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Sample records for sol-gel electrophoresis deposition

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

    Stoch, A.

    1993-01-01

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

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

    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

  3. Fabrication and optical properties of TiO sub 2 nanowire arrays made by sol-gel electrophoresis deposition into anodic alumina membranes

    Lin, Y; Yuan, X Y; Xie, T; Zhang, L D

    2003-01-01

    Ordered TiO sub 2 nanowire arrays have been successfully fabricated into the nanochannels of a porous anodic alumina membrane by sol-gel electrophoretic deposition. After annealing at 500 deg. C, the TiO sub 2 nanowire arrays and the individual nanowires were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and x-ray diffraction (XRD). SEM and TEM images show that these nanowires are dense and continuous with a uniform diameter throughout their entire length. XRD and SAED analysis together indicate that these TiO sub 2 nanowires crystallize in the anatase polycrystalline structure. The optical absorption band edge of TiO sub 2 nanowire arrays exhibits a blue shift with respect of that of the bulk TiO sub 2 owing to the quantum size effect.

  4. A sol-gel-modified poly(methyl methacrylate) electrophoresis microchip with a hydrophilic channel wall.

    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.

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

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

    1992-01-01

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

  6. Deposition of sol-gel sensor spots by nanoimprint lithography and hemi-wicking

    Mikkelsen, Morten Bo Lindholm; Marie, Rodolphe; Hansen, Jan H.

    2011-01-01

    We present a method for homogeneous deposition of sol-gel sensor materials, which enable fabrication of sensor spots for optical pH and oxygen measurements inside plastic containers. A periodic pattern of posts is imprinted into a polycarbonate substrate and, using the principle of hemi-wicking, ......We present a method for homogeneous deposition of sol-gel sensor materials, which enable fabrication of sensor spots for optical pH and oxygen measurements inside plastic containers. A periodic pattern of posts is imprinted into a polycarbonate substrate and, using the principle of hemi...

  7. Site selective generation of sol-gel deposits in layered bimetallic macroporous electrode architectures.

    Lalo, Hélène; Bon-Saint-Côme, Yémima; Plano, Bernard; Etienne, Mathieu; Walcarius, Alain; Kuhn, Alexander

    2012-02-07

    The elaboration of an original composite bimetallic macroporous electrode containing a site-selective sol-gel deposit is reported. Regular colloidal crystals, obtained by a modified Langmuir-Blodgett approach, are used as templates for the electrogeneration of the desired metals in the form of a well-defined layered bimetallic porous electrode. This porous matrix shows a spatially modulated electroactivity which is subsequently used as a strategy for targeted electrogeneration of a sol-gel deposit, exclusively in one predefined part of the porous electrode.

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

    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.

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

    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.

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

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

    2000-01-01

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

  11. Sol-gel synthesis of 45S5 bioglass – Prosthetic coating by electrophoretic deposition

    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.

  12. Optical and electrochromic properties of sol-gel deposited Ti- doped vanadium oxide films

    Oezer, N.; Sabuncu, S.

    1997-01-01

    Because of the yellowish color, vanadium oxide films in the as deposited state is not as favorable as transparent coatings for most elector chromic devices. an interesting possibility to alter the yellowish colours is the doping with other non-absorbing metal oxides. Ti doped vanadium oxide films with various amounts of titanium were synthesized and investigated as transparent counter electrodes for electrochromic transmissive device application. Electrochromic titanium doped vanadium pentoxide (V sub 2 O 5) coatings were prepared by the sol-gel dip coating technique. The coating solutions were synthesized from vanadium tri(isopropoxide) precursors. X-ray diffraction (XRD) studies showed that the sol-gel deposited doped films heat treated at temperatures below 350 degree centigrade, were amorphous, whereas hose heat treated at higher temperatures were slight y crystalline. The optical and electrochemical properties of the Ti doped vanadium oxide films has been investigated in 0.1 m LiClO sub 4 propylene carbonate solution color changes by dropping were noted for all investigated films exhibits good electrochemical cycling (CV) measurements also showed that Ti doped V sub 2 O sub 5 films exhibits good electrochemical cycling reversibility, 'in situ' optical measurement revealed that those films exhibits good electrochemical cycling the spectra range 300 < lambda < 800 nm and change color between yellow and light green. The change in visible transmittance was 25 % for 5% Ti doped film. (author)

  13. Development of vapor deposited silica sol-gel particles for use as a bioactive materials system.

    Snyder, Katherine L; Holmes, Hallie R; VanWagner, Michael J; Hartman, Natalie J; Rajachar, Rupak M

    2013-06-01

    Silica-based sol-gel and bioglass materials are used in a variety of biomedical applications including the surface modification of orthopedic implants and tissue engineering scaffolds. In this work, a simple system for vapor depositing silica sol-gel nano- and micro-particles onto substrates using nebulizer technology has been developed and characterized. Particle morphology, size distribution, and degradation can easily be controlled through key formulation and manufacturing parameters including water:alkoxide molar ratio, pH, deposition time, and substrate character. These particles can be used as a means to rapidly modify substrate surface properties, including surface hydrophobicity (contact angle changes >15°) and roughness (RMS roughness changes of up to 300 nm), creating unique surface topography. Ions (calcium and phosphate) were successfully incorporated into particles, and induced apatitie-like mineral formation upon exposure to simulated body fluid Preosteoblasts (MC3T3) cultured with these particles showed up to twice the adhesivity within 48 h when compared to controls, potentially indicating an increase in cell proliferation, with the effect likely due to both the modified substrate properties as well as the release of silica ions. This novel method has the potential to be used with implants and tissue engineering materials to influence cell behavior including attachment, proliferation, and differentiation via cell-material interactions to promote osteogenesis. Copyright © 2012 Wiley Periodicals, Inc.

  14. Fabrication and Crystal Structure of Sol-Gel Deposited BST Thin Films with Compositional Gradient

    Czekaj D.

    2017-06-01

    Full Text Available In the present research technology of compositionally graded barium strontium titanate Ba1-xSrxTiO3 thin films deposited on stainless steel substrates by sol-gel spin coating followed with thermal annealing at T = 650°C is reported. Results of thermal behavior of the sol-gel derived powders with compositions used for fabrication of graded structure (i.e. with Sr mole fraction x = 0.5, 0.4 and 0.3 are described. X-ray diffraction studies of the phase composition and crystal structure of such complex thin film configuration are given. It was found that gel powders exhibited a large total weight loss of about Δm ≈ 44-47%. Three stages of weight loss took place at temperature ranges: below T ≈ 300°C, at ΔT ≈ 300-500°C and between T = 600°C and T = 800°C. Phase analysis has shown that the dominating phase is Ba0.67Sr0.33TiO3 compound while the second phase is Ba0.7Sr0.3TiO3 or Ba0.5Sr0.5TiO3 for “up-graded” and “down-graded” structure, respectively.

  15. Deposition of tin oxide doped with fluorine produced by sol-gel method and deposited by spray-pyrolysis

    Maia, Paulo Herbert Franca; Lima, Francisco Marcone; Sena, Aline Cosmo de; Silva, Alvaro Neuton; Almeida, Ana Fabiola Leite de; Freire, Francisco Nivaldo Aguiar

    2014-01-01

    Solar energy is one of the most important sources of renewable energy today, but its production is based on silicon cells, expensive and difficult to produce, so the research seek new materials to replace them. This work aims to deposit tin oxide doped with fluorine on the glass substrate using the sol-gel method to provide a working solution and spray pyrolysis technique to perform the deposition. F-SnO2 (FTO) were synthesized by sol-gel method, employing NH_4F and SnCl_2 precursor in an ethanol solution. Before the formation of the gel phase, the entire solution was sprayed, with the aid of a pistol aerographic substrate under heated at 600 °C divided by 50 applications and cooled in the furnace. The substrates had resistances between 10 and 30 S.cm. The energy dispersive x-ray (EDS) revealed the presence of fluorine in the SnO_2 network. (author)

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

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

    2004-01-01

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

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

    Cuong M. Nguyen

    2015-02-01

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

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

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

    2015-01-01

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

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

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

    2016-04-01

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

  20. Zirconia sol-gel coatings deposited on 304 stainless steel for chemical protection in acid media

    Luna, F. Perdomo; Atik, M.; Avaca, Luis A.; Aegerter, M.A.

    1995-01-01

    Zr O 2 thin films were prepared by sol-gel method and using dip-coating technique for deposition on 304 austenitic stainless steel, from sonocatalyzed sols of zirconia alkoxide, isopropanol (Zr(O C 3 H 7 )4/C 3 H 7 OH = 0.5), glacial acetic acid and water (C H 3 CO OH/H 2 O = 0.5). The films were dried at 40 deg C/15 min and thermally treated in the air with a linear variation of 5 deg C/min and two isothermal holdings at 400 deg C during 1 h and afterwards at 800 deg C during several periods of time (up to 20 h). The film thickness ranges between 0.6 and 0.8 μm. Structure and morphology were studied by x-ray diffraction and scanning electron microscopy. The corrosion potential, the corrosion current density, the polarization resistance and the corrosion rate (mpy) in 1,0 N aqueous solution of H 2 SO 4 at room temperature were determined using potentiometric polarization curves with a scanning velocity of 1 mV/s. These films act as a blocking physical layer in the corrosion media and increase the substrate life time in a factor of 7

  1. Zirconia sol-gel coatings deposited on 304 stainless steel for chemical protection in acid media

    Luna, F Perdomo; Atik, M; Avaca, Luis A; Aegerter, M A [Sao Paulo Univ., Sao Carlos, SP (Brazil). Inst. de Fisica

    1996-12-31

    Zr O{sub 2} thin films were prepared by sol-gel method and using dip-coating technique for deposition on 304 austenitic stainless steel, from sonocatalyzed sols of zirconia alkoxide, isopropanol (Zr(O C{sub 3} H{sub 7})4/C{sub 3} H{sub 7} OH = 0.5), glacial acetic acid and water (C H{sub 3} CO OH/H{sub 2} O = 0.5). The films were dried at 40 deg C/15 min and thermally treated in the air with a linear variation of 5 deg C/min and two isothermal holdings at 400 deg C during 1 h and afterwards at 800 deg C during several periods of time (up to 20 h). The film thickness ranges between 0.6 and 0.8 {mu}m. Structure and morphology were studied by x-ray diffraction and scanning electron microscopy. The corrosion potential, the corrosion current density, the polarization resistance and the corrosion rate (mpy) in 1,0 N aqueous solution of H{sub 2} SO{sub 4} at room temperature were determined using potentiometric polarization curves with a scanning velocity of 1 mV/s. These films act as a blocking physical layer in the corrosion media and increase the substrate life time in a factor of 7 16 refs., 3 figs., 1 tab.

  2. Characterizations of multilayer ZnO thin films deposited by sol-gel spin coating technique

    M.I. Khan

    Full Text Available In this work, zinc oxide (ZnO multilayer thin films are deposited on glass substrate using sol-gel spin coating technique and the effect of these multilayer films on optical, electrical and structural properties are investigated. It is observed that these multilayer films have great impact on the properties of ZnO. X-ray Diffraction (XRD confirms that ZnO has hexagonal wurtzite structure. Scanning Electron Microscopy (SEM showed the crack-free films which have uniformly distributed grains structures. Both micro and nano particles of ZnO are present on thin films. Four point probe measured the electrical properties showed the decreasing trend between the average resistivity and the number of layers. The optical absorption spectra measured using UV–Vis. showed the average transmittance in the visible region of all films is 80% which is good for solar spectra. The performance of the multilayer as transparent conducting material is better than the single layer of ZnO. This work provides a low cost, environment friendly and well abandoned material for solar cells applications. Keywords: Multilayer films, Semiconductor, ZnO, XRD, SEM, Optoelectronic properties

  3. Tin dioxide sol-gel derived films doped with platinum and antimony deposited on porous silicon

    Savaniu, C.; Arnautu, A.; Cobianu, C.; Craciun, G.; Flueraru, C.; Zaharescu, M.; Parlog, C.; Paszti, F.; van den Berg, Albert

    1999-01-01

    SnO2 sol-gel derived thin films doped simultaneously with Pt and Sb are obtained and reported for the first time. The Sn sources were tin(IV) ethoxide or tin(II) ethylhexanoate, while hexachloroplatinic acid (H2PtCl6) and antimony chloride (SbCl3) were used as platinum and antimony sources,

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

    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

  5. Diffusion structural analysis study of titania films deposited by sol-gel technique on silica glass

    Balek, V.; Mitsuhashi, T.; Bountseva, I.M.; Haneda, H.; Málek, Z.; Šubrt, Jan

    2003-01-01

    Roč. 26, 1-3 (2003), s. 185-189 ISSN 0928-0707. [International Workshop on Glasses, Ceramics, Hybrids and Nanocomposites from Gels /11./. Abano Terme, 16.09.2001-21.09.2001] Institutional research plan: CEZ:AV0Z4032918 Keywords : titania film * diffusion structural analysis * sol-gel Subject RIV: CA - Inorganic Chemistry Impact factor: 1.546, year: 2003

  6. Functional coatings: the sol-gel approach

    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)

  7. Fast Processing of Sol-Gel TCO

    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

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

    Ozer, N.; Lampert, C.M.

    1995-08-01

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

  9. α Fe2O3 films grown by the spin-on sol-gel deposition method

    Avila G, A.; Carbajal F, G.; Tiburcio S, A.; Barrera C, E.; Andrade I, E.

    2003-01-01

    α-Fe 2 O 3 polycrystalline films with grains larger than 31 nm were grown by the spin-on sol-gel deposition method. The particular sol used was prepared starting from two distinct precursor reagents. Both precursors leaded to similar films. Order within the films was altered by adding tin to the samples. Transmittance measurements confirmed that the hematite phase is obtained by annealing the samples above 400 C and yielded an optical gap of about 2.2 eV, but additional transitions at 2.7 eV were also observed. From RBS measurements it was found that tin inclusion decreases iron content as expected, but also increases oxygen concentration within the films. This last observation was associated to the disorder rise when introducing tin atoms. (Author)

  10. Biocompatibility of bismuth silicate coatings deposited on 316L stainless steel by sol-gel process

    Jorge Hernando Bautista-Ruiz

    2017-01-01

    Full Text Available Películas delgadas de silicato de bismuto (BSO se han fabricado mediante el proceso sol-gel. El sol estable se sintetizó utilizando nitrato de bismuto (III pentahidrato y tetraetil-ortosilicato (TEOS. Las películas fueron depositadas a 1500 rpm mediante la técnica de centrifugado. Los recubrimientos se caracterizaron por microscopía de fuerza atómica (AFM, microscopía electrónica de barrido (SEM, difracción de rayos-X (DRX y se midió el espesor de las películas. El objetivo de este estudio fue evaluar la adhesión y la proliferación en células de osteoblastos, mediante el ensayo MMT, al incubarse sobre películas BSO en sustratos de 316L. Se concluyó que el crecimiento de los osteoblastos es homogéneo en la superficie de las películas, indicando que el medio ofrecido por los recubrimientos no presenta actividad citotóxica y favorece los niveles de crecimiento celular en comparación con los resultados obtenidos para los sustratos de acero inoxidable.

  11. Atomic layer deposition of metal oxide by non-aqueous sol-gel chemistry =

    Marichy, Catherine

    O trabalho apresentado neste manuscrito foi desenvolvido no ambito do programa doutoral intitulado “Deposicao de Camadas Atomicas (ALD) de oxido de metais por sol-gel nao-aquoso”. O objectivo deste trabalho foi a preparacao de hetero-estruturas funcionais por ALD e a sua caracterizacao. Foi desenvolvido um novo processo de deposicao de oxido de estanho a temperatura baixa-moderada, utilizando um metodo ALD nao-aquoso, o qual foi aplicado com sucesso ao revestimento controlado das paredes internas e externas de nanotubos de carbono. Uma vez que a preparacao de nanomateriais funcionais requer uma elevada exatidao do processo de deposicao, foi demonstrada a deposicao precisa de filmes que se adaptem a forma do substrato ou de filmes nano-estruturados constituidos por particulas em varios substratos. Alem disso, foram depositados com grande exatidao varios oxidos de metal em nanotubos de carbono e demonstrou-se a possibilidade de ajustar o revestimento feito por ALD atraves do controlo da funcionalizacao da superficie do substrato nano-estruturado de carbono. As hetero-estruturas obtidas foram posteriormente aplicadas como sensores de gases. O melhoramento verificado na sensibilidade foi atribuido a formacao de heterojuncoes p-n entre o filme de oxido de metais e o suporte. O trabalho desenvolvido tendo como objetivo o controlo do revestimento por ALD atraves da funcionalizacao da superficie do suporte e certamente de interesse para o design de hetero-estruturas funcionais baseadas em substratos de carbono. De facto, durante o ultimo periodo do programa de doutoramento, este conceito foi alargado a funcionalizacao e revestimento com oxidos de metal de fibras de carbono preparadas por “electrospinning”, de forma a melhorar a estabilidade e a atividade eletrocatalitica de catalisadores a base de Pt. Este trabalho foi realizado maioritariamente na Universidade de Aveiro mas tambem na Universidade Nacional de Seul e beneficiou de varias colaboracoes internacionais

  12. Sol-gel deposition and electrical properties of laser irradiated Cu doped TiO2 multilayer thin films

    M.I. Khan

    Full Text Available Multilayer thin films (3, 5 and 7 of 20% copper doped titanium dioxide (Cu:TiO2 have been deposited on glass substrates by sol-gel spin coating method. After deposition, films have been irradiated by a beam of continuous wave diode laser (532 nm for two minutes at the angle of 45°. Structural, surface morphology and electrical properties of films have been investigated by X-rays diffraction (XRD, scanning electron microscope (SEM and four point probe technique respectively. XRD shows the formation of titanium copper oxide. Surface morphology of thin films indicated that the average grain size is increased by increasing the number of layers. The average sheet resistivity of 3, 5 and 7 layers of thin films measured by four point probe technique is 2.2 × 104, 1.2 × 104 and 1.0 × 104 (Ohm-cm respectively. The present study will facilitate a cost effective and environmental friendly study for several properties of materials. Keywords: Cu:TiO2, Multilayer thin films, Diode laser

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

    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.

  14. Advancements in artificial heart valve disks using nano-sized thin films deposited by CVD and sol-gel techniques

    Kousar, Y.; Ali, N.; Neto, V.F.; Mei, S.; Gracio, J.

    2003-01-01

    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 minimise the formation of thrombosis. However, the 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, namely, strength, wear resistance and coefficient of friction. The strength of the material was assessed using Brinell indentation tests. Furthermore, wear resistance and the coefficient of friction values were obtained from the 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 free standing nanocrystalline diamond films (FSND) using the time-modulated chemical vapor deposition (TMCVD) process. Furthermore, the sol-gel technique was used to uniformly coat PyC-HVD with dense, nanocrystalline-titanium oxide (nc-TiO/sub 2/) coatings. The as-grown nc-TiO/sub 2/ coatings were characterized for microstructure using SEM and XRD analysis. (author)

  15. Electrochemically assisted deposition of sol-gel bio-composite with co-immobilized dehydrogenase and diaphorase

    Wang Zhijie [LCPME, UMR 7564, CNRS-Nancy University, 405, rue de Vandoeuvre, 54600 Villers-les-Nancy (France); Etienne, Mathieu, E-mail: mathieu.etienne@lcpme.cnrs-nancy.fr [LCPME, UMR 7564, CNRS-Nancy University, 405, rue de Vandoeuvre, 54600 Villers-les-Nancy (France); Kohring, Gert-Wieland [Mikrobiologie, Universitaet des Saarlandes, Campus, Geb. A1.5, D-66123 Saarbruecken (Germany); Bon-Saint-Come, Yemima; Kuhn, Alexander [Universite Bordeaux, ISM, ENSCPB, 16 avenue Pey Berland, 33607 Pessac (France); Walcarius, Alain [LCPME, UMR 7564, CNRS-Nancy University, 405, rue de Vandoeuvre, 54600 Villers-les-Nancy (France)

    2011-10-30

    We report here that the electrochemically assisted deposition (EAD) of silica thin films can be a good strategy to co-encapsulate D-sorbitol dehydrogenase (DSDH) and diaphorase in an active form. This is achieved via the electrolysis of a hydrolyzed sol containing the biomolecules to initiate the poly-condensation of silica precursors upon electrochemically induced pH increase at the electrode/solution interface. DSDH was found to be very sensitive to the silica gel environment and the addition of a positively-charged polyelectrolyte was necessary to ensure effective operational behavior of the biomolecules. The composition of the sol and the conditions for electrolysis have been optimized with respect to the intensity of the electrochemical response to D-sorbitol oxidation. The K{sub m} of DSDH in the electrodeposited film was in the range of 3 mM, slightly better than the value determined biochemically in solution (6.5 mM). The co-immobilization of DSDH and diaphorase in this way led on the one hand to the possible reduction of NAD{sup +} to NADH (simultaneously to D-sorbitol oxidation) and on the other hand to the safe re-oxidation of the co-factor using a mediator (ferrocenedimethanol) as electron relay. The bioelectrocatalytic response looks promising for electro-enzymatic applications. To support this idea, the EAD of sol-gel bio-composite has been extended to macroporous electrodes displaying a much bigger electroactive surface area.

  16. Deposition of GdVO4:Eu3+ nanoparticles on silica nanospheres by a simple sol gel method

    Liu, Guixia; Hong, Guangyan; Wang, Jinxian; Dong, Xiangting

    2006-07-01

    The deposition and coating of GdVO4:Eu3+ nanoparticles on spherical silica was carried out using a simple sol-gel method at low temperature. The GdVO4:Eu3+-coated silica composites obtained were characterized by differential thermal analysis (DTA), thermogravimetric (TG) analysis, x-ray diffraction (XRD), Fourier-transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), photoluminescence spectra, and kinetic decay. It is found that the ~5 nm GdVO4:Eu3+ nanoparticles coating the silica spheres are crystal in the as-prepared samples and the crystallinity increases with increasing annealing temperature. The composites obtained are spherical in shape with an average size of 100 nm. The GdVO4:Eu3+ nanoparticles are linked with silica cores by a chemical bond. The photoluminescence spectra of the obtained GdVO4:Eu3+-coated silica composites are similar to those of the bulk GdVO4:Eu3+ phosphors. The strongest peak is near 617 nm, which indicates that Eu3+ is located in the low symmetry site with non-inversion centre.

  17. Electrochemically deposited sol-gel-derived silicate films as a viable alternative in thin-film design.

    Deepa, P N; Kanungo, Mandakini; Claycomb, Greg; Sherwood, Peter M A; Collinson, Maryanne M

    2003-10-15

    Sol-gel-derived silicate films were electrochemically deposited on conducting surfaces from a sol consisting of tetramethoxysilane (TMOS). In this method, a sufficiently negative potential is applied to the electrode surface to reduce oxygen to hydroxyl ions, which serves as the catalyst for the hydrolysis and condensation of TMOS. The electrodeposition process was followed by the electrochemical quartz crystal microbalance and cyclic voltammetry. The electrodeposited films were characterized for their surface morphology, porosity, and film thickness using atomic force microscopy, electrochemical probe techniques, surface area and pore size analysis, and profilometry. The electrodeposited films were found to have a completely different surface structure and to be significantly rougher relative to spin-coated films. This is likely due in part to the separation of the gelation and evaporation stages of film formation. The electrodeposited films were found to be permeable to simple redox molecules, such as ruthenium(III) hexaammine and ferrocene methanol. Film thickness can be easily varied from 15 microm by varying the electrode potential from -600 mV to more than -1000 mV, respectively. The electrodeposition process was further applied for the electroencapsulation of redox molecules and organic dyes within the silicate network. Cyclic voltammograms for the gel-entrapped ferrocene methanol (FcCH2OH) and ruthenium(II) tris(bipyridine) (Ru(bpy)3(2+)) exhibited the characteristic redox behavior of the molecules. The electroencapsulation of organic dyes in their "native" form proved to be more difficult because these species typically contain reducible functionalities that change the structure of the dye.

  18. Polythiophene thin films electrochemically deposited on sol-gel based TiO2 for photovoltaic applications

    Valaski, R.; Yamamoto, N.A.D.; Canestraro, C.D.; Micaroni, L.; Mello, R.M.Q.; Quirino, W.G.; Legani, C.; Achete, C.A.; Roman, L.S.; Cremona, M.

    2010-01-01

    In this work, the influence of titanium dioxide (TiO 2 ) thin films on the efficiency of organic photovoltaic devices based on electrochemically synthesized polythiophene (PT) was investigated. TiO 2 films were produced by sol-gel methods with controlled thickness. The best TiO 2 annealing condition was determined through the investigation of the temperature influence on the electron charge mobility and resistivity in a range between 723 K and 923 K. The PT films were produced by chronoamperometric method in a 3-electrode cell under a controlled atmosphere. High quality PT films were produced onto 40 nm thick TiO 2 layer previously deposited onto fluorine doped tin oxide (FTO) substrate. The morphology of PT films grown on both substrates and its strong influence on the device performance and PT minimum thickness were also investigated. The maximum external quantum efficiency (IPCE) reached was 9% under monochromatic irradiation (λ = 610 nm; 1 W/m 2 ) that is three orders of magnitude higher than that presented by PT-homolayer devices with similar PT thickness. In addition, the open-circuit voltage (V oc ) was about 700 mV and the short-circuit current density (J sc ) was 0.03 A/m 2 (λ = 610 nm; 7 W/m 2 ). However, as for the PT-homolayer also the TiO 2 /PT based devices are characterized by antibatic response when illuminated through FTO. Finally, the Fill Factor (FF) of these devices is low (25%), indicating that the series resistance (R s ), which is strongly dependent of the PT thickness, is too large. This large R s value is compensated by TiO 2 /PT interface morphology and by FTO/TiO 2 and TiO 2 /PT interface phenomena producing preferential paths in which the internal electrical field is higher, improving the device efficiency.

