batna (Algeria); Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia); Chtourou, R. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia)

    2011-04-15

    This work presents the annealing temperature effect on the properties of mercury (Hg)-doped titanium dioxide (TiO{sub 2}). Thin films and polycrystalline powders have been prepared by sol-gel process. The structure, surface morphology and optical properties, as a function of the annealing temperature, have been studied by atomic force microscopy (AFM), Raman, reflectance and ellipsometric spectroscopies. In order to determine the transformation points, we have analyzed the xerogel-obtained powder by differential scanning calorimetry (DSC). Raman spectroscopy shows the crystalline anatase and rutile phases for the films annealed at 400 deg. C and 1000 deg. C respectively. The AFM surface morphology results indicate that the particle size increases from 14 to 57 nm by increasing the annealing temperature. The complex index and the optical band gap (E{sub g}) of the films were determined by the spectroscopic ellipsometry analysis. We have found that the optical band gap decreases by increasing the annealing temperature.

  7. Annealing temperature effect on the properties of mercury-doped TiO2 films prepared by sol-gel dip-coating technique

    International Nuclear Information System (INIS)

    Mechiakh, R.; Ben Sedrine, N.; Karyaoui, M.; Chtourou, R.

    2011-01-01

    This work presents the annealing temperature effect on the properties of mercury (Hg)-doped titanium dioxide (TiO 2 ). Thin films and polycrystalline powders have been prepared by sol-gel process. The structure, surface morphology and optical properties, as a function of the annealing temperature, have been studied by atomic force microscopy (AFM), Raman, reflectance and ellipsometric spectroscopies. In order to determine the transformation points, we have analyzed the xerogel-obtained powder by differential scanning calorimetry (DSC). Raman spectroscopy shows the crystalline anatase and rutile phases for the films annealed at 400 deg. C and 1000 deg. C respectively. The AFM surface morphology results indicate that the particle size increases from 14 to 57 nm by increasing the annealing temperature. The complex index and the optical band gap (E g ) of the films were determined by the spectroscopic ellipsometry analysis. We have found that the optical band gap decreases by increasing the annealing temperature.

  8. 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.

  9. Outcome of temperature variation on sol-gel prepared CuO nanostructure properties (optical and dielectric)

    Energy Technology Data Exchange (ETDEWEB)

    Bibi, Maryam [Nano Synthesis Laboratory, Department of Physics, National University of Sciences and Technology, Islamabad (Pakistan); Javed, Qurat-ul-Ain, E-mail: quratulain@sns.nust.edu.pk [Nano Synthesis Laboratory, Department of Physics, National University of Sciences and Technology, Islamabad (Pakistan); Abbas, Hussain [Institute of Avionics & Aeronautics (IAA), Air University, Islamabad (Pakistan); Baqi, Sabah [Nano Synthesis Laboratory, Department of Physics, National University of Sciences and Technology, Islamabad (Pakistan)

    2017-05-01

    The optical and dielectric properties of Copper Oxide (CuO) have made it a fascinating material to be used in solar energy harvesting, gas sensing, optoelectronics and catalytical applications. Focusing on the cost-effectiveness of Sol-gel method, it is employed for nanostructured CuO production. Effect of changing temperature is observed on the formation mechanism of CuO and its properties. The temperature range of 300 °C–500 °C was used in annealing of samples to produce defect free CuO nanomaterial. Prepared material was investigated using phase characterization (X-ray diffraction ‘XRD’) technique, scanning electron microscopy (SEM), UV–Visible absorption spectroscopy and LCR meter. A structural change in prepared CuO was observed from cluster formation to Nano-fibrils by increase in annealing temperature. 11.99 nm–29.17 nm crystallites of CuO were attained by using Debye Scherer formula. A large band gap of 3.15 eV was achieved by increasing the annealing temperature upto 400 °C. For better solar energy harvest, wide band gapped CuO structures are proved to be functional and practical materials. The fabricated CuO nanostructures were found suitable to be used in devices for stabilizing circuit designs for sensitive appliances as well as micro electromechanical systems (mems). - Highlights: • CuO was synthesized by using sol gel method post growth annealing process. • XRD and SEM characterizations confirm the successful synthesis of CuO. • Change in morphology was observed with varying annealing temperature. • Improved optical and dielectric properties were observed.

  10. {sup 90}Y microspheres prepared by sol-gel method, promising medical material for radioembolization of liver malignancies

    Energy Technology Data Exchange (ETDEWEB)

    Łada, Wiesława, E-mail: w.lada@ichtj.waw.pl [Institute of Nuclear Chemistry and Technology, 03-195 Warsaw, Dorodna 16 (Poland); Iller, Edward [National Centre for Nuclear Research, Radioisotope Centre POLATOM, 05-400 Otwock, Andrzej Sołtan 7 (Poland); Wawszczak, Danuta [Institute of Nuclear Chemistry and Technology, 03-195 Warsaw, Dorodna 16 (Poland); Konior, Marcin, E-mail: marcin.konior@polatom.pl [National Centre for Nuclear Research, Radioisotope Centre POLATOM, 05-400 Otwock, Andrzej Sołtan 7 (Poland); Dziel, Tomasz [National Centre for Nuclear Research, Radioisotope Centre POLATOM, 05-400 Otwock, Andrzej Sołtan 7 (Poland)

    2016-10-01

    A new technology for the production of radiopharmaceutical {sup 90}Y microspheres in the form of spherical yttrium oxide grains obtained by sol-gel method has been described. The authors present and discuss the results of investigations performed in the development of new production technology of yttrium microspheres and determination of their physic-chemical properties. The final product has the structure of spherical yttrium oxide grains with a diameter 25–100 μm, is stable and free from contaminants. Irradiation of 20 mg samples of grains with diameter of 20–50 μm in the thermal neutron flux of 1.7 × 10{sup 14} cm{sup −2} s{sup −1} at the core of MARIA research nuclear reactor allowed to obtain microspheres labelled with the {sup 90}Y isotope on the way of the nuclear reaction {sup 89}Y(n, γ){sup 90}Y. Specific activity of irradiated microspheres has been determined by application of absolute triple to double coincidence ratio method (TDCR) and has been evaluated at 190 MBq/mg Y. {sup 90}Y microspheres prepared by the proposed technique can be regarded as a promising medical material for radioembolization of liver malignancies. - Highlights: • Sol-gel methods for preparation of spherical yttrium trioxide grains have been proposed. • Determination condition for irradiation {sup 89}Y{sub 2}O{sub 3} grains in nuclear reactor • Evaluation of specific activity of {sup 90}Y microspheres • Estimation of {sup 90}Y microspheres as promising medical material for radioembolization.

  11. Reddish orange long afterglow phosphor Ca2SnO4:Sm3+prepared by sol-gel method

    International Nuclear Information System (INIS)

    Ju Zhenghua; Zhang Shuihe; Gao Xiuping; Tang Xiaoliang; Liu Weisheng

    2011-01-01

    Highlights: → A promising reddish orange emissive long afterglow phosphor Ca 2 SnO 4 :Sm 3+ prepared by sol-gel method was firstly reported. → The optics properties of Ca 2 SnO 4 :Sm 3+ were discussed. → Very useful tool, thermoluminscent technique was chosen to investigate the traps in the material. The results of thermoluminscent spectra indicating that the depth and number of traps are critical factors in determining their performance. → Furthermore, the phosphorescence mechanism was discussed successfully. → This work provides a potential approach to develop reddish orange light emitting long afterglow phosphor. - Abstract: A reddish orange light emissive long afterglow phosphor, Ca 2 SnO 4 :Sm 3+ was prepared by sol-gel method at lower temperature. The synthesized phosphors were characterized by X-ray diffraction, scanning electron micrograph images, photoluminescence spectra, afterglow decay curves and thermoluminescence spectra. Three emission peaks locate at 565 nm, 609 nm and 655 nm corresponding to CIE chromaticity coordinates of x = 0.53 and y = 0.47, which indicates the reddish orange light emitting. The fluorescent intensity and the afterglow characteristic depends on the concentration of Sm 3+ and the optimized concentration is 1.5 mol%. The afterglow decay curves are well fitted with triple-exponential decay models. The thermoluminescence glow curves show that the Sm 3+ induces suitable trap depth and result in the long afterglow phenomenon, and the corresponding increase or decrease in afterglow is associated with trap concentration, nearly no change in trap depth. The 1.5 mol% Sm 3+ -doped Ca 2 SnO 4 sample has the biggest trap concentration and exhibit the best afterglow characteristic, its' afterglow time is about 1 h. The phosphorescence mechanism of this long afterglow phosphor was discussed.

  12. Study of alumosilicate porcelains: Sol-gel preparation, characterization and erosion evaluated by gravimetric method

    International Nuclear Information System (INIS)

    Bogdanoviciene, Irma; Jankeviciute, Audrone; Pinkas, Jiri; Beganskiene, Aldona; Kareiva, Aivaras

    2008-01-01

    In this paper, the sol-gel synthesis and characteristic properties of kalsilite-type alumosilicates (KAlSiO 4 and K 0.5 Na 0.5 AlSiO 4 ) are reported. The polycrystalline powders were characterized by thermal analysis (TG/DTA), powder X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). Single-phase kalsilite oxides have been obtained after annealing precursor gels for 5 h in the temperature range of 750-850 deg. C. It was demonstrated that crystallinity of the samples slightly depends on the temperature of annealing. From the results obtained, it could be concluded that the KAlSiO 4 solids are composed of the volumetric plate-like grains with no regular size (from 5 μm to 30 μm at 750 deg. C and around 5-50 μm at 850 deg. C). Larger crystallites for mixed potassium-sodium kalsilite have formed (from 10 μm to 80 μm at 750 deg. C and >100 μm at 850 deg. C) in comparison with potassium kalsilite samples). The erosion of obtained dental porcelain samples stored in saliva, beer and Coca-Cola was compared

  13. Tetragonal zirconia quantum dots in silica matrix prepared by a modified sol-gel protocol

    Science.gov (United States)

    Verma, Surbhi; Rani, Saruchi; Kumar, Sushil

    2018-05-01

    Tetragonal zirconia quantum dots (t-ZrO2 QDs) in silica matrix with different compositions ( x)ZrO2-(100 - x)SiO2 were fabricated by a modified sol-gel protocol. Acetylacetone was added as a chelating agent to zirconium propoxide to avoid precipitation. The powders as well as thin films were given thermal treatment at 650, 875 and 1100 °C for 4 h. The silica matrix remained amorphous after thermal treatment and acted as an inert support for zirconia quantum dots. The tetragonal zirconia embedded in silica matrix transformed into monoclinic form due to thermal treatment ≥ 1100 °C. The stability of tetragonal phase of zirconia is found to enhance with increase in silica content. A homogenous dispersion of t-ZrO2 QDs in silica matrix was indicated by the mapping of Zr, Si and O elements obtained from scanning electron microscope with energy dispersive X-ray analyser. The transmission electron images confirmed the formation of tetragonal zirconia quantum dots embedded in silica. The optical band gap of zirconia QDs (3.65-5.58 eV) was found to increase with increase in zirconia content in silica. The red shift of PL emission has been exhibited with increase in zirconia content in silica.

  14. Magnetic studies of cobalt doped barium hexaferrite nanoparticles prepared by modified sol-gel method

    International Nuclear Information System (INIS)

    Shalini, M. Govindaraj; Sahoo, Subasa C.

    2016-01-01

    M-type barium hexaferrite (BaFe_1_2O_1_9) and cobalt doped barium hexaferrite (BaFe_1_1CoO_1_9) nanopowders were synthesized by modified sol-gel auto-combustion technique and were annealed at 900°C in air for 4 hours. The annealed powders were studied in the present work and X-ray diffraction studies showed pure phase formation after annealing. The average grain size in the nanopowder sample was decreased after doping. Magnetization value of 60 emu/g was observed at 300 K for the barium hexaferrite and was reduced to 54 emu/g after doping. The coercivity of 5586 Oe was observed at 300 K for the undoped sample and was found to be decreased in the doped sample. As the measurement temperature was decreased from 300 K to 60 K, magnetization value was increased in both the samples compared to those at 300 K. The coercivity of the undoped sample was found to decrease whereas it was increased for the doped sample at 60 K. The observed magnetic properties may be understood on the basis of modified exchange interaction and anisotropy in the doped sample compared to that of pure barium hexaferrite.

  15. Preparation of soft-agglomerated nano-sized ceramic powders by sol-gel combustion process

    International Nuclear Information System (INIS)

    Feng, Q.; Ma, X.H.; Yan, Q.Z.; Ge, C.C.

    2009-01-01

    The soft-agglomerated Gd 2 BaCuO 5 (Gd211) nano-powders were synthesized by sol-gel combustion process with binary ligand and the special pretreatment on gel. The mechanism of the formation of weakly agglomerated structure was studied in detail. The results showed that network structure in gelation process was found to be a decisive factor for preventing agglomeration of colloidal particles. The removal of free water, coordinated water, and most of hydroxyl groups during pretreatment further inhibited the formation of hydrogen bonds between adjacent particles. The soft-agglomeration of the particles was confirmed by isolated particles in calcined Gd211 powders and in green compact, a narrow monomodal pore size distribution of the green compact and the low agglomeration coefficient of the calcined Gd211 powder. Extension this process to synthesis of BaCeO 3 , BaTiO 3 and Ce 0.8 Sm 0.2 O 1.9 powders, also led to weakly agglomerated nano-powders. It suggests that this method represents a powerful and facile method for the creation of doped and multi-component nano-sized ceramic powders.

  16. 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

  17. Characterization on the electrophoretic deposition of the 8 mol% yttria-stabilized zirconia nanocrystallites prepared by a sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Y.-H. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Kuo, C.-W. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Shih, C.-J. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Hung, I-M. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Fung, K.-Z. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wen, S.-B. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, M.-C. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China)]. E-mail: cjshih@kmu.edu.tw

    2007-02-15

    An 8 mol% yttria-stabilized zirconia (8YSZ) films are electrophoretically deposited on the La{sub 0.8}Sr{sub 0.2}MnO{sub 3} substrate using 8YSZ nanocrystallites prepared by a sol-gel process. Effects of liquid suspension on the particle zeta potential and degree of agglomeration at different pH values are investigated. When the pH value deviates from the point of zero charge (PZC), the adsorption of protons on particle surfaces cause higher zeta potential and well-dispersed suspension. The optimal values of the iodine concentration, applied voltage and deposition time for the electrophoretic deposition of 8YSZ films are also found.

  18. Preparation of LiMO2(M=Co,Ni) cathode materials for intermediate temperature fuel cells by sol-gel processes

    DEFF Research Database (Denmark)

    Tao, S.W.; Wu, Q.Y.; Zhan, Z.L.

    1999-01-01

    LiMO2 (M = Co, Ni) was prepared by complexing sol-gel processes. The phase and thermal stability were characterized by XRD and TG analyses. LiCoO2 and LiNiO2 phases are formed around 400 degrees C and 700 degrees C respectively in our synthesis process. LiNiO2 exhibit higher electrical conductivity...

  19. Preparation of (Bi,Pb)2Sr2Ca2Cu3Ox precursor powders by a modified polyethylene glycol based sol-gel process

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude; Andersen, N.H.

    2002-01-01

    A modified sol-gel process based on polyethylene glycol has been developed for preparing (Bi,Pb)(2)Sr2Ca2Cu3Ox precursor powders in view of Ag-sheeted tape manufacture. A careful control of the pH and concentration temperature yields an amorphous gel, which can be converted to a fine and extremely...

  20. 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.

  1. Correlation between microstructure and optical properties of nano-crystalline TiO{sub 2} thin films prepared by sol-gel dip coating

    Energy Technology Data Exchange (ETDEWEB)

    Mechiakh, R., E-mail: raouf_mechiakh@yahoo.fr [Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar, Batna (Algeria); Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Laboratoire de Ceramiques, Universite Mentouri Constantine (Algeria); Sedrine, N. Ben; Chtourou, R. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Bensaha, R. [Laboratoire de Ceramiques, Universite Mentouri Constantine (Algeria)

    2010-11-15

    Titanium dioxide thin films have been prepared from tetrabutyl-orthotitanate solution and methanol as a solvent by sol-gel dip coating technique. TiO{sub 2} thin films prepared using a sol-gel process have been analyzed for different annealing temperatures. Structural properties in terms of crystal structure were investigated by Raman spectroscopy. The surface morphology and composition of the films were investigated by atomic force microscopy (AFM). The optical transmittance and reflectance spectra of TiO{sub 2} thin films deposited on silicon substrate were also determined. Spectroscopic ellipsometry study was used to determine the annealing temperature effect on the optical properties and the optical gap of the TiO{sub 2} thin films. The results show that the TiO{sub 2} thin films crystallize in anatase phase between 400 and 800 deg. C, and into the anatase-rutile phase at 1000 deg. C, and further into the rutile phase at 1200 deg. C. We have found that the films consist of titanium dioxide nano-crystals. The AFM surface morphology results indicate that the particle size increases from 5 to 41 nm by increasing the annealing temperature. The TiO{sub 2} thin films have high transparency in the visible range. For annealing temperatures between 1000 and 1400 deg. C, the transmittance of the films was reduced significantly in the wavelength range of 300-800 nm due to the change of crystallite phase and composition in the films. We have demonstrated as well the decrease of the optical band gap with the increase of the annealing temperature.

  2. 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

  3. Preparation, characterization, and applications of a novel solid-phase microextraction fiber by sol-gel technology on the surface of stainless steel wire for determination of poly cyclic aromatic hydrocarbons in aquatic environmental samples

    International Nuclear Information System (INIS)

    Es-haghi, Ali; Hosseininasab, Valiallah; Bagheri, Habib

    2014-01-01

    Graphical abstract: - Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. - Abstract: A novel solid-phase microextraction(SPME) fiber was prepared using sol–gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME–GC–MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been evaluated and optimized. In the next step, the validation of the new method have been performed, finding it to be specific in the trace analysis of PAHs, with the limit of detection (LOD) ranging from 0.01 to 0.5 μg L −1 and the linear range from the respective LOD to 200 μg L −1 with RSD amounting to less than 8%. The thermal stability of the fibers was investigated as well and they were found to be durable at 280 °C for 345 min. Furthermore, the proposed method was successfully applied for quantification of PAHs in real water samples

  4. Preparation, characterization, and applications of a novel solid-phase microextraction fiber by sol-gel technology on the surface of stainless steel wire for determination of poly cyclic aromatic hydrocarbons in aquatic environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Es-haghi, Ali, E-mail: a.eshaghi@rvsri.ac.ir [Department of Physico Chemistry, Razi Vaccine and Serum Research Institute, PO Box 31975/148, Karaj (Iran, Islamic Republic of); Hosseininasab, Valiallah; Bagheri, Habib [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, PO Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2014-02-01

    Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. Abstract: A novel solid-phase microextraction(SPME) fiber was prepared using sol–gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME–GC–MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been evaluated and optimized. In the next step, the validation of the new method have been performed, finding it to be specific in the trace analysis of PAHs, with the limit of detection (LOD) ranging from 0.01 to 0.5 μg L⁻¹ and the linear range from the respective LOD to 200 μg L⁻¹with RSD amounting to less than 8%. The thermal stability of the fibers was investigated as well and they were found to be durable at 280 °C for 345 min. Furthermore, the proposed method was successfully applied for quantification of PAHs in real water samples.

  5. 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)

  6. Surface Behavior of Rhodamin and Tartrazine on Silica-Cellulose Sol-Gel Surfaces by Thin Layer Elution

    Directory of Open Access Journals (Sweden)

    Surjani Wonorahardjo

    2016-05-01

    Full Text Available Physical and chemical interactions are the principles for different types of separation systems as the equillibrium dynamics on surface plays a key-role. Surface modification is a way for selective separation at interfaces. Moreover, synthesis of gel silica by a sol-gel method is preferred due to the homogeneity and surface feature easily controlled. Cellulose can be added in situ to modified the silica features during the process. Further application for to study interaction of rhodamin and tartrazine in its surface and their solubilities in mobile phase explains the possibility for their separation. This paper devoted to evaluate the surface behavior in term of adsorption and desorption of tartrazine and rhodamin on silica-cellulose thin layer in different mobile phase. Some carrier liquids applied such as methanol, acetone, n-hexane and chloroform. The result proves tartrazine and rhodamin is separated and have different behavior in different mobile phase. The retardation factors (Rf of the mixtures suggest complexity behavior on silica-cellulose surface.

  7. Lattice Constant Dependence on Particle Size for Ceria prepared from a Citrate Sol-Gel

    International Nuclear Information System (INIS)

    Morris, V N; Farrell, R A; Sexton, A M; Morris, M A

    2006-01-01

    High surface area ceria nanoparticles have been prepared using a citrate solgel precipitation method. Changes to the particle size have been made by calcining the ceria powders at different temperatures, and X-ray methods used to determine their lattice parameters. The particle sizes have been assessed using transmission electron microscopy (TEM) and the lattice parameter found to fall with decreasing particle size. The results are discussed in the light of the role played by surface tension effects

  8. Evaluation of bulk and surfaces absorption edge energy of sol-gel-dip-coating SnO2 thin films

    Directory of Open Access Journals (Sweden)

    Emerson Aparecido Floriano

    2010-12-01

    Full Text Available The absorption edge and the bandgap transition of sol-gel-dip-coating SnO2 thin films, deposited on quartz substrates, are evaluated from optical absorption data and temperature dependent photoconductivity spectra. Structural properties of these films help the interpretation of bandgap transition nature, since the obtained nanosized dimensions of crystallites are determinant on dominant growth direction and, thus, absorption energy. Electronic properties of the bulk and (110 and (101 surfaces are also presented, calculated by means of density functional theory applied to periodic calculations at B3LYP hybrid functional level. Experimentally obtained absorption edge is compared to the calculated energy band diagrams of bulk and (110 and (101 surfaces. The overall calculated electronic properties in conjunction with structural and electro-optical experimental data suggest that the nature of the bandgap transition is related to a combined effect of bulk and (101 surface, which presents direct bandgap transition.

  9. Preparation of nitrogen-doped titania using sol-gel technique and its photocatalytic activity

    International Nuclear Information System (INIS)

    Qin Haoli; Gu Guobang; Liu Song

    2008-01-01

    Yellowish nitrogen-doped titania was produced through sol-gel method at room temperature, with the elemental nitrogen derived from aqua ammonia. The titania catalysts were characterized using TG-DSC, XRD, BET, TEM, and UV-vis diffuse reflectance spectrophotometer. Methyl orange (MO) and 2-mercaptobenzothiazole (MBT) were used in this study as model chemicals and both the adsorption isotherm and photocatalytic activity of the nitrogen-doped titania catalysts were evaluated based on the MO and MBT photodegradation in aqueous solution under UV and visible light, respectively. The results showed that all titania catalysts were anatase. The crystallite size of nitrogen-doped ones increased with the increase of N/Ti proportion, both the adsorption capacity and adsorption equilibrium constants of the nitrogen-doped titania catalysts were improved by the doping of nitrogen. The doping of nitrogen could extend the absorption shoulder into the visible-light region, thus nitrogen-doped titania possessed visible-light activity illustrated by that higher capability of degradation of MO and MBT under the irradiation of visible light, whereas the pure ones showed little such kind of visible-light activity. The kinetics of the MO and MBT photodegradation using different nitrogen-doped titania were also studied, the experiments demonstrated that there was an optimum N/Ti proportion of 4 mol% to exhibit the highest visible-light activity. The UV activity of nitrogen-doped titania catalysts were worse than that of the pure one and Degussa P-25. In addition, nitrogen-doped titania had weakened appreciably activity in the visible-light region as the N/Ti proportion increased, while a reverse relationship exists for the UV light. It was concluded that the enhancement of MO and MBT photodegradation using the nitrogen-doped titania catalysts mainly involved in both the improvement of the organic substrate adsorption in catalysts suspension and the enhancement of the separation of electron

  10. Influence of Ce(III/Ce(IV - supplements on the Characteristics of Humidity Sensors with TiO2 Films Prepared via a Sol-gel Method

    Directory of Open Access Journals (Sweden)

    Kozhukharov, S.

    2013-04-01

    Full Text Available Humidity sensors have been prepared via a sol-gel method to deposit TiO2 films with additions of Ce-compounds on alumina substrates, with interdigitated silver palladium electrodes. Observations by scanning electron microscopy (SEM were performed in order to determine the surface morphology of the respective layers. Structural and compositional characterization was done by X-ray diffraction analysis (XRD, and energy dispersive X-ray spectroscopy (EDX for investigation of the relation between the film structures and the parameters of the respective sensors. The influence of Ce-compounds on the electrical characteristics of the samples as humidity sensing elements has been evaluated by an impedance analyzer.Los sensores de humedad han sido desarrollados mediante el método sol-gel para depositar películas superficiales basadas en TiO2 con adiciones de compuestos de cerio sobre sustratos de corindón y electrodos de aleación de plata y paladio. Se han realizado observaciones mediante el Microscopio Electrónico de Barrido (MEB para determinar la morfología superficial de las capas respectivas. Las caracterizaciones de la estructura y composición han sido realizadas mediante Difracción de Rayos X (DRX y espectroscopía de dispersión energética de rayos X (EDERX, con el fin de investigar la relación entre la estructura de las capas y los parámetros de los sensores respectivos. La influencia de los compuestos de cerio sobre las características eléctricas de los sensores de humedad obtenidos se ha evaluado mediante el análisis de impedancia eléctrica.

  11. Preparation of titanium oxide and metal titanates as powders, thin films, and microspheres by complex sol-gel process

    International Nuclear Information System (INIS)

    Deptula, A.; Olczak, T.; Lada, W.; Chmielewski, A.G.; Jakubaszek, U.; Sartowska, B.; Goretta, K.C.; Alvani, C.; Casadio, S.; Contini, V.

    2006-01-01

    Titanium oxide, for many years an important pigment, has recently been applied widely as a photocatalyst or as supports for metallic catalysts, gas sensors, photovoltaic solar cells, and water and air purification devices. Titanium oxide (TiO 2 ) and titanates based on Ba, Sr and Ca were prepared from commercial solutions of TiCl 4 and HNO 3 . The main preparation steps for the sols consisted of elimination of Cl - by distillation with HNO 3 and addition of metal hydroxides for the titanates. Resulting sols were gelled and used to: (a) prepare irregularly shaped powders by evaporation; (b) produce by a dipping technique thin films on glass, Ag or Ti supports; (c) produce spherical powders (diameters <100 μm) by solvent extraction. Results of thermal and X-ray-diffraction analyses indicated that the temperatures required to form the various compounds were lower than those necessary to form the compounds by conventional solid-state reactions and comparable to those required with use of organometallic based sol-gel methods. Temperatures of formation could be further reduced by addition of ascorbic acid (ASC) to the sols

  12. Effect of ammonium hydroxide on preparation process of YBa2Cu3O7-x superconductor by sol gel method

    Directory of Open Access Journals (Sweden)

    H Arabi

    2006-09-01

    Full Text Available  In this paper the effect of ammonium hydroxide addition to the solution of metallic oxide on sol gel preparation process of YBCO is studied with differential thermal analysis, thermal graviometry and X-ray diffraction. Two samples with and without ammonium hydroxide. Ammonium hydroxide prevents both barium nitrate precipitate during the gel preparation and also unwanted reaction as well as increasing homogeneous product. After drying the gel, the samples heated up to 1050°C in DTA apparatus in order to find more accurate the type and the temperature of reaction during the preparation process. After the initial reactions in the samples, Y2Cu2O5 and 123 phases are created in the range of 780-840°C and then the 123 phase is strengthened at 900-950°C. As shown in X-ray data, 123 was the only phase after this range. In addition ammonium hydroxide support and increase the creation of 123 phase at lower temperature.

  13. 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.

  14. 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.

  15. Preparation of CuAlO2 Thin Films by Sol-Gel Method Using Nitrate Solution Dip-Coating

    Directory of Open Access Journals (Sweden)

    Ehara Takashi

    2016-01-01

    Full Text Available CuAlO2 thin films are prepared by sol-gel dip-coating followed by annealing in nitrogen atmosphere using copper nitrate and aluminum nitrate as metal source materials. X-ray diffraction (XRD patterns show (003, (006 and (009 oriented peaks of CuAlO2 at annealing temperature of 800 – 1000°C. This result indicates that the CuAlO2 films prepared in the present work are c-axis oriented. XRD peak intensity increase with annealing temperature and becomes maximum at 850°C. The CuAlO2 XRD peak decreased at annealing temperature of 900°C with appearance of a peak of CuO, and then increased again with annealing temperature until 1000 °C. The films have bandgap of 3.4 eV at annealing temperature of 850°C in which the transparency becomes the highest. At the annealing temperature of 850°C, scanning electron microscope (SEM observation reveals that the films are consist of amorphous fraction and microcrystalline CuAlO2 fraction.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    2000-01-01

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

  18. ZnO-SiO{sub 2} based nanocomposites prepared by a modified sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Grigorie, Alexandra Carmen [Politehnica University Timisoara, Faculty of Industrial Chemistry and Environmental Engineering, 6 V. Parvan Blv., RO-300223, Timisoara (Romania); Muntean, Cornelia, E-mail: cornelia.muntean@upt.ro [Politehnica University Timisoara, Faculty of Industrial Chemistry and Environmental Engineering, 6 V. Parvan Blv., RO-300223, Timisoara (Romania); Politehnica University Timisoara, Research Institute for Renewable Energy, 2 Piata Victoriei, RO-300006, Timisoara (Romania); Vlase, Titus [West University of Timisoara, 4 V. Parvan Blv., RO-300223, Timisoara (Romania); Locovei, Cosmin [Politehnica University Timisoara, Research Institute for Renewable Energy, 2 Piata Victoriei, RO-300006, Timisoara (Romania); Politehnica University Timisoara, Faculty of Mechanical Engineering, 1 Mihai Viteazul Blv., RO-300222, Timisoara (Romania); Stefanescu, Mircea [Politehnica University Timisoara, Faculty of Industrial Chemistry and Environmental Engineering, 6 V. Parvan Blv., RO-300223, Timisoara (Romania)

    2017-01-15

    This paper presents a study on nanocomposites formation in ZnO-SiO{sub 2} systems with different ZnO:SiO{sub 2} molar ratios (1:4, 1:1, and 4:1), prepared employing a sol-gel method modified by an original procedure. The evolution of ZnO-SiO{sub 2} systems depending on the composition and temperature was studied by thermal analysis, Fourier transform infrared spectroscopy, X-ray diffractometry and transmission electron microscopy. Zn(II) carboxylate was synthesized in situ in hybrid silica gels by redox reaction between zinc nitrate and 1,3-propanediol. Its thermal decomposition at low temperatures led to ZnO dispersed in the pores of silica matrix. Only for the 4:1 system, at 400 and 600 °C, ZnO nanocrystallites (average size ∼9 nm) embedded in the amorphous silica matrix were obtained, the other systems being amorphous. Whatever the mixture composition is, above 600 °C, ZnO reacts with SiO{sub 2} to form zinc silicate. At 800 °C, for both 1:4 and 1:1 systems, poor crystallized β-Zn{sub 2}SiO{sub 4} and α-Zn{sub 2}SiO{sub 4} phases embedded in silica matrix were formed. Increasing the temperature, at 1000 °C, only for 1:1 system, β-Zn{sub 2}SiO{sub 4} phase turned into single phase α-Zn{sub 2}SiO{sub 4} (average crystallites size 28.3 nm). For 4:1 composition, at 800 and 1000 °C, systems consisting of ZnO and α-Zn{sub 2}SiO{sub 4} nanocrystallites dispersed in silica were obtained. - Highlights: • By modified sol-gel method, ZnO/SiO{sub 2} and Zn{sub 2}SiO{sub 4}/SiO{sub 2} nanocomposites were obtained. • ZnO dispersed in silica matrix results from zinc carboxylate thermal decomposition. • Zinc carboxylate was synthesized in situ in hybrid silica gels via redox reaction. • Evolution of ZnO in SiO{sub 2} matrix depends on temperature and system composition.

  19. Preparation of Organic-Inorganic Multifunctional Nanocomposite Coating via Sol-Gel Routes

    International Nuclear Information System (INIS)

    Li Haoying; Chen Yunfa; Ruan Chengxiang; Gao Weimin; Xie Yusheng

    2001-01-01

    The inorganic-organic nanocomposite coatings are prepared on poly(methyl methacrylate) (PMMA) substrate by the spinning technique which involves incorporating homogeneously nanosized ZnO particle into the molecular inorganic-organic hybrid matrices. The hybrid matrices are derived from tetraethoxyasilane (TEOS) and 3-glycidoxypropyltrimethoxyailane (GLYMO). To avoid the destruction of the polymer structure caused by ZnO and modify the interface between nanoparticles and organic groups, ZnO was first surface-coated with SiO 2 from hydrolyzed TEOS using ammonia water as catalyst. The coatings thus obtained are dense, flexible, abrasion resistant and UV absorbent

  20. 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.

