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Sample records for sol-gel derived ferroelectric

  1. Sol-gel derived sorbents

    DOEpatents

    Sigman, Michael E.; Dindal, Amy B.

    2003-11-11

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

  2. Sol-Gel Derived Hafnia Coatings

    NASA Technical Reports Server (NTRS)

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

    2002-01-01

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

  3. Surface photovoltage characterization of sol-gel derived Bi 4Ti 3O 12 ferroelectric thin film on F-doped SnO 2 conducting glass

    NASA Astrophysics Data System (ADS)

    Wang, W. C.; Zheng, H. W.; Liu, X. Y.; Liu, X. S.; Gu, Y. Z.; Zhang, H. R.; Zhang, W. F.

    2010-03-01

    The surface photovoltage response was investigated in partly c-axis oriented Bi 4Ti 3O 12 thin film deposited on fluorine-doped tin oxide conductive glass substrate by a sol-gel technology. The maximum SPV of BiT film reaches 1.8 mV under the dc bias voltage (+1 V) and is three times larger than that under the zero bias. It is also found that the SPV response intensity increases with the increasing positive field, and the intensity of the SPV signal becomes weak with a reverse response when the negative field increases. It is suggested that the SPV is strongly related to the ferroelectric polarization.

  4. Large remanent polarization and small leakage in sol-gel derived Bi(Zn(1/2)Zr(1/2))O3-PbTiO3 ferroelectric thin films.

    PubMed

    Zhang, Linxing; Chen, Jun; Zhao, Hanqing; Fan, Longlong; Rong, Yangchun; Deng, Jinxia; Yu, Ranbo; Xing, Xianran

    2013-01-14

    The applications of ferroelectric thin films such as the sensitivity of nonvolatile ferroelectric random access memories are closely linked with large remnant polarization. The high-T(C) (1-x)Bi(Zn(1/2)Zr(1/2))O(3)-xPbTiO(3) (x = 0.7-0.9) thin films with high (100) orientation were fabricated on Pt(111)/Ti/SiO(2)/Si substrates via a sol-gel method. The thin films could be crystallized well in a phase-pure perovskite structure. The electrical properties of the sol-gel-derived BZZ-PT thin films were investigated. A large remanent polarization with 2P(r) up to 110 μC cm(-2) and a small leakage current of 3.8 × 10(-7) A cm(-2) under an electric field of 150 kV cm(-1) are observed on the 0.2BZZ-0.8PT thin films. Furthermore, a relatively stable polarization fatigue property was achieved, indicating a potential application in high-temperature ferroelectric devices.

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

    SciTech Connect

    Shen Hongfang; Guo Qing; Zhao Zhiman; Cao Guozhong

    2009-11-15

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

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

    SciTech Connect

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

    2004-06-10

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

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

    PubMed

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

    2011-10-01

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

  8. Sol Gel-Derived SBA-16 Mesoporous Material

    PubMed Central

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

    2010-01-01

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

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

    SciTech Connect

    Kueper, T.W.

    1992-05-01

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

  10. Structure and Electrical Properties of Na0.5Bi0.5TiO3 Ferroelectric Thick Films Derived From a Polymer Modified Sol-Gel Method

    PubMed Central

    Ji, Hongfen; Ren, Wei; Wang, Lingyan; Shi, Peng; Chen, Xiaofeng; Wu, Xiaoqing; Yao, Xi; Lau, Sien-Ting; Zhou, Qifa; Shung, K. Kirk

    2011-01-01

    Lead-free Na0.5Bi0.5TiO3 (NBT) ferroelectric thick films were prepared by a poly(vinylpyrrolidone) (PVP) modified sol-gel method. The NBT thick films annealed from 500°C to 750°C exhibit a perovskite structure. The relationship between annealing temperature, thickness, and electrical properties of the thick films has been investigated. The dielectric constants and remnant polarizations of the thick films increase with annealing temperature. The electrical properties of the NBT films show strong thickness dependence. As thickness increases from 1.0 to 4.8 μm, the dielectric constant of the NBT films increases from 620 to 848, whereas the dielectric loss is nearly independent of the thickness. The remnant polarization of the NBT thick films also increases with increasing thickness. The leakage current density first decreases and then increases with film thickness. PMID:21989868

  11. Sol-gel derived contamination resistant antireflective coatings

    NASA Astrophysics Data System (ADS)

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

    2011-02-01

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

  12. Sol-gel derived contamination resistant antireflective coatings

    NASA Astrophysics Data System (ADS)

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

    2010-10-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1992-12-01

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

  14. Sol-gel derived planar waveguides for sensor applications

    NASA Astrophysics Data System (ADS)

    Karasinski, Pawel; Zielonka, Iwona

    2003-09-01

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

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

    PubMed

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

    2003-11-01

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

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

    NASA Astrophysics Data System (ADS)

    Han, Kuo

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

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

    NASA Astrophysics Data System (ADS)

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

    1984-09-01

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

  18. Nanostructured energetic materials derived from sol-gel chemistry

    SciTech Connect

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

    2000-03-15

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

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

    PubMed

    Shchipunov, Yurii A

    2003-12-01

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

  20. Sol-gel derived electrode materials for supercapacitor applications

    NASA Astrophysics Data System (ADS)

    Lin, Chuan

    1998-12-01

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

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

    PubMed

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

    2012-12-18

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-12-01

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

  3. Fabrication and characterization of sol-gel derived 45S5 Bioglass®-ceramic scaffolds.

    PubMed

    Chen, Qi-Zhi; Thouas, George A

    2011-10-01

    Although Bioglass® has existed for nearly half a century its ability to trigger bone formation and tuneable degradability is vastly superior to other bioceramics, such as SiO(2)-CaO bioactive glasses. The sol-gel process of producing glass foams is well established for SiO(2)-CaO compositions, but not yet established for 45S5 composites containing Na(2)O. In this work the sol-gel derived 45S5 Bioglass® has for the first time been foamed into highly porous three-dimensional scaffolds using a surfactant, combined with vigorous mechanical stirring and subsequent sintering at 1000°C for 2 h. It was found that the mechanical strength of the sintered sol-gel derived Bioglass® scaffolds was significantly improved, attributable to the small fraction of material on the pore walls. More importantly, the compressive strength of the three-dimensional scaffolds produced by this surfactant foaming method could be predicted using Gibson and Ashby's closed cell model of porous networks. A comparative experiment revealed that ion release from the sol-gel derived Bioglass® foams was faster than that of counterparts produced by the replication technique. In vitro evaluation using osteoblast-like cells demonstrated that the sol-gel derived 45S5 Bioglass foams supported the proliferation of viable cell populations on the surface of the scaffolds, although few cells were observed to migrate into the virtually closed pores within the foams. Further work should be focused on modifications of the reaction conditions or alternative foaming techniques to improve pore interconnection.

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

    PubMed

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

    2016-09-07

    The purpose of this study was to evaluate the effect of sol-gel derived bioactive coatings on the biaxial flexural strength and fibroblast proliferation of zirconia, aimed to be used as an implant abutment material. Yttrium stabilized zirconia disc-shaped specimens were cut, ground, sintered, and finally cleansed ultrasonically in each of acetone and ethanol for 5 minutes. Three experimental groups (n = 15) were fabricated, zirconia with sol-gel derived titania (TiO2 ) coating, zirconia with sol-gel derived zirconia (ZrO2 ) coating, and non-coated zirconia as a control. The surfaces of the specimens were analyzed through images taken using a scanning electron microscope (SEM), and a non-contact tapping mode atomic force microscope (AFM) was used to record the surface topography and roughness of the coated specimens. Biaxial flexural strength values were determined using the piston-on-three ball technique. Human gingival fibroblast proliferation on the surface of the specimens was evaluated using AlamarBlue assay™. Data were analyzed using a one-way analysis of variance (ANOVA) followed by Tukey's post-hoc test. Additionally, the biaxial flexural strength data was also statistically analyzed with the Weibull distribution. The biaxial flexural strength of zirconia specimens was unaffected (p > 0.05). Weibull modulus of TiO2 coated and ZrO2 coated groups (5.7 and 5.4, respectively) were lower than the control (8.0). Specimens coated with ZrO2 showed significantly lower fibroblast proliferation compared to other groups (p < 0.05). In conclusion, sol-gel derived coatings have no influence on the flexural strength of zirconia. ZrO2 coated specimens showed significantly lower cell proliferation after 12 days than TiO2 coated or non-coated control. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2016.

  5. Use of sol-gel-derived titania coating for direct soft tissue attachment.

    PubMed

    Areva, Sami; Paldan, Hannu; Peltola, Timo; Närhi, Timo; Jokinen, Mika; Lindén, Mika

    2004-08-01

    A firm bond between an implant and the surrounding soft tissue is important for the performance of many medical devices (e.g., stents, canyls, and dental implants). In this study, the performance of nonresorbable and reactive sol-gel-derived nano-porous titania (TiO(2)) coatings in a soft tissue environment was investigated. A direct attachment between the soft tissue and the sol-gel-derived titania coatings was found in vivo after 2 days of implantation, whereas the titanium control implants showed no evidence of soft tissue attachment. The coated implants were in immediate contact with the connective tissue, whereas the titanium controls formed a gap and a fibrous capsule on the implant-tissue interface. The good soft tissue attachment of titania coatings may result from their ability to initiate calcium phosphate nucleation and growth on their surfaces (although the formation of poorly crystalline bonelike apatite does not occur). Thus, the formation of a bonelike CaP layer is not crucial for their integration in soft tissue. The formation of bonelike apatite was hindered by the adsorption of proteins onto the initially formed amorphous calcium phosphate growth centers, thus preventing the dissolution/reprecipitation processes required for the formation of poorly crystalline bonelike apatite. These findings might open novel application areas for sol-gel-derived titania-based coatings.

  6. β-Diketones and their derivatives in sol-gel processes

    NASA Astrophysics Data System (ADS)

    Zolotareva, N. V.; Semenov, V. V.

    2013-10-01

    Published data on the use of β-diketones, metal β-diketonates and some structurally related compounds in sol-gel synthesis of new organic-inorganic hybrid materials are analyzed. Functionalization methods of β-diketones with carbofunctional organosilicon compounds are considered. Ways of insertion of a metal cation into the organic-inorganic hybrid matrix using non-functionalized β-diketonates are demonstrated. Particular attention is devoted to luminescent lanthanide derivatives, which is due to the prospects of practical application of materials obtained from them in photonics, integrated optics and medical diagnosis. The types and properties of most widely used sol-gel monomers and oligomers and the luminescence behaviour of lanthanide β-diketonates and metal-free silica matrices are considered. The bibliography includes 220 references.

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

    PubMed

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

    2006-08-01

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

  8. Sol-gel derived aluminosilicate coatings on alumina as substrate for osteoblasts.

    PubMed

    Leivo, Jarkko; Meretoja, Ville; Vippola, Minnamari; Levänen, Erkki; Vallittu, Pekka; Mäntylä, Tapio A

    2006-11-01

    Rat bone marrow stromal cell differentiation on aluminosilicate 3Al(2)O(3)-2SiO(2) coatings was investigated. Thin ceramic coatings were prepared on alpha-alumina substrates by the sol-gel process and calcined in order to establish an amorphous aluminosilicate ceramic phase with and without nanosized transitional mullite crystals. In addition, coatings of thermally sprayed aluminosilicate and diphasic gamma-alumina-silica nanosized colloids were prepared. Cell culture testing by rat osteoblasts showed good biocompatibility for aluminosilicates with sustained normal osteoblast functions. Despite mutual disparities in physical and chemical nanostructures, the culture findings suggested fairly similar osteoblast response to all tested coatings. The results suggest that topographical frequency parameters and chemical uniformity are important parameters in determining the best conditions for osteoblasts on sol-gel derived aluminosilicate materials.

  9. Structural characterization of some sol-gel derived phosphosilicate glasses

    NASA Astrophysics Data System (ADS)

    Todan, L.; Anghel, E. M.; Osiceanu, P.; Turcu, R. V. F.; Atkinson, I.; Simon, S.; Zaharescu, M.

    2015-04-01

    A comparative study of three phosphosilicate gels of the 90SiO2-10P2O5 composition obtained from tetraethoxysilane and three phosphorous precursors: triethylphosphate (TEP), triethylphosphite (TEPI) and H3PO4 is performed. 29Si and 31P Magic Angle Spining NMR, X-ray Photoelectron, X-ray Fluorescence and Raman spectroscopies as well as TG analysis are used in order to establish phosphorous precursors and annealing influence on composition and structure of the outcome materials. Unlike the three dimensional silicate network made of Si(OSi)x(OH)4-x species, unreacted TEP (100% Q1 condensed phosphorous units) from TEP derived gel and a large amount of isolated phosphorous species (39.7% Q0) in the H3PO4 derived gel are identified. Annealing at 700 °C of the three gels give similar structure with the 90SiO2-10P2O5 glass, excepting the triethylphosphate derived glass that has a much lower P content. Thus, the H3PO4 derived glass at 700 and 1000 °C shows 1.89 and 1.94 times higher P2O5/SiO2 ratios than in the case of the TEP derived one.

  10. Structural, Optical and Electrical Properties of Sol-Gel Derived Titanium Dioxide Thin Film

    NASA Astrophysics Data System (ADS)

    Taşkin, Dilek; Dumludaǧ, Fatih; Altindal, Ahmet

    2007-04-01

    Optical, structural and electrical (dc and ac) properties of sol-gel derived TiO2 film in a wide range of temperature (290 - 652 K) were investigated. XRD analysis was used for investigation the crystallinity of the films. Optical bad gap of the film were determined from transmission spectra. With the examination of the impedance spectra clear differences could be seen in the dependence of ω on both real and imaginary part of impedance between 290 K and 652 K. The impedance response is significantly changed with the increase of temperature.

  11. Entrapment of fluorescence signaling DNA enzymes in sol-gel-derived materials for metal ion sensing.

    PubMed

    Shen, Yutu; Mackey, Gillian; Rupcich, Nicholas; Gloster, Darin; Chiuman, William; Li, Yingfu; Brennan, John D

    2007-05-01

    Three fluorescence signaling DNA enzymes (deoxyribozymes or DNAzymes) were successfully immobilized within a series of sol-gel-derived matrixes and used for sensing of various metal ions. The DNAzymes are designed such that binding of appropriate metal ions induces the formation of a catalytic site that cleaves a ribonucleotide linkage within a DNA substrate. A fluorophore (fluorescein) and a quencher (DABCYL, [4-(4-dimethylaminophenylazo)benzoic acid]) were placed on the two deoxythymidines flanking the ribonucleotide to allow the generation of fluorescence upon the catalytic cleavage at the RNA linkage. In general, all DNAzymes retained at least partial catalytic function when entrapped in either hydrophilic or hydrophobic silica-based materials, but displayed slower response times and lower overall signal changes relative to solution. Interestingly, it was determined that maximum sensitivity toward metal ions was obtained when DNAzymes were entrapped into composite materials containing approximately 40% of methyltrimethoxysilane (MTMS) and approximately 60% tetramethoxysilane (TMOS). Highly polar materials derived from sodium silicate, diglycerylsilane, or TMOS had relatively low signal enhancements, while materials with very high levels of MTMS showed significant leaching and low signal enhancements. Entrapment into the hybrid silica material also reduced signal interferences that were related to metal-induced quenching; such interferences were a significant problem for solution-based assays and for polar materials. Extension of the solid-phase DNAzyme assay toward a multiplexed assay format for metal detection is demonstrated, and shows that sol-gel technology can provide new opportunities for the development of DNAzyme-based biosensors.

  12. A Guided Materials Screening Approach for Developing Quantitative Sol-gel Derived Protein Microarrays

    PubMed Central

    Helka, Blake-Joseph; Brennan, John D.

    2013-01-01

    Microarrays have found use in the development of high-throughput assays for new materials and discovery of small-molecule drug leads. Herein we describe a guided material screening approach to identify sol-gel based materials that are suitable for producing three-dimensional protein microarrays. The approach first identifies materials that can be printed as microarrays, narrows down the number of materials by identifying those that are compatible with a given enzyme assay, and then hones in on optimal materials based on retention of maximum enzyme activity. This approach is applied to develop microarrays suitable for two different enzyme assays, one using acetylcholinesterase and the other using a set of four key kinases involved in cancer. In each case, it was possible to produce microarrays that could be used for quantitative small-molecule screening assays and production of dose-dependent inhibitor response curves. Importantly, the ability to screen many materials produced information on the types of materials that best suited both microarray production and retention of enzyme activity. The materials data provide insight into basic material requirements necessary for tailoring optimal, high-density sol-gel derived microarrays. PMID:24022739

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

    SciTech Connect

    Cervantes, O

    2010-06-01

    Energetic composite powders consisting of sol-gel (SG) derived nanostructured tungsten oxide were produced with various amounts of micrometer-scale tantalum fuel metal. Such energetic composite powders were ignition-tested and results show that the powders are not sensitive to friction, spark and/or impact ignition. Initial consolidation experiments, using the High Pressure Spark Plasma Sintering (HPSPS) technique, on the SG derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The SG derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta - WO3) energetic composite was consolidated to a density of 9.17 g·cm-3 or 93% relative density. In addition, those samples were consolidated without significant pre-reaction of the constituents, thus retaining their stored chemical energy.

  14. Combined removal of SO2 and NO using sol-gel-derived copper oxide coated alumina sorbents/catalysts.

    PubMed

    Buelna, G; Lin, Y S

    2003-09-01

    The present paper reports experimental results on the removal of sulfur dioxide and nitrogen oxide from simulated flue gas using a copper oxide coated on alumina sorbent/catalyst prepared by the sol-gel method. Selective catalytic reduction of nitric oxide by ammonia over sol-gel derived CuO/gamma-Al2O3 sorbents/catalysts with different degrees of sulfation was studied in a fixed-bed packed reactor. The optimum temperature for NO reduction was found at 350 degrees C for both fresh and sulfated catalysts. The properties for simultaneous removal of SO2 and NO by the sol-gel-derived CuO/gamma-Al2O3 sorbents were studied using simulated dry flue gas. The optimum operating temperature for the combined deSO2/deNO operations was identified at 350 degrees C. At the space velocity of 5200 h(-1) and 350 degrees C, a fixed-bed reactor packed with the 7.9 wt% CuO/gamma-Al2O3 sorbent prepared by the sol-gel method offers SO2 sorption capacity of 2.3 mmol g(-1) and NO conversion of 92% with a dry simulated flue gas as the feed. Under these experimental conditions, the sol-gel derived sorbents/catalysts have comparable efficiency for removal of SO2 and NOx as their commercial counterparts. The significantly higher crush strength of the sol-gel derived sorbents/catalysts make them very promising for their use in the copper oxide process for combined removal of SO2 and NOx from flue gas in a single unit operation.

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

    SciTech Connect

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

    2015-09-28

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

  16. Sol-gel reaction stability studied: Influence in the formation temperature and properties of ferroelectric thin films

    SciTech Connect

    Perez, J. Vilarinho, P.M.; Kholkin, A.L.; Almeida, A.

    2009-03-05

    Lead zirconium titanate (PZT) sol-gel solutions were prepared based on distilled lead acetate precursor solutions. A detailed analysis of the distillation effect on the lead precursor and the final PZT solution were carried out by Infrared and Raman techniques. It was found that the increase in the number of distillation steps experienced by the lead precursor solutions removes the constitutional water and increases the lead acetate-2-methoxyethanol interconnectivity; thus improving stability and avoiding the aging effect of the resulting PZT solutions. The thermal decomposition process of the PZT solutions was analyzed based on the thermogravimetric (TG) and differential thermogravimetric analysis (DTA) measurements. It was found that as the number of distillation steps in the lead precursor solutions increases, the decomposition rate increases and the formation temperature of pure perovskite PZT films decreases. X-ray diffraction (XRD) technique was used to study the film phase formation. A pure perovskite phase at 500 deg. C was found by the XRD analysis after the second distillation step. Scanning electron microscope technique was used to carry out the microstructural analysis. Dense microstructure was found in all analyzed films and an incipient columnar grain growth was revealed in PZT films prepared based on lead precursor solution with more than three distillation steps. The dependence of the dielectric, ferroelectric and piezoelectric properties on the number of distillation steps was revealed and a correlation between the distillation process, film microstructure properties and electrical performance was established.

  17. Magnetic, ferroelectric and leakage current properties of gadolinium doped bismuth ferrite thin films by sol-gel method

    NASA Astrophysics Data System (ADS)

    Chen, Hone-Zern; Kao, Ming-Cheng; Young, San-Lin; Hwang, Jun-Dar; Chiang, Jung-Lung; Chen, Po-Yen

    2015-05-01

    Bi0.9Gd0.1FeO3 (BGFO) thin films were fabricated on Pt(111)/Ti/SiO2/Si(100) substrates by using the sol-gel technology. The effects of annealing temperature (400-700 °C) on microstructure and multiferroic properties of thin films were investigated. The X-ray diffraction analysis showed that the BGFO thin films had an orthorhombic structure. The thin films showed ferroelectric and ferromagnetic properties with remanent polarization (2Pr) of 10 μC/cm2, remnant magnetization (2Mr) of 2.4 emu/g and saturation magnetization (Ms) of 5.3 emu/g. A small leakage current density (J) was 4.64×10-8 A/cm2 under applied field 100 kV/cm. It was found that more than one conduction mechanism is involved in the electric field range used in these experiments. The leakage current mechanisms were controlled by Poole-Frenkel emission in the low electric field region and by Schottky emission from the Pt electrode in the high field region.

  18. Sol-gel derived antireflective structures for applications in silicon solar cells

    NASA Astrophysics Data System (ADS)

    Karasiński, Paweł; Skolik, Marcin

    2016-12-01

    This work presents theoretical and experimental results of antireflective coatings (ARCs) obtained for applications in silicon solar cells. ARCs were derived from sol-gel process and dip-coated using silica (SiO2) and titania (TiO2). Theoretical results were obtained using 2×2 transfer matrix calculation method. Technological process of SiO2 and TiO2 thin film fabrication as well as measurement techniques are described in this paper. Strong correlation between theoretical and experimental data is demonstrated. It is shown, that weighted average reflection from a substrate can be reduced ten times with the use of SiO2/TiO2/Si double layer ARCs, when compared to a bare silica substrate.

  19. Organic-inorganic hybrid superhydrophobic surfaces using methyltriethoxysilane and tetraethoxysilane sol-gel derived materials in emulsion

    NASA Astrophysics Data System (ADS)

    Wen, Xiu-Fang; Wang, Kun; Pi, Pi-Hui; Yang, Jin-Xin; Cai, Zhi-Qi; Zhang, Li-juan; Qian, Yu; Yang, Zhuo-Ru; Zheng, Da-feng; Cheng, Jiang

    2011-11-01

    By applying alkaline-catalyzed co-hydrolysis and copolycondensation reactions of tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES) in organic siloxane modified polyacrylate emulsion (OSPA emulsion), we are able to demonstrate the potential for developing a sol-gel derived organic-inorganic hybrid emulsion for a superhydrophobic surface research. TEOS and MTES derived sol-gel moieties can be designed for a physical roughness and hydrophobic characteristic (Si-CH3) of the hybrid superhydrophobic surface, while OSPA emulsion can be endowed for good film-forming property. The effect of formulation parameters on superhydrophobicity and film-forming property was analyzed. The water contact angle (WCA) on the sol-gel derived hybrid film is determined to be 156°, and the contact angle hysteresis is 5° by keeping the mole ratio of TEOS:MTES:C2H5OH:NH3·H2O:AMP-95 at 1:4:30:10:0.63 and the mass percentage of OSPA emulsion at 25%. The nanoparticle-based silica rough surface is observed as the mole ratio of MTES/TEOS at 4:1. The sol-gel derived organic-inorganic hybrid emulsion shows remarkable film-forming property when the mole ratio of MTES/TEOS reaches or exceeds 4:1. With the primer coating, the performance of superhydrophobic film achieve actual use standard. It reveals that this new procedure is an effective shortcut to obtain a superhydrophobic surface with potential applications.

  20. Extradiol dioxygenase-SiO₂ sol-gel modified electrode for catechol and its derivatives detection.

    PubMed

    Zhang, Qiang; Qu, Yuanyuan; Zhang, Xuwang; Zhou, Jiti; Wang, Hongtao

    2011-07-15

    A feasible and sensitive biosensor for catechol and its derivatives using 2,3-dihydroxybiphenyl 1,2-dioxygenase (BphC)-modified glassy carbon electrode was successfully constructed by polyvinyl alcohol-modified SiO₂ sol-gel method. The as-prepared biosensor was characterized by electrochemical impedance spectroscopy, and the surface topography of the film was imaged by atomic force microscope. Liquid chromatography-tandem mass spectrometry was applied to reveal the catalytic mechanism. BphC embedded in SiO₂ gel maintained its bioactivity well and exhibited excellent eletrocatalytical response to both catechol and some of its derivatives (such as 3-methylcatechol and 4-methylcatechol). The biosensor showed a linear amperometric response range between 0.002 mM and 0.8 mM catechol. And the sensitivity was 1.268 mA/(mM cm²) with a detection limit of 0.428 μM for catechol (S/N = 3). Furthermore, the BphC biosensor exhibited perfect selectivity for catechol in the mixtures of catechol and phenol. It was suggested that this flexible protocol would open up a new avenue for designing other ring-cleavage enzyme biosensors, which could be widely used for monitoring various kinds of environmental pollutants.

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

    PubMed

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

    2016-09-20

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

  2. Ferroelectric Properties of CaBi4Ti4O15 Thin Films on Ito/glass Substrates Prepared by Sol-Gel Technology

    NASA Astrophysics Data System (ADS)

    Cheng, Chien-Min; Kuan, Ming-Chang; Chen, Kai-Hunag; Tsai, Jen-Hwan

    In this study, ferroelectric CaBi4Ti4O15 (CBT) thin films prepared by sol-gel method and deposited on ITO/glass substrates for applications in system-on-panel (SOP) devices were fabricated and investigated. The electrical and physical characteristics of as-deposited and annealed CBT thin films for metal-ferroelectric-metal (MFM) structures was discussed and investigated. In addition, the ferroelectric properties in annealed CBT thin films on ITO/glass substrate showed and exhibited clear polarization versus electrical field curves. From p-E curves, the 2Pr value and coercive field of annealed CBT thin films were calculated to be 10μC/cm2 and 180 kV/cm, respectively. Finally, the maximum capacitance, leakage current density, and transmittance within the ultraviolet-visible (UV-vis) spectrum were also investigated and discussed.

  3. Sol-gel-derived AgCl photochromic coating on glass for holographic application

    NASA Astrophysics Data System (ADS)

    Mennig, Martin; Krug, Herbert; Fink-Straube, Claudia; Oliveira, Peter W.; Schmidt, Helmut K.

    1992-12-01

    A sol-gel derived photochromic glass coating of about 1.5 micrometers in thickness is synthesized by infiltration of Ag+ into a predried Na-Al-B-Si gel layer. The formation of small Ag colloids is initiated by a soft heat treatment and the colloids are converted by a HCl vapor treatment into AgCl crystallites of about 40 nm in diameter. The coating darkens by UV irradiation, forming Ag crystallites of about 5 nm in size. This process is completely reversible at 400 degree(s)C and no decay is observed in numerous cycles. An amplitude hologram which acts as a diffraction grating with a grating period of about 10 micrometers can be produced within this layer by a two-wave mixing experiment with laser light of 351 nm wavelength. The diffraction efficiency of this grating is determined to 0.11%. After thermal erasing the diffraction pattern can be rewritten and erased repeatedly without any loss of efficiency.

  4. Structural characterization of sol-gel derived siloxane-oxide materials

    SciTech Connect

    Babonneau, F.; Dire, S.

    1993-12-31

    Sol-gel processing of hybrid siloxane-oxide materials is currently widely investigated due to a large amount of potential applications for these systems. They are usually based on silicon alkoxides and derivatives. Various new materials have been prepared combining a modified silicon alkoxide, diethoxydimethylsilane (DEDMS) and a transition metal alkoxide, M(OR){sub n} with M=Ti and Zr. Transparent monolithic pieces or thick films can be obtained over a wide range of compositions. The hydrolysis process of various preparations was followed by {sup 29}Si liquid NMR, and indicates the formation of Si-O-M bonds. The structure of the final gels was essentially characterized by solid state NMR ({sup 1}H, {sup 13}C and {sup 29}Si) and X-ray absorption spectroscopies (Ti K-edge), and leads to propose structural models for these gels. This study points out that titanium and zirconium alkoxides does not only act as cross linking agents, such as silicon alkoxides, but behave as catalysts for the formation of polydimethylsiloxane chains within the materials.

  5. The influence of sol-gel-derived silica coatings functionalized with betamethasone on adipose-derived stem cells (ASCs).

    PubMed

    Donesz-Sikorska, Anna; Grzesiak, Jakub; Smieszeka, Agnieszk; Krzak, Justyna; Marycz, Krzysztof

    2014-09-01

    Silica-based sol-gel coatings have gained attention in bone therapies and orthopedic applications, due to the biocompatibility and bioactivity, including a high potential for the controlled release both in vitro and in vivo. Bioactive materials are created to facilitate the biocompatibility of orthopedic implants. One of the promising alternatives is biomaterials with immobilized drugs. In this study we demonstrated for the first time novel sol-gel-derived silica coatings with active amino groups (SiO2(NH2)) functionalized with a steroid drug-betamethasone, applied to a substrate 316 L using dip coating technique. The presence of betamethasone in functionalized coatings was directly confirmed by Raman spectroscopy and energy-dispersive X-ray spectroscopic analysis. The wettability was evaluated by the sessile drop method, while the surface free energy was estimated based on the contact angles measured. Our results showed a shift in surface properties from hydrophobic to hydrophilic after application of the coatings. We have investigated the morphology, proliferation factor, and the population doubling time of adipose-derived stem cells for biological purposes. Moreover, the analysis of the distribution and localization of cellular microvesicles was performed to evaluate the influence of functionalized surfaces on cellular cytophysiological activity. Increased proliferation and activation of cells, determined by the observations of microvesicles shedding processes, provided evidence of the availability of the drug. Therefore, we conclude that the sol-gel synthesis proposed here allows to improve the metal substrates and can be successfully used for immobilization of betamethasone. This in turn enables the direct delivery of the drug with implanted material into the wound site, and to stimulate the activity of cells to enhance tissue regeneration.

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

    NASA Astrophysics Data System (ADS)

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

    2001-06-01

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

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

    PubMed

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

    2015-09-28

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

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

    PubMed Central

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

    2015-01-01

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

  10. Surface aspects of sol-gel derived hematite films for the photoelectrochemical oxidation of water.

    PubMed

    Herrmann-Geppert, Iris; Bogdanoff, Peter; Radnik, Jörg; Fengler, Steffen; Dittrich, Thomas; Fiechter, Sebastian

    2013-02-07

    α-Fe(2)O(3) (hematite) photoanodes for the oxygen evolution reaction (OER) were prepared by a cost-efficient sol-gel procedure. Due to low active photoelectrochemical properties observed, it is assumed that the sol-gel procedure leads to hematite films with defects and surface states on which generated charge carriers are recombined or immobilized in trap processes. Electrochemical activation was proven to diminish unfavourable surface groups to some extent. More efficiently, a plasma treatment improves significantly the photoelectrochemical properties of the OER. X-ray photoelectron spectroscopy (XPS) analysis reveals an oxygen enriched surface layer with new oxygen species which may be responsible for the improved electrochemical activity. Due to surface photovoltage an increased fraction of transferred charge carriers from these newly produced surface defects are identified.

  11. Molecular imprinting in sol-gel matrix.

    PubMed

    Gupta, Radha; Kumar, Ashok

    2008-01-01

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

  12. Sol-gel hosts doped with porphyrin derivatives. Part I. Spectroscopy, hole-burning and spectral diffusion

    NASA Astrophysics Data System (ADS)

    Kulikov, S. G.; Veret-Lemarinier, A. V.; Galaup, J. P.; Chaput, F.; Boilot, J. P.

    1997-03-01

    Pure inorganic sol-gel matrices as well as hybrid organic/inorganic xerogels have been doped with porphyrins derivatives and studied using line narrowing techniques. The role of residual hydroxyl groups is investigated. Free-base porphyrins are protonated in pure inorganic hosts, but the matrix acidity is reduced in hybrid matrices or when fluorinated porphyrins derivatives are used. The linear electron-phonon coupling can be controlled with the choice of the organic group in organic/inorganic matrices. Persistent spectral hole widths increase with temperature according a glass-like Tn dependence and evidence of spectral diffusion is shown in one of these systems.

  13. Sol-gel derived precursors to Group 14 semiconductor nanocrystals - Convenient materials for enabling nanocrystal-based applications

    NASA Astrophysics Data System (ADS)

    Veinot, Jonathan G. C.; Henderson, Eric J.; Hessel, Colin M.