  19. In-situ sol-gel synthesis and thin film deposition of Cu(In,Ga)(S,Se)2 solar cells

    Oliveira, L.; Lyubenova, T.; Marti, R.; Fraga, D.; Rey, A.; Carda, J.; Kozhukharov, V.

    2013-01-01

    Full text: Nowadays chalcogenide-based solar cells, like Cu(In,Ga)Se 2 , are competitive in the photovoltaic market, due to its improved performances like higher efficiency (20,3%), long-time stability and excellent durability. In addition, CIGS stand out with an exceptionally high absorption coefficient (more than; 105/cm for 1.5eV) and higher energy photons. These properties make it an excellent candidate as an absorber material for large scale production of photovoltaic modules for building-integrated applications. Traditional methods of manufacture involve vacuum processes including co-evaporation and sputtering that increase production costs. With the aim to lower the expenses by using non-vacuum solution processes we propose an ‘in-situ’ sol-gel synthesis route and direct thin film deposition in the same production step. As a result, we achieved better stoichiometric control, simplicity in the procedure and cost reduction. In this work we describe a procedure to obtain CIGS absorber layer by soft chemistry technique and further deposition onto different substrates. Preparation parameters like precursors, chemical composition, solvents, thermal treatment factors (temperature, time, and atmosphere) were detailed studied. Finally, the resulting materials were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) coupled with Energy dispersive X-ray analysis (EDAX), UV-VIS Spectroscopy among others.; key words: sol-gel synthesis, thin film deposition, photovoltaic modules, solar cells

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

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

    2008-08-15

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

  1. Feasibility study on the sol-gel deposition of nanostructured materials based on oxides and fluorides for coatings on solar collector glazing

    Schueler, A.; Chambrier, E. De

    2005-10-15

    This illustrated annual report reviews work done at the Federal Institute of Technology (EPFL) in Lausanne, Switzerland, on the architectural integration of thermal solar collectors into buildings. This is often limited by their black colour and the visibility of the tubes and corrugations of the absorber sheets. Although a certain freedom in the choice of colour would be desirable, the coloured appearance should not cause excessive performance degradation. Multi-layered thin film interference filters on the collector glazing can produce a coloured reflection while transmitting the non-reflected radiation entirely to the absorber. The paper describes suitable optical interference filters which have been designed and optimised by numerical simulation and that will be manufactured by the sol-gel dip-coating process. Light scattering has to be avoided, which implies a need for particle sizes much smaller than the wavelengths of the incoming light. The paper proposes that corresponding thin films should therefore consist of nano-structured materials. The sol-gel deposition of all proposed materials has been demonstrated successfully. The paper presents the results of the work using various materials including titanium-silicon mixed oxides, gold-silicon dioxide, porous silicon dioxide, magnesium fluoride and quaternary films.

  2. Cu-Doped ZnO Thin Films Deposited by a Sol-Gel Process Using Two Copper Precursors: Gas-Sensing Performance in a Propane Atmosphere

    Heberto Gómez-Pozos

    2016-01-01

    Full Text Available A study on the propane gas-sensing properties of Cu-doped ZnO thin films is presented in this work. The films were deposited on glass substrates by sol-gel and dip coating methods, using zinc acetate as a zinc precursor, copper acetate and copper chloride as precursors for doping. For higher sensitivity values, two film thickness values are controlled by the six and eight dippings, whereas for doping, three dippings were used, irrespective of the Cu precursor. The film structure was analyzed by X-ray diffractometry, and the analysis of the surface morphology and film composition was made through scanning electron microscopy (SEM and secondary ion mass spectroscopy (SIMS, respectively. The sensing properties of Cu-doped ZnO thin films were then characterized in a propane atmosphere, C3H8, at different concentration levels and different operation temperatures of 100, 200 and 300 °C. Cu-doped ZnO films doped with copper chloride presented the highest sensitivity of approximately 6 × 104, confirming a strong dependence on the dopant precursor type. The results obtained in this work show that the use of Cu as a dopant in ZnO films processed by sol-gel produces excellent catalysts for sensing C3H8 gas.

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

    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.

  4. Thoria sol-gel processes

    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)

  5. Sol-Gel Derived, Nanostructured Oxide Lubricant Coatings

    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...

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

    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.

  7. {alpha} Fe{sub 2}O{sub 3} films grown by the spin-on sol-gel deposition method

    Avila G, A.; Carbajal F, G. [Seccion de Electronica del Estado Solido, Departamento de Ingenieria Electrica, CINVESTAV del l.P.N., Av. I.P.N. No. 2508, Apartado Postal 14-740, Mexico 07360, D.F (Mexico); Tiburcio S, A. [Division Posg, lnstituto Tecnologico de Toluca-SEP, P.O. Box 890, 50000 Toluca, Edo. Mex. (Mexico); Barrera C, E. [Departamento de IPH, Area de Ingenieria en Recursos Energeticos, Universidad Autonoma Metropolitana-lztapalapa, Apartado Postal 55-5340, Mexico, D.F. (Mexico); Andrade I, E. [Instituto de Fsica, Universidad Nacional Autononca de Mexico, Apartado Postal 20-364, Mexico 01000, D. F (Mexico)

    2003-07-01

    {alpha}-Fe{sub 2}O{sub 3} polycrystalline films with grains larger than 31 nm were grown by the spin-on sol-gel deposition method. The particular sol used was prepared starting from two distinct precursor reagents. Both precursors leaded to similar films. Order within the films was altered by adding tin to the samples. Transmittance measurements confirmed that the hematite phase is obtained by annealing the samples above 400 C and yielded an optical gap of about 2.2 eV, but additional transitions at 2.7 eV were also observed. From RBS measurements it was found that tin inclusion decreases iron content as expected, but also increases oxygen concentration within the films. This last observation was associated to the disorder rise when introducing tin atoms. (Author)

  8. Nanocrystal/sol-gel nanocomposites

    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.

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

    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.

  10. Effect of both deposition temperature and indium doping on the properties of sol-gel dip-coated SnO2 films.

    Caglar, Mujdat; Atar, Kadir Cemil

    2012-10-01

    Using indium chloride as an In source, In-doped SnO(2) films were fabricated by sol-gel method through dip-coating on borofloat glass substrates. The undoped SnO(2) films were deposited in air between 400 and 600 °C to get optimum deposition temperature in terms of crystal quality and hence In-doped SnO(2) films were deposited in air at 600 °C. The effect of both deposition temperature and In content on structural, morphological, optical and electrical properties was investigated. The crystalline structure and orientation of the films were investigated by X-ray diffraction (XRD) and surface morphology was studied by a field emission scanning electron microscope (FESEM). The compositional analysis of the films was confirmed by energy dispersive X-ray spectrometer (EDS). The absorption band edge of the SnO(2) films shifted from 3.88 to 3.66 eV with In content. The van der Pauw method was used to measure the sheet resistance of the films. The sheet resistance was affected significantly by deposition temperature and In content. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Development of Cotton Fabrics with Durable UV Protective and Self-cleaning Property by Deposition of Low TiO2 Levels through Sol-gel Process.

    Mishra, Anu; Butola, Bhupendra Singh

    2018-01-19

    In this article, the deposition of TiO 2 on cotton fabric using sol-gel technique has been described. Various process routes (pad-dry-cure, pad-dry-hydrothermal and pad-dry-solvothermal) were examined to impart a stable coating of TiO 2 on fabric. The role of precursor concentration, process temperature and time of treatment were studied to aim at a wash durable, UV protective and self-cleaning property in the treated fabric. EDX and ICP-MS techniques were used to examine the add-on percentage of TiO 2 on cotton fabrics treated via different routes. It has been found that the TiO 2 remains largely amorphous and nondurable if it is given a short thermal treatment. To convert the deposited TiO 2 to its anatase crystal form, a prolonged hydrothermal treatment for at least 3 h needs to be given. TiO 2 deposition levels of less than 0.1% were found to be effective in imparting reasonable degree of UV protection and self-cleaning property to the cotton fabric. The self-cleaning ability of the treated fabric against coffee stain was also studied and was found to be related to the process route and the deposition levels of TiO 2 . © 2018 The American Society of Photobiology.

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

    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

  13. Effect of thickness on structural, electrical, optical and magnetic properties of Co and Al doped ZnO films deposited by sol-gel route

    Sharma, Mamta [Department of Electronic Science, University of Delhi South Campus, New Delhi 110021 (India); Mehra, R.M. [Department of Electronic Science, University of Delhi South Campus, New Delhi 110021 (India)], E-mail: rammehra2003@yahoo.com

    2008-12-30

    This paper reports deposition and characterization of Zn{sub 0.94}Co{sub 0.05}Al{sub 0.01}O films of thickness ranging from 70 nm to 400 nm. These films were deposited on a glass (Corning, 7059) substrate using sol-gel route. The films have been characterized to study their structural, electrical, optical and magnetic properties. X-ray diffraction (XRD) and atomic force microscopy (AFM) were used to study the crystallinity and growth mode of the films. The films deposited up to a thickness of 200 nm showed improvement in crystallinity and preferential c-axis orientation. A transition in the growth mode from vertical (c-axis) to lateral (a and b-axis) was observed with further increase in the thickness of the film. The average transmittance of the films for thickness less than 200 nm was above 80% in the visible region which decreased at higher thickness of the film. The resistivity of the film was found to decrease with increase in thickness up to 200 nm. Ferromagnetism, at room temperature, was confirmed for 200 nm and 400 nm thick films.

  14. Effect of thickness on structural, electrical, optical and magnetic properties of Co and Al doped ZnO films deposited by sol-gel route

    Sharma, Mamta; Mehra, R.M.

    2008-01-01

    This paper reports deposition and characterization of Zn 0.94 Co 0.05 Al 0.01 O films of thickness ranging from 70 nm to 400 nm. These films were deposited on a glass (Corning, 7059) substrate using sol-gel route. The films have been characterized to study their structural, electrical, optical and magnetic properties. X-ray diffraction (XRD) and atomic force microscopy (AFM) were used to study the crystallinity and growth mode of the films. The films deposited up to a thickness of 200 nm showed improvement in crystallinity and preferential c-axis orientation. A transition in the growth mode from vertical (c-axis) to lateral (a and b-axis) was observed with further increase in the thickness of the film. The average transmittance of the films for thickness less than 200 nm was above 80% in the visible region which decreased at higher thickness of the film. The resistivity of the film was found to decrease with increase in thickness up to 200 nm. Ferromagnetism, at room temperature, was confirmed for 200 nm and 400 nm thick films.

  15. Effect of Sn-doped on microstructural and optical properties of ZnO thin films deposited by sol-gel method

    Tsay, C.-Y.; Cheng, H.-C.; Tung, Y.-T.; Tuan, W.-H.; Lin, C.-K.

    2008-01-01

    In this study, transparent thin films of Sn-doped ZnO (ZnO:Sn) were deposited onto alkali-free glass substrates by a sol-gel method; the effect of Sn doping on crystallinity, microstructural and optical properties was investigated. The atomic percentages of dopant in ZnO-based sols were Sn/Zn = 0, 1, 2, 3, and 5 at.%. The as-deposited films were pre-heated at 300 deg. C for 10 min and then annealed in air at 500 deg. C for 1 h. The results show that Sn-doped ZnO thin films demonstrate obviously improved surface roughness, enhanced transmittance in the 400-600 nm wavelength range and reduced average crystallite size. Among all of the annealed ZnO-based films in this study, films doped with 2 at.% Sn concentration exhibited the best properties, namely an average transmittance of 90%, an RMS roughness value of 1.92 nm and a resistivity of 9.3 x 10 2 Ω-cm

  16. The Effect of Cerium Ions on the Structure, Porosity and Electrochemical Properties of Si/Zr-Based Hybrid Sol-Gel Coatings Deposited on Aluminum

    Peter Rodič

    2018-04-01

    Full Text Available This study was focused on the synthesis and characterization of Si/Zr-based hybrid sol-gel coatings with and without the addition of cerium(III ions. The coatings were deposited on aluminum aiming to act as an effective and ecologically harmless alternative to toxic chromate coatings. The chemical composition, structure, thermal properties and porosity of the non-doped and Ce-doped coatings containing various Zr contents were examined by Raman spectroscopy and photothermal beam deflection spectroscopy. The corrosion properties of the coated aluminum substrates were studied using AC and DC electrochemical methods in 0.1 M NaCl electrolyte solution. Barrier and protecting properties of the coatings were monitored upon long-term immersion in chloride solution using electrochemical impedance spectroscopy. The effect of cerium ions was two-fold: on the formation of a more condensed Si−O−Zr network structure and on the formation of Ce-based deposits, which diminish the rate of cathodic reaction at the coating/metal interface. These effects acted synergistically and resulted in the creation of the coatings with effective barrier and active corrosion protection.

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

    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.

  18. Sol-gel growth of vanadium dioxide

    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

  19. Sol-gel derived sorbents

    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.

  20. Determinação de diagramas de bandas de energia e da borda de absorção em SnO2, depositado via sol-gel, sobre quartzo Determination of the band energy diagram and absorption fundamental edge in SnO2, deposited via sol-gel, on quartz

    E. A. Floriano

    2009-03-01

    Full Text Available Propriedades ópticas e estruturais de filmes finos de SnO2, depositados sobre substratos de quartzo, são apresentadas. Os filmes são preparados pela técnica de molhamento via sol-gel. Uma avaliação das propriedades eletrônicas do cristal (bulk e das superfícies (110 e (101 do material é também efetuada, através de cálculos baseados em um método mecânico-quântico que utiliza a Teoria do Funcional da Densidade (DFT em conjunto com o funcional hibrido B3LYP. A borda fundamental de absorção, obtida experimentalmente, é então comparada com os diagramas de bandas de energia do bulk e superfícies (110 e (101, calculadas.Optical and structural properties of SnO2 thin films, deposited on quartz substrates, are presented. Films are prepared by the sol-gel-dip-coating technique. An evaluation of the electronic properties of bulk and surfaces (110 and (101 of the material is also carried out, through calculation based on a quantum-mechanical method using the Density Functional Theory (DFT in conjunction with the hybrid functional B3LYP. The absorption fundamental edge, experimentally obtained, is compared to the calculated band energy diagram of bulk and surfaces (110 and (101.

  1. Metal-silica sol-gel materials

    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.

  2. Sol-gel coatings on carbon/carbon composites

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

    1986-01-01

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

  3. Visible emission from Er-doped SnO2 thin films deposited by sol-gel Emissão no visível de filmes finos, depositados via sol-gel, de SnO2 dopados com Er

    L. P. Ravaro

    2007-06-01

    Full Text Available Emission from Er-doped SnO2 thin film deposited via sol-gel by the dip coating technique is obtained in the range 500-700 nm with peak at 530 nm (green. Electron-hole generation in the tin dioxide matrix is used to promote the rare-earth ion excitation. Evaluation of crystallite dimensions through X-ray diffraction results leads to nanoscopic size, what could play a relevant role in the emission spectra. The electron-hole mechanism is also responsible for the excitation of the transition in the 1540 nm range in powders obtained from the same precursor solution of films. The thin film matrix presents a very useful shape for technological application, since it allows integration in optical devices and the application of electric fields to operate electroluminescent devices.Foi obtida emissão de filmes finos de SnO2 dopados com Er no intervalo 500-700 nm, com pico em 530 nm (verde. Esses filmes foram depositados pela técnica de molhamento via sol-gel. A geração de pares elétron-buraco na matriz de SnO2 é usada para promover a excitação do íon terra-rara. A avaliação do tamanho dos cristalitos por meio de resultados de difração de raios X indica dimensões nanoscópicas, o que pode ser relevante para a interpretação do espectro de emissão. O mecanismo de excitação elétron-buraco é também responsável pela excitação da transição no intervalo que inclui 1540 nm em pós obtidos da mesma solução precursora dos filmes. Filmes finos constituem um formato muito útil para aplicações tecnológicas, desde que permite integração em dispositivos ópticos e a aplicação de campos elétricos para operar dispositivos eletroluminescentes.

  4. Influence of Ni doping on phase transformation and optical properties of TiO2 films deposited on quartz substrates by sol-gel process

    Tian Jianjun; Deng Hongmei; Sun Lin; Kong Hui; Yang Pingxiong; Chu Junhao

    2012-01-01

    The Ni-doped TiO 2 films were synthesized on quartz substrates by the sol-gel method. Results from X-ray diffraction and Raman spectra indicate that Ni doping catalyzes the anatase-to-rutile transformation. When Ni content is up to 10 mol%, the transformation has been finished. The dielectric functions of Ni-doped TiO 2 films were extracted by fitting transmittance spectra according to the Adachi's dielectric function model. The optical band gap decreases from 3.64 eV to 3.51 eV with increasing Ni content. The results suggest that the acceleration of phase change and variation of optical properties may be related to defects due to Ni doping.

  5. Characterisation of a new alkoxide sol-gel hydroxyapatite

    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

  6. Sol-gel technology for biomedical engineering

    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)

  7. Sol-gel bonding of silicon wafers

    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

  8. Applications of sol gel ceramic coatings

    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.)

  9. Sol-gel antireflective coating on plastics

    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.

  10. Effects of UV assistance on the properties of al-doped ZnO thin films deposited by sol-gel method

    Tseng, Yung-Kuan; Pai, Feng-Ming; Chen, Yan-Cheng; Wu, Chao-Hsien

    2013-11-01

    We report here the preparation of aluminum doped zinc oxide transparent conductive thin films by a UV-assisted sol-gel method. It was found that UV irradiation creates ozone, which promotes the conductivity and transparency of the films. Boro-silicate glasses are used as substrates; an PGME is used as a solvent; after spin-coating, the films are dried and radiated with UV and then heated to 400°C for decarburization and 500°C for annealing under air. The surface morphologies of the prepared films are observed by FE-SEM and AFM. It was found that the films irradiated with UV-C are smoother and denser. An XRD analysis shows that the films have a typical wurtzite crystalline structure with a c-axis orientation normal to the surface. The electric resistance values measured with a four-point probe show that the films irradiated with UV have better conductivity (at approximately 3.4 × 10-3Ω-cm) than the films that did not undergo UV irradiation. An analysis by visible light spectrometry indicates that the AZO films irradiated with UV are more transparent than the films without UV-irradiation.

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

    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.

  12. Dip coating of sol-gels

    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.

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

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

    2010-08-01

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

  14. Influence of Co doping on structural, optical and magnetic properties of BiFeO3 films deposited on quartz substrates by sol-gel method

    Peng, Lin; Deng, Hongmei; Tian, Jianjun; Ren, Qing; Peng, Cheng; Huang, Zhipeng; Yang, Pingxiong; Chu, Junhao

    2013-03-01

    Multiferroic BiFe1-xCoxO3 (x = 0, 0.03, 0.05, 0.1) thin films have been prepared on quartz substrates using a sol-gel technique. X-ray diffraction data confirms that Co atoms have been successfully incorporated into the host lattice. The scanning electron microscopy (SEM) exhibits that the surface morphologies of BiFe0.97Co0.03O3 and BiFe0.95Co0.05O3 thin films become more compact and uniform. With increasing Co dopant, the position of A1-1 and E-4 modes shift towards the lower wavenumber indicates that Co doping induces structural distortion of BiFeO3. With increasing Co composition, the fundamental absorption edges of BiFe1-xCoxO3 films show red shift. Furthermore, transmittance spectra demonstrates that the optical band gap of BiFe1-xCoxO3 films decreases from 2.66 eV to 2.53 eV with the increase of Co from x = 0 to 0.1. At the wavelength of 720 nm, the refractive index decreases and the extinction coefficient increases with increasing the amount of Co. Optical properties reveal that Co doping in BiFeO3 provides preliminary research for optoelectronic devices and infrared detectors. Compared with BiFeO3 prepared under similar conditions, the remanent magnetization Mr of BiFe1-xCoxO3 (x = 0.03, 0.05, 0.1) thin films significantly enhanced, which provides potential applications in information storage.

  15. Sol-gel synthesis, characterization and optical properties of mercury-doped TiO{sub 2} thin films deposited on ITO glass substrates

    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); Ben Sedrine, N.; 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)

    2011-08-15

    The Hg-doped and undoped nano-crystalline TiO{sub 2} films on ITO glass substrates surface and polycrystalline powders were prepared by sol-gel dip coating technique. The crystal structure and surface morphology of TiO{sub 2} were characterized by means of X-ray diffractometer (XRD), atomic force microscope (AFM), spectrophotometer, Fourier-transform infrared (FTIR), and spectroscopic ellipsometry (SE). The results indicated that the powder of TiO{sub 2}, doped with 5% Hg in room temperature was only composed of the anatase phase whereas in the undoped powder exhibits an amorphous phase were present. After heat treatments of thin films, titanium oxide starts to crystallize at the annealing temperature 400 {sup o}C. The average crystallite size of the undoped TiO{sub 2} films was about 8.17 nm and was increased with Hg-doping in the TiO{sub 2} films. Moreover, the grains distributed more uniform and the surface roughness was greater in the Hg-doped TiO{sub 2} films than in the undoped one. Refractive index and porosity were calculated from the measured transmittance spectrum. The values of the index of refraction are in the range (1.95-2.49) and the porosity is in the range (47-2.8). The coefficient of transmission varies from 60 to 90%. SE study was used to determine the annealing temperature effect on the optical properties in the wavelength range from 0.25 to 2 {mu}m and the optical gap of the Hg-doped TiO{sub 2} thin films.

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

    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.

  17. Sol-gel synthesis of hydroxyapatite

    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. Neutron detector using sol-gel absorber

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

    1999-01-01

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

  19. Hybrid sol-gel optical materials

    Zeigler, John M.

    1992-01-01

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

  20. Electrophoretically active sol-gel processes to backfill, seal, and/or densify porous, flawed, and/or cracked coatings on electrically conductive material

    Panitz, Janda K.; Reed, Scott T.; Ashley, Carol S.; Neiser, Richard A.; Moffatt, William C.

    1999-01-01

    Electrophoretically active sol-gel processes to fill, seal, and/or density porous, flawed, and/or cracked coatings on electrically conductive substrates. Such coatings may be dielectrics, ceramics, or semiconductors and, by the present invention, may have deposited onto and into them sol-gel ceramic precursor compounds which are subsequently converted to sol-gel ceramics to yield composite materials with various tailored properties.

  1. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    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.

  2. Sol-Gel Derived Hafnia Coatings

    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.

  3. Fluorescence metrology of silica sol-gels

    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 ...

  4. Sol-gel additive for systems with inorganic binders

    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)

  5. Potential of sub- and supercritical CO_2 reaction media for sol-gel deposition of silica-based molecular sieve membranes

    Durand, Veronique; Duchateau, Maxime; Drobek, Martin; Julbe, Anne; Hertz, Audrey; Ruiz, Jean-Christophe; Sarrade, Stephane

    2014-01-01

    A new eco-friendly method recently developed in our group has been further investigated for the preparation of gas selective silica-based molecular sieve membranes on/in macroporous tubular ceramic supports without any intermediate layer. The synthesis protocol under sub- and supercritical conditions was based on an 'On-Stream Supercritical Fluid Deposition method' (OS-SFD) applying supercritical carbon dioxide (scCO_2) as an attractive 'green' solvent with easily adjustable properties enabling a controlled solubilisation/reaction of precursors and their transport to the ceramic support. Parameters influencing the final membrane characteristics such as permeates flow rate, calcination treatment and deposition steps have been examined for a selected reaction mixture, transmembrane pressure and defined deposition temperatures. On-line monitoring of the membrane formation process (deposition signature curve) was used in this process. Membrane characteristics are discussed in correlation with their gas permeation properties. The optimized crack-free silica membranes prepared at 50 C have a compact microstructure but a thermal stability limited to 400 C. A second deposition run allowed a recovery of the molecular sieving behaviour with a thermally activated transport for He up to 350 C. These promising results demonstrate the potential of this novel method for the preparation of uniform molecular sieve membranes deposited directly on macroporous supports with virtually zero waste. (authors)

  6. Ring-Resonator/Sol-Gel Interferometric Immunosensor

    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.

  7. Transparent Hydrophobic Coating by Sol Gel Method

    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)

  8. Sol-Gel Chemistry for Carbon Dots.

    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.

  9. Sol-gel bonding of silicon wafers

    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

  10. Sol-Gel Manufactured Energetic Materials

    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.

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

    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

  12. OPTICAL PROPERTIES OF Al:ZnO THIN FILM DEPOSITED BY DIFFERENT SOL-GEL TECHNIQUES: ULTRASONIC SPRAY PYROLYSIS AND DIP-COATING

    Ebru Gungor

    2016-08-01

    Full Text Available Undoped and Al-doped ZnO polycrystalline thin films have been fabricated on glass substrates by using a computer-controlled dip coating (DC and ultrasonic spray pyrolysis (USP systems. The film deposition parameters of DC process were optimized for the samples. In this technique, the substrate was exposed to temperature gradient using a tube furnace. In the study, the other solvent-based technique was conventional USP. The zinc salt and Al salt concentrations in the solution were kept constant as 0.1 M and 2% of Zn salt’s molarity, respectively. The optical properties were compared for the films deposited two different techniques. The optical transmission of Al:ZnO/Glass/Al:ZnO sample dip coated and  the optical transmission of Al:ZnO/Glass sample ultrasonically sprayed were determined higher than 80% in the visible and near infrared region. Experimental optical transmittance spectra of the films in the forms of FilmA/Glass/FilmA and FilmA/glass were used to determine the optical constants. It was observed that the optical band gaps of Al doped ZnO films onto glass substrate were increases with increase of Al content and the absorption edge shifted to the shorter wavelength (blue shift compared with the undoped ZnO thin film.

  13. Ionogel Electrolytes through Sol-Gel Processing

    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

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

    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)

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

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

    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.