  1. Effect of urea on the photoactivity of titania powder prepared by sol-gel method

    International Nuclear Information System (INIS)

    Cheng Ping; Deng Changsheng; Gu Mingyuan; Dai Xiaming

    2008-01-01

    The synthesis of nanocrystalline titania powders from the hydrolysis of Ti(OBu n ) 4 in the presence of urea was investigated. DRS results showed that a redshift occurred in the absorption edge of titania with increasing the content of urea. XRD results indicated that urea showed a retarding effect on the transformation of titania from anatase to rutile. Moreover, the addition of urea resulted in a higher Brunauer-Emmett-Teller (BET) surface area as well as a larger average pore size of TiO 2 nanoparticles. The average pore size of urea/TiO 2 gels calcined at 500 deg. C increased with the increase of urea content, while the specific surface area increased with the amount of urea to reach a maximum at 10% and then decreased with further increase of the amount of urea. The maximal specific surface area of 64.4 m 2 g -1 was obtained for 10% urea/TiO 2 gels calcined at 500 deg. C, which showed an average particle size of 15 nm and pore size distribution in the range of mesopores centered at 5.8 nm. The photocatalytic experiments exhibited that titania nanoparticles prepared in the presence of urea could effectively photodegrade methyl orange under visible light irradiation due to the redshift of the absorption edge. The maximum photoactivity was achieved when the content of urea was 10%, which was attributed to the higher specific surface area

  2. Electrochemical properties of Li2 FeSiO4 /C nanocomposites prepared by sol-gel and hydrothermal methods

    Science.gov (United States)

    Kumar, Ajay; Jayakumar, O. D.; Naik, Vaman M.; Nazri, Gholam A.; Naik, Ratna

    Li2FeSiO4 is considered as potential cathode material for next generation lithium ion batteries because of its high specific theoretical capacity, low cost, and safety. However, it suffers from poor electronic conductivity and slow lithium ion diffusion in the solid phase. To address these issues, we have studied mesoporous Li2FeSiO4/C composites synthesized by sol-gel (SG) and hydrothermal (HT) methods using tri-block copolymer (P123) as carbon source and structure directing agent. The structure and morphology of the composites were characterized by XRD, SEM and TEM and the surface area and pore size distribution were measured by using N2 adsorption/desorption. Galvanostatic cycling, electrochemical impedance spectroscopy, and cyclic voltammetry were used to evaluate the electrochemical performance of the Li2FeSiO4/C composites. The Li2FeSiO4/C (HT) composites show a superior electrochemical performance compared to Li2FeSiO4/C (SG). At C/30 rate, the discharge capacity of Li2FeSiO4/C (HT) reached ~276 mAh/g in the 1.5-4.6 V window and shows better rate capability and stability at high rates. We attribute the improved electrochemical performance of Li2FeSiO4/C (HT) to its large surface area and reduced particle size. The details of the study will be presented.

  3. X-ray line profile analysis of BaTiO3 thin film prepared by sol-gel deposition

    Science.gov (United States)

    Ooi, Zeen Vee; Saif, Ala'eddin A.; Wahab, Yufridin; Jamal, Zul Azhar Zahid

    2017-04-01

    Barium titanate (BaTiO3) thin film was prepared using sol-gel method and spun-coated on SiO2/Si substrate. The phase and crystallinity of the synthesized film were identified using X-ray diffractometer (XRD), which scanned at the range of 20° to 60°. The phase and lattice parameters of the fabricated film were extracted from the recorded XRD patterns using lattice geometry equations. The crystallite size and lattice strain were determined using X-ray line profile analysis (XLPA) with various approaches. The Scherrer equation was applied to the perovskite peaks of the film to explore the size contribution on the peak broadening. Meanwhile, the Williamson-Hall and size-strain plot (SSP) methods were used to review two main independent contributions, i.e. crystallite sizes and lattice strain, on the X-ray line broadening. From the analysis, it is found that Scherrer method gives smallest crystallite size value by ignoring the strain-induced broadening effect. On the other hand, Williamson-Hall and SSP graphs revealed the existence of the lattice strain within the film, which contributes to the broadening in the Bragg peak. The results that analyzed via both techniques show a linear trend with all data points fitted. However, result obtained from SSP method gives better settlement due to the best fit of the data.

  4. Epitaxial growth of Er, Ti doped LiNbO3 films prepared by sol-gel method

    International Nuclear Information System (INIS)

    Takahashi, Makoto; Yoshiga, Tsuyoshi; Kajitani, Naofumi; Takeda, Yuki; Sato, Shoji; Wakita, Koichi; Ohnishi, Naoyuki; Hotta, Kazutoshi; Kurachi, Masato

    2006-01-01

    Erbium (Er 3+ ) doped lithium niobate (LiNbO 3 ) thick films were deposited on z-cut congruent LiNbO 3 (LN) substrate by the sol-gel method from the 0.20 mol/dm 3 precursor solution containing various Er 3+ concentration and 0.10 mol/dm 3 poly(vinyl alcohol) (PVA), and their crystal characteristics were evaluated. The Er 3+ concentration in the LN film was controlled by the Er 3+ concentration in the starting solution. The orientation relationships between Er doped LN films and substrates were determined by X-ray diffraction, Raman spectroscopy, and transmission electron microscopy, and (006) oriented Er doped LN epitaxial layers with parallel epitaxial relationships could be grown on the z-cut LN wafer. Moreover, it was made clear from the electron beam diffraction measurements that the film came to be polycrystalline, when the Er concentration was over 3 mol%. The refractive index of Er-doped LN films decreased with increasing Er concentration. 1.5 mol% Ti: 1.0 mol% Er LN films, which acted as a waveguide, were prepared by our so-gel method. It showed the 1530 nm emission by 980 nm excitation, which was considered to be due to the Er 3+ corresponding to the 4 I 13/2 → 4 I 15/2 transition. (author)

  5. Preparation and Scintillating Properties of Sol-Gel Eu3+, Tb3+ Co-Doped Lu2O3 Nanopowders

    Directory of Open Access Journals (Sweden)

    Joel Moreno Palmerin

    2011-09-01

    Full Text Available Nanocrystalline Eu3+, Tb3+ co-doped Lu2O3 powders with a maximum size of 25.5 nm were prepared by the sol-gel process, using lutetium, europium and terbium nitrates as precursors, and ethanol as a solvent. Differential thermal analysis (DTA and infrared spectroscopy (IR were used to study the chemical changes during the xerogel annealing. After the sol evaporation at 100 °C, the formed gel was annealed from 300 to 900 °C for 30 min under a rich O2 atmosphere, and the yielded product was analyzed by X-ray diffraction (XRD to characterize the microstructural behavior and confirm the crystalline structure. The results showed that Lu2O3 nanopowders start to crystallize at 400 °C and that the crystallite size increases along with the annealing temperature. A transmission electron microscopy (TEM study of samples annealed at 700 and 900 °C was carried out in order to analyze the microstructure, as well as the size, of crystallites. Finally, in regard to scintillating properties, Eu3+ dopant (5 mol%, Tb3+ codoped Lu2O3 exhibited a typical red emission at 611 nm (Do→7F2, furthermore, the effect of Tb3+ molar content (0.01, 0.015 and 0.02% mol on the Eu3+ radioluminiscence was analyzed and it was found that the higher emission intensity corresponds to the lower Tb3+ content.

  6. 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.

  7. Preparation and characterization of ultrafine alumina via sol-gel polymeric route

    Energy Technology Data Exchange (ETDEWEB)

    Ibrahim, D.M. [Ceramic Department, National Research Centre, Dokki, Cairo (Egypt); Abu-Ayana, Y.M. [Polymers and Pigments Department, National Research Centre, Dokki, Cairo (Egypt)], E-mail: yosreya20@gmail.com

    2008-10-15

    Ultrafine alumina powder was prepared through resin formation between urea and formaldehyde. Aluminium stearate soap was introduced during resin preparation. Ethylene glycol was used to terminate the thermosetting reaction. Calcination of the product was carried out at 700, 1000, 1100, 1300 and 1400 deg. C to obtain aluminium oxide. IR and Raman spectroscopic analysis indicated the occupation of Al{sup 3+} at different sites in the polymer network (C=O, -NH{sub 2}, C-O, -NH, and -CH{sub 2}OH). X-ray diffraction of powder calcined at 1000 deg. C revealed the presence of a mixture of {alpha}- and {theta}-alumina together, while a mixture of {alpha}- and {beta}-alumina phases were obtained on calcination at 1400 deg. C. Transmission electron microscope (TEM) examination of the powder fired at 700 deg. C showed uniform grains in the form of clusters with average size between 22.02 and 30.5 nm. Clusters are multi-particles as evident from the electron diffraction pattern. Crystallite size of alumina powder calcined at 1000 deg. C was found to be {approx}25.67 nm, while that of powder calcined at1400 deg. C was {approx}30.52 nm. The calculated specific surface area of alumina powder calcined at 1000 deg. C was 59.17 m{sup 2} g{sup -1}, while that calcined at 1400 deg. C was 49.77 m{sup 2} g{sup -1}.

  8. Spectral features and antibacterial properties of Cu-doped ZnO nanoparticles prepared by sol-gel method

    Science.gov (United States)

    Alireza, Samavati; A, F. Ismail; Hadi, Nur; Z, Othaman; M, K. Mustafa

    2016-07-01

    Zn1-x Cu x O (x = 0.00, 0.01, 0.03, and 0.05) nanoparticles are synthesized via the sol-gel technique using gelatin and nitrate precursors. The impact of copper concentration on the structural, optical, and antibacterial properties of these nanoparticles is demonstrated. Powder x-ray diffraction investigations have illustrated the organized Cu doping into ZnO nanoparticles up to Cu concentration of 5% (x = 0.05). However, the peak corresponding to CuO for x = 0.01 is not distinguishable. The images of field emission scanning electron microscopy demonstrate the existence of a nearly spherical shape with a size in the range of 30-52 nm. Doping Cu creates the Cu-O-Zn on the surface and results in a decrease in the crystallite size. Photoluminescence and absorption spectra display that doping Cu causes an increment in the energy band gap. The antibacterial activities of the nanoparticles are examined against Escherichia coli (Gram negative bacteria) cultures using optical density at 600 nm and a comparison of the size of inhibition zone diameter. It is found that both pure and doped ZnO nanoparticles indicate appropriate antibacterial activity which rises with Cu doping. Project supported by the Universiti Teknologi Malaysia (UTM) (Grant No. R. J1300000.7809.4F626). Dr. Samavati is thankful to RMC for postdoctoral grants.

  9. Effect of sol concentration on the properties of ZnO thin films prepared by sol-gel technique

    International Nuclear Information System (INIS)

    Dutta, M.; Mridha, S.; Basak, D.

    2008-01-01

    ZnO thin films are deposited on the glass substrates by sol-gel drain coating technique by varying the concentration of the sol. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis were used to investigate the effect of sol concentration on the crystallinity and surface morphology of the films. The results show that with increase in sol concentration, the value of full width at half maximum (FWHM) of (0 0 2) peak decreases while the strain first increases and then decreases. The sol with higher concentration results in the increase in the grain size. The studies on the optical properties show that the band gap value increases from 3.27 to 3.3 eV when the sol concentration changes from 0.03 to 0.1 M. The photoconductivity studies reveal that the film for 0.05 M sol shows the maximum photoresponse for ultraviolet (UV) wavelength (<400 nm) which is co-related with the deep-level defects. The growth and decay of the photocurrent is found to be slowest for the same film

  10. Spectral features and antibacterial properties of Cu-doped ZnO nanoparticles prepared by sol-gel method

    International Nuclear Information System (INIS)

    Samavati, Alireza; Nur, Hadi; Othaman, Z; Ismail, A F; Mustafa, M K

    2016-01-01

    Zn 1−x Cu x O (x = 0.00, 0.01, 0.03, and 0.05) nanoparticles are synthesized via the sol-gel technique using gelatin and nitrate precursors. The impact of copper concentration on the structural, optical, and antibacterial properties of these nanoparticles is demonstrated. Powder x-ray diffraction investigations have illustrated the organized Cu doping into ZnO nanoparticles up to Cu concentration of 5% ( x = 0.05). However, the peak corresponding to CuO for x = 0.01 is not distinguishable. The images of field emission scanning electron microscopy demonstrate the existence of a nearly spherical shape with a size in the range of 30–52 nm. Doping Cu creates the Cu–O–Zn on the surface and results in a decrease in the crystallite size. Photoluminescence and absorption spectra display that doping Cu causes an increment in the energy band gap. The antibacterial activities of the nanoparticles are examined against Escherichia coli (Gram negative bacteria) cultures using optical density at 600 nm and a comparison of the size of inhibition zone diameter. It is found that both pure and doped ZnO nanoparticles indicate appropriate antibacterial activity which rises with Cu doping. (paper)

  11. Effect of annealing temperature on the tribological behavior of ZnO films prepared by sol-gel method

    International Nuclear Information System (INIS)

    Lin Liyu; Kim, Dae-Eun

    2009-01-01

    The tribological behavior of zinc oxide (ZnO) films grown on glass and silicon (100) substrates by sol-gel method was investigated. Particularly, the as-coated films were post-annealed at different temperatures in air to investigate the effect of annealing temperature. Crystal structural and surface morphology of the films were measured by X-ray diffraction (XRD) and Atomic Force Microscopy (AFM). XRD patterns and AFM images indicated that the crystallinity and grain size of the films were enhanced and increased, respectively, with temperature. The tribological behavior of films was evaluated by sliding the ZnO films against a Si 3 N 4 ball under 0.5 gf normal load using a reciprocating pin-on-plate tribo-tester. The wear tracks of the films were measured by AFM to quantify the wear resistance of the films. The results showed that the wear resistance of the films could be improved by the annealing process. The wear resistance of the films generally increased with annealing temperature. Specifically, the wear resistance of the films was significantly improved when the annealing temperature was higher than 550 deg. C. The increase in the wear resistance is attributed to the increase in hardness and modulus of the film with annealing temperature

  12. Moessbauer studies of SnO2 powders doped with dilute 57Fe, prepared by a sol-gel method

    International Nuclear Information System (INIS)

    Nomur, K.; Sakuma, J.; Takeda, M.

    2006-01-01

    Diluted magnetic semiconductor (DMS) is prospected as new materials with both semiconductor and magnetic properties. In order to confirm these phenomena, we prepared the powders of SnO 2 doped with various amount of 57 Fe by a sol-gel method. Various compositions of Sn 1-x 57 Fe x O 2 were obtained by mixing some ratio of Fe 3+ nitrate solution and acetylacetonate Sn 4+ complex in the ethylene glycol and citric acid solution. The solutions were evaporated, ashed at around 200 grad C, and finally annealed at 500 grad C, 600 grad C, and 650 grad C, respectively. These Sn 1-x 57 Fe x O 2 (x=0.005, 0.01, 0.03 and 0.05) were measured by XRD, VSM, and Moessbauer spectrometry. The prepared powder samples were confirmed to be a rutile structure, but iron compounds were not detected by XRD. Moessbauer spectra of Sn 1-x 57 Fe x O 2 prepared at 500 grad C were shown in Fig. 1. A small amount of broad sextets were observed in MS spectra of Sn 1-x 57 Fe x O 2 in addition to paramagnetic components. The relative intensity seems to be strong with the decrease of the amount of doped Fe. Moessbauer spectrum at 10 K shows clearly the magnetic components. The magnetic sextet was observed in MS spectra of samples prepared at 650 grad C, but the magnetic behavior weakened because of antiferromagnetic α-Fe 2 O 3 , produced due to the phase separation at high temperatures. (authors)

  13. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Rau, J.V., E-mail: giulietta.rau@ism.cnr.it [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Teghil, R. [Universita della Basilicata, Dipartimento di Chimica ' A.M. Tamburro' , Via dell' Ateneo Lucano, 10-85100 Potenza (Italy); CNR-IMIP U.O.S. di Potenza, Zona Industriale di Tito scalo (PZ) (Italy); Fosca, M. [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Universita di Roma ' La Sapienza' , Dipartimento di Chimica, Piazzale Aldo Moro, 5-00185 Rome (Italy); De Bonis, A. [Universita della Basilicata, Dipartimento di Chimica ' A.M. Tamburro' , Via dell' Ateneo Lucano, 10-85100 Potenza (Italy); CNR-IMIP U.O.S. di Potenza, Zona Industriale di Tito scalo (PZ) (Italy); Cacciotti, I.; Bianco, A. [Universita di Roma ' Tor Vergata' , Dipartimento di Ingegneria Industriale, UR INSTM ' Roma Tor Vergata' , Via del Politecnico, 1-00133 Rome (Italy); Albertini, V. Rossi [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Caminiti, R. [Universita di Roma ' La Sapienza' , Dipartimento di Chimica, Piazzale Aldo Moro, 5-00185 Rome (Italy); Ravaglioli, A. [Parco Torricelli delle Arti e delle Scienze, Via Granarolo, 64-48018 Faenza (Ra) (Italy)

    2012-05-15

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

  15. Laboratory sol-gel preparation of fine fraction of sintered uranium dioxide spheres

    International Nuclear Information System (INIS)

    Landspersky, H.; Tympl, M.

    1984-01-01

    The results are summed up of the laboratory investigation of preparing the fine fraction of sintered uranium dioxide particles from uranyl gel using the method of the mixed reactor and the method of the dual-liquid nozzle, processed by leaching, drying, calcination and sintering. None of the two methods provides monodispersion particles under the given conditions but better control of the throughflow of the liquid media may improve results. Leaching of the fine fraction is very quick and the leaching of most components takes no longer than 5 minutes. In view of the fact that leaching of all components does not proceed at the same rate it is recommended that leaching time be doubled, or that leaching take place in two stages. Azeotropic distillation with chlorinated hydrocarbons is a favourable procedure for obtaining quality material; it is, however, necessary to prevent dried particles from comino. into contact with the water phase condensing on the walls of the distillation vessel and running down onto the surface of the distilling mixture. Calcination at a temperature of 500 degC in a thin layer and sintering at temperatures between 1350 and 1550 degC at an adequate rate of inflow of gaseous media and adequate rate of outflow of reaction wastes results in the production of high quality material whose density exceeds 97 to 98% theoretical density. (author)

  16. Physico-Chemical Characterization and Interfacial Electrochemical Properties of Nanoparticles of Anatase-TiO2 Prepared by the Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Ikram Daou

    2013-07-01

    Full Text Available In this work, we prepared by the sol-gel method titanium dioxide nanoparticles having a large specific area (SBET = 218 m2/g. The isotherm of N2 adsorption-desorption at 77K revealed that it concerns a mesoporous solid with a maximum pore diameter of 43 Å. The X-ray diffraction showed that the solid is constituted of the anatase phase. The transmission electron microscopy revealed us that the synthesized grains of TiO2 are of nanometric sizes (diameter between 8 and 20 nm and manifest under agglomerated shape. The study of its solubility in dispersing phase, by conductometric titrations, showed that the prepared solid is totally insoluble in all the domain of the studied pH. The measured inter-facial electrochemical properties, based on the isotherms of ionic adsorption and the conductometric titrations, are: the point of zero charge found equal to 6,2±0,1, the total number of sites of surface found equal to 5,8 OH/nm2 and the nature of action of the dispersed phase on the dispersing phase which is found organizer of the structure of water. Besides, the difference of the ionizationconstants pK is found superior to 4 for all the adsorbed ions and the constants of surface complexation are independent from the nature of the adsorbed ion.

  17. Characteristics of Nanosize Spinel NixFe3-xO4 Prepared by Sol-Gel Method Using Egg White as Emulsifying Agent

    Directory of Open Access Journals (Sweden)

    Rudy Situmeang

    2015-07-01

    Full Text Available In this study, sol-gel method using egg white as emulsifying agent was applied to prepare nano size spinel NixFe3-xO4 (with x = 0.2–1. Sample preparation was carried out by mixing the solution of Fe(NO33.9 H2O and Ni(NO33.6 H2O with egg white, and then the sample was stirred thoroughly using magnetic stirrer. After freeze–drying process, the sample was subjected to calcination treatment and subsequently characterized. The phase composition was evaluated using the X-ray diffraction (XRD technique, followed by quantitative analysis using Rietveld and Debye-Scherrer Methods. The functionality of the sample was identified using Fourier Transform Infrared (FTIR spectroscopy, and surface morphology and elemental composition were analyzed using scanning electron microscopycoupled with electron dispersive spectroscopy (SEM/EDS. The results of XRD characterization indicated that materials consist of various crystalline phases, with NiFe2O4 as a major phase. FTIR Analysis revealed the existence of both Lewis and Brønsted–Lowry acid sites, with Lewis acid as the prominent site. The sample was found to display relatively homogeneous surface morphology, having the crystallite size in the range of 33 to 61 nm according to the Debye-Scherrer equation. The EDS data indicated that the ratio of Fe/Ni is in agreement with the composition of the raw materials used.

  18. Topography and surface energy dependent calcium phosphate formation on Sol-Gel derived TiO2 coatings.

    Science.gov (United States)

    Järn, Mikael; Areva, Sami; Pore, Viljami; Peltonen, Jouko; Linden, Mika

    2006-09-12

    Heterogeneous nucleation and growth of calcium phosphate (CaP) on sol-gel derived TiO(2) coatings was investigated in terms of surface topography and surface energy. The topography of the coatings was derived from AFM measurements, while the surface energy was determined with contact angle measurements. The degree of precipitation was examined with scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The precipitation of CaP was found to be dependent on both topography and surface energy. A high roughness value when combining the RMS roughness parameter S(q) with the number of local maxima per unit area parameter S(ds) enhances CaP formation. The hydrophilicity of the coating was also found to be of importance for CaP formation. We suggest that the water contact angle, which is a direct measure of the hydrophilicity of the surface, may be used to evaluate the surface energy dependent precipitation kinetics rather than using the often applied Lewis base parameter.

  19. Morphology of one-time coated palladium-alumina composite membrane prepared by sol-gel process and electroless plating technique

    Science.gov (United States)

    Sari, R.; Dewi, R.; Pardi; Hakim, L.; Diana, S.

    2018-03-01

    Palladium coated porous alumina ceramic membrane tube was obtained using a combination of sol-gel process and electroless plating technique. The thickness, structure and composition of palladium-alumina composite membrane were analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM). Palladium particle size was 6.18 to 7.64 nm. Palladium membrane with thickness of approximately 301.5 to 815.1 nm was formed at the outer surface of the alumina layer. EDX data confirmed the formation of palladium-alumina membrane containing 45% of palladium. From this research it shows the combination of sol-gel process and electroless plating technique with one-time coating can produce a homogeneous and smoother palladium nano layer film on alumina substrate.

  20. Preparation and characterization of the titanium dioxide thin films used for pH electrode and procaine drug sensor by sol-gel method

    International Nuclear Information System (INIS)

    Liao Yihung; Chou, J.-C.

    2009-01-01

    We used titanium dioxide (TiO 2 ) as the sensing layer of an ion selective pH sensor electrode, and as the substrate for a procaine drug sensitive membrane sensor. The TiO 2 thin films were prepared using sol-gel spin coating technology. We adopted the Ti(OC 4 H 9 ) 4 as the precursor, and added an ethanol solute to obtain the TiO 2 sol. The sol-gel was spun coated onto the indium tin oxide (ITO) substrate. The drug sensitive membrane was coated on the TiO 2 film. We then measured the I DS -V G curves of the TiO 2 ion selective electrode (ISE) pH sensor in pH buffer solutions that had different pH concentrations using a Keithley 236 Semiconductor Parameter Analyzer instrument. The procaine concentration was measured from 10 -2 M to 10 -6 M with the drug sensitive membrane using a HP 34401A Digital Multimeter. We prepared the TiO 2 ISE pH sensor and obtained a high pH sensitivity of 58.73 mV/pH. Uniform TiO 2 films surface structures, with an average roughness (Ra) of 10.211 nm and root mean square roughness (Rms) of 13.01 nm were obtained. The drift effect of the titanium dioxide ion selective pH sensor electrode is 1.97 mV h -1 . The sensitivity of the procaine drug sensor is 55.03 mV pC -1 between 1.0 x 10 -2 mol L -1 and 1.0 x 10 -6 mol L -1 procaine concentrations. The detection limit is 5.0 x 10 -6 mol L -1 . The response time to reach 90% output voltage is 16 s. Forty seconds are required to reach 95% output voltage. The procaine drug sensor 1 x 10 -3 mol L -1 drift test is 3.64 mV h -1 and the variation in output voltage of the repeated measurement is less than 7.4 mV

  1. Preparation and properties of TiO2 films by complexing agent-assisted sol-gel method. Yuki haiishi wo mochiita sol gel ho ni yoru TiO2 usumaku no sakusei to seishitsu

    Energy Technology Data Exchange (ETDEWEB)

    Nishide, T [Nissan Motor Co. Ltd., Tokyo (Japan); Mizukami, F [National Chemical Laboratory for Industry, Tsukuba (Japan)

    1992-09-01

    In order to control optical properties of TiO2 thin films, the TiO2 films were prepared by the sol-gel method using glycols or their ether derivatives as organic ligands to study the effect of the organic ligands on the refractive indices and crystal phases. Samples were prepared as follows: Organic ligand was added into the ethanol solution of Ti(O-iso-pr) 4, and aqueous nitric acid solution was added after reflux, and sol obtained by subsequent reflux was applied on soda lime glass or silicon wafer substrates, which were baked at 400 to 900 centigrade. Three kinds of ligand such as 2-(2-methoxyethoxy) ethanol were used. Measured items are the film thickness, thermal characteristics, crystal phase and refractive indices of thin films. The key points are as follows: In case of TiO2 thin films on the soda lime glass substrate, the changing pattern of refractive indices by temperature changes with the kind of ligand used and further the peak strength of anatase changes with the kind of ligand used. In case of silicon wafer substrates, the peak strength of anatase and rutile changes with the kind of ligand. The refractive indices and crystal phase can be controlled by properly using the ligand. 7 refs., 11 figs.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2018-04-01

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

  3. Preparation and optical properties of mesoporous TiO2 thin films by a two-step sol-gel technique

    International Nuclear Information System (INIS)

    Kartini, I.; Lu, G.Q.; Meredith, P.; Zhao, X.S.

    2002-01-01

    This paper concerns the preparation of mesoporous titania nanopowders and thin films for use in next generation photoelectrochemical solar cells. We have recently developed a novel method for preparing mesoporous TiO 2 powders using a Two-Step Sol-gel method (TSS). These materials have crystalline domains characteristic of anatase. The first step of the process involves the hydrolysis of titanium isopropoxide in a basic aqueous solution mediated by neutral surfactant. The solid product resulting from Step-1 is then treated in acidified ethanol solution containing a titanium precursor to yield anatase TiO 2 . The resultant powder exhibits a high surface area and large pore volume with uniform mesopores. Slurries made from the resultant powder of Steps 1 and 2 have been used to produce thin titania films on glass slides. The optical and structural properties of these films have been compared to the films made of a commercial titania (Degussa P25, BASF). We will discuss these properties with respect to the possible use of such mesoporous titania films as the wide band gap semiconductor in dye-sensitized nanocrystalline TiO 2 solar cells

  4. Structural and optical studies of nano-structure silica gel doped with different rare earth elements, prepared by two different sol -gel techniques

    International Nuclear Information System (INIS)

    Battisha, I.K.; El Beyally, A.; Seliman, S.I.; El Nahrawi, A.S.

    2005-01-01

    Structural and optical characteristics of pure silica gel (silica-xerogel, SiO 2 ) and doped with different concentrations ranging from 1 up to 6% of some rare earth (REEs) ions such as, praseodymium Pr +3 ,and Europium Eu +3 , Erbium Er +3 and Holmium Ho +3 , ions, in the form of thin film and monolith materials were prepared by sol - gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural and optical features of sol-gel derived monolith and thin films are analyzed and compared, namely the structure of nano-particle monolith and thin film silica-gel samples, based on X-ray diffraction (XRD). The types of structural information obtainable are compared in detail. It is show that the XRD spectra of a-cristobalite are obtained for the two type materials and even by doping with the four REEs ions. Optical measurements of monolith and thin films were also studied and compared, the normal transmission and specular reflection were measured. The refractive index were calculated and discussed

  5. 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

  6. Effect of Y{sub 2}O{sub 3} addition on the crystal growth and sintering behavior of YSZ nanopowders prepared by a sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Kuo, C.-W.; Shen, Y.-H. [Department of Resources Engineering, National Chen Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hung, I-M. [Yuan Ze Fuel Cell Center, Department of Chemical Engineering and Materials Science, Yuan Ze University, 135 Yuan-Tung Road, Chung-Li, Taoyuan 320, Taiwan (China)], E-mail: imhung@saturn.yzu.edu.tw; Wen, S.-B. [General Education Center, Meiho Institute of Technology, 23 Pingguang Road, Neipu, Pingtung 91202, Taiwan (China); Lee, H.-E. [Faculty of Dentistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Wang, M.-C. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China)], E-mail: mcwang@kmu.edu.tw

    2009-03-20

    The effect of Y{sub 2}O{sub 3} (8 mol% {<=} Y{sub 2}O{sub 3} {<=} 10 mol%) addition on the crystal growth and sintering behavior of yttria-stabilized zirconia (YSZ) nanocrystallites prepared by a sol-gel process with various mixtures of ZrOCl{sub 2}.8H{sub 2}O and Y(NO{sub 3}){sub 3}.6H{sub 2}O ethanol-water solutions at low temperatures has been studied. X-ray diffraction (XRD), Brunauer-Emmett-Teller specific surface area analyses (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED) and dilatometric analysis (DA) have been utilized to characterize the YSZ nanocrystallites. Characterization reveals that the YSZ nanopowders are weakly agglomerated. When calcined at various temperatures for 2 h, the crystallite size increases and the surface area of the YSZ powders decreases when the calcination temperature increased from 673 to 1273 K. A nanocrystallite size distribution between 10 and 15 nm is obtained in the TEM examination, which is consistent with the XRD investigation. The activation energy for crystal growth were determined as 5.75 {+-} 0.68, 4.22 {+-} 0.51, and 5.24 {+-} 0.20 kJ/mol for 8, 9 and 10 YSZ precipitates, respectively. The morphology of the YSZ sintered at high temperature indicates the abnormal growth is due to the low activation energy for crystallite growth.

  7. Effect of Y2O3 addition on the crystal growth and sintering behavior of YSZ nanopowders prepared by a sol-gel process

    International Nuclear Information System (INIS)

    Kuo, C.-W.; Shen, Y.-H.; Hung, I-M.; Wen, S.-B.; Lee, H.-E.; Wang, M.-C.

    2009-01-01

    The effect of Y 2 O 3 (8 mol% ≤ Y 2 O 3 ≤ 10 mol%) addition on the crystal growth and sintering behavior of yttria-stabilized zirconia (YSZ) nanocrystallites prepared by a sol-gel process with various mixtures of ZrOCl 2 .8H 2 O and Y(NO 3 ) 3 .6H 2 O ethanol-water solutions at low temperatures has been studied. X-ray diffraction (XRD), Brunauer-Emmett-Teller specific surface area analyses (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED) and dilatometric analysis (DA) have been utilized to characterize the YSZ nanocrystallites. Characterization reveals that the YSZ nanopowders are weakly agglomerated. When calcined at various temperatures for 2 h, the crystallite size increases and the surface area of the YSZ powders decreases when the calcination temperature increased from 673 to 1273 K. A nanocrystallite size distribution between 10 and 15 nm is obtained in the TEM examination, which is consistent with the XRD investigation. The activation energy for crystal growth were determined as 5.75 ± 0.68, 4.22 ± 0.51, and 5.24 ± 0.20 kJ/mol for 8, 9 and 10 YSZ precipitates, respectively. The morphology of the YSZ sintered at high temperature indicates the abnormal growth is due to the low activation energy for crystallite growth

  8. CdO thin films based on the annealing temperature differences prepared by sol-gel method and their heterojunction devices

    Science.gov (United States)

    Soylu, M.; Yazici, T.

    2017-12-01

    Undoped CdO films were prepared on glass substrate and p-type silicon wafer using sol-gel spin coating method. The structural and optical properties of the films were investigated as a function of the annealing temperature. X-ray diffraction (XRD) patterns reveal that the films are formed from CdO with cubic crystal structure and (1 1 1) preferred orientation. It is seen that good crystallinity is due to the high annealing temperature. The surface morphology of the CdO films was found to be depending on the annealing temperature, showing cauliflower like structure. Optical band gaps for annealing temperature of 250 °C and 450 °C were found to be 2.49 eV and 2.27 eV, respectively, showing a decrease with raising temperature. Optics parameters such as extinction coefficient, refractive index, and surface-volume energy loss were determined with spectrophotometric analysis as a function of annealing temperature. CdO/p-Si heterojunction structure showed weak rectifying behavior. The diode parameters were found to be depending on annealing temperature. The results are encouraging to get better conjunction with CdO thin film component at optimize annealing temperature.