    2009-11-01

    Semiconductor nanocrystals are intriguing because of their electronic, optical, and chemical characteristics. Silicon nanocrystals (Si-NCs) of sub-5 nm dimension are of particular interest due to their intense photoluminescent response and the promise of linking silicon photonics and electronics. Other related nanomaterials of technological importance include SiC and Ge. The following contribution describes key experimental findings pertaining to synthetic methodology, investigation of nanodomain formation and growth, as determined by X-ray powder diffraction (XRD) and photoluminescence (PL) spectroscopy for a series of sol-gel derived prepolymers suitable for preparing Group 14 based nanocrystal containing composites.

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

    NASA Astrophysics Data System (ADS)

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

    2008-08-01

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

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

    NASA Astrophysics Data System (ADS)

    Selmi, Fathi A.

    This thesis consists of two areas of research: (1) sol-gel processing of Ba_{rm 1-x}Sr_{rm x} TiO_3 ceramics and their dielectric properties measurement; and (2) microwave versus conventional sintering of ceramics such as Al_2 O_3, Ba_{ rm 1-x}Sr_{rm x}TiO_3, Sb-doped SnO _2 and YBa_2Cu _3O_7. Sol-gel powders of BaTiO_3, SrTiO_3, and their solid solutions were synthesized by the hydrolysis of titanium isopropoxide and Ba and Sr methoxyethoxides. The loss tangent and dielectric constant of both sol-gel and conventionally prepared and sintered Ba_{rm 1-x}Sr _{rm x}TiO _3 ceramics were investigated at high frequencies. The sol-gel prepared ceramics showed higher dielectric constant and lower loss compared to those prepared conventionally. Ba _{rm 1-x}Sr _{rm x}TiO_3 ceramics were tunable with applied bias, indicating the potential use of this material for phase shifter applications. Porous Ba_{0.65}Sr _{0.35}TiO_3 was also investigated to lower the dielectric constant. Microwave sintering of alpha -Al_2O_3 and SrTiO_3 was investigated using an ordinary kitchen microwave oven (2.45 GHz; 600 Watts). The use of microwaves with good insulation of alpha -Al_2O_3 and SrTiO_3 samples resulted in their rapid sintering with good final densities of 96 and 98% of the theoretical density, respectively. A comparison of grain size for conventionally and microwave sintered SrTiO_3 samples did not show a noticeable difference. However, the grain size of microwave sintered alpha-Al_2O _3 was found to be larger than that of conventionally sintered sample. These results show that rapid sintering of ceramics can be achieved by using microwave radiation. The sintering behavior of coprecipitated Sb-doped SnO_2 was investigated using microwave power absorption. With microwave power, samples were sintered at 1450^circC for 20 minutes and showed a density as high as 99.9% of theoretical. However, samples fired in a conventional electric furnace at the same temperature for 4 hours showed only

  16. Identification of Ti clusters during nucleation and growth of sol-gel-derived TiO2 nanoparticles.

    PubMed

    Simonsen, Morten Enggrob; Søgaard, Erik Gydesen

    2013-01-01

    In the present work, electrospray ionization mass spectrometry (ESI-MS) was used to investigate the titanium clusters present during nucleation and growth of sol-gel derived TiO2 nanoparticles. Depending on the alkoxide precursor used, Ti clusters of different sizes were identified [titanium isopropoxide (TTIP)-11-12 Ti atoms, titanium butoxide (TTB)-10-11 Ti atoms and titanium tetraethoxide (TTE)-5-7 Ti atoms]. The Ti-O-Ti backbone/core of the titanium clusters were found to be quite stable after formation and do not easily break up into smaller clusters. The results of this investigation suggest that these clusters are used as building blocks in the growth during the induction period. The h-ratio (n H2O/n alcoxide) and the pH were not found to influence the identity of the Ti clusters present during nucleation of the growth of sol-gel derived TiO2 nano-particles, although the induction period was greatly influenced. The reactivity of the alkoxy group are OEt > OPri > OBu. The difference in reactivity of the alkoxides is generally believed to be due to the increasing size of the alkoxy group which causes sterical hindrance during the nucleophilic substitution reaction.

  17. Sol-gel derived nanoscale bioactive glass (NBG) particles reinforced poly(ε-caprolactone) composites for bone tissue engineering.

    PubMed

    Lei, Bo; Shin, Kwan-Ha; Noh, Da-Young; Jo, In-Hwan; Koh, Young-Hag; Kim, Hyoun-Ee; Kim, Sung Eun

    2013-04-01

    This study investigated the effect of the addition of sol-gel derived nanoscale bioactive glass (NBG) particles on the mechanical properties and biological performances of PCL polymer, in order to evaluate the potential applications of PCL/NBG composites for bone tissue regeneration. Regardless of the NBG contents (10, 20, and 30 wt.%), the NBG particles, which were synthesized through the sol-gel process using polyethylene glycol (PEG) polymer as a template, could be uniformly dispersed in the PCL matrix, while generating pores in the PCL/NBG composites. The elastic modulus of the PCL/NBG composites increased remarkably from 89±11 MPa to 383±50 MPa with increasing NBG content from 0 to 30 wt.%, while still showing good ultimate tensile strength in the range of 15-19 MPa. The hydrophilicity, water absorption and degradation behavior of the PCL/NBG composites were also enhanced by the addition of the NBG particles. Furthermore, the PCL/NBG composite with a NBG content of 30 wt.% showed significantly enhanced in vitro bioactivity and cellular response compared to those of the pure PCL.

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

  19. Electrochemical characterization of thio sol-gel derived titanium sulfide (TiS{sub 2}) powders with unique morphologies

    SciTech Connect

    Sriram, M.A.; Kumta, P.N.

    1996-12-31

    A novel thio sol-gel process utilizing titanium alkoxide as the metal source has been used to synthesize TiS{sub 2} powders exhibiting uniquely different morphologies. The pure alkoxide and its partially modified form using benzene sulfonic acid (BSA) have been reacted with H{sub 2}S to yield a solid precursor. Upon heat treatment in flowing H{sub 2}S the precursors were converted to TiS{sub 2} exhibiting distinctly different morphologies. These powders have been characterized for their chemical stoichiometry (using X-ray diffraction). At the same time the sulfide was also prepared using conventional techniques involving the reaction of the individual elements in a sealed evacuated quartz ampoule at elevated temperatures of 500{degrees}C. The morphologies of both, the thio sol-gel derived and conventionally synthesized powders have been compared using scanning electron microscopy (SEM). Preliminary electrochemical tests were also performed by fabricating test cathodes of these materials and using them in {open_quotes}hockey puck{close_quotes} cells incorporating lithium as both the anode and the reference electrodes. These studies were conducted to analyze the effect of the different morphologies of the synthesized powders on their electrochemical performance.

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

    SciTech Connect

    Shiquan Tao

    2006-12-31

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

  1. Magnetization and Magnetocaloric Effect in Sol-Gel Derived Nanocrystalline Copper-Zinc Ferrite.

    PubMed

    Anwar, M S; Ahmed, Faheem; Koo, Bon Heun

    2015-02-01

    We report the sol-gel synthesis and magnetocaloric effect in nanocrystalline copper-zinc ferrite (Cu0.5Zn0.5Fe2O4). The synthesized powder was characterized by using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and magnetization measurements. The XRD results confirm the formation of single phase spinel structure. The average particle size was found to be ~58 nm. FE-SEM results suggested that the nanoparticles are agglomerated and spherical in shape. Magnetization measurement reveals that Cu0.5Zn0.5Fe2O4 nanoparticles exhibit transition temperature (Tc) above room temperature. The maximum magnetic entropy change (ΔSM)max shows interesting behaviour and was found to vary with the applied magnetic field. This nanopowder can be considered as potential material for magnetic refrigeration above room temperature.

  2. Optical, dielectric and morphological studies of sol-gel derived nanocrystalline TiO2 films.

    PubMed

    Vishwas, M; Sharma, Sudhir Kumar; Narasimha Rao, K; Mohan, S; Gowda, K V Arjuna; Chakradhar, R P S

    2009-10-15

    Nanocrystalline TiO(2) films have been synthesized on glass and silicon substrates by sol-gel technique. The films have been characterized with optical reflectance/transmittance in the wavelength range 300-1000 nm and the optical constants (n, k) were estimated by using envelope technique as well as spectroscopic ellipsometry. Morphological studies have been carried out using atomic force microscope (AFM). Metal-Oxide-Silicon (MOS) capacitor was fabricated using conducting coating on TiO(2) film deposited on silicon. The C-V measurements show that the film annealed at 300 degrees C has a dielectric constant of 19.80. The high percentage of transmittance, low surface roughness and high dielectric constant suggests that it can be used as an efficient anti-reflection coating on silicon and other optical coating applications and also as a MOS capacitor.

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

  4. Optical and morphological properties of sol gel derived titanium dioxide films

    NASA Astrophysics Data System (ADS)

    Sharma, A. B.; Sharma, S. K.; M, Vishwas; Rao, K. Narasimha

    2015-08-01

    Titanium oxide (Titania) thin films were synthesized on different substrates via the sol-gel dip-coating method using alkoxide solution. Some selected samples were also prepared with different percentage of Lead (Pb). The influence of Pb addition in precursor sol on the optical properties of titanium dioxide thin films was studied. The optical transmittance in the visible region has increased with increase in weight percentage of lead. The refractive index was slightly decreased with Pb addition. Crystallization of these coatings was achieved through thermal annealing at temperatures above 400 °C. The structural properties and surface morphology of the crystallized coatings were studied by Scanning Electron Microscopy. Increase in average grain size from 250 nm to 350 nm with increase in Pb concentration is observed. Films were appeared to more coarse with increase in Pb addition. An increase in Pb addition resulted increase in average roughness from 12 nm to 25 nm.

  5. Thermal stability of a modified sol-gel derived hydroxyapatite nanopowders

    NASA Astrophysics Data System (ADS)

    Herradi, S.; El Bali, B.; Khaldi, M.; Lachkar, M.

    2017-03-01

    Hydroxyapatite Ca10(PO4)6(OH)2 (HA) powder was successfully synthesized by a modified sol-gel method using a solution of calcium nitrate in ethanol, along with a solution of diammonium hydrogen phosphate in water and NH4OH as starting materials. The Ca/P molar ratio was maintained at 1.67. The powder was subjected to furnace and microwave heating to compare the decomposition of HA and study the crystallite sizes. It was found that microwave heated powders were pure HAP up to 230°C with absence of secondary phases. However, XRD patterns show that furnace heated powders convert completely to β-TCP when treated at 750°C and 1000°C. This result was confirmed by the absence of hydroxyl bands in the FT-IR spectra for these temperatures.

  6. Optical and morphological properties of sol gel derived titanium dioxide films

    SciTech Connect

    Sharma, A. B.; Sharma, S. K.; M, Vishwas; Rao, K. Narasimha

    2015-08-28

    Titanium oxide (Titania) thin films were synthesized on different substrates via the sol-gel dip-coating method using alkoxide solution. Some selected samples were also prepared with different percentage of Lead (Pb). The influence of Pb addition in precursor sol on the optical properties of titanium dioxide thin films was studied. The optical transmittance in the visible region has increased with increase in weight percentage of lead. The refractive index was slightly decreased with Pb addition. Crystallization of these coatings was achieved through thermal annealing at temperatures above 400 °C. The structural properties and surface morphology of the crystallized coatings were studied by Scanning Electron Microscopy. Increase in average grain size from 250 nm to 350 nm with increase in Pb concentration is observed. Films were appeared to more coarse with increase in Pb addition. An increase in Pb addition resulted increase in average roughness from 12 nm to 25 nm.

  7. Active fibers from sol-gel derived granulated silica: state of the art and potential

    NASA Astrophysics Data System (ADS)

    Romano, Valerio; Sandoz, Frederic

    2010-10-01

    In the recent past we have studied the granulated silica method as a versatile and cost effective way of fiber preform production. We have used the sol-gel technology combined with a laser-assisted remelting step to produce high homogeneity Rare Earth or Transition Metal - activated microsized particles for the fiber core. For the fiber cladding pure or index-raised granulated Silica has been employed. Silica glass tubes, appropriately filled with these granular materials, are then drawn to fibers, eventually after an optional quality enhancing vitrification step. The process offers a high degree of compositional flexibility with respect to dopants; it further facilitates to achieve high concentrations even in cases when several dopants are used. By this "rapid preform production" technique, that is also ideally suited for the preparation of microstructured optical fibers, several fibers ranging from broadband emitters, PCFs and large mode area fibers have been produced and will be presented here.

  8. Characterization of the structure of sol-gel-derived hydroxyapatite thin films

    NASA Astrophysics Data System (ADS)

    Lopatin, Craig Michael

    The synthesis and processing of hydroxyapatite (Ca10[PO 4]6[OH]2, HA) thin films was investigated. Films 10 to 900 nm thick were synthesized using solution chemistry sol-gel techniques and processed under various conditions. Analytical chemistry techniques (NMR, TLC, titration) were used to study the initial reactions. It was found that several key sol-gel synthesis steps were either absent (hydrolysis) or minimally present (network formation). These results are consistent with the findings that the films have little skeletal structure, but are composed of crystalline aggregates and inter-granular pores. Ion-implantation using silicon ions was used to densify the films from a density of 36% (of fully dense HA) to 83%. High temperature annealing was also used to densify the films, and 40% densification could be achieved after firing at 800°C. While larger densification can be reached at higher temperatures, the film transforms from HA to other calcium phosphate phases. The kinetics of transformation from the amorphous gel state was studied using X-ray diffraction (XRD), and Time-Temperature-Transformation (TTT) curves were constructed. These curves demonstrated that the transformation kinetics are extremely rapid and likely related to the short chain phosphate groups (dimers and trimers) present in the amorphous gel. Thus, high temperature sintering, even using rapid heating rates, can not be used to achieve high densities. A new technique, solute impregnation, was developed to further characterize the porosity of the films. The results of the solute impregnation tests demonstrated that (a) the films have an open pore structure and (b) high temperature firing and ion implantation decreased the porosity of the films. Studies with transmission electron microscopy demonstrated that the porosity is due to inter-granular pores, and that the grains were essentially fully dense, a result confirmed by pycnometry. These results are consistent with the observation that the

  9. Sol-gel derived silica/siloxane composite materials: The effect of loading level and catalyst activity on silica domain formation

    SciTech Connect

    Black, E.P.; Ulibarri, T.A.; Beaucage, G.; Schaefer, D.W.; Assink, R.A.; Bergstrom, D.F.; Giwa-Agbomeirele, P.A.; Burns, G.T.

    1993-11-01

    Currently, the production of in situ reinforcement in polymeric systems by sol-gel methods is undergoing rapid development. However, understanding of synthesis/structure/property relationships is still lacking. In order to produce sol-gel derived composite materials with sufficient mechanical properties for commercial applications, this deficit of information must be addressed. We have completed a detailed investigation of in situ silica growth in polydimethylsiloxane (PDMS)/tetraethylorthosilicate (TEOS) systems. Factors which affect the domain growth, such as catalyst activity and silica loading, have been examined by solid state {sup 29}Si NMR, SEM, mechanical testing and small angle neutron scattering.

  10. Antibacterial effects of sol-gel-derived bioactive glass nanoparticle on aerobic bacteria.

    PubMed

    Mortazavi, V; Nahrkhalaji, M Mehdikhani; Fathi, M H; Mousavi, S B; Esfahani, B Nasr

    2010-07-01

    The aim of this work was to evaluate the antibacterial effect of bioactive glass nanopowders. The 58S, 63S, and 72S compositions were prepared via the sol-gel technique. Characterization techniques such as X-ray diffraction, transmission electron microscopy (TEM), Zetasizer, and X-ray fluorescent were used. The antibacterial activity was studied using Escherichia coli, Pseudomonas aeruginosa, Salmonella typhi, and Staphylococcus aureus. Cytotoxicity of the samples was evaluated using mouse fibroblast L929 cell line. The chemical compositions of the prepared samples were as predicted, and the particle size of the samples with an amorphous structure mainly ranged over 20-90 nm. At broth concentrations below 50 mg/mL, they showed no antibacterial activity. The 58S showed the highest antibacterial activity with the minimum bactericidal concentrations of 50 and 100 mg/mL for E. coli plus S. aureus and for P. aeruginosa, respectively. The 63S exhibited bactericidal and bacteriostatic effects on E. coli and S. aureus at concentrations of 100 and 50 mg/mL, respectively, at an minimum bactericidal concentrations of 100 mg/mL. However, 72S bioactive glass nanopowder showed no antibacterial effect. They showed no cytotoxicity. It was concluded that bioactive glass nanopowders could be considered as good candidates for the treatment of oral bone defects and root canal disinfection. (c) 2010 Wiley Periodicals, Inc. J Biomed Mater Res, 2010.

  11. Sol-gel derived fluor-hydroxyapatite biocoatings on zirconia substrate.

    PubMed

    Kim, Hae-Won; Kong, Young-Min; Bae, Chang-Jun; Noh, Yoon-Jung; Kim, Hyoun-Ee

    2004-07-01

    Fluor-hydroxyapatite (FHA) film was coated on a zirconia (ZrO(2)) substrate by a sol-gel method. An appropriate amount of F ions was incorporated into the hydroxyapatite (HA) during the preparation of the sols. The apatite phase began to crystallize after heat treatment at 400 degrees C, and increased in intensity above 500 degrees C. No decomposition was detected by X-ray diffraction analyses up to 800 degrees C, which illustrates the high thermal stability of the FHA films. The films showed a uniform and dense morphology with a thickness of approximately 1 microm after a precisely controlled heat treatment process. These FHA films adhered firmly to the zirconia substrate, representing notable adhesion strengths of approximately 70 MPa after heat treatment above 500 degrees C. The dissolution rate of the FHA coating layer varied according to the heat treatment temperature, which was closely related to the film crystallinity. The dissolution rate of the FHA film was lower than that of the HA film, suggesting the possibility of a functional gradient coating of HA and FHA. The MG63 cells seeded onto the FHA films proliferated in a similar manner to those seeded onto pure HA ceramic and a plastic control.

  12. Effect of aging temperature on formation of sol-gel derived fluor-hydroxyapatite nanoparticles.

    PubMed

    Joughehdoust, S; Behnamghader, A; Jahandideh, R; Manafi, S

    2010-04-01

    Synthetic hydroxyapatite (HA) has been recognized as one of the most important bone substitute materials in orthopaedics and dentistry over past few decades because of its chemical and biological similarity to the mineral phase of human bone. One solution for reduction the solubility of HA in biological environments is replacing F- by OH in HA structure and forming fluor-hydroxyapatite (FHA) solid solution. In this paper, FHA nanoparticles were successfully synthesized by a sol-gel method. Also, the influence of aging temperature on formation of FHA powder was studied. Equimolar solutions of calcium nitrate tetrahydrate, triethyl phosphite and ammonium fluoride in ethanol were used as Ca, P and F precursors. After aging at different temperatures, the synthesized powders were heat treated at 550 degrees C. The powders were investigated with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), selected area electron diffraction pattern (SAED), energy dispersive analysis of X-ray (EDAX) and zetasizer measurement. The results of XRD proved the presence of fluorapatite (FA) and HA in all samples. In addition, the formation of FHA was confirmed by FT-IR results. XRD studies also showed that the crystallites were in nanometric scale. At the same time, this result was in good agreement with the result of zetasizer analysis.

  13. Electrochemical Urea Biosensor Based on Sol-gel Derived Nanostructured Cerium Oxide

    NASA Astrophysics Data System (ADS)

    Ansari, Anees A.; Azahar, Md; Malhotra, B. D.

    2012-04-01

    Urease (Urs) and glutamate dehydrogenase (GLDH) have been co-immobilized onto a nanostructured-cerium oxide (Nano-CeO2) film deposited onto a indium-tin-oxide (ITO) coated glass substrate by dip-coating via sol-gel process for urea detection. This nanostructured film has characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR), Scanning electron microscope (SEM) and electrochemical techniques, respectively. The particle size of the Nano-CeO2 film has been found to be 23 nm. Electrochemcial response (CV) studies show that Ur-GLDH/Nano-CeO2/ITO bioelectrode is found to be sensitive in the 10-80 mg/dL urea concentration range and can detect urea concentration upto 0.1 mg/dL level. The value of Michaelis-Menten constant (Km) estimated using Lineweaver-Burke plot found as 6.09 mg/dL indicates enhancement in the affinity and/or activity of enzyme attached to their nanobiocomposite. This bioelectrode retained 95% of enzyme activity after 6 months at 4°C.

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

    PubMed

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

    2008-01-01

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

  15. Preparation of sol-gel derived microcrystalline corundum abrasives with hexagonal platelets

    NASA Astrophysics Data System (ADS)

    Li, Na; Zhu, Yu-Mei; Gao, Kai; Li, Zhi-Hong

    2013-01-01

    The effects of different additives on the mechanical properties, microstructures, and wear behavior of corundum abrasives were investigated. When the number of additive phases increases, the sintering temperature and wear rate decrease, while the densification and mechanical properties increase. The additive SiO2 is responsible for the development of equiaxed grains, whereas both CaO and MgO promote the development of platelike grains. By controlling the molar ratio of additives, it is possible to obtain different microstructures. With SiO2-MgO-CaO (molar ratio, 2:1:1) as the additives and nano α-Al2O3 powders as the seed, microcrystalline corundum abrasives with hexagonal platelets were obtained using sol-gel process by sintering at 1300°C for 0.5 h. The average diameter and thickness of hexagonal platelets are 1.38 μm and 360 nm respectively, the single-particle compressive strength is 26.44 N, and the wear rate is (3.06±0.21)×10-7 mm3/(N·m).

  16. Surface properties of in vitro bioactive and non-bioactive sol-gel derived materials.

    PubMed

    Viitala, R; Jokinen, M; Peltola, T; Gunnelius, K; Rosenholm, J B

    2002-08-01

    The acid-base properties of several in vitro bioactive (able to form bone mineral-like calcium phosphate on their surfaces) and non-bioactive sol-gel processed oxides are studied. The amount of Lewis acid sites was calculated from the pyridine adsorption using the Langmuir adsorption model. The Henry adsorption model was used in cases where no specific affinity between the adsorbent and the probe molecule was observed. The results were used to calculate the specific amounts of acidic and basic sites on SiO2- and TiO2-based materials. The zeta potential was measured for dip-coated TiO2 films, calcium- and phosphate-doped TiO2 films and for a non-bioactive Al2O3 film. Also, the calcium phosphate formation in simulated body fluid on in vitro bioactive TiO2 film was studied with zeta potential measurements. The results showed dependence on the negative surface charge and the important role of calcium adsorption in the beginning of the calcium phosphate formation. Surface topography of the films was investigated with atomic force microscopy, including a detailed analysis of the peak heights and distribution over cross sections. It was observed that in vitro bioactivity was strongly dependent on the nanoscale dimensions. Consequently, the in vitro calcium phosphate formation seems to be due to both the chemical interactions and the surface structure.

  17. Synthesis and in vitro investigation of sol-gel derived bioglass-58S nanopowders

    NASA Astrophysics Data System (ADS)

    Joughehdoust, S.; Manafi, S.

    2012-03-01

    The aim of this research is the synthesis of bioglass-58S nanopowders by sol-gel method. Also, the effect of aging time of parent sols on the morphology, structure and particle size was investigated. Bioglass-58S powders were analyzed by X-ray diffraction patterns (XRD), Fourier transform infrared spectroscopy (FTIR), zetasizer instrument, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The XRD results showed that the powder is amorphous and glassy. According to FTIR spectroscopy, silicate bonds were formed in all powders. Zetasizer curves proved that the particle sizes of the powders and agglomerates have increased with aging time. The SEM images confirmed these results, too. Additionally, the TEM observations revealed that the increase of aging time caused the growth of grains with the size between 50-200 nm. The in vitro biological behavior of bioglass-58S powders were investigated by immersing the bioglass discs (made from the powders) in the simulated body fluid (SBF). The XRD patterns and SEM images confirmed the formation of the hydroxyapatite (HA) phase.

  18. Sol-gel-derived silica films with tailored microstructures for applications requiring organic dyes

    SciTech Connect

    Logan, M.N.; Prabakar, S.; Brinker, C.J. |

    1994-09-01

    A three-step sol-gel process was developed to prepare organic dye-doped thin films with tailored porosity for applications in chemical sensing and optoelectronics. Varying the acid- and base-catalyzed hydrolysis steps of sols prepared from tetraethoxysilane with identical final H{sub 2}O/Si ratios, dilution factors and pH resulted in considerably different distributions of the silicate polymers in the sol (determined by {sup 29}Si NMR) and considerably different structures for the polymer clusters (determined by SAXS). During film formation these kinetic effects cause differences in the packing and collapse of the silicate network, leading to thin films with different refractive indices and volume fraction porosities. Under conditions where small pore-plugging species were avoided, the porosities of as-deposited films could be varied by aging the sol prior to film deposition. This strategy, which relies on the growth and aggregation of fractal polymeric clusters, is compatible with the low temperature and near neutral pH requirements of organic dyes.

  19. Multifunctional sol-gel derived thin film based on nanocrystaline hydroxyapatite powders

    NASA Astrophysics Data System (ADS)

    El hadad, A. A.; Barranco, V.; Jiménez-Morales, A.; Peon, E.; Galván, J. C.

    2010-11-01

    The aim of this work was to prepare bioactive hydroxyapatite coatings by sol-gel method and to study the effect of thermal treatment temperature upon the bioactivity and corrosion protection of these coatings on Ti6Al4V alloy. The application of (DTA/TGA) and (XRD) has provided valuable information about the phase transformation, mass loss, identification of the phases developed, crystallite size and degree of crystallinity. (SEM/EDX) has been applied to study the surface morphology of coated samples before and after immersion in simulated body fluid (SBF) to detect the biomimetic precipitation of the bonelike apatite. The obtained results show that all the prepared samples are ceramic nanocrystalline with crystal structure and composition like hydroxyapatite, with little deviations from that present in the human bone. The bioactivity of the studied samples is found to be closely related to the thermal treatments applied. That is, the bioactivity decreases as the temperature of the thermal treatment increase. Coatings from such prepared hydroxyapatite sol have been accomplished by dip-coating technique on non-toxic Ti6Al4V alloy for biomedical applications. The corrosion behaviour of the resulting hydroxyapatite coatings in a (SBF) has been studied by electrochemical impedance spectroscopy (EIS). The hydroxyapatite coated Ti6Al4V alloy displayed excellent bioactivity when soaked in the (SBF) and acceptable corrosion protection behaviour.

  20. Sol-gel-derived hybrid materials multi-doped with rare-earth metal ions

    NASA Astrophysics Data System (ADS)

    Zelazowska, E.; Rysiakiewicz-Pasek, E.; Borczuch-Laczka, M.; Cholewa-Kowalska, K.

    2012-06-01

    Four different hybrid organic-inorganic materials based on TiO2-SiO2 matrices with organic additives and doped with rare-earth metal ions (III) from the group of europium, cerium, terbium, neodymium, dysprosium and samarium, were synthesized by sol-gel method. Tetraethyl orthosilicate, titanium (IV) isopropoxide and organic compounds, such as butyl acrylate, butyl methacrylate, ethyl acetoacetate, ethylene glycol dimethacrylate, ethyl acetate, propylene carbonate, organic solvents and certain inorganic salts were used in the synthesis. The inorganic part of the sols, which were used in the synthesis of all the hybrid materials, was prepared separately and then the organic parts were added. The materials obtained were aged for three weeks at room temperature and then heated in an electric oven for three hours at temperatures of 80 °C-150 °C. Scanning electron microscopy equipped with energy dispersive X-ray spectroscopy (SEM/EDX); X-ray diffraction (XRD); Fourier transform infrared spectroscopy (KBr technique); 29Si magic-angle spinning nuclear magnetic resonance; and fluorescence spectroscopy were used for the examination of morphology, microstructure and luminescence properties, respectively. Photoluminescence properties with relatively intense narrow emission lines of Tb, Eu, Dy, Nd, Sm respectively to the RE-ions doping, were observed for all the hybrid materials.

  1. Sol-Gel-Derived Hydroxyapatite-Carbon Nanotube/Titania Coatings on Titanium Substrates

    PubMed Central

    Ji, Xiaoli; Lou, Weiwei; Wang, Qi; Ma, Jianfeng; Xu, Haihong; Bai, Qing; Liu, Chuantong; Liu, Jinsong

    2012-01-01

    In this paper, hydroxyapatite-carbon nanotube/titania (HA-CNT/TiO2) double layer coatings were successfully developed on titanium (Ti) substrates intended for biomedical applications. A TiO2 coating was firstly developed by anodization to improve bonding between HA and Ti, and then the layer of HA and CNTs was coated on the surface by the sol-gel process to improve the biocompatibility and mechanical properties of Ti. The surfaces of double layer coatings were uniform and crack-free with a thickness of about 7 μm. The bonding strength of the HA-CNT/TiO2 coating was higher than that of the pure HA and HA-CNT coatings. Additionally, in vitro cell experiments showed that CNTs promoted the adhesion of preosteoblasts on the HA-CNT/TiO2 double layer coatings. These unique surfaces combined with the osteoconductive properties of HA exhibited the excellent mechanical properties of CNTs. Therefore, the developed HA-CNT/TiO2 coatings on Ti substrates might be a promising material for bone replacement. PMID:22606041

  2. Characterization in vitro studies and antibacterial properties on a sol-gel derived silver incorporated bioglass

    NASA Astrophysics Data System (ADS)

    Bouhazma, S.; Chajri, S.; Khaldi, M.; Sadiki, M.; Barkai, H.; Elabed, S.; Ibnsouda Koraichi, S.; El Bali, B.; Lachkar, M.

    2017-03-01

    The SiO2-CaO, SiO2-CaO-P2O5 and SiO2-CaO-P2O5-Ag2O glass systems were synthesized by the sol-gel technique and characterized with different techniques such as X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), and Environmental Scanning Electron Microscopy (ESEM). In vitro bioactivity tests were performed in Simulated Body Fluid (SBF). The antibacterial action of 65S5Ag (65%SiO2 + 24%CaO + 6%P2O5 + 5% Ag2O) is attributed exclusively to the leaching of Ag+ ions from the glass matrix. The activity of SiO2-CaO-P2O5-Ag2O was compared with that of its binary and ternary counterpart glass system. The concentrations of Ag-bioglass, in the range of 0.05 mg/mL of culture medium, were found to inhibit the growth of these bacteria.

  3. Adsorption characteristics of sol gel-derived zirconia for cesium ions from aqueous solutions.

    PubMed

    Yakout, Sobhy M; Hassan, Hisham S

    2014-07-01

    Zirconia powder was synthesized via a sol gel method and placed in a batch reactor for cesium removal investigation. X-ray analysis and Fourier transform infrared spectroscopy were utilized for the evaluation of the developed adsorbent. The adsorption process has been investigated as a function of pH, contact time and temperature. The adsorption is strongly dependent on the pH of the medium whereby the removal efficiency increases as the pH turns to the alkaline range. The process was initially very fast and the maximum adsorption was attained within 60 min of contact. A pseudo-second-order model and homogeneous particle diffusion model (HPDM) were found to be the best to correlate the diffusion of cesium into the zirconia particles. Furthermore, adsorption thermodynamic parameters, namely the standard enthalpy, entropy, and Gibbs free energy, were calculated. The results indicate that cesium adsorption by zirconia is an endothermic (ΔH>0) process and good affinity of cesium ions towards the sorbent (ΔS>0) was observed.

  4. Sol-gel-derived hydroxyapatite-carbon nanotube/titania coatings on titanium substrates.

    PubMed

    Ji, Xiaoli; Lou, Weiwei; Wang, Qi; Ma, Jianfeng; Xu, Haihong; Bai, Qing; Liu, Chuantong; Liu, Jinsong

    2012-01-01

    In this paper, hydroxyapatite-carbon nanotube/titania (HA-CNT/TiO(2)) double layer coatings were successfully developed on titanium (Ti) substrates intended for biomedical applications. A TiO(2) coating was firstly developed by anodization to improve bonding between HA and Ti, and then the layer of HA and CNTs was coated on the surface by the sol-gel process to improve the biocompatibility and mechanical properties of Ti. The surfaces of double layer coatings were uniform and crack-free with a thickness of about 7 μm. The bonding strength of the HA-CNT/TiO(2) coating was higher than that of the pure HA and HA-CNT coatings. Additionally, in vitro cell experiments showed that CNTs promoted the adhesion of preosteoblasts on the HA-CNT/TiO(2) double layer coatings. These unique surfaces combined with the osteoconductive properties of HA exhibited the excellent mechanical properties of CNTs. Therefore, the developed HA-CNT/TiO(2) coatings on Ti substrates might be a promising material for bone replacement.

  5. Characterization of the bioactive and mechanical behavior of dental ceramic/sol-gel derived bioactive glass mixtures.

    PubMed

    Abbasi, Zahra; Bahrololoum, Mohammad E; Bagheri, Rafat; Shariat, Mohammad H

    2016-02-01

    Dental ceramics can be modified by bioactive glasses in order to develop apatite layer on their surface. One of the benefits of such modification is to prolong the lifetime of the fixed dental prosthesis by preventing the formation of secondary caries. Dental ceramic/sol-gel derived bioactive glass mixture is one of the options for this modification. In the current study, mixtures of dental ceramic/bioactive glass with different compositions were successfully produced. To evaluate their bioactive behavior, prepared samples were immersed in a simulated body fluid at various time intervals. The prepared and soaked specimens were characterized using Fourier transform infrared spectroscopy, X-ray diffractometry and scanning electron microscopy. Since bioactive glasses have deleterious effects on the mechanical properties of dental ceramics, 3-point bending tests were used to evaluate the flexural strength, flexural strain, tangent modulus of elasticity and Weibull modulus of the specimens in order to find the optimal relationship between mechanical and bioactive properties.