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

    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

  18. Resistividade do filme depositado via sol-gel e estado de oxidação do dopante Ce na matriz SnO2 Resistivity of the film deposited via sol-gel and oxidation state of Ce doping in SnO2 matrix

    L. V. A. Scalvi

    2011-06-01

    Full Text Available Incorporação de Ce3+ ou Ce4+ em filmes finos de SnO2 depositados via sol-gel-dip-coating aumenta drasticamente a resistividade elétrica. No primeiro caso, temos comportamento aceitador do dopante, levando a matriz à alta compensação de carga. Por outro lado, para Ce4+, verifica-se aumento na largura da região de depleção do contorno de grão, resultando em maior espalhamento de elétrons. Medidas de caracterização elétrica sob pressão ambiente levam à barreiras de potencial mais altas do que as medidas sob vácuo, devido a adsorção de oxigênio na superfície das partículas. A presença de Ce3+ aumenta a transmitância no infravermelho, o que significa menor quantidade de elétrons livres. Dados de XANES confirmam que o tratamento térmico a 550 ºC dos filmes, ainda que promova oxidação parcial para Ce4+, preserva uma quantidade significativa (em torno de 60% no estado Ce3+. Espectroscopia Raman mostra a evolução dos modos de vibração intra-grãos de SnO2 com o aumento da temperatura de tratamento térmico.Incorporation of Ce3+ or Ce4+ in sol-gel dip-coating SnO2 thin films increases drastically its electrical resistivity. In the first case, it is due the acceptor-like nature of the doping ion, leading the matrix to high charge compensation. On the other hand, for Ce+4 doped samples, it is verified a broadening of the grain boundary depletion layer. Measurements under room pressure leads to higher intergrain potential barriers when compared to measurements carried out under vacuum conditions, due to oxygen adsorption at particles surface. The presence of Ce3+ increases the infrared transmittance, which means a lower free electron concentration. XANES data confirms that the thermal annealing at 550 ºC of thin films, although promotes oxidation to Ce4+, still keeps a significantly amount (about 60% of ions in the oxidation state Ce3+. Raman spectroscopy data show the evolution of the SnO2 bulk vibration modes with

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

    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. Current and future possibilities of sol-gel process

    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)

  1. Industrial applications of sol-gel technology

    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

  2. Sol-gel precursors and products thereof

    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##

  3. Sol-gel method for encapsulating molecules

    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.

  4. Bioorganically doped sol-gel materials containing amyloglucosidase activity

    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.

  5. Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

    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…

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

    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

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

    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.

  8. Self-Healing Corrosion Protective Sol-Gel Coatings

    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

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

    Yu Jiuhong; Ju Huangxian

    2003-01-01

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

  10. Hydrogen permeation through sol-gel-coated iron during galvanostatic charging

    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

  11. Foldable and Cytocompatible Sol-gel TiO2 Photonics.

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

    2015-09-07

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

  12. Superconductive ceramics obtained with sol gel method

    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

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

    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.

  14. Generation of amorphous ceramic capacitor coatings on titanium using a continuous sol-gel process

    Dixon, B.G.; Walsh, M.A. III; Phillips, P.G.; Morris, R.S.

    1995-01-01

    Thin amorphous films of ceramic capacitor materials were successfully deposited using sol-gel chemistry onto titanium wire using a continuous, computer controlled process. By repeatedly depositing and calcining very thin layers of material, smooth and even coats can be produced. Surface analyses revealed the layered nature of these thin coats, as well as the amorphous nature of the ceramic. The electrical properties of the better coatings, all composed of niobium, bismuth, zinc oxides, were then evaluated. copyright 1995 Materials Research Society

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

    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

  16. Sol-gel preparation of uranium oxide spheres

    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)

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

    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.

  18. Cholesterol biosensor based on a plastic optical fibre with sol-gel: structural analysis and sensing properties

    Razo-Medina, D. A.; Trejo-Durán, M.; Alvarado-Méndez, E.

    2018-02-01

    In this paper, we report the design and characterization of an optical fibre cholesterol biosensor by using sol-gel immobilization technique. The cholesterol enzyme is encapsulated inside of the sol-gel film onto an end of a plastic optical fibre. Two film deposition methods (Dip-Coating and Immersion) were studied. The morphology analysis and sensing properties permit us to determine the best film deposition to sense cholesterol concentration. The range of measured is 4.4-5.2 mM in real time and our results were validated by comparing them with other previously published results. The biosensor is portable, simple cheap, and easy to use.

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

    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.

  20. Electrophoretic Porosimetry of Sol-Gels

    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.

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

    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...

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

    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...

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

    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...

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

    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

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

    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.

  6. Sol-gel process for thermal reactor fuel fabrication

    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

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

    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.

  8. Vapor phase modification of sol-gel derived titania (TiO{sub 2}) surfaces

    Piwonski, Ireneusz [University of Lodz, Department of Chemical Technology and Environmental Protection, Pomorska 163, 90-236 Lodz (Poland)]. E-mail: irek@uni.lodz.pl; Ilik, Aneta [University of Lodz, Department of Chemical Technology and Environmental Protection, Pomorska 163, 90-236 Lodz (Poland)

    2006-12-30

    Chemical vapor deposition (CVD) method was used in titania surface modification. Titania layers were obtained in sol-gel process and prepared as thin films on silicon wafers in dip-coating method. In order to define the influence of modification on titania surface properties (e.g., friction), various types of fluoroalkylsilanes were used. The effectiveness of the modification was monitored by FT-IR spectroscopy. The topography and frictional measurements were investigated with the use of atomic force microscopy (AFM)

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

    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.

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

    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

  11. A Review of Photocatalysts Prepared by Sol-Gel Method for VOCs Removal

    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.

  12. Incorporation of europium III complex into nanoparticles and films obtained by the Sol-Gel methodology

    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.

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

    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

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

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

    2014-12-01

    The black citrus aphid, also known as the tea aphid, (Toxoptera aurantii Boyer) attacks economically important crops, including tea (Camellia sinensis (L.) O. Kuntze). In the current study, silica sol-gel formulations were screened to find one that could carry and release C. sinensis plant volatiles to lure black citrus aphids in a greenhouse. The common plant volatile trans-2-hexen-1-al was used as a model molecule to screen for suitable sol-gel formulations. A zNose (Electronic Sensor Technology, Newbury Park, CA) transportable gas chromatograph was used to continuously monitor the volatile emissions. A sol-gel formulation containing tetramethyl orthosilicate and methyltrimethoxysilane in an 8:2 (vol:vol) ratio was selected to develop a slow-release dispenser. The half-life of trans-2-hexen-1-al in the sol-gel dispenser increased slightly with the volume of this compound in the dispenser. Ten different volatiles were tested in the sol-gel dispenser. Alcohols of 6-10 carbons had the longest half-lives (3.01-3.77 d), while esters of 6-12 carbons had the shortest (1.53-2.28 d). Release of these volatiles from the dispensers could not be detected by the zNose after 16 d (cis-3-hexenyl acetate) to 26 d (3,7-dimethylocta-1,6-dien-3-ol). In greenhouse experiments, trans-2-hexen-1-al and cis-3-hexen-1-ol released from the sol-gel dispensers attracted aphids for ≍17 d, and release of these volatiles could not be detected by the zNose after ≍24 d. The sol-gel dispensers performed adequately for the slow release of plant volatiles to trap aphids in the greenhouse. © 2014 Entomological Society of America.

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

    Fang, Jonathan

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

  16. Percutaneous external fixator pins with bactericidal micron-thin sol-gel films for the prevention of pin tract infection.

    Qu, Haibo; Knabe, Christine; Radin, Shula; Garino, Jonathan; Ducheyne, Paul

    2015-09-01

    Risk of infection is considerable in open fractures, especially when fracture fixation devices are used to stabilize the fractured bones. Overall deep infection rates of 16.2% have been reported. The infection rate is even greater, up to 32.2%, with external fixation of femoral fractures. The use of percutaneous implants for certain clinical applications, such as percutaneous implants for external fracture fixation, still represents a challenge today. Currently, bone infections are very difficult to treat. Very potent antibiotics are needed, which creates the risk of irreversible damage to other organs, when the antibiotics are administered systemically. As such, controlled, local release is being pursued, but no such treatments are in clinical use. Herein, the use of bactericidal micron-thin sol-gel films on metallic fracture fixation pins is reported. The data demonstrates that triclosan (2,4,4'-trichloro-2'-hydroxydiphenylether), an antimicrobial agent, can be successfully incorporated into micron-thin sol-gel films deposited on percutaneous pins. The sol-gel films continuously release triclosan in vitro for durations exceeding 8 weeks (longest measured time point). The bactericidal effect of the micron-thin sol-gel films follows from both in vitro and in vivo studies. Inserting percutaneous pins in distal rabbit tibiae, there were no signs of infection around implants coated with a micron-thin sol-gel/triclosan film. Healing had progressed normally, bone tissue growth was normal and there was no epithelial downgrowth. This result was in contrast with the results in rabbits that received control, uncoated percutaneous pins, in which abundant signs of infection and epithelial downgrowth were observed. Thus, well-adherent, micron-thin sol-gel films laden with a bactericidal molecule successfully prevented pin tract infection. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

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

    2012-07-01

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

  18. Structural Evolution and Stability of Sol-Gel Biocatalysts

    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)

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

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

    1990-01-01

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

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

    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.

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

    Piwonski, Ireneusz

    2009-01-01

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

  2. Electrochemical behaviour of ceramic yttria stabilized zirconia on carbon steel synthesized via sol-gel process

    Crespo, M.A. Dominguez; Murillo, A. Garcia; Torres-Huerta, A.M.; Yanez-Zamora, C.; Carrillo-Romo, F. de J

    2009-01-01

    Chromate conversion coatings have been widely applied for the corrosion of different metallic substrates. However, the waste containing Cr 6+ has many limitations due to the environmental consideration and health hazards. An interesting alternative seems to be the deposition on metallic surface of thin layers of yttria or zirconia or both by the sol-gel process. In this study, Ytttria and Yttria stabilized zirconia (YSZ, 8% Y 2 O 3 ) thin films were used for coating commercial carbon steel substrates by sol-gel method and the dip-coating process. The evolution of organic compounds up to crystallization process as a function of heat treatments was study by FT-IR spectroscopy. The structure and morphology of the coatings were analysed using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The anticorrosion performance of the coatings has been evaluated by using electrochemical techniques in an aggressive media (3.5 wt.% NaCl). The corrosion behaviour of sol-gel method was compared with traditional chromate conversion coatings. Differences in the electrochemical behaviour of YSZ coatings are related to the development of microcracks during the sintering process and to the presence of organic compounds during growth film. Electrochemical results showed that sol-gel YSZ and Y 2 O 3 coatings can act as protective barriers against wet corrosion; however yttria films displayed low adhesion to substrate. The corrosion parameters provide an explanation of the role of each film and show a considerable increase in the corrosion resistance for coated samples in comparison to the bare steel samples.

  3. Electrochemical behaviour of ceramic yttria stabilized zirconia on carbon steel synthesized via sol-gel process

    Crespo, M.A. Dominguez, E-mail: mdominguezc@ipn.m [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Murillo, A. Garcia; Torres-Huerta, A.M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Yanez-Zamora, C. [Estudiante del postgrado en Tecnologia Avanzada del CICATA-IPN, Unidad Altamira, km 14.5, Carr. Tampico-Puerto Industrial. C.P. 89600, Altamira, Tamaulipas (Mexico); Carrillo-Romo, F. de J [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico)

    2009-08-26

    Chromate conversion coatings have been widely applied for the corrosion of different metallic substrates. However, the waste containing Cr{sup 6+} has many limitations due to the environmental consideration and health hazards. An interesting alternative seems to be the deposition on metallic surface of thin layers of yttria or zirconia or both by the sol-gel process. In this study, Ytttria and Yttria stabilized zirconia (YSZ, 8% Y{sub 2}O{sub 3}) thin films were used for coating commercial carbon steel substrates by sol-gel method and the dip-coating process. The evolution of organic compounds up to crystallization process as a function of heat treatments was study by FT-IR spectroscopy. The structure and morphology of the coatings were analysed using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The anticorrosion performance of the coatings has been evaluated by using electrochemical techniques in an aggressive media (3.5 wt.% NaCl). The corrosion behaviour of sol-gel method was compared with traditional chromate conversion coatings. Differences in the electrochemical behaviour of YSZ coatings are related to the development of microcracks during the sintering process and to the presence of organic compounds during growth film. Electrochemical results showed that sol-gel YSZ and Y{sub 2}O{sub 3} coatings can act as protective barriers against wet corrosion; however yttria films displayed low adhesion to substrate. The corrosion parameters provide an explanation of the role of each film and show a considerable increase in the corrosion resistance for coated samples in comparison to the bare steel samples.

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

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

    1988-01-01

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

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

    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.

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

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

    2004-01-01

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

  7. Sol-gel-state of hydrated zirconium dioxide

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

    1995-01-01

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

  8. Silica scintillating materials prepared by sol-gel methods

    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

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

    Danchova, Nina; Gutzov, Stoyan

    2014-01-01

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

  10. Sol-gel processing with inorganic metal salt precursors

    Hu, Zhong-Cheng

    2004-10-19

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

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

    Rita B. Figueira

    2015-04-01

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

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

    Congdon, James W [Aiken, SC

    2009-03-17

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

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

    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...

  14. Stoichiometric hydroxyapatite obtained by precipitation and sol gel processes

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

    2005-07-01

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

  15. Neutron detector based on lithiated sol-gel glass

    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.

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

    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.

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

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

    1998-01-01

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

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

    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)

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

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

    2016-01-01

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

  20. Luminescent hybrid porphyrinosilica obtained by sol gel chemistry

    Neri Cláudio Roberto

    2003-01-01

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

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

    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.

  2. New Functionalized Sol-Gel Hybrid Sorbent Coating for Stir Bar Sorptive Extraction of Selected Non-Steroidal Anti Inflammatory Drugs in Human Urine Samples

    Mashkurah Abd Rahim; Wan Aini Wan Ibrahim; Zainab Ramli; Mohd Marsin Sanagi

    2015-01-01

    A new sol-gel hybrid material, methyltrimethoxysilane-cyanopropyltriethoxysilane (MTMOS-CNPrTEOS) was successfully synthesized and used as a coating material in stir bar sorptive extraction (SBSE) of selected non-steroidal anti-inflammatory drugs (NSAIDs) in urine samples. The MTMOS-CNPrTEOS hybrid was synthesized by hydrolysis and condensation of MTMOS and CNPrTEOS in the presence of trifluoroacetic acid as catalyst via sol-gel method. Several factors influencing the synthesized sol-gel hybrid MTMOS-CNPrTEOS process such as mole ratio of MTMOS-CNPrTEOS, NaOH concentrations as etching solution, etching time, coating time and water content were investigated and optimized in this study. The optimum synthesis conditions obtained were 1:1 mol ratio of MTMOS-CNPrTEOS, 1 M NaOH as etching solution, 60 min etching time, 2 h coating time and 6 mmol water. The sol-gel hybrid MTMOS-CNPrTEOS synthesized under the optimum conditions was used to determine selected NSAIDs in human urine samples using normal stacking mode capillary electrophoresis with ultraviolet detection. MTMOS-CNPrTEOS SBSE method demonstrated good linearity (60 to 20,000 μg L -1 ) with excellent coefficient of determination (r 2 > 0.9990). The sol-gel hybrid MTMOS-CNPrTEOS SBSE method showed low limit of detection (35 - 41 μg L -1 ) with good precision (RSD < 6 %, n = 3) and excellent extraction recoveries (83.5 - 98.9 %) for the selected NSAIDs. The sol-gel hybrid MTMOS-CNPrTEOS SBSE method demonstrated good potential as an alternative sorbent in SBSE method for NSAIDs. (author)

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

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

    2013-01-01

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

  4. Sol-Gel Thin Films for Plasmonic Gas Sensors

    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

  5. Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

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

    2018-01-01

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

  6. Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

    Jolanta Gąsiorek

    2018-01-01

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

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

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

    2018-01-26

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

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

    Zheng, Kai; Boccaccini, Aldo R

    2017-11-01

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

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

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

    2000-01-01

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

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

    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.

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

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

    2003-06-23

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

  12. Ultraviolet Stimulated Emission from Sol-Gel Spin Coated ZnO Thin Films

    Ahmed S. Razeen

    2017-01-01

    Full Text Available Low cost ultraviolet stimulated emission has been generated using optical excitation of ZnO thin films deposited by sol-gel spin coating on n+ As-doped 100 Si-substrate. The number of deposited layers and the heat treatment have been investigated to obtain a film that can generate stimulated emission under optical excitation. The optimum condition for preparation of the film has been presented. X-ray diffraction and scanning electron microscope have been used for structural and morphological investigations. Input-output intensity dependence and spectral width, peak emission wavelength, and the quantum efficiency versus the pump intensity have been presented. A quantum efficiency of about 24.2% has been reported, a power exponent higher than 8 has been obtained in input-output intensity dependence, and a threshold of about 23 Mw/cm2 has been evaluated for the samples. The mechanism by which stimulated emission occurs has been discussed. The results show that sol-gel spin coating is a promising method for generating ultraviolet stimulated emission from ZnO thin films.

  13. Spectroellipsometric study of the sol-gel nanocrystalline ITO multilayer films

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

    2004-05-01

    Tin-doped indium oxide (ITO) thin films have been deposited by sol-gel process using 'sols' of indium and tin isopropoxides. The thickness of one deposited ITO layer is approximately 50 nm. The desired thickness was obtained by 1-5 successive depositions. The XTEM cross-sectional view of an ITO sample with five depositions showed a clear delimitation of the layers with an alternating structure dense/porous ITO layers. The void fraction in porous regions varies between 20 and 25%. Cubic bixbyite In{sub 2}O{sub 3} nanocrystals with size of 10-20 nm and no phases separation of tin oxide were observed. The optical properties of the films have been investigated by optical transmission and spectroscopic ellipsometry. Reliable optical constants and porosity are obtained only with the model of internal structure based on XTEM results.

  14. Investigation of sol-gel antireflective coatings

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

    1984-03-01

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

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

    1989-09-01

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

  16. Synthesis of phthalocyanine doped sol-gel materials

    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

  17. Atomic force microscopy study of TiO2 sol-gel films thermally treated under NH3 atmosphere

    Trapalis, C.; Todorova, N.; Anastasescu, M.; Anastasescu, C.; Stoica, M.; Gartner, M.; Zaharescu, M.; Stoica, T.

    2009-01-01

    Multilayered TiO 2 films were obtained by sol-gel and dipping deposition on quartz substrate followed by thermal treatment under NH 3 atmosphere. In an attempt to understand the close relationship between microstructural characteristics and the synthesis parameters, a systematic research of the structure and the morphology of NH 3 modified TiO 2 sol-gel films by XRD and Atomic Force Microscopy is reported. The surface morphology has been evaluated in terms of grains size, fractal dimension and surface roughness. For each surface, it was found a self-similar behavior (with mean fractal dimension in the range of 2.67-3.00) related to an optimum morphology favorable to maintain a nano-size distribution of the grains. The root mean square (RMS) roughness of the samples was found to be in the range of 0.72-6.02 nm.

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

    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.

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

    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.

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

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

    2018-05-03

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

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

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

    2005-01-01

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

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

    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

  3. Physical vapor deposition of Er.sup.3+./sup.: Yb.sub.3./sub.Al.sub.5./sub.O.sub.12./sub. thin films from sol-gel derived targets

    Hlásek, T.; Rubešová, K.; Jakeš, V.; Nováček, M.; Oswald, Jiří; Fitl, P.; Siegel, J.; Macháč, P.

    2016-01-01

    Roč. 60, č. 4 (2016), s. 285-290 ISSN 0862-5468 Institutional support: RVO:68378271 Keywords : PLD * electron beam deposition * thin film * ytterbium-aluminium garnet * erbium Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.439, year: 2016

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

    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)

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

    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)

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

    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)

  7. Synthesis of lithium doped zinc oxide by sol gel

    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)

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

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

    1993-04-01

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

  9. Sol-gel synthesis and characterization of lithiummolybdosilicate glass

    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)

  10. Moment scaling at the sol-gel transition

    Botet, R.

    1998-01-01

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

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

    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)

  12. Modified sol-gel coatings for biotechnological applications

    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.

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

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

    2009-03-20

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

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

    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)

  15. Sol-gel TiO2 colloidal suspensions and nanostructured thin films: structural and biological assessments

    Quartapelle Procopio, Elsa; Colombo, Valentina; Santo, Nadia; Sironi, Angelo; Lenardi, Cristina; Maggioni, Daniela

    2018-02-01

    The role of substrate topography in phenotype expression of in vitro cultured cells has been widely assessed. However, the production of the nanostructured interface via the deposition of sol-gel synthesized nanoparticles (NPs) has not yet been fully exploited. This is also evidenced by the limited number of studies correlating the morphological, structural and chemical properties of the grown thin films with those of the sol-gel ‘brick’ within the framework of the bottom-up approach. Our work intends to go beyond this drawback presenting an accurate investigation of sol-gel TiO2 NPs shaped as spheres and rods. They have been fully characterized by complementary analytical techniques both suspended in apolar solvents, by dynamic light scattering (DLS) and nuclear magnetic resonance (NMR) and after deposition on substrates (solid state configuration) by transmission electron microscopy (TEM) and powder x-ray diffraction (PXRD). In the case of suspended anisotropic rods, the experimental DLS data, analyzed by the Tirado-Garcia de la Torre model, present the following ranges of dimensions: 4-5 nm diameter (∅) and 11-15 nm length (L). These results are in good agreement with that obtained by the two solid state techniques, namely 3.8(9) nm ∅ and 13.8(2.5) nm L from TEM and 5.6(1) ∅ and 13.3(1) nm L from PXRD data. To prove the suitability of the supported sol-gel NPs for biological issues, spheres and rods have been separately deposited on coverslips. The cell response has been ascertained by evaluating the adhesion of the epithelial cell line Madin-Darby canine kidney. The cellular analysis showed that titania films promote cell adhesion as well clustering organization, which is a distinguishing feature of this type of cell line. Thus, the use of nanostructured substrates via sol-gel could be considered a good candidate for cell culture with the further advantages of likely scalability and interfaceability with many different materials usable as supports.

  16. Sol-gel TiO2 colloidal suspensions and nanostructured thin films: structural and biological assessments.

    Procopio, Elsa Quartapelle; Colombo, Valentina; Santo, Nadia; Sironi, Angelo; Lenardi, Cristina; Maggioni, Daniela

    2018-02-02

    The role of substrate topography in phenotype expression of in vitro cultured cells has been widely assessed. However, the production of the nanostructured interface via the deposition of sol-gel synthesized nanoparticles (NPs) has not yet been fully exploited. This is also evidenced by the limited number of studies correlating the morphological, structural and chemical properties of the grown thin films with those of the sol-gel 'brick' within the framework of the bottom-up approach. Our work intends to go beyond this drawback presenting an accurate investigation of sol-gel TiO 2 NPs shaped as spheres and rods. They have been fully characterized by complementary analytical techniques both suspended in apolar solvents, by dynamic light scattering (DLS) and nuclear magnetic resonance (NMR) and after deposition on substrates (solid state configuration) by transmission electron microscopy (TEM) and powder x-ray diffraction (PXRD). In the case of suspended anisotropic rods, the experimental DLS data, analyzed by the Tirado-Garcia de la Torre model, present the following ranges of dimensions: 4-5 nm diameter (∅) and 11-15 nm length (L). These results are in good agreement with that obtained by the two solid state techniques, namely 3.8(9) nm ∅ and 13.8(2.5) nm L from TEM and 5.6(1) ∅ and 13.3(1) nm L from PXRD data. To prove the suitability of the supported sol-gel NPs for biological issues, spheres and rods have been separately deposited on coverslips. The cell response has been ascertained by evaluating the adhesion of the epithelial cell line Madin-Darby canine kidney. The cellular analysis showed that titania films promote cell adhesion as well clustering organization, which is a distinguishing feature of this type of cell line. Thus, the use of nanostructured substrates via sol-gel could be considered a good candidate for cell culture with the further advantages of likely scalability and interfaceability with many different materials usable as supports.

  17. Sol-gel derived antireflective coatings for silicon

    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.

  18. Sol-gel based sensor for selective formaldehyde determination

    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.

  19. Sol-gel based sensor for selective formaldehyde determination

    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.

  20. Sol-gel applications for ceramic membrane preparation

    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.

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

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

    2016-09-27

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

  2. Nanostructured energetic materials derived from sol-gel chemistry

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

    2000-01-01

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

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

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

    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

  5. Transparent conducting sol-gel ATO coatings for display applications by an improved dip coating technique

    Guzman, G.; Dahmani, B.; Puetz, J.; Aegerter, M.A.

    2006-01-01

    Transparent conducting coatings of sol-gel ATO (antimony-doped tin oxide) were used to improve surface smoothness of commercial sputter-deposited ITO (indium tin oxide) coatings for application as display electrodes. In order to overcome the deteriorating evaporation-cooling during dip coating, the coating solution was heated moderately to 25 deg. C thus providing the substrate with the required heat. This way, the surface roughness of the ITO could be reduced with an only 45 nm thick ATO coating to R pv = 3.8 nm (R a = 0.4 nm) compared to 31 nm (3.8 nm) for the ITO substrate. Another benefit of such additional coating is the possibility to tailor surface properties of the electrodes in wide ranges. This was used to increase the work function of the ITO substrate from initially 4.3-4.6 eV to about 4.8-5.2 eV by the ATO coating

  6. Low Loss Sol-Gel TiO2 Thin Films for Waveguiding Applications

    Alexis Fischer

    2013-03-01

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

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

    Benoit, Florence

    2015-01-01

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

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

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

    2008-01-01

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

  9. Sol-gel synthesis and optical properties of titanium dioxide thin film

    Ullah, Irfan; Khattak, Shaukat Ali; Ahmad, Tanveer; Saman; Ludhi, Nayab Ali

    2018-03-01

    The titanium dioxide (TiO2) is synthesized by sol-gel method using titanium-tetra-iso-propoxide (TTIP) as a starting material, and deposited on the pre-cleaned glass substrate using spin coating technique at optimized parameters. Energy dispersive X-ray (EDX) spectroscopy confirms successful TiO2 growth. The optical properties concerning the transmission and absorption spectra show 85% transparency and 3.28 eV wide optical band gap for indirect transition, calculated from absorbance. The exponential behavior of absorption edge is observed and attributed to the localized states electronic transitions, curtailed in the indirect band gap of the thin film. The film reveals decreasing refractive index with increasing wavelength. The photoluminescence (PL) study ascertains that luminescent properties are due to the surface defects.