  9. Preparation of new crystal forms via photochemical, mechanochemical and sol-gel methods

    OpenAIRE

    D’Agostino, Simone

    2012-01-01

    This work of thesis involves various aspects of crystal engineering. Chapter 1 focuses on crystals containing crown ether complexes. Aspects such as the possibility of preparing these materials by non-solution methods, i.e. by direct reaction of the solid components, thermal behavior and also isomorphism and interconversion between hydrates are taken into account. In chapter 2 a study is presented aimed to understanding the relationship between hydrogen bonding capability and shape of the...

  10. Aggregation and growth of ZnO quantum dots prepared from sol-gel chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Santilli, C.V.; Pulcinelli, S.H.; Caetano, B.L. [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Araraquara, SP (Brazil); Briois, V.B [Synchrotron SOLEIL, Saint-Aubin (France)

    2016-07-01

    Full text: Herein we discuss in depth the mechanisms of growth control of ZnO quantum dots (Q-dot) prepared from the zinc oxy-acetate ethanolic solution by the addition of LiOH. Through in situ monitoring of Q-dot radii and of aggregation index calculated from UV-Vis absorption spectra and small-angle X-ray scattering (SAXS) the aggregation and growth of ZnO nanocrystal was well described from two kinetic models: during the first step (t< 50 min) the structural evolution is controlled by the coalescence caused by the oriented attachment between the nanocrystal aggregates while at the advanced time (t> 50 min) the Q-dot coarsening follows the Ostwald ripening (OR) mechanism. From the higher oriented attachment efficiency observed here as compared with early reported synthesis using NaOH and KOH, we propose an universal mechanism to control coalescence and coarsening of ZnO nanocrystal provided from the shield caused by the adsorption of the alkali cation. From X-ray diffraction and transmission electron microscopy results we demonstrate that this mechanism is also useful to prepare Q-dot powders with controlled size. (author)

  11. Sol-gel preparation of lead magnesium niobate (PMN) powders and thin films

    Science.gov (United States)

    Boyle, T.J.

    1999-01-12

    A method of preparing a lead magnesium niobium oxide (PMN), Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}, precursor solution by a solvent method wherein a liquid solution of a lead-complex PMN precursor is combined with a liquid solution of a niobium-complex PMN precursor, the combined lead- and niobium-complex liquid solutions are reacted with a magnesium-alkyl solution, forming a PMN precursor solution and a lead-based precipitate, and the precipitate is separated from the reacted liquid PMN precursor solution to form a precipitate-free PMN precursor solution. This precursor solution can be processed to form both ferroelectric powders and thin films. 3 figs.

  12. PREPARATION OF TITANIA SOL-GEL COATINGS CONTAINING SILVER IN VARIOUS FORMS AND MEASURING OF THEIR BACTERICIDAL EFFECTS AGAINST E. COLI

    Directory of Open Access Journals (Sweden)

    Diana Horkavcova

    2015-09-01

    Full Text Available The work describes titania coatings containing various forms of silver applied on a titanium substrate by a dip-coating sol-gel technique. Silver was added into the basic titania sol in form of colloid particles of Ag, crystals of AgNO3, particles of AgI, particles of Ag3PO4 and Ag3PO4 developed in situ (in the sol by reaction of AgNO3 with added calcium phosphate (brushite or monetite. Mechanically and chemically treated titanium substrates were dipped at a constant rate into individual types of sols. Subsequently, they were slowly fired. The fired coatings contained microcracks. All over the surface there were evenly distributed spherical nanoparticles of silver (Ag, AgNO3 or microcrystals of AgI and Ag3PO4. The prepared coatings were tested under static conditions for their bactericidal effects against gram-negative bacteria Escherichia coli (E. coli. The coated substrates were immersed into a suspension of E. coli in physiological solution for 24 and 4 hours. The basic titania coatings with no silver demonstrated no bactericidal properties. Very good bactericidal effect against E. coli in both types of bactericidal test showed the titania coatings with AgNO3, Ag3PO4 crystals and Ag3PO4 developed in situ.

  13. Effect of Sn doping on structural, mechanical, optical and electrical properties of ZnO nanoarrays prepared by sol-gel and hydrothermal process

    Science.gov (United States)

    Agarwal, Manish Baboo; Sharma, Akash; Malaidurai, M.; Thangavel, R.

    2018-05-01

    Undoped and Sn doped Zinc oxide nanorods were prepared by two step process: initially growth of seed layers by sol-gel spin coating technique and then zinc oxide nanorods by hydrothermal process using the precursors zinc nitrate hexahydrate, hexamine and tin chloride. The effects on the electrical, optical, mechanical and structural properties for various Sn concentrations were studied. The crystalline phase determination from X-ray diffraction (XRD) confirms that Sn doped ZnO nanorods have hexagonal wurtzite structure. The variations of stress and strain with different doping concentration of Sn in ZnO nanorods were studied. The doping effect on electrical properties and optical bandgap is estimated by current voltage characteristics and absorbance spectra respectively. The surface morphology was studied with field emission scanning electron microscope (FESEM), which shows that the formation of hexagonal nanorods arrays with increasing Sn concentration. The calculated value of Young's modulus of elasticity (Y) for all the samples remains same. These results can be used in optoelectronic devices.

  14. Sol-gel electrospinning preparation of hybrid carbon silica nanofibers for extracting organophosphorus pesticides prior to analyzing them by gas chromatography-ion mobility spectrometry.

    Science.gov (United States)

    Jafari, Mohammad T; Saraji, Mohammad; Kermani, Mansoure

    2018-07-13

    Carbon-silica hybrid nanofibers as high performance coatings for solid-phase microextraction fibers were used for analyzing some pesticides by using gas chromatography-corona discharge ion mobility spectrometry. To that end, the fibers were prepared by carbonizing sol-gel based on electrospun polyacrylonitrile and tetraethyl orthosilicate nanofibers as carbon and silica precursors, respectively. Different parameters affecting the electrospinning and the extraction processes including spinning distance, voltage, feeding rate, stirring rate, salt concentration, temperature and extraction time were optimized by response surface methodology. The method involved deionized water samples spiked with pesticides at different concentration levels. The calibration curves were linear in the ranges of 0.1-20 and 0.05-20 μg L -1 with determination coefficients (R 2 ) of 0.9976 and 0.9928 for malathion and chlorpyrifos, respectively. The limits of detection of 0.032 and 0.019 μg L -1 and the limits of quantification of 0.1 and 0.05 μg L -1 were found for malathion and chlorpyrifos, respectively. Acceptable reproducibility values were obtained with relative standard deviations (RSD, n = 3) lower than 6 and 15%, for intra-day and inter-day precision, respectively. Finally, the relative recoveries of the proposed method were calculated in the range of 80-111% for real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Synthesis and Characterization of Nanostructure Tio2/Anthraquenone (AQ Prepared by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Fadhela M. Hussein

    2017-11-01

    Full Text Available sol–gel technique conducted to synthesize nano titanium dioxide with anthraquenone (AQ relatively in acidic pH. Nanoparticles were characterized using techniques like, Scanning Electrion Microscope (SEM, Atomic Force Microscope (AFM, UV-Visible Spectrioscopy, X-ray diffraction (XRD, Fourier transform infrared (FT-IR, SEM picture display that the TiO2/AQ is spherical in style, the band gap of TiO2/AQ nanoparticle is (3.05eV, BET and BJH analysis provides Pore volume and specific Surface area and the kinetic studie Suggest that the reaction is pseudo first order and the rate of reaction was reduce with rising initial concentration for p-Nitrotolune.

  16. Superhydrophobic properties induced by sol-gel routes on copper surfaces

    Science.gov (United States)

    Raimondo, M.; Veronesi, F.; Boveri, G.; Guarini, G.; Motta, A.; Zanoni, R.

    2017-11-01

    Superhydrophobic surfaces are attracting increasing attention in different fields such as energy, transportation, building industry and electronics, as they exhibit many interesting properties such as high water repellence, anti-fogging, anti-corrosion, anti-fouling and self-cleaning abilities. Here, superhydrophobic nanostructured hybrid materials obtained by depositing alumina nanoparticles on copper surfaces via dip coating in Al2O3 sol are presented. Two different preparation routes were explored, based on either an alcoholic or an aqueous Al2O3 sol, and the resulting wetting properties were compared. Wettability measurements showed that when the alcoholic sol is used superhydrophobicity is attained, with values of water contact angle very close to the upper limit of 180°, while highly hydrophobic coatings are obtained with the aqueous sol. These findings were further supported by electron microscopy and X-ray photoelectron spectroscopy, which revealed that the surface layer deposited on Cu is more homogenous and richer in alumina nanoparticles when the alcoholic sol was used. Durability of the superhydrophobic coating was assessed by performing ageing tests in chemically aggressive environments. A remarkable resistance is displayed by the superhydrophobic coating in acid environment, while alkaline conditions severely affect its properties. Such behaviors were investigated by XPS and FE-SEM measurements, which disclosed the nature of the surface reactions under the different conditions tested. The present results underline that a thorough investigation of surface morphology, chemical composition and wetting properties reveals their strongly connection and helps optimizing the combination of substrate nanostructuring and suitable chemical coating for an improved durability in different aggressive environments.

  17. Thin TiO2 Films Prepared by Inkjet Printing of the Reverse Micelles Sol-Gel Composition

    Czech Academy of Sciences Publication Activity Database

    Morozová, Magdalena; Klusoň, Petr; Krýsa, Josef; Dzik, P.; Veselý, M.; Šolcová, Olga

    2011-01-01

    Roč. 160, č. 1 (2011), s. 371-378 ISSN 0925-4005 R&D Projects: GA ČR GD203/08/H032; GA ČR GA104/09/0694; GA AV ČR KAN400720701 Institutional research plan: CEZ:AV0Z40720504 Keywords : sol-gel * titanium oxide * inkjet printing Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.898, year: 2011

  18. Preparation of Flame Retardant Polyacrylonitrile Fabric Based on Sol-Gel and Layer-by-Layer Assembly.

    Science.gov (United States)

    Ren, Yuanlin; Huo, Tongguo; Qin, Yiwen; Liu, Xiaohui

    2018-03-23

    This paper aims to develop a novel method, i.e., sol-gel combined with layer-by-layer assembly technology, to impart flame retardancy on polyacrylonitrile (PAN) fabrics. Silica-sol was synthesized via the sol-gel process and acted as cationic solution, and phytic acid (PA) was used as the anionic medium. Flame-retardant-treated PAN fabric (FR-PAN) could achieve excellent flame retardancy with 10 bilayer (10BL) coating through layer-by-layer assembly. The structure of the fabrics was characterized by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The thermal stability and flame retardancy were evaluated by thermogravimetric (TG) analysis, cone calorimetry (CC) and limiting oxygen index (LOI). The LOI value of the coated fabric was up to 33.2 vol % and the char residue at 800 °C also increased to 57 wt %. Cone calorimetry tests revealed that, compared to the control fabric, the peak of heat release rate (PHRR) and total heat release (THR) of FR-PAN decreased by 66% and 73%, respectively. These results indicated that sol-gel combined with layer-by-layer assembly technique could impart PAN fabric with satisfactory flame-retardant properties, showing an efficient flame retardant strategy for PAN fabric.

  19. Preparation, characterization and luminescence of Sm~(3+) or Eu~(3+) doped Sr_2CeO_4 by a modified sol-gel method

    Institute of Scientific and Technical Information of China (English)

    张春祥; 史建设; 杨绪杰; 陆路德; 汪信

    2010-01-01

    Superfine Sr2CeO4:RE3+ (RE=Eu, Sm) phosphors were synthesized at relatively low temperature by a modified sol-gel method using nitrates as raw materials, ethylenediaminetetraacetic acid (EDTA) as complexing agent. Single phase phosphors could be obtained at calcination temperature above 800 °C and pH value higher than 6.4 of initial solution. The as-prepared powders consisted of uniform crotch-like grains. The preparation process was monitored by thermogravimetric and differential thermal analysis (TG-DTA) ...

  20. Nanocrystalline sol-gel TiO{sub 2}-SnO{sub 2} coatings: Preparation, characterization and photo-catalytic performance

    Energy Technology Data Exchange (ETDEWEB)

    Kaleji, Behzad Koozegar [Department of Materials Engineering, Faculty of Engineering, Tarbiat Modares University, P.O. Box 14115-143, Tehran (Iran, Islamic Republic of); Sarraf-Mamoory, Rasoul, E-mail: rsarrafm@modares.ac.ir [Department of Materials Engineering, Faculty of Engineering, Tarbiat Modares University, P.O. Box 14115-143, Tehran (Iran, Islamic Republic of)

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer SnO{sub 2} additive enhanced significantly photo-catalytic properties of TiO{sub 2} based thin film for remove of organic compounds. Black-Right-Pointing-Pointer Structural and optical properties are dependent on dopant concentration. Black-Right-Pointing-Pointer TiO{sub 2}-SnO{sub 2} nanocrystalline thin film is promising for photocatalytic properties in visible light. -- Abstract: In this study, preparation of SnO{sub 2} (0-30 mol% SnO{sub 2})-TiO{sub 2} dip-coated thin films on glazed porcelain substrates via sol-gel process has been investigated. The effects of SnO{sub 2} on the structural, optical, and photo-catalytic properties of applied thin films have been studied by X-ray diffraction, Raman spectroscopy, and scanning electron microscopy. Surface topography and surface chemical state of thin films were examined by atomic force microscopy and X-ray photoelectron spectroscopy. XRD patterns showed an increase in peak intensities of the rutile crystalline phase by increasing the SnO{sub 2} content. The prepared Sn doped TiO{sub 2} photo-catalyst films showed optical absorption in the visible light area exhibited excellent photo-catalytic ability for the degradation of methylene blue under visible light irradiation. Best photo-catalytic activity of Sn doped TiO{sub 2} thin films was measured in the TiO{sub 2}-15 mol% SnO{sub 2} sample by the Sn{sup 4+} dopants presented substitution Ti{sup 4+} into the lattice of TiO{sub 2} increasing the surface oxygen vacancies and the surface hydroxyl groups.

  1. 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.

  2. Application of response surface methodology for degradation of methyl orange with TiO{sub 2} sol-gel sulphated Ti; Aplicacion de metodologia de superficie de respuesta para la degradacion de naranja de metilo con TiO{sub 2} sol-gel sulfatado

    Energy Technology Data Exchange (ETDEWEB)

    Del Angel S, M. T.; Garcia A, R. [Instituto Tecnologico de Ciudad Madero, Av. 1o. de Mayo y Sor Juana I. de la Cruz, Col. Los Mangos, 89440 Ciudad Madero, Tamaulipas (Mexico); Garcia A, P.; Lagunes G, L. M. [Universidad Juarez Autonoma de Tabasco, Division Academica de Ciencias Agropecuarias, Av. Universidad s/n, Zona de la Cultura, Col. Magisterial, 86040 Villahermosa, Tabasco (Mexico); Cabrera C, E. G., E-mail: shish_kko@yahoo.com.mx [Instituto Tecnologico de Villahermosa, Carretera Villahermosa-Frontera Km. 3.5, Cd. Industrial, 86010 Villahermosa, Tabasco (Mexico)

    2015-06-01

    In this work we report the implementation of the response surface methodology for the optimization of photo catalytic degradation of methyl orange dye (MO) using as photo catalyst sulphated TiO{sub 2} prepared by sol-gel method. The variables studied were ph of the solution (3-11), catalyst concentration (0.1-1 g/L), and MO concentration (10-30 ppm). The effects of these parameters over the degradation of MO were evaluated according to a Box-Behnken design. The only crystal structure identified by X-ray diffraction was anatase phase. The optimum conditions for the photo catalytic degradation of MO according to the methodology applied were ph 6.0, 17.78 ppm MO concentration at each concentration level of the catalyst. (Author)

  3. Surface engineering of artificial heart valve disks using nanostructured thin films deposited by chemical vapour deposition and sol-gel methods.

    Science.gov (United States)

    Jackson, M J; Robinson, G M; Ali, N; Kousar, Y; Mei, S; Gracio, J; Taylor, H; Ahmed, W

    2006-01-01

    Pyrolytic carbon (PyC) is widely used in manufacturing commercial artificial heart valve disks (HVD). Although PyC is commonly used in HVD, it is not the best material for this application since its blood compatibility is not ideal for prolonged clinical use. As a result thrombosis often occurs and the patients are required to take anti-coagulation drugs on a regular basis in order to minimize the formation of thrombosis. However, anti-coagulation therapy gives rise to some detrimental side effects in patients. Therefore, it is extremely urgent that newer and more technically advanced materials with better surface and bulk properties are developed. In this paper, we report the mechanical properties of PyC-HVD, i.e. strength, wear resistance and coefficient of friction. The strength of the material was assessed using Brinell indentation tests. Furthermore, wear resistance and coefficient of friction values were obtained from pin-on-disk testing. The micro-structural properties of PyC were characterized using XRD, Raman spectroscopy and SEM analysis. Also in this paper we report the preparation of freestanding nanocrystalline diamond films (FSND) using the time-modulated chemical vapour deposition (TMCVD) process. Furthermore, the sol-gel technique was used to uniformly coat PyC-HVD with dense, nanocrystalline-titanium oxide (nc-TiO2) coatings. The as-grown nc-TiO2 coatings were characterized for microstructure using SEM and XRD analysis.

  4. 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…

  5. Influence of preparation methods of microwave, sol-gel, and hydrothermal on structural and optical properties of lanthania nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Goharshadi, Elaheh K.; Mahvelati, Tahereh; Yazdanbakhsh, Mohammad [Ferdowsi Univ., Mashhad (Iran, Islamic Republic of). Dept. of Chemistry

    2016-01-15

    In this work, the nearly pure hexagonal phase of lanthania nanoparticles (NPs) was successfully synthesized using three methods: microwave, sol-gel, and hydrothermal. The samples were characterized using nine techniques including powder X-ray powder diffraction, thermogravimetry, transmission electron microscopy, scanning electron microscopy, field emission microscopy, energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, far infrared spectroscopy, and ultraviolet-visible absorption spectroscopy. This study showed that the method of synthesizing lanthania NPs can affect the size, which in turn has impact on structural, morphological, and optical properties.

  6. Up-conversion luminescence application in Er3+: TiO2 thin film prepared by dip coating sol-gel route

    International Nuclear Information System (INIS)

    Badr, Y.; Battisha, I.K.; Salah, A.; Salem, M.A.

    2008-01-01

    Sol-gel derived nano-crystalline titanium dioxide films doped with 1 up to 5% Er 3+ ions were prepared by dip coating sol-gel method. The coating sol was obtained by hydrolysis of Ti(OC 4 H 9 ) 4 in ethanol/HCI solution. The FT-Raman and the X-ray diffraction (XRD) were carried out to determine the crystal structure of the prepared samples. The morphology SEM and the cross-sectional of the film were used to characterize the microstructure and the thickness of the prepared film. It is shown that relative homogeneous, crack-free and transparent film was achieved via dipping process at 500 deg C. After the excitation with laser diode at wavelength 808 nm, visible (Vis) and infrared (IR) up-conversion emissions were evidenced in the thin film samples under investigation. The up-conversion was found to depend strongly on the Er 3+ ion concentrations. The visible emission was found to be at 540, 560, 590 and 640 nm for thin film. They are attributed to intra-4f transition of Er 3+ ions and assigned to the ( 2 H 11/2 + 4 S 3/2 ) and 4 F 9/2 , which are populated through excited state absorption (ESA) for 808 nm excitation. (author)

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

    Science.gov (United States)

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

    2017-05-01

    A new approach for removal of indigo carmine blue (IC) dye which is extensively used in jeans manufacture was successfully performed on novel mesoporous [LDH] nanoparticles prepared by sol-gel route using CTAB as shape and pore directing agent. The physicochemical features were monitored by X-ray diffraction (XRD), Fourier transformer infra-red (FTIR), N 2 adsorption-desorption isotherm, Field emission electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). The influence of reaction parameters affecting dye adsorption including contact time, initial dye concentration, pH and temperature were investigated. Textural analysis and HRTEM images indicate the existence of mesoporous spherical nanoparticles of size = 26 nm connected to each other's and embedded large numbers of mesopores of average pore radius = 43.5 Å. A successful adsorption of IC on LDH nanoparticles of surface area = 85.6 m 2 /g at various pH with maximum adsorption capacity = 62.8 mg/g at pH = 9.5. Langmuir model is more favorable to describe the adsorption of IC rather than Freundlich model which reflecting the preferential formation of monolayer on the surface of LDH. Both film diffusion and the intraparticle diffusion affect the dye adsorption. The values of enthalpy change (ΔH) for and (ΔS) are + 28.18 and + 0.118 kJ/mol, respectively indicating that the removal process is endothermic. The results indicated that LDH nanoparticles conserved a good activity even after five consecutive cycles of reuse. Our results suggest that mesoporous LDH nanoparticles are considered a potential novel adsorbent for remediation of wastewater containing IC. Copyright © 2017 Elsevier Ltd. All rights reserved.

  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. Gelatin/nano-hydroxyapatite hydrogel scaffold prepared by sol-gel technology as filler to repair bone defects.

    Science.gov (United States)

    Raucci, Maria Grazia; Demitri, Christian; Soriente, Alessandra; Fasolino, Ines; Sannino, Alessandro; Ambrosio, Luigi

    2018-07-01

    This study reports on the development of a scaffold with a gradient of bioactive solid signal embedded in the biodegradable polymer matrix by combining a sol-gel approach and freeze-drying technology. The chemical approach based on the sol-gel transition of calcium phosphates ensures the particles dispersion into the gelatin matrix and a direct control of interaction among COOH gelatin /Ca 2+ ions. Morphological analysis demonstrated that on the basis of the amount of inorganic component and by using specific process conditions, it is possible to control the spatial distribution of nanoparticles around the gelatin helix. In fact, methodology and formulations were able to discriminate between the different hydroxyapatite concentrations and their respective morphology. The good biological response represented by good cell attachment, proliferation and increased levels of alkaline phosphatase as an indicator of osteoblastic differentiation of human mesenchymal stem cells toward the osteogenic lineage, demonstrating the effect of bioactive solid signals on cellular behavior. Furthermore, the inhibition of reactive oxygen species production by composite materials predicted potential anti-inflammatory properties of scaffolds thus confirming their biocompatibility. Indeed, these interesting biological results suggest good potential application of this scaffold as filler to repair bone defects. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 106A: 2007-2019, 2018. © 2018 Wiley Periodicals, Inc.

  10. Characterization of the calcium-fluoroaluminosilicate glass prepared by a non-hydrolytic sol-gel route for future dental application as glass ionomer cement

    Directory of Open Access Journals (Sweden)

    Alexandre Cestari

    2009-06-01

    Full Text Available Glass ionomer cements are widely employed in dentistry due to their physical, biological and mainly anti-caries properties. Glass ionomers consist of an aluminosilicate glass matrix modified with other elements, and they contain large quantities of fluorine. In this study, we report on the preparation of calcium-fluoroaluminosilicate glasses by a nonhydrolytic sol-gel route as an alternative approach to obtaining alumina-silica matrices. The glass powders were prepared via the non-hydrolytic sol-gel method, by mixing AlCl3, SiCl4, CaF2, AlF3, NaF, and AlPO4. The powders were studied by thermal analysis (TG/DTA/DSC, photoluminescence (PL, nuclear magnetic resonance (NMR27Al-29Si, and X ray diffraction (XRD. TG/DTA/DSC analyses revealed a constant mass loss due to structural changes during the heating process, which was confirmed by NMR and PL. A stable aluminosilicate matrix with potential future application as a glass ionomer base was obtained.

  11. Preparation of the polyelectrolyte complex hydrogel of biopolymers via a semi-dissolution acidification sol-gel transition method and its application in solid-state supercapacitors

    Science.gov (United States)

    Zhao, Jian; Chen, Yu; Yao, Ying; Tong, Zong-Rui; Li, Pu-Wang; Yang, Zi-Ming; Jin, Shao-Hua

    2018-02-01

    Hydrogels have drawn many attentions as the solid-state electrolytes in flexible solid-state supercapacitors (SCs) recently. Among them, the polyelectrolyte complex hydrogel (PECH) electrolytes of natural polymers are more competitive because of their environmentally friendly property and low cost. However, while mixing two biopolymer solutions with opposite charges, the strong electrostatic interactions between the cationic and anionic biopolymers may result in precipitates instead of hydrogels. Here we report a novel method, semi-dissolution acidification sol-gel transition (SD-A-SGT), for the preparation of the PECH of chitosan (CTS) and sodium alginate (SA), with the controllable sol-gel transition and uniform composition and successfully apply it as the hydrogel electrolyte of solid-state supercapacitors (SCs). The CTS-SA PECH exhibits an extremely high ionic conductivity of 0.051 S·cm-1 and reasonable mechanical properties with a tensile strength of 0.29 MPa and elongation at break of 109.5%. The solid-state SC fabricated with the CTS-SA PECH and conventional polyaniline (PANI) nanowire electrodes provided a high specific capacitance of 234.6 F·g-1 at 5 mV·s-1 and exhibited excellent cycling stability with 95.3% capacitance retention after 1000 cycles. Our work may pave a novel avenue to the preparation of biodegradable PECHs of full natural polymers, and promote the development of environmentally friendly electronic devices.

  12. Microstructural changes in NiFe{sub 2}O{sub 4} ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

    Energy Technology Data Exchange (ETDEWEB)

    Chauhan, Lalita, E-mail: chauhan.lalita5@gmail.com; Sreenivas, K. [Department of Physics & Astrophysics, University of Delhi, Delhi-110007 (India); Bokolia, Renuka

    2016-05-23

    Structural properties of Nickel ferrite (NiFe{sub 2}O{sub 4}) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe{sub 2}O{sub 4} powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe{sub 2}O{sub 4} ceramics with a uniform microstructure and a large grain size.

  13. Microstructural changes in NiFe_2O_4 ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

    International Nuclear Information System (INIS)

    Chauhan, Lalita; Sreenivas, K.; Bokolia, Renuka

    2016-01-01

    Structural properties of Nickel ferrite (NiFe_2O_4) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe_2O_4 powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe_2O_4 ceramics with a uniform microstructure and a large grain size.

  14. Microstructural changes in NiFe2O4 ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

    Science.gov (United States)

    Chauhan, Lalita; Bokolia, Renuka; Sreenivas, K.

    2016-05-01

    Structural properties of Nickel ferrite (NiFe2O4) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe2O4 powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe2O4 ceramics with a uniform microstructure and a large grain size.

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. Double-Layer Surface Modification of Polyamide Denture Base Material by Functionalized Sol-Gel Based Silica for Adhesion Improvement.

    Science.gov (United States)

    Hafezeqoran, Ali; Koodaryan, Roodabeh

    2017-09-21

    Limited surface treatments have been proposed to improve the bond strength between autopolymerizing resin and polyamide denture base materials. Still, the bond strength of autopolymerizing resins to nylon polymer is not strong enough to repair the fractured denture effectively. This study aimed to introduce a novel method to improve the adhesion of autopolymerizing resin to polyamide polymer by a double layer deposition of sol-gel silica and N-2-(aminoethyl)-3-aminopropyltrimethoxysilane (AE-APTMS). The silica sol was synthesized by acid-catalyzed hydrolysis of tetraethylorthosilicate (TEOS) as silica precursors. Polyamide specimens were dipped in TEOS-derived sol (TS group, n = 28), and exposed to ultraviolet (UV) light under O 2 flow for 30 minutes. UV-treated specimens were immersed in AE-APTMS solution and left for 24 hours at room temperature. The other specimens were either immersed in AE-APTMS solution (AP group, n = 28) or left untreated (NT group, n = 28). Surface characterization was investigated by fourier transform infrared spectroscopy (FTIR) and atomic force microscopy (AFM). Two autopolymerizing resins (subgroups G and T, n = 14) were bonded to the specimens, thermocycled, and then tested for shear bond strength with a universal testing machine. Data were analyzed with one-way ANOVA followed by Tukey's HSD (α = 0.05). FTIR spectra of treated surfaces confirmed the chemical modification and appearance of functional groups on the polymer. One-way ANOVA revealed significant differences in shear bond strength among the study groups. Tukey's HSD showed that TS T and TS G groups had significantly higher shear bond strength than control groups (p = 0.001 and p < 0.001, respectively). Moreover, bond strength values of AP T were statistically significant compared to controls (p = 0.017). Amino functionalized TEOS-derived silica coating is a simple and cost-effective method for improving the bond strength between the autopolymerizing resin and polyamide

  20. Preparation of transparent sol-gel films containing europium, terbium, and ytterbium cations from 4-(3'-triethoxysilylpropylimino)pent-2-en-2-ol

    International Nuclear Information System (INIS)

    Semenov, V.V.; Cherepennikova, N.F.; Kuznetsova, O.V.; Melenskova, N.V.; Bushuk, B.A.; Bushuk, S.B.; Kal'vinkovskaya, Yu.A.; Duglas, V.E.

    2007-01-01

    A reaction of 3-aminopropyl(triethoxy)silane with acetylacetone gave a mixture of two isomeric carbon-functionalized organosilicon compounds capable of complexation and sol-gel polymerization. These were 4-(3'-triethoxysilylpropylimino)pent-2-en-2-ol (EtO) 3 Si-CH 2 CH 2 CH 2 -N=C(Me)CH=C(Me)OH (Ia, 83%) and 4-(3'-triethoxysilylpropylamino)pent-3-en-2-one (EtO) 3 Si-CH 2 CH 2 CH 2 -NH-C(Me)=CH-C(O)Me (Ib, 17%). With acetylacetone trimethylsilyl ether instead of acetylacetone itself, compound Ia and silylated derivatives (Me 3 SiO) n (EtO) 3-n Si-CH 2 CH 2 CH 2 -N=C(Me)CH=C(Me)OH were obtained as admixture in 84 and 16% yields, respectively. Reactions of ligands Ia and Ib with europium and terbium propan-2-olates afforded the corresponding complexes. Formulations of lanthanide complexes, oligodimethylsiloxanediols, and 3-aminopropyl(triethoxy)silane were used to prepare transparent sol-gel films. The photoluminescence spectra of the films show narrow bands due to Eu 3+ or Tb 3+ emission. Emission from the organosilicon matrix appears as a broad band at 430 to 435 nm [ru

  1. Structural and magnetic properties of Mg-Zn ferrites (Mg1−xZnxFe2O4) prepared by sol-gel method

    International Nuclear Information System (INIS)

    Reyes-Rodríguez, Pamela Yajaira; Cortés-Hernández, Dora Alicia; Escobedo-Bocardo, José Concepción; Almanza-Robles, José Manuel; Sánchez-Fuentes, Héctor Javier; Jasso-Terán, Argentina; De León-Prado, Laura Elena; Méndez-Nonell, Juan; Hurtado-López, Gilberto Francisco

    2017-01-01

    In this study, the Mg 1−x Zn x Fe 2 O 4 nanoparticles (x=0–0.9) were prepared by sol-gel method. These ferrites exhibit an inverse spinel structure and the lattice parameter increases as the substitution of Zn 2+ ions is increased. At lower Zn content (0.1≤x≤0.5), saturation magnetization (Ms) increases, while it decreases at higher Zn content (x≥6). The remnant magnetization (0.17–2.0 emu/g) and coercive field (6.0–60 Oe) indicate a ferrimagnetic behavior. The average core diameter of selected ferrites is around 15 nm and the nanoparticles morphology is quasi spherical. The heating ability of some Mg 0.9 Zn 0.1 Fe 2 O 4 and Mg 0.7 Zn 0.3 Fe 2 O 4 aqueous suspensions indicates that the magnetic nanoparticles can increase the medium temperature up to 42 °C in a time less than 10 min - Highlights: • Magnetic nanoparticles of Mg 1−x Zn x Fe 2 O 4 were synthesized by sol-gel method. • Nanoparticles showing a single spinel crystalline structure were obtained. • Aqueous suspensions of Mg 0.7 Zn 0.3 Fe 2 O 4 and Mg 0.9 Zn 0.1 Fe 2 O 4 show heating ability.

  2. 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.

  3. 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

  4. 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.

  5. 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.

  6. Effect of La and W dopants on dielectric and ferroelectric properties of PZT thin films prepared by sol-gel process

    International Nuclear Information System (INIS)

    Xiao, Mi; Zhang, Zebin; Zhang, Weikang; Zhang, Ping

    2018-01-01

    La or W-doped lead zirconate titanate thin films (PLZT or PZTW) were prepared on platinized silicon substrates by sol-gel process. The effects of La or W dopant on the phase development, microstructure, dielectric and ferroelectric characteristics of films were studied. For PLZT films, the optimum doping concentration was found to be 2 mol%. While for PZTW films, the dielectric and ferroelectric properties were found to be improved as the doping concentration increased. The fatigue properties of PLZT and PZTW thin films were also investigated, the results showed that A- or B-site donor doping could improve the fatigue properties of PZT thin films. The theory of oxygen vacancy was used to explain the performance improvement caused by donor doping. (orig.)