  6. Regulation of cellular behaviors of fibroblasts related to wound healing by sol-gel derived bioactive glass particles.

    PubMed

    Xie, Weihan; Chen, Xiaofeng; Miao, Guohou; Tang, Jieying; Fu, Xiaoling

    2016-10-01

    Sol-gel derived bioactive glass (BG) holds great potential in the application of skin repair. However, the specific regulation of BG on skin cells is still unclear and demands more investigation. Herein, we synthesized sol-gel derived BGs with different compositions (60S, 70S, 80S, and 90S) and found 90S BGs (90 mol % SiO2 , 6 mol % CaO, 4 mol % P2 O5 ) exhibited the best supportiveness for the proliferation of normal human foreskin fibroblasts. Thus, 90S BG particles were used as a model to systematically study the wound healing related cellular response of fibroblasts to BGs. Time-lapse imaging revealed a promoted fibroblast motility stimulated by 90S BG particles. Results on the expression of extracellular matrix (ECM) related genes illustrated that 90S BG particles modulated the synthesis capacity for critical ECM molecules including type I collagen, type III collagen, fibronectin, and tenascin-C. Moreover, the myofibroblastic differentiation of fibroblasts was greatly inhibited by 90S BG particles. Further analysis on the intracellular signaling pathways demonstrated that 90S BG particles down-regulated the collagen synthesis and fibroblast-to-myofibroblast differentiation via TGF-β1-Smad2 signaling, evidenced by the decreased expression levels of TGF-β receptor I and its downstream effector Smad2. Our study provided a further understanding of the specific regulation of 90S BG particles on fibroblasts, which may guide the future design of BG based wound dressing and benefit the clinical application of BG particles in skin repair. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 2420-2429, 2016.

  7. The effect of heat treatment on the physical properties of sol-gel derived ZnO thin films

    NASA Astrophysics Data System (ADS)

    Raoufi, Davood; Raoufi, Taha

    2009-03-01

    Zinc oxide (ZnO) thin films were deposited on microscope glass substrates by sol-gel spin coating method. Zinc acetate (ZnAc) dehydrate was used as the starting salt material source. A homogeneous and stable solution was prepared by dissolving ZnAc in the solution of monoethanolamine (MEA). ZnO thin films were obtained after preheating the spin coated thin films at 250 °C for 5 min after each coating. The films, after the deposition of the eighth layer, were annealed in air at temperatures of 300 °C, 400 °C and 500 °C for 1 h. The effect of thermal annealing in air on the physical properties of the sol-gel derived ZnO thin films are studied. The powder and its thin film were characterized by X-ray diffractometer (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure (JCPDS 36-1451) and show the c-axis grain orientation. Increasing annealing temperature increased the c-axis orientation and the crystallite size of the film. The annealed films are highly transparent with average transmission exceeding 80% in the visible range (400-700 nm). The measured optical band gap values of the ZnO thin films were between 3.26 eV and 3.28 eV, which were in the range of band gap values of intrinsic ZnO (3.2-3.3 eV). SEM analysis of annealed thin films has shown a completely different surface morphology behavior.

  8. Microstructure and ferroelectric properties of Bi 3.2Y 0.8Ti 3O 12 thin films prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Kao, M. C.; Chen, H. Z.; Young, S. L.; Shi, J. B.; Lin, C. H.

    2008-05-01

    Yttrium-substituted bismuth titanate (Bi 3.2Y 0.8Ti 3O 12, BYT) thin films were successfully deposited on Pt(1 1 1)/Ti/SiO 2/Si(1 0 0) substrates by spin coating with a sol-gel technology and rapid thermal annealing. The effects of annealing temperature (500-800 °C) on microstructure and electrical properties of thin films were investigated. X-ray diffraction analysis shows that the BYT thin films have a bismuth-layered perovskite structure with preferred (1 1 7) orientation. The intensities of (1 1 7) peaks increases with increasing annealing temperature. With the increase of annealing temperature from 500 to 800 °C, the grain size of BYT thin films increases. The highly (1 1 7)-oriented BYT thin films exhibit a high-remnant polarization (2 Pr) of 58 μC/cm 2 and a low-coercive field (2 Ec) of 116 kV/cm, fatigue free characteristics up to >10 8 switching cycles. The leakage current density ( J) were 4.38×10 -8 A/cm 2 at 200 kV/cm. These results indicate that the highly (1 1 7)-oriented BYT thin film is useful in nonvolatile ferroelectric random access memory applications.

  9. Combinatorial methods in sol-gel technology

    NASA Astrophysics Data System (ADS)

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

    2000-05-01

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

  10. The Osteogenic Properties of Multipotent Mesenchymal Stromal Cells in Cultures on TiO2 Sol-Gel-Derived Biomaterial

    PubMed Central

    Marycz, Krzysztof; Śmieszek, Agnieszka; Grzesiak, Jakub; Siudzińska, Anna; Marędziak, Monika; Donesz-Sikorska, Anna; Krzak, Justyna

    2015-01-01

    The biocompatibility of the bone implants is a crucial factor determining the successful tissue regeneration. The aim of this work was to compare cellular behavior and osteogenic properties of rat adipose-derived multipotent stromal cells (ASCs) and bone marrow multipotent stromal cells (BMSCs) cultured on metallic substrate covered with TiO2 sol-gel-derived nanolayer. The morphology, proliferation rate, and osteogenic differentiation potential of both ASCs and BMSCs propagated on the biomaterials were examined. The potential for osteogenic differentiation of ASCs and BMSCs was determined based on the presence of specific markers of osteogenesis, that is, alkaline phosphatase (ALP), osteopontin (OPN), and osteocalcin (OCL). Additionally, the concentration of calcium and phosphorus in extracellular matrix was determined using energy-dispersive X-ray spectroscopy (SEM-EDX). Obtained results showed that TiO2 layer influenced proliferation activity of ASCs, which manifested by shortening of population doubling time and increase of OPN secretion. However, characteristic features of cells morphology and growth pattern of cultures prompted us to conclude that ultrathin TiO2 layer might also enhance osteodifferentiation of BMSCs. Therefore in our opinion, both populations of MSCs should be used for biological evaluation of biomaterials compatibility, such results may enhance the area of investigations related to regenerative medicine. PMID:25710015

  11. Luminescent features of novel sol-gel derived lanthanide multi-doped oxyfluoride nano-structured phosphors for white LED

    NASA Astrophysics Data System (ADS)

    Gouveia-Neto, Artur S.; da Silva, Andréa F.; Bueno, Luciano A.; Costa, Ernande B.

    2011-03-01

    Rare-earth doped oxyfluoride 75SiO2:25PbF2 nano-structured phosphors for white-light-emitting diodes were synthesized by thermal treatment of precursor sol-gel derived glasses. Room temperature luminescence features of Eu3+, Sm3+, Tb3+, Eu3+/Tb3+ and Sm3+/Tb3+ ions incorporated into low-phonon-energy PbF2 nanocrystals dispersed in the aluminosilicate glass matrix and excited with UV(395 nm) and blue(405 nm) light emitting diodes was investigated. The luminescence spectra exhibited strong emission signals in the red(600, 610, 625, 646 nm), green(548, and 560 nm) and blue(485 nm) wavelength regions. White-light emission was observed in Sm/Tb and Eu/Tb double-doped activated phosphors employing UV-LED excitation at 395 nm. The dependence of the luminescence emission intensities upon annealing temperature, and rare-earth concentration was also examined. The results indicated that there exist optimum annealing temperature and activator ion concentration in order to obtain intense visible emission light with high color rendering index. The study suggest that the nanocomposite phosphor based upon 75SiO2:25PbF2 host herein reported is a promising contender for white-light LED applications.

  12. Characteristic coordination structure around Nd Ions in sol-gel-derived Nd-Al-codoped silica glasses.

    PubMed

    Funabiki, Fuji; Kajihara, Koichi; Kaneko, Ken; Kanamura, Kiyoshi; Hosono, Hideo

    2014-07-24

    Al codoping can improve the poor solubility of rare-earth ions in silica glasses. However, the mechanism is not well understood. The coordination structure around Nd ions in sol-gel-derived Nd-Al-codoped silica glasses with different Al content was investigated by optical and pulsed electron paramagnetic resonance spectroscopies. Both tetrahedral AlO4 and octahedral AlO6 units were observed around Nd ions as ligands. The average total number of these two types of ligands for each Nd(3+) ion was ∼ 2 irrespective of Al content and was larger by 1-2 orders of magnitude than that calculated for a uniform distribution of codopant ions (∼ 0.08-0.25). With increasing Al content, AlO4 units disappeared and AlO6 units became dominant. The preferential coordination of AlOx (x = 4, 6) units to Nd ions enabled the amount of Al necessary to dissolve Nd ions uniformly in silica glass at a relatively low temperature of 1150-1200 °C to be minimized, and the conversion of AlO4 units to AlO6 units around Nd ions caused the asymmetry of the crystal field at the Nd sites to increase and the site-to-site distribution to decrease.

  13. Development of beta-tricalcium phosphate/sol-gel derived bioactive glass composites: physical, mechanical, and in vitro biological evaluations.

    PubMed

    Hesaraki, Saeed; Safari, Mojgan; Shokrgozar, Mohammad Ali

    2009-10-01

    In this study, composites of beta-tricalcium phosphate (beta-TCP) and sol gel derived bioactive glass (10, 25, and 40 wt %) based on the SiO(2)-CaO-MgO-P(2)O(5) system were prepared and sintered at 1000-1200 degrees C. The mechanical properties were investigated by measuring bending strength, Vickers hardness and fracture toughness. Structural properties were evaluated by XRD and SEM analysis, and the biological properties were studied by soaking the samples in simulated body fluid (SBF) and in contact with osteoblastic cell for viability assay. When the samples were sintered at 1200 degrees C, the mechanical strength increased, up to 34%, by increasing the amount of bioactive glass phase. In contrast, it decreased when the samples were sintered at 1000 and 1100 degrees C. The results showed that the strength could be improved up to 56% when more firing period was used. Incorporation of the bioactive glass phase into beta-TCP increased the microhardness but did not significantly change the fracture toughness. Phase analysis revealed that beta-TCP or magnesium-substituted beta-TCP was the main crystalline phase of the composites beside some calcium silicate crystallized in the bioactive glass phase. Plenty precipitation of calcium phosphate layer onto the surfaces of the beta-TCP/bioactive glass composites soaked in SBF indicated superior bioactivity of these materials compared to pure beta-TCP without any precipitation. The ability of beta-TCP/bioactive glass composites to support the growth of human osteoblastic cells was considerably better than that of pure beta-TCP. These results may be used to indicate which compositions and processing conditions can provide appropriate materials for hard tissue regeneration.

  14. Controlling the degradation rate of AZ91 magnesium alloy via sol-gel derived nanostructured hydroxyapatite coating.

    PubMed

    Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan

    2013-10-01

    Magnesium (Mg) alloys have been introduced as new generation of biodegradable orthopedic materials in recent years since it has been proved that Mg is one of the main minerals required for osseous tissue revival. The main goal of the present study was to establish a desired harmony between the necessities of orthopedic patient body to Mg(2+) ions and degradation rate of the Mg based implants as a new class of biodegradable/bioresorbable materials. This prospect was followed by providing a sol-gel derived nanostructured hydroxyapatite (n-HAp) coating on AZ91 alloy using dip coating technique. Phase structural analysis, morphology study, microstructure characterization, and functional group identification were performed using X-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. The prepared samples were immersed in simulated body fluid in order to study the formation of apatite-like precipitations, barricade properties of the n-HAp coating, and to estimate the dosage of released Mg(2+) ions within a specified and limited time of implantation. Electrochemical polarization tests were carried out to evaluate and compare the corrosion behavior of the n-HAp coated and uncoated samples. The changes of the in vitro pH values were also evaluated. Results posed the noticeable capability of n-HAp coating on stabilizing alkalization behavior and improving the corrosion resistance of AZ91 alloy. It was concluded that n-HAp coated AZ91 alloy could be a good candidate as a type of biodegradable implant material for biomedical applications.

  15. In vitro toxicity assessment of extracts derived from sol-gel coatings on polycarbonate intended to be used in food contact applications.

    PubMed

    Séverin, Isabelle; Lionti, Krystelle; Dahbi, Laurence; Loriot, Catherine; Toury, Bérangère; Chagnon, Marie-Christine

    2016-07-01

    Polycarbonate is a widely used polymer in food contact applications all around the world. However, due to the potential release of Bisphenol A (BPA) during repeated washing cycles, its use becomes compromised as BPA is known for being an endocrine disruptor for rodents. In order to tackle this issue, sol-gel coatings based on organoalkoxysiloxane were developed on PC, to act as a physical barrier. To this end, two sol-gel systems based on tetraethylorthosilicate (TEOS), methyltriethoxysilane (MTES) and 3-glycidyloxypropyltriethoxysilane (GPTES), three common sol-gel precursors, were prepared. The coatings derived from the latter two systems were then studied with regards to their potential toxicity in vitro. Migration tests were performed in food simulants, and the maximal migration was obtained in ethanol 10% (v/v) for one system and in isooctane for the other one. In vitro genotoxicity was assessed with the Ames test (OECD 471) and the micronucleus assay (OECD 487), and no genotoxic effect was observed. Moreover, the estrogenic activity of the extracts was studied with a transcriptional activation assay using transient transfection in human cells; none of the extracts was found estrogenic. These negative in vitro results are highly promising for the future use of these new barrier coating formulations onto food contact materials.

  16. Hybrid Sol-Gel-Derived Films That Spontaneously Form Complex Surface Topographies.

    PubMed

    Destino, Joel F; Jones, Zachary R; Gatley, Caitlyn M; Zhang, Yi; Craft, Andrew K; Detty, Michael R; Bright, Frank V

    2016-10-04

    Surface patterns over multiple length scales are known to influence various biological processes. Here we report the synthesis and characterization of new, two-component xerogel thin films derived from carboxyethylsilanetriol (COE) and tetraethoxysilane (TEOS). Atomic force microscopy (AFM) reveals films surface with branched and hyper branched architectures that are ∼2 to 30 μm in diameter, that extend ∼3 to 1300 nm above the film base plane with surface densities that range from 2 to 77% surface area coverage. Colocalized AFM and Raman spectroscopy show that these branched structures are COE-rich domains, which are slightly stiffer (as shown from phase AFM imaging) and exhibit lower capacitive force in comparison with film base plane. Raman mapping reveals there are also discrete domains (≤300 nm in diameter) that are rich in COE dimers and densified TEOS, which do not appear to correspond with any surface structure seen by AFM.

  17. Stimuli-Triggered Sol-Gel Transitions of Polypeptides Derived from α-Amino Acid N-Carboxyanhydride (NCA) Polymerizations.

    PubMed

    He, Xun; Fan, Jingwei; Wooley, Karen L

    2016-02-18

    The past decade has witnessed significantly increased interest in the development of smart polypeptide-based organo- and hydrogel systems with stimuli responsiveness, especially those that exhibit sol-gel phase-transition properties, with an anticipation of their utility in the construction of adaptive materials, sensor designs, and controlled release systems, among other applications. Such developments have been facilitated by dramatic progress in controlled polymerizations of α-amino acid N-carboxyanhydrides (NCAs), together with advanced orthogonal functionalization techniques, which have enabled economical and practical syntheses of well-defined polypeptides and peptide hybrid polymeric materials. One-dimensional stacking of polypeptides or peptide aggregations in the forms of certain ordered conformations, such as α helices and β sheets, in combination with further physical or chemical cross-linking, result in the construction of three-dimensional matrices of polypeptide gel systems. The macroscopic sol-gel transitions, resulting from the construction or deconstruction of gel networks and the conformational changes between secondary structures, can be triggered by external stimuli, including environmental factors, electromagnetic fields, and (bio)chemical species. Herein, the most recent advances in polypeptide gel systems are described, covering synthetic strategies, gelation mechanisms, and stimuli-triggered sol-gel transitions, with the aim of demonstrating the relationships between chemical compositions, supramolecular structures, and responsive properties of polypeptide-based organo- and hydrogels.

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

    SciTech Connect

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

    2007-11-15

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

  19. A new precursor for the immobilization of enzymes inside sol-gel-derived hybrid silica nanocomposites containing polysaccharides.

    PubMed

    Shchipunov, Yurii A; Karpenko, Tat'yana Yu; Bakunina, Irina Yu; Burtseva, Yuliya V; Zvyagintseva, Tat'yana N

    2004-01-30

    Tetrakis(2-hydroxyethyl) orthosilicate (THEOS) introduced by Hoffmann et al. (J. Phys. Chem. B., 106 (2002) 1528) was first used to prepare hybrid nanocomposites containing various polysaccharides and immobilize enzymes in these materials. Two different types of O-glycoside hydrolyses (EC3.2.1), 1-->3-beta-D-glucanase LIV from marine mollusk Spisula sacchalinensis and alpha-D-galactosidase from marine bacterium Pseudoalteromonas sp. KMM 701, were taken for the immobilization. To reveal whether the polysaccharide inside the hybrid material influences the enzyme entrapment and functioning, negatively charged xanthan, cationic derivative of hydroxyethylcellulose and uncharged locust bean gum were examined. The mechanical properties of these nanocomposites were characterized by a dynamic rheology and their structure by a scanning electron microscopy. It was found that 1-->3-beta-D-glucanase was usually immobilized without the loss of its activity, while the alpha-D-galactosidase activity in the immobilized state depended on the polysaccharide type of material. An important point is that the amount of immobilized enzymes was small, comparable to their content in the living cells. It was shown by the scanning electron microscopy that the hybrid nanocomposites are sufficiently porous that allows the enzymatic substrates and products to diffuse from an external aqueous solution to the enzymes, whereas protein molecules were immobilized firmly and not easily washed out of the silica matrix. A sharp increase of the enzyme lifetime (more than a hundred times) was observed after the immobilization. As established, the efficient entrapment of enzymes is caused by few advantages of new precursor over the currently used TEOS and TMOS: (i) organic solvents and catalysts are not needed owing to the complete solubility of THEOS in water and the catalytic effect of polysaccharides on the sol-gel processes; (ii) the entrapment of enzymes can be performed at any pH which is suitable

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

    SciTech Connect

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

    2005-09-01

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

  1. Fabrication of regular TiO2 nanoporous films derived by combining nanoimprint technique with sol-gel method.

    PubMed

    Zhong, Peng; Que, Wenxiu; Zhang, Jin

    2010-11-01

    In this paper, honeycomb-like regular TiO2 nanoporous films deposited on different substrates including ITO glass and silicon wafer are fabricated by combining a nanoimprint technique with a sol-gel method. A novel soft polymer mold containing a thin layer of polymethylmethacrylate and a thicker layer of polydimethylsiloxane, which is obtained from an anodic aluminum oxide template, is carried out for the nanoimprint process. TiO2 precursor solution prepared by the sol-gel processing is used as the nanoimprinted material. After imprinting, the polydimethylsiloxane back layer is easily peeled off before the polymethylmethacrylate mold is chemically removed to avoid any demolding problem. The SEM images show that the honeycomb-like regular nanostructure of the initial anodic aluminum oxide template can be preserved completely on TiO2 via this method, and the XRD results indicate that there is a crystalline transition from amorphous to anatase of TiO2 after 450 degrees C heat treatment.

  2. Nanocrystal/sol-gel nanocomposites

    DOEpatents

    Petruska, Melissa A.; Klimov, Victor L.

    2007-06-05

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

  3. Nanocrystal/sol-gel nanocomposites

    SciTech Connect

    Petruska, Melissa A; Klimov, Victor L

    2012-06-12

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

  4. The evaluation of physical properties and in vitro cell behavior of PHB/PCL/sol-gel derived silica hybrid scaffolds and PHB/PCL/fumed silica composite scaffolds.

    PubMed

    Ding, Yaping; Yao, Qingqing; Li, Wei; Schubert, Dirk W; Boccaccini, Aldo R; Roether, Judith A

    2015-12-01

    PHB/PCL/sol-gel derived silica hybrid scaffolds (P5S1S) and PHB/PCL/fumed silica composite scaffolds (P5S1N) with a 5:1 organic/inorganic ratio were fabricated through a combination of electrospinning and sol-gel methods and dispersion electrospinning, respectively. In contrast to the silica nanoparticle aggregates appearing on the fiber surface of P5S1N, smooth and uniform fibers were obtained for P5S1S. The fiber diameter distribution, tensile strength, thermal gravimetric analysis (TGA), and cellular behavior of both types of scaffolds were characterized and studied. The tensile strength results and TGA indicated that the interfacial interaction between the organic and the inorganic phase was enhanced in P5S1S over the nanocomposite scaffolds, and cells exhibited significantly higher alkaline phosphate activity (ALP) for P5S1S, which makes P5S1S hybrid scaffolds candidate materials for bone tissue engineering applications.

  5. Effect of aluminum on the formation of silver metal quantum dots in sol-gel derived alumino-silicate glass film.

    PubMed

    Kim, Bok Hyeon; Son, Dong Hoon; Ju, Seongmin; Jeong, Chaehwan; Boo, Seongjae; Kim, Cheol Jin; Hanl, Won-Taek

    2006-11-01

    The effect of aluminum incorporation on silver metal quantum dots formation in the alumino-silicate glass film processed by sol-gel process was investigated. The sol-gel derived glass was coated onto the silica glass plate by spin coating with the mixture solution of tetraethyl orthosilicate (TEOS), C2H5OH, H2O, AgNO3, Al(NO3)3. 39H2O, and HNO3 with the molar ratios of Ag/Si = 0.12 and Al/Si varying from 0 to 0.12. The formation of the silver metal quantum dots was confirmed by the measurements of the UV/VIS optical spectra, the X-ray diffraction patterns, and the transmission electron microscope images. While the radius of silver metal quantum dots increased with the increase of aluminum concentration, the concentration of the silver metal quantum dots decreased. The formation of the silver metal quantum dots was found strongly suppressed by incorporation of aluminum ions in the glass. The change in the glass structure due to the aluminum incorporation was investigated by the analysis of the Raman spectra. The silver ions in the glass contributed to form stable (Al:Ag)O4 tetrahedra by pairing with aluminum ions and thus clustering of silver metal quantum dots was hindered.

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  7. Selective disordering of InAs/InGaAs dots-in-a-well structure patterned with sol-gel derived SiO{sub 2} strips imprinted by soft mold technique

    SciTech Connect

    Chia, C. K.; Suryana, M.; Low, H. Y.; Zhao, W.; Hopkinson, M.

    2008-08-18

    Selective impurity free vacancy disordering of InAs/InGaAs quantum dot (QD) structures imprinted with sol-gel derived SiO{sub 2} strips via a polyethylene terepthalate soft mold has been investigated. Wavelength blueshift of up to 220 nm for areas capped with the sol-gel derived SiO{sub 2} is demonstrated. The imprinted SiO{sub 2} strips were used as hard mask for plasma etching of GaAs ridge waveguide structures and were found to have similar hardness as the SiO{sub 2} prepared by plasma-enhanced chemical vapor deposition. QD intermixing using sol-gel derived SiO{sub 2} with step-thickness profile was demonstrated, and a one-step SiO{sub 2} imprinting technique for multiple band gap QD intermixing is proposed.

  8. Chances and limitations of sol-gel-derived metal oxide and chalcogenide nanocomposites for optic and photonic application

    NASA Astrophysics Data System (ADS)

    Schmidt, Helmut K.

    1997-07-01

    Sol-gel technologies represent a powerful tool for making almost all kinds of transparent materials with interesting optical or photonic properties. During the last two decades, a large number of materials, mainly in form of coatings, have been developed. It is to say that the materials properties would be suitable for many applications. Draw- backs in many cases are processing, chemical engineering for quality-assured material production, availability of materials, skills for combining chemistry, engineering and device making in academia as well as in many industries, especially SMEs. These definitions in combination with the lack of knowledge lead to a situation that despite of the interesting prospects the industrial breakthrough has still not yet taken place.

  9. Influence of Eu(3+) doping content on antioxidant properties of Lu2O3 sol-gel derived nanoparticles.

    PubMed

    Olvera Salazar, Arturo; García Hernández, Margarita; López Camacho, Perla Yolanda; López Marure, Arturo; Reyes de la Torre, Adriana Isabel; Morales Ramírez, Ángel de Jesús; Hernández Santiago, Felipe; Aguilera Vázquez, Luciano

    2016-12-01

    This paper presents the synthesis of pure and europium-doped lutetium oxide (Lu2O3) powders prepared by sol-gel method. The influence of europium ion concentration into Lu2O3 nanocrystallites was investigated for first time in an in vitro system using a modified ABTS radical cation decolorization assay to determine the antioxidant activity. The crystalline structure of Lu2O3 and Eu:Lu2O3 powders was elucidated by XRD obtaining cubic phase in all system without secondary products in accordance with FT-IR results. By TEM and Scherrer equation, it was determined that Lu2O3 and Eu:Lu2O3 powders presented nearly spherical particle morphology with crystallites sizes in the range of 8 to 13nm. The antioxidant assays results revealed that europium ion enhance Lu2O3 powders antioxidant properties, showing that 12.5mol% of europium is sufficient to reach its maximum capacity.

  10. Sol-Gel-Derived Lithium Superionic Conductor Li1.5Al0.5Ge1.5(PO4)3 Electrolyte for Solid-State Lithium-Oxygen Batteries

    DTIC Science & Technology

    2014-03-12

    AFRL-RQ-WP-TP-2015-0055 SOL-GEL-DERIVED LITHIUM SUPERIONIC CONDUCTOR LI1.5AL0.5GE1.5(PO4)3 ELECTROLYTE FOR SOLID -STATE LITHIUM -OXYGEN...2014 4. TITLE AND SUBTITLE SOL-GEL-DERIVED LITHIUM SUPERIONIC CONDUCTOR LI1.5AL0.5GE1.5(PO4)3 ELECTROLYTE FOR SOLID -STATE LITHIUM -OXYGEN BATTERIES...attracting a great deal of attention as a solid electrolyte for lithium -oxygen (Li- O2) batteries due to its high ionic conductivity. In this study, LAGP

  11. Photocatalytic activity and characterization of sol-gel-derived Ni-doped TiO2-coated active carbon composites

    NASA Astrophysics Data System (ADS)

    Bhosale, R. R.; Pujari, S. R.; Lande, M. K.; Arbad, B. R.; Pawar, S. B.; Gambhire, A. B.

    2012-11-01

    Ni-doped, TiO2-coated active carbon (Ni-TiO2/AC) were prepared by a sol-gel method. The effect of supports, including TiO2 and active carbon (AC), on the molecular structure and photocatalytic activity of nickel oxide for complete decomposition of methylene blue has been examined with respect to the content of Ni on the catalyst surface. The photocatalytic activities of the Ni-TiO2/AC composites were evaluated in the decomposition of methylene blue solution under visible-light irradiation. The results indicate that Ni-TiO2/AC has a higher efficiency in decomposition of methylene blue than TiO2 and TiO2/AC. This was attributed to the different functions of active carbon and nickel species. First, nanosize TiO2 particles on composites were not reunited, possible because active carbon retards transformation of anatase into rutile and decrease the crystallite size. Second, production of high concentrations of organic compound near Ni-TiO2. Third, carbon in active carbon causes some of the TiO2 to reduce to Ti3+ ions, which prevents electron-hole pair recombination. It was found that the addition of Ni to TiO2 sol could suppress the grain growth of TiO2 crystals and increase the hydroxyl content on the surface of TiO2/AC. The photocatalytic efficiency and activity of the composites remained good, even after three cycles.

  12. Structural, Morphological and Antibacterial Investigation of Ag-Impregnated Sol-Gel-Derived 45S5 NanoBioglass Systems.

    PubMed

    Durgalakshmi, D; Balakumar, S; Raja, C Ashok; George, Rani P; Mudali, U Kamachi

    2015-06-01

    An increasing percentage of ageing population requires 30-year survivability of orthopedic devices that is not possible with the current bioinert materials, having a maximum of 15-year survivability. To satisfy this growing need, a shift is needed from replacement of tissues to regeneration of tissues. This is highly possible through the use of silica-bioactive glasses. However, a failure of implant can occur due to infections even by using such materials. Advances in using silver for antibacterial applications have been commercialized. However, higher concentrations of silver also lead to toxic effects. In this study, nanoBioglass 45S5 (NBG) and Ag-NBG were synthesized by using sol-gel method followed by solution-phase method, respectively. The bioactive crystals such as Na2Ca2Si3O9, CaCO3, and AgPO3, very much needed in the field of bone tissue engineering and in antibacterial strategies, were obtained in the NBG Matrix. The morphological investigation of NBG with 1 mM Ag+ concentrations shows the nanospikes arrangement of size 30-40 nm with spherical porous structure of size 10-20 nm, which supports the formation of collagen molecular fibrils on the surface of NBG matrices and enhances osseointegration. Both gram-positive and gram-negative strains show higher antibacterial activity for nanoBioglass with 1 mM Ag+ concentration.

  13. Low dark current metal-semiconductor-metal ultraviolet photodetectors based on sol-gel-derived TiO2 films

    NASA Astrophysics Data System (ADS)

    Xie, Yannan; Huang, Huolin; Yang, Weifeng; Wu, Zhengyun

    2011-01-01

    The titanium dioxide (TiO2) films prepared by sol-gel processing were used to fabricate metal-semiconductor-metal ultraviolet photodetectors. A very low dark current of 5.38 pA (current density of 3.84 nA/cm2) at 5 V bias is obtained, which is ascribed to the high effective Schottky barrier between Au and TiO2 films. The x-ray photoelectron spectroscopy analysis demonstrates that the concentration of oxygen vacancies is very low in the surface of the TiO2 films, which is responsible for the high effective Schottky barrier. The devices exhibit a cutoff wavelength at about 380 nm and a large UV-to-visible rejection ratio (340 versus 400 nm) of three orders of magnitude. The peak responsivity of the devices is 17.5 A/W at 5 V bias, indicating the presence of internal photoconductive gain induced by desorption of oxygen on the TiO2 surface.

  14. Structural studies of the NaCaPO 4-SiO 2 sol-gel derived materials

    NASA Astrophysics Data System (ADS)

    Sitarz, M.; Rokita, M.; Handke, M.; Galuskin, E.

    2003-06-01

    Structural studies of the NaCaPO 4-SiO 2 materials have been carried out. Amorphous materials from this system, after controlled crystallization process, can be used as potential nanomaterials. Structural studies of nanomaterials are of fundamental importance in view their future applications. Materials of different [PO 4] 3-/[SiO 4] 4- tetrahedra proportion have been prepared. Na + and Ca 2+ cations have compensated the negative charge of the lattice. Amorphous and crystalline materials have been obtained by sol-gel as well as conventional melting methods. The XRD phase identification has enabled amorphous and crystalline materials identification and suggests the separation of phosphorus and silicate crystalline phases. The obtained materials were examined using the electron scanning microscope and EDX spectrometer. Analysis of electron scanning microscope maps shows considerable inhomogeneity of crystalline samples. Fluctuations in ions distribution, in case of amorphous materials, have been noted too. DTA investigations have enabled to find the probable characteristic temperatures of glass crystallization. Detailed infrared spectroscopy measurements have been carried out. The spectra of obtained materials have been compared with the spectra of cristobalite. Spectroscopic studies confirm the inhomogeneity of materials.

  15. Sol-gel derived mesoporous cobalt silica catalyst: Synthesis, characterization and its activity in the oxidation of phenol

    NASA Astrophysics Data System (ADS)

    Andas, Jeyashelly; Adam, Farook; Rahman, Ismail Ab.

    2014-10-01

    Highly mesoporous cobalt silica rice husk catalysts with (5-15 wt.%) Co2+ loading were prepared via a simple sol-gel technique at room temperature. The successful insertion of cobalt ions into silica matrix was evidenced from FT-IR, NMR, XPS and AAS analyses. Preservation of the mesoporosity nature of silica upon incorporating Co2+ was confirmed from the N2-sorption studies. The topography and morphology viewed by TEM analysis differs as the cobalt concentration varies from 5 to 15 wt.%. Parallel pore channels and spherical nanoparticles of 9.44 nm were achieved for cobalt silica catalysts with 10 and 15 wt.% respectively. Cobalt catalysts were active in the liquid-phase oxidation of phenol with H2O2 as an oxygen source. The performances of the catalysts were greatly influenced by various parameters such as reaction temperature, catalyst amount, molar ratio of substrate to oxidant, nature of solvent, metal loading and homogeneous precursor salt. Water served as the best reaction medium for this oxidation system. The regeneration studies confirmed cobalt catalyst could be reused for five cycles without experiencing large loss in the conversion. Both leaching and reusability studies testified that the catalysts were truly heterogeneous.