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

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

    2010-01-01

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

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

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

    2014-08-01

    Orthopedic injuries constitute the majority of wounds sustained by U.S. soldiers in recent conflicts. The risk of infection is considerable with fracture fixation devices. In this pilot study, we examined the use of unique bactericidal micron-thin sol-gel films on fracture fixation devices and their ability to prevent and eradicate infections. External fixation was studied with micron-thin sol-gel coated percutaneous pins releasing triclosan and inserted medially into rabbit tibiae. A total of 11 rabbits received percutaneous pins that were either uncoated or sol-gel/triclosan coated. Internal fracture fixation was also studied using sol-gel coated intramedullary (IM) nails releasing vancomycin in the intramedullary tibiae. Six sheep received IM nails that were coated with a sol-gel film that either contained vancomycin or did not contain vancomycin. All animals were challenged with Staphylococcus aureus around the implant. Animals were euthanized at 1 month postoperative. Rabbits receiving triclosan/sol-gel coated percutaneous pins did not show signs of infection. Uncoated percutaneous pins had a significantly higher infection rate. In the sheep study, there were no radiographic signs of osteomyelitis with vancomycin/sol-gel coated IM nails, in contrast to the observations in the control cohort. Hence, the nanostructured sol-gel controlled release technology offers the promise of a reliable and continuous delivery system of bactericidals from orthopedic devices to prevent and treat infection. Reprint & Copyright © 2014 Association of Military Surgeons of the U.S.

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

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

    2015-01-01

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

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

    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

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

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

    2004-01-01

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

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

    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.

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

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

    2006-01-01

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

  17. Modified Au nanoparticles-imprinted sol-gel, multiwall carbon nanotubes pencil graphite electrode used as a sensor for ranitidine determination.

    Rezaei, B; Lotfi-Forushani, H; Ensafi, A A

    2014-04-01

    A new, simple, and disposable molecularly imprinted electrochemical sensor for the determination of ranitidine was developed on pencil graphite electrode (PGE) via cyclic voltammetry (CV). The PGEs were coated with MWCNTs containing the carboxylic functional group (f-MWCNTs), imprinted with sol-gel and Au nanoparticle (AuNPs) layers (AuNP/MIP-sol-gel/f-MWCNT/PGE), respectively, to enhance the electrode's electrical transmission and sensitivity. The thin film of molecularly imprinted sol-gel polymers with specific binding sites for ranitidine was cast on modified PGE by electrochemical deposition. The AuNP/MIP-sol-gel/f-MWCNT/PGE thus developed was characterized by electrochemical impedance spectroscopy (EIS) and CV. The interaction between the imprinted sensor and the target molecule was also observed on the electrode by measuring the current response of 5.0mMK3[Fe(CN)6] solution as an electrochemical probe. The pick currents of ranitidine increased linearly with concentration in the ranges of 0.05 to 2.0μM, with a detection limit of (S/N=3) 0.02μM. Finally, the modified electrode was successfully employed to determine ranitidine in human urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    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.

  19. Recobrimento da liga Ti-6Al-4V com hidroxiapatita pelo método sol-gel e sua aplicação a hastes femorais não-cimentadas Coating of Ti-6Al-4V alloy with hydroxyapatite by using sol-gel method and its application to non-cemented femoral stem

    E. P. Avés

    2008-12-01

    Full Text Available O recobrimento de ligas metálicas com cerâmicas bioativas visa acelerar a formação óssea ao redor do implante, contribuindo para a sua estabilização. Neste trabalho estudou-se a fase cerâmica de hidroxiapatita depositada pelo processo sol-gel em chapas da liga metálica Ti-6Al-4V. A camada de recobrimento foi caracterizada por microscopia eletrônica de varredura, por difração de raios X e sua adesão ao substrato foi avaliada pelo teste de cisalhamento O teste de citocompatibilidade mostrou que o processo de recobrimento por sol-gel não promoveu morte celular significativamente maior que o controle (p > 0,05. Além disso, hastes femorais removidas de pacientes (explantes foram adequadamente recobertas utilizando-se o processo sol-gel.The coating of metallic alloys with bioactive ceramics aims to accelerate bone formation around the implant, contributing to its fixation. In this paper, the deposition of hydroxyapatite ceramic on Ti-6Al-4V alloy sheets by the sol-gel method was studied. The coating layer was characterized by scanning electron microscopy, X-ray diffraction and its adhesion to substrate was evaluated by shear testing. The citocompatibility test shows that the sol-gel coating did not provoke the cell death significantly higher than the control (p > 0.05. Moreover, femoral stems removed from patient (explants were adequately coated using the sol-gel process.

  20. Synthesis of ZNO nanoparticles by Sol-Gel processing

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

    2011-01-01

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

  1. Polymer sol-gel composite inverse opal structures.

    Zhang, Xiaoran; Blanchard, G J

    2015-03-25

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

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

    Juanda, D.; Sambodo Daru, G.

    1998-01-01

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

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

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

    2008-01-01

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

  4. Manufacture of Regularly Shaped Sol-Gel Pellets

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

    2006-01-01

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

  5. Sol-Gel Glass Holographic Light-Shaping Diffusers

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

    2005-01-01

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

  6. 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

    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.

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

    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.

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

    2015-10-19

    Catalysts in Sol -Gel Matrices 5a. CONTRACT NUMBER 5b. GRANT NUMBER N00014-09-1-0217 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Detty, Michael R. 5d...Technical Report for ONR N00014-09-1-0217 Minimally Adhesive, Advanced Non-toxic Coatings of Dendrimeric Catalysts in Sol -Gel Matrices Michael R. Detty, PI...Environmentally benign sol -gel antifouling and foul-releasing coatings. Ace. Chem. Res. 2014, 47, 678-687. 11) Alberto, E. E.; Müller, L. M

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

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

    2017-03-01

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

  10. Comparative microstructure and electrical property studies of lead scandium tantalate thin films as prepared by LDCVD, sol-gel and sputtering techniques

    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

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

    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

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

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

    2009-01-01

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

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

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

    2010-01-01

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

  14. Structural and electrochemical behavior of sol-gel ZrO2 ceramic film on chemically pre-treated AZ91D magnesium alloy

    Li Qing; Chen Bo; Xu Shuqiang; Gao Hui; Zhang Liang; Liu Chao

    2009-01-01

    In the present investigation sol-gel-based ZrO 2 ceramic film was obtained using zirconium acetate as the precursor material. The film was deposited on AZ91D magnesium alloy by a dip-coating technique. An uniform stannate conversion coating as chemical pretreatment was employed as an intermediate layer prior to deposition of the ZrO 2 film in order to provide advantage for the formation of sol-gel-based ZrO 2 layer. The corrosion properties, structure, composition and morphology of these coatings on AZ91D magnesium alloy were studied by potentiodynamic polarization tests, EIS, XRD, SEM, respectively. According to the electrochemical tests, the corrosion resistance of AZ91D magnesium alloy was found to be greatly improved by means of this new environment-friendly surface treatment.

  15. Sol-gel derived electrode materials for supercapacitor applications

    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.

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

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

    2000-10-01

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

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

    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.

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

    Rubia F. S. Lenza

    2002-10-01

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

  19. Porous olivine composites synthesized by sol-gel technique

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

    2006-02-28

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

  20. The chemistry of plutonium in sol-gel processes

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

    1978-01-01

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

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

    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.

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

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

    2008-01-01

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

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

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

    2008-01-01

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

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

    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.

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

    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.

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

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

    2017-07-13

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

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

    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.

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

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

    Akorede

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

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

    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

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

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

    2011-02-21

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

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

    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.

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

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

    2016-03-04

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

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

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

    2008-01-01

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

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

    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

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

    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.)

  17. Sol-Gel TiO2 thin films sensitized with the mulberry pigment cyanidin

    Emerson Henrique de Faria

    2007-12-01

    Full Text Available TiO2 films have various applications, among them solar cells and photodegradation of pollutants. In this study, we investigated TiO2 films functionalized with the organic dye cyanidin extracted from black mulberry (Morus nigra. The TiO2 was functionalized by the sol-gel method and the film was deposited on glass substrates by dip-coating. Our aim was to investigate the interaction between the semiconductor and the dye, as well as the influence of the velocity and number of deposits on the characteristics of the film. Using ultraviolet-visible spectroscopy, we observed a shift from the maximum absorption band at 545 nm for the dye’s ethanol solution to 595 nm for the film, indicating interaction of the cyanidin with the TiO2. The absorption spectra in the infrared region of the functionalized TiO2 particles showed bands characteristic of the oxide and indicated their interaction with the dye. Using profilometry and m-line techniques, we found that the films presented thicknesses in the order of 100 nm. A SEM analysis confirmed the high density of the films.

  18. Doped indium nitride thin film by sol-gel spin coating method

    Lee, Hui San; Ng, Sha Shiong; Yam, Fong Kwong

    2017-12-01

    In this study, magnesium doped indium nitride (InN:Mg) thin films grown on silicon (100) substrate were prepared via sol-gel spin coating method followed by nitridation process. A custom-made tube furnace was used to perform the nitridation process. Through this method, the low dissociation temperature issue of InN:Mg thin films can be solved. The deposited InN:Mg thin films were investigated using various techniques. The X-rays diffraction results revealed that two intense diffraction peaks correspond to wurtzite structure InN (100), and InN (101) were observed at 29° and 33.1° respectively. Field emission scanning electron microscopy images showed that the surface of the films exhibits densely packed grains. The elemental composition of the deposited thin films was analyzed using energy dispersive X-rays spectroscopy. The detected atomic percentages for In, N, and Mg were 43.22 %, 3.28 %, and 0.61 % respectively. The Raman spectra showed two Raman- and infrared-active modes of E2 (High) and A1 (LO) of the wurtzite InN. The band gap obtained from the Tauc plot showed around 1.74 eV. Lastly, the average surface roughness measured by AFM was around 0.133 µm.

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

    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.

  20. Wafer scale lead zirconate titanate film preparation by sol-gel method using stress balance layer

    Lu Jian; Kobayashi, Takeshi; Yi Zhang; Maeda, Ryutaro; Mihara, Takashi

    2006-01-01

    In this paper, platinum/titanium (Pt/Ti) film was introduced as a residual stress balance layer into wafer scale thick lead zirconate titanate (PZT) film fabrication by sol-gel method. The stress developing in PZT film's bottom electrode as well as in PZT film itself during deposition were analyzed; the wafer curvatures, PZT crystallizations and PZT electric properties before and after using Pt/Ti stress balance layer were studied and compared. It was found that this layer is effective to balance the residual stress in PZT film's bottom electrode induced by thermal expansion coefficient mismatch and Ti diffusion, thus can notably reduce the curvature of 4-in. wafer from - 40.5 μm to - 12.9 μm after PZT film deposition. This stress balance layer was also found effective to avoid the PZT film cracking even when annealed by rapid thermal annealing with heating-rate up to 10.5 deg. C/s. According to X-ray diffraction analysis and electric properties characterization, crack-free uniform 1-μm-thick PZT film with preferred pervoskite (001) orientation, excellent dielectric constant, as high as 1310, and excellent remanent polarization, as high as 39.8 μC/cm 2 , can be obtained on 4-in. wafer

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

    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.

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

    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

  3. Encapsulation of Polymer Colloids in a Sol-Gel Matrix. Direct-Writing of Coassembling Organic-Inorganic Hybrid Photonic Crystals.

    Mikosch, Annabel; Kuehne, Alexander J C

    2016-03-22

    The spontaneous self-assembly of polymer colloids into ordered arrangements provides a facile strategy for the creation of photonic crystals. However, these structures often suffer from defects and insufficient cohesion, which result in flaking and delamination from the substrate. A coassembly process has been developed for convective assembly, resulting in large-area encapsulated colloidal crystals. However, to generate patterns or discrete deposits in designated places, convective assembly is not suitable. Here we experimentally develop conditions for direct-writing of coassembling monodisperse dye-doped polystyrene particles with a sol-gel precursor to form solid encapsulated photonic crystals. In a simple procedure the colloids are formulated in a sol-gel precursor solution, drop-cast on a flat substrate, and dried. We here establish the optimal parameters to form reproducible highly ordered photonic crystals with good optical performance. The obtained photonic crystals interact with light in the visible spectrum with a narrow optical stop-gap.

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

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

    2018-01-01

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

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

    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.

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

    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.

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

    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.

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

    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.

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

    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.

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

    Angelini, P.; Bond, W.D.; Caputo, A.J.; Mack, J.E.; Lackey, W.J.; Lee, D.A.; Stinton, D.P.

    1980-01-01

    The sol-gel process is being developed for the solidification and isolation of high-level nuclear fuel waste. Three gelation methods are being developed for producing alternative waste forms. These include internal gelation for producing spheres of up to 1 mm diam suitable for coating, external gelation, and water extraction methods for producing material suitable for alternate ceramic processing. In this study internal gelation has been used to produce ceramic spheres of various alternative nuclear waste compositions. A gelation system capable of producing 100-g batches has been assembled and used for development. Waste forms containing up to 70 wt % simulated Savannah River Plant waste have been produced. Dopants such as Cs, Sr, Nd, Ru, and Mo were used in some experiments to observe side waste streams and sintering effects. Synroc microspheres were coated with both low-density carbon, high-density impermeable carbon, high-temperature dense SiC, and SiC deposited at temperatures near 900 0 C. Other gelation methods and other alternative waste forms are being developed

  11. Optical Constants of Crystallized TiO2 Coatings Prepared by Sol-Gel Process

    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.

  12. Enhanced fatigue characteristics of sol-gel derived PZT thin films

    Shim, Donghyun; Pak, Jaemoon; Nam, Kuangwoo; Park, Gwangweo

    2008-01-01

    Pb(Zr,Ti)O 3 (PZT) thin films with Zr/Ti ratio of 52:48 were deposited on Pt/Ti/SiO 2 /Si substrates using the sol-gel method. Since the conditions of heat-treatment play a great role in film growth, post-annealing processes were conducted under different environments. After standard processing, films were annealed at 600 deg. C in three different atmosphere-air, O 2 and a two-step process conducted in air for 30 min and then in O 2 ambient, all done for 10 min. Through electron microscopy and X-ray diffraction, we found that all films were crack-free and highly (1 1 1) oriented. Hysteresis measurements showed a generally large polarization value. The fatigue properties differ drastically for all processes, showing an abnormal behaviour near the end of the measurement. The hysteresis loops before and after 1 x 10 10 switching cycles have been slightly changed in both shape and magnitude. Such abnormality and fatigue-free property is an unusual result for PZT films prepared on conventional Pt/Ti/SiO 2 /Si substrates

  13. Thickness controlled sol-gel silica films for plasmonic bio-sensing devices

    Figus, Cristiana, E-mail: cristiana.figus@dsf.unica.it; Quochi, Francesco, E-mail: cristiana.figus@dsf.unica.it; Artizzu, Flavia, E-mail: cristiana.figus@dsf.unica.it; Saba, Michele, E-mail: cristiana.figus@dsf.unica.it; Marongiu, Daniela, E-mail: cristiana.figus@dsf.unica.it; Mura, Andrea; Bongiovanni, Giovanni [Dipartimento di Fisica - University of Cagliari, S.P. Km 0.7, I-09042 Monserrato (Canada) (Italy); Floris, Francesco; Marabelli, Franco; Patrini, Maddalena; Fornasari, Lucia [Dipartimento di Fisica - University of Pavia, Via Agostino Bassi 6, I-27100 Pavia (PV) (Italy); Pellacani, Paola; Valsesia, Andrea [Plasmore S.r.l. -Via Grazia Deledda 4, I-21020 Ranco (Vatican City State, Holy See) (Italy)

    2014-10-21

    Plasmonics has recently received considerable interest due to its potentiality in many fields as well as in nanobio-technology applications. In this regard, various strategies are required for modifying the surfaces of plasmonic nanostructures and to control their optical properties in view of interesting application such as bio-sensing, We report a simple method for depositing silica layers of controlled thickness on planar plasmonic structures. Tetraethoxysilane (TEOS) was used as silica precursor. The control of the silica layer thickness was obtained by optimizing the sol-gel method and dip-coating technique, in particular by properly tuning different parameters such as pH, solvent concentration, and withdrawal speed. The resulting films were characterized via atomic force microscopy (AFM), Fourier-transform (FT) spectroscopy, and spectroscopic ellipsometry (SE). Furthermore, by performing the analysis of surface plasmon resonances before and after the coating of the nanostructures, it was observed that the position of the resonance structures could be properly shifted by finely controlling the silica layer thickness. The effect of silica coating was assessed also in view of sensing applications, due to important advantages, such as surface protection of the plasmonic structure.

  14. Au Nanoparticle Sub-Monolayers Sandwiched between Sol-Gel Oxide Thin Films

    Della Gaspera, Enrico; Menin, Enrico; Sada, Cinzia

    2018-01-01

    Sub-monolayers of monodisperse Au colloids with different surface coverage have been embedded in between two different metal oxide thin films, combining sol-gel depositions and proper substrates functionalization processes. The synthetized films were TiO2, ZnO, and NiO. X-ray diffraction shows the crystallinity of all the oxides and verifies the nominal surface coverage of Au colloids. The surface plasmon resonance (SPR) of the metal nanoparticles is affected by both bottom and top oxides: in fact, the SPR peak of Au that is sandwiched between two different oxides is centered between the SPR frequencies of Au sub-monolayers covered with only one oxide, suggesting that Au colloids effectively lay in between the two oxide layers. The desired organization of Au nanoparticles and the morphological structure of the prepared multi-layered structures has been confirmed by Rutherford backscattering spectrometry (RBS), Secondary Ion Mass Spectrometry (SIMS), and Scanning Electron Microscopy (SEM) analyses that show a high quality sandwich structure. The multi-layered structures have been also tested as optical gas sensors. PMID:29538338

  15. AZO Thin Films by Sol-Gel Process for Integrated Optics

    Azzedine Boudrioua

    2013-07-01

    Full Text Available Undoped and aluminum-doped zinc oxide (AZO thin films are prepared by the sol-gel process. Zinc acetate dihydrate, ethanol, and monoethanolamine are used as precursor, solvent, and stabilizer, respectively. In the case of AZO, aluminum nitrate nonahydrate is added to the precursor solution with an atomic percentage equal to 1 and 2 at.% Al. The multi thin layers are deposited by spin-coating onto glass substrates, and are transformed into ZnO upon annealing at 550 °C. Films display a strong preferential orientation, with high values for the Texture Coefficients (TC of the (002 direction (TC(002 ≈ 3. The structural, morphological, and optical properties of the thin films as a function of aluminum content have been investigated using X-Ray Diffraction (XRD, Atomic Force Microscopy (AFM, and Scanning Electronic Microscopy (SEM. Waveguiding properties of the thin films have been also studied using m-lines spectroscopy. The results indicate that the films are monomodes at 632.8 nm with optical propagation optical losses estimated around 1.6 decibel per cm (dB/cm.

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

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

    2003-01-01

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

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

    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.

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

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

    1989-01-01

    NMR investigations on the ORNL process for sol-gel synthesis of microspherical nuclear fuel (UO 2 ), has been useful in sorting out the chemical mechanism in the sol-gel steps. 13 C, 15 N, and 1 H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C 6 H l2 N 4 ) has revealed near quantitative stability of this adamantane-like compound in the sol-Gel process, contrary to its historical role as an ammonia source for gelation from the worldwide technical literature. 17 0 NMR of uranyl (UO 2 ++ ) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, [(UO 2 ) 3 (μ 3 -O)(μ 2 -OH) 3 ] + , induced by basic hydrolysis with the HMTA gelation agent. Spectroscopic results show that trimer condensation occurs during sol-gel processing leading to layered polyanionic hydrous uranium oxides in which HMTAH + is occluded as an ''intercalation'' cation. Subsequent sol-gel processing of microspheres by ammonia washing results in in-situ ion exchange and formation of a layered hydrous ammonium uranate with a proposed structural formula of (NH 4 ) 2 [(UO 2 ) 8 O 4 (OH) 10 ] · 8H 2 0. This compound is the precursor to sintered U0 2 ceramic fuel

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

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

    2004-02-03

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

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

    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.

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

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

    2005-01-01

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

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

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

    2016-09-20

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

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

    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.

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

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

    2005-04-08

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

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

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

    2017-12-19

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

  6. Synthesis, characterization and in vitro bioactivity of sol-gel-derived SiO2-CaO-P2O5-MgO bioglass

    Saboori, A.; Rabiee, M.; Moztarzadeh, F.; Sheikhi, M.; Tahriri, M.; Karimi, M.

    2009-01-01

    In this study, the synthesis of SiO 2 -CaO-P 2 O 5 -MgO bioactive glass was performed by the sol-gel method. Sol-gel-derived bioglass material was produced both in powder and in discs form by uniaxial pressing, followed by sintering at 700 deg. C. The obtained material was evaluated by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) analyses. The biocompatibility evaluation of the formed glass was assessed through in vitro cell culture [alkaline phosphatase (AP) activity of osteoblasts] experiments and immersion studies in simulated body fluid (SBF) for different time intervals while monitoring the pH changes and the concentration of calcium, phosphorus and magnesium in the SBF medium. The SEM, XRD and FTIR studies were conducted before and after soaking of the material in SBF. At first, an amorphous calcium phosphate was formed; after 7 days this surface consisted of deposited crystalline apatite. The present investigation also revealed that the sol-gel derived quaternary bioglass system has the ability to support the growth of human fetal osteoblastic cells (hFOB 1.19). Finally, this material proved to be non-toxic and compatible for the proposed work in segmental defects in the goat model in vivo

  7. Poly(aniline) nanowires in sol-gel coated ITO: A pH-responsive substrate for planar supported lipid bilayers

    Ge, Chenhao; Orosz, Kristina S.; Armstrong, Neal R.; Saavedra, S. Scott

    2011-01-01

    Facilitated ion transport across an artificial lipid bilayer coupled to a solid substrate is a function common to several types of bioelectronic devices based on supported membranes, including biomimetic fuel cells and ion channel biosensors. Described here is fabrication of a pH-sensitive transducer composed of a porous sol-gel layer derivatized with poly(aniline) (PANI) nanowires grown from an underlying planar indium-tin oxide (ITO) electrode. The upper sol-gel surface is hydrophilic, smooth, and compatible with deposition of a planar supported lipid bilayer (PSLB) formed via vesicle fusion. Conducting tip AFM was used to show that the PANI wires are connected to the ITO, which convert this electrode into a potentiometric pH sensor. The response to changes in the pH of the buffer contacting the PANI nanowire/sol-gel/ITO electrode is blocked by the very low ion permeability of the overlying, fluid PSLB. The feasibility of using this assembly to monitor facilitated proton transport across the PSLB was demonstrated by doping the membrane with lipophilic ionophores that respond to a transmembrane pH gradient, which produced an apparent proton permeability several orders of magnitude greater than values measured for undoped lipid bilayers. PMID:21707069

  8. Effect of sol-age on the surface and optical properties of sol-gel derived mesoporous zirconia thin films

    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.

  9. 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.

    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

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

    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.

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

    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)

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

    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.

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

    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

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

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

    2015-10-28

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

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

    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

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

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

    2012-12-18

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

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

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

    1992-01-01

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

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

    Schmidt, Helmut

    1998-01-01

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

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

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

    2016-09-27

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

  20. Sol-gel synthesis of lanthanum-gallate-based ceramic coatings

    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

  1. Fundamental electrochemiluminescence characteristics of fluorine-doped tin oxides synthesized by sol-gel combustion.

    Moon, B H; Chaoumead, A; Sung, Y M

    2013-10-01

    Fluorine-doped tin oxide (FTO) materials synthesized by sol-gel combustion method were investigated for electrochemical luminescence (ECL) application. Effects of sol-gel combustion conditions on the structures and morphology of the porous FTO (p-FTO) materials were studied. ECL efficiency of p-FTO-based cell was about 251 cd/m2 at 4 V bias, which is higher than the sell using only FTO electrodes (102.8 cd/m2). The highest intensity of the emitting light was obtained at the wavelength of about 610 nm. The porous FTO layer was effective for increasing ECL intensities.

  2. Application of sol-gel process on the elaboration of SnO2 based ceramics

    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

  3. Micro- and nanostructured sol-gel-based materials for optical chemical sensing (2005–2015)

    Barczak, Mariusz; McDonagh, Colette; Wencel, Dorota

    2016-01-01

    This review (with 172 references) highlights the progress made in the past 10 years in silica sol-gel-based materials for use in optical chemical sensing. Following an introduction, the processes leading to the sol-gel-based and ormosil materials, their printability and methods for characterisation are discussed. Then various classes of optical sensors, with a focus on sensors for pH values, oxygen, carbon dioxide, ammonia (also in dissolved form), and heavy metal ions are described. A further section covers nanoparticle-based optical sensors mainly for use in intracellular sensing of the above species. Recent developments in this area are also emphasised and future trends discussed. (author)

  4. Positron annihilation lifetime studies of sol-gel transition of carrageenan gels

    Wakabayashi, Y.; Ito, K.; Li, H.L.; Ujihara, Y.

    1996-01-01

    Positron annihilation lifetime measurement was applied to study the sol-gel transition of anionic polysaccharide aqueous solutions in terms of free-volume parameters the size, intensity, and size distribution of free volumes of the gelation of K-form κ-carrageenan solutions as a function of temperature. Slight variations of free volume size and intensity against temperature were observed near 295 K. The correlation of free-volume data with other physical properties vibrational spectra (IR and Raman), conductivity, SAXS, elastic measurement, differential scanning calorimetry were investigated to understand the mechanism of sol-gel transition of carrageenan. (author)

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

    Stiegman, Albert E.