  7. Effect of La and W dopants on dielectric and ferroelectric properties of PZT thin films prepared by sol-gel process

    Science.gov (United States)

    Xiao, Mi; Zhang, Zebin; Zhang, Weikang; Zhang, Ping

    2018-01-01

    La or W-doped lead zirconate titanate thin films (PLZT or PZTW) were prepared on platinized silicon substrates by sol-gel process. The effects of La or W dopant on the phase development, microstructure, dielectric and ferroelectric characteristics of films were studied. For PLZT films, the optimum doping concentration was found to be 2 mol%. While for PZTW films, the dielectric and ferroelectric properties were found to be improved as the doping concentration increased. The fatigue properties of PLZT and PZTW thin films were also investigated, the results showed that A- or B-site donor doping could improve the fatigue properties of PZT thin films. The theory of oxygen vacancy was used to explain the performance improvement caused by donor doping.

  8. Synthesis and characterization of hollow {alpha}-Fe{sub 2}O{sub 3} sub-micron spheres prepared by sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Leon, Lizbet, E-mail: lizbetlf@gmail.com; Bustamante, Angel; Osorio, Ana; Olarte, G. S. [Universidad Nacional Mayor de San Marcos (Peru); Santos Valladares, Luis De Los, E-mail: ld301@cam.ac.uk; Barnes, Crispin H. W. [University of Cambridge, Cavendish Laboratory (United Kingdom); Majima, Yutaka [Tokyo Institute of Technology, Materials and Structures Laboratory (Japan)

    2011-11-15

    In this work we report the preparation of magnetic hematite hollow sub-micron spheres ({alpha}-Fe{sub 2}O{sub 3}) by colloidal suspensions of ferric nitrate nine-hydrate (Fe(NO{sub 3}){sub 3}{center_dot}9H{sub 2}O) particles in citric acid solution by following the sol-gel method. After the gel formation, the samples were annealed at different temperatures in an oxidizing atmosphere. Annealing at 180 Degree-Sign C resulted in an amorphous phase, without iron oxide formation. Annealing at 250 Degree-Sign C resulted in coexisting phases of hematite, maghemite and magnetite, whereas at 400 Degree-Sign C, only hematite and maghemite were found. Pure hematite hollow sub-micron spheres with porous shells were formed after annealing at 600 Degree-Sign C. The characterization was performed by X-ray diffraction (XRD), Moessbauer spectroscopy (MS) and scanning electron microscopy (SEM).

  9. 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.))

  10. Preparation of poly (2-hydroxyethyl methacrylate -co-acrylamide) hydrogels by gamma radiation: sol-gel analysis, swelling kinetic and mechanical behaviour

    International Nuclear Information System (INIS)

    Rapado Paneque, Manuel; Concepcion Villanueva, Daniel; Peniche, Carlos; Rosiak, Janusz M.

    2006-01-01

    2 hydroxyethyl methacrylate (HEMA) / acrylamide (Am) hydrogels were prepared by simultaneous radiation induced cross linking copolymerization. The G values of cross linking and degradation, gelation dose and further radiation parameters were estimated by sol/gel analysis. The dynamic swelling behaviour at 37 grade centigrade of these kind of materials was studied. The influence of the absorbed dose on the swelling degree at different pH was studied. It was observed that the kinetics is in good agreement with the second order diffusion kinetics proposed by Schott. The degree of cross linking was found to increase with the adsorbed dose and influence the mechanical properties to some extend. The molar mass of chain between the network cross links was estimated

  11. Preparation and studies of Eu3+ and Tb3+ co-doped Gd2O3 and Y2O3 sol-gel scintillating films

    International Nuclear Information System (INIS)

    Morales Ramirez, A. de J; Garcia Murillo, A.; Carrillo Romo, F. de J; Ramirez Salgado, J.; Le Luyer, C.; Chadeyron, G.; Boyer, D.; Moreno Palmerin, J.

    2009-01-01

    Eu 3+ (2.5 at.%) and Tb 3+ (0.005-0.01 at.%) co-doped gadolinium and yttrium oxide (Gd 2 O 3 and Y 2 O 3 ) powders and films have been prepared using the sol-gel process. High density and optical quality thin films were prepared with the dip-coating technique. Gadolinium (III) 2,4-pentadionate and yttrium (III) 2,4-pentadionate were used as precursors, and europium and terbium in their nitrate forms were used as doping agents. Chemical and structural analyses (infrared spectroscopy, X-ray diffraction and high-resolution transmission electron microscopy) were conducted on both sol-gel precursor powders and dip-coated films. The morphology of thin films heat-treated at 700 o C was studied by means of atomic force microscopy. It was shown that the highly dense and very smooth films had a root mean roughness (RMS) of 2 nm ± 0.2 (A = 0.0075 Tb 3+ ) and 24 nm ± 3.0 (B = 0.01 Tb 3+ ). After treatment at 700 o C, the crystallized films were in the cubic phase and presented a polycrystalline structure made up of randomly oriented crystallites with grain sizes varying from 20 to 60 nm. The X-ray induced emission spectra of Eu 3+ - and Tb 3+ -doped Gd 2 O 3 and Y 2 O 3 powders showed that Tb 3+ contents of 0.005, 0.0075 and 0.01 at.% affected their optical properties. Lower Tb 3+ concentrations (down to 0.005 at.%) in both systems enhanced the light yield.

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

    Science.gov (United States)

    Liu, Dean-Mo; Chen, I-Wei

    2001-01-01

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

  13. Preparation and optical properties of ZnGa{sub 2}O{sub 4}:Cr{sup 3+} thin films derived by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Weiwei [School of Physics and Nuclear Energy Engineering, Beihang University, No. 37 XueYuan Road, HaiDian District, Beijing 100191 (China); Zhang Junying, E-mail: zjy@buaa.edu.cn [School of Physics and Nuclear Energy Engineering, Beihang University, No. 37 XueYuan Road, HaiDian District, Beijing 100191 (China); Li Yuan; Chen Ziyu; Wang Tianmin [School of Physics and Nuclear Energy Engineering, Beihang University, No. 37 XueYuan Road, HaiDian District, Beijing 100191 (China)

    2010-05-01

    ZnGa{sub 2}O{sub 4}:Cr{sup 3+} thin films with bright red emission were synthesized using a sol-gel process, characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Auger electron spectroscopy (AES) and UV-vis and fluorescence spectrophotometry measurements. Effects of calcining temperature, film thickness, calcining duration and substrates on the crystal structure and photoluminescent property have been investigated. It is found that the crystallinity, Ga/Zn ratio and band gap energy (E{sub g}) are significant factors influencing optical characteristics, while the nature of substrates affect the surface morphologies of ZnGa{sub 2}O{sub 4}:Cr{sup 3+} thin films.

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

    Directory of Open Access Journals (Sweden)

    R. Ajay Kumar

    2017-04-01

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

  15. Optimization of Catalytic Ozonation Process for Formaldehyde Mineralization from Synthetic Wastewater by Fe/MgO Nanoparticles Synthesis by Sol-Gel Method by Response Surface Model

    Directory of Open Access Journals (Sweden)

    Ghorban Asgari

    2014-09-01

    Full Text Available Background: Design experiment stages of formalin mineralization process by center composition design (CCD cause ease of work, reducing the number of samples, increasing the accuracy of optimized conditions and the interaction parameters determined during the process. The aim of this study was optimization of catalytic ozonation process for formaldehyde mineralization from synthetic wastewater by Fe/MgO nanoparticles synthesis by sol-gel method by response surface model. Methods: This experimental study was conducted in a semi-batch reactor, using a RSM by taking 3 factors in the final stage of pH (7-9, reaction time (10-20 min and catalyst dose (1.1-1.3 g/L was investigated. Synthesis of nanoparticles was done by sol-gel method. The results were analyzed by Design Expert 7.0.1 software. Results: The results showed that the process was dependent on the parameters studied and changing each parameter, affected the process efficiency and other parameters. The optimum conditions predicted for the process was 86.51% of mineralization efficiency. Optimum condition included pH=8.82, reaction time of 20 minute and catalyst dose of 1.3 g/L. The correlation coefficient for the process was determined 0.91. Conclusion: Using a statistical model could reduce the number of experiments, the accuracy and the prediction process. The catalytic ozonation process has the ability to remove formaldehyde with high efficiency and the process was environmental friendly.

  16. Short communication: Evaluation of a sol-gel-based stainless steel surface modification to reduce fouling and biofilm formation during pasteurization of milk.

    Science.gov (United States)

    Liu, Dylan Zhe; Jindal, Shivali; Amamcharla, Jayendra; Anand, Sanjeev; Metzger, Lloyd

    2017-04-01

    Milk fouling and biofilms are common problems in the dairy industry across many types of processing equipment. One way to reduce milk fouling and biofilms is to modify the characteristics of milk contact surfaces. This study examines the viability of using Thermolon (Porcelain Industries Inc., Dickson, TN), a sol-gel-based surface modification of stainless steel, during thermal processing of milk. We used stainless steel 316L (control) and sol-gel-modified coupons in this study to evaluate fouling behavior and bacterial adhesion. The surface roughness as measured by an optical profiler indicated that the control coupons had a slightly smoother finish. Contact angle measurements showed that the modified surface led to a higher water contact angle, suggesting a more hydrophobic surface. The modified surface also had a lower surface energy (32.4 ± 1.4 mN/m) than the control surface (41.36 ± 2.7 mN/m). We evaluated the susceptibility of control and modified stainless steel coupons to fouling in a benchtop plate heat exchanger. We observed a significant reduction in the amount of fouled layer on modified surfaces. We found an average fouling weight of 19.21 mg/cm 2 and 0.37 mg/cm 2 on the control and modified stainless steel coupons, respectively. We also examined the adhesion of Bacillus and biofilm formation, and observed that the modified stainless steel surface offered greater resistance to biofilm formation. Overall, the Thermolon-modified surface showed potential in the thermal processing of milk, offering significantly lower fouling and bacterial attachment than the control surface. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  17. 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.

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

    Directory of Open Access Journals (Sweden)

    Garcia-Gonzalez, L.

    2011-02-01

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

  19. Corrosion behavior of TiO{sub 2}-NiO nanocomposite thin films on AISI 316L stainless steel prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Cheraghi, H., E-mail: hoch2020@yahoo.com [Materials Science and Engineering Department, Iran University of Science and Technology (IUST), P.O. Box: 16765163, Narrmak Street, Tehran (Iran, Islamic Republic of); Shahmiri, M., E-mail: mshahmiri@iust.ac.ir [Materials Science and Engineering Department, Iran University of Science and Technology (IUST), P.O. Box: 16765163, Narrmak Street, Tehran (Iran, Islamic Republic of); Sadeghian, Z. [Research Institute of Petroleum Industry (RIPI), P.O. Box: 14857-3311, West Blvd. Azadi Sport Complex, Tehran (Iran, Islamic Republic of)

    2012-11-01

    TiO{sub 2}-NiO nanocomposite thin films were deposited on the 316L stainless steel using sol-gel method by a dip coating technique. Different techniques such as differential thermal analysis, thermogravimetric analysis, X-ray diffraction, Fourier transform infrared spectrometry, scanning electron microscopy and scanning probe microscopy were carried out in order to characterize the structure of the coatings. The corrosion resistance of the coatings was evaluated by using Tafel polarization and electrochemical impedance spectroscopy tests of uncoated and coated specimens in a 3.5% NaCl solution at room temperature. It was found that to obtain desirable structure in coatings, the coatings should be calcined at 600 Degree-Sign C for one and half hour. NiTiO{sub 3}, anatase and rutile were the phases obtained in different calcination conditions in air atmosphere. The results of corrosion tests indicated that with increasing the dipping times from 2 to 4, the corrosion current density first decreases but when increasing the dipping times to 6, it increases. Also the corrosion current density decreased from 186.7 nA.cm{sup -2} (uncoated steel) to 34.21 nA.cm{sup -2} (80%TiO{sub 2}-20%NiO) and corrosion potential increased from - 150.2 mV (uncoated steel) to - 107.3 mV (67%TiO{sub 2}-33%NiO). - Highlights: Black-Right-Pointing-Pointer TiO{sub 2}-NiO thin films were deposited on the 316L stainless steel using sol-gel method. Black-Right-Pointing-Pointer Different compositions, annealing times and temperatures resulted in various phases. Black-Right-Pointing-Pointer Films having different compositions showed various surface morphologies. Black-Right-Pointing-Pointer Films having a composition of 80%TiO{sub 2}-20%NiO showed a good corrosion protection.

  20. 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.

  1. 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.

  2. 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

  3. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-29

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  6. 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

  7. 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

  8. Physical properties of N{sub x}TiO{sub 2} prepared by sol-gel route

    Energy Technology Data Exchange (ETDEWEB)

    Brahimi, Razika [Laboratory of Storage and Valorization of Renewable Energies, Faculty of Chemistry, U.S.T.H.B., BP 32, 16111, El-Alia, Algiers (Algeria); Centre of Research in Physical and Chemical Analysis (CRAPC) BP 248, RP 16004, Algiers (Algeria); Bessekhouad, Yassine, E-mail: ybessekhouad@yahoo.fr [Laboratory of Storage and Valorization of Renewable Energies, Faculty of Chemistry, U.S.T.H.B., BP 32, 16111, El-Alia, Algiers (Algeria); National Veterinary High School, BP 161-El Harrach, Algiers (Algeria); Trari, Mohamed [Laboratory of Storage and Valorization of Renewable Energies, Faculty of Chemistry, U.S.T.H.B., BP 32, 16111, El-Alia, Algiers (Algeria)

    2012-09-15

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

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

    Directory of Open Access Journals (Sweden)

    Xu Gui-Long

    2011-12-01

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

  10. Microleakage and antibacterial properties of ZnO and ZnO:Ag nanopowders prepared via a sol-gel method for endodontic sealer application

    Energy Technology Data Exchange (ETDEWEB)

    Shayani Rad, M.; Kompany, A. [Ferdowsi University of Mashhad, Materials and Electroceramics Laboratory, Department of Physics, Faculty of Sciences (Iran, Islamic Republic of); Khorsand Zak, A., E-mail: alikhorsandzak@gmail.com [Esfarayen University, Nanotechnology Laboratory (Iran, Islamic Republic of); Javidi, M.; Mortazavi, S. M. [Mashhad University of Medical Sciences, Dental Material Research Centre, Department of Endodontics, Faculty of Dentistry (Iran, Islamic Republic of)

    2013-09-15

    One of the most important problems in dentistry is the microleakage, whether apical or coronal, which may cause failure of root canal therapy. The aim of this study is to prepare suitable sealer to decrease the microleakage of the root canals as well as having good antibacterial property. Pure ZnO and ZnO:Ag nanopowders were synthesized via sol gel method using gelatin as polymerization agent calcined at different temperatures of 500, 600, and 700 Degree-Sign C for 8 h. The prepared samples were characterized using X-ray diffraction and transition electron microscopy. The microleakage and antibacterial properties of the prepared samples were investigated and compared with zinc oxide eugenol (ZOE) and epoxy resin sealer (AH26), which are commonly used in dentistry as sealers. The results showed that the synthesized pure ZnO and ZnO:Ag nanopowders exhibit better microleakage and antibacterial properties in comparison with ZOE and AH26 sealers, and therefore are more suitable filling materials to be used as sealer in root canal treatment.

  11. Antimony (V) oxide adsorbed on a silica-zirconia mixed oxide obtained by the sol-gel processing method: preparation and acid properties

    International Nuclear Information System (INIS)

    Zaitseva, Galina; Gushikem, Yoshitaka

    2002-01-01

    The preparation, degree of dispersion, thermal stability and Lewis and Broensted acidity of antimony (V) oxide adsorbed on Si O 2 /Zr O 2 mixed oxide, previously prepared by the sol-gel processing method, are described herein. The samples Si O 2 /Zr O 2 /Sb 2 O 5 , with compositions (in wt %): (a) Zr= 8.1 and Sb= 6.3; (b) Zr= 14.9 and Sb= 11.4, were prepared. Scanning electron microscopy images connected to a X-ray energy dispersive spectrometer showed that both metals, Zr and Sb, were highly dispersed in the matrices. The X-ray diffraction patterns of Si O 2 /Zr O 2 /Sb 2 O 5 heated at different temperatures showed that, up to 1023 K, the matrix was amorphous. At 1273 K a crystalline phase of Zr O 2 (baddeleyite) was observed and raising the temperature to 1573 K, crystalline phases of Si O 2 (cristobalite) and presumably of Zr O 2 /Sb 2 O 5 were observed. Using pyridine as a molecular probe, Broensted acid sites on the Si O 2 /Zr O 2 /Sb 2 O 5 matrix, heat treated up to 523 K, were shown to be very stable. (author)

  12. Structural and optical properties of Tb and Na-Tb co-doped Ca3V2O8 phosphors prepared by sol-gel process

    Science.gov (United States)

    Parab, Shambhu S.; Salker, A. V.

    2018-01-01

    A malic acid assisted sol-gel route was successfully employed to prepare two distinct series of green emitting Ca3V2O8 phosphors. In the first series, Tb was solely doped whereas in the second series Na and Tb were doped simultaneously in the Ca3V2O8 crystal lattice. X-ray diffraction studies proved the utility of adopted preparative method by confirming the monophasic formation of all compounds from both the series. Spectral analysis like Raman spectroscopy, UV-DRS were undertaken to analyse the local structure, crystallinity and absorptive characteristics. XPS validated the presence of desired oxidation states of all the elements present. Finally, photoluminescence studies were done to elucidate the scope of prepared compounds as green emitting phosphors and also to understand the effect of both doping schemes on the luminescence. Intense green emission was observed in both the cases. Tb concentration of 0.08 was found to be optimum in case of Tb singly doped compounds whereas Tb = 0.12 showed highest intensity among the Na-Tb co-doped samples. Moreover, a red shift in the excitation wavelength was observed after Na doping signifying a change in the local electronic environment which in turn has affected the luminescence pattern. Local crystallinity and vacancy concentrations were found to have a major say on the emission intensities.

  13. Antimony (V Oxide Adsorbed on a Silica-Zirconia Mixed Oxide Obtained by the Sol-Gel Processing Method: Preparation and Acid Properties

    Directory of Open Access Journals (Sweden)

    Zaitseva Galina

    2002-01-01

    Full Text Available The preparation, degree of dispersion, thermal stability and Lewis and Brphinsted acidity of antimony (V oxide adsorbed on SiO2/ZrO2 mixed oxide, previously prepared by the sol-gel processing method, are described herein. The samples SiO2/ZrO2/Sb2O5, with compositions (in wt %: (a Zr= 8.1 and Sb= 6.3; (b Zr= 14.9 and Sb= 11.4, were prepared. Scanning electron microscopy images connected to a X-ray energy dispersive spectrometer showed that both metals, Zr and Sb, were highly dispersed in the matrices. The X-ray diffraction patterns of SiO2/ZrO2/Sb2O5 heated at different temperatures showed that, up to 1023 K, the matrix was amorphous. At 1273 K a crystalline phase of ZrO2 (baddeleyite was observed and raising the temperature to 1573 K, crystalline phases of SiO2 (cristobalite and presumably of ZrO2/Sb2O5 were observed. Using pyridine as a molecular probe, Brphinsted acid sites on the SiO2/ZrO2/Sb2O5 matrix, heat treated up to 523 K, were shown to be very stable.

  14. 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

    application, and the waterborne nature of sol-gel coatings all support the diffusion of these paints to efficiently reduce the accumulation of fouling layers on valued surfaces immersed in marine or fluvial waters. Furthermore, sol-gel glassy coatings are transparent and can be effectively applied to optical devices, windows, and solar panels used in lake, fluvial, or marine environments. Sol-gel technology is eminently versatile, and the first generation sol-gel paints have already shown good performance. Even so, vast opportunities still exist for chemists to develop novel sol-gel derived coatings to both prevent biofouling and enhance the hydrodynamic properties of boat and ship hulls. Moreover, researchers have prepared and applied multifunctional sol-gel coatings providing protection against both biofouling and corrosion. They have tested these in the marine environment with good preliminary results. In this Account, we discuss some of our new strategies for the controlled functionalization of surfaces for the development of efficient antifouling and foul-releasing systems and summarize the main achievements with biocidal and nonbiocidal sol-gel coatings. We conclude by giving insight into the marine coatings and sol-gel products markets, providing arguments to justify our conclusion that the sol-gel coatings technology is now a mature platform for the development of economically viable and environmentally friendly antifouling and foul-release formulations of enhanced performance.

  15. 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.)

  16. Impact of Overlapping Fe/TiO2 Prepared by Sol-Gel and Dip-Coating Process on CO2 Reduction

    Directory of Open Access Journals (Sweden)

    Akira Nishimura

    2016-01-01

    Full Text Available Fe-doped TiO2 (Fe/TiO2 film photocatalyst was prepared by sol-gel and dip-coating process to extend its photoresponsivity to the visible spectrum. To promote the CO2 reduction performance with the photocatalyst, some types of base materials used for coating Fe/TiO2, which were netlike glass fiber and Cu disc, were investigated. The characterization of prepared Fe/TiO2 film coated on netlike glass fiber and Cu disc was analyzed by SEM and EPMA. In addition, the CO2 reduction performance of Fe/TiO2 film coated on netlike glass disc, Cu disc, and their overlap was tested under a Xe lamp with or without ultraviolet (UV light, respectively. The results show that the concentration of produced CO increases by Fe doping irrespective of base material used under the illumination condition with UV light as well as that without UV light. Since the electron transfer between two overlapped photocatalysts is promoted, the peak concentration of CO for the Fe/TiO2 double overlapping is approximately 1.5 times as large as the Fe/TiO2 single overlapping under the illumination condition with UV light, while the promotion ratio is approximately 1.1 times under that without UV light.

  17. Pt/Pb(Zr, Ti)O3/Pt capacitor with excellent fatigue properties prepared by sol-gel process applied to FeRAM

    International Nuclear Information System (INIS)

    Jia Ze; Ren Tianling; Zhang Zhigang; Liu Tianzhi; Wen Xinyi; Hu Hong; Shao Tianqi; Xie Dan; Liu Litian

    2006-01-01

    Lead zirconate titanate (PZT) film is prepared on Pt/Ti/SiO 2 /Si substrate by proposed processes based on the sol-gel method and rapid thermal anneal (RTA). The ratio of Zr/Ti in the PZT film is 40/60. The PZT film has a mixture of perovskite orientations in which the (110) orientation is dominant. The Pt/PZT/Pt capacitor has remanent polarization of approximately 28.8 μC cm -2 and coercive voltage of approximately 0.76 V at 3 V voltage amplitude. The Pt/PZT/Pt capacitor has excellent fatigue properties. Switch polarizations decrease to 93.1% after 6 x 10 12 switch cycles. The excellent fatigue properties result from the ameliorations of PZT/Pt interface conditions, restraining Pb volatilization and the directions of crystal domains in the RTA process. Some electric properties of the PZT capacitor proposed are contrasted with those of PZT capacitors with a different anneal process in the preparation

  18. Preparation of ErMnO3 by Sol-gel Method and its Photocatalytic Activity for Removal of Methyl Orange from Water

    Science.gov (United States)

    Xie, X. Y.; Yang, J. N.; Yu, L. L.; Min, J. Y.; Sun, D. D.; Tang, P. S.; Chen, H. F.

    2018-05-01

    The single phase perovskite ErMnO3 was synthesized using Er(NO3)3, manganese acetate, citric acid and urea by a facile sol-gel method. The gel of ErMnO3 precursor was kept for 36 hours in 100 °C oven to get the xerogel. Then, the xerogel was calcined at 800 °C for 12 hours in muffle furnace to prepare single phase ErMnO3. The prepared sample was characterized by thermogravimetry differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). Under ultraviolet light, the photocatalytic activity of ErMnO3 was studied with methyl orange of 20 mg/L as the simulated sewage. The results show that the ErMnO3 sample particle size distribution is relatively uniform, the average grain size is mainly around 100 nm. The photocatalytic experiment demonstrates that ErMnO3 is highly photocatalytic activity for removal of methyl orange from water. When methyl orange of 20 mg/L is degraded for 120 min in the presence of ErMnO3, the degradation rate of methyl orange can reach about 95%. The degradation of methyl orange accords with first order kinetic model in presence ErMnO3 sample, and the apparent rate constant is 0.022 min-1.

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

    Directory of Open Access Journals (Sweden)

    Norhafizah Mohd Rasdi

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

  20. 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.

  1. Facile and green preparation of novel adsorption materials by combining sol-gel with ion imprinting technology for selective removal of Cu(II) ions from aqueous solution

    Science.gov (United States)

    Ren, Zhongqi; Zhu, Xinyan; Du, Jian; Kong, Delong; Wang, Nian; Wang, Zhuo; Wang, Qi; Liu, Wei; Li, Qunsheng; Zhou, Zhiyong

    2018-03-01

    A novel green adsorption polymer was prepared by ion imprinted technology in conjunction with sol-gel process under mild conditions for the selective removal of Cu(II) ions from aqueous solution. Effects of preparation conditions on adsorption performance of prepared polymers were studied. The ion-imprinted polymer was prepared using Cu(II) ion as template, N-[3-(2-aminoethylamino) propyl] trimethoxysilane (AAPTMS) as functional monomer and tetraethyl orthosilicate (TEOS) as cross-linker. Water was used as solvent in the whole preparation process. The imprinted and non-imprinted polymers were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), atomic force microscope (AFM), Brunauer, Emmett and Teller (BET) and zeta potential. Three-dimensional network structure was formed and functional monomer was successfully cross-linked into the network structure of polymers. Effects of adsorption conditions on adsorption performance of prepared polymers were studied too. The pH value is of great influence on adsorption behavior. Adsorption by ion-imprinted polymer was fast (adsorption equilibrium was reached within 60 min). The adsorption capacity of Cu(II) ion-imprinted polymer was always larger than that of non-imprinted polymer. Pseudo-second-order kinetics model and Freundlich isotherm model fitted well with adsorption data. The maximum adsorption capacity of Cu(II) ion-imprinted polymer was 39.82 mg·g-1. However, the preparation conditions used in this work are much milder than those reported in literatures. The Cu(II) ion-imprinted polymer showed high selectivity and relative selectivity coefficients for Pb(II), Ni(II), Cd(II) and Co(II). In addition, the prepared ion-imprinted polymer could be reused several times without significant loss of adsorption capacity.

  2. Preparation and corrosion resistance studies of nanometric sol-gel-based CeO2 film with a chromium-free pretreatment on AZ91D magnesium alloy

    International Nuclear Information System (INIS)

    Zhang Shiyan; Li Qing; Chen Bo; Yang Xiaokui

    2010-01-01

    Magnesium alloy, although valuable, is reactive and requires protection before it can be applied in many fields. In this study, a novel protective environmental-friendly gradient coating was performed on AZ91D magnesium alloy by non-chromate surface treatments, which consisted of phytic acid chemical conversion coating and the sol-gel-based CeO 2 thin film. The surface morphologies, microstructure and composition of the coatings were investigated by scanning electron microscopy (SEM), energy disperse spectroscopy (EDS) and X-ray diffraction (XRD), respectively. The corrosion resistance of the coatings was evaluated by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) in 3.5 wt.% NaCl solution. The effects of the concentration, layers, temperature of heat treatment of CeO 2 sol on the anti-corrosion properties of the gradient coating for magnesium were also investigated. The results showed that the gradient coating was mainly composed of crystalline CeO 2 . According to the results of electrochemical tests, the corrosion resistance of AZ91D magnesium alloy was found to be greatly improved by means of this new environmental-friendly surface treatment.

  3. 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

  4. The role of Ar plasma treatment in generating oxygen vacancies in indium tin oxide thin films prepared by the sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Hwang, Deuk-Kyu [Department of Materials Science and Engineering, Yonsei University, 50 Yonsei-ro, Seoul, 03722 (Korea, Republic of); Misra, Mirnmoy; Lee, Ye-Eun [Department of BioNano Technology, Gachon University, 1342 Seong-nam dae-ro, Seong-nam si, Gyeonggi-do, 13120 (Korea, Republic of); Baek, Sung-Doo [Department of Materials Science and Engineering, Yonsei University, 50 Yonsei-ro, Seoul, 03722 (Korea, Republic of); Myoung, Jae-Min, E-mail: jmmyoung@yonsei.ac.kr [Department of Materials Science and Engineering, Yonsei University, 50 Yonsei-ro, Seoul, 03722 (Korea, Republic of); Lee, Tae Il, E-mail: t2.lee77@gachon.ac.kr [Department of BioNano Technology, Gachon University, 1342 Seong-nam dae-ro, Seong-nam si, Gyeonggi-do, 13120 (Korea, Republic of)

    2017-05-31

    Highlights: • Indium tin oxide thin film with about 41 nm thickness was obtained by the sol-gel process. • Thin film exhibited low resistivity. • Sheet resistance of thin film decreases with Ar plasma treatment time. • Ar plasma treatment on thin film does not alter the crystal structure and optical properties of the ITO thin-film. • There is no significant change in oxygen vacancies after 20 min of plasma treatment. - Abstract: Argon (Ar) plasma treatment was carried out to reduce the sheet resistance of indium tin oxide (ITO) thin films. The Ar plasma treatment did not cause any significant changes to the crystal structure, surface morphology, or optical properties of the ITO thin films. However, an X-ray photoelectron spectroscopy study confirmed that the concentration of oxygen vacancies in the film dramatically increased with the plasma treatment time. Thus, we concluded that the decrease in the sheet resistance was caused by the increase in the oxygen vacancy concentration in the film. Furthermore, to verify how the concentration of oxygen vacancies in the film increased with the Ar plasma treatment time, cumulative and continuous plasma treatments were conducted. The oxygen vacancies were found to be created by surface heating via the outward thermal diffusion of oxygen atoms from inside the film.

  5. Preparation and characterization of hybrid materials of epoxy resin type bisphenol a with silicon and titanium oxides by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Carrillo C, A.; Osuna A, J. G., E-mail: acc.carrillo@gmail.com [Universidad Autonoma de Coahuila, Facultad de Ciencias Quimicas, Blvd. Venustiano Carranza y Jose Cardenas Valdes, 25000 Saltillo, Coahuila (Mexico)

    2011-07-01

    Hybrid materials were synthesized from epoxy resins as a result bisphenol type A-silicon oxide and epoxy resin bisphenol type A-titanium oxide were obtained. The synthesis was done by sol-gel process using tetraethyl orthosilicate (Teos) and titanium isopropoxide (I Ti) as inorganic precursors. The molar ratio of bisphenol A to the inorganic precursors was the studied variable. The materials were characterized by thermal analysis, infrared spectroscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy. The hybrid nature of the materials was demonstrated through thermal analysis and infrared spectroscopy. In both systems, as the amount of alkoxide increased, the bands described above were more defined. This behavior indicates the interactions between the resin and the alkoxides. Hybrids with Teos showed a smoother and homogeneous surface in its entirety, without irregularities. Hybrids with titanium isopropoxide had low roughness. Both Teos and I Ti hybrids showed a decrease on the atomic weight percentage of carbon due to a slight reduction of the organic part on the surface. (Author)

  6. Preparation and characterization of hybrid materials of epoxy resin type bisphenol a with silicon and titanium oxides by sol-gel process

    International Nuclear Information System (INIS)

    Carrillo C, A.; Osuna A, J. G.

    2011-01-01

    Hybrid materials were synthesized from epoxy resins as a result bisphenol type A-silicon oxide and epoxy resin bisphenol type A-titanium oxide were obtained. The synthesis was done by sol-gel process using tetraethyl orthosilicate (Teos) and titanium isopropoxide (I Ti) as inorganic precursors. The molar ratio of bisphenol A to the inorganic precursors was the studied variable. The materials were characterized by thermal analysis, infrared spectroscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy. The hybrid nature of the materials was demonstrated through thermal analysis and infrared spectroscopy. In both systems, as the amount of alkoxide increased, the bands described above were more defined. This behavior indicates the interactions between the resin and the alkoxides. Hybrids with Teos showed a smoother and homogeneous surface in its entirety, without irregularities. Hybrids with titanium isopropoxide had low roughness. Both Teos and I Ti hybrids showed a decrease on the atomic weight percentage of carbon due to a slight reduction of the organic part on the surface. (Author)

  7. Preparation of macroporous zirconia monoliths from ionic precursors via an epoxide-mediated sol-gel process accompanied by phase separation

    International Nuclear Information System (INIS)

    Guo, Xingzhong; Song, Jie; Lvlin, Yixiu; Yang, Hui; Nakanishi, Kazuki; Kanamori, Kazuyoshi

    2015-01-01

    Monolithic macroporous zirconia (ZrO 2 ) derived from ionic precursors has been successfully fabricated via the epoxide-mediated sol-gel route accompanied by phase separation in the presence of propylene oxide (PO) and poly(ethylene oxide) (PEO). The addition of PO used as an acid scavenger mediates the gelation, whereas PEO enhances the polymerization-induced phase separation. The appropriate choice of the starting compositions allows the production of a macroporous zirconia monolith with a porosity of 52.9% and a Brunauer–Emmett–Teller (BET) surface area of 171.9 m 2 · g −1 . The resultant dried gel is amorphous, whereas tetragonal ZrO 2 and monoclinic ZrO 2 are precipitated at 400 and 600 °C, respectively, without spoiling the macroporous morphology. After solvothermal treatment with an ethanol solution of ammonia, tetragonal ZrO 2 monoliths with smooth skeletons and well-defined mesopores can be obtained, and the BET surface area is enhanced to 583.8 m 2 · g −1 . (paper)

  8. Effect of citric acid on material properties of ZnGa2O4:Cr3+ nanopowder prepared by sol-gel method

    Science.gov (United States)

    Hussen, Megersa K.; Dejene, Francis B.; Gonfa, Girma G.