  16. Effects of lithium doping on microstructure, electrical properties, and chemical bonds of sol-gel derived NKN thin films

    SciTech Connect

    Lin, Chun-Cheng; Chen, Chan-Ching; Weng, Chung-Ming; Chu, Sheng-Yuan; Tsai, Cheng-Che

    2015-02-28

    Highly (100/110) oriented lead-free Li{sub x}(Na{sub 0.5}K{sub 0.5}){sub 1−x}NbO{sub 3} (LNKN, x = 0, 0.02, 0.04, and 0.06) thin films are fabricated on Pt/Ti/SiO{sub 2}/Si substrates via a sol-gel processing method. The lithium (Li) dopants modify the microstructure and chemical bonds of the LNKN films, and therefore improve their electrical properties. The optimal values of the remnant polarization (P{sub r} = 14.3 μC/cm{sup 2}), piezoelectric coefficient (d{sub 33} = 48.1 pm/V), and leakage current (<10{sup −5} A/cm{sup 2}) are obtained for a lithium addition of x = 0.04 (i.e., 4 at. %). The observation results suggest that the superior electrical properties are the result of an improved crystallization, a larger grain size, and a smoother surface morphology. It is shown that the ion transport mechanism is dominated by an Ohmic behavior under low electric fields and the Poole-Frenkel emission effect under high electric fields.

  17. Effect of Fe incorporation on the optical behavior of ZnO thin films prepared by sol-gel derived spin coating techniques

    NASA Astrophysics Data System (ADS)

    Rakkesh, R. Ajay; Malathi, R.; Balakumar, S.

    2013-02-01

    In this work, Fe doped Zinc Oxide (ZnO) thin films were fabricated on the glass substrate by sol-gel derived spin coating technique. X-ray Diffraction studies revealed that the obtained pure and Fe doped ZnO thin films were in the wurtzite and spinel phase respectively. The three well defined Raman lines at 432, 543 and 1091 cm-1 also confirmed the lattice structure of the ZnO thin film has wurtzite symmetry. While doping Fe atoms in the ZnO, there was a significant change in the phase from wurtzite to spinel structure; owing to Fe (III) ions being incorporated into the lattice through substitution of Zn (II) ions. Room temperature PL spectra showed that the role of defect mediated red emissions at 612 nm was due to radial recombination of a photogenerated hole with an electron that belongs to the Fe atoms, which were discussed in detail.

  18. Microstructure and Electrical Properties of Sol-Gel Derived Pb(Mg1/3Nb2/3)0.7Ti0.3O3 Thin Films with Single Perovskite Phase

    NASA Astrophysics Data System (ADS)

    Fan, Huiqing; Kim, Hyoun-Ee

    2002-11-01

    Sol-gel derived Pb(Mg1/3Nb2/3)0.7Ti0.3O3 (PMNT) thin films were prepared by sping coating using a PbO cover coat technique, and investigated by X-ray diffraction (XRD), auger electron spectroscopy (AES), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The phase development of the PMNT film was significantly affected by the final annealing time. A perovskite PMNT film was obtained after annealing at 850°C for 1 min. The electrical properties of the perovskite PMNT films were analyzed, by measuring the temperature and frequency dependence of dielectric properties, as well as the polarization hysteresis loop. The relaxor-like behavior and relatively low dielectric constant of the PMNT film is thought to be related to needle-like ferroelectric domains, which were formed due to self-coarsening of the polar microregion along the preferred orientation, as a result of extensive defects in the PMNT films.

  19. Sol-gel derived silica/chitosan/Fe3O4 nanocomposite for direct electrochemistry and hydrogen peroxide biosensing

    NASA Astrophysics Data System (ADS)

    Satvekar, R. K.; Rohiwal, S. S.; Tiwari, A. P.; Raut, A. V.; Tiwale, B. M.; Pawar, S. H.

    2015-01-01

    A novel strategy to fabricate hydrogen peroxide third generation biosensor has been developed from sol-gel of silica/chitosan (SC) organic-inorganic hybrid material assimilated with iron oxide magnetic nanoparticles (Fe3O4). The large surface area of Fe3O4 and porous morphology of the SC composite facilitates a high loading of horseradish peroxidase (HRP). Moreover, the entrapped enzyme preserves its conformation and biofunctionality. The fabrication of hydrogen peroxide biosensor has been carried out by drop casting of the SC/F/HRP nanocomposite on glassy carbon electrode (GCE) for study of direct electrochemistry. The x-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) confirms the phase purity and particle size of as-synthesized Fe3O4 nanoparticles, respectively. The nanocomposite was characterized by UV-vis spectroscopy, fluorescence spectroscopy and Fourier transform infrared (FTIR) for the characteristic structure and conformation of enzyme. The surface topographies of the nanocomposite thin films were investigated by scanning electron microscopy (SEM). Dynamic light scattering (DLS) was used to determine the particle size distribution. The electrostatic interactions of the SC composite with Fe3O4 nanoparticles were studied by the zeta potential measurement. Electrochemical impedance spectroscopy (EIS) of the SC/F/HRP/GCE electrode displays Fe3O4 nanoparticles as an excellent candidate for electron transfer. The SC/F/HRP/GCE exhibited a pair of well-defined quasi reversible cyclic voltammetry peaks due to the redox couple of HRP-heme Fe (III)/Fe (II) in pH 7.0 potassium phosphate buffer. The biosensor was employed to detect H2O2 with linear range of 5 μM to 40 μM and detection limit of 5 μM. The sensor displays excellent selectivity, sensitivity, good reproducibility and long term stability.

  20. Thermal decomposition and crystallization of aqueous sol-gel derived zirconium acetate gels occurring during the preparation of ceramic coatings

    NASA Astrophysics Data System (ADS)

    Geiculescu, Araldina Corina

    1998-12-01

    A sol-gel procedure using an aqueous zirconium acetate precursor was used to form continuous, crack- and bridge-free zirconia coatings on graphite fibers. A comprehensive understanding of the precursor's structure and structural evolution during the sol to gel and gel to solid transitions is required to control the properties of the coating. Decomposition of the gel prepared by desiccation of the solution of zirconium acetate and pyrolyzed to form crystalline zirconia powders in N2, Air and O2 and the transformations occurring during pyrolysis to 800°C was investigated. Three transition temperatures were detected: the amorphous-to-cubic (am-c), cubic-to-tetragonal (c-t) and tetragonal-to-monoclinic (t-m) transition. The presence of molecular oxygen decreased the crystallization temperature, increased the grain size of the tetragonal crystals formed and decreased the temperature at which the t-m transformation was initiated. Decomposition and transition temperatures occurring in the pyrolysis and the polymorph distribution were dependent on the pH of the precursor solution and on the presence of additive anions such as chloride, nitrate or sulfate. Lowering the pH of the precursor solution produced changes in the relative concentration of zirconium complexes present in the solution and, hence, reduced the carbon content in the crystalline zirconia obtained by pyrolysis at 555°C and reduced transition temperatures. The presence of counterions altered the ratio of m/t polymorph in the zirconia powders because of the structural and compositional changes in the precursor gel. Controlling the chemistry involved in crystal formation results in controlling the polymorph composition, consequently gaining control of the properties of the coating of graphite fibers.

  1. Sol-gel derived Al and Ga co-doped ZnO thin films: An optoelectronic study

    NASA Astrophysics Data System (ADS)

    Ebrahimifard, Reza; Golobostanfard, Mohammad Reza; Abdizadeh, Hossein

    2014-01-01

    Al and Ga co-doped ZnO (AGZO) thin films with different doping contents of 0.5-4 at.% were synthesized via sol-gel route using dip coating method and the results were compared to the single doped specimens Al:ZnO (AZO) and Ga:ZnO (GZO). All samples were highly transparent in visible region (T > 85%) with band gap values around 3.3 eV. Introduction of Al and Ga to the ZnO crystal structure decreased the crystallinity and reduced the particle size of the films. Electrical resistivity was investigated and engineered in this study as the main parameter. Single doped samples showed reduction of resistivity compared to the un-doped ZnO. In this regard, Ga was more efficient than Al in decreasing the electrical resistivity. Furthermore, samples with 1 at.% Al and 1 at.% Ga showed the minimum amount of electrical resistivity. Co-doping was performed with two different approaches including variable doping content (Al + Ga ≠ cte) and constant doping content (Al + Ga = 0.5, 1, and 2 at.%) for the sake of the comparison with single doped samples. Samples with Al = 1 at.% and Ga = 1 at.% showed the lowest electrical resistivity in AGZO samples of former approach. However, in latter approach the lowest resistivity was obtained in Al + Ga = 2 at.% sample. The results proved the capability of co-doped samples in optoelectronic industry regarding partially substitution of expensive Ga with Al and obtaining co-doped AGZO transparent conductive thin films with lower resistivity compared to conventional AZO thin films and also achieving commercial advantages compared to costly GZO thin films.

  2. Effects of tantalum doping on microstructure and ferroelectric properties of Bi 4Ti 3O 12 thin films prepared by a sol-gel method

    NASA Astrophysics Data System (ADS)

    Kao, M. C.; Chen, H. Z.; Young, S. L.; Chuang, B. N.; Jiang, W. W.; Song, J. S.; Jhan, S. S.; Chiang, J. L.; Wu, L. T.

    2012-01-01

    Tantalum-substituted Bi 4Ti 3O 12 (Bi 4Ti 3- x/5 Ta x/5 O 12, BTTO) thin films were fabricated on Pt(111)/Ti/SiO 2/Si(100) substrates by sol-gel technology. The effects of various processing parameters, including Ta content ( x=0˜0.08) and annealing temperature (500˜800 °C), on the growth and properties of thin films were investigated. X-ray diffraction analysis shows that the BTTO thin films have a bismuth-layered perovskite structure with preferred (117) orientation. With the increase of Ta content, the grain size of film decreased slightly, and highly (117)-oriented BTTO films were obtained in the composition of x=0.06. Ta doping on the B-site of Bi 4Ti 3O 12 could induce the distortion of oxygen octahedral and decrease the oxygen vacancy concentration by a compensating effect. The highly (117)-oriented BTTO thin films with x=0.06 exhibits the maximum remanent polarization (2 Pr) of 50 μC/cm 2 and a low coercive field (2 Ec) of 104 kV/cm, fatigue free characteristics up to ≧ 10 8 switching cycles.

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

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

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

  4. Sintering Effects on Morphology, Thermal Stability and Surface Area of Sol-Gel Derived Nano-Hydroxyapatite Powder

    SciTech Connect

    Kapoor, Seema; Batra, Uma; Kohli, Suchita

    2011-12-12

    Hydroxyapatite (HAP) ceramics have been recognized as substitute materials for bone and teeth in orthopedic and dentistry field due to their chemical and biological similarity to human hard tissue. The nanosized and nanocrystalline forms of HAP have great potential to revolutionize the hard tissue-engineering field, starting from bone repair and augmentation to controlled drug delivery systems. This paper reports the synthesis of biomimetic nano-hydroxyapatite (HAP) by sol-gel method using calcium nitrate tetrahydrate (CNT) and potassium dihydrogen phosphate (KDP) as calcium and phosphorus precursors, respectively to obtain a desired Ca/P ratio of 1.67. Deionized water was used as a diluting media for HAP sol preparation and ammonia was used to adjust the pH to 11. After aging, the HAP gel was dried at 55 deg. C and sintered to different temperatures (200 deg. C, 400 deg. C, 600 deg. C, 800 deg. C, 1000 deg. C and 1200 deg. C). The dried and sintered powders were characterized for phase composition using Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The particle size and morphology was studied using transmission electron microscopy (TEM). The thermal behavior of the dried HAP nanopowder was studied in the temperature range of 55 deg. C to 1000 deg. C using thermal gravimetric analyser (TGA). The BET surface area of absorbance was determined by Nitrogen adsorption using Brunauer-Emmett-Teller (BET) method. The presence of characteristic peaks of the phosphate and OH groups in FTIR spectrums confirmed the formation of pure HAP in dried as well as sintered powders. XRD results also confirmed the formation of stoichiometric nano-HAP. Sintering revealed that with increase in temperature, both the crystallinity and crystallite size of nano-HAP particles increased. The synthesized nano-HAP powder was found to be stable upto 1000 deg. C without any additional phase other than HAP, whereas peak of {beta}-TCP (tricalcium phosphate) was observed

  5. Sintering Effects on Morphology, Thermal Stability and Surface Area of Sol-Gel Derived Nano-Hydroxyapatite Powder

    NASA Astrophysics Data System (ADS)

    Kapoor, Seema; Batra, Uma; Kohli, Suchita

    2011-12-01

    Hydroxyapatite (HAP) ceramics have been recognized as substitute materials for bone and teeth in orthopedic and dentistry field due to their chemical and biological similarity to human hard tissue. The nanosized and nanocrystalline forms of HAP have great potential to revolutionize the hard tissue-engineering field, starting from bone repair and augmentation to controlled drug delivery systems. This paper reports the synthesis of biomimetic nano-hydroxyapatite (HAP) by sol-gel method using calcium nitrate tetrahydrate (CNT) and potassium dihydrogen phosphate (KDP) as calcium and phosphorus precursors, respectively to obtain a desired Ca/P ratio of 1.67. Deionized water was used as a diluting media for HAP sol preparation and ammonia was used to adjust the pH to 11. After aging, the HAP gel was dried at 55 °C and sintered to different temperatures (200 °C, 400 °C, 600 °C, 800 °C, 1000 °C and 1200 °C). The dried and sintered powders were characterized for phase composition using Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The particle size and morphology was studied using transmission electron microscopy (TEM). The thermal behavior of the dried HAP nanopowder was studied in the temperature range of 55 °C to 1000 °C using thermal gravimetric analyser (TGA). The BET surface area of absorbance was determined by Nitrogen adsorption using Brunauer-Emmett-Teller (BET) method. The presence of characteristic peaks of the phosphate and OH groups in FTIR spectrums confirmed the formation of pure HAP in dried as well as sintered powders. XRD results also confirmed the formation of stoichiometric nano-HAP. Sintering revealed that with increase in temperature, both the crystallinity and crystallite size of nano-HAP particles increased. The synthesized nano-HAP powder was found to be stable upto 1000 °C without any additional phase other than HAP, whereas peak of β-TCP (tricalcium phosphate) was observed at 1200 °C. Photomicrograph of

  6. BNT-BT0.08 wires derived from sol-gel precursor and their piezoelectric behavior

    NASA Astrophysics Data System (ADS)

    Cernea, M.; Pintilie, L.; Trupina, L.; Vasile, B. S.; Chirila, C.; Pasuk, I.

    2013-05-01

    Lead-free piezoelectric (Bi0.5Na0.5)0.92Ba0.08TiO3, (abbreviated as BNT-BT0.08) wires were prepared using its corresponding precursor sol and, a polycarbonate template membrane. The polycarbonate membrane used has a thickness of 30 μm and pore diameter of 300 nm. Uniform surface morphology of the wires with average diameter of 145 nm and a length of about 20 μm was obtained when the concentration of the sol was 0.3 M. The ferroelectric and piezoelectric properties of an individual BNT-BT0.08 wire were investigated using the PFM technique. The hysteresis loops between the PFM phase and DC bias and, the characteristic butterfly loops of the PFM amplitude versus DC bias, indicated a ferroelectric and piezoelectric behavior of as-obtained BNT-BT0.08 wires.

  7. Sol-gel-derived NiO/NiAl{sub 2}O{sub 4} oxygen carriers for chemical-looping combustion by coal char

    SciTech Connect

    Haibo Zhao; Liming Liu; Baowen Wang; Di Xu; Linlin Jiang; Chuguang Zheng

    2008-03-15

    This paper focuses on the investigation of Ni-based oxygen carriers for CLC by coal char. First, Al(OC{sub 3}H{sub 7}){sub 3} and Ni(NO{sub 3}){sub 2} are selected as the main raw materials to prepare sol-gel-derived NiO/NiAl{sub 2}O{sub 4} oxygen carriers. The oxygen carrier with a mass content of 60% NiO, a sintering temperature of 1300{sup o}C, and a sintering time of 6 h performs comparatively well. Second, the reduction reaction of the NiO/NiAl{sub 2}O{sub 4} oxygen carriers with char and the circular reduction/oxidation reactions of the NiO/NiAl{sub 2}O{sub 4} oxygen carriers with char/air or hydrogen/air are carried out in a thermogravimetric analysis (TGA) instrument to investigate the reactivities and chemical life of the prepared NiO/NiAl{sub 2}O{sub 4} oxygen carriers. The experimental results show that (a) when the TGA temperature is higher than 850{sup o}C, NiO/NiAl{sub 2}O{sub 4} starts to react with coal char rapidly, which indicates that CLC of coal char using NiO/NiAl{sub 2}O{sub 4} as oxygen carriers is a feasible technology of energy utilization in principle; (b) NiO/NiAl{sub 2}O{sub 4}, which maintains its activity over single-cycle reduction/oxidation reactions with char/air or multiple-cycle reduction/oxidation reactions with hydrogen/air, exhibits extremely good recyclablity; (c) the porous beehive structure of the NiO/NiAl{sub 2}O{sub 4} particle is maintained, and the sintering behavior between different particles is not observed during cyclic studies. Those experimental results prove the sol-gel-derived oxygen carrier NiO/NiAl{sub 2}O{sub 4} is capable of being used in chemical-looping combustion fueled by coal char or H{sub 2}. 51 refs., 5 figs., 5 tabs.

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

    SciTech Connect

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

    2010-07-15

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

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

    PubMed

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

    2015-01-01

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

  10. Carbon nanotubes incorporated with sol-gel derived La(OH)3 nanorods as platform to simultaneously determine ascorbic acid, dopamine, uric acid and nitrite.

    PubMed

    Zhang, Yu; Yuan, Ruo; Chai, Yaqin; Zhong, Xia; Zhong, Huaan

    2012-12-01

    A novel material, sol-gel derived La(OH)(3) nanorods (La(OH)(3)NRs) with excellent film forming ability was prepared, and it was first designed to incorporate with carbon nanotubes (CNTs) to modify glassy carbon electrode (GCE) to simultaneously voltammetric determine ascorbic acid (AA), dopamine (DA), uric acid (UA), and nitrite (NO(2)(-)). Cyclic voltammetry (CV), transmission electron microscopy (TEM), and X-ray diffraction (XRD) were employed to characterize the sensor. Under optimal conditions, the linear response range for AA, DA, UA, and NO(2)(-) were 0.5 μmol L(-1) to 1.46 mmol L(-1), 50 nmol L(-1) to 35.36 μmol L(-1), 50 nmol L(-1) to 0.79 mmol L(-1), and 0.55 μmol L(-1) to 0.72 mmol L(-1), respectively and the detection limits were 1.67 μmol L(-1), 1.67 nmol L(-1), 1.67 nmol L(-1), and 0.18 μmol L(-1). The sensor demonstrated well stability, high selectivity and sensitivity. More importance, this material can be extended to construct other electrochemical sensors by the immobilization of enzymes and antibodies.

  11. Wood-Based Nanocomposite Derived by in Situ Formation of Organic-Inorganic Hybrid Polymer within Wood via a Sol-Gel Method.

    PubMed

    Dong, Xiaoying; Zhuo, Xiao; Wei, Jie; Zhang, Gang; Li, Yongfeng

    2017-03-06

    Solid wood materials and wood-plastic composites as two kinds of lightweight materials are attracting great interest from academia and industry due to their green and recycling nature. However, the relatively lower specific strength limits their wider applications. In particular, solid wood is vulnerable to moisture and decay fungi in nature, resulting in its poor durability for effectively long-term utilization. Inspired from the porous structure of wood, we propose a new design to build a wood-based nanocomposite with higher specific strength and satisfactory durability by in situ generation of organic-inorganic hybrid polymer within wood via a sol-gel method. The derived composite has 50-1200% improvement of impact toughness, 56-192% improvement of tensile strength, and 110-291% improvement of flexural strength over those of typical wood-plastic composites, respectively; and even 34% improvement of specific tensile strength than that of 36A steel; 208% enhancement of hardness; and 156% enhancement of compression strength than those of compared solid wood, respectively; as well as significantly improved dimensional stability and decay resistance over those of untreated natural wood. Such materials could be potentially utilized as lightweight and high-strength materials for applications in construction and automotive industries. This method could be extended to constitute other inorganic nanomaterials for novel organic-inorganic hybrid polymer within wood.

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

    SciTech Connect

    Not Available

    1994-11-01

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

  13. Nanocrystal/sol-gel nanocomposites

    DOEpatents

    Klimov, Victor L.; Petruska, Melissa A.

    2010-05-25

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

  14. Surface enhanced Raman scattering activity of TiN thin film prepared via nitridation of sol-gel derived TiO2 film

    NASA Astrophysics Data System (ADS)

    Dong, Zhanliang; Wei, Hengyong; Chen, Ying; Wang, Ruisheng; Zhao, Junhong; Lin, Jian; Bu, Jinglong; Wei, Yingna; Cui, Yi; Yu, Yun

    2015-10-01

    Surface-enhanced Raman scattering (SERS) is a powerful and non-destructive analytical technique tool for chemical and biological sensing applications. Metal-free SERS substrates have recently been developed by using semiconductor nanostructures. The optical property of TiN film is similar to that of gold. Besides that, its good chemical inertness and thermodynamic stability make TiN thin film an excellent candidate for SERS. In order to investigate its SERS activity, the TiN thin film was successfully prepared via direct nitridation of the sol-gel derived TiO2 thin film on the quartz substrate using ammonia gas as reducing agent. The crystallite structures and morphology of TiN thin film were determined by XRD, RAMAN and FE-SEM. The results show that the thin film obtained is cubic titanium nitride with a lattice parameter of 4.2349 Å. The surface of TiN thin film is rough and with the particles of 50 nm in average sizes. The thickness of TiN thin film is about 130 nm. The TiN thin film displays a surface Plasmon resonance absorption peak at around 476 nm, which can lead to a strong enhancement of the EM field on the interface. The Raman signal of the probe molecule R6G was greatly enhanced through TiN thin film substrates. The enhancement factor is about 4.1×103 and the detection limit achieves 10-6 M for R6G. The TiN thin film substrate also shows a good reproducibility of SERS performance. The results indicate that TiN thin film is an attractive material with potential application in SERS substrates.

  15. Transferability and Adhesion of Sol-Gel-Derived Crystalline TiO2 Thin Films to Different Types of Plastic Substrates.

    PubMed

    Amano, Natsumi; Takahashi, Mitsuru; Uchiyama, Hiroaki; Kozuka, Hiromitsu

    2017-01-31

    Anatase thin films were prepared on various plastic substrates by our recently developed sol-gel transfer technique. Polycarbonate (PC), poly(methyl methacrylate) (PMMA), polyethylene terephthalate (PET), polyethylene (PE), polypropylene (PP), polyether ether ketone (PEEK), and polyvinylidene chloride (PVDC) were employed as plastic substrates. A Si(100) substrate was first coated with a polyimide (PI)/polyvinylpyrrolidone (PVP) mixture layer, and an alkoxide-derived titania gel film was deposited on it by spin-coating. The resulting titania gel film was heated to 600 °C, during which the PI/PVP layer decomposed and the gel film was converted into a 60 nm thick anatase film. The anatase film was then transferred from the Si(100) substrate to the plastic substrate. This was achieved by heating the plastic/anatase/Si(100) stack in a near-infrared image furnace to 120-350 °C, depending on the type of plastic substrate, under unidirectional pressure. The anatase film cracked during transfer to PE, PP, PEEK, and PVDC substrates but did not crack during transfer to PC, PMMA, and PET substrates. The fraction of the total film area that was successfully transferred was assessed with the aid of image analysis. This fraction tended to be large for plastics with C═O and C-O groups and small for those without these groups. The film/substrate adhesion assessed by cross-cut tape tests also tended to be high for plastics with C═O and C-O groups and low for those without these groups. The adhesion to plastics without C═O or C-O groups could be enhanced and their transfer area fraction increased by oxidizing the native plastic surface by ultraviolet-ozone treatment prior to transfer.

  16. Ferroelectric PLZT thick films grown by poly(1-vinylpyrrolidone-co-vinyl acetate) (PVP/VA)-modified sol-gel process

    SciTech Connect

    Hu, Zhongqiang; Ma, Beihai; Li, Meiya; Koritala, Rachel E.; Balachandran, Uthamalingam

    2016-03-01

    We report the growth of ferroelectric Pb0.92La0.08Zr0.52Ti0.48O3 (PLZT) thick films using a poly(1-vinylpyrrolidone-co-vinyl acetate) (PVP/VA)-modified sol–gel process. A per-coating thickness of ≈0.66 μm has been demonstrated using PVP/VA-modified solution, which is more than doubled that of the PLZT films grown by PVP-modified method, and nearly 6 times the per-coating thickness of films prepared by conventional sol–gel process. PLZT thick films grown on LNO/Ni substrates exhibited denser microstructure, higher remanent polarization (11 μC/cm2) and dielectric tunability (45%), lower leakage current density (≈1.2 × 10-8 A/cm2), and higher breakdown strength (≈1.6 MV/cm) than those for the samples grown on PtSi substrates. These results demonstrated great potential of using PVP/VA-modified sol–gel process for high power film capacitor applications.

  17. Sol-Gel Glasses

    NASA Technical Reports Server (NTRS)

    Mukherjee, S. P.

    1985-01-01

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

  18. In-situ transmission electron microscopy crystallization studies of sol-gel-derived barium titanate thin films

    SciTech Connect

    Gust, M.C.; Mecartney, M.L.; Evans, N.D.; Momoda, L.A.

    1997-11-01

    Barium titanate (BaTiO{sub 3}) thin films that were derived from methoxypropoxide precursors were deposited onto (100) Si, Pt/Ti/SiO{sub 2}/(100) Si, and molecular-beam-epitaxy-grown (MBE-grown) (100) BaTiO{sub 3} on (100) Si substrates by spin coating. The crystallization behavior of the amorphous-gel films was characterized using in-situ transmission electron microscopy heating experiments, glancing-angle X-ray diffraction, and differential thermal analysis/thermogravimetric analysis. Amorphous-gel films crystallized at a temperature of {approximately}600 C to an intermediate nanoscale (5--10 nm) barium titanium carbonate phase, presumably BaTiO{sub 2}CO{sub 3}, that subsequently transformed to nanocrystalline (20--50 nm) BaTiO{sub 3}. Random nucleation in the bulk of the gel film was observed on all substrates. In addition, oriented growth of BaTiO{sub 3} was concurrently observed on MBE-grown BaTiO{sub 3} on (100) Si. High-temperature decomposition of the intermediate carbonate phase contributed to nanometer-scale residual porosity in the films. High concentrations of water of hydrolysis inhibited the formation of the intermediate carbonate phase; however, these sols precipitated and were not suitable for spin coating.

  19. Metal-silica sol-gel materials

    NASA Technical Reports Server (NTRS)

    Stiegman, Albert E. (Inventor)

    2002-01-01

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

  20. Photorefractive sol-gel materials

    SciTech Connect

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

    1996-12-31

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

  1. Sol-gel precursors and products thereof

    DOEpatents

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

    2017-02-14

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

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

    NASA Technical Reports Server (NTRS)

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

    1995-01-01

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

  3. Study of catalytic properties of sol-gel-derived CoO x -SiO2 film systems by the example of the growth of carbon nanomaterials

    NASA Astrophysics Data System (ADS)

    Levitskii, V. S.; Maksimov, A. I.; Moshnikov, V. A.; Terukov, E. I.

    2014-07-01

    Film catalytic samples in the Si-Co-O system in the composition range from 15 to 90 mol % Co have been prepared using the sol-gel technology. Carbon nanomaterials have been fabricated by pyrolytic synthesis using these films as catalysts. Raman spectroscopy of materials has shown that multiwalled carbon nanotubes are formed by pyrolysis on catalytic films containing Co3O4. The dependence of the carbon material length on the synthesis time has been considered. It has been shown that the average growth rate of tubes and fibers is ˜3 μm/min.

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

  5. Site-selective spectroscopy in Sm(3+)-doped sol-gel-derived nano-glass-ceramics containing SnO(2) quantum dots.

    PubMed

    Yanes, A C; Velázquez, J J; Del-Castillo, J; Méndez-Ramos, J; Rodríguez, V D

    2008-07-23

    Nano-glass-ceramics of composition 95SiO(2)-5SnO(2) doped with 0.4 Sm(3+) (mol%) were synthesized by the thermal treatment of precursor sol-gel glasses. Structural and luminescence measurements were carried out. The precipitated SnO(2) nanocrystals in the glass matrix constitute a wide bandgap quantum-dot system with size comparable to the bulk exciton Bohr radius. A site-selective excitation, by energy transfer from the semiconductor host, reveals that a fraction of the Sm(3+) ions are incorporated in the SnO(2) nanocrystals, whereas the rest remains in the silica glassy phase. An evolution in the Sm(3+) emission spectra has been observed when the SnO(2) nanocrystals are excited with different UV wavelengths, which has been ascribed to selective excitation of nanocrystal sets with predetermined size.

  6. Optical and electrical properties study of sol-gel derived Cu{sub 2}ZnSnS{sub 4} thin films for solar cells

    SciTech Connect

    Guo, B. L.; Liu, X. J.; Li, A. D. E-mail: adli@nju.edu.cn; Chen, Y. H.; Liu, W. C. E-mail: adli@nju.edu.cn

    2014-09-15

    The fabrication of environmental-friendly Cu{sub 2}ZnSnS{sub 4} (CZTS) thin films with pure kesterite phase is always a challenge to researchers in the field of solar cells. We introduce a simple non-vacuum sol-gel method to fabricate kesterite CZTS films. Ethylenediamine is used as the chelating agent and stabilizer and plays an important role in preparing stable precursor. X-ray diffraction, Raman and scanning electron microscopy studies suggest that the microstructure and optical properties of CZTS films depend strongly on annealing temperatures. The temperature dependence of conductivity of 500 °C annealed CZTS film shows that the Mott law dominates in the low temperature region and thermionic emission is predominant at high temperatures.

  7. Optical and electrical properties study of sol-gel derived Cu2ZnSnS4 thin films for solar cells

    NASA Astrophysics Data System (ADS)

    Guo, B. L.; Chen, Y. H.; Liu, X. J.; Liu, W. C.; Li, A. D.

    2014-09-01

    The fabrication of environmental-friendly Cu2ZnSnS4 (CZTS) thin films with pure kesterite phase is always a challenge to researchers in the field of solar cells. We introduce a simple non-vacuum sol-gel method to fabricate kesterite CZTS films. Ethylenediamine is used as the chelating agent and stabilizer and plays an important role in preparing stable precursor. X-ray diffraction, Raman and scanning electron microscopy studies suggest that the microstructure and optical properties of CZTS films depend strongly on annealing temperatures. The temperature dependence of conductivity of 500 °C annealed CZTS film shows that the Mott law dominates in the low temperature region and thermionic emission is predominant at high temperatures.

  8. Effect of magnesia on the degradability and bioactivity of sol-gel derived SiO2-CaO-MgO-P2O5 system glasses.

    PubMed

    Ma, J; Chen, C Z; Wang, D G; Jiao, Y; Shi, J Z

    2010-11-01

    Mesoporous 58SiO(2)-(38-x)CaO-xMgO-4P(2)O(5) glasses (where x=0, 5, 10 and 20 mol%) have been prepared by the sol-gel synthesis route. The effects of the substitution of MgO for CaO on glass degradation and bioactivity were studied in tris-(hydroxymethyl)-aminomethane and hydrochloric acid buffer solution (Tris-HCl) and simulated body fluid (SBF), respectively. It is observed that the synthesized glasses with various MgO contents possess the similar textural properties. The studies of in vitro degradability and bioactivity show that the rate of glass degradation gradually decreases with the increase of MgO and the formation of apatite layer on glass surface is retarded. The influences of the composition upon glass properties are explained in terms of their internal structures.

  9. Sol-gel synthesis of Y xGd 2- xSiO 5:Eu 3+ phosphors derived from the in situ assembly of multicomponent hybrid precursors

    NASA Astrophysics Data System (ADS)

    Huang, Honghua; Yan, Bing

    2006-04-01

    Using rare earth coordination polymers with salicylic acid as precursors for the luminescence species Y xGd 2- xSiO 5:Eu 3+, composing the polyvinyl alcohol (PVA) as dispersing media, nanophosphors of Y xGd 2- xSiO 5:Eu 3+ ( x = 0.10, 0.25, 0.50, 0.75, 0.90) with different molar ratio of Y and Gd were synthesized by the sol-gel process. Both X-ray diffraction and scanning electronic microscope show that these materials have the nanometer size of 100-200 nm. These nanometer materials exhibit red emission at 612 nm. When x = 0.5, Y 0.5Gd 1.5SiO 5:Eu 3+ shows the strongest emission intensity comparing with other molar ratio of Y to Gd.