    1995-01-01

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

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

    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.

  7. Processing and mechanical behavior of Nicalon{reg_sign}/SiC composites with sol-gel derived oxide interfacial coatings

    Shanmugham, S.; Liaw, P.K. [Tennessee Univ., Knoxville, TN (United States). Dept. of Materials Science and Engineering

    1996-10-01

    Recent analytical and finite element modeling studies have indicated that low modulus interface materials are desirable for obtaining Nicalon/SiC composites with good toughness. Two oxides, Al titanate and mullite, were chosen on this basis as interface materials. The oxide and C coatings were deposited by sol-gel and CVD, respectively. Nicalon/SiC composites with oxide/C and C/oxide/C interfaces were fabricated and evaluated for flexure strength in the as-processed and oxidized conditions. Composites with C/oxide/C interfaces retained considerable strength and damage-tolerant behavior even after 500 h oxidation at 1000 C in air. The C/oxide/C interface shows promise as a viable oxidation-resistant interface alternative to C or BN interfaces.

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

    Xiaodong Wang

    2012-12-01

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

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

    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.

  10. The adhesion strength and residual stress of colloidal-sol gel derived β-Tricalcium-Phosphate/Fluoridated-Hydroxyapatite biphasic coatings

    Cheng Kui; Zhang, Sam; Weng Wenjian; Khor, Khiam Aik; Miao Shundong; Wang Yongsheng

    2008-01-01

    β-tricalcium phosphate (β-TCP) powders are embedded in a fluoridated hydroxyapatite (FHA) matrix to form β-TCP-FHA composites via colloidal-sol gel method. This composite layer is deposited on top of a FHA layer to form a β-TCP-FHA/FHA biphasic coating. The effect of the nanosized powder on the residual stress is characterized through the X-ray diffraction peak shift. The powder incorporation increases the residual stress, while a large amount of β-TCP (Ca powder /Ca sol ratio is higher than 1/2) results in less gel shrinkage that partially compensates the mismatch of thermal expansion coefficient and thus the residual stress. Despite the elevated residual stress as more powders are embedded, the coating adhesion strength remains virtually constant: around 430 mN-500 mN in scanning scratch test

  11. Characterization of nanocrystalline ZnO:Al films by sol-gel spin coating method

    Gareso, P. L., E-mail: pgareso@gmail.com; Rauf, N., E-mail: pgareso@gmail.com; Juarlin, E., E-mail: pgareso@gmail.com [Department of Physics, Faculty of Mathematics and Natural Sciences, Hasanuddin University, Makassar 90245 (Indonesia); Sugianto,; Maddu, A. [Department of Physics, Faculty of Mathematics and Natural Sciences, Bogor Institute of Culture, IPB Bogor (Indonesia)

    2014-09-25

    Nanocrystalline ZnO films doped with aluminium by sol-gel spin coating method have been investigated using optical transmittance UV-Vis and X-ray diffraction (X-RD) measurements. ZnO films were prepared using zinc acetate dehydrate (Zn(CH{sub 3}COO){sub 2}@@‡2H{sub 2}O), ethanol, and diethanolamine (DEA) as a starting material, solvent, and stabilizer, respectively. For doped films, AlCl{sub 3} was added to the mixture. The ZnO:Al films were deposited on a transparent conductive oxide (TCO) substrate using spin coating technique at room temperature with a rate of 3000 rpm in 30 sec. The deposited films were annealed at various temperatures from 400°C to 600°C during 60 minutes. The transmittance UV-Vis measurement results showed that after annealing at 400°C, the energy band gap profile of nanocrystalline ZnO:Al film was a blue shift. This indicated that the band gap of ZnO:Al increased after annealing due to the increase of crystalline size. As the annealing temperature increased the bandgap energy was a constant. In addition to this, there was a small oscillation occurring after annealing compared to the as–grown samples. In the case of X-RD measurements, the crystalinity of the films were amorphous before annealing, and after annealing the crystalinity became enhance. Also, X-RD results showed that structure of nanocrystalline ZnO:Al films were hexagonal polycrystalline with lattice parameters are a = 3.290 Å and c = 5.2531 Å.

  12. Studies of (3-mercaptopropyl)trimethoxylsilane and bis(trimethoxysilyl)ethane sol-gel coating on copper and aluminum.

    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.

  13. Improving the scratch resistance of sol-gel metal oxide coatings cured at 250 C through use of thermogenerated amines

    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

  14. On the healing mechanism of sol-gel derived hybrid materials containing dynamic di-sulfide bonds

    AbdolahZadeh, M.; Esteves, A.C.C.; Van der Zwaag, S.; Garcia Espallargas, S.J.

    2013-01-01

    Sol-gel technology is increasingly being used in coatings for corrosion protection and adhesion improvement. So far, the self-healing concept in sol-gel coatings has only been approached from extrinsic healing perspective (i.e. use of nano and micro carriers of corrosion inhibitors) [1]. Despite the

  15. Nanostructured sol-gel coatings doped with cerium nitrate as pre-treatments for AA2024-T3

    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

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

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

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

    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.

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

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

    2014-02-18

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

  19. Indirect rapid prototyping of sol-gel hybrid glass scaffolds for bone regeneration - Effects of organic crosslinker valence, content and molecular weight on mechanical properties.

    Hendrikx, Stephan; Kascholke, Christian; Flath, Tobias; Schumann, Dirk; Gressenbuch, Mathias; Schulze, F Peter; Hacker, Michael C; Schulz-Siegmund, Michaela

    2016-04-15

    We present a series of organic/inorganic hybrid sol-gel derived glasses, made from a tetraethoxysilane-derived silica sol (100% SiO2) and oligovalent organic crosslinkers functionalized with 3-isocyanatopropyltriethoxysilane. The material was susceptible to heat sterilization. The hybrids were processed into pore-interconnected scaffolds by an indirect rapid prototyping method, described here for the first time for sol-gel glass materials. A large panel of polyethylene oxide-derived 2- to 4-armed crosslinkers of molecular weights ranging between 170 and 8000Da were incorporated and their effect on scaffold mechanical properties was investigated. By multiple linear regression, 'organic content' and the 'content of ethylene oxide units in the hybrid' were identified as the main factors that determined compressive strength and modulus, respectively. In general, 3- and 4-armed crosslinkers performed better than linear molecules. Compression tests and cell culture experiments with osteoblast-like SaOS-2 cells showed that macroporous scaffolds can be produced with compressive strengths of up to 33±2MPa and with a pore structure that allows cells to grow deep into the scaffolds and form mineral deposits. Compressive moduli between 27±7MPa and 568±98MPa were obtained depending on the hybrid composition and problems associated with the inherent brittleness of sol-gel glass materials could be overcome. SaOS-2 cells showed cytocompatibility on hybrid glass scaffolds and mineral accumulation started as early as day 7. On day 14, we also found mineral accumulation on control hybrid glass scaffolds without cells, indicating a positive effect of the hybrid glass on mineral accumulation. We produced a hybrid sol-gel glass material with significantly improved mechanical properties towards an application in bone regeneration and processed the material into macroporous scaffolds of controlled architecture by indirect rapid prototyping. We were able to produce macroporous materials

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

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

    2015-01-01

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

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

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

    2015-01-01

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

  2. Influencia del tratamiento térmico sobre el espesor y porosidad de películas delgadas de ZrO2 obtenidas por la ruta sol-gel

    Caruso, R.

    2004-04-01

    Full Text Available The present work is aimed to investigate the thermal densification mechanisms of sol-gel zirconia thin films deposited by dip coating, with particular emphasis on thickness and porosity evolution at different firing treatments (100-1100ºC. For this purpose, we have only used data from transmission spectrum. Implications for controlled design of sol-gel zirconia films will be considered.El este trabajo se investigan los mecanismos de densificación de películas delgadas de zirconia obtenidas por vía sol-gel y depositadas mediante la técnica dip-coating. Nuestro interés se centra en la determinación del espesor y porosidad de películas tratadas a temperaturas en el rango 100-1100 ºC. Para ello, se ha utilizado exclusivamente la técnica de espectrofotometría. Los resultados de este trabajo tienen interés para el diseño controlado de recubrimientos sol-gel de ZrO2.

  3. Organization in sol-gel polymerization of methacrylate co-oligomers containing trimethoxysilylpropyl methacrylate

    Vraštil, J.; Matějka, Libor; Špaček, V.; Večeřa, M.; Prokůpek, L.

    2005-01-01

    Roč. 46, č. 25 (2005), s. 11232-11240 ISSN 0032-3861 Institutional research plan: CEZ:AV0Z40500505 Keywords : organic-inorganic hybrid * sol-gel process * oligomers Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.849, year: 2005

  4. Analysis and theory of gas transport in microporous sol-gel derived ceramic membranes

    de Lange, R.S.A.; de Lange, Rob; Keizer, Klaas; Burggraaf, Anthonie; Burggraaf, A.J.

    1995-01-01

    Sol-gel modification of mesoporous alumina membranes is a very successful technique to improve gas separation performance. Due to the formed microporous top layer, the membranes show activated transport and molecular sieve-like separation factors. This paper concentrates on the mechanism of

  5. Study of positron lifetime spectrum for Zn O varistor ceramics fabricated by Sol-gel route

    Li Xigui; Wei Shutao; Zhang Ruiying; Cheng Guosheng; Dai Xianqi; Zhang Jincang; Xing Huaimin

    2000-01-01

    An investigation of positron lifetime spectrum for ZnO varistor ceramics fabricated by Sol-gel route was carried out. The relationship between lifetime parameters and the densification and nonlinear coefficient α was given. The dependence of electrical properties on sintering temperature and duration was discussed

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

    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.

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

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

    1981-01-01

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

  8. Silica-Based Sol-Gel Coating on Magnesium Alloy with Green Inhibitors

    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.

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

    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.

  10. Sol-gel/hydrothermal synthesis of mixed metal oxide of Titanium and ...

    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 ...

  11. Influence of p H on optical properties of nano structure sol-gel-derived silica films

    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.

  12. Patterned transparent zinc oxide films produced by sol-gel embossing

    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.)

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

    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.

  14. Analysis of coupled mass transfer and sol-gel reaction in a two-phase system

    Castelijns, H.J.; Huinink, H.P.; Pel, L.; Zitha, P.L.J.

    2006-01-01

    The coupled mass transfer and chemical reactions of a gel-forming compound in a two-phase system were studied in detail. Tetra-methyl-ortho-silicate (TMOS) is often used as a precursor in sol-gel chemistry to produce silica gels in aqueous systems. TMOS can also be mixed with many hydrocarbons

  15. Nanocrystalline Ni-Zn ferrites prepared by sol-gel method

    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

  16. Sol-gel immobilization of serine proteases for application in organic solvents

    van Unen, D.J.; Engbersen, Johannes F.J.; Reinhoudt, David

    2001-01-01

    The serine proteases α-chymotrypsin, trypsin, and subtilisin Carlsberg were immobilized in a sol-gel matrix and the effects on the enzyme activity in organic media are evaluated. The percentage of immobilized enzyme is 90% in the case of α-chymotrypsin and the resulting specific enzyme activity in

  17. Sol-gel coatings of ceramic fibres for composites with ceramic matrix

    Maier, B.; Grathwohl, G.; Spallek, M.; Pannhorst, W.

    1992-01-01

    The aim of this work was to show the feasibility in principle of sol-gel coating of ceramic reinforcement components for composites from technical aspects as well. The complexity of the coating task rises with the transition from individual fibres to bundles of fibres of different thickness to weaves, and finally to composites. (orig.) [de

  18. The increase in pH during aging of porous sol-gel silica spheres

    Titulaer, M.K.; Kegel, W.K.; Jansen, J.B.H.; Geus, John W.

    1994-01-01

    The increase in pH in the hydrothermal fluid is studied after hydrothermal aging of porous silica gel spheres of 1–3 mm diameter. The porous silica spheres are formed by the sol-gel process from a supersaturated silica solution. The increase of the pH of the hydrothermal solution affects the silica

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

    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.

  20. Sol-gel coatings on large area glass sheets for electrochromic devices

    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

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

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

    1991-01-01

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

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

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

    2015-01-01

    A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification. PMID:26411484

  3. Gel stabilization in chelate sol-gel preparation of Bi-2223 superconductors

    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

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

    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.

  5. Epoxy-based organic-inorganic nanocomposite coatings and films prepared by sol-gel process

    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

  6. Supercritical fluid extraction of silicone oil from uranate microspheres prepared by sol-gel process

    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)

  7. Blade-coated sol-gel indium-gallium-zinc-oxide for inverted polymer solar cell

    Yan-Huei Lee

    2016-11-01

    Full Text Available The inverted organic solar cell was fabricated by using sol-gel indium-gallium-zinc-oxide (IGZO as the electron-transport layer. The IGZO precursor solution was deposited by blade coating with simultaneous substrate heating at 120 °C from the bottom and hot wind from above. Uniform IGZO film of around 30 nm was formed after annealing at 400 °C. Using the blend of low band-gap polymer poly[(4,8-bis-(2-ethylhexyloxy-benzo(1,2-b:4,5-b’dithiophene-2,6-diyl-alt- (4-(2-ethylhexanoyl-thieno [3,4-b]thiophene--2-6-diyl] (PBDTTT-C-T and [6,6]-Phenyl C71 butyric acid methyl ester ([70]PCBM as the active layer for the inverted organic solar cell, an efficiency of 6.2% was achieved with a blade speed of 180 mm/s for the IGZO. The efficiency of the inverted organic solar cells was found to depend on the coating speed of the IGZO films, which was attributed to the change in the concentration of surface OH groups. Compared to organic solar cells of conventional structure using PBDTTT-C-T: [70]PCBM as active layer, the inverted organic solar cells showed significant improvement in thermal stability. In addition, the chemical composition, as well as the work function of the IGZO film at the surface and inside can be tuned by the blade speed, which may find applications in other areas like thin-film transistors.

  8. Active corrosion protection of AA2024 by sol-gel coatings with corrosion inhibitors =

    Yasakau, Kiryl

    A industria aeronautica utiliza ligas de aluminio de alta resistencia para o fabrico dos elementos estruturais dos avioes. As ligas usadas possuem excelentes propriedades mecanicas mas apresentam simultaneamente uma grande tendencia para a corrosao. Por esta razao essas ligas necessitam de proteccao anticorrosiva eficaz para poderem ser utilizadas com seguranca. Ate a data, os sistemas anticorrosivos mais eficazes para ligas de aluminio contem cromio hexavalente na sua composicao, sejam pre-tratamentos, camadas de conversao ou pigmentos anticorrosivos. O reconhecimento dos efeitos carcinogenicos do cromio hexavalente levou ao aparecimento de legislacao banindo o uso desta forma de cromio pela industria. Esta decisao trouxe a necessidade de encontrar alternativas ambientalmente inocuas mas igualmente eficazes. O principal objectivo do presente trabalho e o desenvolvimento de pretratamentos anticorrosivos activos para a liga de aluminio 2024, baseados em revestimentos hibridos produzidos pelo metodo sol-gel. Estes revestimentos deverao possuir boa aderencia ao substrato metalico, boas propriedades barreira e capacidade anticorrosiva activa. A proteccao activa pode ser alcancada atraves da incorporacao de inibidores anticorrosivos no pretratamento. O objectivo foi atingido atraves de uma sucessao de etapas. Primeiro investigou-se em detalhe a corrosao localizada (por picada) da liga de aluminio 2024. Os resultados obtidos permitiram uma melhor compreensao da susceptibilidade desta liga a processos de corrosao localizada. Estudaram-se tambem varios possiveis inibidores de corrosao usando tecnicas electroquimicas e microestruturais. Numa segunda etapa desenvolveram-se revestimentos anticorrosivos hibridos organico-inorganico baseados no metodo sol-gel. Compostos derivados de titania e zirconia foram combinados com siloxanos organofuncionais a fim de obter-se boa aderencia entre o revestimento e o substrato metalico assim como boas propriedades barreira. Testes

  9. Characterization of ceramic sol-gel coatings as an alternative chemical conversion treatment on commercial carbon steel

    Dominguez-Crespo, M.A.; Garcia-Murillo, A.; Torres-Huerta, A.M.; Carrillo-Romo, F.J.; Onofre-Bustamante, E.; Yanez-Zamora, C.

    2009-01-01

    Sol-gel yttria-stabilized zirconia (YSZ) thin films were prepared on commercial carbon steel sheets by dip-coating technique followed by a low temperature heat treatment (473, 573, and 673 K for 1 h) in order to improve both corrosion properties and adhesion. For comparison, zirconia (ZrO 2 ) coatings have been also analyzed. Electrochemical techniques, Fourier Transform Infrared (FT-IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the anticorrosion behavior of the coatings in a 3.5 wt% NaCl solution. The adhesion with a polyester organic coating was evaluated by the pull-off technique. The typical thickness of the deposited layers ranged from 1 to 1.3 μm depending on process parameters. The obtained results indicated that sol-gel ZrO 2 and YSZ coatings without an organic coating can act as protective barriers against wet corrosion during the first hours, but they fail when the time exposure is longer than 1 day. However, when synthesized films were used as a pre-treatment and an organic coating was added (top-coated), the anticorrosive and adhesion properties were strongly affected by the temperature of the treatment, and an increase in both properties was observed at higher temperatures. The structural and morphological characteristics of the coating provide an explanation of the role of each film in the electrochemical behavior in this aggressive medium. Comparing both systems, YSZ displayed greater protective and adhesion values than exhibited for ZrO 2 which can be correlated with the stabilization of the cubic phase

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

    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.

  11. Iron specificity of a biosensor based on fluorescent pyoverdin immobilized in sol-gel glass

    2011-01-01

    Two current technologies used in biosensor development are very promising: 1. The sol-gel process of making microporous glass at room temperature, and 2. Using a fluorescent compound that undergoes fluorescence quenching in response to a specific analyte. These technologies have been combined to produce an iron biosensor. To optimize the iron (II or III) specificity of an iron biosensor, pyoverdin (a fluorescent siderophore produced by Pseudomonas spp.) was immobilized in 3 formulations of porous sol-gel glass. The formulations, A, B, and C, varied in the amount of water added, resulting in respective R values (molar ratio of water:silicon) of 5.6, 8.2, and 10.8. Pyoverdin-doped sol-gel pellets were placed in a flow cell in a fluorometer and the fluorescence quenching was measured as pellets were exposed to 0.28 - 0.56 mM iron (II or III). After 10 minutes of exposure to iron, ferrous ion caused a small fluorescence quenching (89 - 97% of the initial fluorescence, over the range of iron tested) while ferric ion caused much greater quenching (65 - 88%). The most specific and linear response was observed for pyoverdin immobilized in sol-gel C. In contrast, a solution of pyoverdin (3.0 μM) exposed to iron (II or III) for 10 minutes showed an increase in fluorescence (101 - 114%) at low ferrous concentrations (0.45 - 2.18 μM) while exposure to all ferric ion concentrations (0.45 - 3.03 μM) caused quenching. In summary, the iron specificity of pyoverdin was improved by immobilizing it in sol-gel glass C. PMID:21554740

  12. rhEGF-containing thermosensitive and mucoadhesive polymeric sol-gel for endoscopic treatment of gastric ulcer and bleeding.

    Maeng, Jin Hee; So, Jung Won; Kim, Jungju; Kim, In Ae; Jung, Ji Hoon; Min, Kyunghyun; Lee, Don Haeng; Yang, Su-Geun

    2014-03-01

    Gastrointestinal endoscopy is a standard diagnostic tool for gastrointestinal ulcers and cancer. In this study, we have developed recombinant human epidermal growth factor-containing ulcer-coating polymeric sol-gel for endoscopic application. Chitosan and pluronic F127 were employed for their thermoresponsive and bioadhesive properties. At temperatures below 21, polymeric sol-gel remains liquid during endoscopic application and transforms to gel at body temperature after application on ulcers. In an in vitro cellular wounding assay, recombinant human epidermal growth factor sol-gel significantly enhanced the cell migration and decreased the wounding area (68%) compared to nontreated, recombinant human epidermal growth factor solution, and sol-gel without recombinant human epidermal growth factor (42, 49, and 32 % decreased at day 1). The in vivo ulcer-healing study was performed in an acetic acid-induced gastric ulcer rat model and proved that our recombinant human epidermal growth factor endoscopic sol-gel facilitated the ulcer-healing process more efficiently than the other treatments. Ulcer sizes in the recombinant human epidermal growth factor sol-gel group were decreased 2.9- and 2.1-fold compared with those in the nontreated group on days 1 and 3 after ulceration, respectively. The mucosal thickness in the recombinant human epidermal growth factor sol-gel group was significantly increased compared to that in the nontreated group (3.2- and 6.9-fold on days 1 and 3 after ulceration, respectively). In a gastric retention study, recombinant human epidermal growth factor sol-gel stayed on the gastric mucosa more than 2 h after application. The present study suggests that recombinant human epidermal growth factor sol-gel is a prospective candidate for treating gastric ulcers via endoscopic application.

  13. Sol-gel processes and materials. November 1971-October 1989 (Citations from the US Patent data base). Report for November 1971-October 1989

    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.)

  14. Sol-gel processes and materials. January 1970-August 1989 (Citations from the US Patent data base). Report for January 1970-August 1989

    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.)

  15. A Urea Biosensor from Stacked Sol-Gel Films with Immobilized Nile Blue Chromoionophore and Urease Enzyme

    Alqasaimeh, Muawia Salameh; Heng, Lee Yook; Ahmad, Musa

    2007-01-01

    An optical urea biosensor was fabricated by stacking several layers of sol-gel films. The stacking of the sol-gel films allowed the immobilization of a Nile Blue chromoionophore (ETH 5294) and urease enzyme separately without the need of any chemical attachment procedure. The absorbance response of the biosensor was monitored at 550 nm, i.e. the deprotonation of the chromoionophore. This multi-layer sol-gel film format enabled higher enzyme loading in the biosensor to be achieved. The urea op...

  16. Homogenous smooth sol gel films doped with organic compounds for nonlinear optics

    Vasiliu, I.C. [INOE 2000 — National Institute for Optoelectronics, 409 Atomistilor Str., Magurele, Bucharest, RO 077125 (Romania); Ionita, I., E-mail: i_ionita@yahoo.com [UB — University of Bucharest, 405 Atomistilor Str., Magurele, Bucharest, RO 077125 (Romania); Matei, A. [INFLPR — National Institute for Laser, Plasma and Radiation Physics, 409 Atomistilor Str., Magurele, Bucharest, RO 077125 (Romania); Elisa, M.; Iordanescu, R.; Feraru, I.; Emandi, A. [INOE 2000 — National Institute for Optoelectronics, 409 Atomistilor Str., Magurele, Bucharest, RO 077125 (Romania)

    2016-02-29

    The demand for protection of various types of optical sensors from laser-beam pulses has resulted in the search for optical limiting devices that have the property of being transparent at low intensity of light (normal light), but no transparent towards high intensity (laser) light. Organic material with nonlinear optical (NLO) properties as reverse saturable absorption and two-photon absorption can be used for optical limiting with the advantage of a very fast response and self-activation. A promising approach in the fabrication of thin films by low cost/easy use deposition methods for second-order nonlinear optics is sol–gel technique. The present paper reports on the sol–gel synthesis of some pyrazolone derivative doped SiO{sub 2}–P{sub 2}O{sub 5} smooth and homogenous films (Root mean square roughness (Rq) = 1.1 nm) using as precursors tetraethylorthosilicate (TEOS) and phosphoric acid (H{sub 3}PO{sub 4}). The structure of the deposited azo-derivatives doped thin films was examined by Fourier transform infrared spectroscopy and atomic force microscopy, while their optical properties of the films by UV–VIS spectroscopy. The nonlinear optical efficiencies due to the interaction of the NLO-active chromophores with the inorganic matrix have a significant influence on the second harmonic generation capabilities that was measured using a femtosecond Ti:Sapphire laser. The properties of the films were investigated and correlated with the concentration of the organic dopant and the thermal treatment temperature. - Highlights: • We obtained pyrazolone derivative doped SiO{sub 2}–P{sub 2}O{sub 5} smooth and homogenous films. • The pyrazolone derivative presents SHG characteristics by itself. • Thin sol gel films doped with organic compounds with NLO properties. • Temperature of thermal treatment and aging time can improve NLO properties of films. • We found that 150 °C and 28 h aging time give the maximum performance in SHG response.

  17. Manufacture of amorphous and poly-crystalline materials with the sol-gel process; Fabricacion de materiales amorfos y policristalinos con la ruta sol-gel

    Castaneda-Contreras, J. [Centro Universitario de Los Lagos, Universidad de Guadalajara, Guadalajara, Jalisco (Mexico)

    2006-01-15

    The sun-gel process is a chemical route that allows the manufacture of amorphous and poly-crystalline materials in a relatively simple way. New materials can be obtained, materials that through the traditional manufacture methods, are very difficult to obtain, such as oxide combinations (SiO{sub 2}, TiO{sub 2}, ZrO{sub 2}, etc.), and that, when being produced by traditional methods, they run the risk of being contaminated with rare earth ions or organic dyes. The unique structures, micro- structures and compounds that can be made with the sun-gel process open many possibilities for practical applications, to name a few: the manufacture of optical components, preforms for optical fibers, dielectric coatings, superconductors, waveguides, nanoparticles, solar cells, etc. [Spanish] El proceso sol-gel es una ruta quimica que permite fabricar materiales amorfos y policristalinos de forma relativamente sencilla. Se pueden obtener nuevos materiales que a traves de los metodos tradicionales de fabricacion son muy dificiles de obtener, tales como combinaciones de oxidos (SiO{sub 2}, TiO{sub 2}, ZrO{sub 2}, etc.), y que, de ser producidos por metodos tradicionales corren el riesgo de contaminarse con iones de tierras raras o colorantes organicos. Las estructuras unicas, micro estructuras y compuestos que pueden hacerse con el proceso sol-gel abren muchas posibilidades para aplicaciones practicas, por nombrar algunas, la fabricacion de componentes opticos, preformas para fibras opticas, recubrimientos dielectricos, superconductores, guias de onda, nanoparticulas, celdas solares, etc.