    2018-05-01

    This paper reports the material properties of Cr3+ (1.0 mol%)-doped ZnGa2O4 nanopowders prepared by citric acid-assisted sol-gel method with metal cations (Zn + Ga) to citric (M:CA) molar ratios of (1:0.5, 1:1, 1:3 and 1:4). The X-ray diffraction (XRD) results show that the synthesized nanoparticles are cubic structured and concentration of citric acid did not affect the structure. The scanning electron microscope (SEM) shows that the increase of the M:CA molar ratio favors the formation of smaller nano particle of ZnGa2O4:Cr3+. The photoluminescence (PL) is found to be maximum for sample with M:CA ratio of 1:1. Further increase in citric acid leads to significant decrease in the PL intensity. Energy-dispersive X-ray spectroscopy (EDS) measurement confirms the presence of the Zn, Ga, O and Cr ions. Ultraviolet-visible (UV-Vis) spectrophotometer measurement shows an increase in reflectance in visible region and the energy band gap was found to decrease with an increase in citric acid molar ratio. The emission spectra, particle size and photoluminescence lifetimes are comparable with reports on bioimaging applications.

  9. Structural and Luminescence Properties of Lu2O3:Eu3+ F127 Tri-Block Copolymer Modified Thin Films Prepared by Sol-Gel Method

    Science.gov (United States)

    de Jesus Morales Ramírez, Angel; Hernández, Margarita García; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Palmerin, Joel Moreno; Velazquez, Dulce Yolotzin Medina; Jota, María Luz Carrera

    2013-01-01

    Lu2O3:Eu3+ transparent, high density, and optical quality thin films were prepared using the sol-gel dip-coating technique, starting with lutetium and europium nitrates as precursors and followed by hydrolysis in an ethanol-ethylene glycol solution. Acetic acid and acetylacetonate were incorporated in order to adjust pH and as a sol stabilizer. In order to increment the thickness of the films and orient the structure, F127 Pluronic acid was incorporated during the sol formation. Structural, morphological, and optical properties of the films were investigated for different F127/Lu molar ratios (0–5) in order to obtain high optical quality films with enhanced thickness compared with the traditional method. X-ray diffraction (XRD) shows that the films present a highly oriented cubic structure beyond 1073 K for a 3-layer film, on silica glass substrates. The thickness, density, porosity, and refractive index evolution of the films were investigated by means of m-lines microscopy along with the morphology by scanning electron microscope (SEM) and luminescent properties. PMID:28809336

  10. Nanocrystalline sol-gel Nb{sub 2}O{sub 5} coatings. Preparation, characterisation and application to photovoltaic cell, lithium battery and eletrochromic device

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Yeping

    2002-07-01

    Thick and thin films of Nb{sub 2}O{sub 5} have been prepared by the sol-gel process using cheap niobium pentachloride as precursor and a new synthesis route. The microstructure of the films was tailored by adding poly(ethylene glycol) (PEG) and carbon soot into the sol and varying the sintering temperature. The thesis describes the properties of the sols and their influence on the properties of the resulting nanocrystalline Nb{sub 2}O{sub 5} films as electrodes in dye sensitised solar cells, electrochromic devices and rechargeable lithium batteries. A solar light-to-electric conversion efficiency of Ru(II) sensitised Nb{sub 2}O{sub 5} solar cell as high as 7% under 120 W/m{sup 2} illumination was obtained. An equivalent electric circuit of the dye sensitised electrode/electrolyte interface based on the electrochemical impedance spectroscopy was modelled and found to fit all the results. The values obtained for the electric elements from the simulation of the results were found to relate material parameters to the cell performance and their influence on the cell performance are illustrated. The electrochromism and Li{sup +}-charge and discharge of the Nb{sub 2}O{sub 5} films exhibited also good performance. (orig.)

  11. Polarization fatigue resistance of Ca-doped Pb(Zr0.52Ti0.48)O3 thin films prepared by the sol-gel method

    International Nuclear Information System (INIS)

    Wei, T.; Wang, Y.; Zhu, C.; Dong, X.W.; Xia, Y.D.; Zhu, J.S.; Liu, J.-M.

    2008-01-01

    The ferroelectric and polarization fatigue characteristics of Pb 1-x Ca x (Zr 0.52 Ti 0.48 )O 3 (PCZT) thin films prepared using the sol-gel method were studied. The Ca-doping slightly suppresses the ferroelectricity of Pb(Zr 0.52 Ti 0.48 )O 3 (PZT) because of the quantum paraelectric behavior of CaTiO 3 . Compared with PZT thin films, the PCZT (x=0.2) thin films show enhanced fatigue resistance at room temperature, further emphasized by the almost fatigue-free behavior at 100 K. The temperature-dependent dc-conductivity suggests a decrease of the oxygen vacancy density by almost 20 times and a slightly declined activation energy U for oxygen vacancies, upon increasing of the Ca-doping content from 0.0 to 0.2. It is argued that the improved fatigue endurance is ascribed to the decreasing density of oxygen vacancies due to the Ca-doping, although the lowered activation energy of oxygen vacancies is unfavorable. (orig.)

  12. Preparation of Si/TiO2 Composite by the Sol-Gel Method Using As the Lithium-Ion Battery Anode

    Science.gov (United States)

    Wang, Quanwei; Ban, Yueqin; Zhou, Hengwei; Zhang, Lili; Huang, Yineng; Shao, Weiquan; Chen, Shaou

    2017-10-01

    Si was a promising anode material for next-generation LIBs due to its extremely large capacity of 4200mAh/g (Li4.4Si phase). However, during repeated lithium insertion/extraction processes, the accompanied huge volume change (400%) induced the structural failure of the active material and resulted in rapid capacity fading. To overcome this problem, Si/TiO2 composite with different mole ratio were prepared by the sol-gel method. The inclusion of TiO2 not only worked as a stable electric conductive pathway but also buffered the volume expansion of the Si during the process of charging and discharging. The Si/TiO2 composite with different mole ratio of 1:2, 1:3, 1:4 electrode reaches 480mAh/g, 2590mAh/g and 980mAh/g, and it delivered a charge capacity of 461mAh/g, 2510mAh/g and 891mAh/g at the first cycle, corresponding to an initial coulombic efficiency of 96%, 96% and 91%. In contrast, the cell with the pure Si nanoparticle exhibited an initial discharge/charge capacity of 48 and 33mAh/g, respectively, which was much lower than the Si/TiO2 composite electrode.

  13. Mossbauer, Raman and X-ray diffraction studies of superparamagnetic NiFe2O4 nanoparticles prepared by sol-gel auto-combustion method

    International Nuclear Information System (INIS)

    Ahlawat, Anju; Sathe, V.G.; Reddy, V.R.; Gupta, Ajay

    2011-01-01

    Superparamagnetic nickel ferrite single phase nanoparticles with the average crystallite size of ∼9 nm have been synthesized at a low temperature (220 o C) by the sol-gel auto-combustion method. In the present study the as prepared powder was further calcined at different temperatures for 4 h, resulting in nanoparticles of larger size. The nanoparticles exhibited superparamagnetic behavior and changes in cation distribution as revealed by the Mossbauer, Raman and X-ray diffraction studies. The Mossbauer spectra collected at 5 K and under 5 T applied magnetic field showed mixed spinel structure and canted spin order for the nanoparticles, whereas there is collinear spin order with inverse spinel structure for larger particles. The vibrational spectra of the nanoparticles showed a redshift and broadening in the Raman line shape due to confinement effects. - Highlights: → Mossbauer spectra show a canting angle of 48 o for the nanoparticle samples measured at 5 K and 5 T applied magnetic field, the highest canting angle obtained so far in NiFe 2 O 4 nanoparticles. Site inversion in nanoparticles, thus converting it from inverse spinel to mixed spinel structure. → X-ray diffraction results showed a change in sign for the strain of the nanoparticle sample that showed mixed spinel structure. → Our Raman measurements showed a redshift and broadening for nanoparticle samples that is generally interpreted as a signature of quantum confinement.

  14. Structural, optical and NO{sub 2} gas sensing properties of ZnMgO thin films prepared by the sol gel method

    Energy Technology Data Exchange (ETDEWEB)

    Chebil, W., E-mail: chbil.widad@live.fr [Unité de Service Commun de Recherche « High resolution X-ray diffractometer », Département de Physique, Université de Monastir, Faculté des Sciences de Monastir, Avenue de l’Environnement, 5019, Monastir (Tunisia); Laboratoire Physico-chimie des Matériaux, Département de Physique, Université de Monastir, Faculté des Sciences de Monastir, Avenue de l' environnement, 5019 Monastir (Tunisia); Boukadhaba, M.A. [Unité de Service Commun de Recherche « High resolution X-ray diffractometer », Département de Physique, Université de Monastir, Faculté des Sciences de Monastir, Avenue de l’Environnement, 5019, Monastir (Tunisia); Laboratoire Physico-chimie des Matériaux, Département de Physique, Université de Monastir, Faculté des Sciences de Monastir, Avenue de l' environnement, 5019 Monastir (Tunisia); Madhi, I. [Laboratoire de Photovoltaïque, Centre de Recherche et des Technologies de l’Energie, Technopole de Borj-Cédria, BP 95, 2050, Hammam-Lif (Tunisia); and others

    2017-01-15

    In this present work, ZnO and ZnMgO thin films prepared by a sol-gel process were deposited on glass substrates via spin coating technique. The structural, morphological and optical properties of the obtained films were investigated. X-ray diffraction study revealed that all layers exhibit a hexagonal wurtzite structure without any secondary phase segregation. The atomic force microscopy (AFM) depicts that the grains size of ours samples decreases as magnesium content increases. The absorption spectra obtained on ZnMgO thin films show a band gap tuning from 3.19 to 3.36 eV, which is also consistent with blue shifting of near-band edge PL emission, measured at low temperature. The incorporated amount of magnesium was calculated and confirmed by EDX. The gas sensing performances were tested in air containing NO{sub 2} for different operating temperatures. The experimental result exhibited that ZnMgO sensors shows a faster response and recovery time than the ZnO thin films. The resistivity and the sensor response as function of Mg content were also investigated.

  15. A study of PbTiO sub 3 crystallization in pure and composite nanopowders prepared by the sol-gel technique

    CERN Document Server

    Cernansky, M; Kral, K; Krupkova, R

    2002-01-01

    In this investigation the crystallization of PbTiO sub 3 upon annealing of pure nanopowders and PbTiO sub 3 -SiO sub 2 (1:1 v/v) nanocomposite powders prepared by the sol-gel technique was studied. Using x-ray diffraction phase analysis, the start of PbTiO sub 3 crystallization in pure PbTiO sub 3 powders was detected at 400 sup o C. Distinct crystallization of PbTiO sub 3 in PbTiO sub 3 -SiO sub 2 nanocomposites starts at 700 sup o C, whereas SiO sub 2 remains amorphous. There are indications that an interface interaction between the PbTiO sub 3 and the SiO sub 2 phase plays an important role in hindering the crystallization of PbTiO sub 3. The particle size (size of coherently scattering regions) was estimated from the broadening of the x-ray diffraction line profiles. The average size of PbTiO sub 3 nanocrystallites increases with temperature and time of annealing, the influence of temperature being more significant than that of the annealing time. Differential scanning calorimetry confirmed the results of...

  16. Characteristics and optical properties of iron ion (Fe{sup 3+})-doped titanium oxide thin films prepared by a sol-gel spin coating

    Energy Technology Data Exchange (ETDEWEB)

    Wang, M.C. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Lin, H.J. [Department of Materials Science and Engineering, National United University, 1 Lein-Da, Kung-Ching Li, Miao-Li 36003, Taiwan (China)], E-mail: hjlin@nuu.edu.tw; Yang, T.S. [Department of Materials Science and Engineering, National United University, 1 Lein-Da, Kung-Ching Li, Miao-Li 36003, Taiwan (China)

    2009-04-03

    Titanium dioxide (TiO{sub 2}) thin films doping of various iron ion (Fe{sup 3+}) concentrations have been prepared on a glass substrate by the sol-gel spin coating process. Characteristics and optical properties of TiO{sub 2} thin films doping of various Fe content were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), ultraviolet-visible spectroscopy (UV-vis) and spectroscopic ellipsometry. The crystalline phase of TiO{sub 2} thin films comprised only the anatase TiO{sub 2}, but the crystallinity decreased when the Fe{sup 3+} content increased from 0 to 25.0 wt%. During the Fe{sup 3+} addition to 25.0 wt%, the phase of TiO{sub 2} thin film still maintained the amorphous state. The absorption edge of TiO{sub 2} thin films shifted towards longer wavelengths (i.e. red shifted) from 355 to 415 nm when the Fe{sup 3+}-doped concentration increased from 0 to 25.0 wt%. The values of the refractive index (n), and extinction coefficient (k), decreased with an increasing Fe{sup 3+} content. Moreover, the band-gap energy of TiO{sub 2} thin films also decreased from 3.29 to 2.83 eV with an increase in the Fe{sup 3+} content from 0 to 25.0 wt%.

  17. 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.

  18. 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.

  19. Influences of the iron ion (Fe3+)-doping on structural and optical properties of nanocrystalline TiO2 thin films prepared by sol-gel spin coating

    International Nuclear Information System (INIS)

    Ben Naceur, J.; Mechiakh, R.; Bousbih, F.; Chtourou, R.

    2011-01-01

    Titanium dioxide (TiO 2 ) thin films doping of various iron ion (Fe 3+ ) concentrations were deposited on silicon (Si) (100) and quartz substrates by sol-gel Spin Coating technique followed by a thermal treatment at 600 deg. C. The structure, surface morphology and optical properties, as a function of the doping, have been studied by X-ray diffractometer (XRD), Raman, ultraviolet-visible (UV-vis) and Spectroscopic Ellipsometry (SE). XRD and Raman analyzes of our thin films show that the crystalline phase of TiO 2 thin films comprised only the anatase TiO 2 , but the crystallinity decreased when the Fe 3+ content increased from 0% to 20%. During the Fe 3+ addition to 20%, the phase of TiO 2 thin film still maintained the amorphous state. The grain size calculated from XRD patterns varies from 29.3 to 22.6 nm. The complex index and the optical band gap (E g ) of the films were determined by the spectroscopic ellipsometry analysis. We have found that the optical band gap decreased with an increasing Fe 3+ content.

  20. 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

  1. Simple Preparation of ZnO Nano-layer by Sol-Gel Method as Active Electrode in P3HT/ZnO Heterojunction Solar Cell

    Science.gov (United States)

    Aprilia, Annisa; Herman, Hidayat, Rahmat

    2010-10-01

    Highly transparent undoped ZnO thin films have been prepared on glass and indium tin oxide substrates with simple process by sol-gel route and dip-coating deposition. Gel precursor of ZnO was prepared from zinc acetat dehydrate solution in methanol with the addition of trietylamine as stabilizing agent. Thin layer of gel precursor was prepared by dip coating and then followed by calcination at 400° C for 5 minute in air atmosphere. The thickness of the resulted ZnO thin film produced by ten times coating is about 150 nm. The films shows high transmittance larger than 98% in the visible region (400-800 nm). Absorption is observed in the UV region with absorption onset at about 390 nm indicating varying band gap between 3.18 eV until 3.23 eV depending on the number of coating layer. The AFM image shows that the films seems to be constructed from random stacking of nano-sized ZnO particle in the order of 50 nm. Among the prepared samples, the lowest resistivity is about 1.8×107 Ωm observed in the five-layer coating film. In order to fabricate solar cell structure, P3HT was deposited onto the ZnO thin film layer by spin casting technique and then followed by metal (Au) layer deposition by thermal evaporation. The formed solar cell has the inverted type solar cell with ITO/ZnO/P3HT/Au configuration. By the insertion ZnO layer, the photocurrent was improved by more than ten orders of magnitude in comparison to that of without ZnO layer. The measured photocurrent decreases at large number of coating layer which is supposed to be related with the current limitation by the effective carrier path length in ZnO layer.

  2. Preparation and characterization of multi-walled carbon nanotube/hydroxyapatite nanocomposite film dip coated on Ti-6Al-4V by sol-gel method for biomedical applications: an in vitro study.

    Science.gov (United States)

    Abrishamchian, Alireza; Hooshmand, Tabassom; Mohammadi, Mohammadreza; Najafi, Farhood

    2013-05-01

    In the present research, the introduction of multi-walled carbon nanotubes (MWCNTs) into the hydroxyapatite (HA) matrix and dip coating of nanocomposite on titanium alloy (Ti-6Al-4V) plate was conducted in order to improve the performance of the HA-coated implant via the sol-gel method. The structural characterization and electron microscopy results confirmed well crystallized HA-MWCNT coating and homogenous dispersion of carbon nanotubes in the ceramic matrix at temperatures as low as 500 °C. The evaluation of the mechanical properties of HA and HA/MWCNT composite coatings with different weight percentages of MWCNTs showed that the addition of low concentrations of MWCNTs (0.5 and 1 wt.%) had improved effect on the mechanical properties of nanocomposite coatings. Moreover, this in vitro study ascertained the biocompatibility of the prepared sol-gel-derived HA/MWCNT composite coatings. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. 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

  4. (0 0 2-oriented growth and morphologies of ZnO thin films prepared by sol-gel method

    Directory of Open Access Journals (Sweden)

    Guo Dongyun

    2016-09-01

    Full Text Available Zinc acetate was used as a starting material to prepare Zn-solutions from solvents and ligands with different boiling temperature. The ZnO thin films were prepared on Si(1 0 0 substrates by spin-coating method. The effect of baking temperature and boiling temperature of the solvents and ligands on their morphologies and orientation was investigated. The solvents and ligands with high boiling temperature were favorable for relaxation of mechanical stress to form the smooth ZnO thin films. As the solvents and ligands with low boiling temperature were used to prepare Zn-solutions, the prepared ZnO thin films showed (0 0 2 preferred orientation. As n-propanol, 2-methoxyethanol, 2-(methylaminoethanol and monoethanolamine were used to prepare Zn-solutions, highly (0 0 2-oriented ZnO thin films were formed by adjusting the baking temperature.

  5. 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.

  6. Preparation of YBa2Cu3O7-x superconducting solutions and films from alkoxide-based precursors using sol-gel method and investigation of their chemical reaction mechanisms

    International Nuclear Information System (INIS)

    Mutlu, Ibrahim Halil; Acun, Hediye; Celik, Erdal; Turkmen, Hasan

    2007-01-01

    In the development of coated superconductors sol-gel technique has been widely used as an effective processing method, especially in making long-length wires and tapes. However, one drawback associated with the deposition of YBa 2 Cu 3 O 7-x and Gd 2 O 3 buffer layer on Ni tape is the adhesion characteristic at interfaces YBCO-Gd 2 O 3 and Gd 2 O 3 -NiO and NiO-Ni substrate. In this paper, two strategies for adhesion enhancement of multilayered ceramic oxide coatings on Ni substrate were proposed: (1) formation of chemical bonds through surface condensation reactions, and development of ceramic networks through diffusion of alkoxide precursors. The current research has focused on the fabrication and adhesion of YBCO coatings on buffered Ni substrate using nine solutions prepared from Y, Ba and Cu alkoxides, solvent and chelating agent. Only two of YBCO solutions were successfully obtained while the rest of them were unsuccessful. Among these solutions we scrutinized chemical reaction mechanisms of a successful and an unsuccessful solution for comparison. How the chemical bonds and solubility were affected by the acids, base and solvents used in the solutions was demonstrated. It was shown that pH of the solution, homogeneity of the solution and gelation, steric affect of the chemicals in sol-gel solutions are significant issues to obtain high quality superconducting YBCO thin films. In addition, X-ray diffraction (XRD) was used to analyze phase structure of YBCO and compare results of chemical reactions obtained by a chemdraw programme. Scanning electron microscope (SEM) studies was carried out to examine microstructures of YBCO films produced from alkoxide precursors, solvent, chelating agent and modifying liquid chemical materials such as triethanolamine or ammonium hydroxide. It was found to be YBCO, Gd 2 O 3 , NiO and Ni phases in YBCO/Gd 2 O 3 /Ni sample from XRD analysis. That the solution prepared by using triethanolamine provided the best film quality and

  7. 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

  8. Preparation of Aligned ZnO Nanorod Arrays on Sn-Doped ZnO Thin Films by Sonicated Sol-Gel Immersion Fabricated for Dye-Sensitized Solar Cell

    Directory of Open Access Journals (Sweden)

    I. Saurdi

    2014-01-01

    Full Text Available Aligned ZnO Nanorod arrays are deposited on the Sn-doped ZnO thin film via sonicated sol-gel immersion method. The structural, optical, and electrical properties of the Sn-doped ZnO thin films were investigated. Results show that the Sn-doped ZnO thin films with small grain size (~20 nm, high average transmittance (96% in visible region, and good resistivity 7.7 × 102 Ω·cm are obtained for 2 at.% Sn doping concentration. The aligned ZnO nanorod arrays with large surface area were also obtained for 2 at.% Sn-doped ZnO thin film. They were grown on sol-gel derived Sn-doped ZnO thin film, which acts as a seed layer, via sonicated sol-gel immersion method. The grown aligned ZnO nanorod arrays show high transmittance at visible region. The fabricated dye-sensitised solar cell based on the 2.0 at.% Sn-doped ZnO thin film with aligned ZnO nanorod arrays exhibits improved current density, open-circuit voltage, fill factor, and conversion efficiency compared with the undoped ZnO and 1 at.% Sn-doped ZnO thin films.

  9. UV and visible activation of Cr(III)-doped TiO2 catalyst prepared by a microwave-assisted sol-gel method during MCPA degradation.

    Science.gov (United States)

    Mendiola-Alvarez, S Y; Guzmán-Mar, J L; Turnes-Palomino, G; Maya-Alejandro, F; Hernández-Ramírez, A; Hinojosa-Reyes, L

    2017-05-01

    Photocatalytic degradation of 4-chloro-2-methylphenoxyacetic acid (MCPA) in aqueous solution using Cr(III)-doped TiO 2 under UV and visible light was investigated. The semiconductor material was synthesized by a microwave-assisted sol-gel method with Cr(III) doping contents of 0.02, 0.04, and 0.06 wt%. The catalyst was characterized using X-ray powder diffraction (XRD), scanning electron microscopy (SEM), nitrogen physisorption, UV-Vis diffuse reflectance spectroscopy (DRS), and atomic absorption spectroscopy (AAS). The photocatalytic activity for the photodegradation of MCPA was followed by reversed-phase high-performance liquid chromatography (HPLC) and total organic carbon (TOC) analysis. The intermediates formed during degradation were identified using gas chromatography-mass spectrometry (GC-MS). Chloride ion evolution was measured by ion chromatography. Characterization results showed that Cr(III)-doped TiO 2 materials possessed a small crystalline size, high surface area, and mesoporous structure. UV-Vis DRS showed enhanced absorption in the visible region as a function of the Cr(III) concentration. The Cr(III)-doped TiO 2 catalyst with 0.04 wt% of Cr(III) was more active than bare TiO 2 for the degradation of MCPA under both UV and visible light. The intermediates identified during MCPA degradation were 4-chloro-2-methylphenol (CMP), 2-(4-hydroxy-2-methylphenoxy) acetic acid (HMPA), and 2-hydroxybuta-1,3-diene-1,4-diyl-bis (oxy)dimethanol (HBDM); the formation of these intermediates depended on the radiation source.

  10. 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.

  11. 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.

  12. Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: bonding to titanium and scanning electron microscopy.

    Science.gov (United States)

    Tredwin, Christopher J; Georgiou, George; Kim, Hae-Won; Knowles, Jonathan C

    2013-05-01

    Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) production has been characterised and optimised by the sol-gel method and the dissolution and biological properties of these materials were investigated. It was the objective of this study to investigate the potential bond strength and interaction of these materials with titanium. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the FHA and FA sol-gels. Using a spin coating technique the sol-gels were coated onto commercially pure titanium disks and crystallised at various temperatures. Using scanning electron microscopy (SEM) and elemental analysis, the surface characteristics, coating thickness and interaction of the Ti substrate and coating were investigated. The bond strengths of the coating to the Ti were investigated using an Instron Universal Load Testing Machine. Statistical analysis was performed with a two-way analysis of variance and post hoc testing with a Bonferroni correction. (1) Coating speed inversely influenced the coating thickness. (2) Increasing fluoride ion substitution and heating temperature significantly increased bond strength and (3) increasing fluoride ion substitution increased the coating thickness. FHA and FA synthesised using the sol-gel technique may offer a superior alternative to coating titanium implants with HA and plasma spraying. HA, FHA and FA materials synthesised by the sol-gel method may also have a use as bone grafting materials. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  13. Electro-Caloric Properties of BT/PZT Multilayer Thin Films Prepared by Sol-Gel Method.

    Science.gov (United States)

    Kwon, Min-Su; Lee, Sung-Gap; Kim, Kyeong-Min

    2018-09-01

    In this study, Barium Titanate (BT)/Lead Zirconate Titanate (PZT) multilayer thin films were fabricated by the spin-coating method on Pt (200 nm)/Ti (10 nm) SiO2 (100 nm)/P-Si (100) substrates using BaTiO3 and Pb(Zr0.90Ti0.10)O3 metal alkoxide solutions. The coating and heating procedure was repeated several times to form the multilayer thin films. All of BT/PZT multilayer thin films show X-ray diffraction patterns typical to a polycrystalline perovskite structure and a uniform and void free grain microstructure. The thickness of the BT and PZT film by one-cycle of drying/sintering was approximately 50 nm and all of the films consisted of fine grains with a flat surface morphology. The electrocaloric properties of BT/PZT thin films were investigated by indirect estimation. The results showed that the temperature change ΔT can be calculated as a function of temperature using Maxwell's relation; the temperature change reaches a maximum value of ~1.85 °C at 135 °C under an applied electric field of 260 kV/cm.

  14. 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.

  15. 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)

  16. 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

  17. 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.

  18. Influence of temperature in TL signal induced by gamma radiation in zircon prepared by sol gel via; Influencia de la temperatura en la senal TL inducida por la radiacion gamma en zirconia preparada via solgel

    Energy Technology Data Exchange (ETDEWEB)

    Salas, P.; Castano, V.M. [Instituto de Fisica, UNAM, Laboratorio Juriquilla, A.P. 1-1010, 76001 Queretaro (Mexico); Mendoza A, D.; Gonzalez M, P.R. [ININ, Mexico, D.F. (Mexico); Rosa C, E. de la [Centro de Investigaciones en Optical, Leon, Gto. (Mexico)

    2000-07-01

    In this work, it was realized a study of the temperature effects in thermoluminescent signal (Tl) induced by gamma radiation in zircon, which was prepared by the sol gel method. According to the obtained results, the zircon thermically treated at 500 C or over is sensitive to radiation. This sensitivity is increased when the temperature in study is augmented, moreover, the Tl spectra form also is modified with the temperature increment. The samples thermically treated at 750 C or over present a linear response in the dose interval 27 to 165 Gy; therefore, such materials result promissories for dosimetric purposes. (Author)

  19. Surface chemistry and moisture sorption properties of wood coated with multifunctional alkoxysilanes by sol-gel process

    DEFF Research Database (Denmark)

    Tshabalala, M.A.; Kingshott, P.; VanLandingham, M.R.

    2003-01-01

    penetrated the outer surface layers of the wood and condensed with hydroxyls that may not be readily accessible to the high molecular weight HDTMOS. Once attached to such sites, it is reasonable to assume that some of these surface derivatives of MTMOS condensed with other molecules of MTMOS and HDTMOS...

  20. Studying Structural, Optical, Electrical, and Sensing Properties of Nanocrystalline SnO2:Cu Films Prepared by Sol-Gel Method for CO Gas Sensor Application at Low Temperature

    Science.gov (United States)

    Al-Jawad, Selma M. H.; Elttayf, Abdulhussain K.; Saber, Amel S.

    Nanocrystalline SnO2 and SnO2:Cu thin films derived from SnCl2ṡ2H2O precursors have been prepared on glass substrates using sol-gel dip-coating technique. The deposited film was 300±20nm thick and the films were annealed in air at 500∘C for 1h. Structural, optical and sensing properties of the films were studied under different preparation conditions, such as Cu-doping concentration of 2%, 4% and 6wt.%. X-ray diffraction studies show the polycrystalline nature with tetragonal rutile structure of SnO2 and Cu:SnO2 thin films. The films have highly preferred orientation along (110). The crystallite size of the prepared samples reduced with increasing Cu-doping concentrations and the addition of Cu as dopants changed the structural properties of the thin films. Surface morphology was determined through scanning electron microscopy and atomic force microscopy. Results show that the particle size decreased as doping concentration increased. The films have moderate optical transmission (up to 82.4% at 800nm), and the transmittance, absorption coefficient and energy gap at different Cu-doping concentration were measured and calculated. Results show that Cu-doping decreased the transmittance and energy gap whereas it increased the absorption coefficient. Two peaks were noted with Cu-doping concentration of 0-6wt.%; the first peak was positioned exactly at 320nm ultraviolet emission and the second was positioned at 430-480nm. Moreover, emission bands were noticed in the photoluminescence spectra of Cu:SnO2. The electrical properties of SnO2 films include DC electrical conductivity, showing that the films have two activation energies, namely, Ea1 and Ea2, which increase as Cu-doping concentration increases. Cudoped nanocrystalline SnO2 gas-sensing material has better sensitivity to CO gas compared with pure SnO2.

  1. 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.

  2. Excellent Passivation of p-Type Si Surface by Sol-Gel Al2O3 Films

    International Nuclear Information System (INIS)

    Hai-Qing, Xiao; Chun-Lan, Zhou; Xiao-Ning, Cao; Wen-Jing, Wang; Lei, Zhao; Hai-Ling, Li; Hong-Wei, Diao

    2009-01-01

    Al 2 O 3 films with a thickness of about 100 nm synthesized by spin coating and thermally treated are applied for field-induced surface passivation of p-type crystalline silicon. The level of surface passivation is determined by techniques based on photoconductance. An effective surface recombination velocity below 100 cm/s is obtained on 10Ω ·cm p-type c-Si wafers (Cz Si). A high density of negative fixed charges in the order of 10 12 cm −2 is detected in the Al 2 O 3 films and its impact on the level of surface passivation is demonstrated experimentally. Furthermore, a comparison between the surface passivation achieved for thermal SiO 2 and plasma enhanced chemical vapor deposition SiN x :H films on the same c-Si is presented. The high negative fixed charge density explains the excellent passivation of p-type c-Si by Al 2 O 3 . (cross-disciplinary physics and related areas of science and technology)

  3. Thermal and Mechanical Properties of Novolac-Silica Hybrid Aerogels Prepared by Sol-Gel Polymerization in Solvent-Saturated Vapor Atmosphere

    Directory of Open Access Journals (Sweden)

    Mohamad Mehdi Seraji1, Seraji

    2015-05-01

    Full Text Available Nowadays organic–inorganic hybrid aerogel materials have attracted increasing interests due to improved thermal and mechanical properties. In the present research, initially, novolac type phenolic resin-silica hybrid gels with different solid concentrations were synthesized using sol-gel polymerization in solvent-saturatedvapor atmosphere. The hybrid gels were dried at air atmosphere through ambient drying process. This method removed the need for costly and risky supercritical drying process. The yields of the obtained hybrid aerogels increased with less shrinkage in comparison with conventional sol-gel process. The precursor of silica phase in this study was tetraethoxysilane and inexpensive novolac resin was used as a reinforcing phase. The results of FTIR analysis confirmed the simultaneous formation of silica and novolac gels in the hybrid systems. The resultant hybrid aerogels showed a nanostructure hybrid network with high porosity (above 80% and low density (below 0.25 g/cm3. Nonetheless, higher content of silica resulted in more shrinkage in the hybrid aerogel structure due to the tendency of the silica network to shrink more during gelation and drying process. The SEM images of samples exhibited a continuous network of interconnected colloidal particles formed during sol-gel polymerization with mean particle size of less than 100 nanometers. Si mapping analysis showed good distribution of silica phase throughout the hybrid structure. The results demonstrated improvements in insulation properties and thermal stability of novolac-silica aerogel with increasing the silica content. The results of compressive strength showed that the mechanical properties of samples declined with increasing the silica content.