  10. Preferred crystal orientation of sol-gel-derived Bi4-xLaxTi3O12 thin films on silicon substrates.

    PubMed

    Tajiri, Takayuki; Sumitani, Kazushi; Haruki, Rie; Kohno, Atsushi

    2007-12-01

    Polycrystalline thin films of La-substituted bismuth titanate (BLT) were formed directly on p-type Si(100) substrates by using sol-gel and spin coat methods. The BLT film and interfacial layer between BLT and Si were quantitatively investigated by the X-ray reflectivity method. Also, crystal orientations of sub-100-nm-thick BLT thin films were confirmed by X-ray diffraction using a synchrotron radiation source. The preferred c-axis orientation normal to the surface depended on the crystallization temperature. The difference in the preferred c-axis orientations of the BLT films caused the difference in the hysteresis voltage width in the capacitance-voltage characteristics of Au/BLT/p-Si structures. Furthermore, the c-axis of the Bilayered structure was preferentially oriented and aligned in the in-plane direction.

  11. Influence of (Co-Mn) co-doping on the microstructures, optical properties of sol-gel derived ZnO nanoparticles

    NASA Astrophysics Data System (ADS)

    Neena, D.; Shah, A. H.; Deshmukh, K.; Ahmad, H.; Fu, D. J.; Kondamareddy, K. K.; Kumar, P.; Dwivedi, R. K.; Sing, V.

    2016-03-01

    A systematic investigation on the synthesis, characterization, optical and magnetic properties of (Co-Mn) co doped ZnO nanoparticles synthesized by sol-gel method is reported. Structural, Optical and magnetic properties of present sample have been characterized by X-ray diffraction (XRD), UV-VIS-NIR spectroscopy and VSM techniques. The single- phased wurtzite structure has been confirmed by XRD analysis. The nanoparticles nature of the samples and their crystallinity has been investigated by TEM measurements. Optical studies revealed red shift (3.315-3.289 eV) with increasing Mn doping concentration in the absorbance spectrum. Magnetization studies showed that Zn0.7Co0.2Mn0.1O exhibits ferromagnetic behavior.

  12. Investigation of the structure and composition of film sol-gel-derived CoO x -SiO2 systems

    NASA Astrophysics Data System (ADS)

    Levitskii, V. S.; Maksimov, A. I.; Moshnikov, V. A.; Terukov, E. I.

    2014-02-01

    Samples of Si-Co-O ranging in composition from 15 to 90% of cobalt content have been synthesized by the sol-gel technology. The results of atomic force microscopy have demonstrated that the preliminary centrifugation of the solutions makes it possible to control the size of the nanospheres obtained in the stage of sol formation. For diagnostics of the phase composition of the film and bulk materials, Raman spectroscopy and X-ray powder diffraction analysis have been used. The results of X-ray powder diffraction analysis and Raman spectroscopy have revealed that the nanospheres belong to the Co3O4 spinel phase. It has been found that there is a correlation between the positions of the Raman band maxima and the nanosphere size.

  13. Biomass-Derived Heteroatom-Doped Carbon Aerogels from a Salt Melt Sol-Gel Synthesis and their Performance in Li-S Batteries.

    PubMed

    Schipper, Florian; Vizintin, Alen; Ren, Jiawen; Dominko, Robert; Fellinger, Tim-Patrick

    2015-09-21

    An ionothermal sol-gel strategy to synthesize hierarchically porous carbon aerogels doped with different heteroatoms is presented by using biomass precursors in a scalable process. Morphologically similar but chemically different materials are used to study the influence of heteroatoms in Li-S batteries. The materials show capacities as high as 1290 mAh g(-1) in the first cycle using 50 wt % S loading. Heteroatom doping reduces the capacity fading and the polarization throughout cycling. Zeta potential measurements reveal positive surface charges for heteroatom-doped carbons and indicate attractive interactions with polysulfides causing reduced fading. A polysulfide-selective sorption study reveals strongly different adsorption behavior depending on the carbon's chemical composition. Interestingly, the polysulfide fraction is also crucial. The results indicate that improved adsorption of long-chain polysulfides to doped carbons is related to improved capacity retention.

  14. Sol-gel antireflective coating on plastics

    DOEpatents

    Ashley, Carol S.; Reed, Scott T.

    1990-01-01

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

  15. Sol-gel antireflective coating on plastics

    DOEpatents

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

    1988-01-26

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

  16. Sol-gel deposited electrochromic coatings

    SciTech Connect

    Ozer, N.; Lampert, C.M.

    1995-06-01

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

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

    PubMed

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

    2012-03-18

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

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

    PubMed

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

    2016-08-17

    A pH-responsive surface molecularly imprinted poly(ionic liquids) (MIPILs) was prepared on the surface of multiwall carbon nanotubes (MWCNTs) by a sol-gel technique. The material was synthesized using a 3-aminopropyl triethoxysilane modified multiwall carbon nanotube (MWCNT-APTES) as the substrate, bovine serum albumin (BSA) as the template molecule, an alkoxy-functionalized IL 1-(3-trimethoxysilyl propyl)-3-methyl imidazolium chloride ([TMSPMIM]Cl) as both the functional monomer and the sol-gel catalyst, and tetraethoxysilane (TEOS) as the crosslinking agent. The molecular interaction between BSA and [TMSPMIM]Cl was quantitatively evaluated by UV-vis spectroscopy prior to polymerization so as to identify an optimal template/monomer ratio and the most suitable pH value for the preparation of the MWCNTs@BSA-MIPILs. This strategy was found to be effective to overcome the problems of trial-and-error protocol in molecular imprinting. The optimum synthesis conditions were as follows: template/monomer ratio 7:20, crosslinking agent content 2.0-2.5 mL, temperature 4 °C and pH 8.9 Tris-HCl buffer. The influence of incubation pH on adsorption was also studied. The result showed that the imprinting effect and selectivity improved significantly with increasing incubation pH from 7.7 to 9.9. This is mainly because the non-specific binding from electrostatic and hydrogen bonding interactions decreased greatly with the increase of pH value, which made the specific binding affinity from shape selectivity strengthened instead. The polymers synthesized under the optimal conditions were then characterized by BET surface area measurement, FTIR, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The adsorption capacity, imprinting effect, selective recognition and reusability were also evaluated. The as-prepared MWCNTs@BSA-MIPILs were also found to have a number of advantages including high surface area (134.2 m(2) g(-1)), high adsorption capacity (55.52

  19. Strain-induced crystallization in elastomeric polymer networks prepared in solution and sol-gel derived high-temperature organic-inorganic hybrid materials

    NASA Astrophysics Data System (ADS)

    Premachandra, Jagath Kumara

    Cross-linking polymer chains in solution should bring about fewer inter-chain entanglements in the resulting network. The subsequent drying of this network should compress the chains into a "super-contracted" state. The opposing effects of these changes on strain-induced crystallization in cis-1,4-polyisoprene networks formed in solution were investigated. Higher elongations were required to achieve strain-induced crystallinity in the networks prepared at higher dilutions, suggesting that in this regard the compressed states of the chains was more important than their reduced entangling. The constrained-junction theory was applied to strain-induced crystallization in the above networks. The stress-strain isotherms generated from this theory were in satisfactory agreement with experiment. It was found that the constraint parameter kappa decreases with increase in dilution during cross-linking mainly due to the fact that cross-linking in solution decreases chain interpenetration. The dependence of hydrolysis and condensation of gamma-ureidopropyltrimethoxysilane on pH in the water-methanol system at 23sp°C was investigated by FTIR spectroscopy. Quantitative analysis of rates of hydrolysis showed that gamma-ureidopropyltrimethoxysilane is most stable in the water-methanol system at pH 7.7. The rate of overall condensation of silanols produced by the hydrolysis was qualitatively analyzed. These silanol groups are relatively more stable around pH 4.87. The mechanical properties, thermal stability and water absorption of high-temperature sulfopolybenzobisthiazole-silica hybrid materials were investigated. The use of a bonding agent N,N-diethylaminopropyltrimethoxysilane facilitated the interfacial bonding between the organic and inorganic phases in these materials prepared through the sol-gel process. Tensile modulus, thermal stability and the resistant to water absorption were increased with increase in silica content in the resulting composites

  20. Preparation and application of the sol-gel-derived acrylate/silicone co-polymer coatings for headspace solid-phase microextraction of 2-chloroethyl ethyl sulfide in soil.

    PubMed

    Liu, Mingming; Zeng, Zhaorui; Fang, Huaifang

    2005-05-27

    Three types of novel acrylate/silicone co-polymer coatings, including co-poly(methyl acrylate/hydroxy-terminated silicone oil) (MA/OH-TSO), co-poly(methyl methacrylate/OH-TSO) (MMA/OH-TSO) and co-poly(butyl methacrylate/OH-TSO) (BMA/OH-TSO), were prepared for the first time by sol-gel method and cross-linking technology and subsequently applied to headspace solid-phase microextraction (HS-SPME) of 2-chloroethyl ethyl sulfide (CEES), a surrogate of mustard, in soil. The underlying mechanisms of the coating process were discussed and confirmed by IR spectra. The selectivity of the three types of sol-gel-derived acrylate/silicone coated fibers was studied, and the BMA/OH-TSO coated fibers exhibited the highest extraction ability to CEES. The concentration of BMA and OH-TSO in sol solution was optimized, and the BMA/OH-TSO (3:1)-coated fibers possessed the highest extraction efficiency. Compared with commercially available polyacrylate (PA) fiber, the sol-gel-derived BMA/OH-TSO (3:1) fibers showed much higher extraction efficiency to CEES. Therefore, the BMA/OH-TSO (3:1)-coated fibers were chosen for the analysis of CEES in soil matrix. The reproducibility of coating preparation was satisfactory, with the RSD 2.39% within batch and 3.52% between batches, respectively. The coatings proved to be quite stable at high temperature (to 350 degrees C) and in different solvents (organic or inorganic), thus their lifetimes (to 150 times) are longer than conventional fibers. Extraction parameters, such as the volume of water added to the soil, extraction temperature and time, and the ionic strength were optimized. The linearity was from 0.1 to 10 microg/g, the limit of detection (LOD) was 2.7 ng/g, and the RSD was 2.19%. The recovery of CEES was 88.06% in agriculture soil, 92.61% in red clay, and 101.95% in sandy soil, respectively.

  1. Influence of surfactant and annealing temperature on optical properties of sol-gel derived nano-crystalline TiO2 thin films.

    PubMed

    Vishwas, M; Sharma, Sudhir Kumar; Rao, K Narasimha; Mohan, S; Gowda, K V Arjuna; Chakradhar, R P S

    2010-03-01

    Titanium dioxide thin films have been synthesized by sol-gel spin coating technique on glass and silicon substrates with and without surfactant polyethylene glycol (PEG). XRD and SEM results confirm the presence of nano-crystalline (anatase) phase at an annealing temperature of 300 degrees C. The influence of surfactant and annealing temperature on optical properties of TiO(2) thin films has been studied. Optical constants and film thickness were estimated by Swanepoel's (envelope) method and by ellipsometric measurements in the visible spectral range. The optical transmittance and reflectance were found to decrease with an increase in PEG percentage. Refractive index of the films decreased and film thickness increased with the increase in percentage of surfactant. The refractive index of the un-doped TiO(2) films was estimated at different annealing temperatures and it has increased with the increasing annealing temperature. The optical band gap of pure TiO(2) films was estimated by Tauc's method at different annealing temperature.

  2. In vitro antibacterial evaluation of sol-gel-derived Zn-, Ag-, and (Zn + Ag)-doped hydroxyapatite coatings against methicillin-resistant Staphylococcus aureus.

    PubMed

    Samani, S; Hossainalipour, S M; Tamizifar, M; Rezaie, H R

    2013-01-01

    Hydroxyapatite (HAp) coatings were applied using sol-gel method. Phosphor pentoxide and calcium nitrate were used as phosphorous and calcium precursors, respectively. Zinc nitrate and silver nitrate were used as substitute of calcium in HAp structure. As a base concentration, 1.5 wt %Ag and 2.5 wt %Zn were used. The weight percent of Ag was increased at 0.3 wt% and Zn content was scaled down at 0.5 wt%. Phase analysis and chemical bonds of synthesized materials were studied by XRD and FTIR. Antibacterial activity of Ag- and Zn-doped samples against methicilin-resistant Staphylococcus aureus (MRSA) were assessed by the plate-counting method. The XRD and FTIR results proved formation of HAp compound. Colony counting showed that silver and zinc ions prevent proliferation and growth of MRSA. Interestingly, co-presence of metal ions improves the antibacterial effectiveness of the coatings and the combined effect was greater than sum of the individual effects when each was administered alone. Overall, synergism between antibacterial activities of Zn(2+) and Ag(+) ions against MRSA can be suggested. Thus, cell toxicity decreases and biocompatibility increases without any decrement in antibacterial activity.

  3. [Solid-phase microextraction coupled with capillary electrophoresis for doping analysis of propranolol enantiomers in urine using a sol-gel derived calix [4] arene fiber].

    PubMed

    Zhou, Xingwang; Li, Xiujuan; Zeng, Zhaorui

    2006-01-01

    A new type fiber coated with diglycidyloxy calix [4] arene/hydroxy-terminated silicone oil (diglycidyloxy-C [4] arene/OH-TSO) made by sol-gel method was prepared for capillary electrophoresis (CE) sample pretreatment. By using headspace solid-phase microextraction (HS-SPME) combined with a novel back-extraction facility coupled off-line to capillary zone electrophoresis (CZE), the determination of propranolol enantiomers in urine was achieved with combination of ultrasonic back-extraction and field amplified sample injection (FASI) technologies. Extraction and back-extraction parameters were optimized. The clean-up effect and preconcentration effect were realized without derivatization during the SPME process in terms of this strongly polar and thermally stable compound. Preconcentration of the sample by calix [4] arene fiber increased the sensitivity, yielding a limit of detection (LOD) of 0.01 mg/L by CZE-diode array detection (DAD). Method repeatability (relative standard deviations (RSD) < 6.5%) and fiber reusability (> 150 extraction procedures) were observed over a wide linear range of propranolol (0.05 - 10 mg/L) in urine samples. Compared with commercial SPME stationary phases, the new coating showed higher extraction efficiency and this SPME-CZE-DAD procedures could meet the demand of minimum required performance limits (MRPL) set by the World Anti-Doping Agency (WADA) for the detection of propranolol in urine samples.

  4. First observation of sol-gel derived Al:CsZnO/CsZnO bilayer thin film for solar cells application

    NASA Astrophysics Data System (ADS)

    Ahmadi, Mehdi; Rashidi Dafeh, Sajjad; Alinazmabadi, Saeid

    2016-10-01

    In this research, we fabricated CsZnO and Al:CsZnO/CsZnO bilayer thin films grown by the spin-coating-assisted sol-gel method on ITO substrate. The influence of diverse velocity of spin-coating (500, 1000, 1500, 2000, 2500 and 3000RPM) and also annealing times (30, 60, 90, 120, 150 and 180min) on the characteristics of the ZnO thin film was examined. The samples were examined by X-ray diffraction, scanning electron microscopy, Uv-Vis spectrometer and conductivity measurement. With the optimization of the velocity of spin-coating (2500RPM) and annealing times (60min), we fabricated Al:CsZnO/CsZnO bilayer thin films with diverse dopant concentration. By comparing the effect of dopant concentration with different dopant ratio (0, 0.5, 1.0 and 2%), 0.5% of CsZnO and Al:CsZnO/CsZnO bilayer was found as the most effective doping level with the best conductivity properties among the selected doping concentrations.

  5. Influences of film thickness and annealing temperature on properties of sol-gel derived ZnO-SnO2 nanocomposite thin film

    NASA Astrophysics Data System (ADS)

    Lee, Sang-Min; Joo, Young-Hee; Kim, Chang-Il

    2014-11-01

    In this study, ZnO-SnO2 nanocomposite thin film was prepared on glass substrates with different film thicknesses and annealing temperatures through a sol-gel method. From the results of thermogravimetric analysis (TGA), it was deduced that the ZnO-SnO2 thin film could be sufficiently formed at approximately 500 °C. The XRD patterns showed enhanced crystallinity of the ZnO-SnO2 thin film with increasing film thickness and annealing temperature. However, it was also revealed that the crystallinity deteriorated when the film thickness and annealing temperature are 270 nm and 700 °C, respectively. The variation in electrical resistivity corresponded to intensities of the (0 0 2) diffraction peaks shown in the XRD patterns. It was also found that the increase of film thickness and annealing temperature led to rougher surface morphology and to an increase in grain size. The optical properties deteriorated with increasing film thickness and annealing temperature of the ZnO-SnO2 thin films.

  6. Influence of heat treatment on bond strength and corrosion resistance of sol-gel derived bioglass-ceramic coatings on magnesium alloy.

    PubMed

    Shen, Sibo; Cai, Shu; Xu, Guohua; Zhao, Huan; Niu, Shuxin; Zhang, Ruiyue

    2015-05-01

    In this study, bioglass-ceramic coatings were prepared on magnesium alloy substrates through sol-gel dip-coating route followed by heat treatment at the temperature range of 350-500°C. Structure evolution, bond strength and corrosion resistance of samples were studied. It was shown that increasing heat treatment temperature resulted in denser coating structure as well as increased interfacial residual stress. A failure mode transition from cohesive to adhesive combined with a maximum on the measured bond strength together suggested that heat treatment enhanced the cohesion strength of coating on the one hand, while deteriorated the adhesion strength of coating/substrate on the other, thus leading to the highest bond strength of 27.0MPa for the sample heat-treated at 450°C. This sample also exhibited the best corrosion resistance. Electrochemical tests revealed that relative dense coating matrix and good interfacial adhesion can effectively retard the penetration of simulated body fluid through the coating, thus providing excellent protection for the underlying magnesium alloy.

  7. Synthesis, characterization and application of sol-gel derived mesoporous TiO{sub 2} nanoparticles for dye-sensitized solar cells

    SciTech Connect

    Khan, M. Alam; Shaheer Akhtar, M.; Yang, O-Bong

    2010-12-15

    Nanocrystalline mesoporous titania of anatase crystal phase were prepared by sol-gel route by varying calcination (400 C and 600 C) conditions, and the photo-electrochemical properties were investigated for dye-sensitized solar cell applications. The TTIP precursor in n-heptane solvent with ratio of water to TTIP (5:1) was found to be effective substrate for the working electrodes. The overall conversion efficiency of 7.59% was achieved under 1 sun irradiation with open circuit voltage of 0.77 V, current density of 17.00 mA/cm{sup 2} and FF of 51.12. The high efficiency of the 400 C calcined sample were attributed to its mesopores, high BET surface area (80.1 m{sup 2}/g) and large pore volume of prepared titania substrate which provide better surface for the absorption of dye, improves light harvesting efficiency and better charge injection. The prepared samples were characterized by XRD, small angle XRD, FE-SEM, TEM, IPCE, I-V curve, BET surface area and BJH plot techniques. (author)

  8. Effects of rare earth ions (Tb, Ce, Eu, Dy) on the thermoluminescence characteristics of sol-gel derived and γ-irradiated SiO2 nanoparticles.

    PubMed

    Bajpai, Namrata; Tiwari, Ashish; Khan, S A; Kher, R S; Bramhe, Namita; Dhoble, S J

    2014-09-01

    Highly pure SiO2 and SiO2 :RE nanoparticles were synthesized by the sol-gel method. The morphological, structural and optical properties of the nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). XRD results indicate that all the samples studied were free from impurities. SEM/TEM results indicate that the samples were well dispersed. Surface characterization of the nanocrystals by Fourier transform infrared spectroscopy has been carried out and the structure of surface-bound SiO2 based on spectral analysis is proposed. Thermoluminescence (TL) characteristics were investigated to study the influence of rare earth dopants (Tb, Ce, Eu, Dy) on SiO2 matrix subjected to 0.5 kG (1 h) γ-irradiation. Among these rare earth elements, Eu(3+) was found to be the most efficient dopant for SiO2 showing maximum thermoluminescence intensity. SiO2 :Eu0.5 seems to be a promising candidate for use as a TL dosimeter.

  9. Sol-gel-derived bioactive glass containing SiO2-MgO-CaO-P2O5 as an antibacterial scaffold.

    PubMed

    Fooladi, Abbas Ali Imani; Hosseini, Hamideh Mahmoodzadeh; Hafezi, Forough; Hosseinnejad, Fatemeh; Nourani, Mohammad Reza

    2013-06-01

    Bioactive glass (BG) composites with a base of SiO2-Na2O-CaO-P2O5 are biocompatible biomaterials. The assessment of their abilities for medical applications has interested researchers. We produced a BG-containing SiO2-MgO-CaO-P2O5 by the sol-gel method. To determine the antibacterial effects, we analyzed the minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) properties of this product on three microorganisms, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa, known causative agents for biofilm formation on implant surfaces. In addition, we performed the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay to study the cytotoxic effects of our composite on animal cells. Our results demonstrated that our BG product inhibited the growth of bacteria in a concentration-dependent manner without any cytotoxic effects. Therefore, our BG product can be utilized as an appropriate implant for treating bone and tooth defects.

  10. Morphological and optical properties of sol-gel derived 6SrO·6BaO·7Al 2O 3 thin films

    NASA Astrophysics Data System (ADS)

    Chavhan, P. M.; Sharma, Anubha; Sharma, R. K.; Kaushik, N. K.

    2010-01-01

    A novel 6SrO·6BaO·7Al 2O 3 (S6B6A7) thin film deposited onto soda lime float glass via sol-gel dip coating technique is reported. The morphological and compositional properties of the S6B6A7 thin films have been investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) revealing that the films were composed of S6B6A7 nanoparticles. The optical properties of the S6B6A7 films are affected by sol concentration, film thickness and annealing temperature as revealed by UV-vis transmittance. The transparency of S6B6A7 films improved on increasing annealing temperature up to 450 °C in air. The S6B6A7 films prepared using 2, 5, and 8 (wt.%) sols and annealed at 450 °C exhibit an average transmittance of over ˜91% in wide visible range.

  11. Organic-inorganic crosslinked and hybrid membranes derived from sulfonated poly(arylene ether sulfone)/silica via sol-gel process

    NASA Astrophysics Data System (ADS)

    Feng, Shaoguang; Shang, Yuming; Wang, Yingzi; Xie, Xiaofeng; Mathur, V. K.; Xu, Jingming

    A series of covalently crosslinkable organic-inorganic hybrid membranes have been prepared from sulfonated poly(arylene ether sulfone) (SPAES) with pendant propenyl moiety and various amounts of vinyl substituted silica via sol-gel process which are then thermally crosslinked in the presence of benzoyl peroxide (BPO) initiator. The obtained membranes are characterized in terms of oxidative stability, thermal property, ion exchange capacity (IEC), water uptake, swelling ratio in methanol aqueous solution, proton conductivity, and methanol permeability coefficient. The results indicate that the oxidative stability and thermal stability of the hybrid membranes are improved. Moreover, introduction of silica reduces the water uptake and methanol swelling of membranes. The swelling ratio of membranes in 2 mol L -1 methanol aqueous solution at 80 °C slowly decreases from 26 to 19% with the increase of SiO 2 content from 0 to 12 wt.%. Furthermore, with the increase in silica content, the methanol permeability coefficient of the hybrid membranes decreases at first and then increases. When the silica content reaches 8 wt.%, the methanol permeability coefficient is at the minimum of 6.02 × 10 -7 cm 2 s -1, a 2.64-fold decrease compared with that of the pristine SPAES membrane. Moreover, the proton conductivity is found to be at about 95% of that of pristine polymer at that silica content.

  12. The influence of silver nanostructures formed in situ in silica sol-gel derived films on the rate of Förster resonance energy transfer.

    PubMed

    Holmes-Smith, A Sheila; McDowell, Gary R; Toury, Marion; McLoskey, David; Hungerford, Graham

    2012-02-01

    The efficiency of Förster resonance energy transfer (FRET) can be enhanced in the presence of a metal. Herein, we demonstrate the increased efficiency for a novel model sensor system where FRET is shown to occur between Rhodamine 6G in the bulk sol-gel matrix and Texas Red, which is held a fixed distance away by covalent attachment onto a silane spacer. Silver colloids are formed using light to initiate the reduction of a silver salt, which can be achieved at controlled locations within the film. Both the fluorescence intensity and lifetime maps and analysis indicate that an enhanced FRET efficiency has been achieved in the presence of silver nanoparticles. An increase in efficiency of 1.2-1.5 times is demonstrated depending on the spacer used. The novelty of our approach lies in the method of silver-nanoparticle formation, which allows for the accurate positioning of the silver nanoparticles and hence selective fluorescence enhancement within a biocompatible host material. Our work gives a practical demonstration of metal-enhanced FRET and demonstrates the ability of such systems to be developed for molecular-recognition applications that could find use in lab-on-a-chip technologies.

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

    NASA Technical Reports Server (NTRS)

    Chu, Chung-tse; Zheng, Haixing

    1996-01-01

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

  14. Processing and mechanical behavior of Nicalon/SiC and Nextel/SiC composites with sol-gel derived oxide interfacial coatings

    NASA Astrophysics Data System (ADS)

    Shanmugham, Subramaniam

    Mullite and aluminum titanate precursor sols were developed for coating applications. High temperature X-ray diffraction studies in air identified that mullite crystallizes between 950sp°C and 1050sp°C, while aluminum titanate forms between 1200sp°C and 1400sp°C. The crystallization temperature of mullite was lowered by 100sp°C compared to those reported in the literature. Nicalon tows are embrittled during the formation of mullite at 1000sp°C, and hence, there is a need to protect the fibers by a relatively inert material during the sol-gel oxide processing. The aluminum titanate formation temperature is high and would damage Nicalon and Nextel fibers. However, Nicalon fibers dip-coated in an aluminum titanate sol and heat-treated at 1000sp°C for up to 10 h in air, forming an alumina-titania (Alsb2Osb3-TiOsb2) mixture, were not embrittled. Based on the non-embrittlement of the fibers, the Alsb2Osb3-TiOsb2 mixture was chosen as an alternative to aluminum titanate for an interface material. To study the effect of protecting the fibers by an inert material during sol-gel oxide coating, oxide/C, and C/oxide/C interfaces were considered for Nicalon/SiC and Nextel/SiC composites. Since composites with C/oxide/C interfaces exhibited higher flexural strengths than composites with oxide/C interfaces in the as-processed condition, C/oxide/C interfaces were studied. Also, Nicalon/SiC composites with C/oxide/C interfaces retained damage-tolerant behavior and substantial amount of their as-processed strengths even after 24 h oxidation at 1000sp°C in air than Nextel/SiC composites with C/oxide/C interfaces. On these basis, Nicalon/SiC composites with C/oxide/C interfaces were chosen for further investigation. Transmission electron microscopy studies identified that the obtained oxide coatings were very thin ($73%). Nicalon/SiC composites with C/oxide/C interfaces performed poorly at 750spcircC, so Nicalon/SiC composites with BN/oxide/BN interfaces were fabricated and

  15. Simultaneous, real-time measurement of nitric oxide and oxygen dynamics during cardiac ischemia-reperfusion of the rat utilizing sol-gel-derived electrochemical microsensors.

    PubMed

    Kang, Sung Wook; Kim, Ok Kyun; Seo, Bochan; Lee, Sung Ho; Quan, Fu Shi; Shin, Jae Ho; Lee, Gi-Ja; Park, Hun-Kuk

    2013-11-13

    In this study, we simultaneously measured nitric oxide (NO) and oxygen (O2) dynamics in the myocardium during myocardial ischemia-reperfusion (IR) utilizing sol-gel modified electrochemical NO and O2 microsensors. In addition, we attempted to clarify the correlation between NO release in the ischemic period and O2 restoration in the myocardium after reperfusion, comparing a control heart with a remote ischemic preconditioning (RIPC)-treated heart as an attractive strategy for myocardial protection. Rat hearts were randomly divided into two groups: a control group (n=5) and an RIPC group (n=5, with RIPC treatment). Myocardia that underwent RIPC treatment (182±70 nM, p<0.05) released more NO during the ischemic period than those of the control group (63±41 nM). The restoration value of oxygen tension (pO2) in the RIPC group significantly increased and was restored to pre-ischemic levels (92.6±36.8%); however, the pO2 of the control group did not increase throughout the reperfusion period (5.7±7.5%, p=0.001). Myocardial infarct size measurements revealed a significant decrease in cell death in the myocardium region of the RIPC group (41.44±6.42%, p=0.001) compared with the control group (60.05±10.91%). As a result, we showed that the cardioprotective effect of RIPC could be attributed to endogenous NO production during the ischemic period, which subsequently promoted reoxygenation in post-ischemic myocardia during early reperfusion. Our results suggest that the promotion of endogenous formation during an ischemic episode might be helpful as a therapeutic strategy for protecting the myocardium from IR injury. Additionally, our NO and O2 perm-selective microsensors could be utilized to evaluate the effect of drug or treatment.

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

    SciTech Connect

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

    1995-04-01

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

  17. Sol-gel optical coatings for lasers, 3

    SciTech Connect

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

    1995-12-01

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

  18. Neutron detector using sol-gel absorber

    DOEpatents

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

    1999-01-01

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

  19. Hybrid sol-gel optical materials

    DOEpatents

    Zeigler, J.M.

    1993-04-20

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

  20. Hybrid sol-gel optical materials

    DOEpatents

    Zeigler, John M.

    1993-01-01

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

  1. Hybrid sol-gel optical materials

    DOEpatents

    Zeigler, John M.

    1992-01-01

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

  2. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna

    1992-01-01

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

  3. Up-conversion in sol-gel derived nano-glass-ceramics comprising NaYF 4 nano-crystals doped with Yb 3+, Ho 3+ and Tm 3+

    NASA Astrophysics Data System (ADS)

    Santana-Alonso, A.; Méndez-Ramos, J.; Yanes, A. C.; del-Castillo, J.; Rodríguez, V. D.

    2010-07-01

    NaYF 4 is an excellent host material for rare-earth ions presenting very high efficiencies in up-conversion processes. Thus, nano-glass-ceramics containing NaYF 4 nano-crystals emerge as promising candidates for general lighting appliances and integrated optical devices. Here we report highly transparent sol-gel derived nano-glass-ceramics comprising Yb 3+-Ho 3+ and Yb 3+-Ho 3+-Tm 3+ co-doped NaYF 4 nano-crystals. A structural analysis by means of X-ray diffraction measurements confirmed the formation of NaYF 4 nano-crystals during thermal treatment. Luminescence features have been related to the crystallinity degree of the samples. Violet, blue, green and red up-conversion emissions were obtained under infrared excitation at 980 nm and corresponding mechanisms involved have been analysed. Additionally, the total visible up-conversion emission has been quantified in terms of the standard chromaticity coordinates. In particular, an overall colour emission, very close to the standard equal energy white-light illumination point of the chromaticity diagram, was obtained in the Yb 3+-Ho 3+-Tm 3+ triply-doped samples.

  4. Innovative materials based on sol gel technology

    NASA Astrophysics Data System (ADS)

    Reisfeld, Renata; Saraidarov, Tsiala

    2006-01-01

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

  5. Droplet Spreading with Sol-Gel Transition

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

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

  6. Ring-Resonator/Sol-Gel Interferometric Immunosensor

    NASA Technical Reports Server (NTRS)

    Bearman, Gregory; Cohen, David

    2007-01-01

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

  7. Sol-Gel Manufactured Energetic Materials

    DOEpatents

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

    2005-05-17

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

  8. Sol-gel manufactured energetic materials

    DOEpatents

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

    2003-12-23

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

  9. Sol-gel based optical chemical sensors

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

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

  10. Ferroelectric Self-Assembled PbTiO3 Perovskite Nanostructures Onto (100)SrTiO3 Substrates From a Novel Microemulsion Aided Sol-Gel Preparation Method

    SciTech Connect

    Calzada, M.L.; Torres, M.; Fuentes-Cobas, L.E.; Mehta, A.; Ricote, J.; Pardo, L.; /Madrid, ICM

    2007-10-17

    A novel preparation method, which involves the use of microemulsions, sol-gel chemistry and chemical solution deposition, has been developed in this work for the preparation of layers of PbTiO3 nanostructures supported on SrTiO3 substrates. A transparent solution was first prepared by mixing a PbTiO3 precursor sol and a microemulsion formed by water, cyclohexane and the surfactant Brij 30 (polyoxyethylene(4) lauryl ether). The solution was deposited onto the SrTiO3 substrate by spin-coating and dried under controlled conditions (temperature, time and relative humidity) to favor the rearrangement of the micelles in the deposited coat. After a rapid thermal treatment of crystallization at 650 C, nanostructures with uniform sizes of 40 nm diameter and showing periodicity in some zones of the substrate are obtained. The analysis of these nanostructures by grazing-incidence x-ray synchrotron radiation indicates that they have a perovskite structure with a <100> preferred orientation and that they are under strained conditions. Thermal treatments at higher temperatures produce the collapse of the ordered nanoparticles' network and the formation of larger isolated particles of PbTiO3 with a truncated-pyramid morphology. Piezoresponse force microscopy studies demonstrate that the spontaneous polarization of these PbTiO3 nanostructures can be switched and that they have piezoelectric activity. These results support the fabrication strategy here proposed as a promising approach for the preparation of nanoferroelectrics onto substrates of possible interest in future nanoelectronic devices.

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

    SciTech Connect

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

    2009-02-13

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

  12. Ionogel Electrolytes through Sol-Gel Processing

    NASA Astrophysics Data System (ADS)

    Horowitz, Ariel I.