  18. Porphyrinosilica and metalloporphyrinosilica: hybrid organic-inorganic materials prepared by sol-gel processing

    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.

  19. Innovative Formulation Combining Al, Zr and Si Precursors to Obtain Anticorrosion Hybrid Sol-Gel Coating

    Clément Genet

    2018-05-01

    Full Text Available The aim of our study is to improve the aluminium alloy corrosion resistance with Organic-Inorganic Hybrid (OIH sol-gel coating. Coatings are obtained from unusual formulation with precursors mixing: glycidoxypropyltrimethoxysilane (GPTMS, zirconium (IV propoxide (TPOZ and aluminium tri-sec-butoxide (ASB. This formulation was characterized and compared with sol formulations GPTMS/TPOZ and GPTMS/ASB. In each formulation, a corrosion inhibitor, cerium (III nitrate hexahydrate, is employed to improve the corrosion performance. Coatings obtained from sol based on GPTMS/TPOZ/ASB have good anti-corrosion performances with Natural Salt Spray (NSS resistance of 500 h for a thickness lower than 4 µm. Contact angle measurement showed a coating hydrophobic behaviour. To understand these performances, nuclear magnetic resonance (NMR analyses were performed, results make sol-gel coating condensation evident and are in very good agreement with previous results.

  20. Innovative Formulation Combining Al, Zr and Si Precursors to Obtain Anticorrosion Hybrid Sol-Gel Coating.

    Genet, Clément; Menu, Marie-Joëlle; Gavard, Olivier; Ansart, Florence; Gressier, Marie; Montpellaz, Robin

    2018-05-10

    The aim of our study is to improve the aluminium alloy corrosion resistance with Organic-Inorganic Hybrid (OIH) sol-gel coating. Coatings are obtained from unusual formulation with precursors mixing: glycidoxypropyltrimethoxysilane (GPTMS), zirconium (IV) propoxide (TPOZ) and aluminium tri-sec-butoxide (ASB). This formulation was characterized and compared with sol formulations GPTMS/TPOZ and GPTMS/ASB. In each formulation, a corrosion inhibitor, cerium (III) nitrate hexahydrate, is employed to improve the corrosion performance. Coatings obtained from sol based on GPTMS/TPOZ/ASB have good anti-corrosion performances with Natural Salt Spray (NSS) resistance of 500 h for a thickness lower than 4 µm. Contact angle measurement showed a coating hydrophobic behaviour. To understand these performances, nuclear magnetic resonance (NMR) analyses were performed, results make sol-gel coating condensation evident and are in very good agreement with previous results.

  1. Enhanced optical band-gap of ZnO thin films by sol-gel technique

    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.

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

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

    2018-02-15

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

  3. Synthesis and Characterization of Oxide Dispersion Strengthened Ferritic Steel via a Sol-Gel Route

    Sun Qinxing; Zhang Tao; Wang Xianping; Fang Qianfeng; Hu Jing; Liu Changsong

    2012-01-01

    Nanocrystalline oxide dispersion strengthened (ODS) ferritic steel powders with nominal composition of Fe-14Cr-3W-0.3Ti-0.4Y 2 O 3 are synthesized using sol-gel method and hydrogen reduction. At low reduction temperature the impurity phase of CrO is detected. At higher reduction temperature the impurity phase is Cr 2 O 3 which eventually disappears with increasing reduction time. A pure ODS ferritic steel phase is obtained after reducing the sol-gel resultant products at 1200°C for 3 h. The HRTEM and EDS mapping indicate that the Y 2 O 3 particles with a size of about 15 nm are homogenously dispersed in the alloy matrix. The bulk ODS ferritic steel samples prepared from such powders exhibit good mechanical performance with an ultimate tensile stress of 960 MPa.

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

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

    2009-01-01

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

  5. Sol gel based fiber optic sensor for blook pH measurement

    Grant, S. A.; Glass, R. S.

    1996-01-01

    This paper describes a fiber-optic pH sensor based upon sol-gel encapsulation of a self-referencing dye, seminaphthorhodamine-1 carboxylate (SNARF-1C). The simple sol-gel fabrication procedure and low coating leachability are ideal for encapsulation and immobilization of dye molecules onto the end of an optical fiber. A miniature bench-top fluorimeter system was developed for use with the optical fiber to obtain pH measurements. Linear and reproducible responses were obtained in human blood in the pH range 6.8 to 8.0, which encompasses the clinically-relevant range. Therefore, this sensor can be considered for in vivo use

  6. Porphyrinosilica and metalloporphyrinosilica: hybrid organic-inorganic materials prepared by sol-gel processing

    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.

  7. Zr alkoxide chain effect on the sol-gel synthesis of lithium metazirconate

    Pfeiffer, Heriberto; Bosch, Pedro; Bulbulian, Silvia

    2003-01-01

    Lithium metazirconate (Li 2 ZrO 3 ) was synthesized by the sol-gel method, using four different Zr alkoxides: zirconium ethoxide, zirconium iso-propoxide, zirconium propoxide and zirconium butoxide. The syntheses were made under two different catalytic regimes, acid and basic. The resulting powders were mixtures of Li 2 ZrO 3 and ZrO 2 . The best yield of Li 2 ZrO 3 (100%) was obtained when the sol-gel reaction was developed with lithium methoxide and zirconium ethoxide under acid catalysis regime. This study establishes that, for base-catalyzed reactions the ZrO 2 formation decreases when the alkyl-chain increases in the alkoxides. By contrast, for acid-catalyzed reactions the ZrO 2 formation increases as the alkyl-chain increases. Finally, when Zr propoxide and Zr iso-propoxide were used, the Li 2 ZrO 3 amounts were different due to steric effects

  8. Melting Behavior of Organic Nanocrystals Grown in Sol-gel Matrices

    Sanz, N.; Boudet, A.; Ibanez, A.

    2002-01-01

    We have characterized the thermal stability of organic nanocrystals grown in the pores of sol-gel matrices. The structure has been measured with transmission electron microscopy (TEM) analysis. Depending on the nature of organic molecules and sol-gel matrices, we have modified the dye-matrix interactions and the interfacial structure between nanocrystals and gel-glasses. When the dye-matrix interactions are weak (Van der Waals' bonds), the corresponding interfacial structure observed by TEM is sharp and the nanocrystals melt below the bulk melting point. On the other hand, when the dye-matrix interactions are strong (hydrogen bonds), the interfacial structure is fuzzy and a great superheating of organic nanocrystals is observed in comparison to the bulk melting point of the dye

  9. A sol-gel method to synthesize indium tin oxide nanoparticles

    Xiuhua Li; Xiujuan xu; Xin Yin; Chunzhong Li; Jianrong Zhang

    2011-01-01

    Transparent conductive indium tin oxide (ITO) nanoparticles were synthesized by a novel sol-gel method.Granulated indium and tin were dissolved in HNO3 and partially complexed with citric acid.A sol-gel process was induced when tertiary butyl alcohol was added dropwise to the above solution.ITO nanoparticles with an average crystallite size of 18.5 nm and surface area of 32.6 m2/g were obtained after the gel was heat-treated at 700 C.The ITO nanoparticles showed good sinterability,the starting sintering temperature decreased sharply to 900 C,and the 1400 C sintered pellet had a density of 98.1 % of theoretical density (TD).

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

    Tao, Shiquan; Singh, Jagdish P.; Winstead, Christopher B.

    2006-05-02

    An optical fiber moisture sensor that can be used to sense moisture present in gas phase in a wide range of concentrations is provided, as well techniques for making the same. The present invention includes a method that utilizes the light scattering phenomenon which occurs in a porous sol-gel silica by coating an optical fiber core with such silica. Thus, a porous sol-gel silica polymer coated on an optical fiber core forms the transducer of an optical fiber moisture sensor according to an embodiment. The resulting optical fiber sensor of the present invention can be used in various applications, including to sense moisture content in indoor/outdoor air, soil, concrete, and low/high temperature gas streams.

  11. Dissolution testing of intermediary products in uranium dioxide production by the sol-gel method

    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.)

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

    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.

  13. Optical characterization of Er-implanted ZnO films formed by sol-gel method

    Fukudome, T.; Kaminaka, A.; Isshiki, H.; Saito, R.; Yugo, S.; Kimura, T.

    2003-01-01

    In this paper, we report on the 1.54 μm photoluminescence (PL) of Er-implanted ZnO thin films formed by a sol-gel method on Si substrates. In spite of the polycrystalline structure of the sol-gel ZnO thin films, they showed strong PL emissions due to the near band edge recombination at 375 nm as well as the Er-related luminescence at 1.54 μm. The Er-related luminescence showed no decrease (quench) in the intensity up to the Er concentration of 1.5 x 10 21 cm -3 . The PL intensity of Er-implanted ZnO at 1.54 μm was found to be as strong as Er-doped PS (porous Si) at 20 K, and the intensity reduced to 1/3 at room temperature

  14. Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

    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.

  15. Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

    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.

  16. Comparative study of ZnO thin films prepared by different sol-gel route

    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.   

  17. Exploratory experiments on the feasibility of Th and Pu sol-gel particles

    Vanhellemont, G.; Beullens, J.; Bairiot, H.

    1965-05-01

    The sol-gel process as developed by the O.E.C.D. Dragon Project has been applied by the Plutonium Project at Mol to determine the feasibility of producing spherical particles containing Th02, Pu02 and C, in the proportions necessary to fabricate thorium-plutonium carbide kernels for irradiation specimens and for fuel cartridges for the Dragon Reactor Experiment. The process has been extended successfully to the preparation of thorium and plutonium gels, having a significant excess of carbon, with the object of evaluating the feasibility of the sol-gel process for the production of Th, C-10 type kernels. Other experiments have been performed to test the feasibility of incorporating U02 powder into the gel spheres. By using this technique, U to Th ratios of up to 9:1 have been obtained. (author)

  18. Microcontroller based instrumentation for the fuel pin preparation facility by sol-gel method

    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)

  19. Effect of sintering time at low temperature on the properties of IGZO TFTs fabricated by using the sol-gel process

    Choi, Jun Hyuk; Shim, Jong Hyun; Hwang, Soo Min

    2010-01-01

    We explored the application of the sol-gel process technique to the fabrication of InGaZnO (IGZO) thin film transistors (TFTs). We fabricated IGZO TFTs by using the sol-gel method and evaluated the effect of the sintering time on the electrical properties of the IGZO system with an atomic ratio of In:Ga:Zn = 2:1:1. In the process, IGZO precursor solutions were prepared by mixing In nitrate, Ga nitrate, and Zn acetate and were then deposited on a p-type Si-wafer covered with a thermally grown SiO 2 layer by spin-coating. The sintering process was performed for 3 h, 6 h or 12 h at 300 .deg. C in the ambient atmosphere. The source/drain electrodes of the TFT devices were fabricated using Al thermal evaporation. For all of the samples, a low off current (∼10 -1 1 A) and on-to-off current ratio (∼ 5 x 10 4 ) were obtained in their transfer curves. The saturation mobility increased with increasing sintering time: for the samples sintered for 3 h, 6 h and 12 h, the saturation mobilities were calculated to be 0.825 cm 2 /Vs, 1.65 cm 2 /Vs, and 2.06 cm 2 /Vs, respectively. Based on the XPS and TEM analyses, the enhancement of the mobility was attributed to the increase in the number of oxygen vacancies and the nanocrystalline structure in the amorphous matrix with increasing sintering time. These results demonstrate for the potential application of sol-gel processed IGZO devices on flexible polymer substrates.

  20. Sol-gel derived bioactive coating on zirconia: Effect on flexural strength and cell proliferation.

    Shahramian, Khalil; Leminen, Heidi; Meretoja, Ville; Linderbäck, Paula; Kangasniemi, Ilkka; Lassila, Lippo; Abdulmajeed, Aous; Närhi, Timo

    2017-11-01

    The purpose of this study was to evaluate the effect of sol-gel derived bioactive coatings on the biaxial flexural strength and fibroblast proliferation of zirconia, aimed to be used as an implant abutment material. Yttrium stabilized zirconia disc-shaped specimens were cut, ground, sintered, and finally cleansed ultrasonically in each of acetone and ethanol for 5 minutes. Three experimental groups (n = 15) were fabricated, zirconia with sol-gel derived titania (TiO 2 ) coating, zirconia with sol-gel derived zirconia (ZrO 2 ) coating, and non-coated zirconia as a control. The surfaces of the specimens were analyzed through images taken using a scanning electron microscope (SEM), and a non-contact tapping mode atomic force microscope (AFM) was used to record the surface topography and roughness of the coated specimens. Biaxial flexural strength values were determined using the piston-on-three ball technique. Human gingival fibroblast proliferation on the surface of the specimens was evaluated using AlamarBlue assay™. Data were analyzed using a one-way analysis of variance (ANOVA) followed by Tukey's post-hoc test. Additionally, the biaxial flexural strength data was also statistically analyzed with the Weibull distribution. The biaxial flexural strength of zirconia specimens was unaffected (p > 0.05). Weibull modulus of TiO 2 coated and ZrO 2 coated groups (5.7 and 5.4, respectively) were lower than the control (8.0). Specimens coated with ZrO 2 showed significantly lower fibroblast proliferation compared to other groups (p sol-gel derived coatings have no influence on the flexural strength of zirconia. ZrO 2 coated specimens showed significantly lower cell proliferation after 12 days than TiO 2 coated or non-coated control. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 2401-2407, 2017. © 2016 Wiley Periodicals, Inc.

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

    Kapusuz, Derya; Durucan, Caner

    2017-07-01

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

  2. Processing of non-oxide ceramics from sol-gel methods

    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.

  3. In situ ion-beam analysis and modification of sol-gel zirconia thin films

    Levine, T.E.; Mayer, J.W.

    1995-01-01

    We report the investigation of ion-beam-induced densification of sol-gel zirconia thin films via in situ ion backscattering spectrometry. We have irradiated three regions of a sample with neon, argon, and krypton ions. For each ion species, a series of irradiation and analysis steps were performed using an interconnected 3 MV tandem accelerator. The technique offers the advantages of minimizing the variation of experimental parameters and sequentially monitoring the densification phenomenon with increasing ion dose

  4. Performance of the sol-gel method for the preparation of optical fibers

    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

  5. Fabrications and properties of doped porous polysiloxane sol-gel layers on optical fibers

    Berková, Daniela; Sedlář, Miroslav; Matějec, Vlastimil; Kašík, Ivan; Chomát, Miroslav; Abdelghani, A.; Jaffrezic-Renault, N.; Lacroix, M.

    1998-01-01

    Roč. 13, 1/3 (1998), s. 569-573 ISSN 0928-0707. [Glasses, Ceramics, Hybrids and Nanocomposites from Gels - SOL-GEL'97 /9./. Sheffield, 31.08.1997-05.09.1997] R&D Projects: GA ČR GA102/95/0871; GA ČR GA102/96/0939 Keywords : nonelectric sensing devices * optical fibres Subject RIV: JB - Sensors, Measurment, Regulation Impact factor: 1.526, year: 1997

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

    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.

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

    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)

  8. Microstructure of Zirconia-Based Sol-Gel Glasses Studied by SANS

    Ryukhtin, Vasyl; Strunz, Pavel; Kopitsa, G. P.; Ezdakova, K. V.; Gubanova, N. N.; Ivanov, V. K.; Baranchikov, A. Y.; Angelov, Borislav; Feoktistov, A.; Pipich, V.; Levinský, P.

    2015-01-01

    Roč. 128, č. 4 (2015), s. 582-584 ISSN 0587-4246. [ISPMA 13 - 13th INTERNATIONAL SYMPOSIUM ON PHYSICS OF MATERIALS. Praha, 31.08.2014 - 04.09.2014] R&D Projects: GA ČR GB14-36566G; GA MŠk LM2011019 Institutional support: RVO:61389013 ; RVO:61389005 Keywords : sol-gel method * SANS * USANS Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.525, year: 2015

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

    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.

  10. Development of novel sol-gel indicators (SGI's) for in-situ environmental measurements

    Livingston, R.R.; Wicks, G.G.; Baylor, L.C.; Whitaker, M.J.

    1993-01-01

    Organic indicator molecules have been incorporated in a porous sol- gel matrix coated on the end of a fiber-optic lens assembly to create sensors for in situ environmental measurements. Probes have been made that are sensitive to pH and uranyl concentration. The use of fiber optics allows the probe to be lowered into a well or bore hole, while support equipment such as a spectrophotometer and computer may be situated hundreds of meters away

  11. Sol-gel-derived mesoporous silica films with low dielectric constants

    Seraji, S.; Wu, Yun; Forbess, M.; Limmer, S.J.; Chou, T.; Cao, Guozhong [Washington Univ., Seattle, WA (United States). Dept. of Materials Science and Engineering

    2000-11-16

    Mesoporous silica films with low dielectric constants and possibly closed pores have been achieved with a multiple step sol-gel processing technique. Crack-free films with approximately 50% porosity and 0.9 {mu}m thicknesses were obtained, a tape-test revealing good adhesion between films and substrates or metal electrodes. Dielectric constants remained virtually unchanged after aging at room temperature at 56% humidity over 6 days. (orig.)

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

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

    2011-01-01

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

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

    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.

  14. Acquisition of a Scanning Ultrasound Analyzer for Gelation and Drying Studies in Sol-Gel Ceramic Coatings and Monoliths

    Archer, Lynden

    1997-01-01

    The overall goal of this research project was to develop a fundamental understanding of how colloid chemistry influences structure and properties of ceramic monoliths fabricated by sol-gel synthesis...

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

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

    2016-08-25

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

  16. Modified thermoresponsive Poloxamer 407 and chitosan sol-gels as potential sustained-release vaccine delivery systems

    Kojarunchitt, Thunjiradasiree; Baldursdottir, Stefania; Dong, Yao-Da

    2015-01-01

    Thermoresponsive, particle-loaded, Poloxamer 407 (P407)-Pluronic-R® (25R4) or chitosan-methyl cellulose (MC) formulations were developed as single-dose, sustained release vaccines. The sol-gels, loaded either with a particulate vaccine (cubosomes) or soluble antigen (ovalbumin) and adjuvants (Quil...... the chitosan-MC sol-gels sustained the release of antigen up to at least 14 days after administration. The chitosan-MC sol-gels stimulated both cellular and humoral responses. The inclusion of cubosomes in the sol-gels did not provide a definitive beneficial effect. Further analysis of the formulations...... with small-angle X-ray scattering (SAXS) revealed that while cubosomes were stable in chitosan-MC gels they were not stable in P407-25R4 formulations. The reason for the mixed response to cubosome-loaded vehicles requires more investigation, however it appears that the cubosomes did not facilitate...

  17. Vanadium dioxide formed by the sol-gel process

    Potember, R.S.; Speck, K.R.; Hu, H.S.

    1990-01-01

    This patent describes a process for the deposition of a crystalline vanadium dioxide thin film. It comprises: providing a solution comprising a vanadium tetraalkoxide and solvent; allowing hydrolysis and condensation reactions to progressively form a homogeneous sol from the solution, applying a coating of the sol to the substrate; allowing a gel to form from the sol on the substrate by evaporating the solvent; dehydrating the gel by heat treatment under an inert atmosphere to form the crystalline vanadium dioxide film

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

    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.

  19. Sol-gel derived flexible silica aerogel as selective adsorbent for water decontamination from crude oil.

    Abolghasemi Mahani, A; Motahari, S; Mohebbi, A

    2018-04-01

    Oil spills are the most important threat to the sea ecosystem. The present study is an attempt to investigate the effects of sol-gel parameters on seawater decontamination from crude oil by use of flexible silica aerogel. To this goal, methyltrimethoxysilane (MTMS) based silica aerogels were prepared by two-step acid-base catalyzed sol-gel process, involving ambient pressure drying (APD) method. To investigate the effects of sol-gel parameters, the aerogels were prepared under two different acidic and basic pH values (i.e. 4 and 8) and varied ethanol/MTMS molar ratios from 5 to 15. The adsorption capacity of the prepared aerogels was evaluated for two heavy and light commercial crude oils under multiple adsorption-desorption cycles. To reduce process time, desorption cycles were carried out by using roll milling for the first time. At optimum condition, silica aerogels are able to uptake heavy and light crude oils with the order of 16.7 and 13.7, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Amperometric detector for gas chromatography based on a silica sol-gel solid electrolyte.

    Steinecker, William H; Miecznikowski, Krzysztof; Kulesza, Pawel J; Sandlin, Zechariah D; Cox, James A

    2017-11-01

    An electrochemical cell comprising a silica sol-gel solid electrolyte, a working electrode that protrudes into a gas phase, and reference and counter electrodes that contact the solid electrolyte comprises an amperometric detector for gas chromatography. Under potentiostatic conditions, a current related to the concentration of an analyte in the gas phase is produced by its oxidation at the three-phase boundary among the sol-gel, working electrode, and the gas phase. The sol-gel is processed to contain an electrolyte that also serves as a humidistat to maintain a constant water activity even in the presence the gas chromatographic mobile phase. Response was demonstrated toward a diverse set of analytes, namely hydrogen, 1,2-ethandithiol, phenol, p-cresol, and thioanisole. Using flow injection amperometry of hydrogen with He as the carrier gas, 90% of the steady-state current was achieved in < 1s at a flow rate of 20mLmin -1 . A separation of 1,2-ethandithiol, phenol, p-cresol, and thioanisole at a 2.2mLmin -1 flow rate was achieved with respective detection limits (k = 3 criterion) of 4, 1, 3, and 70 ppmv when the working electrode potential was 800mV. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    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.

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

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

    2006-01-01

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

  3. Effect of Precursor Concentration of MgO nanostructure by using Sol-Gel Method

    V.T. Srisuvetha

    2017-04-01

    Full Text Available MgO thin flims have been prepared on substrates by a novel and simple sol-gel method using magnesium nitrate and collusion as starting material.The MgO nano catalyst with good sensor crystallization were obtained after annealing at 100°C Magnesium oxide was prepared by sol-gel method. The method involves the hydrolysis of magnesium alkoxide in the presence of acid or basic catalysts followed by a Oxalic acid reaction. The synthesized solids were characterized by IR spectroscopy X-ray diffraction electron microscopy. Ultraviolet visible absorbance measurement photoluminescence and Raman scattering spectra. X-ray diffraction (XRD characterization showed the formation of smaller particles after sol gel irradiation the structure and morphology of the MgO particles were analyzed byXRD. These articles were used for FTIR spectroscopic measurement and spectra were collected. In EDS we calculated the peak intensity the SEM the images of metal oxide.UV (Ultra Violet refers to adsorption spectroscopy optical properties of assorption, band gap energy.This means if use light in the visible and adjacent ranges.

  4. Colloidal sol-gel synthesis of oxides: application to the precursors of nuclear fuels

    Gossard, Alban

    2014-01-01

    One of the main objectives for the future nuclear fuel cycle is the recycling of the minor actinides. Different options are considered: their integration into a new fuel for a prospect of a closed fuel cycle or their transmutation in order to significantly decrease the long-term radiotoxicity of ultimate wastes. In both cases, the synthesis of new advanced materials integrating the actinides jointly is required. Sol-gel processes allow the organization of the material at the colloidal scale or the insertion of controlled porosity using 'templates'. Furthermore, the possibility to work in a 'wet environment' prevents the formation of pulverulent powders which are contaminant in the case of materials incorporating radioactive elements. The main purpose of this work is to demonstrate the adaptability of this route to the nuclear field. Firstly, a methodology of synthesis from a colloidal sol-gel route was set up on a non-radioactive zirconium-based system in order to characterize and understand of the different mechanisms of this synthesis. Then, studies on shaping, including insertion of porosity, were performed. Zirconia monoliths have been obtained thanks to a coupling between a colloidal sol-gel process and the formation of an emulsion stabilized by clusters of solid particles. Finally, a transposition of this work to an uranium-based system was introduced, pointing out different promising perspectives specially concerning the possibilities of shaping of the final material. (author) [fr

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

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

    2006-01-01

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

  6. MICROSTRUCTURE CHARACTERISTIC OF ALUMINUM TITANATE SYNTHESIED BY BOTH SOLID- STATE AND SOL-GEL PROCESSES

    M. Khosravi Saghezchi

    2015-12-01

    Full Text Available A comparing study on formation and microstructure features of aluminum titanate is investigated through both solid-state and sol-gel processes. Aluminum titanate formed by firing at 1350ºC and 1450ºC for 4h in solid-state process. In the sol-gel process formation of submicron sized particles is followed by addition of sucrose into the transparent sol. XRD analysis was confirmed the formation of aluminum titanate at 1400ºC  in lower duration of calcination (3h without any additives in the sol-gel process. In this work 2wt% MgO is added to the samples as the additive for forming acceleration of aluminum titanate. The influence of MgO addition and heat treatment are studied on phase formation and microstructure development of aluminum titanate in both procedures. Additive optimizes aluminum titanate formation at lower temperatures (1300-1350ºC. Phase and microstructure studies of Mg containing samples optimally show significance in aluminum titanate formation.