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

    Science.gov (United States)

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

    2016-08-01

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

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

    Directory of Open Access Journals (Sweden)

    Bahar Khodadadi

    2017-01-01

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

  6. 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

  7. 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...

  8. 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.

  9. SOL-GEL SILICA-BASED Ag–Ca–P COATINGS WITH AGRESSIVE PRETREATMENT OF TITANIUM SUBSTRATE

    Directory of Open Access Journals (Sweden)

    ELENA BORSHCHEVA

    2011-12-01

    Full Text Available The aim of the experiment was the obtaining of thin silica coatings on titanium by sol-gel method, using mechanical (SiC - paper No.180 and chemical (leaching in HF pretreatments of the titanium substrates. The solutions were based on TEOS. For the sol-gel dipping process 4 different solutions were prepared: silica, silica with AgNO3 and silica + AgNO3 with brushite (CaHPO4·2H2O or monetite (CaHPO4 powders. The solutions were aged for 7 and 14 days at laboratory temperature. After sol-gel dip-coating process the samples were dried and fired. The adhesion of fired coatings was measured by tape test according to ASTM procedure and the bioactivity of the coatings was tested using in vitro test. The surfaces of the samples after firing, tape test and in vitro test were observed with the optical and electron microscopes. The firing results showed that silica-silver coatings did not change, brushite sol-gel coatings have cracked and the monetite sol-gel coatings have cracked also, but less than brushite ones. In spite of coating´s crackings, the square’s frames made on the surfaces were without any breakdowns after tape tests and the adhesion of all coatings was very good, classified by the highest grade 5. The results of in vitro tests showed that all coatings interacted with simulated body fluid (SBF. After exposition in SBF the new layer formed on substrates. In case of 7 days aged coatings containing brushite the new layer was uniform and compact. In case of 7 days aged coatings containing monetite the new layer was formed by crystals aggregated tightly together. The monetite and brushite coatings prepared from 14 days aged sol were the same as previous ones, but they were thicker. X-ray analyses after in vitro test confirmed dellaite, titanate and hydroxyapatite phases.

  10. 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)

  11. 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.

  12. Growth of Gd{sub 2}O{sub 3} coherent layers on UO{sub 2} microsphere surface via sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Ribeiro, Luciana S.; Silva, Edilaine F.; Oliveira, Felipe W.F.; Pereira, Yara S.; Brandão, Alisson F.C.; Santos, Ana Maria M.; Lameiras, Fernando S.; Reis, Sergio C.; Pedrosa, Tércio A.; Santos, Armindo, E-mail: santosa@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-07-01

    In this work, we synthesized and characterized UO{sub 2}-Gd{sub 2}O{sub 3} nuclear fuel via three routes, aiming to solve the problems arising from the addition of Gd{sub 2}O{sub 3} in UO{sub 2} matrix. By the industrial route, the mixture of powders (UO{sub 2}, <90 μ and 6 wt% Gd{sub 2}O{sub 3} <10 μm) results in pellets with 91% TD at 1677 °C/H{sub 2}/4 h. By the mixed route, the formation of Gd{sub 2}O{sub 3} coherent layers on UO{sub 2} powder (particles <90 μ) and microsphere (225 μm) surface produced UO{sub 2} - 6 wt% Gd{sub 2}O{sub 3} pellets with 95% (powder; 1625 °C/H{sub 2}/4 hr) and 83% (microsphere; 1677°C/H{sub 2}/4 hr) TD. By the sol-gel route, we obtained UO{sub 2} - 6 wt% Gd{sub 2}O{sub 3} in a deagglomerated (powder; <70 μm) or agglomerated microsphere 232 μm) form whose pellets reached > 97% (powder) and >98% (microsphere) TI) at 1677 °C/H{sub 2}/4h. According to XRD, OM, and SEM/EDS analysis, the referred three routes do not form a complete solid solution of UO{sub 2}-Gd{sub 2}O{sub 3} at the temperatures and time of sintering used; Gd{sub 2}O{sub 3} granule islands are present in the pellets originating from these routes. The obtained results suggest that the topological arrangement and the deficient nanostructuring of UO{sub 2} and Gd{sub 2}O{sub 3} phases, either in the raw material (powder and microsphere) as in their compacts, are the cause of low densification and irregular distribution of Gd{sub 2}O{sub 3} in UO{sub 2} matrix; mixing of U and Gd at the molecular level does not form a solid solution; and the mixed route is a good alternative to the industrial route. (author)

  13. 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

  14. 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

  15. 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.)

  16. 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.

  17. Size Effects on Magnetic Properties of Ni0.5Zn0.5Fe2O4 Prepared by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Min Zhang

    2013-01-01

    Full Text Available Ni0.5Zn0.5Fe2O4 particles with different particle sizes have been synthesized by sol-gel method. X-ray diffraction results show that all the samples are pure cubic spinel structure with their sizes ranging from 9 to 96 nm. The lattice constant significantly decreases with further increasing annealing temperature. The magnetic measurements show superparamagnetic nature below the particle size of 30 nm, while others show ferrimagnetic nature above the corresponding blocking temperature. The blocking temperature increases with the increase in particle size, which can be explained by Stoner-Wohlfarth theory. The saturation magnetization increases as the particle size increases, which can be explained by the cation redistribution on tetrahedral A and octahedral B sites and the domain wall motion. The variation of coercivity as a function of particle size is based on the domain structure.

  18. Optical investigation of Tb{sup 3+}-doped Y{sub 2}O{sub 3} nanocrystals prepared by Pechini-type sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Back, M., E-mail: m.back@hotmail.it; Massari, A.; Boffelli, M.; Gonella, F.; Riello, P.; Cristofori, D. [Universita Ca' Foscari di Venezia and INSTM, Dipartimento di Scienze Molecolari e Nanosistemi (Italy); Ricco, R.; Enrichi, F., E-mail: enrichi@civen.org [CIVEN (Coordinamento Interuniversitario Veneto per le Nanotecnologie) (Italy)

    2012-03-15

    We report an optical study of Tb{sup 3+}-doped Y{sub 2}O{sub 3} nanocrystals synthesized by Pechini-type sol-gel method. The particles are investigated in terms of size and morphology by means of X-ray diffraction and transmission electron microscopy analysis. It is shown how the simple Pechini method allows for the growth of monocrystalline nanoparticles with a volume-weighted average size of about 30 nm. The optical properties of Tb{sup 3+} in the host lattice are studied in terms of PL, PLE, and lifetimes. Moreover, a correlation between the type of decay curves, the emission and excitation bands' shapes, and the site location of the emitting Tb{sup 3+} in the host material Y{sub 2}O{sub 3} is proposed.

  19. Direct crystallization of perovskite phase in PMN-PT thin films prepared by polyvinylpyrrolidone modified sol-gel processing and their properties

    International Nuclear Information System (INIS)

    Du, Z.H.; Zhang, T.S.; Zhu, M.M.; Ma, J.

    2009-01-01

    A modified sol-gel processing has been developed by using polyvinylpyrrolidone (PVP) as modifier and lead nitrate as lead source to synthesize (1-x)Pb(Mg 1/3 ,Nb 2/3 )O 3 -xPbTiO 3 (PMN-PT) thin films with x=0.23-0.43. With PVP additions, perovskite phase could directly crystallize from amorphous films at the temperature as low as 430 deg. C via bypassing the metastable phase-pyrochlore and crystallinity was significantly enhanced. The PVP addictives have been optimized with molecular weight 1/3 ,Nb 2/3 )O 3 -PbTiO 3 films via bypassing pyrochlore phase.

  20. Microstructure investigation on micropore formation in microporous silica materials prepared via a catalytic sol-gel process by small angle X-ray scattering.

    Science.gov (United States)

    Shimizu, Wataru; Hokka, Junsuke; Sato, Takaaki; Usami, Hisanao; Murakami, Yasushi

    2011-08-04

    The so-called sol-gel technique has been shown to be a template-free, efficient way to create functional porous silica materials having uniform micropores. This appears to be closely linked with a postulation that the formation of weakly branched polymer-like aggregates in a precursor solution is a key to the uniform micropore generation. However, how such a polymer-like structure can precisely be controlled, and further, how the generated low-fractal dimension solution structure is imprinted on the solid silica materials still remain elusive. Here we present fabrication of microporous silica from tetramethyl orthosilicate (TMOS) using a recently developed catalytic sol-gel process based on a nonionic hydroxyacetone (HA) catalyst. Small angle X-ray scattering (SAXS), nitrogen adsorption porosimetry, and transmission electron microscope (TEM) allowed us to observe the whole structural evolution, ranging from polymer-like aggregates in the precursor solution to agglomeration with heat treatment and microporous morphology of silica powders after drying and hydrolysis. Using the HA catalyst with short chain monohydric alcohols (methanol or ethanol) in the precursor solution, polymer-like aggregates having microscopic correlation length (or mesh-size) micropores with diameters 2 nm) in the solid product due to apertures between the particle-like aggregates. The data demonstrate that the extremely fine porous silica architecture comes essentially from a gaussian polymer-like nature of the silica aggregates in the precursor having the microscopic mesh-size and their successful imprint on the solid product. The result offers a general but significantly efficient route to creating precisely designed fine porous silica materials under mild condition that serve as low refractive index and efficient thermal insulation materials in their practical applications.

  1. 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

  2. Monolithic lithium-based aerogels via dispersed inorganic sol-gel method

    International Nuclear Information System (INIS)

    Xiao Shufang; Zhou Bin; Du Ai; Xu Xiang; Yang Xiaoyun; Shen Jun; Wu Guangming; Zhang Zhihua; Wan Huijun

    2008-01-01

    Monolithic lithium-based aerogels were prepared by poly acrylic acid (PAA) and propylene oxide (PO) via the dispersed inorganic sol-gel method and drying with CO 2 supercritical fluid dry process. The density of the prepared sample is about 150 g/m 3 . The microstructure of the lithium-based aerogels was characterized by TEM, IR, XPS and BET. The results show that the material mainly contains Li, C and O element s. BET surface area is up to 18.9 m 2 /g. (authors)

  3. 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.)

  4. 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.)

  5. 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.

  6. 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.

  7. 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

  8. 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

  9. Preparation of nanospinels NiMn{sub x}Fe{sub 2-x}O{sub 4} using sol-gel method and their applications on removal of azo dye from aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Khosravi, Iman [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad 917791436 (Iran, Islamic Republic of); Yazdanbakhsh, Mohammad, E-mail: myazdan@um.ac.ir [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad 917791436 (Iran, Islamic Republic of); Goharshadi, Elaheh K. [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad 917791436 (Iran, Islamic Republic of); Center of Nano Research, Ferdowsi University of Mashhad, Mashhad 91799 (Iran, Islamic Republic of); Youssefi, Abbas [Par -e- Tavous Research Institute, Mashhad 91000 (Iran, Islamic Republic of)

    2011-11-01

    Highlights: {yields} The nanospinels, NiMn{sub x}Fe{sub 2-x}O{sub 4} (x = 0.05, 0.1, 0.3, 0.5, 0.7, and 1), prepared by Sol-gel method. {yields} The nanospinels prepared, have been used for removal of approximately 90% of reactive blue 5 within 1 min. {yields} The degradation of RB5 dye, follows merely an adsorption process. - Abstract: In this paper, nanospinels NiMn{sub x}Fe{sub 2-x}O{sub 4} (x = 0.05, 0.1, 0.3, 0.5, 0.7, and 1) were prepared by sol-gel method in the presence of nitrate-metal-ethylene glycol (EG) polymerized complex. The nanospinels were characterized using thermogravimetry analysis (TGA), X-ray powder diffraction (XRD), Fourier infrared spectroscopy (FTIR), and transmission electron microscope (TEM). The adsorption of an azo dye, reactive blue 5 (RB5), from water was determined using the prepared nanospinels. The effect of operational parameters such as the initial dye concentration, the concentration of nanospinels, temperature, and pH on the degradation of dye was investigated. The adsorption process follows second-order kinetics and Arrhenius behavior. Two common models, the Langmuir and Freundlich isotherms were used to investigate the interaction of dye and nanospinels. The isotherm evaluations revealed that the Freundlich model provides better fit to the experimental data than that of the Langmuir model. The photocatalytic degradation of RB5 at pH 1 under UV irradiation was examined. The results showed that the degradation of RB5 dye follows merely an adsorption process.

  10. 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.

  11. Administration of a Sol-Gel Formulation of Phenylephrine Using Low-Temperature Hollow Microneedle for Treatment of Intermittent Fecal Incontinence.

    Science.gov (United States)

    Lee, Hyunji; Park, Jung-Hwan; Park, Jung Ho

    2017-12-01

    A low temperature hollow microneedle system was devised to deliver sol-gel transition formulation near the surface of the skin for extended release and local delivery of drug by a non-invasive method. This new system can improve treatment of intermittent fecal incontinence. The low-temperature system was integrated with a hollow microneedle to maintain the low temperature of the sol formulation. Various sol-gel formulations using Pluronic F-127 (PF-127) and Hydroxy-propyl-methyl-cellulose (HPMC) were prepared, and their gelation temperature, flow property, and diffusion retardation were observed. Resting anal sphincter pressure in response to a phenylephrine (PE) sol-gel formulation was measured using an air-charged catheter. The biocompatibility of the sol-gel PE formulation was evaluated by observing the immunological response. When the PF-127 25%, HPMC 1% and PE formulation (PF25-HPMC1-PE) was injected through the peri-anal skin of the rat in vivo, the highest pressure on the anal sphincter muscle occurred at 6-8 h and anal pressure increased and lasted twice as long as with the phosphate-buffered saline (PBS)-PE formulation. There was no significant difference in the number of mast cells after administration into the rat in vivo between the PF25-HPMC1-PE formulation and the PBS-PE formulation. The combination of a low-pain hollow microneedle system and an injectable sol-gel formulation improved the efficacy of treatment of intermittent fecal incontinence. A low-temperature hollow microneedle system using a sol-gel formulation has many applications in medical treatments that require depot effect, local targeting, and pain control.

  12. 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.

  13. Effect of ion nitriding on the crystal structure of 3 mol% Y2O3-doped ZrO2 thin-films prepared by the sol-gel method

    International Nuclear Information System (INIS)

    Ortiz, A.L.; Diaz-Parralejo, A.; Borrero-Lopez, O.; Guiberteau, F.

    2006-01-01

    We investigated the effect of ion nitriding on the crystal structure of 3 mol% Y 2 O 3 -doped ZrO 2 (3YSZ) thin-films prepared by the sol-gel method. For this purpose, we used X-ray diffractometry to determine the crystalline phases, the lattice parameters, the crystal sizes, and the lattice microstrains, and glow discharge-optical emission spectroscopy to obtain the depth profiles of the elemental chemical composition. We found that nitrogen atoms substitute oxygen atoms in the 3YSZ crystal, thus leading to the formation of unsaturated-substitutional solid solutions with reduced lattice parameters and Zr 0.94 Y 0.06 O 1.72 N 0.17 stoichiometric formula. We also found that ion nitriding does not affect the grain size, but does generate lattice microstrains due to the increase in point defects in the crystalline lattice

  14. Effect of Cu-doping on structural and electrical properties of Ni0.4-xCu0.3+xMg0.3Fe2O4 ferrites prepared using sol-gel method

    Science.gov (United States)

    Dhaou, Mohamed Houcine

    2018-06-01

    Ni0.4-xCu0.3+xMg0.3Fe2O4 spinel ferrites were prepared by sol-gel technique. X-ray diffraction results indicate that ferrite samples have a cubic spinel-type structure with ? space group. The electrical properties of the studied samples using complex impedance spectroscopy technique have been investigated as a function of frequency at different temperatures. We found that the addition of copper in Ni0.4-xCu0.3+xMg0.3Fe2O4 ferrite system can improve its conductivity. Dielectric properties have been discussed in terms of hopping of charge carriers between Fe2+ and Fe3+ ions. For all samples, frequency dependence of the imaginary part of impedance (Z") shows the existence of relaxation phenomenon. The appropriate equivalent circuit configuration for modeling the Nyquist plots of impedance is of the type of (Rg + Rgb//Cgb).

  15. Preparation of Pb(Zr0.52Ti0.48)O3 thin films on Pt/RuO2 double electrode by a new sol-gel route

    International Nuclear Information System (INIS)

    Kim, S.; Choi, Y.; Kim, C.; Oh, Y.

    1997-01-01

    Pb(Zr 0.52 Ti 0.48 )O 3 (PZT) thin film on Pt/RuO 2 double electrode was successfully prepared by using new alkoxide endash alkanolamine, sol-gel method. It was observed that the use of Pt/RuO 2 double electrode reduced leakage current, resulting in a marked improvement in the leakage characteristics and more reliable capacitors. Typical P-E hysteresis behavior was observed even at low applied voltage of 5 V, manifesting greatly improved remanance and coercivity. Fatigue and breakdown characteristic, measured at 5 V, showed stable behavior and no degradation in polarization was observed up to 10 11 cycles.copyright 1997 Materials Research Society

  16. Preparation and studies of Eu{sup 3+} and Tb{sup 3+} co-doped Gd{sub 2}O{sub 3} and Y{sub 2}O{sub 3} sol-gel scintillating films

    Energy Technology Data Exchange (ETDEWEB)

    Morales Ramirez, A. de J, E-mail: amoralesra@ipn.m [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada (CICATA) Unidad Altamira Instituto Politecnico Nacional Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Depto. de Ingenieria Metalurgica, ESIQIE-Instituto Politecnico Nacional UPALM C.P. 07738, Mexico D.F. (Mexico); Garcia Murillo, A.; Carrillo Romo, F. de J [Depto. de Ingenieria Metalurgica, ESIQIE-Instituto Politecnico Nacional UPALM C.P. 07738, Mexico D.F. (Mexico); Ramirez Salgado, J. [Programa de Ingenieria Molecular, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas No. 152, CP 07730, Mexico D.F. (Mexico); Le Luyer, C. [LPCML, CNRS-UMR 5620/Universite Claude Bernard Lyon 1/69622 Villeurbanne Cedex (France); Chadeyron, G.; Boyer, D. [Laboratoire des Materiaux Inorganiques, CNRS-UMR 6002, Universite Blaise Pascal, 24 Ave des Landais F 63177 Aubiere Cedex (France); Moreno Palmerin, J. [Depto. de Ingenieria Metalurgica, ESIQIE-Instituto Politecnico Nacional UPALM C.P. 07738, Mexico D.F. (Mexico)

    2009-10-30

    Eu{sup 3+} (2.5 at.%) and Tb{sup 3+} (0.005-0.01 at.%) co-doped gadolinium and yttrium oxide (Gd{sub 2}O{sub 3} and Y{sub 2}O{sub 3}) powders and films have been prepared using the sol-gel process. High density and optical quality thin films were prepared with the dip-coating technique. Gadolinium (III) 2,4-pentadionate and yttrium (III) 2,4-pentadionate were used as precursors, and europium and terbium in their nitrate forms were used as doping agents. Chemical and structural analyses (infrared spectroscopy, X-ray diffraction and high-resolution transmission electron microscopy) were conducted on both sol-gel precursor powders and dip-coated films. The morphology of thin films heat-treated at 700 {sup o}C was studied by means of atomic force microscopy. It was shown that the highly dense and very smooth films had a root mean roughness (RMS) of 2 nm {+-} 0.2 (A = 0.0075 Tb{sup 3+}) and 24 nm {+-} 3.0 (B = 0.01 Tb{sup 3+}). After treatment at 700 {sup o}C, the crystallized films were in the cubic phase and presented a polycrystalline structure made up of randomly oriented crystallites with grain sizes varying from 20 to 60 nm. The X-ray induced emission spectra of Eu{sup 3+}- and Tb{sup 3+}-doped Gd{sub 2}O{sub 3} and Y{sub 2}O{sub 3} powders showed that Tb{sup 3+} contents of 0.005, 0.0075 and 0.01 at.% affected their optical properties. Lower Tb{sup 3+} concentrations (down to 0.005 at.%) in both systems enhanced the light yield.

  17. 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.

  18. The Preparation of TiO₂ Film by the Sol-Gel Method and Evaluation of Its Self-Cleaning Property.

    Science.gov (United States)

    Liang, Yu; Sun, Sijia; Deng, Tongrong; Ding, Hao; Chen, Wanting; Chen, Ying

    2018-03-19

    TiO₂ sol was produced by the sol-gel method through the hydrolysis and the aging of tetrabutyl titanate and the TiO₂ film was obtained by dipping and uniform lifting of the acid-treated and ultrasound-treated clean glass slides into the TiO₂ sol followed by aging, drying, and calcination. The effect of the hydrolysis control agents to the formed sol was researched and the crystalline state, the morphology, and the photocatalytic properties of the products after calcination were characterized. The structural morphology, the contact angles before and after illumination, and the self-cleaning properties of the TiO₂ film were characterized as well. The results showed that by using acetylacetone as the hydrolysis control agent, the formed TiO₂ sol had relatively high stability. The product after the calcination of the TiO₂ sol was of single anatase type with crystalline size of 18-20 nm and it could degrade nearly 100% of methylene blue after 90 min illumination. The formed TiO₂ film is compact, continuous, smooth, and had the properties of super-hydrophilicity (after 30 min illumination due to its contact angle decreasing from 21° to nearly 0°) and anti-fogging capability, which indicated its excellent self-cleaning property.

  19. Humidity Sensitivity of MgCr2O4-TiO2-LiO2 Ceramics Sensor Prepared by Sol-Gel Routes

    Directory of Open Access Journals (Sweden)

    H. Y. He

    2010-05-01

    Full Text Available 79.5MgCr2O4–19.5TiO2–Li2O porous ceramics were investigated as a humidity sensor. The sensors obtain by a cold isostatic pressing and sintering of the fine MgCr2O4 and TiO2 and LiCO3 powders. The MgCr2O4 and TiO2 powders were respectively synthesized by sol-gel methods. The effects of sintering temperature on the humidity sensitivity of sensors were studied by measuring electrical resistance in different conditions of relative humidity (R.H. at 27 °C. The results indicated that the calcining temperature obviously affected the resistance variation of the sensor in range of 11.3-84.7 % RH. The resistance variation was small at the calcining temperature of 600 oC for 2 h. With increasing calcining temperature, the resistance variation increased to 5.4×104% and 7.0×104 % at 800 oC and 1000 oC for 2 h, but decreased to 3.1×104 % at 1200 oC for 2 h respectively. The response times are 25 s and 35 s respectively for humidity adsorption and humidity desorption between 11.3 %RH and 84.7 %RH.

  20. Preparation by Poly(Acrylic Acid) Sol-Gel Method and Thermoelectric Properties of γ-Na x CoO2 Bulk Materials

    Science.gov (United States)

    Li, Xiaoyu; Zhang, Li; Tang, Xinfeng

    2017-11-01

    γ-Na x CoO2 single-phase powders have been synthesized by a poly(acrylic acid) (PAA) sol-gel (SG) method, and γ-Na x CoO2 bulk ceramic fabricated using spark plasma sintering. The effects of the PAA concentration on the sample phase composition and morphology were investigated. The thermoelectric properties of the γ-Na x CoO2 bulk ceramic were also studied. The results show that the PAA concentration did not significantly affect the crystalline phase of the product. However, agglomeration of γ-Na x CoO2 crystals was suppressed by the steric effect of PAA. The Na x CoO2 bulk ceramic obtained using the PAA SG method had higher crystallographic anisotropy, better chemical homogeneity, and higher density than the sample obtained by solid-state reaction (SSR), leading to improved thermoelectric performance. The PAA SG sample had power factor (in-plane PF = σS 2) of 0.61 mW m-1 K-2 and dimensionless figure of merit ( ZT) along the in-plane direction of 0.19 at 900 K, higher than for the SSR sample (in-plane PF = 0.51 mW m-1 K-2, in-plane ZT = 0.17). These results demonstrate that a simple and feasible PAA SG method can be used for synthesis of Na x CoO2 ceramics with improved thermoelectric properties.

  1. Preparation of layered oxide Li(Co1/3Ni1/3Mn1/3)O2 via the sol-gel process

    Institute of Scientific and Technical Information of China (English)

    ZHANG Wen; LIU Hanxing; HU Chen; ZHU Xianjun; LI Yanxi

    2008-01-01

    To obtain homogenous layered oxide Li(Co1/3Ni1/3Ni1/3Mn1/3)O2 as a lithium insertion positive electrode material,the sol-gel process using citric acid as a chelating agent was applied.The material Li(Co1/3,Ni1/3Mn1/3)O2 was synthesized at different calcination temperatures.XRD experiment indicated that the hyered Li(Co1/3Ni1/3Mn1/3)O2material could he synthesized at a lower temperature of 800℃,and the oxidation state of Co,Ni,and Mn in the cathode confirmed by XPS were +3,+2,and +4,respectively.SEM observations showed that the synthesized material could form homogenous particle morphology with the particle size of about 200nm In spite of different calcination temperatures,the charge-discharge curves of all the samples for the initial cycle were similar,and the cathode synthesized at 900℃ showed a small irreversible capacity loss of 11.24% and a high discharge capacity of 212.2 mAh.g-1 in the voltage range of 2.9-4.6 V.

  2. Influence of sintering temperature on microstructures and energy-storage properties of barium strontium titanate glass-ceramics prepared by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Jia; Zhang, Yong; Song, Xiaozhen; Zhang, Qian; Yang, Dongliang; Chen, Yongzhou [Beijing Key Laboratory of Fine Ceramics, State Key Laboratory of New Ceramics and Fine Processing, Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing, 100084 (China)

    2015-12-15

    The sol-gel processing, microstructures, dielectric properties and energy-storage properties of barium strontium titanate glass-ceramics over the sintering temperature range of 1000-1150 C were studied. Through the X-ray diffraction result, it is revealed that the crystallinity increases as the sintering temperature increased from 1000 to 1080 C and has reached a steady-state regime above 1100 C. Scanning electron microscopy images showed that with the increase of sintering temperature, the crystal size increased. Dielectric measurements revealed that the increase in the sintering temperature resulted in a significant increase in the dielectric constant, a strong sharpness of the temperature-dependent dielectric response and a pronounced decrease of the temperature of the dielectric maximum. The correlation between charge spreading behavior and activation energies of crystal and glass was discussed by the employment of the impedance spectroscopy studies. As a result of polarization-electric field hysteresis loops, both the charged and discharged densities increased with increasing sintering temperature. And the maximum value of energy storage efficiency was found to occur at 1130 C. Finally, the dependence of released energy and power densities calculated from the discharged current-time (I-t) curves on the sintering temperature was studied. The relationship between the energy storage properties and microstructure was correlated. Polarization-electric field hysteresis loops for the BST glass-ceramics sintered at different temperatures. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  3. Crystallization kinetics and growth mechanism of 8 mol% yttria-stabilized zirconia (8YSZ) nano-powders prepared by a sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Kuo, C.-W. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Lee, Y.-H. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hung, I-M. [Department of Chemical Engineering and Materials Science, Yuan Ze University, 135 Far-East Road, Chung-Li, Taoyuan, Taiwan (China); Wang, M.-C. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Wen, S.-B. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Fung, K.-Z. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Shih, C.-J. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China)], E-mail: cjshih@kmu.edu.tw

    2008-04-03

    Eight mol% yttria-stabilized zirconia (8YSZ) gel powders were synthesized at 348 K for 2 h using ZrOCl{sub 2}.8H{sub 2}O and Y(NO{sub 3}){sub 3}.6H{sub 2}O as starting materials in an ethanol-water solution by a sol-gel process. The crystallization kinetics and growth mechanism of the 8YSZ gel powders have been investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The XRD results and SAED pattern show that the 8YSZ gel powders calcined at 773 K for 2 h is a cubic ZrO{sub 2}. The activation energy for the crystallization of the cubic ZrO{sub 2} formation in the 8YSZ gel powders is determined as 231.76 kJ/mol by a non-isothermal DTA method. Both growth morphology parameter (n) and crystallization mechanism index (m) are close to 3.0, indicating that the bulk nucleation is dominant in the cubic ZrO{sub 2} formation. The TEM examination shows that the cubic ZrO{sub 2} has a spherical-like morphology with a size ranging from 10 to 20 nm.

  4. Crystallization kinetics and growth mechanism of 8 mol% yttria-stabilized zirconia (8YSZ) nano-powders prepared by a sol-gel process

    International Nuclear Information System (INIS)

    Kuo, C.-W.; Lee, Y.-H.; Hung, I-M.; Wang, M.-C.; Wen, S.-B.; Fung, K.-Z.; Shih, C.-J.

    2008-01-01

    Eight mol% yttria-stabilized zirconia (8YSZ) gel powders were synthesized at 348 K for 2 h using ZrOCl 2 .8H 2 O and Y(NO 3 ) 3 .6H 2 O as starting materials in an ethanol-water solution by a sol-gel process. The crystallization kinetics and growth mechanism of the 8YSZ gel powders have been investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The XRD results and SAED pattern show that the 8YSZ gel powders calcined at 773 K for 2 h is a cubic ZrO 2 . The activation energy for the crystallization of the cubic ZrO 2 formation in the 8YSZ gel powders is determined as 231.76 kJ/mol by a non-isothermal DTA method. Both growth morphology parameter (n) and crystallization mechanism index (m) are close to 3.0, indicating that the bulk nucleation is dominant in the cubic ZrO 2 formation. The TEM examination shows that the cubic ZrO 2 has a spherical-like morphology with a size ranging from 10 to 20 nm

  5. 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

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. Structural and magnetic properties of Mg-Zn ferrites (Mg{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4}) prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Reyes-Rodríguez, Pamela Yajaira, E-mail: pamela2244_4@hotmail.com [Cinvestav-Unidad Saltillo, Av. Industrial Metalúrgica #1062, Parque Industrial Saltillo-Ramos Arizpe, CP 25900, México (Mexico); Cortés-Hernández, Dora Alicia; Escobedo-Bocardo, José Concepción; Almanza-Robles, José Manuel; Sánchez-Fuentes, Héctor Javier; Jasso-Terán, Argentina; De León-Prado, Laura Elena [Cinvestav-Unidad Saltillo, Av. Industrial Metalúrgica #1062, Parque Industrial Saltillo-Ramos Arizpe, CP 25900, México (Mexico); Méndez-Nonell, Juan [Centro de Investigación en Materiales Avanzados, Ave. Miguel Cervantes #120, Complejo Industrial Chihuahua, CP 31109 Chihuahua, México (Mexico); Hurtado-López, Gilberto Francisco [Centro de Investigación en Química Aplicada, Blvd. Enrique Reyna Hermosillo #140, CP 25294 Saltillo, Coahuila, México (Mexico)

    2017-04-01

    In this study, the Mg{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} nanoparticles (x=0–0.9) were prepared by sol-gel method. These ferrites exhibit an inverse spinel structure and the lattice parameter increases as the substitution of Zn{sup 2+} ions is increased. At lower Zn content (0.1≤x≤0.5), saturation magnetization (Ms) increases, while it decreases at higher Zn content (x≥6). The remnant magnetization (0.17–2.0 emu/g) and coercive field (6.0–60 Oe) indicate a ferrimagnetic behavior. The average core diameter of selected ferrites is around 15 nm and the nanoparticles morphology is quasi spherical. The heating ability of some Mg{sub 0.9}Zn{sub 0.1}Fe{sub 2}O{sub 4} and Mg{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} aqueous suspensions indicates that the magnetic nanoparticles can increase the medium temperature up to 42 °C in a time less than 10 min - Highlights: • Magnetic nanoparticles of Mg{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} were synthesized by sol-gel method. • Nanoparticles showing a single spinel crystalline structure were obtained. • Aqueous suspensions of Mg{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} and Mg{sub 0.9}Zn{sub 0.1}Fe{sub 2}O{sub 4} show heating ability.

  11. 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.