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

  13. Preparation and characterization of urease-encapsulated biosensors in poly(vinyl alcohol)-modified silica sol-gel materials.

    PubMed

    Tsai, Hsiao-chung; Doong, Ruey-an

    2007-08-30

    The microenvironments of the sol-gel-derived urease biosensors in terms of elemental ratio, surface morphology, specific surface area and pore size were investigated to characterize the physicochemical properties of poly(vinyl alcohol) (PVA)-modified sol-gel materials. X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and surface area analyzer were used to identify the surface species, topography and pore distribution of the organically doped sol-gel network. XPS results showed that stoichiometric ratios of oxygen-to-silicon in sol-gel materials were in the range 2.08-2.11. The sol-gel materials were partially dried and negatively charged, which retained 6-8% water content to maintain urease activity. The surface morphology of the sol-gel altered obviously when macromolecules were encapsulated, resulting in the increase in surface mean roughness from 0.207 to 2.636 nm. The specific surface area decreased dramatically after the immobilization of biomolecules and organic additives, which clearly depicts that PVA and urease were co-encapsulated into the sol-gel network. However, there still exist enough pore volumes for analytes to mass transport. The apparent Michaelis-Menten constant value (Km) of the encapsulated urease was similar to that in solution and the overall catalytic efficiency in PVA-doped sol-gel-derived glasses only decreased by a factor of 3.2 relative to the value in solution. In addition, the analytical performance of the entrapped urease in PVA-doped sol-gel materials was examined by determining the Cu(II) concentration in aqueous solution. The analytical range of Cu(II) was in the range 2x10(-6) to 2x10(-2) M with a detection limit of 1.5 microg L(-1). Results obtained in this study demonstrate a strategy for maintaining urease activity for biomedical and environmental applications.

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

    NASA Technical Reports Server (NTRS)

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

    2002-01-01

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

  15. Ultrafast Sol-Gel Synthesis of Graphene Aerogel Materials

    SciTech Connect

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

    2015-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1994-09-01

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

  17. The Sol-Gel-Xerogel Transition

    DTIC Science & Technology

    1993-11-01

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

  18. Sol-gel optical coatings for lasers, 2

    SciTech Connect

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

    1995-11-01

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

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

    PubMed

    Mercadé-Prieto, Ruben; Gunasekaran, Sundaram

    2009-05-19

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

  20. Photocurable bioactive bone cement based on hydroxyethyl methacrylate-poly(acrylic/maleic) acid resin and mesoporous sol gel-derived bioactive glass.

    PubMed

    Hesaraki, S

    2016-06-01

    This paper reports on strong and bioactive bone cement based on ternary bioactive SiO2-CaO-P2O5 glass particles and a photocurable resin comprising hydroxyethyl methacrylate (HEMA) and poly(acrylic/maleic) acid. The as-cured composite represented a compressive strength of about 95 MPa but it weakened during soaking in simulated body fluid, SBF, qua its compressive strength reached to about 20 MPa after immersing for 30 days. Biodegradability of the composite was confirmed by reducing its initial weight (~32%) as well as decreasing the molecular weight of early cured resin during the soaking procedure. The composite exhibited in vitro calcium phosphate precipitation in the form of nanosized carbonated hydroxyapatite, which indicates its bone bonding ability. Proliferation of calvarium-derived newborn rat osteoblasts seeded on top of the composite was observed during incubation at 37 °C, meanwhile, an adequate cell supporting ability was found. Consequently, it seems that the produced composite is an appropriate alternative for bone defect injuries, because of its good cell responses, high compressive strength and ongoing biodegradability, though more in vivo experiments are essential to confirm this assumption.

  1. Sol-gel method for encapsulating molecules

    DOEpatents

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

    2002-01-01

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

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

    DOEpatents

    Malik, Abdul; Shearrow, Anne M.

    2017-01-31

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

  3. Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

    ERIC Educational Resources Information Center

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

    2010-01-01

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

  4. Chemical preparation of ferroelectric mesoporous barium titanate thin films: drastic enhancement of Curie temperature induced by mesopore-derived strain.

    PubMed

    Suzuki, Norihiro; Jiang, Xiangfen; Salunkhe, Rahul R; Osada, Minoru; Yamauchi, Yusuke

    2014-09-01

    Mesoporous barium titanate (BT) thin films are synthesized by a surfactant-assisted sol-gel method. The obtained mesoporous BT thin films show enhanced ferroelectricity due to the effective strains induced by mesopores. The Curie temperature (T(c)) of the mesoporous BT reaches approximately 470 °C.

  5. Schiff base mediated sol-gel polymerization

    SciTech Connect

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

    1996-12-31

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

  6. Sol-gel processing of energetic materials

    SciTech Connect

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

    1997-08-18

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

  7. Renewable-surface sol-gel derived carbon ceramic electrode fabricated by [Ru(bpy)(tpy)Cl]PF6 and its application as an amperometric sensor for sulfide and sulfur oxoanions.

    PubMed

    Salimi, Abdollah; Pourbeyram, Sima; Amini, Mohamad Kazem

    2002-12-01

    A highly sensitive and fast responding sensor for the determination of thiosulfate, sulfite, sulfide and dithionite is described. It consists of a chemically modified carbon ceramic composite electrode (CCE) containing [Ru(bpy)(tpy)Cl]PF6 complex that was constructed by the sol-gel technique. A reversible redox couple of Ru(II)/Ru(III) was observed as a solute in acetonitrile solution and as a component of carbon based conducting composite electrode. Electrochemical behavior and stability of modified CCE were investigated by cyclic voltametry, the apparent electron transfer rate constant (kappa(S)) and transfer coefficient (a) were determined by cyclic voltametry which were about 28 s(-1) and 0.43 respectively. Electrocatalytic oxidation of S(2-), SO3(2-), S2O4(2-) and S2O3(2-) were effective at the modified electrode at significantly reduced overpotentials and in the pH range 1-11. Optimum pH values for amperometric detection of thiosulfate, dithionite, sulfide and sulfite are 7, 9, 2 and 2. Under the optimized conditions the calibration curves are linear in the concentration ranges 1-500, 3-80, 2-90 and 1-100 microM for S2O3(2-), SO3(2-), S2- and S2O4(2-) determination. The detection limit (signal to noise is 3) and sensitivity are 0.5 and 12, 2.8 and 6, 1.6 and 8, and 0.65 microM and 80 nA microM(-1) for thiosulfate, sulfite, sulfide and dithionite detection. The modified carbon ceramic electrode doped with Ru-complex shows good reproducibility, a short response time (t < 2 s), remarkable long term stability (> 6 month) and especially good surface renewability by simple mechanical polishing (RSD for eight successive polishing is 2%). The advantages of this sulfur compound amperometric detector based on ruthenium doped CCE are high sensitivity, inherent stability at a broader pH range, excellent catalytic activity, less expense and simplicity of preparation in comparison with recently published papers. This sensor can be used as a chromatographic detector for

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

    DTIC Science & Technology

    1989-09-10

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

  9. Preparation and complex characterization of silica holmium sol-gel monoliths.

    PubMed

    Cacaina, D; Areva, S; Laaksonen, H; Simon, S; Ylänen, H

    2011-01-01

    Amorphous, sol-gel derived SiO(2) are known to biocompatible and bioresorbable materials. Biodegradable and inert materials containing radioactive isotopes have potential application as delivery vehicles of the beta radiation to the cancer tumors inside the body. Incorporation of holmium in the sol-gel derived SiO(2) could lead to the formation of a biodegradable material which could be used as carrier biomaterial for the radiation of radioactive holmium to the various cancer sites. The homogeneity of the prepared sol-gel silica holmium monoliths was investigated by Back Scattered Electron Imaging of Scanning Electron Microscope equipped with Energy Dispersive X-ray Analysis, X-ray Induced Photoelectron Spectroscopy and Nuclear Magnetic Resonance Spectroscopy. The biodegradation of the monoliths was investigated in Simulated Body Fluid and TRIS (Trizma pre-set Crystals) solution. The results show that by suitable tailoring of the sol-gel processing parameters holmium can be homogeneously incorporated in the silica matrix with a controlled biodegradation rate.

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

    PubMed

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

    2014-02-18

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

  11. Gradient Index Lenses From Sol-Gel Layering.

    DTIC Science & Technology

    2008-02-15

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

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

    DTIC Science & Technology

    1987-11-01

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

  13. Oxide Ceramic Fibers by the Sol-Gel Methods

    DTIC Science & Technology

    1989-02-10

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

  14. Sol-gel entrapped cobalt complex

    SciTech Connect

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

    2003-03-15

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

  15. Electrophoretic Porosimetry of Sol-Gels

    NASA Technical Reports Server (NTRS)

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

    2000-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1990-01-01

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

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

    PubMed

    Chen, Xiaohong; Wilson, George S

    2004-09-28

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

  18. Prospects of sol-gel technology towards luminescent materials

    NASA Astrophysics Data System (ADS)

    Reisfeld, R.

    2001-02-01

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

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

    PubMed

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

    2013-07-01

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

  20. Perovskite phase transformation in 0.65Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-0.35PbTiO{sub 3} nanoparticles derived by sol-gel

    SciTech Connect

    Singh, Satyendra; Krupanidhi, S. B.

    2012-01-15

    Fabrication of 0.65Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-0.35PbTiO{sub 3} (PMN-PT) nanoparticles with an average size of about 40 nm and their phase transformation behavior from pyrochlore to perovskite phase is investigated. A novel sol-gel method was used for the synthesis of air-stable and precipitate-free diol-based sol of PMN-PT which was dried and partially calcined at 450 deg. C for 1 h to decompose organics and bring down the free energy barrier for perovskite crystallization and then finally annealed in the temperature range 600 to 700 deg. C. Annealed at around 700 deg. C for 1 h, PMN-PT gel powder exhibited nanocrystalline morphology with perovskite phase as confirmed by the transmission electron microscopy and X-ray diffraction techniques.

  1. CROSS-DISCIPLINARY PHYSICS AND RELATED AREAS OF SCIENCE AND TECHNOLOGY: Effect of Annealing Conditions on Properties of Sol-Gel Derived Al-Doped ZnO Thin Films

    NASA Astrophysics Data System (ADS)

    Gao, Mei-Zhen; Zhang, Feng; Liu, Jing; Sun, Hui-Na

    2009-08-01

    Transparent conductive Al-doped ZnO (AZO) thin films are prepared on normal glass substrates by the sol-gel spin coating method. The effects of drying conditions, annealing temperature and cooling rate on the structural, electrical and optical properties of AZO films are investigated by x-ray diffraction, scanning electron microscopy, the four-point probe method and UV-VIS spectrophotometry, respectively. The deposited films show a hexagonal wurtzite structure and high preferential c-axis orientation. As the drying temperature increases from 100°C to 300°C the resistivity of AZO films decreases dramatically. In contrast to the annealed films cooled in a furnace and in air, the resistivity of the annealed film which is cooled at -15°C is greatly reduced. Increasing the cooling rate dramatically increases the electrical conductivity of AZO films.

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

    PubMed

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

    2014-12-01

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

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

    NASA Astrophysics Data System (ADS)

    Fang, Jonathan

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

  4. MOS solar cells with oxides deposited by sol-gel spin-coating techniques

    SciTech Connect

    Huang, Chia-Hong; Chang, Chung-Cheng; Tsai, Jung-Hui

    2013-06-15

    The metal-oxide-semiconductor (MOS) solar cells with sol-gel derived silicon dioxides (SiO{sub 2}) deposited by spin coating are proposed in this study. The sol-gel derived SiO{sub 2} layer is prepared at low temperature of 450 Degree-Sign C. Such processes are simple and low-cost. These techniques are, therefore, useful for largescale and large-amount manufacturing in MOS solar cells. It is observed that the short-circuit current (I{sub sc}) of 2.48 mA, the open-circuit voltage (V{sub os}) of 0.44 V, the fill factor (FF) of 0.46 and the conversion efficiency ({eta}%) of 2.01% were obtained by means of the current-voltage (I-V) measurements under AM 1.5 (100 mW/cm{sup 2}) irradiance at 25 Degree-Sign C in the MOS solar cell with sol-gel derived SiO{sub 2}.

  5. Sol-gel production of bioactive nanocoatings for medical applications. Part 1: an introduction.

    PubMed

    Ben-Nissan, Besim; Choi, Andy H

    2006-10-01

    Coatings offer the possibility of modifying the surface properties of surgical-grade materials to achieve improvements in performance, reliability and biocompatibility. Sol-gel-derived coatings demonstrate promise owing to their relative ease of production, ability to form a physically and chemically pure and uniform coating over complex geometric shapes and potential to deliver exceptional mechanical properties owing to their nanocrystalline structure. Other advantages unique to sol-gel include the production of a homogeneous material, since mixing takes place on the atomic scale, and its relatively low processing temperature avoids decomposition of the coating materials and limits the damage to metallic substrate materials as a result of exposure to elevated temperatures. A range of materials can be adapted easily for a number of biomedical and engineering applications.

  6. Glucose microbiosensor based on alumina sol-gel matrix/electropolymerized composite membrane.

    PubMed

    Chen, Xiaohong; Hu, Yibai; Wilson, George S

    2002-12-01

    A procedure is described that provides co-immobilization of enzyme and bovine serum albumin (BSA) within an alumina sol-gel matrix and a polyphenol layer permselective for endogenous electroactive species. BSA has first been employed for the immobilization of glucose oxidase (GOx) on a Pt electrode in a sol-gel to produce a uniform, thin and compact film with enhanced enzyme activity. Electropolymerization of phenol was then employed to form an anti-interference and protective polyphenol film within the enzyme layer. In addition, a stability-reinforcing membrane derived from (3-aminopropyl)-trimethoxysilane was constructed by electrochemically-assisted crosslinking. This hybrid film outside the enzyme layer contributed both to the improved stability and to permselectivity. The resulting glucose sensor was characterized by a short response time (<10 s), high sensitivity (10.4 nA/mM mm(2)), low interference from endogenous electroactive species, and a working lifetime of at least 60 days.

  7. Sol-gel technologies for multimode waveguide structures

    NASA Astrophysics Data System (ADS)

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

    2002-06-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2004-01-01

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

  9. Sol-gel processing with inorganic metal salt precursors

    DOEpatents

    Hu, Zhong-Cheng

    2004-10-19

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

  10. Silica scintillating materials prepared by sol-gel methods

    SciTech Connect

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

    1993-12-31

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

  11. Influence of calcinated and non calcinated nanobioglass particles on hardness and bioactivity of sol-gel-derived TiO2-SiO2 nano composite coatings on stainless steel substrates.

    PubMed

    Dadash, Mohammad Saleh; Karbasi, Saeed; Esfahani, Mojtaba Nasr; Ebrahimi, Mohammad Reza; Vali, Hojatollah

    2011-04-01

    Thick films of calcinated and non calcinated nanobioglass (NBG)-titania composite coatings were prepared on stainless steel substrates by alkoxide sol-gel process. Dip-coating method was used for the films preparation. The morphology, structure and composition of the nano composite films were evaluated using environmental scanning electron microscope, X-ray diffraction and Fourier transform infrared spectroscope. The SEM investigation results showed that prepared thick NBG-titania films are smooth and free of macrocracking, fracture or flaking. The grain size of these films was uniform and nano scale (50-60 nm) which confirmed with TEM. Also FTIR confirmed the presence of Si-O-Si bands on the calcinated NBG-titania films. The hardness of the prepared films (TiO(2)-calcinated NBG and TiO(2)-Non calcinated NBG) was compared by using micro hardness test method. The results verified that the presence of calcinated NBG particles in NBG-titania composite enhanced gradually the mechanical data of the prepared films. The in vitro bioactivity of these films was discussed based on the analysis of the variations of Ca and P concentrations in the simulated body fluid (SBF) and their surface morphologies against immersion time. Surface morphology and Si-O-Si bands were found to be of great importance with respect to the bioactivity of the studied films. The results showed that calcinated NBG-titania films have better bioactivity than non calcinated NBG-titania films.

  12. THE THICKNESS DEPENDENCE OF OXYGEN PERMEABILITY IN SOL-GEL DERIVED CGO-COFE2O4 THIN FILMS ON POROUS CERAMIC SUBSTRATES: A SPUTTERED BLOCKING LAYER FOR THICKNESS CONTROL

    SciTech Connect

    Brinkman, K

    2009-01-08

    Mixed conductive oxides are a topic of interest for applications in oxygen separation membranes as well as use in producing hydrogen fuel through the partial oxidation of methane. The oxygen flux through the membrane is governed both by the oxygen ionic conductivity as well as the material's electronic conductivity; composite membranes like Ce{sub 0.8}Gd{sub 0.2}O{sub 2-{delta}} (CGO)-CoFe{sub 2}O{sub 4} (CFO) use gadolinium doped ceria oxides as the ionic conducting material combined with cobalt iron spinel which serves as the electronic conductor. In this study we employ {approx} 50 nm sputtered CeO{sub 2} layers on the surface of porous CGO ceramic substrates which serve as solution 'blocking' layers during the thin film fabrication process facilitating the control of film thickness. Films with thickness of {approx} 2 and 4 microns were prepared by depositing 40 and 95 separate sol-gel layers respectively. Oxygen flux measurements indicated that the permeation increased with decreasing membrane thickness; thin film membrane with thickness on the micron level showed flux values an order of magnitude greater (0.03 {micro}mol/cm{sup 2} s) at 800 C as compared to 1mm thick bulk ceramic membranes (0.003 {micro}mol/cm{sup 2}).

  13. A needle trap device packed with a sol-gel derived, multi-walled carbon nanotubes/silica composite for sampling and analysis of volatile organohalogen compounds in air.

    PubMed

    Heidari, Mahmoud; Bahrami, Abdolrahman; Ghiasvand, Ali Reza; Shahna, Farshid Ghorbani; Soltanian, Ali Reza

    2013-06-27

    A needle trap device (NTD) packed with silica composite of multi-walled carbon nanotubes (MWCNTs) prepared based on sol-gel technique was utilized for sampling and analysis of volatile organohalogen compounds (HVOCs) in air. The performance of the NTD packed with MWCNTs/silica composite as sorbent was examined in a variety of sampling conditions and was compared with NTDs packed with PDMS as well as SPME with Carboxen/PDMS-coated fibers. The limit of detection of NTDs for the GC/MS detection system was 0.01-0.05 ng mL(-1) and the limit of quantitation was 0.04-0.18 ng mL(-1). The RSD were 1.1-7.8% for intra-NTD comparison intended for repeatability of technique. The NTD-MWCNTs/silica composite showed better analytical performances compared to the NTD-PDMS composite and had the same analytical performances when compared to the SPME-Carboxen/PDMS fibers. The results show that NTD-MWCNTs-GC/MS is a powerful technique for active sampling of occupational/environmental pollutants in air.

  14. Conformal sol-gel coatings on three-dimensional nanostructured templates

    NASA Astrophysics Data System (ADS)

    Weatherspoon, Michael R.

    Sol-gel processing techniques, such as spin coating and dip coating, have successfully been utilized over the past several decades to apply conformal coatings on planar substrates; however, controlled film growth on three-dimensional (3-D) nanostructured templates using the sol-gel process remains a significant challenge. Obstacles such as, uncontrolled hydrolyzation and condensation of metal alkoxide precursors on nanostructured surfaces are a few of the obstacles which lead to coatings with undesirable thicknesses and excess inorganic particles. A little over a decade ago, a surface sol-gel process was developed which utilizes stepwise film growth of anhydrous metal alkoxide precursors with hydroxylated surfaces. The surface sol-gel process provides control over the applied coating thickness and is viewed as a wet chemical analog to atomic layer deposition (ALD). The work presented in this dissertation has focused on applying conformal sol-gel derived coatings with controlled thicknesses on 3-D nanostructured templates. The templates utilized in this work were derived from biological species, such as diatoms and butterflies, as well as a synthetic photoresist polymer (SU-8). Coatings were applied on the templates using a conventional reflux/evaporation deposition process and a custom-built computer controlled surface sol-gel pumping system. The coatings applied using the reflux/evaporation process yielded conformal coatings with uncontrolled film thicknesses whereas the coatings applied using the surface sol-gel process yielded conformal coatings with controlled thicknesses. Barium titanate and europium-doped barium titanate coatings were applied on diatom frustules using the reflux/evaporation deposition process. The silica-based diatom frustules had to first be converted into magnesia/silicon composite replicas using a gas/solid displacement reaction to render the template chemically compatible with the barium titanate-based coating. Conformal titanate

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

    DOEpatents

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

    2000-01-01

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

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

    DOEpatents

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

    2002-11-26

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

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

    DOEpatents

    Congdon, James W.

    2009-03-17

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

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

    EPA Science Inventory

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

  19. Photolithography fabrication of sol-gel ridge waveguides

    NASA Astrophysics Data System (ADS)

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

    1998-07-01

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

  20. Inorganic Sensing Using Organofunctional Sol-Gel Materials

    PubMed Central

    Carrington, Nathan A.; Xue, Zi-Ling

    2007-01-01

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

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

    PubMed

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

    2013-07-28

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

  2. Sol-gel chemistry by ring-opening polymerization

    SciTech Connect

    RAHIMIAN,KAMYAR; LOY,DOUGLAS A.

    2000-02-07

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

  3. On sol-gel derived Au-enriched TiO2 and TiO2-ZrO2 photocatalysts and their investigation in photocatalytic reduction of carbon dioxide

    NASA Astrophysics Data System (ADS)

    Matějová, Lenka; Kočí, Kamila; Reli, Martin; Čapek, Libor; Matějka, Vlastimil; Šolcová, Olga; Obalová, Lucie

    2013-11-01

    Gold-enriched TiO2 and TiO2-ZrO2 and their parent counterparts were prepared by using the sol-gel process controlled within the reverse micelles environment, followed by impregnation in AuCl3 solution. Catalysts were characterized by organic elementary analysis (OEA), inductively coupled plasma mass spectrometry (ICP MS), N2 physisorption, powder X-ray diffraction (XRD), transmission electron microscopy (TEM) combined with electron diffraction, UV-vis spectroscopy, and tested in CO2 photocatalytic reduction. The performance of photocatalysts iluminated by UV-lamp with the wavelenght maximum at 254 nm was decreasing in the order TiO2-ZrO2 > Au/TiO2-ZrO2 > TiO2 > Au/TiO2 > TiO2 Evonic P25. The photocatalytic performance decrease over Au/TiO2-ZrO2 and Au/TiO2, compared to their parent counterparts, can be explained by the presence of too large Au particles, which block the oxide surface and either reduce the light absorption capability of the catalysts, or serve as the recombination centres. Higher photocatalytic performance of the amorphous TiO2-ZrO2 than of the nanocrystalline TiO2 can be ascribed to the enlarged surface area and higher photoactivity of titania-zirconia oxide mixture under the UV lamp with the wavelenght maximum at 254 nm. With regard to crystalline materials the appropriate anatase crystallite-size plays a key role in performance of CO2 photocatalytic reduction. Moreover, correlation between the adsorption edge and the anatase crystallite-size was revealed.

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

    SciTech Connect

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

    1990-01-01

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

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

    PubMed

    Shankhwar, Nisha; Srinivasan, A

    2016-05-01

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

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

    PubMed

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

    2004-04-07

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

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

    NASA Astrophysics Data System (ADS)

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

    1994-10-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2001-01-01

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

  9. Nanostructured Energetci Matreials with sol-gel Chemistry

    SciTech Connect

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

    2003-11-18

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

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

    SciTech Connect

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

    2013-11-27

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

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

    PubMed

    Della Gaspera, Enrico; Martucci, Alessandro

    2015-07-13

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

  12. Sol-Gel Thin Films for Plasmonic Gas Sensors

    PubMed Central

    Della Gaspera, Enrico; Martucci, Alessandro

    2015-01-01

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

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

    SciTech Connect

    Hurd, A.J.

    1995-03-01

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

  14. Sol-Gel Processing of Neodymia-Silica Glass

    NASA Astrophysics Data System (ADS)

    Pope, Edward John Andrew

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

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

    NASA Technical Reports Server (NTRS)

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

    2000-01-01

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

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

    PubMed

    Kaneko, Tsukasa; Iwata, Kazuki; Kobayashi, Makiko

    2015-09-01

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

  17. Development of polymeric materials for sol-gel waveguides

    NASA Astrophysics Data System (ADS)

    Kusevic, Maja; Hiltunen, Marianne

    2002-06-01

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

  18. Evolution of microstructure in mixed niobia-hybrid silica thin films from sol-gel precursors.

    PubMed

    Besselink, Rogier; Stawski, Tomasz M; Castricum, Hessel L; ten Elshof, Johan E

    2013-08-15

    The evolution of structure in sol-gel derived mixed bridged silsesquioxane-niobium alkoxide sols and drying thin films was monitored in situ by small-angle X-ray scattering. Since sol-gel condensation of metal alkoxides proceeds much faster than that of silicon alkoxides, the incorporation of d-block metal dopants into silica typically leads to formation of densely packed nano-sized metal oxide clusters that we refer as metal oxide building blocks in a silica-based matrix. SAXS was used to study the process of niobia building block formation while drying the sol as a thin film at 40-80°C. The SAXS curves of mixed niobia-hybrid silica sols were dominated by the electron density contrast between sol particles and surrounding solvent. As the solvent evaporated and the sol particles approached each other, a correlation peak emerged. Since TEM microscopy revealed the absence of mesopores, the correlation peak was caused by a heterogeneous system of electron-rich regions and electron poor regions. The regions were assigned to small clusters that are rich in niobium and which are dispersed in a matrix that mainly consisted of hybrid silica. The correlation peak was associated with the typical distances between the electron dense clusters and corresponded with distances in real space of 1-3 nm. A relationship between the prehydrolysis time of the silica precursor and the size of the niobia building blocks was observed. When 1,2-bis(triethoxysilyl)ethane was first hydrolyzed for 30 min before adding niobium penta-ethoxide, the niobia building blocks reached a radius of 0.4 nm. Simultaneous hydrolysis of the two precursors resulted in somewhat larger average building block radii of 0.5-0.6 nm. This study shows that acid-catalyzed sol-gel polymerization of mixed hybrid silica niobium alkoxides can be rationalized and optimized by monitoring the structural evolution using time-resolved SAXS.

  19. Structural and optoelectronic characterization of TiO2 films prepared using the sol gel technique

    NASA Astrophysics Data System (ADS)

    Jiménez González, A. E.; Gelover Santiago, S.

    2007-07-01

    TiO2 is a versatile material that makes for fascinating study in any of its several physical forms: monocrystal, polycrystal, powder or thin film. Its enhanced photosensitivity to UV radiation and excellent chemical stability in acidic and aqueous media point to its excellent potential for use in a variety of applications, such as solar cells, electronic devices, chemical sensors and photocatalysts. Of late, thin films of TiO2 have permitted the study of physical and chemical properties that are almost impossible to examine in powders. Using the sol-gel technique, it was possible to prepare TiO2 films, and to specifically modify their characteristic properties by means of annealing treatments. Optical measurements carried out on sol-gel derived films produced results similar to those found in films prepared using the sputtering technique. The use of TiO2 films facilitates the study of the behaviour of crystalline structure, grain size, photoresponse, electrical conductivity in both darkness and light and energy band gap (Eg) as a function of treatment temperature. For the first time, it has been demonstrated that the photoconductivity of TiO2 becomes apparent at a treatment temperature of 350 °C, which means that below this temperature the material is not photosensitive. The photosensitivity (S) of TiO2 films prepared by the sol-gel technique reaches values between 100 and 104, surpassing by more than two orders of magnitude the photosensitivity of TiO2 in powder form. In addition, it was possible to study the surface crystalline structure, where TEM studies clearly revealed both the polycrystalline order and the atomic arrangements of the TiO2 films. Our findings will afford us an opportunity to better study the nature of TiO2 and to enhance its performance with respect to the above-mentioned applications.

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

    PubMed

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

    2013-06-15

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

  1. Synthesis of phthalocyanine doped sol-gel materials

    NASA Technical Reports Server (NTRS)

    Dunn, Bruce

    1993-01-01

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

  2. Mediator-free phenol sensor based on titania sol-gel encapsulation matrix for immobilization of tyrosinase by a vapor deposition method.

    PubMed

    Yu, Jiuhong; Liu, Songqin; Ju, Huangxian

    2003-12-30

    A novel amperometric phenol sensor was constructed by immobilizing tyrosinase in a titania sol-gel matrix. The tyrosinase entrapped sol-gel film was obtained with a vapor deposition method, which simplified the traditional sol-gel process and avoided the shrinkage and cracking of conventional sol-gel-derived glasses. This matrix provided a microenvironment for retaining the native structure and activity of the entrapped enzyme and a very low mass transport barrier to the enzyme substrates. Phenol could be oxidized by dissolving oxygen in presence of immobilized tyrosinase to form a detectable product, which was determined at -150 mV without any mediator. The phenol sensor exhibited a fast response (less than 5 s) and sensitivity as high as 103 microA/mM, which resulted from the porous structure and high enzyme loading of the sol-gel matrix. The linear range for phenol determination was from 1.2x10(-7) to 2.6x10(-4) M with a detection limit of 1.0x10(-7) M. The apparent Michaelis-Menten constant of the encapsulated tyrosinase was calculated to be (0.29+/-0.02) mM. The stability of the biosensor was also evaluated.

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

    PubMed

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

    2014-07-01

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

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

    NASA Astrophysics Data System (ADS)

    McLean, Michael M.

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

  5. Effect of ethanol variation on the internal environment of sol-gel bulk and thin films with aging.

    PubMed

    Gupta, R; Mozumdar, S; Chaudhury, N K

    2005-10-15

    Sol-gel derived bulk and thin films were prepared from different compositions at low pH ( approximately 2.0) containing varying concentrations of ethanol from 15 to 60% at constant water (H(2)O)/tetraethyl-orthosilicate (TEOS) ratio (R=4). The fluorescence microscopic and spectroscopic measurements on fluorescent probe, Hoechst 33258 (H258) entrapped in these compositions were carried out at different days of storage to monitor the effects of concentration of ethanol on the internal environment of sol-gel materials. Fluorescence microscopic observations on sol-gel thin films, prepared by dip coating technique depicted uniform and cracked surface at withdrawal speed 1cm/min (high speed) and 0.1cm/min (low speed) respectively, which did not change during aging. Fluorescence spectral measurements showed emission maximum of H258 at approximately 535 nm in fresh sols at all concentrations of ethanol which depicted slight blue shift to 512 nm during aging in bulk. No such spectral shift has been observed in sol-gel thin films coated at high speed whereas thin films coated at low speed clearly showed an additional band at approximately 404 nm at 45 and 60% concentration of ethanol after about one month of storage. Analysis of the fluorescence lifetime data indicated single exponential decay (1.6-1.8 ns) in fresh sol and from third day onwards, invariably double exponential decay with a short (tau(1)) and a long (tau(2)) component were observed in sol-gel bulk with a dominant tau(1) at approximately 1.2 ns at all concentrations of ethanol. A double exponential decay consisting of a short component (tau(1)) at approximately 0.2 ns and a long component (tau(2)) at approximately 3.5 ns were observed at all ethanol concentrations in both fresh and aged sol-gel thin films. Further, distribution analysis of lifetimes of H258 showed two mean lifetimes with increased width in aged bulk and thin films. These results are likely to have strong implications in designing the internal

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

    DTIC Science & Technology

    2001-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1997-08-01

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

  8. Durable hydrophobic sol-gel finishing for textiles

    NASA Astrophysics Data System (ADS)

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

    2015-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

  11. Ceria nanoparticles vis-à-vis cerium nitrate as corrosion inhibitors for silica-alumina hybrid sol-gel coating

    NASA Astrophysics Data System (ADS)

    Lakshmi, R. V.; Aruna, S. T.; Sampath, S.

    2017-01-01

    The present work provides a comparative study on the corrosion protection efficiency of defect free sol-gel hybrid coating containing ceria nanoparticles and cerium nitrate ions as corrosion inhibitors. Less explored organically modified alumina-silica hybrid sol-gel coatings are synthesized from 3-glycidoxypropyltrimethoxysilane and aluminium-tri-sec-butoxide. The microemulsion derived nanoparticles and the hybrid coatings are characterized and compared with coatings containing cerium nitrate. Corrosion inhibiting capability is assessed using electrochemical impedance spectroscopy. Scanning Kelvin probe measurements are also conducted on the coatings for identifying the apparent corrosion prone regions. Detailed X-ray photoelectron spectroscopy (XPS) analysis is carried out to comprehend the bonding and corrosion protection rendered by the hybrid coatings.

  12. Magnetic nanosized rare earth iron garnets R3Fe5O12: Sol-gel fabrication, characterization and reinspection

    NASA Astrophysics Data System (ADS)

    Opuchovic, Olga; Kareiva, Aivaras; Mazeika, Kestutis; Baltrunas, Dalis

    2017-01-01

    The magnetic nanosized rare earth iron garnets (R3Fe5O12, where R=Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) were prepared by an aqueous sol-gel method. Herein we present, that all these garnets can be obtained by this effective synthesis method simply by changing the temperature of the final annealing. It was also demonstrated, that a different annealing temperature leads to a different particle size distribution of the final product. The SEM analysis results revealed that the smallest particles were formed in the range of 75-130 nm. The phase purity and structure of the rare earth iron garnets were estimated using XRD analysis and Mössbauer spectroscopy. Magnetic properties were determined by magnetization measurements. The relation between the particle size, composition and magnetic properties of the sol-gel derived garnets were also discussed in this study.