  7. Antioxidant Sol-Gel Improves Cutaneous Wound Healing in Streptozotocin-Induced Diabetic Rats

    Lee, Yen-Hsien; Chang, Jung-Jhih; Chien, Chiang-Ting; Yang, Ming-Chien; Chien, Hsiung-Fei

    2012-01-01

    We examined the effects of vitamin C in Pluronic F127 on diabetic wound healing. Full-thickness excision skin wounds were made in normal and diabetic Wistar rats to evaluate the effect of saline, saline plus vitamin C (antioxidant sol), Pluronic F127, or Pluronic F127 plus vitamin C (antioxidant sol-gel). The rate of wound contraction, the levels of epidermal and dermal maturation, collagen synthesis, and apoptosis production in the wound tissue were determined. In vitro data showed that after 6 hours of air exposure, the order of the scavenging abilities for HOCl, H2O2, and O2  − was antioxidant sol-gel > antioxidant saline > Pluronic F127 = saline. After 7 and 14 days of wound injury, the antioxidant sol-gel improved wound healing significantly by accelerated epidermal and dermal maturation, an increase in collagen content, and a decrease in apoptosis formation. However, the wounds of all treatments healed mostly at 3 weeks. Vitamin C in Pluronic F127 hastened cutaneous wound healing by its antioxidant and antiapoptotic mechanisms through a good drug delivery system. This study showed that Pluronic F127 plus vitamin C could potentially be employed as a novel wound-healing enhancer. PMID:22919368

  8. Sol-Gel Material-Enabled Electro-Optic Polymer Modulators

    Himmelhuber, Roland; Norwood, Robert A.; Enami, Yasufumi; Peyghambarian, Nasser

    2015-01-01

    Sol-gels are an important material class, as they provide easy modification of material properties, good processability and are easy to synthesize. In general, an electro-optic (EO) modulator transforms an electrical signal into an optical signal. The incoming electrical signal is most commonly information encoded in a voltage change. This voltage change is then transformed into either a phase change or an intensity change in the light signal. The less voltage needed to drive the modulator and the lower the optical loss, the higher the link gain and, therefore, the better the performance of the modulator. In this review, we will show how sol-gels can be used to enhance the performance of electro-optic modulators by allowing for designs with low optical loss, increased poling efficiency and manipulation of the electric field used for driving the modulator. The optical loss is influenced by the propagation loss in the device, as well as the losses occurring during fiber coupling in and out of the device. In both cases, the use of sol-gel materials can be beneficial due to the wide range of available refractive indices and low optical attenuation. The influence of material properties and synthesis conditions on the device performance will be discussed. PMID:26225971

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

    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.

  10. Determination of Insulator-to-Semiconductor Transition in Sol-Gel Oxide Semiconductors Using Derivative Spectroscopy.

    Lee, Woobin; Choi, Seungbeom; Kim, Kyung Tae; Kang, Jingu; Park, Sung Kyu; Kim, Yong-Hoon

    2015-12-23

    We report a derivative spectroscopic method for determining insulator-to-semiconductor transition during sol-gel metal-oxide semiconductor formation. When an as-spun sol-gel precursor film is photochemically activated and changes to semiconducting state, the light absorption characteristics of the metal-oxide film is considerable changed particularly in the ultraviolet region. As a result, a peak is generated in the first-order derivatives of light absorption ( A' ) vs. wavelength (λ) plots, and by tracing the peak center shift and peak intensity, transition from insulating-to-semiconducting state of the film can be monitored. The peak generation and peak center shift are described based on photon-energy-dependent absorption coefficient of metal-oxide films. We discuss detailed analysis method for metal-oxide semiconductor films and its application in thin-film transistor fabrication. We believe this derivative spectroscopy based determination can be beneficial for a non-destructive and a rapid monitoring of the insulator-to-semiconductor transition in sol-gel oxide semiconductor formation.

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

    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

  12. Fabrication and characterization of sol-gel based nanoparticles for drug delivery

    Yadav, Reeta

    Nanogels are cross linked polymeric sol-gel based nanoparticles that offer an interior network for incorporation and protection of biomolecules, exhibiting unique advantages for polymer based delivery systems. We have successfully synthesized stable sol-gel nanoparticles by means of [a] silicification reactions using cationic peptides like polylysine as gelating agents, and [b] lyophilization of sol-gels. Macromolecules such as Hemoglobin and Glucose Oxidase and small molecules such as Sodium Nitroprusside (SNP) and antibiotics were encapsulated within the nanogels. We have used transmission electron microscopy, dynamic light scattering, zeta potential analysis, and spectroscopy to perform a physicochemical characterization of the nanogels resulting from the two approaches. Our studies have indicated that the nanogel encapsulated proteins and small molecules remain intact, stable and functional. A Hydrogen Peroxide (H2O2) and Nitric Oxide (NO) generating drug carrier was synthesized using these nanogels and the effect of generation of H2O2 from Glucose Oxidase encapsulated nanogels and NO from SNP encapsulated nanogels was tested on E.coli. The results show that the nanoparticles exert antimicrobial activity against E.Coli, in addition NO generating nanogels potentiated H2O2 generating nanogels induced killing. These data suggest that these NO and H2O2 releasing nanogels have the potential to serve as a novel class of antimicrobials for the treatment of multidrug resistant bacteria. The unique properties of these protein/drug incorporated nanogels raise the prospect of fine tailoring to specific applications such as drug delivery and bio imaging.

  13. Hybrid titanium dioxide/PS-b-PEO block copolymer nanocomposites based on sol-gel synthesis

    Gutierrez, J; Tercjak, A; Garcia, I; Peponi, L; Mondragon, I

    2008-01-01

    The poly(styrene)-b-poly(ethylene oxide) (SEO) amphiphilic block copolymer, with two different molecular weights, has been used as a structure directing agent for generating nanocomposites of TiO 2 /SEO via the sol-gel process. SEO amphiphilic block copolymers are designed with a hydrophilic PEO-block which can interact with inorganic molecules, as well as a hydrophobic PS-block which builds the matrix. The addition of different amounts of sol-gel provokes strong variations in the self-assembled morphology of TiO 2 /SEO nanocomposites with respect to the neat block copolymer. As confirmed by atomic force microscopy (AFM), TiO 2 /PEO-block micelles get closer, forming well-ordered spherical domains, in which TiO 2 nanoparticles constitute the core surrounded by a corona of PEO-blocks. Moreover, for 20 vol% sol-gel the generated morphology changes to a hexagonally ordered structure for both block copolymers. The cylindrical structure of these nanocomposites has been confirmed by the two-dimensional Fourier transform power spectrum of the corresponding AFM height images. Affinity between titanium dioxide precursor and PEO-block of SEO allows us to generate hybrid inorganic/organic nanocomposites, which retain the optical properties of TiO 2 , as evaluated by UV-vis spectroscopy

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

    Samanidou, Victoria; Kehagia, Maria; Kabir, Abuzar; Furton, Kenneth G

    2016-03-31

    Highly selective and efficient chloramphenicol imprinted sol-gel silica based inorganic polymeric sorbent (sol-gel MIP) was synthesized via matrix imprinting approach for the extraction of chloramphenicol in milk. Chloramphenicol was used as the template molecule, 3-aminopropyltriethoxysilane (3-APTES) and triethoxyphenylsilane (TEPS) as the functional precursors, tetramethyl orthosilicate (TMOS) as the cross-linker, isopropanol as the solvent/porogen, and HCl as the sol-gel catalyst. Non-imprinted sol-gel polymer (sol-gel NIP) was synthesized under identical conditions in absence of template molecules for comparison purpose. Both synthesized materials were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and nitrogen adsorption porosimetry, which unambiguously confirmed their significant structural and morphological differences. The synthesized MIP and NIP materials were evaluated as sorbents for molecularly imprinted solid phase extraction (MISPE) of chloramphenicol in milk. The effect of critical extraction parameters (flow rate, elution solvent, sample and eluent volume, selectivity coefficient, retention capacity) was studied in terms of retention and desorption of chloramphenicol. Competition and cross reactivity tests have proved that sol-gel MIP sorbent possesses significantly higher specific retention and enrichment capacity for chloramphenicol compared to its non-imprinted analogue. The maximum imprinting factor (IF) was found as 9.7, whereas the highest adsorption capacity of chloramphenicol by sol-gel MIP was 23 mg/g. The sol-gel MIP was found to be adequately selective towards chloramphenicol to provide the necessary minimum required performance limit (MRPL) of 0.3 μg/kg set forth by European Commission after analysis by LC-MS even without requiring time consuming solvent evaporation and sample reconstitution step, often considered as an integral part in solid phase extraction work-flow. Intra and

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

    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.

  16. Structure/Property Relationships for Sol-gel Derived YBa2Cu3O7-d and SrTiO3 Films

    Dawley, Jeff; Clem, Paul; Siegal, Michael; Overmyer, Don

    2001-03-01

    Solution deposition of c-axis oriented YBa2Cu3O7-d (YBCO) films on buffered RABiT substrates is a potential method for rapid, low cost production of superconducting tapes for power transmission and other applications. For this work, 100-250 nm thick YBCO and SrTiO3 (STO) films have been prepared by spin-coating and dip-coating sol-gel solutions onto LaAlO3 (100) and RABiT Ni (200) substrates. Biaxially textured STO coatings have been deposited on LaAlO3 and RABiT Ni by using a "templating" technique and controlling growth temperature and pO2. YBCO films grown on STO coated LaAlO3 possess comparable superconducting properties to YBCO films grown directly on LaAlO3 ( 1 MA/cm2 at 77K), indicating that a high quality STO layer does not degrade the crystalline quality of the YBCO. The effects of processing parameters on the STO buffer layer and novel processing techniques for decreasing the processing time and simplifying the integration of sol-gel YBCO with Ni substrates will be discussed. Sandia is a multiprogram laboratory operated by Sandia Corp., a Lockheed Martin Company, for the US Dept. Of Energy under contract DE-AC04-94A185000.

  17. Co3O4/TiO2 films obtained by laser ablation and sol-gel for the reaction of oxygen liberation in alkaline medium

    Perez A, J.; Fernandez V, S. M.; Escobar A, L.; Jimenez B, J.

    2008-01-01

    The laser ablation technique known as Pulsed Laser Deposition (PLD) is used for obtaining thin films of TiO 2 /SnO 2 , which was later modified with Co 3 O 4 by PLD or by sol-gel technique. The films were characterized by X-ray diffraction, ultraviolet Vis and Raman spectroscopies, scanning electron microscopy and energy analysis of the dispersed X-rays produced by Auger decay. The anatase phase with particles of nano metric size was obtained by depositing the titanium dioxide in argon atmosphere. The Co 3 O 4 films obtained by PLD on the TiO 2 showed the same morphology. The electrocatalytic activity of the films that were used as photo anodes for the reaction of oxygen liberation was carried out in the darkness, with environment light and the light emitted by a xenon lamp. The current density was higher for films of Co 3 O 4 /TiO 2 /SnO 2 obtained by PLD that for cobalt dioxide of mixed valence obtained by sol-gel. (Author)

  18. Scratch resistance of SiO2 and SiO2 - ZrO2 sol-gel coatings on glass-ceramic obtained by sintering

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

    2013-01-01

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

  19. Photocatalytic Graphene-TiO2 Thin Films Fabricated by Low-Temperature Ultrasonic Vibration-Assisted Spin and Spray Coating in a Sol-Gel Process

    Fatemeh Zabihi

    2017-05-01

    Full Text Available In this work, we communicate a facile and low temperature synthesis process for the fabrication of graphene-TiO2 photocatalytic composite thin films. A sol-gel chemical route is used to synthesize TiO2 from the precursor solutions and spin and spray coating are used to deposit the films. Excitation of the wet films during the casting process by ultrasonic vibration favorably influences both the sol-gel route and the deposition process, through the following mechanisms. The ultrasound energy imparted to the wet film breaks down the physical bonds of the gel phase. As a result, only a low-temperature post annealing process is required to eliminate the residues to complete the conversion of precursors to TiO2. In addition, ultrasonic vibration creates a nanoscale agitating motion or microstreaming in the liquid film that facilitates mixing of TiO2 and graphene nanosheets. The films made based on the above-mentioned ultrasonic vibration-assisted method and annealed at 150 °C contain both rutile and anatase phases of TiO2, which is the most favorable configuration for photocatalytic applications. The photoinduced and photocatalytic experiments demonstrate effective photocurrent generation and elimination of pollutants by graphene-TiO2 composite thin films fabricated via scalable spray coating and mild temperature processing, the results of which are comparable with those made using lab-scale and energy-intensive processes.

  20. Sol-Gel Entrapped Levonorgestrel Antibodies: Activity and Structural Changes as a Function of Different Polymer Formats

    Shalev, Moran; Miriam, Altstein

    2011-01-01

    The paper describes development of a sol-gel based immunoaffinity method for the steroid hormone levonorgestrel (LNG) and the effects of changes in the sol-gel matrix format on the activity of the entrapped antibodies (Abs) and on matrix structure. The best sol-gel format for Ab entrapment was found to be a tetramethoxysilane (TMOS) based matrix at a TMOS:water ratio of 1:8, containing 10% polyethylene glycol (PEG) of MW 0.4 kDa. Addition of higher percentages of PEG or a higher MW PEG did not improve activity. No activity was obtained with a TMOS:water ratio of 1:12, most likely because of the very dense polymer that resulted from these polymerization conditions. Only minor differences in the non-specific binding were obtained with the various formats. TMOS was found to be more effective than tetrakis (2-hydroxyethyl)orthosilicate (THEOS) for entrapment of anti-levonorgestrel (LNG) Abs. However, aging the THEOS-based sol-gel for a few weeks at 4 °C stabilized the entrapped Abs and increased its binding capacity. Confocal fluorescent microscopy with fluorescein isothiocyanate (FITC) labeled immunoglobulines (IgGs) entrapped in the sol-gel matrix showed that the entrapped Abs were distributed homogenously within the gel. Scanning electron microscopy (SEM) images have shown the diverse structures of the various sol-gel formats and precursors. PMID:28880001

  1. Study of Optical Humidity Sensing Properties of Sol-Gel Processed TiO2 and MgO Films

    B. C. Yadav

    2007-04-01

    Full Text Available Paper reports a comparative study of humidity sensing properties of TiO2 and MgO films fabricated by Sol-gel technique using optical method. One sensing element of the optical humidity sensor presented here consists of rutile structured two-layered TiO2 thin film deposited on the base of an isosceles glass prism. The other sensing element consists of a film of MgO deposited by same technique on base of the prism. Light from He-Ne laser enters prism from one of refracting faces of the prism and gets reflected from the glass-film interface, before emerging out from its other isosceles face. This emergent beam is allowed to pass through an optical fiber. Light coming out from the optical fiber is measured with an optical power meter. Variations in the intensity of light caused by changes in humidity lying in the range 5%RH to 95%RH have been recorded. MgO film shows better sensitivity than TiO2 film.

  2. Structural, optical and magnetic properties of nanocrystalline Co-doped ZnO thin films grown by sol-gel

    Kayani, Zohra Nazir; Shah, Iqra; Zulfiqar, Bareera; Sabah, Aneeqa [Lahore College for Women Univ., Lahore (Pakistan); Riaz, Saira; Naseem, Shahzad [Univ. of the Punjab, Lahore (Pakistan). Centre of Excellence in Solid State Physics

    2018-04-01

    Cobalt-doped ZnO thin films have been deposited using a sol-gel route by changing the number of coats on the substrate from 6 to 18. This project deals with various film thicknesses by increasing the number of deposited coats. The effect of thickness on structural, magnetic, surface morphology and optical properties of Co-doped ZnO thin film was studied. The crystal structure of the Co-doped ZnO films was investigated by X-ray diffraction. The films have polycrystalline wurtzite hexagonal structures. A Co{sup 2+} ion takes the place of a Zn{sup 2+} ion in the lattice without creating any distortion in its hexagonal wurtzite structure. An examination of the optical transmission spectra showed that the energy band gap of the Co-doped ZnO films increased from 3.87 to 3.97 eV with an increase in the number of coatings on the substrate. Ferromagnetic behaviour was confirmed by measurements using a vibrating sample magnetometer. The surface morphology of thin films was assessed by scanning electron microscope. The grain size on the surface of thin films increased with an increase in the number of coats.

  3. Optical Properties of Sol-Gel Nb2O5 Films with Tunable Porosity for Sensing Applications

    Rosen Georgiev

    2015-01-01

    Full Text Available Thin Nb2O5 films with tunable porosity are deposited by the sol-gel and evaporation induced self-assembly methods using organic template Pluronic PE6100 with different molar fractions with respect to NbCl5 used as a precursor for synthesis of Nb sol. Surface morphology and structure of the films are studied by Transmission Electron Microscopy and Selected Area Electron Diffraction. The optical characterization of the films is carried out through reflectance spectra measurements of the films deposited on silicon substrates and theoretical modeling in order to obtain refractive index, extinction coefficient, and thickness of the films. The overall porosity of the films and the amount of adsorbed acetone vapors in the pores are quantified by means of Bruggeman effective medium approximation using already determined optical constants. The sensing properties of the samples are studied by measuring both the reflectance spectra and room-temperature photoluminescence spectra prior to and after exposure to acetone vapors and liquid, respectively. The potential of using the studied mesoporous Nb2O5 films for chemooptical sensing is demonstrated and discussed.

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

    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.

  5. Methods for and products of processing nanostructure nitride, carbonitride and oxycarbonitride electrode power materials by utilizing sol gel technology for supercapacitor applications

    Huang, Yuhong; Wei, Oiang; Chu, Chung-tse; Zheng, Haixing

    2001-01-01

    Metal nitride, carbonitride, and oxycarbonitride powder with high surface area (up to 150 m.sup.2 /g) is prepared by using sol-gel process. The metal organic precursor, alkoxides or amides, is synthesized firstly. The metal organic precursor is modified by using unhydrolyzable organic ligands or templates. A wet gel is formed then by hydrolysis and condensation process. The solvent in the wet gel is then be removed supercritically to form porous amorphous hydroxide. This porous hydroxide materials is sintered to 725.degree. C. under the ammonia flow and porous nitride powder is formed. The other way to obtain high surface area nitride, carbonitride, and oxycarbonitride powder is to pyrolyze polymerized templated metal amides aerogel in an inert atmosphere. The electrochemical capacitors are prepared by using sol-gel prepared nitride, carbonitride, and oxycarbonitride powder. Two methods are used to assemble the capacitors. Electrode is formed either by pressing the mixture of nitride powder and binder to a foil, or by depositing electrode coating onto metal current collector. The binder or coating is converted into a continuous network of electrode material after thermal treatment to provide enhanced energy and power density. Liquid electrolyte is soaked into porous electrode. The electrochemical capacitor assembly further has a porous separator layer between two electrodes/electrolyte and forming a unit cell.

  6. Grafting the sol-gel based sorbents by diazonium salts: a novel approach toward unbreakable capillary microextraction.

    Bagheri, Habib; Bayat, Parisa; Piri-Moghadam, Hamed

    2013-11-29

    The present work deals with a novel approach for grafting a sol-gel based sorbent, using diazonium salts for preparation of an unbreakable capillary microextraction (CME) device in on-line combination with high performance liquid chromatography (HPLC). The use of diazonium salts modifier allowed all types of metallic and non-metallic substrates to be used without any limitation. Substrates including copper, brass, stainless steel and polytetrafluoroethylene (PTFE) were chosen to be functionalized by chemical or electrochemical reduction of 4-amino phenyl acetic acid. Then, 3-(trimethoxysilyl)propylamine (3TMSPA) was selected as the precursor and the only reagent for preparation of the desired surface chemical bonded sorbent. The presence of chemical bond between substrate, diazonium salts and 3TMSPA is more probably responsible for thermal and solvent stability and long lifetime of the prepared sorbent. Characterization of the aryl group formation on the various substrates along with the prepared sorbents was thoroughly investigated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and thermogravimetry analysis (TGA). Typically, one of the prepared sorbents, deposited on the inner surface of the copper tube, was selected for assessing the developed method. The CME device was used for on-line extraction of atrazine, ametryn and terbutryn, as model compounds, from the aquatic media. After extraction, the HPLC mobile phase was used for on-line desorption and elution of the extracted analytes from the CME loop, containing the grafted sol-gel based sorbent, through the HPLC column. Figures of merit of the developed method were also obtained in which the linearity for the analytes was in the range of 30-1000μgL(-1). The value of LOD (S/N=3) for all analytes was 10μgL(-1) and the RSD% values (n=5) were all below 9.4% at the 500μgL(-1) level. Applicability of the developed method was examined by analyzing some real water samples in

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

    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.

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

    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.

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

    Haruvy, Yair; Liedtke, Volker

    2003-09-01

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

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

    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

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

    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)

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

    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.

  13. Optimization of sol-gel technique for coating of metallic substrates by hydroxyapatite using the Taguchi method

    Pourbaghi-Masouleh, M.; Asgharzadeh, H.

    2013-08-01

    In this study, the Taguchi method of design of experiment (DOE) was used to optimize the hydroxyapatite (HA) coatings on various metallic substrates deposited by sol-gel dip-coating technique. The experimental design consisted of five factors including substrate material (A), surface preparation of substrate (B), dipping/withdrawal speed (C), number of layers (D), and calcination temperature (E) with three levels of each factor. An orthogonal array of L18 type with mixed levels of the control factors was utilized. The image processing of the micrographs of the coatings was conducted to determine the percentage of coated area ( PCA). Chemical and phase composition of HA coatings were studied by XRD, FT-IR, SEM, and EDS techniques. The analysis of variance (ANOVA) indicated that the PCA of HA coatings was significantly affected by the calcination temperature. The optimum conditions from signal-to-noise ( S/N) ratio analysis were A: pure Ti, B: polishing and etching for 24 h, C: 50 cm min-1, D: 1, and E: 300 °C. In the confirmation experiment using the optimum conditions, the HA coating with high PCA of 98.5 % was obtained.

  14. Investigation of Electrical, Optical and GaS Sensing properties Sol-Gel Derived WO3 Thin Films

    Dumludag, F.

    2008-01-01

    Tungsten oxide (WO 3 ) is a wide band gap n-type semiconductor. Thin films of WO 3 are considerable interest because of their potential applications in electrochromic devices, and gas sensors. In this work, WO 3 thin films were deposited on IDT (Interdigital electrodes) by a sol-gel dipping process. Precursor solution was prepared by dissolving of tungstic acid in ammonia. We investigated d.c. and a.c. (40 Hz-100 KHz) electrical properties of the films in the temperature range of 293K and 473K in vacuum ambient (10 - 2 mbar). We observed frequency dependent conductivity behavior at high frequencies. Absorption spectra of the film showed that a maximum absorption occurred at 330 nm. We also investigated the response of the films to vapors of the volatile organic compounds (acetone, chloroform, toluene, ethanol, ammonia) and water vapor. The films showed no sensitivity to the test gases at room temperature. Concentration of the vapors were controlled by mass flowmeters. All the measurement system was computerized

  15. Biocompatibility and Corrosion Protection Behaviour of Hydroxyapatite Sol-Gel-Derived Coatings on Ti6Al4V Alloy

    El Hadad, Amir A.; Peón, Eduardo; García-Galván, Federico R.; Barranco, Violeta; Parra, Juan; Jiménez-Morales, Antonia; Galván, Juan Carlos

    2017-01-01

    The aim of this work was to prepare hydroxyapatite coatings (HAp) by a sol-gel method on Ti6Al4V alloy and to study the bioactivity, biocompatibility and corrosion protection behaviour of these coatings in presence of simulated body fluids (SBFs). Thermogravimetric/Differential Thermal Analyses (TG/DTA) and X-ray Diffraction (XRD) have been applied to obtain information about the phase transformations, mass loss, identification of the phases developed, crystallite size and degree of crystallinity of the obtained HAp powders. Fourier Transformer Infrared Spectroscopy (FTIR) has been utilized for studying the functional groups of the prepared structures. The surface morphology of the resulting HAp coatings was studied by Scanning Electron Microscopy (SEM). The bioactivity was evaluated by soaking the HAp-coatings/Ti6Al4V system in Kokubo’s Simulated Body Fluid (SBF) applying Inductively Coupled Plasma (ICP) spectrometry. 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide (MTT) and Alamar blue cell viability assays were used to study the biocompatibility. Finally, the corrosion behaviour of HAp-coatings/Ti6Al4V system was researched by means of Electrochemical Impedance Spectroscopy (EIS). The obtained results showed that the prepared powders were nanocrystalline HAp with little deviations from that present in the human bone. All the prepared HAp coatings deposited on Ti6Al4V showed well-behaved biocompatibility, good bioactivity and corrosion protection properties. PMID:28772455

  16. Visible light active Au:TiO2 nanocomposite photoanodes for water splitting: Sol-gel vs. sputtering

    Naseri, N.; Sangpour, P.; Moshfegh, A.Z.

    2011-01-01

    In this study, pure TiO 2 and Au:TiO 2 nanocomposite thin films are both synthesized using sol-gel and RF reactive co-sputtering methods. Physical and photoelectrochemical properties of the thin films deposited by each method are compared. The optical density spectra and scanning electron microscopy images of the Au:TiO 2 films reveal formation of gold nanoparticles in the all nanocomposite films synthesized by two methods. Moreover, the optical bandgap energy of the thin films decreases with addition of Au nanoparticles. X-ray photoelectron spectroscopy indicates that the presence of gold in metallic state and the formation of TiO 2 is stoichiometric. The photoelectrochemical properties of the TiO 2 and Au:TiO 2 thin films are characterized by using a compartment cell containing KOH solution as electrolyte. It is found that in the pure systems, TiO 2 sputtered films shows a higher photocurrent under visible light illumination while a reverse result is obtained for the Au:TiO 2 systems. In addition, photoirradiation on electrode/electrolyte (EE) and substrate/electrode (SE) interfaces for the sputtered samples reveals the EE illumination enhances the photoresponse of the layers as compared to SE case.