  12. Evaluation of hybrid sol-gel incorporated with nanoparticles as nano paint

    International Nuclear Information System (INIS)

    Jameel, Zainab N.; Haider, Adawiya J.; Taha, Samar Y.; Gangopadhyay, Shubhra; Bok, Sangho

    2016-01-01

    A coating with self-cleaning characteristics has been developed using a TiO_2/SiO_2 hybrid sol-gel, TiO_2 nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO_2 nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO_2 nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO_2 phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO_2 NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

  13. Evaluation of hybrid sol-gel incorporated with nanoparticles as nano paint

    Energy Technology Data Exchange (ETDEWEB)

    Jameel, Zainab N., E-mail: zeinb76-alrekbe@yahoo.com; Haider, Adawiya J., E-mail: adawiyahaider@yahoo.com [Nanotechnology and Advanced Materials Research Center, The University of Technology, Baghdad (Iraq); Taha, Samar Y., E-mail: samarjam2002@yahoo.com [College of Science for Women, University of Baghdad, Baghdad (Iraq); Gangopadhyay, Shubhra, E-mail: gangopadhyays@missouri.edu; Bok, Sangho, E-mail: BokSa@missouri.edu [Department of Electrical and Computer, University of Missouri, Engineering, Building West, Columbia, Missouri 65211 (United States)

    2016-07-25

    A coating with self-cleaning characteristics has been developed using a TiO{sub 2}/SiO{sub 2} hybrid sol-gel, TiO{sub 2} nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO{sub 2} nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO{sub 2} nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO{sub 2} phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO{sub 2} NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

  14. Photoelectrochemical performance of Mn-TiO{sub 2} thin films mounted on FTO prepared by sol-gel spin coating

    Energy Technology Data Exchange (ETDEWEB)

    Chen, J.C.; Song, G.H. [National Central Univ., Taoyuan, Taiwan (China). Dept. of Mechanical Engineering; Lu, C.W. [Jen-Teh Junior College, Hou- Lung, Taiwan (China). Dept. of Information Management; Tseng, C.J. [National Central Univ., Chung-Li, Taoyuan County, Taiwan (China). Dept. of Mechanical Engineering; Cheng, K.W. [Chang Gung Univ., Tao-Yuan, Taiwan (China). Dept. of Chemical and Materials Engineering

    2009-07-01

    Tin oxide (TiO{sub 2}) sol-gels with Mn{sup 2+} molar ratios ranging from 0 to 0.1 per cent were used to form nano-structured Mn(x)Ti(1-x)O(2) thin films. A layer-by-layer spincoating (LLSC) technique was used, in which 10 very thin and uniform coating layers of Mn(x)Ti(1-x)O(2) were deposited on fluorine doped tin oxide (FTO) glass. Properties of the thin films were determined as a function of annealing temperature and molar ratio of the Mn{sup 2+} ions by X-ray diffraction (XRD), scanning electron microscopy (SEM), Atomic Force microscopy (AFM) and photoelectrochemical (PEC) measurements. The PEC measurements were obtained in a dry-type three-electrode cell consisting of sample, platinized and reference Ag/AgCl electrodes. The results revealed that the Mn(x)Ti(1-x)O(2) thin films have better structure and electrochemical characteristics when the annealing temperature is 550 degrees C. The TiO{sub 2} thin films with Mn{sup 2+} ions also had higher photocurrent than undoped TiO{sub 2}. The optimum Mn{sup 2+} loading in this study was found to be 0.1 ml per cent. The maximum photocurrent of Mn(0.1)Ti(0.9)O(2) thin films is about 0.68 mA/cm2 when the bias potential is 0.8 V (vs.Ag/AgCl).

  15. Synthesis and physical properties of TEOS-based silica aerogels prepared by two step (acid-base) sol-gel process

    International Nuclear Information System (INIS)

    Venkateswara Rao, A.; Bhagat, S.D.

    2004-01-01

    The experimental results on the synthesis and physical properties of tetra-ethoxy-silane- (TEOS) based silica aerogels produced by two step (acid-base) sol-gel process, are reported. The oxalic acid (A) and NH 4 OH (B) concentrations were varied from 0 to 0.1 M and from 0.4 to 3 M, respectively. Monolithic and transparent aerogels have been obtained for the values of A=0.001 M and B=1 M. The effect of time interval (t) before the base catalyst (NH 4 OH) addition to the acidic sol was studied from 0 to 72 h. The time interval at t=24 h of NH 4 OH addition was found to be the best, in terms of low volume shrinkage, high optical transmission and monolithicity. The molar ratio of EtOH/TEOS (S) was varied from 3 to 7.5. Monolithic and transparent aerogels were obtained for an S value of 6.9. Also, the effects of molar ratio of acidic water, i.e., H 2 O/TEOS (W1) and basic water, i.e., H 2 O/TEOS (W2) on the physical properties of the aerogels have been studied. Highly transparent (about 90%) and monolithic aerogels with lower volume shrinkage ( 2 O):basic (H 2 O). The results are discussed by taking into consideration the hydrolysis and poly-condensation reactions. The aerogels were characterized by scanning electron microscopy (SEM), optical transmission, bulk density, volume shrinkage and porosity measurements. (authors)

  16. 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.

  17. 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)

  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. Methylene blue degradation by NaTaO3 sol-gel doped with Sm and La

    International Nuclear Information System (INIS)

    Torres-Martinez, Leticia M.; Cruz-Lopez, Arquimedes; Juarez-Ramirez, Isaias; Meza-de la Rosa, Ma. Elena

    2009-01-01

    In this work, NaTaO 3 compounds doped with 1 M% of La and Sm, were prepared by the sol-gel (SG) method and solid state (SS) reaction; and tested as photocatalysts on the degradation of methylene blue (MB) under UV light. The structural characterization by X-ray powder diffraction revealed that the crystallization of the NaTaO 3 phase prepared by the sol-gel method started at 600 deg. C, reaching maximum crystallization at 800 deg. C. It was determined that the presence of Sm and La retard the crystallization of the NaTaO 3 phase. On the other hand, the compounds synthesized in this work showed particle sizes in the nanometric scale, as it was observed by scanning electron microscopy (SEM). The specific surface area of the compounds synthesized by the sol-gel method, showed values 4 times higher than those obtained by the solid state reaction, favoring their functional and photocatalytic performance in the methylene blue degradation. In addition, the best photocatalytic performance was shown by the NaTaO 3 doped with Sm and heated at 600 deg. C, having a half-life time of 65 min.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. Synthesis of Alkylpoly glucoside from Dextrose-Decanol in the Presence of Silicotungstic Acid Sol-Gel Catalyst

    International Nuclear Information System (INIS)

    Izazi Azzahidah Amin; Mohd Ambar Yarmo; Nik Idris Nik Yusoff

    2013-01-01

    The purpose of this study is to synthesis alkylpoly glucoside via condensation of decanol with dextrose in the presence of heterogenous catalyst. In this study, silicotungstic acid sol-gel (STSG) prepared using sol-gel was used as solid acid catalyst. The catalyst was characterized using BET surface area measurement, X-ray Diffraction (XRD) and X-ray Photoelectron Spectroscopy (XPS) surface analysis. The final product was easy to be separated from catalyst without the need of a further neutralization. Silicotungstic acid sol-gel has been found efficient to be solid catalyst for synthesis alkylpoly glucosides. Condensation reaction was carried out 8 hours at 110-120 degree Celsius under vacuum condition at 10 mmHg. The determination of decyl glucoside has been achieved by LC/ ESI-MS/ MS (ToF) giving a mass peak at m/z = 343.2 correspond to the m/z of [M+Na] + . Alkylpoly glucoside produced was analysed by FTIR, 1 H and 13 C NMR spectrometric technique. (author)

  6. Silica doped with lanthanum sol-gel thin films for corrosion protection

    Energy Technology Data Exchange (ETDEWEB)

    Abuin, M. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Serrano, A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); Llopis, J. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Garcia, M.A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); IMDEA Nanoscience, Fco. Tomas y Valiente 7, 28049 Madrid (Spain); Carmona, N., E-mail: n.carmona@fis.ucm.es [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain)

    2012-06-01

    We present here anticorrosive silica coatings doped with lanthanum ions for the protection of metallic surfaces as an alternative to chromate (VI)-based conversion coatings. The coatings were synthesized by the sol-gel method starting from silicon alkoxides and two different lanthanum precursors: La (III) acetate hydrate and La (III) isopropoxide. Artificial corrosion tests in acid and alkaline media showed their effectiveness for the corrosion protection of AA2024 aluminum alloy sheets for coating prepared with both precursors. The X-ray absorption Near Edge Structure and X-ray Absorption Fine Structure analysis of the coatings confirmed the key role of lanthanum in the structural properties of the coating determining its anticorrosive properties. - Highlights: Black-Right-Pointing-Pointer Silica sol-gel films doped with lanthanum ions were synthesized. Black-Right-Pointing-Pointer Films from lanthanum-acetate and La-alkoxide were prepared for comparison purposes. Black-Right-Pointing-Pointer La-acetate is an affordable chemical reactive preferred for the industry. Black-Right-Pointing-Pointer Films properties were explored by scanning electron microscopy and X-Ray absorption spectroscopy. Black-Right-Pointing-Pointer An alternative to anticorrosive pre-treatments for metallic surfaces is suggested.

  7. 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.

  8. 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.

  9. 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 ...

  10. Synthesis of phthalocyanine doped sol-gel materials

    Science.gov (United States)

    Dunn, Bruce

    1993-01-01

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

  11. The influence of the matrix structure on the oxidation of aniline in a silica sol-gel composite

    International Nuclear Information System (INIS)

    Widera, J.; Kijak, A.M.; Ca, D.V.; Pacey, G.E.; Taylor, R.T.; Perfect, H.; Cox, J.A.

    2005-01-01

    Mesoporous and microporous silica matrices were formed on indium tin oxide electrodes for liquid-phase voltammetry and as monoliths for solid-state voltammetry of aniline. The pore structure, which was verified by scanning probe microscopy and by surface area measurement, was directed by either control of pH during sol-gel processing or by inclusion of a templating agent. Whether aniline was included as a dopant in the sol-gel or as a component of the contacting liquid, the pore size influenced the coupling of the product of its electrochemical oxidation. With microporous silica, the dominant products were dimers and related short-chain products whereas with mesoporous silica, polymerization was suggested. As a step toward the formation of polyaniline (PANI) that is covalently anchored to the sol-gel, the electrochemistry of aniline was investigated using composites prepared from sols comprising tetraethyl orthosilicate (TEOS), 3-aminophenyl-[3-triethoxylsilyl)-propyl] urea (ormosil), and aniline in various ratios. Combinatorial chemistry identified that the optimum combination of silica precursors in terms of obtaining PANI was a 1:12 mole ratio of ormosil:TEOS

  12. Fabrication of optical chemical ammonia sensors using anodized alumina supports and sol-gel method.

    Science.gov (United States)

    Markovics, Akos; Kovács, Barna

    2013-05-15

    In this comparative study, the fabrication and the sensing properties of various reflectometric optical ammonia gas sensors are described. In the first set of experiments the role of the support material was investigated on four different sensor membranes. Two of them were prepared by the adsorption of bromocresol green indicator on anodized aluminum plates. The applied anodizing voltages were 12 V and 24 V, which resulted in different dynamic ranges and response times for gaseous ammonia. The sol-gel method was used for the preparation of the other batch of sensors. These layers were coated on anodized aluminum plates (24 V) and on standard microscope cover glasses. In spite of the identical sensing chemistry, slightly different response times were measured merely because of the aluminum surface porosity. Gas molecules can remain entrapped in the pores, which results in delayed recovery time. On the other hand, the porous oxide film provides excellent adhesion, making the anodized aluminum an attractive support for the sol-gel layer. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Hydrogen Production by Steam Reforming of Liquefied Natural Gas (LNG) Over Nickel-Phosphorus-Alumina Xerogel Catalyst Prepared by a Carbon-Templating Epoxide-Driven Sol-Gel Method.

    Science.gov (United States)

    Bang, Yongju; Park, Seungwon; Han, Seung Ju; Yoo, Jaekyeong; Choi, Jung Ho; Kang, Tae Hun; Lee, Jinwon; Song, In Kyu

    2016-05-01

    A nickel-phosphorus-alumina xerogel catalyst was prepared by a carbon-templating epoxide-driven sol-gel method (denoted as CNPA catalyst), and it was applied to the hydrogen production by steam reforming of liquefied natural gas (LNG). For comparison, a nickel-phosphorus-alumina xerogel catalyst was also prepared by a similar method in the absence of carbon template (denoted as NPA catalyst). The effect of carbon template addition on the physicochemical properties and catalytic activities of the catalysts in the steam reforming of LNG was investigated. Both CNPA and NPA catalysts showed excellent textural properties with well-developed mesoporous structure. However, CNPA catalyst retained a more reducible nickel aluminate phase than NPA catalyst. XRD analysis of the reduced CNPA and NPA catalysts revealed that nickel sintering on the CNPA catalyst was suppressed compared to that on the NPA catalyst. From H2-TPD and CH4-TPD measurements of the reduced CNPA and NPA catalysts, it was also revealed that CNPA catalyst with large amount of hydrogen uptake and strong hydrogen-binding sites showed larger amount of methane adsorption than NPA catalyst. In the hydrogen production by steam reforming of LNG, CNPA catalyst with large methane adsorption capacity showed a better catalytic activity than NPA catalyst.

  14. 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.

  15. 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)

  16. Reversible conversion between AgCl and Ag in AgCl-doped RSiO{sub 3/2}-TiO{sub 2} films prepared by a sol-gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Kawamura, Go, E-mail: gokawamura@ee.tut.ac.jp [Department of Electrical and Electronic Information Engineering, Toyohashi University of Technology, Toyohashi, Aichi 441-8580 (Japan); Tsurumi, Yuuki [Department of Environmental and Life Sciences, Toyohashi University of Technology, Toyohashi, Aichi 441-8580 (Japan); Muto, Hiroyuki [Department of Electrical and Electronic Information Engineering, Toyohashi University of Technology, Toyohashi, Aichi 441-8580 (Japan); Department of Environmental and Life Sciences, Toyohashi University of Technology, Toyohashi, Aichi 441-8580 (Japan); Sakai, Mototsugu; Inoue, Mitsuteru [Department of Electrical and Electronic Information Engineering, Toyohashi University of Technology, Toyohashi, Aichi 441-8580 (Japan); Matsuda, Atsunori [Department of Electrical and Electronic Information Engineering, Toyohashi University of Technology, Toyohashi, Aichi 441-8580 (Japan); Department of Environmental and Life Sciences, Toyohashi University of Technology, Toyohashi, Aichi 441-8580 (Japan)

    2011-10-17

    Highlights: {center_dot} The reversible redox behavior between AgCl and Ag in RSiO{sub 3/2}-TiO{sub 2} film is studied. {center_dot} TiO{sub 2} component induces Cl to remain in the film after conversion of AgCl to Ag. {center_dot} The survival of Cl is essential for reconversion of Ag to AgCl. {center_dot} The film shows potential to be applied as rewritable holographic material. - Abstract: The reversible redox behavior exhibited by AgCl-doped organosilsesquioxane-titania gel films is studied. Films prepared by the sol-gel method show reversible color changes with blue laser irradiation and subsequent heat treatment, which is based on the formation of Ag and AgCl nanoparticles, respectively. Two-beam interference exposure experiments reveal that the films have potential to be applied as rewritable holographic materials. A large titania content is essential for the conversion of Ag to AgCl because it induces the Cl to remain near the Ag nanoparticles during blue laser irradiation, allowing the Cl to react with neighboring Ag nanoparticles to reform AgCl upon subsequent heat treatment.

  17. Preparation and characterization of sol-gel derived 4%La{sub 2}O{sub 3}-Al{sub 2}O{sub 3} ceramic membrane on clay-based supports

    Energy Technology Data Exchange (ETDEWEB)

    Ersoy, B. [Afyon Kocatepe Univ., Mining Engineering Dept., AFYON (Turkey); Gunay, V. [TUBITAK-MRC, MCTRI, Gebze-KOCAELI (Turkey)

    2004-07-01

    In this work, {gamma}-Al{sub 2}O{sub 3} membrane layer (4 wt% La{sub 2}O{sub 3}+96% Al{sub 2}O{sub 3}) was coated on the clay based porous support by using the sol-gel coating. The coating solution was prepared by using boehmite (AlOOH), La-nitrate (La{sub 2}(NO{sub 3}){sub 3}.6H{sub 2}O), PVA, distilled water and HNO{sub 3}. The thickness of the {gamma}-Al{sub 2}O{sub 3} membrane layer was between 5-7 {mu}m. Two unprocessed clay samples which were supplied from Kutahya and Balikesir regions, were used to produce supports for the membranes. Porosities of the supports were varied from 25 to 40% depending on sintering temperatures. Mean pore diameter of the supports were between 0.01-1{mu}m. The mean pore diameter of 4wt%La{sub 2}O{sub 3} - Al{sub 2}O{sub 3} membrane layer was around 11 nm and total pore area was 113 m{sup 2} / g at 1000 C for 1 hour. (orig.)

  18. Magnetic property and Mössbauer analysis of SrSn{sub 1−x}Fe{sub x}O{sub 3} prepared by a sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Nomura, Kiyoshi, E-mail: dqf10204@nifty.com [Tokyo University of Science, Photocatalysis International Research Center (Japan); Suzuki, Shigeyo; Koike, Yuya [Meiji University, Department of Science and Engineering (Japan); Li, Hongling [The University of Tokyo, Graduate School of Engineering (Japan); Okazawa, Atsushi [The University of Tokyo, Graduate School of Arts and Sciences (Japan); Kojima, Norimichi [Toyota Physical and Chemical Research Institute (Japan)

    2016-12-15

    The dilute magnetic properties of SrSn{sub 1−x}Fe{sub x}O{sub 3} (x = 0.01 − 0.15) prepared by sol-gel and thermal decomposition methods were investigated by {sup 57}Fe Mössbauer spectrometry, magnetometry, and X-ray diffractometry. It was found that SrSnO{sub 3} doped with 2–8 % Fe show weak ferromagnetism although only paramagnetic doublets are observed in {sup 57}Fe Mössbauer spectra at room temperature (RT), whereas SrSnO{sub 3} doped with 10–15 % Fe show relatively strong ferromagnetism, and the sextets are additionally observed in the {sup 57}Fe Mössbauer spectra at RT. The weak ferromagnetism by doping 2–8 % Fe is considered to be caused by the induced magnetic defects, and the ferromagnetism by doping 10–15 % Fe are considered mainly due to the magnetic coupling between dilute Fe {sup 3+} partially substituted at Sn {sup 4+} sites in the orthorhombic structure of SrSnO{sub 3−δ} accompanying the oxygen deficiencies. It is further remarkable that poor crystalline 8 % Fe doped SrSnO{sub 3−δ} obtained by annealing at 600 {sup ∘}C shows relatively high saturation magnetization and low coercivity.

  19. Ferroelectric and piezoelectric properties of non-stoichiometric Sr1-xBi2+2x/3Ta2O9 ceramics prepared from sol-gel derived powders

    International Nuclear Information System (INIS)

    Jain, Rajni; Gupta, Vinay; Mansingh, Abhai; Sreenivas, K.

    2004-01-01

    Ceramic compositions of strontium bismuth tantalate (SBT) [Sr 1-x Bi 2+2x/3 Ta 2 O 9 ] with x = 0.0, 0.15, 0.30, 0.45 prepared from a sol-gel process have been studied. Stoichiometric and non-stoichiometric phases stable within the series have been investigated for their structural, dielectric, ferroelectric, and piezoelectric properties. Sintering at 1000 deg. C produces a single homogeneous phase up to x = 0.15. With x > 0.15 an undesirable BiTaO 4 phase is detected and a higher sintering temperature (1100 deg. C) prevents the formation of this phase. The ferroelectric to paraelectric phase transition temperature (T c ) increases linearly from 325 to 455 deg. C up to x = 0.30, and with x > 0.30, it tends to deviate from the linear behavior. At x = 0.45 a broad and a weak transition is observed and the peak value of dielectric constant (ε' max ) is significantly reduced. The piezoelectric coefficient (d 33 ), remnant polarization (2P r ), and coercive field (2E c ) values increase linearly up to x = 0.30. The degradation in the electrical properties for x > 0.30 are attributed to the presence of undesirable BiTaO 4 phase, which is difficult to identify by X-ray powder diffraction analysis (XRD) due to the close proximity of the peaks positions of BiTaO 4 and the SBT phase

  20. Effect of ion nitriding on the crystal structure of 3 mol% Y{sub 2}O{sub 3}-doped ZrO{sub 2} thin-films prepared by the sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Ortiz, A.L. [Departamento de Electronica e Ingenieria Electromecanica, Escuela de Ingenierias Industriales, Universidad de Extremadura, Badajoz 06071 (Spain)]. E-mail: alortiz@unex.es; Diaz-Parralejo, A. [Departamento de Electronica e Ingenieria Electromecanica, Escuela de Ingenierias Industriales, Universidad de Extremadura, Badajoz 06071 (Spain); Borrero-Lopez, O. [Departamento de Electronica e Ingenieria Electromecanica, Escuela de Ingenierias Industriales, Universidad de Extremadura, Badajoz 06071 (Spain); Guiberteau, F. [Departamento de Electronica e Ingenieria Electromecanica, Escuela de Ingenierias Industriales, Universidad de Extremadura, Badajoz 06071 (Spain)

    2006-06-30

    We investigated the effect of ion nitriding on the crystal structure of 3 mol% Y{sub 2}O{sub 3}-doped ZrO{sub 2} (3YSZ) thin-films prepared by the sol-gel method. For this purpose, we used X-ray diffractometry to determine the crystalline phases, the lattice parameters, the crystal sizes, and the lattice microstrains, and glow discharge-optical emission spectroscopy to obtain the depth profiles of the elemental chemical composition. We found that nitrogen atoms substitute oxygen atoms in the 3YSZ crystal, thus leading to the formation of unsaturated-substitutional solid solutions with reduced lattice parameters and Zr{sub 0.94}Y{sub 0.06}O{sub 1.72}N{sub 0.17} stoichiometric formula. We also found that ion nitriding does not affect the grain size, but does generate lattice microstrains due to the increase in point defects in the crystalline lattice.

  1. 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)

  2. 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)

  3. 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)

  4. 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)

  5. 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)

  6. 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)

  7. 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.

  8. 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

    We present a novel approach to the synthesis of inorganic sol-gel microspheres for encapsulating organic and bioactive molecules, and controlling their subsequent release kinetics. The bioactive species are incorporated, at ambient temperature, into the inorganic particles using an emulsion gelation process. Independent control of the release rate (by adapting the nanostructure of the internal pore network to the physico-chemical properties of the bioactive molecules) and particle size (by tailoring the emulsion chemistry) is demonstrated. Sol-gel chemistry has been shown to be a flexible technique for producing inorganic silica matrices with tailored microstructures, which can be used for the encapsulation and controlled release of organic and bioactive molecules. The present paper extends this concept by combining sol-gel chemistry with an emulsion approach for producing inorganic particles with controlled dimensions, and demonstrates how the particle size and microstructure can be independently controlled. Sol-Gel Chemistry and Encapsulation of Model Compounds. A stock solution of 4-(2-hydroxy-l-naphthylazo) benzene sulfonic acid (Orange II) was produced by dissolving Orange II in water (0.1 wt%), and adjusting the pH to the required value. Sol-gel solutions were subsequently prepared by mixing the aqueous solution with tetramethylorthosilicate (TMOS) and methanol (MeOH), to achieve H 2 O:TMOS (W] and MeOH:TMOS mole ratios (D) of four. The resulting solution was stirred and left to age at ambient temperature for one day. A transparent emulsion was prepared by mixing selected surfactants and organic solvents. The surfactants used included sorbitan monooleate, sorbitan monolaurate and bis-2-ethylhexylsulfo-succinate (AOT), while the organic phase was typically chosen from the group consisting of kerosene, hexane, heptane, octane, decane, dodecane and cyclohexane. The sol-gel solution was added to the emulsion, and the resulting mixture was stirred at 500 rpm for

  9. A concetration-dependent model for silver colloids in nanostructured sol-gel materials

    Science.gov (United States)

    Garcia-Macedo, Jorge A.; Franco, Alfredo; Renteria, Victor; Valverde-Aguilar, Guadalupe

    2005-08-01

    We report on the physical modelling of the photoconductive response of nanostructured sol-gel films in function of the silver nitrate concentration (ions and colloids). This model considers several factors as the silver nitrate concentration and the transport parameters obtained. The model is compared with others commonly used. 2d-hexagonal nanostructured sol-gel thin films were prepared by dip-coating method using a non-ionic diblock copolymer Brij58 (surfactant) to produce channels into the film. Silver colloids (metallic Ag0 nanoparticles ) were obtained by spontaneous reduction process of Ag+ ions to Ag0. These nanoparticles were deposited into the channels formed by the surfactant. The structure was identified by X-ray diffraction and TEM. An absorption band located at 430 nm was detected by optical absorption; it corresponds to the plasmon surface. Fit to this band with modified Gans theory is presented. Photoconductivity studies were performed on films with silver ions and films with silver colloids to characterized their mechanisms of charge transport in the darkness and under illumination at 420, 633 nm wavelengths. Transport parameters were calculated. The films with silver colloids exhibit a photovoltaic effect stronger than the films with silver ions. While, the last ones possesses a photoconductivity behaviour.

  10. Influences of the iron ion (Fe{sup 3+})-doping on structural and optical properties of nanocrystalline TiO{sub 2} thin films prepared by sol-gel spin coating

    Energy Technology Data Exchange (ETDEWEB)

    Ben Naceur, J. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Mechiakh, R., E-mail: raouf_mechiakh@yahoo.fr [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar, Batna (Algeria); Bousbih, F.; Chtourou, R. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia)

    2011-10-01

    Titanium dioxide (TiO{sub 2}) thin films doping of various iron ion (Fe{sup 3+}) concentrations were deposited on silicon (Si) (100) and quartz substrates by sol-gel Spin Coating technique followed by a thermal treatment at 600 deg. C. The structure, surface morphology and optical properties, as a function of the doping, have been studied by X-ray diffractometer (XRD), Raman, ultraviolet-visible (UV-vis) and Spectroscopic Ellipsometry (SE). XRD and Raman analyzes of our thin films show that the crystalline phase of TiO{sub 2} thin films comprised only the anatase TiO{sub 2}, but the crystallinity decreased when the Fe{sup 3+} content increased from 0% to 20%. During the Fe{sup 3+} addition to 20%, the phase of TiO{sub 2} thin film still maintained the amorphous state. The grain size calculated from XRD patterns varies from 29.3 to 22.6 nm. The complex index and the optical band gap (E{sub g}) of the films were determined by the spectroscopic ellipsometry analysis. We have found that the optical band gap decreased with an increasing Fe{sup 3+} content.

  11. 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.

  12. 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.

  13. 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.

  14. Ferroelectric self-assembled PbTiO{sub 3} perovskite nanostructures onto (100)SrTiO{sub 3} substrates from a novel microemulsion aided sol-gel preparation method

    Energy Technology Data Exchange (ETDEWEB)

    Calzada, M L [Institucion Ciencia de Materiales de Madrid (CSIC), Cantoblanco, E-28049 Madrid (Spain); Torres, M [Institucion Ciencia de Materiales de Madrid (CSIC), Cantoblanco, E-28049 Madrid (Spain); Fuentes-Cobas, L E [Centro de Investigacion en Materiales Avanzados, Chihuahua (Mexico); Mehta, A [Stanford Synchrotron Radiation Laboratory, Menlo Park, CA (United States); Ricote, J [Institucion Ciencia de Materiales de Madrid (CSIC), Cantoblanco, E-28049 Madrid (Spain); Pardo, L [Institucion Ciencia de Materiales de Madrid (CSIC), Cantoblanco, E-28049 Madrid (Spain)

    2007-09-19

    A novel preparation method, which involves the use of microemulsions, sol-gel chemistry and chemical solution deposition, has been developed in this work for the preparation of layers of PbTiO{sub 3} nanostructures supported on SrTiO{sub 3} substrates. A transparent solution was first prepared by mixing a PbTiO{sub 3} precursor sol and a microemulsion formed by water, cyclohexane and the surfactant Brij 30 (polyoxyethylene(4) lauryl ether). The solution was deposited onto the SrTiO{sub 3} substrate by spin-coating and dried under controlled conditions (temperature, time and relative humidity) to favor the rearrangement of the micelles in the deposited coat. After a rapid thermal treatment of crystallization at 650 deg. C, nanostructures with uniform sizes of {approx}40 nm diameter and showing periodicity in some zones of the substrate are obtained. The analysis of these nanostructures by grazing-incidence x-ray synchrotron radiation indicates that they have a perovskite structure with a <100> preferred orientation and that they are under strained conditions. Thermal treatments at higher temperatures produce the collapse of the ordered nanoparticles' network and the formation of larger isolated particles of PbTiO{sub 3} with a truncated-pyramid morphology. Piezoresponse force microscopy studies demonstrate that the spontaneous polarization of these PbTiO{sub 3} nanostructures can be switched and that they have piezoelectric activity. These results support the fabrication strategy here proposed as a promising approach for the preparation of nanoferroelectrics onto substrates of possible interest in future nanoelectronic devices.

  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.; 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

  16. 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

  17. 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.

  18. 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.)

  19. 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)

  20. Formation of ZnO-Cd(OH){sub 2} core-shell nanoparticles by sol-gel method: An approach to modify surface chemistry for stable and enhanced green emission

    Energy Technology Data Exchange (ETDEWEB)

    Mishra, Rupali, E-mail: rupalimishra@rediffmail.co [Department of Physics, University of Allahabad, Allahabad-211002 (India); Nanophosphor Application Centre, University of Allahabad, Allahabad-211002 (India); Yadav, Raghvendra S.; Pandey, Avinash C. [Department of Physics, University of Allahabad, Allahabad-211002 (India); Nanophosphor Application Centre, University of Allahabad, Allahabad-211002 (India); Sanjay, Sharda. S. [Department of Chemistry, Ewing Christian College, Allahabad (India); Dar, Chitra [Department of Physics, University of Allahabad, Allahabad-211002 (India)

    2010-03-15

    We report the formation of highly stable and luminescent ZnO-Cd(OH){sub 2} core-shell nanoparticles by simple introduction of cadmium salt in the initial precursor solution, used to synthesize ZnO nanoparticles by sol-gel route. The cadmium to zinc salt concentration ratio has been also varied to control the growth of ZnO nanoparticles at the smaller particle size. Formation of ZnO-Cd(OH){sub 2} core-shell nanostructure has been confirmed by X-ray diffraction (XRD), energy dispersive analysis of X-rays (EDAX) and X-ray photoelectron spectroscopy (XPS). UV-vis absorption spectroscopy exhibits blue-shift in absorption edge on increasing cadmium concentrations. The photoluminescence emission spectra showed the remarkably stable and enhanced visible (green) emission from suspended ZnO-Cd(OH){sub 2} nanoparticles in comparison to bare ZnO nanoparticles. It is postulated that Cd(OH){sub 2} layer at the surface of ZnO nanoparticles prevents the agglomeration of nanoparticles and efficiently assists the trapping of hole at the surface site, a first step necessary for visible emission. The Fourier transform infrared spectroscopy (FTIR) also supports our assumption about surface chemistry.

  1. 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.

  2. 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.

  3. 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

  4. 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)

  5. 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.

  6. 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

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

  8. 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

  9. 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

  10. Influence of Ba/Fe mole ratios on magnetic properties, crystallite size and shifting of X-ray diffraction peaks of nanocrystalline BaFe12O19 powder, prepared by sol gel auto combu

    Science.gov (United States)

    Suastiyanti, Dwita; Sudarmaji, Arif; Soegijono, Bambang

    2012-06-01

    Barium hexaferrite BaFe12O19 (BFO) is of great importance as permanent magnets, particularly for magnetic recording as well as in microwave devices. Nano-crystalline BFO powders were prepared by sol gel auto combustion method in citric acid - metal nitrates system. Hence the mole ratios of Ba/Fe were variated at 1:12; 1:11.5 and 1:11. Ratio of cation to fuel was fixed at 1:1. An appropriate amount of amonia solution was added dropwise to this solution with constant stirring until the PH reached 7 in all cases. Heating at 850oC for 10 hours for each sample to get final formation of BFO nanocrystalline. The data from XRD showing the lattice parameters a,c and the unit-cell volume V, confirm that BFO with ratio 1:12 has same crystall parameters with ratio 1:11. Ratio of Ba/Fe 1:12 and 1:11 have diffraction pattern similarly at almost each 2 θ for each samples. Ratio of Ba/Fe 1: 11.5 has the finest crystallite size 22 nm. Almost diffraction pattern peaks of Ba/Fe 1:11.5 move to the left from of Ba/Fe 1:12 then return to diffraction pattern of Ba/Fe 1:12 for Ba/Fe 1:11. SEM observations show the particle size less than 100 nm and the same shape for each sample. Ratio of Ba/Fe 1: 12 gives the highest intrinsic coercive Hc = 427.3 kA/m. The highest remanent magnetization is at ratio 1:11 with Mr = 0.170 T. BFO with mole ratio 1:11.5 has the finest grain 22 nm, good magnetic properties and the highest value of best FoM 89%.