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

    NASA Astrophysics Data System (ADS)

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

    2017-01-01

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

  14. Excimer UV-assisted rapid thermal annealing of PbLa(Zr ,Ti)O3 thin films by a sol-gel deposition method

    NASA Astrophysics Data System (ADS)

    Shannigrahi, S. R.; Lim, X.; Tay, F. E. H.

    2007-01-01

    Excimer UV-assisted rapid thermal annealing (UV-RTA) process has been employed to fabricate sol-gel derived ferroelectric Pb0.97La0.03(Zr0.53Ti0.47)O3 (PLZT) thin films on Pt /Ti/SiO2/Si substrates. X-ray diffraction analysis showed that the single phase PLZT thin film can be achieved at a relatively low processing temperature of 580°C. The films appeared to have improved dielectric properties with dielectric constant (ɛ) and loss (tanδ) values of 3300 and 0.03 at 1kHz, respectively. Comparatively good remnant polarization (Pr) value of 36μCcm-2 and coercive field (Ec) value of 60kVcm-1 along with a good fatigue resistance up to 1010 switching cycles have been observed. This method of fabrication of the Pb-based material with the aid of UV-RTA at a comparatively lower temperature opens the door for their better employability in the Si integrated circuit technology.

  15. Sol gel-fluorination synthesis of amorphous magnesium fluoride

    NASA Astrophysics Data System (ADS)

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

    2006-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

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

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

    NASA Astrophysics Data System (ADS)

    Hales, Matthew; Martens, Wayde; Steinberg, Theodore

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

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

    SciTech Connect

    McClure, Zachary D.; Padilla Cintron, Cristina

    2016-09-27

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

  20. Sol-gel applications for ceramic membrane preparation

    NASA Astrophysics Data System (ADS)

    Erdem, I.

    2017-02-01

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

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

    NASA Astrophysics Data System (ADS)

    Schmidt, Helmut K.; Mennig, Martin

    2000-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

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

  3. Nanostructured Energetic Materials with Sol-Gel Methods

    SciTech Connect

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

    2003-11-25

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

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

    PubMed

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

    2002-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-11-01

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

  6. Functionalized silicate sol-gel-supported TiO2-Au core-shell nanomaterials and their photoelectrocatalytic activity.

    PubMed

    Pandikumar, Alagarsamy; Murugesan, Sepperumal; Ramaraj, Ramasamy

    2010-07-01

    The N-[3-(trimethoxysilyl)propyl]ethylenediamine (EDAS) derived silicate matrix supported core-shell TiO(2)-Au nanoparticles (EDAS/(TiO(2)-Au)(nps)) were prepared by NaBH(4) reduction of HAuCl(4) precursor on preformed TiO(2) nanoparticles in the presence of EDAS monomer. The core-shell (TiO(2)-Au)(nps) nanoparticles were stabilized by the amine functional group of the EDAS silicate sol-gel network. The potential application of this EDAS/(TiO(2)-Au)(nps) modified electrode toward the photoelectrochemical oxidation of methanol was explored. The EDAS/(TiO(2)-Au)(nps) modified electrode showed a 12-fold enhancement in the catalytic activity toward photoelectrooxidation of methanol when compared to TiO(2) dispersed in EDAS silicate sol-gel matrix. This improved photoelectrochemical performance is explained on the basis of beneficial promotion of interfacial charge transfer processes of the EDAS/(TiO(2)-Au)(nps) nanocomposite. A methanol oxidation peak current density of 12.3 mA cm(-2) was achieved at an optimum loading of Au(nps) on TiO(2) particles. This novel amine functionalized EDAS silicate sol-gel stabilized core-shell (TiO(2)-Au)(nps) nanomaterial could be an excellent candidate for the photocatalytic and photoelectrochemical applications.

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

    PubMed

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

    2010-10-01

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

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

    PubMed

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

    2014-08-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1997-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2010-01-01

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

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

    DOEpatents

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

    2006-06-06

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

  12. Manufacture of Regularly Shaped Sol-Gel Pellets

    NASA Technical Reports Server (NTRS)

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

    2006-01-01

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

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

    SciTech Connect

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

    2000-05-09

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

  14. Holographic gratings in hybrid sol-gel films

    NASA Astrophysics Data System (ADS)

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

    2003-08-01

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

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

    NASA Astrophysics Data System (ADS)

    Kucharski, Stanisław; Janik, Ryszard

    2005-09-01

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

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

    SciTech Connect

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

    1992-03-19

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

  17. Sol-Gel Glass Holographic Light-Shaping Diffusers

    NASA Technical Reports Server (NTRS)

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

    2005-01-01

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

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

    PubMed

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

    2014-11-06

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

  19. Spectroscopic study of protoporphyrin IX zinc(II) encapsulated in sol-gel glass.

    PubMed

    Zaitoun, Mohammed A

    2005-06-01

    Previous studies indicated that the organization of native porphyrins and their intentionally designated derivatives in solid substrates is of current interest because of the biological and practical importance of these compounds. In this paper, we report herein for the first time the incorporation of a functionalized diacid, protoporphyrin IX Zn(II) (Zn-pp-IX), successfully in a silica based transparent organic-inorganic hybrid material by choosing proper alkoxy silane containing amino-group via the sol-gel method. The entrapped guest was diagnosed using UV-vis sectrophotometry, emission spectroscopy, and infrared spectrometry; the properties of the encapsulated porphyrin were compared to those of the compound in solution. The results indicate that Zn-pp-IX is well distributed and homogeneously in the glass.

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

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey; Selvaduray, Guna; Leiser, Daniel

    1992-01-01

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

  1. Improving endothelialization on 316L stainless steel through wettability controllable coating by sol-gel technology

    NASA Astrophysics Data System (ADS)

    Wang, Mingqi; Wang, Yao; Chen, Yijie; Gu, Hongchen

    2013-03-01

    Rapid endothelialization by surface coverage is considered as a way to increase blood compatibility of the vascular stent and reduce smooth muscle cell (SMC) mediated restenosis. Coatings on 316L stainless steels with different wettabilities and similar topographies were obtained through sol-gel process by regulating the proportions of tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES). Adhesion and proliferation of vascular endothelial cells (EC) and SMC on these substrates have been evaluated by cell numbers, cell morphology, and expression of cytoskeletal protein. Results showed that EC and SMC responded differently to the coated surfaces. Enhanced endothelialization of bare 316L was found at the moderately hydrophilic coating (contact angle 45.3°) which exhibited effective inhibition of SMC and negligible influence on EC. These results are expected to lay foundation for the solution of the vascular restenosis which was mainly derived from the hyperplasia of SMC.

  2. Photophysics and nonlinear optics based on dye-doped sol- gel silica

    NASA Astrophysics Data System (ADS)

    Lam, Sio Kuan

    1998-11-01

    This thesis reports our recent study on the laser and nonlinear optical properties of organic dye-doped sol-gel silica. Eosin Y and Erythrosin B were successfully incorporated in sol gel derived silica. Time resolved spectroscopic study was performed to investigate the dynamics of triplet state of dye molecules in silica gel matrix. Room temperature phosphorescence and delayed fluorescence were observed for both eosin Y and erythrosin B trapped in sol-gel silica. The quantum yields of fluorescence, phosphorescence and delayed fluorescence were measured in vacuum at room temperature and low temperature (at 97°K) respectively. Delayed fluorescence was not observed at low temperature. Quenching of phosphorescence of dye-doped silica gel by oxygen was observed and discussed in term of Stern-Volmer model. The quenching constant was determined as 0.0125 mbar-1 and 0.013 mbar-1 for eosin and erythrosin respectively. Study on nonlinear optical behaviors of dyes in silica gel was also performed. Absorption saturation was observed for eosin Y and the saturation intensity was found to be 1.05 W/cm2. The third order susceptibility X(3) was determined to be 3.1 × 10-3 esu. Optical phase conjugation was demonstrated in eosin Y doped dry silica gel by degenerate four wave mixing. The highest steady state reflectivity of OPC obtained was about 1.15 × 10-4. The intensity dependence of the OPC reflectivity was discussed with Abrams-Lind model. The transient behavior of OPC reflectivity was discussed using the Silberberg model. Aberration correction of the beam image was also demonstrated with DFWM on eosin Y doped silica gel. For silica gel doped with laser dyes, narrow linewidth laser action was achieved. Using a double grating resonator cavity, one grating serving as the beam expander and the other for tuning, laser output linewidth as narrow as 3.3 GHz was realized. The output wavelengths were 560 nm, 474 nm and 378 nm for R6G, Courmarin 460 and Exalite 377 respectively

  3. Acrylate-silica polymer nanocomposites obtained by sol-gel reactions. Structure, properties and scaffold preparation

    NASA Astrophysics Data System (ADS)

    Rodriguez Hernandez, Jose Carlos

    The manuscript deals with the development and characterization of hybrid materials based on poly(hydroxyethyl acrylate) (hereafter PHEA) reinforced by the inclusion of an amorphous silica phase. Both phases were simultaneously synthesized: the organic phase underwent a free radical polymerization reaction induced by the small addition of a thermal initiator (benzoyl peroxide); besides, silica (SiO2) was polymerized by an acid catalyzed sol-gel reaction of the silicon alkoxide tetraethoxysilane (hereafter TEOS). The sol-gel reaction conditions where silicon dioxide is formed influence the final silica structure: degree of condensation, linear versus branched intermediate species, average size, and so on. Some of the key parameters to control SiO2 topology on sol-gel derived composites include the catalyst nature used to increase the alkoxide reactivity (as well as its amount, pH), the available water to hydrolyze the silica precursor (referred to the stoichiometric amount needed to fully hydrolyze one molecule of TEOS) and ratio between the organic and inorganic phases on the final hybrid. The former (catalyst) and the second (water) conditions were fixed so as to synthesize materials with silica average sizes around tens of nanometres (nanocomposites); the latter, the relative ratio between organic and inorganic phases, was systematically changed. Besides, it is introduced a methodology to prepare a new kind of scaffolds made by nanocomposites whose pore morphology consists of a cylindrical channel mesh, which are perpendicular between themselves. The procedure is based on the well-known method of intermediate templates, this time prepared by a stack of woven fabrics which are first pressed and afterwards sintered. After the filling of the holes left inside the template by the monomeric solution and subsequent thermal polymerization, templates are removed by the selective solvent of the material it is made up. A suitable template preparation is found to be crucial

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

    NASA Astrophysics Data System (ADS)

    Barhoum, Moussa

    fabricated optical materials. Finally, magnetic functionalization studies of sol-gel derived Co-ion doped titania thin films using superconducting quantum interference device (SQUID) magnetometry and an attempt to measure their magneto-optical properties using a home-built Faraday rotation setup are discussed. The experimental limitations in reliably measuring magnetization responses of these thin films are introduced and discussed in detail. The summary and outlook chapters summarize the scientific significance of each research project and briefly introduce ongoing research based on the work and the results presented in this dissertation.

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

    PubMed

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

    2009-07-17

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

  6. Domain walls and ferroelectric reversal in corundum derivatives

    NASA Astrophysics Data System (ADS)

    Ye, Meng; Vanderbilt, David

    2017-01-01

    Domain walls are the topological defects that mediate polarization reversal in ferroelectrics, and they may exhibit quite different geometric and electronic structures compared to the bulk. Therefore, a detailed atomic-scale understanding of the static and dynamic properties of domain walls is of pressing interest. In this work, we use first-principles methods to study the structures of 180∘ domain walls, both in their relaxed state and along the ferroelectric reversal pathway, in ferroelectrics belonging to the family of corundum derivatives. Our calculations predict their orientation, formation energy, and migration energy and also identify important couplings between polarization, magnetization, and chirality at the domain walls. Finally, we point out a strong empirical correlation between the height of the domain-wall-mediated polarization reversal barrier and the local bonding environment of the mobile A cations as measured by bond-valence sums. Our results thus provide both theoretical and empirical guidance for future searches for ferroelectric candidates in materials of the corundum derivative family.

  7. Glucose biosensor based on covalent immobilization of enzyme in sol-gel composite film combined with Prussian blue/carbon nanotubes hybrid.

    PubMed

    Fu, Guanglei; Yue, Xiuli; Dai, Zhifei

    2011-05-15

    A novel electrochemical glucose biosensor was developed based on in situ covalent immobilization of glucose oxidase (GOx) by one-pot chitosan (CS)-incorporated sol-gel process in the presence of Prussian blue deposited multi-walled carbon nanotubes hybrids (PB/MWNTs) using 3-isocyanatopropyltriethoxysilane (ICPTES) as both a sol-gel precursor and a covalent coupling agent for GOx and CS. The electrode modified with the PB/MWNTs-GOx-CS-ICPTES sol-gel composite film showed good electrical conductivity and effective low-potential electron transfer mediation toward H2O2 reduction attributed to the incorporation of PB/MWNTs. The biosensor exhibited a linear response to glucose in the concentration range from 2.5×10(-5) to 1.3×10(-3) M with a correlation coefficient of 0.9998, a detection limit of 7.5×10(-6) M, a low response time (10s ), good sensitivity and high anti-interference ability. Compared with the control biosensor based on the traditional tetraethoxysilane derived sol-gel composite film, the biosensor showed a similarly small apparent Michaelis-Menten constant of 3.67 mM but much higher electrochemical and biosensing stability.

  8. Progress in the fabrication of optical fibers by the sol-gel-based granulated silica method

    NASA Astrophysics Data System (ADS)

    Pilz, S.; Najafi, H.; El Sayed, A.; Boas, J.; Kummer, D.; Scheuner, J.; Etissa, D.; Ryser, M.; Raisin, P.; Berger, S.; Romano, V.

    2016-04-01

    Novel special optical fibers nowadays can take advantage of several new preform production techniques. During the last years we have devoted our attention to the granulated silica method. It is one of the variants of the powder-in-tube technique and potentially offers a high degree of freedom regarding the usable dopants, the maximum possible dopant concentration, the homogeneity of the dopants, the geometry and minimal refractive index contrast. We developed and refined an approach for the production of doped granulated silica material based on the sol-gel process. Here, we present material analysis results of an ytterbium (Yb) doped, aluminum (Al) and phosphorous (P) co-doped glass on the basis of our sol-gel glass based granulated silica method as well as first measurements of two LMA fibers obtained from this material. For the material analysis we used advanced analysis techniques, such as HAADF-STEM and STEM-EDX spectroscopy to determine the composition of the material and the distribution of the dopants and the codopants. The chemical mapping of the STEM-EDX shows an extremely homogeneous distribution of the dopants and co-dopants in nano-scale. Based on self-made LMA fibers, we measured the refractive index contrast of the sol-gelbased granulated silica derived core compared to the pure silica cladding. In addition we quantified optical characteristics such as the emission and absorption spectrum. The measured upper state lifetime of the optical active dopant ytterbium was 0.99ms, which in turn confirms the homogeneous distribution of the Yb atoms. The propagation losses were determined to be 0.2dB/m at 633nm and 0.02414dB/m at1550nm.

  9. Microwave sintering of sol-gel derived abrasive grain

    DOEpatents

    Plovnick, Ross; Celikkaya, Ahmet; Blake, Rodger D.

    1997-01-01

    A method is provided for making microwave-sintered, free flowing alpha alumina-based ceramic abrasive grain, under conditions effective to couple microwaves with calcined alpha alumina-based abrasive gain precursor and sinter it at a temperature of at least about 1150.degree. C.

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

    PubMed

    Hayes, J D; Malik, A

    1997-07-18

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

    Lead-free barium zirconate-titanate/barium calcium-titanate, [(BaZr0.2Ti0.80)O3]1-x-[(Ba0.70Ca0.30)TiO3]x (x = 0.10, 0.15, 0.20) (BZT-BCT) ceramics with high dielectric constant, low dielectric loss and moderate electric breakdown field were prepared by the sol-gel synthesis technique. X-ray diffraction patterns revealed tetragonal crystal structure and this was further confirmed by Raman spectra. Well-behaved ferroelectric hysteresis loops and moderate polarizations (spontaneous polarization, Ps ~ 3-6 µC cm-2) were obtained in these BZT-BCT ceramics. Frequency-dependent dielectric spectra confirmed that ferroelectric diffuse phase transition (DPT) exists near room temperature. Scanning electron microscope images revealed monolithic grain growth in samples sintered at 1280 °C. 1000/ɛ versus (T) plots revealed ferroelectric DPT behaviour with estimated γ values of ~1.52, 1.51 and 1.88, respectively, for the studied BZT-BCT compositions. All three compositions showed packing-limited breakdown fields of ~47-73 kV cm-1 with an energy density of 0.05-0.6 J cm-3 for thick ceramics (>1 mm). Therefore these compositions might be useful in Y5V-type capacitor applications.

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

    PubMed

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

    2017-03-01

    Synthesis of tetragonal ZrO2 by both conventional sol-gel and ultrasound-assisted sol-gel methods and using a non-ionic surfactant Tween-20, was performed. A porous microstructure composed of nanometric particles was observed. Tetragonal ZrO2 was obtained using a low heat treatment temperature of powders, 500°C by both methods. A higher crystallinity and a shorter reaction time were observed when ultrasound was used in the sol-gel method due to the cavitation phenomenon.

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

    NASA Astrophysics Data System (ADS)

    Mikalsen, Erik Arthur

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

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

    NASA Astrophysics Data System (ADS)

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

    2006-02-01

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

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

    SciTech Connect

    RAHIMIAN,KAMYAR; LOY,DOUGLAS A.

    2000-05-01

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

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

    PubMed

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

    2003-01-01

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

  17. /dopamine films prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  18. Sol-gel template synthesis of semiconductor nanostructures

    SciTech Connect

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

    1997-03-01

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

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

    PubMed

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

    2005-03-02

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1989-12-01

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

  3. Thin Film Deposition Using SOL-GEL Technology

    NASA Astrophysics Data System (ADS)

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

    1983-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2007-12-01

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

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

    SciTech Connect

    Li, Binghui; Gonzalez, R.D.

    1996-10-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1987-01-01

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

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

    PubMed

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

    2013-05-14

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

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

    DOEpatents

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

    2000-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2002-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-01-01

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

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

    PubMed

    Morosanova, Elena I

    2012-12-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2001-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2003-01-01

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

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

    PubMed

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

    2011-02-21

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

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

    NASA Technical Reports Server (NTRS)

    Bansal, Narottam P.

    1989-01-01

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

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

    PubMed

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

    2013-03-01

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

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

    PubMed

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

    2011-06-01

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

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

    PubMed

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

    2016-03-04

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

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

    PubMed

    Allhusen, John S; Conboy, John C

    2013-11-27

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1997-10-01

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

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

    NASA Astrophysics Data System (ADS)

    Thoř, Tomáš; Václavík, Jan

    2016-11-01

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

  4. Study of the structure and interface of NiTi SMA/FC composite films prepared by the sol-gel method

    SciTech Connect

    Liu, Q.S. Liu, Y.F.; Ma, X.; Han, X.

    2008-02-15

    Ferroelectric ceramic (FC) films were prepared on a NiTi shape memory alloy (NiTi SMA) substrate by the sol-gel method. The effect of the heat treatment temperature on the crystallization of both the NiTi SMA and ferroelectric ceramic is discussed. The heterostructure of the interface was characterized by scanning electron microscopy and X-ray diffraction. The results indicate that aging reactions in the NiTi SMA substrate were restricted by the presence of the ceramic film. Also, the transitional TiO{sub 2} layer produced in-situ by the oxidation of the surface of the NiTi SMA substrate improves the adhesion between the ceramic film and NiTi SMA.

  5. Temperature-dependent electrical, elastic and magnetic properties of sol-gel synthesized Bi0.9Ln0.1FeO3 (Ln = Nd, Sm)

    NASA Astrophysics Data System (ADS)

    Schiemer, J.; Withers, R. L.; Carpenter, M. A.; Liu, Y.; Wang, J. L.; Norén, L.; Li, Q.; Hutchison, W.

    2012-03-01

    This report details correlated electrical, mechanical and magnetic behaviour in BiFeO3 ceramics doped with 10% Ln (Ln = Sm, Nd) ions on the Bi, or perovskite A, site and synthesized by a sol-gel method. The ceramics exhibit bulk piezoelectric and ferroelectric properties and clear ferroelectric domain patterns through piezoresponse force microscopy. Resonant ultrasound spectroscopy, dielectric spectroscopy and magnetometry studies show correlated magnetoelectromechanical behaviour and the existence of weak ferromagnetism for both compositions. An anomaly with simultaneous mechanical and magnetic signatures is discovered in both materials near room temperature, while previously reported transitions and anomalies are found to exhibit electro- and/or magnetomechanical coupling. Magnetism is significantly enhanced in the Sm doped sample, which is a promising multiferroic material.

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

    PubMed

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

    2012-11-01

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

  7. Ferroelectric nanofibers with an embedded optically nonlinear benzothiazole derivative

    NASA Astrophysics Data System (ADS)

    Baptista, Rosa M. F.; Isakov, Dmitry; Raposo, M. Manuela M.; Belsley, Michael; Bdikin, Igor; Kholkin, Andrei L.; Costa, Susana P. G.; de Matos Gomes, Etelvina

    2014-07-01

    We report measurements of the molecular first hyperpolarizability, thermal stability, photophysical, piezoelectric, and ferroelectric properties of a benzothiazole derivative bearing an arylthiophene π-conjugated bridge both in solution and when embedded into a poly ( l-lactic acid) matrix in the form of electrospun fibers with an average diameter of roughly 500 nm. The embedded nanocrystalline phenylthienyl-benzothiazole with crystal sizes of about 1.4 nm resulted in a good piezoelectric response from these functionalized electrospun fibers, indicative of a polar crystalline structure.

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

    DTIC Science & Technology

    2006-05-31

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

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

    PubMed

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

    2016-08-01

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

  10. Structural, optical and electrical properties of delafossite CuGaO2 films grown by sol-gel method

    NASA Astrophysics Data System (ADS)

    Han, M. J.; Huang, T.; Zhang, J. Z.; Li, Y. W.; Hu, Z. G.

    2013-12-01

    Transparent p-type conductive CuGaO2 films have been fabricated on sapphire substrates by sol-gel method. The stable sol solution for CuGaO2 were formed by copper(II) acetate monohydrate and gallium(III) nitrate hydrate, and the c-axis orientation of CuGaO2 films were strengthened with increasing annealing temperature. The pure phase CuGaO2 film was obtained at 900°C for 30 min in N2 atmosphere, and its microstructure, compositions, optical and electrical properties were analyzed. It was found that the sol-gel derived CuGaO2 films show a high optical transparency (60-80%) in the visible region, the direct and indirect band gaps were approximately 3.56 and 3.24 eV, respectively. It shows a crossover from the thermal activation behavior to that of three-dimensional variable range hopping from the temperature-dependent electrical conductivity at about 160 K.

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

    NASA Astrophysics Data System (ADS)

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

    2008-04-01

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

  12. Diamond nanoparticles as a way to improve electron transfer in sol-gel L-lactate biosensing platforms.

    PubMed

    Briones, M; Casero, E; Vázquez, L; Pariente, F; Lorenzo, E; Petit-Domínguez, M D

    2016-02-18

    In the present work, we have included for the first time diamond nanoparticles (DNPs) in a sol-gel matrix derived from (3-mercaptopropyl)-trimethoxysilane (MPTS) in order to improve electron transfer in a lactate oxidase (LOx) based electrochemical biosensing platform. Firstly, an exhaustive AFM study, including topographical, surface potential (KFM) and capacitance gradient (CG) measurements, of each step involved in the biosensing platform development was performed. The platform is based on gold electrodes (Au) modified with the sol-gel matrix (Au/MPTS) in which diamond nanoparticles (Au/MPTS/DNPs) and lactate oxidase (Au/MPTS/DNPs/LOx) have been included. For the sake of comparison, we have also characterized a gold electrode directly modified with DNPs (Au/DNPs). Secondly, the electrochemical behavior of a redox mediator (hydroxymethyl-ferrocene, HMF) was evaluated at the platforms mentioned above. The response of Au/MPTS/DNPs/LOx towards lactate was obtained. A linear concentration range from 0.053 mM to 1.6 mM, a sensitivity of 2.6 μA mM(-1) and a detection limit of 16 μM were obtained. These analytical properties are comparable to other biosensors, presenting also as advantages that DNPs are inexpensive, environment-friendly and easy-handled nanomaterials. Finally, the developed biosensor was applied for lactate determination in wine samples.

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

    NASA Astrophysics Data System (ADS)

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

    1997-02-01

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

  14. Nonlinear optical absorption and switching properties of gold nanoparticle doped SiO2-TiO2 sol-gel films.

    PubMed

    Venkatram, N; Kumar, R Sai Santosh; Rao, D Narayana; Medda, S K; De, Sucheta; De, Goutam

    2006-07-01

    The nonlinear optical absorption and switching properties of sol-gel derived of Au nanoparticle doped SiO2-TiO2 sol-gel films having different Au-surface plasmon absorption positions are reported in this paper. The Au nanoparticles are embedded in SiO2 and SiO2-TiO2 mixed glassy film matrices with different refractive index values. To study the nonlinear absorption properties, lasers with three different wavelengths are used. The optical switching behavior is studied by using the pump-probe technique with 532 nm as the excitation wavelength. Ground state conduction band, surface plasmon band, and the free carrier band are taken as three level model to explain theoretically the obtained RSA and SA behaviors.

  15. Preparation of new Calix[4]arene-immobilized biopolymers for enhancing catalytic properties of Candida rugosa lipase by sol-gel encapsulation.

    PubMed

    Ozyilmaz, Elif; Sayin, Serkan

    2013-08-01

    The article describes preparation of new calixarene biopolymers consisting of the immobilization of convenience calixarene derivative onto cellulose and chitosan biopolymers, and the encapsulation of these calixarene biopolymers with Candida rugosa lipase within a chemical inert sol-gel supported by polycondensation with tetraethoxysilane and octyltriethoxysilane. The catalytic properties of immobilized lipase were evaluated into model reactions employing the hydrolysis of p-nitrophenylpalmitate and the enantioselective hydrolysis of naproxen methyl esters from racemic prodrugs in aqueous buffer solution/isooctane reaction system. The resolution studies using sol-gel support have observed more improvement in the enantioselectivity of naproxen E = 300 with Cel-Calix-E than with encapsulated lipase without calixarene-based materials. Furthermore, the encapsulated lipase (Cel-Calix-E) was still retained about 39 % of their conversion ratios after the fifth reuse in the enantioselective reaction.

  16. Surface modification of stainless steel orthopedic implants by sol-gel ZrTiO4 and ZrTiO4-PMMA coatings.

    PubMed

    Salahinejad, E; Hadianfard, M J; Macdonald, D D; Sharifi Asl, S; Mozafari, M; Walker, K J; Rad, A Tahmasbi; Madihally, S V; Vashaee, D; Tayebi, L

    2013-08-01

    In this paper, the biocompatibility of a medical-grade stainless steel coated with sol-gel derived, nanostructured inorganic ZrTiO4 and hybrid ZrTiO4-PMMA thin films is correlated with surface characteristics. The surfaces of the samples are characterized by atomic force microscopy, the sessile drop technique, and electrochemical corrosion experiments. The viability of adult human mesenchymal stem cells on the surfaces after one day of culture is also assessed quantitatively and morphologically. According to the results, both of the coatings improve the hydrophilicity, corrosion resistance, and thereby cytocompatibility of the substrate. Despite the higher corrosion protection by the hybrid coating, the sample coated with the inorganic thin film exhibits a better cell response, suggesting the domination of wettability. In summary, the ZrTiO4-based sol-gel films can be considered to improve the biocompatibility of metallic implants.

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

    PubMed

    Jaiswal, Swarna; McHale, Patrick; Duffy, Brendan

    2012-06-01

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

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

    PubMed

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

    2016-01-01

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

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

    PubMed

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

    2009-05-29

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

  20. Poly(methyl methacrylate)-titania hybrid materials by sol-gel processing

    SciTech Connect

    Zhang, J.; Luo, S.; Gui, L.; Tang, Y.

    1996-12-31

    Sol-gel derived Poly(methyl methacrylate)-titania hybrid materials were synthesized by using acrylic acid or allyl acetylacetone (3-allyl-2,4-pentanedione) as coupling agents. Titanium butoxide modified with acrylic acid (or titanium isopropoxide modified with allyl acetylacetone) was hydrolyzed to produce a titania network, and then poly (methyl methacrylate) (PMMA) chains formed in situ through a radical polymerization were chemically bonded to the forming titania network to synthesize a hybrid material. Transparent hybrid materials with different contents of titania were achieved. With the increase of the titania content, the colors of the products changed form yellow to dark red. The synthesis process was investigated step by step by using FTIR spectroscopy, and the experimental results demonstrated that acrylate or acetylacetonato groups bound to titanium remain in the final hybrid materials. The thermal stability of the hybrid materials was considerably improved relative to pure PMMA. Field emission scanning electron microscopy (FE-SEM) analyses showed the hybrid materials are porous and pore diameters vary from 10nm to 100nm. The hybrid materials using allyl acetylacetone as the coupling agent exhibited thermochromic effects that both pure PMMA and titania do not have.

  1. Determination of bisphenol A in wine by sol-gel immunoaffinity chromatography, HPLC and fluorescence detection.

    PubMed

    Brenn-Struckhofova, Z; Cichna-Markl, M

    2006-11-01

    The paper presents a highly selective analytical method for the determination of traces of bisphenol A (BPA) in wine and the results of a survey 59 wine samples sourced from vats (steel, wood and plastic), glass bottles and Tetra briks. The procedure consists of sample clean-up by sol-gel immunoaffinity chromatography followed by determination of BPA by high-performance liquid chromatography and fluorescence detection. The method has a limit of detection (LOD) (S/N = 3) of 0.1 ng ml-1 and a limit of quantitation (LOQ) (S/N = 6) of 0.2 ng ml-1. In 13 of 59 wine samples, the BPA concentration was below the LOQ. The mean and median for all wine samples with BPA concentrations above the LOQ were 0.58 and 0.40 ng ml-1, respectively. These values - the first set of data on BPA in wine - are far lower than previously published BPA levels derived from migration experiments using wine simulants. Experiments carried out by submerging plastic stoppers in ethanol-water (11 : 89, v/v) up to 11 weeks indicated that detectable amounts of BPA can be leached from some stoppers.

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

    PubMed

    Seyyal, Emre; Malik, Abdul

    2017-04-29

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

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

    PubMed

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

    2015-10-28

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

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

    PubMed

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

    2013-03-13

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

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

    NASA Technical Reports Server (NTRS)

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

    1981-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Lobnik, Aleksandra; Niederreiter, Karlheinz; Uray, Georg

    1999-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2006-06-01

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

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

    NASA Astrophysics Data System (ADS)

    Ciuciumis, Alina; Cernica, Ileana

    2007-05-01

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

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

    SciTech Connect

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

    1996-08-01

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

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

    SciTech Connect

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

    1992-11-03

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

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

    DOEpatents

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

    2016-09-27

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

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

    SciTech Connect

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

    1999-08-09

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

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

    NASA Astrophysics Data System (ADS)

    Wojcik, Anna B.; Klein, Lisa C.

    1993-12-01

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

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

    PubMed

    Babooram, Keshwaree; Narain, Ravin

    2009-01-01

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

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

    NASA Technical Reports Server (NTRS)

    Stiegman, Albert E.

    1995-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-10-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-11-01

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

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

    SciTech Connect

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

    1996-12-31

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

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

    NASA Astrophysics Data System (ADS)

    Kobayashi, Makiko; Matsumoto, Makoto

    2016-07-01

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

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

    NASA Astrophysics Data System (ADS)

    Moreshead, William V.