  17. Structure and optical properties of nanocrystalline NiO thin film synthesized by sol-gel spin-coating method

    Al-Ghamdi, A.A. [King Abdulaziz University, Faculty of Science, Physics Department, Jeddah (Saudi Arabia); Mahmoud, Waleed E., E-mail: w_e_mahmoud@yahoo.co [King Abdulaziz University, Faculty of Science, Physics Department, Jeddah (Saudi Arabia); Suez Canal University, Faculty of Science, Physics Department, Ismailia (Egypt); Yaghmour, S.J.; Al-Marzouki, F.M. [King Abdulaziz University, Faculty of Science, Physics Department, Jeddah (Saudi Arabia)

    2009-11-03

    NiO thin film was prepared by sol-gel spin-coating method. This thin film annealed at T = 600 deg. C. The structure of NiO thin film was investigated by means of X-ray diffraction (XRD) technique and scanning electron microscopy (SEM). The optical properties of the deposited film were characterized from the analysis of the experimentally recorded transmittance and reflectance data in the spectral wavelength range of 300-800 nm. The values of some important parameters of the studied films are determined, such as refractive index (n), extinction coefficient (k), optical absorption coefficient (alpha) and band energy gap (E{sub g}). According to the analysis of dispersion curves, it has been found that the dispersion data obeyed the single oscillator of the Wemple-DiDomenico model, from which the dispersion parameters and high-frequency dielectric constant were determined. In such work, from the transmission spectra, the dielectric constant (epsilon{sub i}nfinity), the third-order optical nonlinear susceptibility chi{sup (3)}, volume energy loss function (VELF) and surface energy loss function (SELF) were determined.

  18. Low-cost growth of magnesium doped gallium nitride thin films by sol-gel spin coating method

    Amin, N. Mohd; Ng, S. S.

    2018-01-01

    Low-cost sol-gel spin coating growth of magnesium (Mg) doped gallium nitride (GaN) thin films with different concentrations of Mg was reported. The effects of the Mg concentration on the structural, surface morphology, elemental compositions, lattice vibrational, and electrical properties of the deposited films were investigated. X-ray diffraction results show that the Mg-doped samples have wurtzite structure with preferred orientation of GaN(002). The crystallite size decreases and the surface of the films with pits/pores were formed, while the crystalline quality of the films degraded as the Mg concentration increases from 2% to 6. %. All the Raman active phonon modes of the wurtzite GaN were observed while a broad peak attributed to the Mg-related lattice vibrational mode was detected at 669 cm-1. Hall effect results show that the resistivity of the thin films decreases while the hole concentration and hall mobility of thin films increases as the concentration of the Mg increases.

  19. Biocompatibility and Corrosion Protection Behaviour of Hydroxyapatite Sol-Gel-Derived Coatings on Ti6Al4V Alloy

    Amir A. El Hadad

    2017-01-01

    Full Text Available The aim of this work was to prepare hydroxyapatite coatings (HAp by a sol-gel method on Ti6Al4V alloy and to study the bioactivity, biocompatibility and corrosion protection behaviour of these coatings in presence of simulated body fluids (SBFs. Thermogravimetric/Differential Thermal Analyses (TG/DTA and X-ray Diffraction (XRD have been applied to obtain information about the phase transformations, mass loss, identification of the phases developed, crystallite size and degree of crystallinity of the obtained HAp powders. Fourier Transformer Infrared Spectroscopy (FTIR has been utilized for studying the functional groups of the prepared structures. The surface morphology of the resulting HAp coatings was studied by Scanning Electron Microscopy (SEM. The bioactivity was evaluated by soaking the HAp-coatings/Ti6Al4V system in Kokubo’s Simulated Body Fluid (SBF applying Inductively Coupled Plasma (ICP spectrometry. 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide (MTT and Alamar blue cell viability assays were used to study the biocompatibility. Finally, the corrosion behaviour of HAp-coatings/Ti6Al4V system was researched by means of Electrochemical Impedance Spectroscopy (EIS. The obtained results showed that the prepared powders were nanocrystalline HAp with little deviations from that present in the human bone. All the prepared HAp coatings deposited on Ti6Al4V showed well-behaved biocompatibility, good bioactivity and corrosion protection properties.

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

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

    2017-10-18

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

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

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

    2018-01-30

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

  2. Sol-gel Derived Warfarin - Silica Composites for Controlled Drug Release.

    Dolinina, Ekaterina S; Parfenyuk, Elena V

    2017-01-01

    Warfarin, commonly used anticoagulant in clinic, has serious shortcomings due to its unsatisfactory pharmacodynamics. One of the efficient ways for the improvement of pharmacological and consumer properties of drugs is the development of optimal drug delivery systems. The aim of this work is to synthesize novel warfarin - silica composites and to study in vitro the drug release kinetics to obtain the composites with controlled release. The composites of warfarin with unmodified (UMS) and mercaptopropyl modified silica (MPMS) were synthesized by sol-gel method. The composite formation was confirmed by FTIR spectra. The concentrations of warfarin released to media with pH 1.6, 6.8 and 7.4 were measured using UV spectroscopy. The drug release profiles from the solid composites were described by a series of kinetic models which includes zero order kinetics, first order kinetics, the modified Korsmeyer-Peppas model and Hixson-Crowell model. The synthesized sol-gel composites have different kinetic behavior in the studied media. In contrast to the warfarin composite with unmodified silica, the drug release from the composite with mercaptopropyl modified silica follows zero order kinetics for 24 h irrespective to the release medium pH due to mixed mechanism (duffusion + degradation and/or disintegration of silica matrix). The obtained results showed that warfarin - silica sol-gel composites have a potential application for the development of novel oral formulation of the drug with controlled delivery. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

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

    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.

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

    Giulio Gorni

    2018-01-01

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

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

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

    2004-01-01

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

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

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

    2018-01-01

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

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

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

    2003-01-01

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

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

    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.

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

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

    2015-01-01

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

  10. Sol-gel fabrication and optical absorption properties of C-NiO nanocomposite coatings

    Tile, N

    2010-12-01

    Full Text Available stream_source_info Tile1_2010.pdf.txt stream_content_type text/plain stream_size 1961 Content-Encoding ISO-8859-1 stream_name Tile1_2010.pdf.txt Content-Type text/plain; charset=ISO-8859-1 Sol-gel fabrication and optical... is compact and porous 0 500 1000 1500 2000 2500 3000 0 50 100 150 200 250 1375.55 1585.58 In te n s it y ( a rb . u n it s ) Raman shift (cm -1 ) EDS confirms NiO while Raman reveals a presence of predominantly graphite...

  11. Synthesis and sintering of nanocrystalline hydroxyapatite powders by citric acid sol-gel combustion method

    Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

    2004-01-01

    The citric acid sol-gel combustion method has been used for the synthesis of nanocrystalline hydroxyapatite (HAP) powder from calcium nitrate, diammonium hydrogen phosphate and citric acid. The phase composition of HAP powder was characterized by X-ray powder diffraction analysis (XRD). The morphology of HAP powder was observed by transmission electron microscope (TEM). The HAP powder has been sintered into microporous ceramic in air at 1200 deg. C with 3 h soaking time. The microstructure and phase composition of the resulting HAP ceramic were characterized by scanning electron microscope (SEM) and XRD, respectively. The physical characterization of open porosity and flexural strength have also been carried out

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

    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

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

    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.

  14. Novel Materials through Non-Hydrolytic Sol-Gel Processing: Negative Thermal Expansion Oxides and Beyond

    Cora Lind

    2010-04-01

    Full Text Available Low temperature methods have been applied to the synthesis of many advanced materials. Non-hydrolytic sol-gel (NHSG processes offer an elegant route to stable and metastable phases at low temperatures. Excellent atomic level homogeneity gives access to polymorphs that are difficult or impossible to obtain by other methods. The NHSG approach is most commonly applied to the preparation of metal oxides, but can be easily extended to metal sulfides. Exploration of experimental variables allows control over product stoichiometry and crystal structure. This paper reviews the application of NHSG chemistry to the synthesis of negative thermal expansion oxides and selected metal sulfides.

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

    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.

  16. Nano sized La2Co2O6 double perovskite synthesized by sol gel method

    Solanki, Neha; Lodhi, Pavitra Devi; Choudhary, K. K.; Kaurav, Netram

    2018-05-01

    We report here the synthesis of double perovskite La2Co2O6 (LCO) compound by a sol gel route method. The double perovskite structure of LCO system was confirmed via X-ray diffraction (XRD) analysis. Further, the lattice parameter, unit cell volume and bond length were refined by means of rietveld analysis using the full proof software. Debye Scherer formula was used to determine the particle size. The compound crystallized in triclinic structure with space group P-1 in ambient condition. We also obtained Raman modes from XRD spectra of poly-crystalline LCO sample. These results were interpreted for the observation of phonon excitations in this compound.

  17. ENEA contribution to the development of the sol-gel technologies

    Vatteroni, R.; Arcangeli, G.; Borrello, A.; Majani, C.; Picconi, C.

    1994-11-01

    Compared with conventional ceramic processes, the Sool-Gel technology, invented at the end of sixties for the preparation of ceramic nuclear fuel, seems suitable for obtaining pure and homogeneous fine grade precursors with a deeper control of chemical purity and crystallinity. In the frame of some agreements with other italianrResearch institutes, ENEA (Italian Agency for New Technologies, Energy and Environment) has applied the Sol-Gel technologies to the development of a few advanced ceramic materials; some of these particular applications are described in this report

  18. Fabrication of silica glass containing yellow oxynitride phosphor by the sol-gel process

    Segawa, Hiroyo; Yoshimizu, Hisato; Hirosaki, Naoto; Inoue, Satoru, E-mail: SEGAWA.Hiroyo@nims.go.jp [National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan)

    2011-06-15

    We have prepared silica glass by the sol-gel method and studied its ability to disperse the Ca-{alpha}-SiAlON:Eu{sup 2+} phosphor for application in white light emitting diodes (LEDs). The emission color generated by irradiating doped glass with a blue LED at 450 nm depended on the concentration of SiAlON and the glass thickness, resulting in nearly white light. The luminescence efficiency of 1-mm-thick glass depended on the SiAlON concentration, and was highest at 4 wt% SiAlON.

  19. Low-temperature sol-gel synthesis of NaZr2P3O12

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

    1990-01-01

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

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

    Powers, Kevin William

    1998-12-01

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

  1. Synthesis of hybrid sol-gel coatings for corrosion protection of we54-ae magnesium alloy

    Hernández-Barrios, C A; Peña, D Y; Coy, A E; Duarte, N Z; Hernández, L M; Viejo, F

    2013-01-01

    The present work shows some preliminary results related to the synthesis, characterization and corrosion evaluation of different hybrid sol-gel coatings applied on the WE54-AE magnesium alloy attending to the two experimental variables, i.e. the precursors ratio and the aging time, which may affect the quality and the electrochemical properties of the coatings resultant. The experimental results confirmed that, under some specific experimental conditions, it was possible to obtain homogeneous and uniform, porous coatings with good corrosion resistance that also permit to accommodate corrosion inhibitors

  2. Sol-gel system study of Zr O2- Co3 O-4

    Cerri, J.A.; Matos, E.M.R.; Longo, E.; Varela, J.A.; Santos, C.O.P.

    1992-01-01

    Phases present in the system Zr O 2 + Co 3 O 4 were studied through X-Ray diffraction. The processing of the powder was developed through a modified sol-gel method, where the precursors Zr O (N O 3)2 and Co (N O 3)2 were in an ethanol solution. To verify the influence of CO 3 O 4 on the stabilization and phases formation, the crystallite size and the lattice parameter were determined considering as standard, the system without cobalt. (author)

  3. Synthesis of Copper-Based Transparent Conductive Oxides with Delafossite Structure via Sol-Gel Processing

    Götzendörfer, Stefan

    2011-01-01

    Starting off with solubility experiments of possible precursors, the present study reveals the whole development of a sol gel processing route for transparent p type semiconductive thin films with delafossite structure right to the fabrication of functional p-n junctions. The versatile sol formulation could successfully be modified for several oxide compositions, enabling the synthesis of CuAlO2, CuCrO2, CuMnO2, CuFeO2 and more. Although several differences in the sintering behaviour of powde...

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

    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...

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

    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)

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

    Hours, T.

    1988-01-01

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

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

    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.

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

    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

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

    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.

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

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

    2013-10-01

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

  11. Co{sub 3}O{sub 4}/TiO{sub 2} films obtained by laser ablation and sol-gel for the reaction of oxygen liberation in alkaline medium; Peliculas de Co{sub 3}O{sub 4}/TiO{sub 2} obtenidas por ablacion laser y sol-gel para la reaccion de desprendimiento de oxigeno en medio alcalino

    Perez A, J.; Fernandez V, S. M.; Escobar A, L.; Jimenez B, J. [Departamento de Quimica, ININ, Carretera Mexico-Toluca s/n, Ocoyoacac, Estado de Mexico (Mexico)

    2008-07-01

    The laser ablation technique known as Pulsed Laser Deposition (PLD) is used for obtaining thin films of TiO{sub 2}/SnO{sub 2}, which was later modified with Co{sub 3}O{sub 4} by PLD or by sol-gel technique. The films were characterized by X-ray diffraction, ultraviolet Vis and Raman spectroscopies, scanning electron microscopy and energy analysis of the dispersed X-rays produced by Auger decay. The anatase phase with particles of nano metric size was obtained by depositing the titanium dioxide in argon atmosphere. The Co{sub 3}O{sub 4} films obtained by PLD on the TiO{sub 2} showed the same morphology. The electrocatalytic activity of the films that were used as photo anodes for the reaction of oxygen liberation was carried out in the darkness, with environment light and the light emitted by a xenon lamp. The current density was higher for films of Co{sub 3}O{sub 4}/TiO{sub 2}/SnO{sub 2} obtained by PLD that for cobalt dioxide of mixed valence obtained by sol-gel. (Author)

  12. Synthesis of Titania-supported Copper Nanoparticles via Refined Alkoxide Sol-gel Process

    Wu, Jeffrey C.S.; Tseng, I.-Hsiang; Chang, W.-C.

    2001-01-01

    Nanoparticles of titania and copper-loaded titania were synthesized by a refined sol-gel method using titanium butoxide. Unlike the conventional sol-gel procedure of adding water directly, the esterification of anhydrous butanol and glacial acetic acid provided the hydrolyzing water. In addition, acetic acid also served as a chelating ligand to stabilize the hydrolysis-condensation process and minimize the agglomeration of titania. Following the hydrolysis, Cu/TiO 2 was prepared by adding copper chloride to titania sol. The sol was dried, then calcined at 500 deg. C to remove organics and transformed to anatase titania which was verified by XRD. Cu/TiO 2 was further hydrogen-reduced at 300 deg. C. The recovery of Ti was exceeded by an average of 95% from titanium butoxide. TEM micrographs show that the Cu/TiO 2 particles are near uniform. The average crystallite sizes are 17-20 nm estimated from the peak broadening of XRD spectra. The bandgaps of TiO 2 and reduced Cu/TiO 2 range from 2.70 to 3.15 eV estimated from the diffusive reflective UV-Vis spectra. XPS analysis shows that Cu 2p 3/2 is 933.4 eV indicating primary Cu 2 O form on the TiO 2 supports. The binding energy of Ti does not exhibit chemical shift suggesting negligible interaction of Cu cluster and TiO 2 support

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

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

    2010-05-03

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

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

    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.

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

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

    1999-01-01

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

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

    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

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

    Sharma, Mamta; Mehra, R.M.

    2010-01-01

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

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

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

    2004-01-01

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

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

    Rula M. Allaf

    2014-01-01

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

  20. Fabrication of mesoporous silica nanoparticles by sol gel method followed various hydrothermal temperature

    Purwaningsih, Hariyati; Pratiwi, Vania Mitha; Purwana, Siti Annisa Bani; Nurdiansyah, Haniffudin; Rahmawati, Yenny; Susanti, Diah

    2018-04-01

    Rice husk is an agricultural waste that is potentially used as natural silica resources. Natural silica claimed to be safe in handling, cheap and can be generate from cheap resource. In this study mesoporous silica was synthesized using sodium silicate extracted from rice husk ash. This research's aim are to study the optimization of silica extraction from rice husk, characterizing mesoporous silica from sol-gel method and surfactant templating from rice husk and the effect of hydrothermal temperature on mesoporous silica nanoparticle (MSNp) formation. In this research, rice husk was extracted with sol-gel method and was followed by hydrothermal treatment; several of hydrothermal temperatures were 85°C, 100°C, 115°C, 130°C and 145° for 24 hours. X-ray diffraction analysis was identified of α-SiO2 phase and NaCl compound impurities. Scherer's analysis method for crystallite size have resulted 6.27-40.3 nm. FTIR results of silica from extraction and MSNp indicated Si-O-Si bonds on the sample. SEM result showed the morphology of the sample that has spherical shape and smooth surface. TEM result showed particle size ranged between 69,69-84,42 nm. BET showed that the pore size classified as mesoporous with pore diameter size is 19,29 nm.

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

    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.

  2. Development of fluorocarbon/silica composites via sol/gel process

    Ferreira, Max P.; Maria, Daniel A.; Gomes, Luiza M.F.

    2009-01-01

    Fluorocarbon/silica composites have interesting physical-chemical properties, combining the great resistance to chemical products, the electric insulation, and the thermal stability of fluorine polymers with the optical, magnetic, and dielectric properties of silica. Due to the unique mechanical, thermal, and dielectric properties of fluorocarbon and silica composites, there is interest in their application in the development of fuel cells, the production of integrated circuit boards (ICB), and packages for the transportation of integrated circuits. The sol-gel process is a chemical route to prepare ceramic materials with specific properties that are hard or impossible to obtain by conventional methods. Fluorocarbon/silica composites were obtained by the sol-gel method from tetramethoxysilane - TMOS and fluorinated hydrocarbons with low molecular weight and main chains with 10 - 20 carbon atoms previously obtained from PTFE scraps irradiated with a 60 Co γ source in oxygen atmosphere with a dose of 1 MGy. Syntheses were performed in 125-mL reaction flasks in basic medium at 35 deg C and in acid medium at 60 deg C with N-N dimethylformamide as a chemical additive for drying control. After synthesis, the material was thermally treated in an oven with electronic temperature control. The monoliths obtained were characterized by Fourier transform infrared spectroscopy (FTIR), electron microprobe and by a standard nitrogen adsorption-desorption technique. (author)

  3. Synthesis of Titania-supported Copper Nanoparticles via Refined Alkoxide Sol-gel Process

    Wu, Jeffrey C. S.; Tseng, I.-Hsiang; Chang, Wan-Chen

    2001-06-01

    Nanoparticles of titania and copper-loaded titania were synthesized by a refined sol-gel method using titanium butoxide. Unlike the conventional sol-gel procedure of adding water directly, the esterification of anhydrous butanol and glacial acetic acid provided the hydrolyzing water. In addition, acetic acid also served as a chelating ligand to stabilize the hydrolysis-condensation process and minimize the agglomeration of titania. Following the hydrolysis, Cu/TiO2 was prepared by adding copper chloride to titania sol. The sol was dried, then calcined at 500°C to remove organics and transformed to anatase titania which was verified by XRD. Cu/TiO2 was further hydrogen-reduced at 300°C. The recovery of Ti was exceeded by an average of 95% from titanium butoxide. TEM micrographs show that the Cu/TiO2 particles are near uniform. The average crystallite sizes are 17-20 nm estimated from the peak broadening of XRD spectra. The bandgaps of TiO2 and reduced Cu/TiO2 range from 2.70 to 3.15 eV estimated from the diffusive reflective UV-Vis spectra. XPS analysis shows that Cu 2p3/2 is 933.4 eV indicating primary Cu2O form on the TiO2 supports. The binding energy of Ti does not exhibit chemical shift suggesting negligible interaction of Cu cluster and TiO2 support.

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

    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.

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

    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.

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

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

    2001-11-01

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

  7. Synthesis and characterization of NiO nanopowder by sol-gel process

    Ningsih, Sherly Kasuma Warda [Department of Chemistry, Faculty of Mathematics and Natural Sciences Padang State University, Kampus Air Tawar, Jl. Prof. Dr. Hamka, West Sumatera, 25161, Indonesia Email: sherly-kasuma@yahoo.com (Indonesia)

    2015-09-30

    Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms were produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.

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

    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

    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. Phospholipid Fatty Acids as Physiological Indicators of Paracoccus denitrificans Encapsulated in Silica Sol-Gel Hydrogels

    Josef Trögl

    2015-02-01

    Full Text Available The phospholipid fatty acid (PLFA content was determined in samples of Paracoccus denitrificans encapsulated in silica hydrogel films prepared from prepolymerized tetramethoxysilane (TMOS. Immediately after encapsulation the total PLFA concentration was linearly proportional to the optical density (600 nm of the input microbial suspension (R2 = 0.99. After 7 days this relationship remained linear, but with significantly decreased slope, indicating a higher extinction of bacteria in suspensions of input concentration 108 cells/mL and higher. trans-Fatty acids, indicators of cytoplasmatic membrane disturbances, were below the detection limit. The cy/pre ratio (i.e., ratio of cyclopropylated fatty acids (cy17:0 + cy19:0 to their metabolic precursors (16:1ω7 + 18:1ω7, an indicator of the transition of the culture to a stationary growth-phase, decreased depending on co-immobilization of nutrients in the order phosphate buffer > mineral medium > Luria Broth rich medium. The ratio, too, was logarithmically proportional to cell concentration. These results confirm the applicability of total PLFA as an indicator for the determination of living biomass and cy/pre ratio for determination of nutrient limitation of microorganisms encapsulated in sol-gel matrices. This may be of interest for monitoring of sol-gel encapsulated bacteria proposed as optical recognition elements in biosensor construction, as well as other biotechnological applications.

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

    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.

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

    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.

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

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

    2018-05-01

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

  14. The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

    Ales Styskalik

    2017-05-01

    Full Text Available This review is devoted to non-hydrolytic sol-gel chemistry. During the last 25 years, non-hydrolytic sol-gel (NHSG techniques were found to be attractive and versatile methods for the preparation of oxide materials. Compared to conventional hydrolytic approaches, the NHSG route allows reaction control at the atomic scale resulting in homogeneous and well defined products. Due to these features and the ability to design specific materials, the products of NHSG reactions have been used in many fields of application. The aim of this review is to present an overview of NHSG research in recent years with an emphasis on the syntheses of mixed oxides, silicates and phosphates. The first part of the review highlights well known condensation reactions with some deeper insights into their mechanism and also presents novel condensation reactions established in NHSG chemistry in recent years. In the second section we discuss porosity control and novel compositions of selected materials. In the last part, the applications of NHSG derived materials as heterogeneous catalysts and supports, luminescent materials and electrode materials in Li-ion batteries are described.

  15. Composite Biomaterials Based on Sol-Gel Mesoporous Silicate Glasses: A Review

    Baino, Francesco; Fiorilli, Sonia; Vitale-Brovarone, Chiara

    2017-01-01

    Bioactive glasses are able to bond to bone and stimulate the growth of new tissue while dissolving over time, which makes them ideal materials for regenerative medicine. The advent of mesoporous glasses, which are typically synthesized via sol-gel routes, allowed researchers to develop a broad and versatile class of novel biomaterials that combine superior bone regenerative potential (compared to traditional melt-derived glasses) with the ability of incorporating drugs and various biomolecules for targeted therapy in situ. Mesoporous glass particles can be directly embedded as a bioactive phase within a non-porous (e.g., microspheres), porous (3D scaffolds) or injectable matrix, or be processed to manufacture a surface coating on inorganic or organic (macro)porous substrates, thereby obtaining hierarchical structures with multiscale porosity. This review provides a picture of composite systems and coatings based on mesoporous glasses and highlights the challenges for the future, including the great potential of inorganic–organic hybrid sol-gel biomaterials. PMID:28952496

  16. Colloidal probe dynamics in gelatin solution during the sol-gel transition.

    Hong, Wei; Xu, Guozhi; Ou, Xiaogang; Sun, Weixiang; Wang, Tao; Tong, Zhen

    2018-05-16

    The dynamics of the colloidal probes in a gelatin solution during the time-dependent sol-gel transition was investigated by multi-particle tracking. The relationship between the relaxation of the medium at the critical gel point and the mean square displacement of the probes was elucidated. Based on this understanding, the critical gel point of gelatin and the corresponding critical exponent n were unambiguously determined by the loss angle criterion and the time-cure superposition. The shift factors of the latter are further used to estimate the time/length-scale evolution of the gelatin during the sol-gel transition. The growth of the medium length scale crossed with the two measuring length scales successively at the pre-gel regime. Coinciding with the length-scale crossovers, the probability density function (PDF) of the probe displacements displayed two transient peaks of non-Gaussianity. In the post-gel regime, the third peak of Gaussianity suggested inhomogeneity in the gel network. The non-Gaussianity results from the bifurcation of diffusivity. The present work showed that the non-Gaussian dynamics of the probes are not the direct equivalence of that of the medium, but an effect of length-scale coupling.

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

    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.

  18. Assembly of polymer micelles through the sol-gel transition for effective cancer therapy.

    Khaliq, Nisar Ul; Oh, Keun Sang; Sandra, Febrina Carolina; Joo, Yeonhee; Lee, Juhyung; Byun, Youngro; Kim, In-San; Kwon, Ick Chan; Seo, Jae Hong; Kim, Sang Yoon; Yuk, Soon Hong

    2017-06-10

    Photo-induced apoptosis-targeted chemotherapy (PIATC) was designed and characterized to propose a new protocol for improved chemotherapy. Intratumoral injection was selected as the mode of administration of the anticancer drug, doxorubicin (DOX). To extend the retention time of DOX at the tumor parenchyma, in-situ gel formation was induced through the sol-gel transition of the Pluronic NPs containing a prodrug of DOX or a photosensitizer. The prodrug (DEVD-S-DOX) was designed to be inactive with a peptide moiety (Aspartic acid-Glutamic acid-Valine-Aspartic acid: DEVD) linked to DOX and to be cleaved into free DOX by caspase-3 expressed with apoptosis. For reactive oxygen species (ROS)-mediated apoptosis, photo-irradiation with methylene blue (MB, photosensitizer) was utilized. The sol-gel transition of the Pluronic NPs containing reactive species, DEVD-S-DOX or MB, was examined by measuring the cloud point and the gel strength in response to temperature change. ROS-mediated apoptosis was observed by measuring the ROS and membrane integrity with induced apoptosis. The in vivo antitumor efficacy of PIATC was measured with a cardiotoxicity assay in tumor-bearing mice. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Yuan Yuan; Liu Changsheng; Zhang Yuan; Shan Xiaoqian

    2008-01-01

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

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

    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.