  11. Ferroelectric and piezoelectric properties of non-stoichiometric Sr{sub 1-x}Bi{sub 2+2x/3}Ta{sub 2}O{sub 9} ceramics prepared from sol-gel derived powders

    Energy Technology Data Exchange (ETDEWEB)

    Jain, Rajni [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India); Gupta, Vinay [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India); Mansingh, Abhai [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India); Sreenivas, K. [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India)]. E-mail: kondepudysreenivas@rediffmail.com

    2004-09-15

    Ceramic compositions of strontium bismuth tantalate (SBT) [Sr{sub 1-x}Bi{sub 2+2x/3}Ta{sub 2}O{sub 9}] with x = 0.0, 0.15, 0.30, 0.45 prepared from a sol-gel process have been studied. Stoichiometric and non-stoichiometric phases stable within the series have been investigated for their structural, dielectric, ferroelectric, and piezoelectric properties. Sintering at 1000 deg. C produces a single homogeneous phase up to x = 0.15. With x > 0.15 an undesirable BiTaO{sub 4} phase is detected and a higher sintering temperature (1100 deg. C) prevents the formation of this phase. The ferroelectric to paraelectric phase transition temperature (T{sub c}) increases linearly from 325 to 455 deg. C up to x = 0.30, and with x > 0.30, it tends to deviate from the linear behavior. At x = 0.45 a broad and a weak transition is observed and the peak value of dielectric constant ({epsilon}'{sub max}) is significantly reduced. The piezoelectric coefficient (d{sub 33}), remnant polarization (2P{sub r}), and coercive field (2E{sub c}) values increase linearly up to x = 0.30. The degradation in the electrical properties for x > 0.30 are attributed to the presence of undesirable BiTaO{sub 4} phase, which is difficult to identify by X-ray powder diffraction analysis (XRD) due to the close proximity of the peaks positions of BiTaO{sub 4} and the SBT phase.

  12. The influence of charge transfers effects in monazite-type LaVO{sub 4} and perovskite-type LaVO{sub 3} prepared by sol-gel acrylamide polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Herrera-Pérez, G., E-mail: guillermo.herrera@cimav.edu.mx [CONACYT Research Fellow. Centro de Investigación en Materiales Avanzados (CIMAV), Miguel de Cervantes 120, Chihuahua 31136, Chihuahua (Mexico); Jiménez-Mier, J. [Instituto de Ciencias Nucleares, Universidad Nacional Autónoma de México, 04510 Mexico D. F (Mexico); Yang, W.-L. [The Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Reyes-Rojas, A.; Fuentes-Cobas, L.E. [Department of Physics of Materials Department. Centro de Investigación en Materiales Avanzados (CIMAV), Miguel de Cervantes 120, Chihuahua 31136, Chihuahua (Mexico)

    2016-08-15

    Highlights: • We elucidate the electronic structure through the vanadium L{sub 2,3} edge in LaVO{sub 4} by XAS. • The interpretation of XAS spectrum was performed by the multiplet calculation. • Our results suggest that LaVO{sub 4} can be considered in the charge transfer regime. - Abstract: Core-hole spectroscopy such as X-ray absorption spectroscopy (XAS) is useful to determine the electronic structure of strongly correlated and strongly hybridized compounds such as vanadates. Monazite-type LaVO{sub 4} and perovskite-type LaVO{sub 3} are good candidates to elucidate the electronic structure through the vanadium L{sub 2,3} edge. LaVO{sub 4} was prepared by sol-gel acrylamide polymerization and solid-state reaction. LaVO{sub 3} was obtained by reduction of LaVO{sub 4} using Zr as gatherer. Monoclinic crystal phase for LaVO{sub 4} and orthorhombic crystal phase for LaVO{sub 3} were confirmed by the Rietveld refinement of X-ray diffraction patterns. XAS comparison between Vanadium L{sub 2,3} edge confirms the presence of V{sup 5+} for the monazite and V{sup 3+} for the orthorhombic perovskite. Multiplet calculations including crystal field and charge transfer effects (CTM) were performed in order to elucidate the tetragonal (D{sub 4h} symmetry) parameters Dq, Ds and Dt, the charge transfer energy Δ, and d-d Coulomb repulsion energy U parameters. CTM confirms for LaVO{sub 3} the strong V 3d–O 2p hybridization with a significant contribution of covalent character due to the delocalization of 3d electrons. For LaVO{sub 4} this work suggest the reclassification of this band insulator as charge transfer insulator that shows a significant contribution of ionic character.

  13. 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.

  14. 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.

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

    Science.gov (United States)

    Han, Kuo

    conduction are still open issues to be addressed before full potential can be realized. Herein we report the percolative composites based on ferroelectric poly(vinylidene fluoride-co-chlorotrifluoroethylene) as the matrix and sol-gel derived SiO2 coated reduced graphene oxide nanosheets as the filler. By capitalizing on the SiO2 surface layers which have high electrical resistivity and breakdown strength, the composites exhibit superior dielectric performance as compared to the respective composites containing bare reduced graphene oxide nanosheet fillers. In addition to greatly reduced dielectric loss, little change in dielectric loss has been observed within medium frequency range (ie. 300 KHz-3 MHz) in the prepared composites even with a filler concentration beyond the percolation threshold, indicating significantly suppressed energy dissipation and the feasibility of using the conductor-insulator composites beyond the percolation threshold. Moreover, remarkable breakdown strength of 80 MV/m at the percolation threshold has been achieved in the composite, which far exceeds those of conventional percolative composites (lower than 0.1 MV/m in most cases) and thus enables the applications of the percolative composites at high electric fields. This work offers a new avenue to the percolative polymer composites exhibiting high permittivity, reduced loss and excellent breakdown strength for electrical energy storage applications. Flexible piezoelectric materials have attracted extensive attention because they can provide a practical way to scavenge energy from the environment and motions. It also provides the possibility to fabricate wearable and self-powered energy generator for powering small electronic devices. In the dissertation a new composite including BTO 3D structure and PDMS has been successfully fabricated using the sol-gel process. The structure, flexibility, dielectric and piezoelectric properties have been well studied. The new material shows a high g33 value of

  16. Sol-gel process for preparing YBa2Cu4O8 precursors from Y, Ba, and Cu acidic acetates/ammonia/ascorbic acid systems

    International Nuclear Information System (INIS)

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

    1995-08-01

    Sols were prepared by addition of ammonia to acidic acetate solutions of Y 3+ , Ba 2+ , and Cu 2+ . Ascorbic acid was added to a part of the sol. The resultant sols were gelled to a shard, a film, or microspheres by evaporation at 60 C or by extraction of water from drops of emulsion suspended in 2-ethylhexanol-1. Addition of ethanol to the sols facilitated the formation of gel films, fabricated by a dipping technique, on glass or silver substrates. At 100 C, gels that were formed in the presence of ascorbic acid were perfectly amorphous, in contrast to the crystalline acetate gels. Conversion of the amorphous ascorbate gels to final products was easier than for the acetate gels. The quality of coatings prepared from ascorbate gels was superior to that of acetate gel coatings

  17. 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)

  18. 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

  19. Reagentless D-sorbitol biosensor based on D-sorbitol dehydrogenase immobilized in a sol-gel carbon nanotubes-poly(methylene green) composite.

    Science.gov (United States)

    Wang, Zhijie; Etienne, Mathieu; Urbanova, Veronika; Kohring, Gert-Wieland; Walcarius, Alain

    2013-04-01

    A reagentless D-sorbitol biosensor based on NAD-dependent D-sorbitol dehydrogenase (DSDH) immobilized in a sol-gel carbon nanotubes-poly(methylene green) composite has been developed. It was prepared by durably immobilizing the NAD(+) cofactor with DSDH in a sol-gel thin film on the surface of carbon nanotubes functionalized with poly(methylene green). This device enables selective determination of D-sorbitol at 0.2 V with a sensitivity of 8.7 μA mmol(-1) L cm(-2) and a detection limit of 0.11 mmol L(-1). Moreover, this biosensor has excellent operational stability upon continuous use in hydrodynamic conditions.

  20. Structural and physicochemical properties of nickel manganite NiMn{sub 2}O{sub 4-δ}synthesized by sol-gel and ultra sound assisted methods

    Energy Technology Data Exchange (ETDEWEB)

    Alburquenque, D. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Metallurgy Department, USACH, Ave Ecuador 3469, Santiago 9170124 (Chile); Troncoso, L.; Denardin, J.C. [Physics Department, USACH, Ave. Ecuador 3493, Santiago 9170124 (Chile); Butera, A. [Atomic Center, CNEA, Ito. Balseiro, Bariloche Rio Negro 84000 (Argentina); Padmasree, K.D. [Cinvestav, U.Saltillo, Monterrey Km 13.5, Saltillo CP 25900 (Mexico); Ortiz, J.; Herrera, F. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Marco, J.F. [Institute of Physical Chemistry “Rocasolano”, CSIC, Serrano 119, Madrid 28006 (Spain); Gautier, J.L., E-mail: juan.gautier@usach.cl [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile)

    2016-07-05

    In this work we present the structural, magnetic and surface characterization of the ceramic nickel manganite oxide NiMn{sub 2}O{sub 4-δ} synthesized by two methods: sol-gel and ultrasound-assisted sol-gel using nitrate salts as precursors. We have characterized the non-stoichiometric samples NiMn{sub 2}O{sub 4-δ} using different physicochemical analyses. X-ray diffraction and Rietveld refinement of the X-ray data indicated that the samples crystallize in the Fd3m space group characteristic of cubic spinel-related oxides. The specific surface area of the oxides was 1.3 m{sup 2}/g (SG) and 16.3 m{sup 2}/g (UASG). SEM results showed particle agglomerates of 1.05 μm (SG) and 0.85 μm (UASG). Temperature dependence magnetization measurements were performed and a ferrimagnetic transition was identified at 103 K and 105 K depending on the preparation method (SG and UASG, respectively). The observed Curie constant was found to vary from 7.4 to 7.7 cm{sup 3} K mol{sup −1} and hysteretic magnetization vs. applied field curves at different temperatures were obtained. XPS studies of these oxides reveal the presence of Ni{sup 2+}, Mn{sup 2+}, Mn{sup 3+} and Mn{sup 4+} ions at the surface. A probable ionic distribution as a function of the synthesis method is proposed. - Highlights: • Nickel manganite was synthesized by sol gel synthesis and a novel ultrasound-assisted sol gel method. . • Bulk and surface cation distributions are proposed. • Physicochemical properties, including magnetic and surface area measurements, were studied for both types of samples.

  1. 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

  2. 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

  3. The use of silica gel prepared by sol-gel method and polyurethane foam as microbial carriers in the continuous degradation of phenol.

    Science.gov (United States)

    Brányik, T; Kuncová, G; Páca, J

    2000-08-01

    A mixed microbial culture was immobilized by entrapment into silica gel (SG) and entrapment/ adsorption on polyurethane foam (PU) and ceramic foam. The phenol degradation performance of the SG biocatalyst was studied in a packed-bed reactor (PBR), packed-bed reactor with ceramic foam (PBRC) and fluidized-bed reactor (FBR). In continuous experiments the maximum degradation rate of phenol (q(s)max) decreased in the order: PBRC (598 mg l(-1) h(-1)) > PBR (PU, 471 mg l(-1)h(-1)) > PBR(SG, 394 mg l(-1) h(-1)) > FBR (PU, 161 mg l(-1) h(-1)) > FBR (SG, 91 mg l(-1) h(-1)). The long-term use of the SG biocatalyst in continuous phenol degradation resulted in the formation of a 100-200 microm thick layer with a high cell density on the surface of the gel particles. The abrasion of the surface layer in the FBR contributed to the poor degradation performance of this reactor configuration. Coating the ceramic foam with a layer of cells immobilized in colloidal SiO2 enhanced the phenol degradation efficiency during the first 3 days of the PBRC operation, in comparison with untreated ceramic packing.

  4. Growth orientation and superconducting properties of YBa2Cu3O7-δ films prepared by the low-fluorine sol-gel process

    International Nuclear Information System (INIS)

    Lei Li; Zhao Gaoyang; Xu Hui; Zhao Juanjuan

    2010-01-01

    YBa 2 Cu 3 O 7-δ (YBCO) films were deposited on (100)-oriented LaAlO 3 (LAO) single crystal substrates by the dip-coating process using low-fluorine solution. Their microstructures were characterized with the aid of X-ray diffractometry, scanning electron microscopy and high-resolution transmission electron microscopy. Their superconducting properties were measured by the standard four-probe method. The experiment results show that the film obtained under high enough humidity conditions exhibits better c-axis texture and superconducting properties than the film under a relatively low humidity conditions. Based on the classical nucleation and chemical reaction thermodynamics theory, the underlying crystalline and growth mechanisms of YBCO films under certain humidity conditions are explained in combination with our experimental results. It is suggested that the unreacted intermediate phases such as BaF 2 and CuO aggregated in the YBCO grain boundary will cause lattice distortion in the YBCO matrix and further induce the formation of a-axis oriented YBCO grains as crystallization proceeds. Therefore, it is believed that the relative content of water vapor within the heat-treatment atmosphere plays quite an important role in the preparation of c-axis oriented YBCO film with good superconducting properties. (semiconductor materials)

  5. Synthesis of nanoparticles of magnetite by sol-gel and precipitation methods: study of chemical composition and structure

    International Nuclear Information System (INIS)

    Picasso, Gino; Vega, Jaime; Uzuriaga, Rosario; Ruiz, Gean Pieer

    2012-01-01

    In this work, nanoparticles based on magnetite have been prepared by sol-gel and precipitation methods. In the first case two variants have been applied: by growing of sol starting from nitrate precursor and ethylene glycol as solvent and to control the reduction process and force hydrolysis and steric control prepared from ferrum sulfate precursor and sodium citrate. In the second case the starting material was sulfate precursor, ammonium hydroxide as precipitaing agent and ethylene glycol as surfactant. The samples have been characterized by X-ray diffraction technique (XRD), adsorption-desorption of N 2 (BET equation model) and Moessbauer spectroscopy. XRD patterns of all samples showed typical peaks of magnetite which were detected in the following positions: 30,06 o , 35,42 o , 62,55 o . Average specific surface quantified by BET method was ranging from 40 to 50 m 2 /g with isotherm type IV corresponding to mesoporous surface. Moessbauer spectra of sample prepared from sol-gel (gel growing) carried out at home temperature detected the presence of 2 sextets consisting in 2 type of sites: first one due to octahedral positions (Fe 2+ , Fe 3+ ) and the second one due to tetrahedral positions (Fe 3+ ). Grain size of magnetite samples, evaluated by Scherrer equation and specific surface area, was ranging from 2 to 20 nm. (author).

  6. 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.

  7. Sol-gel formed spherical nanostructured titania based liquefied petroleum gas sensor

    Science.gov (United States)

    Sabhajeet, S. R.; Yadav, B. C.; Sonker, Rakesh K.

    2018-05-01

    The present work reports the preparation of Titania(TiO2) thin film by sol-gel technique and its Liquefied Petroleum Gas (LPG) sensing. TiO2 exists in numerous phases possessing different structural properties like amorphous, anatase or anatase/rutile mixed phases. The structural analysis confirmed the formation of TiO2 having an average crystallite size 21 nm. SEM showed the regular and porous surface morphology. The band gap of the material was found as 3.65 eV. This film was employed for LPG sensing and variations in resistance with exposure of LPG were observed. Sensor response (S) as a function of time was calculated and its maximum value was found as 2.8 for 4% vol. of LPG with a response and recovery times of 240 sec and 248 sec respectively.

  8. 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.

  9. 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 ...

  10. 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

  11. 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

  12. 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##

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. Effects of inorganic acids and divalent hydrated metal cations (Mg(2+), Ca(2+), Co(2+), Ni(2+)) on γ-AlOOH sol-gel process.

    Science.gov (United States)

    Zhang, Jian; Xia, Yuguo; Zhang, Li; Chen, Dairong; Jiao, Xiuling

    2015-11-07

    In-depth understanding of the sol-gel process plays an essential role in guiding the preparation of new materials. Herein, the effects of different inorganic acids (HCl, HNO3 and H2SO4) and divalent hydrated metal cations (Mg(2+), Ca(2+), Co(2+), Ni(2+)) on γ-AlOOH sol-gel process were studied based on experiments and density functional theory (DFT) calculations. In these experiments, the sol originating from the γ-AlOOH suspension was formed only with the addition of HCl and HNO3, but not with H2SO4. Furthermore, the DFT calculations showed that the strong adsorption of HSO4(-) on the surface of the γ-AlOOH particles, and the hydrogen in HSO4(-) pointing towards the solvent lead to an unstable configuration of electric double layer (EDL). In the experiment, the gelation time sequence of γ-AlOOH sol obtained by adding metal ions changed when the ionic strength was equal to or greater than 0.198 mol kg(-1). The DFT calculations demonstrated that the adsorption energy of hydrated metal ions on the γ-AlOOH surface can actually make a difference in the sol-gel process.

  18. 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

  19. 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

  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. 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.

  2. 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

  3. 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.

  4. 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.

  5. Fabrication of carbon microcapsules containing silicon nanoparticles-carbon nanotubes nanocomposite by sol-gel method for anode in lithium ion battery

    International Nuclear Information System (INIS)

    Bae, Joonwon

    2011-01-01

    Carbon microcapsules containing silicon nanoparticles (Si NPs)-carbon nanotubes (CNTs) nanocomposite (Si-CNT-C) have been fabricated by a surfactant mediated sol-gel method followed by a carbonization process. Silicon nanoparticles-carbon nanotubes (Si-CNT) nanohybrids were produced by a wet-type beadsmill method. To obtain Si-CNT nanocomposites with spherical morphologies, a silica precursor (tetraethylorthosilicate, TEOS) and polymer (PMMA) mixture was employed as a structure-directing medium. Thus the Si-CNT/Silica-Polymer microspheres were prepared by an acid catalyzed sol-gel method. Then a carbon precursor such as polypyrrole (PPy) was incorporated onto the surfaces of pre-existing Si-CNT/silica-polymer to generate Si-CNT/Silica-Polymer-PPy microspheres. Subsequent thermal treatment of the precursor followed by wet etching of silica produced Si-CNT-C microcapsules. The intermediate silica/polymer must disappear during the carbonization and etching process resulting in the formation of an internal free space. The carbon precursor polymer should transform to carbon shell to encapsulate remaining Si-CNT nanocomposites. Therefore, hollow carbon microcapsules containing Si-CNT nanocomposites could be obtained (Si-CNT-C). The successful fabrication was confirmed by scanning electron microscopy (SEM) and X-ray diffraction (XRD). These final materials were employed for anode performance improvement in lithium ion battery. The cyclic performances of these Si-CNT-C microcapsules were measured with a lithium battery half cell tests. - Graphical Abstract: Carbon microcapsules containing silicon nanoparticles (Si NPs)-carbon nanotubes (CNTs) nanocomposite (Si-CNT-C) have been fabricated by a surfactant mediated sol-gel method. Highlights: → Polymeric microcapsules containing Si-CNT transformed to carbon microcapsules. → Accommodate volume changes of Si NPs during Li ion charge/discharge. → Sizes of microcapsules were controlled by experimental parameters.

  6. 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

  7. 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.

  8. 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.)

  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. Fabrication and study of sol-gel ZnO films for use in Si-based heterojunction photovoltaic devices

    Directory of Open Access Journals (Sweden)

    Daniya Mukhamedshina

    2017-12-01

    Full Text Available This paper considers the use of zinc oxide thin films prepared via the sol-gel route as an n-type layer in heterojunction ZnO/Si solar cells. The ZnO films were prepared via a simple spin-coating technique using zinc acetate dihydrate as a zinc precursor, isopropanol as a solvent and monoethanolamine as a stabilizing agent. Optical, structural and morphological properties of ZnO were investigated for thin films grown from sol-gel solutions with different concentrations both on glass and silicon substrates. As such, a distribution of crystallite sizes and surface topology parameters corresponding to various zinc acetate dihydrate concentrations were obtained to elucidate optimal film deposition conditions. Correlation between thin film morphology and structural characteristics of ZnO thin films was made based on atomic-force microscopy studies. Finally, our results on fabrication, characterization and simulation of ZnO/Si heterojunctions for use as photovoltaic devices are presented. Although noticeable rectifying and photovoltaic properties were observed for Al/Si/ZnO/Ti/Au devices, there appears to exist a considerable room for device improvement with simulation studies suggesting that efficiencies of the order of 24% may be obtained for devices with optimal silicon wafer passivation, i.e. with lifetimes of the order of 1000 μs.

  11. Fast and efficient proteolysis by reusable pepsin-encapsulated magnetic sol-gel material for mass spectrometry-based proteomics applications.

    Science.gov (United States)

    Kayili, H Mehmet; Salih, Bekir

    2016-08-01

    Hydrophobic silicon-based material having magnetic properties was fairly synthesized by a classical sol-gel approach. Pepsin enzyme was encapsulated in the sol-gel material and the enzyme activity was evaluated in consequence of the digestion of some common proteins such as α- and β-casein, cytochrome c, myoglobin, and bovine serum albumin (BSA) both in a single protein batch and in the protein mixture. The optimum digestion time of the studied proteins using pepsin-encapsulated magnetic sol-gel material was found to be 20min. To produce the magnetic sol-gel material for convenient and easy proteomics applications, Fe3O4 was doped inside sol-gel material during the gelation step. It was observed that the activity of encapsulated pepsin was not affected by the amount of Fe3O4. Poly(ethylene glycol) was also inserted in sol-gel bulk to obtain suitable roughness and increase the hydrophilicity of the material surface to let protein molecules reach to the sol-gel material easily. The digestion of the protein mixture and non-fat bovine milk was performed with the pepsin-encapsulated magnetic sol-gel material and the digested solutions were analyzed using SDS-PAGE, MALDI-TOF-MS and LC-MS/MS for the protein identification. Reusability of the pepsin-encapsulated sol-gel material was examined and it was determined that they could be used at least 20 times. Finally, IgG digestions with a fast incubation time period were carried out using pepsin-encapsulated sol-gel material for generation of (Fab)2 product to evaluate the kinetic performance of the material. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. 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.

  13. Effects of phosphorus-doping on energy band-gap, structural, surface, and photocatalytic characteristics of emulsion-based sol-gel derived TiO{sub 2} nano-powder

    Energy Technology Data Exchange (ETDEWEB)

    Ganesh, Ibram, E-mail: ibramganesh@arci.res.in

    2017-08-31

    Highlights: • Reported a novel route to synthesize high specific surface area P-doped TiO{sub 2} nano-powder photocatalysts. • Established methylene blue dye-sensitization mechanism of TiO{sub 2} photocatalyst. • Established the effects of methylene blue adsorption on the surface, structural and photocatalytic activity of P-doped TiO{sub 2}. • Established true quantum efficiency determination method for TiO{sub 2} photocatalysis. - Abstract: Different amounts of phosphorus (P)-doped TiO{sub 2} (PDT) nano-powders (P = 0–10 wt.%) were synthesized by following a new emulsion-based sol-gel (EBSG) route and calcined at 400 °C–800 °C for 6 h. These calcined PDT powders were then thoroughly characterized by means of XRD, XPS, SEM, FT-IR, FT-Raman, DRS, BET surface area, zeta-potential, cyclic-voltammetry and photocatalytic evaluation using methylene blue (MB) as a model-pollutant and established the effects of phosphorous doping on structural, surface, band-gap energy, and photocatalytic characteristics of TiO{sub 2} nano-powder formed in EBSG route. The characterization results suggest that the EBSG derived TiO{sub 2} nano-powder after calcination at 400 °C for 6 h is in the form of anatase phase when it was doped with <8 wt.% P, and it is in the amorphous state when doped with >8 wt.% P. Furthermore, these EBSG derived PDT powders own high negative zeta-potentials, high specific surface areas (up to >250 m{sup 2}/g), and suitable band-gap energies (<3.34 eV). Surprisingly, these PDT powders exhibit very high MB adsorption (up to 50%) from its aqueous 0.01 mM, 0.02 mM and 0.03 mM solutions during 30 min stirring in the dark, whereas, the commercial Degussa P-25 TiO{sub 2} nano-powder shows no adsorption. Among various photocatalysts investigated in this study, the 1 wt.% P-doped TiO{sub 2} nano-powder formed in EBSG route exhibited the highest photocatalytic activity for MB degradation reaction.

  14. 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

  15. 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.

  16. A new sol-gel synthesis of 45S5 bioactive glass using an organic acid as catalyst.

    Science.gov (United States)

    Faure, J; Drevet, R; Lemelle, A; Ben Jaber, N; Tara, A; El Btaouri, H; Benhayoune, H

    2015-02-01

    In this paper a new sol-gel approach was explored for the synthesis of the 45S5 bioactive glass. We demonstrate that citric acid can be used instead of the usual nitric acid to catalyze the sol-gel reactions. The substitution of nitric acid by citric acid allows to reduce strongly the concentration of the acid solution necessary to catalyze the hydrolysis of silicon and phosphorus alkoxides. Two sol-gel powders with chemical compositions very close to that of the 45S5 were obtained by using either a 2M nitric acid solution or either a 5mM citric acid solution. These powders were characterized and compared to the commercial Bioglass®. The surface properties of the two bioglass powders were assessed by scanning electron microscopy (SEM) and by Brunauer-Emmett-Teller method (BET). The Fourier transformed infrared spectroscopy (FTIR) and the X-ray diffraction (XRD) revealed a partial crystallization associated to the formation of crystalline phases on the two sol-gel powders. The in vitro bioactivity was then studied at the key times during the first hours of immersion into acellular Simulated Body Fluid (SBF). After 4h immersion into SBF we clearly demonstrate that the bioactivity level of the two sol-gel powders is similar and much higher than that of the commercial Bioglass®. This bioactivity improvement is associated to the increase of the porosity and the specific surface area of the powders synthesized by the sol-gel process. Moreover, the nitric acid is efficiently substituted by the citric acid to catalyze the sol-gel reactions without alteration of the bioactivity of the 45S5 bioactive glass. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. 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

  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. 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...

  1. 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...

  2. 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...

  3. 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.

  4. Separation of oligopeptides, nucleobases, nucleosides and nucleotides using capillary electrophoresis/electrochromatography with sol-gel modified inner capillary wall.

    Science.gov (United States)

    Svobodová, Jana; Kofroňová, Olga; Benada, Oldřich; Král, Vladimír; Mikšík, Ivan

    2017-09-29

    The aim of this article is to study the modification of an inner capillary wall with sol-gel coating (pure silica sol-gel or silica sol-gel containing porphyrin-brucine conjugate) and determine its influence on the separation process using capillary electrophoresis/electrochromatography method. After modification of the inner capillary surface the separation of analytes was performed using two different phosphate buffers (pH 2.5 and 9.0) and finally the changes in electrophoretic mobilities of various samples were calculated. To confirm that the modification of the inner capillary surface was successful, the parts of the inner surfaces of capillaries were observed using scanning electron microscopy. The analytes used as testing samples were oligopeptides, nucleosides, nucleobases and finally nucleotides. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. 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.

  6. 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.

  7. 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.)

  8. 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.

  9. A Novel Microdialysis Glucose Sensor System Based on Co-immobilizing on AU Micro-Electrode by SOL-GEL Technique

    National Research Council Canada - National Science Library

    Yu, Ping

    2001-01-01

    .... The sensor is based on co_immobilizing glucose oxidase (COD) with the catalase by sol-gel technique on the surface of the silicon bases with two pattern of An microelectrodes. A graduated ("sandwich...

  10. Use of CdSe/ZnS luminescent quantum dots incorporated within sol-gel matrix for urea detection

    International Nuclear Information System (INIS)

    Duong, Hong Dinh; Rhee, Jong Il

    2008-01-01

    In this work, urea detection techniques based on the pH sensitivity of CdSe/ZnS QDs were developed using three types of sol-gel membranes: a QD-entrapped membrane, urease-immobilized membrane and double layer consisting of a QD-entrapped membrane and urease-immobilized membrane. The surface morphology of the sol-gel membranes deposited on the wells in a 24-well microtiter plate was investigated. The linear detection range of urea was in the range of 0-10 mM with the three types of sol-gel membranes. The urea detection technique based on the double layer consisting of the QD-entrapped membrane and urease-immobilized membrane resulted in the highest sensitivity to urea due to the Michaelis-Menten kinetic parameters. That is, the Michaelis-Menten constant (K m =2.0745 mM) of the free urease in the QD-entrapped membrane was about 4-fold higher than that (K m =0.549 mM) of the immobilized urease in the urease-immobilized membrane and about 12-fold higher than that (K m =0.1698 mM) of the immobilized urease in the double layer. The good stability of the three sol-gel membranes for urea sensing over 2 months showed that the use of sol-gel membranes immobilized with QDs or an enzyme is suitable for biomedical and environmental applications

  11. Use of CdSe/ZnS luminescent quantum dots incorporated within sol-gel matrix for urea detection.

    Science.gov (United States)

    Duong, Hong Dinh; Rhee, Jong Il

    2008-09-19

    In this work, urea detection techniques based on the pH sensitivity of CdSe/ZnS QDs were developed using three types of sol-gel membranes: a QD-entrapped membrane, urease-immobilized membrane and double layer consisting of a QD-entrapped membrane and urease-immobilized membrane. The surface morphology of the sol-gel membranes deposited on the wells in a 24-well microtiter plate was investigated. The linear detection range of urea was in the range of 0-10mM with the three types of sol-gel membranes. The urea detection technique based on the double layer consisting of the QD-entrapped membrane and urease-immobilized membrane resulted in the highest sensitivity to urea due to the Michaelis-Menten kinetic parameters. That is, the Michaelis-Menten constant (K(m)=2.0745mM) of the free urease in the QD-entrapped membrane was about 4-fold higher than that (K(m)=0.549mM) of the immobilized urease in the urease-immobilized membrane and about 12-fold higher than that (K(m)=0.1698mM) of the immobilized urease in the double layer. The good stability of the three sol-gel membranes for urea sensing over 2 months showed that the use of sol-gel membranes immobilized with QDs or an enzyme is suitable for biomedical and environmental applications.

  12. 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.

  13. 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.

  14. 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.

  15. 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)

  16. 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.

  17. Structural and electrical characteristics of ZrO2-TiO2 thin films by sol-gel method

    International Nuclear Information System (INIS)

    Hsu, Cheng-Hsing; Tseng, Ching-Fang; Lai, Chun-Hung; Tung, Hsin-Han; Lin, Shih-Yao

    2010-01-01

    In this paper, we investigated electrical properties and microstructures of ZrTiO 4 (ZrO 2 -TiO 2 ) thin films prepared by the sol-gel method on ITO substrates at different annealing temperatures. All films exhibited ZrTiO 4 (1 1 1) and (1 0 1) orientations perpendicular to the substrate surface, and the grain size increased with increase in the annealing temperature. A low leakage current density of 2.06 x 10 -6 A/cm 2 was obtained for the prepared films. Considering the primary memory switching behavior of ZrTiO 4 , ReRAM based on ZrTiO 4 shows promise for future nonvolatile memory applications.

  18. 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.

  19. Immobilization of cholesterol esterase and cholesterol oxidase onto sol-gel films for application to cholesterol biosensor

    International Nuclear Information System (INIS)

    Singh, Suman; Singhal, Rahul; Malhotra, B.D.

    2007-01-01

    Cholesterol oxidase (ChOx) and cholesterol esterase (ChEt) have been covalently immobilized onto tetraethylorthosilicate (TEOS) sol-gel films. The tetraethylorthosilicate sol-gel/ChEt/ChOx enzyme films thus prepared have been characterized using scanning electron microscopic (SEM), UV-vis spectroscopic, Fourier-transform-infrared (FTIR) spectroscopic and amperometric techniques, respectively. The results of photometric measurements carried out on tetraethylorthosilicate sol-gel/ChEt/ChOx reveal thermal stability up to 55 deg. C, response time as 180 s, linearity up to 780 mg dL -1 (12 mM), shelf life of 1 month, detection limit of 12 mg dL -1 and sensitivity as 5.4 x 10 -5 Abs. mg -1 dL -1

  20. Immobilization of cholesterol esterase and cholesterol oxidase onto sol-gel films for application to cholesterol biosensor

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Suman [Central Mechanical Engineering Research Institute, G. Avenue, Durgapur 713209, West Bengal (India); Singhal, Rahul [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Marg, New Delhi 110012 (India); Malhotra, B.D. [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Marg, New Delhi 110012 (India)]. E-mail: bansi.malhotra@gmail.com

    2007-01-23

    Cholesterol oxidase (ChOx) and cholesterol esterase (ChEt) have been covalently immobilized onto tetraethylorthosilicate (TEOS) sol-gel films. The tetraethylorthosilicate sol-gel/ChEt/ChOx enzyme films thus prepared have been characterized using scanning electron microscopic (SEM), UV-vis spectroscopic, Fourier-transform-infrared (FTIR) spectroscopic and amperometric techniques, respectively. The results of photometric measurements carried out on tetraethylorthosilicate sol-gel/ChEt/ChOx reveal thermal stability up to 55 deg. C, response time as 180 s, linearity up to 780 mg dL{sup -1} (12 mM), shelf life of 1 month, detection limit of 12 mg dL{sup -1} and sensitivity as 5.4 x 10{sup -5} Abs. mg{sup -1} dL{sup -1}.

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