    1988-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2005-03-01

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

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

    SciTech Connect

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

    2014-10-21

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

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

    EPA Science Inventory

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

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

    NASA Astrophysics Data System (ADS)

    Motalebi, Abolfazl; Nasr-Esfahani, Mojtaba

    2013-06-01

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

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

    PubMed

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

    2014-06-21

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

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

    PubMed Central

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

    2015-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

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

    PubMed

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

    2015-01-01

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

  9. Foldable and Cytocompatible Sol-gel TiO2 Photonics

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1991-01-01

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

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

    PubMed

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

    2013-02-01

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

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

    DOEpatents

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

    2000-01-01

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

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

    PubMed

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

    2016-10-07

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

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

    PubMed

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

    2016-11-17

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

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

    PubMed

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

    2009-05-30

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

  16. Foldable and Cytocompatible Sol-gel TiO2 Photonics.

    PubMed

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

    2015-09-07

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

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

    PubMed Central

    2012-01-01

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

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

    PubMed

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

    2015-10-07

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

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

    PubMed

    Boury, Bruno; Corriu, Robert J P

    2002-04-21

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

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

    NASA Astrophysics Data System (ADS)

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

    2012-06-01

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

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

    PubMed

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

    2013-01-01

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

  2. Foldable and Cytocompatible Sol-gel TiO2 Photonics

    PubMed Central

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

    2015-01-01

    Integrated photonics provides a miniaturized and potentially implantable platform to manipulate and enhance the interactions between light and biological molecules or tissues in in-vitro and in-vivo settings, and is thus being increasingly adopted in a wide cross-section of biomedical applications ranging from disease diagnosis to optogenetic neuromodulation. However, the mechanical rigidity of substrates traditionally used for photonic integration is fundamentally incompatible with soft biological tissues. Cytotoxicity of materials and chemicals used in photonic device processing imposes another constraint towards these biophotonic applications. Here we present thin film TiO2 as a viable material for biocompatible and flexible integrated photonics. Amorphous TiO2 films were deposited using a low temperature (<250 °C) sol-gel process fully compatible with monolithic integration on plastic substrates. High-index-contrast flexible optical waveguides and resonators were fabricated using the sol-gel TiO2 material, and resonator quality factors up to 20,000 were measured. Following a multi-neutral-axis mechanical design, these devices exhibit remarkable mechanical flexibility, and can sustain repeated folding without compromising their optical performance. Finally, we validated the low cytotoxicity of the sol-gel TiO2 devices through in-vitro cell culture tests. These results demonstrate the potential of sol-gel TiO2 as a promising material platform for novel biophotonic devices. PMID:26344823

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

    NASA Astrophysics Data System (ADS)

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

    2007-05-01

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

  4. Selection and elution of aptamers using nanoporous sol-gel arrays with integrated microheaters.

    PubMed

    Park, Seung-Min; Ahn, Ji-Young; Jo, Minjoung; Lee, Dong-Ki; Lis, John T; Craighead, Harold G; Kim, Soyoun

    2009-05-07

    RNA and DNA aptamers that bind to target molecules with high specificity and affinity have been a focus of diagnostics and therapeutic research. These aptamers are obtained by SELEX (Systematic Evolution of Ligands by EXponential enrichment) often requiring more than 10 successive cycles of selection and amplification, where each cycle normally takes 2 days per cycle of SELEX. Here, we have demonstrated the use of sol-gel arrays of proteins in a microfluidic system for efficient selection of RNA aptamers against multiple target molecules. The microfluidic chip incorporates five sol-gel binding droplets, within which specific target proteins are imbedded. The droplets are patterned on top of individually addressable electrical microheaters used for selective elution of aptamers bound to target proteins in the sol-gel droplets. We demonstrate that specific aptamers bind their respective protein targets and can be selectively eluted by micro-heating. Finally, our microfluidic SELEX system greatly improved selection efficiency, reducing the number of selection cycles needed to produce high affinity aptamers. The process is readily scalable to larger arrays of sol-gel-embedded proteins. To our knowledge, this is the first demonstration of a chip-based selection of aptamers using microfluidics, thereby allowing development of a high throughput and efficient SELEX procedures.

  5. Air Vehicle Technology Integration Program (AVTIP). Delivery Order 0004: Advanced Sol-Gel Adhesion Processes

    DTIC Science & Technology

    2002-04-01

    AFRL-ML-WP-TR-2003-4173 AIR VEHICLE TECHNOLOGY INTEGRATION PROGRAM (AVTIP) Delivery Order 0004: Advanced Sol-Gel Adhesion Processes Kay Y...2001 – 03/31/2002 5a. CONTRACT NUMBER F33615-00-D-3052 5b. GRANT NUMBER 4. TITLE AND SUBTITLE AIR VEHICLE TECHNOLOGY INTEGRATION PROGRAM

  6. Nitric Oxide Sensors Obtained Through the Entrapment of Iron Complexes in Sol-Gel Matrix

    DTIC Science & Technology

    2002-04-05

    iron complexes in sol-gel matrix Juliana C. Biazzotto, Jodo F. Borin, Roberto Mendonga Faria’ and Carlos F.O Graeff Departamento de Fisica e...Matemdtica-FFCLRP-USP, Av. Bandeirantes 3900, 14040-901 Ribeirdo Preto, Brazil 1-Instituto de Fisica de S~o Carlos-USP, C.P. 369, 13560-970 Sdo Carlos, Brazil

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

    SciTech Connect

    Shoup, S.S.; Paranthamam, M.; Beach, D.B.; Kroeger, D.M.; Goyal, A.

    2000-06-20

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

  8. Investigation of an automated cleaning system for LMJ coating sol-gel process

    NASA Astrophysics Data System (ADS)

    Lavastre, E.; Fontaine, S.; Bergez, R.; Wender, P.; Cormont, P.; Pellegrini, C.; Beaurain, L.; Belleville, P.

    2008-09-01

    The French Commission for Atomic Energy is currently involved in a project which consists in the construction of a 2MJ/500TW (351nm) laser, so called LMJ (Megajoule-class laser) devoted to Inertial Confinement Fusion (ICF) research in France[1]. For this high power lasers, the sol-gel process[2] has been selected for 95% of laser optical coated area because of room temperature and atmospheric pressure conditions with guarantee for high optical and laser induced damage threshold (LIDT) performances at a low cost compared to conventional vacuum deposition processes. The production rate of sol-gel coatings for the LMJ optical components will require an automated cleaning surface step during sol-gel process. We are investigating a spraying system and wash cycles compatible with the two sol-gel deposition methods: dip and laminar-flow coating. The challenge is to achieve the same cleaned optical surfaces as manual process without using organic solvents. Therefore the main specifications of the cleaning quality are the following ones: a high surface energy over all optical sides (up to 400×400 mm2 area) and no degradation of polished sides (surface defects and LIDT). We present the metrologies carried out and the first results obtained from different wash cycles. These one mainly consist in measurement of contact angles, defects inspections under specific lighting conditions and LIDT tests. Several parameters of wash cycles have been investigated such as washing and rinsing temperatures, water quality, type and concentration of detergents, wettability effects...

  9. A Sol-Gel-Modified Poly(methyl methacrylate) Electrophoresis Microchip with a Hydrophilic Channel Wall

    SciTech Connect

    Chen, Gang; Xu, Xuejiao; Lin, Yuehe; Wang, Joseph

    2007-07-27

    A sol-gel method was employed to fabricate a poly(methyl methacrylate) (PMMA) electrophoresis microchip that contains a hydrophilic channel wall. To fabricate such a device, tetraethoxysilane (TEOS) was injected into the PMMA channel and was allowed to diffuse into the surface layer for 24 h. After removing the excess TEOS, the channel was filled with an acidic solution for 3 h. Subsequently, the channel was flushed with water and was pretreated in an oven to obtain a sol-gel-modified PMMA microchip. The water contact angle for the sol-gel-modified PMMA was 27.4° compared with 66.3° for the pure PMMA. In addition, the electro-osmotic flow increased from 2.13×10-4 cm2 V-1 s-1 for the native-PMMA channel to 4.86×10-4 cm2 V-1 s-1 for the modified one. The analytical performance of the sol-gel-modified PMMA microchip was demonstrated for the electrophoretic separation of several purines, coupled with amperometric detection. The separation efficiency of uric acid increased to 74 882.3 m-1 compared with 14 730.5 m-1 for native-PMMA microchips. The result of this simple modification is a significant improvement in the performance of PMMA for microchip electrophoresis and microfluidic applications.

  10. Planar optical integrated circuits based on UV-patternable sol-gel technology

    NASA Astrophysics Data System (ADS)

    Sabattie, Jean-Marc; MacCraith, Brian D.; Mongey, Karen; Charmet, Jerome; O'Dwyer, Kieran; Pez, Mathias M.; Quentel, Francois; Thierry, Dean

    2003-03-01

    Planar lightwave circuits (PLCs) made from photo-patternable sol-gel materials are attracting considerable R&D interest. This is due to the advantages they offer for applications in optical telecommunications and their compatibility with existing silicon technology process equipment. In particular, the ability to produce devices compatible with silica optical fibres using a straightforward, environmentally friendly, photolithographic process is very attractive. The approach is now well-established in the literature and typically involves the incorporation of an acrylate moiety in the sol-gel precursor mixture, thereby providing a photo-polymerisability function. In this work, we report on the fabrication of passive optical components and devices designed for datacomms applications using visible diode lasers or the 1st telecom window. Silica-based sol-gel waveguides have been integrated in an opto-electronic multichip module (OE-MCM) demonstrator for optical interconnect applications. We have fabricated an 8-channel transmitter module for parallel optical interconnects (POI) based on 2 sub-modules: (a) an optical interface sub-assembly based on photo-patterned sol-gel optical waveguides, and (b) an optoelectronic component sub-module comprising an array of VCSELs. We describe here the fabrication, characterization and performance of the optical components and a POI Transmitter chip.

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

    SciTech Connect

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

    2009-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-03-01

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

  13. Microwave dielectric properties of BNT-BT0.08 thin films prepared by sol-gel technique

    NASA Astrophysics Data System (ADS)

    Huitema, L.; Cernea, M.; Crunteanu, A.; Trupina, L.; Nedelcu, L.; Banciu, M. G.; Ghalem, A.; Rammal, M.; Madrangeas, V.; Passerieux, D.; Dutheil, P.; Dumas-Bouchiat, F.; Marchet, P.; Champeaux, C.

    2016-04-01

    We report for the first time the microwave characterization of 0.92(Bi0.5Na0.5)TiO3-0.08BaTiO3 (BNT-BT0.08) ferroelectric thin films fabricated by the sol-gel method and integrated in both planar and out-of-plane tunable capacitors for agile high-frequency applications and particularly on the WiFi frequency band from 2.4 GHz to 2.49 GHz. The permittivity and loss tangent of the realized BNT-BT0.08 layers have been first measured by a resonant cavity method working at 12.5 GHz. Then, we integrated the ferroelectric material in planar inter-digitated capacitors (IDC) and in out-of-plane metal-insulator-metal (MIM) devices and investigated their specific properties (dielectric tunability and losses) on the whole 100 MHz-15 GHz frequency domain. The 3D finite-elements electromagnetic simulations of the IDC capacitances are fitting very well with their measured responses and confirm the dielectric properties determined with the cavity method. While IDCs are not exhibiting an optimal tunability, the MIM capacitor devices with optimized Ir/MgO(100) bottom electrodes demonstrate a high dielectric tunability, of 30% at 2.45 GHz under applied voltages as low as 10 V, and it is reaching 50% under 20 V voltage bias at the same frequency. These high-frequency properties of the MIM devices integrating the BNT-BT0.08 films, combining a high tunability under low applied voltages indicate a wide integration potential for tunable devices in the microwave domain and particularly at 2.45 GHz, corresponding to the widely used industrial, scientific, and medical frequency band.

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

    PubMed Central

    2011-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-05-01

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

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

    SciTech Connect

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

    1989-01-01

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

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

    SciTech Connect

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

    1989-12-31

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

  18. Large-area sol-gel optical coatings for the Megajoule Laser prototype

    NASA Astrophysics Data System (ADS)

    Pegon, Philippe M.; Germain, Chantal V.; Rorato, Yannick R.; Belleville, Philippe F.; Lavastre, Eric

    2004-02-01

    In the field of thin film coatings, sol-gel (SG) process is an alternative to the conventional Physical Vapor Deposition (PVD) techniques. Sol-gel process is particularly competitive on large-area or fragile substates by taking advantage of various liquid phase deposition techniques performed at room temperature and atmospheric pressure, coupled with the versatility of organo-metallic chemistry. Developed by the French Commission for Atomic Energy (CEA) since 1985 for its former high-power lasers generation, optimized sol-gel coatings proved also very resistant to laser energy. In 1998, THALES Angenieux (TAGX) was selected by CEA to provide all the sol-gel coatings dedicated to the French Laser MegaJoule (LMJ) prototype, named Ligne d'Integration Laser (LIL). In cooperation with Saint-Etienne Pole Optique et Vision (POV), TAGX initiated the building of a sol-gel technological platform (SGPF) aimed at demonstrating the feasibility of production of optical and functional coatings on large area substrates. A technology transfer was performed by CEA (Le Ripault) to TAGX focusing on the manufacture mainly of single-layer antireflective coatings (SLAR), but also of multi-layer AR-coatings and of multi-layered highly reflective (HR)-coatings. Since beginning of 2001 and using SGPF equipments, TAGX successfully coated within specificaitons and schedule most of the 300 optics required for LIL activation. After this 2 years 1/2 production campaign in pre-industrial conditions, we can now analyse the advantages of each deposition technique used, the repeatability of the several processes, and the performance of the various coatings.

  19. Low temperature and UV curable sol-gel coatings for long lasting optical fiber biosensors

    NASA Astrophysics Data System (ADS)

    Otaduy, D.; Villar, A.; Gomez-Herrero, E.; Goitandia, A. M.; Gorritxategi, E.; Quintana, I.

    2010-04-01

    The use of optical fibers as sensing element is increasing in clinical, pharmaceutical and industrial applications. Excellent light delivery, long interaction length, low cost and ability not only to excite the target molecules but also to capture the emitted light from the targets are the hallmarks of optical fiber as biosensors. In biosensors based on fiber optics the interaction with the analyte can occur within an element of the optical fiber. One of the techniques for this kind of biosensors is to remove the fiber optic cladding and substitute it for biological coatings that will interact with the parameter to sensorize. The deposition of these layers can be made by sol-gel technology. The sol-gel technology is being increasingly used mainly due to the high versatility to tailor their optical features. Incorporation of suitable chemical and biochemical sensing agents have allowed determining pH, gases, and biochemical species, among others. Nonetheless, the relatively high processing temperatures and short lifetime values mean severe drawbacks for a successful exploitation of sol-gel based coated optical fibres. With regard to the latter, herein we present the design, preparation and characterization of novel sol-gel coated optical fibres. Low temperature and UV curable coating formulations were optimized to achieve a good adhesion and optical performance. The UV photopolymerizable formulation was comprised by glycidoxypropyltrimethoxysilane (GLYMO), Tetraethylorthosilicate (TEOS) and an initiator. While the thermoset coating was prepared by using 3-aminopropyltrimethoxysilane, GLYMO, and TEOS as main reagents. Both curable sol-gel coated fibres were analysed by FTIR, SEM and optical characterization. Furthermore, in the present work a new technique for silica cladding removal has been developed by ultra-short pulses laser processing, getting good dimensional accuracy and surface integrity.

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

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

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

  1. Ferroelectric properties of PZT/BFO multilayer thin films prepared using the sol-gel method.

    PubMed

    Jo, Seo-Hyeon; Lee, Sung-Gap; Lee, Young-Hie

    2012-01-05

    In this study, Pb(Zr0.52Ti0.48)O3/BiFeO3 [PZT/BFO] multilayer thin films were fabricated using the spin-coating method on a Pt(200 nm)/Ti(10 nm)/SiO2(100 nm)/p-Si(100) substrate alternately using BFO and PZT metal alkoxide solutions. The coating-and-heating procedure was repeated several times to form the multilayer thin films. All PZT/BFO multilayer thin films show a void-free, uniform grain structure without the presence of rosette structures. The relative dielectric constant and dielectric loss of the six-coated PZT/BFO [PZT/BFO-6] thin film were approximately 405 and 0.03%, respectively. As the number of coatings increased, the remanent polarization and coercive field increased. The values for the BFO-6 multilayer thin film were 41.3 C/cm2 and 15.1 MV/cm, respectively. The leakage current density of the BFO-6 multilayer thin film at 5 V was 2.52 × 10-7 A/cm2.

  2. Molecularly Imprinted Sol-Gel-Based QCM Sensor Arrays for the Detection and Recognition of Volatile Aldehydes.

    PubMed

    Liu, Chuanjun; Wyszynski, Bartosz; Yatabe, Rui; Hayashi, Kenshi; Toko, Kiyoshi

    2017-02-16

    The detection and recognition of metabolically derived aldehydes, which have been identified as important products of oxidative stress and biomarkers of cancers; are considered as an effective approach for early cancer detection as well as health status monitoring. Quartz crystal microbalance (QCM) sensor arrays based on molecularly imprinted sol-gel (MISG) materials were developed in this work for highly sensitive detection and highly selective recognition of typical aldehyde vapors including hexanal (HAL); nonanal (NAL) and bezaldehyde (BAL). The MISGs were prepared by a sol-gel procedure using two matrix precursors: tetraethyl orthosilicate (TEOS) and tetrabutoxytitanium (TBOT). Aminopropyltriethoxysilane (APT); diethylaminopropyltrimethoxysilane (EAP) and trimethoxy-phenylsilane (TMP) were added as functional monomers to adjust the imprinting effect of the matrix. Hexanoic acid (HA); nonanoic acid (NA) and benzoic acid (BA) were used as psuedotemplates in view of their analogous structure to the target molecules as well as the strong hydrogen-bonding interaction with the matrix. Totally 13 types of MISGs with different components were prepared and coated on QCM electrodes by spin coating. Their sensing characters towards the three aldehyde vapors with different concentrations were investigated qualitatively. The results demonstrated that the response of individual sensors to each target strongly depended on the matrix precursors; functional monomers and template molecules. An optimization of the 13 MISG materials was carried out based on statistical analysis such as principle component analysis (PCA); multivariate analysis of covariance (MANCOVA) and hierarchical cluster analysis (HCA). The optimized sensor array consisting of five channels showed a high discrimination ability on the aldehyde vapors; which was confirmed by quantitative comparison with a randomly selected array. It was suggested that both the molecularly imprinting (MIP) effect and the matrix

  3. Molecularly Imprinted Sol-Gel-Based QCM Sensor Arrays for the Detection and Recognition of Volatile Aldehydes

    PubMed Central

    Liu, Chuanjun; Wyszynski, Bartosz; Yatabe, Rui; Hayashi, Kenshi; Toko, Kiyoshi

    2017-01-01

    The detection and recognition of metabolically derived aldehydes, which have been identified as important products of oxidative stress and biomarkers of cancers; are considered as an effective approach for early cancer detection as well as health status monitoring. Quartz crystal microbalance (QCM) sensor arrays based on molecularly imprinted sol-gel (MISG) materials were developed in this work for highly sensitive detection and highly selective recognition of typical aldehyde vapors including hexanal (HAL); nonanal (NAL) and bezaldehyde (BAL). The MISGs were prepared by a sol-gel procedure using two matrix precursors: tetraethyl orthosilicate (TEOS) and tetrabutoxytitanium (TBOT). Aminopropyltriethoxysilane (APT); diethylaminopropyltrimethoxysilane (EAP) and trimethoxy-phenylsilane (TMP) were added as functional monomers to adjust the imprinting effect of the matrix. Hexanoic acid (HA); nonanoic acid (NA) and benzoic acid (BA) were used as psuedotemplates in view of their analogous structure to the target molecules as well as the strong hydrogen-bonding interaction with the matrix. Totally 13 types of MISGs with different components were prepared and coated on QCM electrodes by spin coating. Their sensing characters towards the three aldehyde vapors with different concentrations were investigated qualitatively. The results demonstrated that the response of individual sensors to each target strongly depended on the matrix precursors; functional monomers and template molecules. An optimization of the 13 MISG materials was carried out based on statistical analysis such as principle component analysis (PCA); multivariate analysis of covariance (MANCOVA) and hierarchical cluster analysis (HCA). The optimized sensor array consisting of five channels showed a high discrimination ability on the aldehyde vapors; which was confirmed by quantitative comparison with a randomly selected array. It was suggested that both the molecularly imprinting (MIP) effect and the matrix

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

    PubMed

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

    2014-03-01

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

  5. Novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as solid phase extraction sorbent for organophosphorus pesticides.

    PubMed

    Wan Ibrahim, Wan Aini; Veloo, Krishna Veni; Sanagi, Mohd Marsin

    2012-03-16

    A novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was produced and applied as sorbent for solid phase extraction (SPE). Five selected organophosphorus pesticides (OPPs) were employed as model compounds to evaluate the extraction performance of the synthesized sol-gel organic-inorganic hybrid MTMOS-TEOS. Analysis was performed using gas chromatography-mass spectrometry. Several important SPE parameters were optimized. Under the optimum extraction conditions, the method using the sol-gel organic-inorganic hybrid MTMOS-TEOS as SPE sorbent showed good linearity in the range of 0.001-1 μg L(-1), good repeatability (RSD 2.1-3.1%, n=5), low limits of detection at S/N=3 (0.5-0.9 pg mL(-1)) and limit of quantification (1-3 pg mL(-1), S/N=10). The performance of the MTMOS-TEOS SPE was compared to commercial C18 Supelclean SPE since C18 SPE is widely used for OPPs. The MTMOS-TEOS SPE method LOD was 500-600 × lower than the LOD of commercial C18 SPE. The LOD achieved with the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent allowed the detection of these OPPs in drinking water well below the level set by European Union (EU) at 0.1 μg L(-1) of each pesticides. The developed MTMOS-TEOS SPE method was successfully applied to real sample analysis of the selected OPPs from several water samples and its application extended to the analysis of several fruits samples. Excellent recoveries and RSDs of the OPPs were obtained from the various water samples (recoveries: 97-111%, RSDs 0.4-2.8%, n=3) and fruit samples (recoveries: 96-111%), RSDs 1-4%, n=5) using the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent. Recoveries and RSDs of OPPs from river water samples and fruit samples using C18 Supelclean SPE sorbent were 91-97%, RSD 0.9-2.6, n=3 and 86-96%, RSD 3-8%, n=5, respectively). The novel sol-gel hybrid MTMOS-TEOS SPE sorbent demonstrate the potential as an alternative inexpensive extraction sorbent for OPPs with higher sensitivity for

  6. Fiber-optic chemical sensors using sol-gel membranes and photocatalysts

    NASA Astrophysics Data System (ADS)

    Nivens, Delana Amber Gajdosik

    Fiber-optic sensors have been developed that incorporate multi-layer organo-silica sol-gel membranes. Multilayer sol-gel sensors have been designed to offer improved stability over other sol-gel membranes and to measure COsb2 and the unreactive analytes trichloroethylene and perchloroethylene. Single layer pH sensors were fabricated using a base-catalyzed organo-silica sol-gel containing organosilane coupling agents. A base catalyst was found to be better suited for complete incorporation of the aminopropyltriethoxysilane used to attach dye molecules. This allows the production of optically transparent gels that respond to pH in less than 15 seconds. Dual layer COsb2 sensors use the pH sol-gel layer overcoated with a hydrophobic ORganically MOdified SIlica sol-gel membrane (ORMOSIL). The ORMOSIL reduces much of the pH cross sensitivity found in gas sensors and allows fast, reversible diffusion of COsb2. The sensors respond to COsb2 gas within 10 seconds and dissolved COsb2 in 2 minutes. COsb2 sensors have been found to be stable and reproducible for 12 months when stored dry and at least 6 months when stored in buffer. Many volatile organochloride compounds (VOC's) have been difficult to measure using current fiber-optic sensor transduction schemes. The three-layer optical sensor described here incorporates a TiOsb2/SiOsb2 membrane to degrade VOC's into smaller, detectable products, Hsp+, Clsp- and COsb2. Upon exposure to UV light, TiOsb2, a semiconductor with a bandgap of 3.2 eV, produces highly reactive electron-hole pairs that photodegrade organic compounds. The products produced on the TiOsb2 surface diffuse into the nearby indicator membrane where they are detected. Carbon dioxide and protons produced are detected by the pH sensitive indicator layer described above. Preliminary data for the measurement of VOC's indicates that the detection limit for PCE is less than 1.65 ppm in the headspace (10 ppm in solution). Photocatalysis is also used to measure uranyl

  7. Efficient dual-wavelength excitation of Tb3+ emission in rare-earth doped KYF4 cubic nanocrystals dispersed in silica sol-gel matrix

    NASA Astrophysics Data System (ADS)

    del-Castillo, J.; Yanes, A. C.; Santana-Alonso, A.; Méndez-Ramos, J.

    2014-11-01

    Energy transfer from Ce3+ to Tb3+ ions under UV excitation, giving rise to visible emissions, is investigated in sol-gel derived transparent nano-glass-ceramics containing cubic KYF4 nanocrystals, for different doping concentrations of rare-earth ions. Moreover, visible emissions of Tb3+ are also obtained under near-infrared excitation through energy transfer from Yb3+ ions by means of cooperative up-conversion processes. Thus, Ce3+-Tb3+-Yb3+ doped nano-glass-ceramics can be activated in a dual-wavelength mode yielding efficient blue-green emissions of particular interest in photovoltaic silicon solar cells and white-light emitting diodes.

  8. Protein-templated gold nanoclusters sequestered within sol-gel thin films for the selective and ratiometric luminescence recognition of Hg2+

    NASA Astrophysics Data System (ADS)

    Hofmann, Carrie M.; Essner, Jeremy B.; Baker, Gary A.; Baker, Sheila N.

    2014-04-01

    Sequestration of bovine serum albumin (BSA)-stabilized gold nanoclusters (AuNCs@BSA) prepared using microwave assistance within sol-gel-derived mesoporous silica films permits the selective and highly sensitive quenchometric detection of aqueous Hg2+ (limit of detection = 600 pM) with luminescence signal arising from oxidized BSA allowing for an analytically robust and reliable ratiometric detection. Overall, this work highlights a number of important advances, including the highest luminescence quantum yield reported to date for a protein-templated luminescent noble metal nanocluster (13%) made possible using a microwave-mediated synthesis followed by cold incubation. We also demonstrate the clear advantage of exploiting the luminescence signal arising from oxidized BSA as an internal reference to generate selectivity of response to Hg2+. A careful Stern-Volmer quenching analysis reveals the persistence of two unique quenching sites for AuNCs@BSA entrapped within a sol-gel-derived glass, a minor population of which is unquenchable. Finally, based on these AuNCs@BSA nanosensors, we advise a path forward for paper-based indicator strip detection of heavy metals in aqueous streams, the implementation of which can be performed using the unaided eye, making it a meaningful approach for routine screening and in resource-limited situations.Sequestration of bovine serum albumin (BSA)-stabilized gold nanoclusters (AuNCs@BSA) prepared using microwave assistance within sol-gel-derived mesoporous silica films permits the selective and highly sensitive quenchometric detection of aqueous Hg2+ (limit of detection = 600 pM) with luminescence signal arising from oxidized BSA allowing for an analytically robust and reliable ratiometric detection. Overall, this work highlights a number of important advances, including the highest luminescence quantum yield reported to date for a protein-templated luminescent noble metal nanocluster (13%) made possible using a microwave

  9. Synthesis and enhanced thermal stability of albumins@alumina: towards injectable sol-gel materials.

    PubMed

    Rutenberg, Avi; Vinogradov, Vladimir V; Avnir, David

    2013-06-25

    A major obstacle to the introduction of bioactively-doped sol-gel based materials for medical applications has been the fact that silica - the most widely studied sol-gel material - despite being a GRAS material, which is widely used as an additive in foods and drug formulations, is still not approved by regulatory agencies for intramuscular injections. Here we point to a potential solution to this problem by shifting the weight to alumina, which is approved for injections as the most common immunization adjuvant. Towards the achievement of this goal we describe the development of protein entrapment methods tailored to alumina, and show high thermal stability of protein-dopants, using a newly developed DSC methodology for this purpose.

  10. Sol-gel co-assembly of hollow cylindrical inverse opals and inverse opal columns.

    PubMed

    Haibin, Ni; Ming, Wang; Wei, Chen

    2011-12-19

    A facile approach of fabricating hollow cylindrical inverse opals and inverse opal columns by sol-gel co-assembly method was proposed. Polystyrene (PS) colloidal suspension added with hydrolyzed silicate precursor solution was used to self-assemble composite colloidal crystals which consist of PS colloidal crystal template and infiltrated silica gel in the interstitial of microspheres. Continuous hollow cylindrical composite colloidal crystal films have been produced on capillaries' outside and internal surface. Composite colloidal crystal columns which filling up the interior of a capillary were fabricated by pressure assisted sol-gel co-assembly method. Hollow cylindrical inverse opals and inverse opal columns were obtained after removing PS colloidal crystal from the composite colloidal crystal. Optical properties of the silica hollow cylindrical inverse opals were characterized by transmission spectrum and a stop band was observed. Structure and optical properties of the inverse opal columns were investigated.

  11. The porosity of sol-gel silica thin films for optrode applications

    SciTech Connect

    Harris, T.M.; Knobbe, E.T.

    1995-12-01

    Porous silica thin films produced by sol-gel processing are being considered for use in optical sensor (optrode) applications. In this study, thin films were produced by dip-coating onto glass slides. The porosity was then measured indirectly, by determining the amount of methylene blue adsorption on each slide. Using this technique, it has been determined that the {open_quotes}two-step{close_quotes} sol-gel process provides a greater surface area than the acid-catalyzed process. With the two-step process, increasing the amount of solvent (ethanol) and decreasing the rate of slide withdrawal from the sol provided increased surface area when normalized to the mass of the deposit.

  12. Cotton Fabric Surface Modification by Sol-Gel Deposition of ZnO Thin Films

    NASA Astrophysics Data System (ADS)

    Vihodceva, S.; Kukle, S.

    2012-08-01

    One of the main tasks of research is to impact the additional value on natural textiles by adding to them ultraviolet (UV) absorption and antimicrobial protection properties with ZnO nano-level coatings. ZnO shows high absorption in the UV region of the light spectrum, in comparison with organic absorbers conventionally used in the textile industry shows no significant degradation, is stable and classified as non-toxic material. Nanosols were prepared by using the sol-gel process. In this work comparison of samples coated by nanosols with zinc acetate (Zn (CH3COO)2-2H2O) and zinc sulphate (ZnSO4) was made. Scanning electron microscopy (SEM) was used to examine the nature of the surface modification with ZnO coating by the sol-gel technique as also after exploitation of samples; energy dispersive X-ray spectroscopy was used for the analysis of elemental composition of coated fabric samples.

  13. Nanocrystalline indium tin oxide fabricated via sol-gel combustion for electrochemical luminescence cells.

    PubMed

    Chaoumead, Accarat; Kim, Tae-Woo; Park, Min-Woo; Sung, Youl-Moon

    2012-04-01

    Nanoporous indium tin oxide (ITO) was synthesized via a sol-gel combustion hybrid method using Ketjenblack as a fuel. The effects of the sol-gel combustion conditions on the structures and morphology of the ITO particles were studied. The size of the nanoporous powder was found to be 20-30 nm in diameter. The layer of the nanoporous ITO electrode (-10 microm thickness) with large surface area (-360 m2/g) was fabricated for an electrochemical luminescence (ECL) cell. At 4 V bias, the ECL efficiency of the cell consisting of the nanoporous ITO layer was approximately 1050 cd/m2, which is significantly higher than the cell using only the FTO electrode (450 cd/m2). The nanoporous ITO layer was effective in increasing the ECL intensities.

  14. Fluor-hydroxyapatite sol-gel coating on titanium substrate for hard tissue implants.

    PubMed

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

    2004-08-01

    Hydroxyapatite (HA) and fluor-hydroxyapatite (FHA) films were deposited on a titanium substrate using a sol-gel technique. Different concentrations of F- were incorporated into the apatite structure during the sol preparation. Typical apatite structures were obtained for all coatings after dipping and subsequent heat treatment at 500 degrees C. The films obtained were uniform and dense, with a thickness of approximately 5 microm. The dissolution rate of the coating layer decreased with increasing F- incorporation within the apatite structure, which demonstrates the possibility of tailoring the solubility by a functional gradient coating of HA and FHA. The cell proliferation rate on the coating layer decreased slightly with increasing F- incorporation. The alkaline phosphatase (ALP) activity of the cells on all the HA and FHA coated samples showed much higher expression levels compared to pure Ti. This confirmed the improved activity of cell functions on the substrates with the sol-gel coating treatment.

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

    DOEpatents

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

    2006-05-02

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

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

    NASA Astrophysics Data System (ADS)

    Raghu, P.; Naveen, C. S.; Shailaja, J.; Mahesh, H. M.

    2016-05-01

    Transparent ZnO thin films were prepared using different molar concentration (0.1 M, 0.2 M & 0.8 M) of zinc acetate on soda lime glass substrates by the sol-gel spin coating technique. The optical properties revealed that the transmittance found to decrease with increase in molar concentration. Absorption edge showed that the higher concentration film has increasingly red shifted. An increased band gap energy of the thin films was found to be direct allowed transition of ˜3.9 eV exhibiting their relevance for photovoltaic applications. The extinction coefficient analysis revealed maximum transmittance with negligible absorption coefficient in the respective wavelengths. The results of ZnO thin film prepared by sol-gel technique reveal its suitability for optoelectronics and as a window layer in solar cell applications.

  17. The Physics of Evaporation-Induced Assembly of Sol-Gel Materials

    SciTech Connect

    HURD,ALAN J.; STEINBERG,LEV

    2000-07-24

    Remarkable materials ordered at the nanoscale emerge when a sol-gel solution becomes co-organized with a surfactant. At sufficiently high concentration, the surfactant forms crystalline or liquid-crystalline arrays of micelles in the presence of the sol-gel, and as gelation proceeds the arrays become locked into the gel. Recent experiments demonstrate that the degree of order in the resulting mesoporous ceramic phase can be enhanced and controlled by continuous dip coating in which the solution, initially dilute, evolves through the critical micelle concentration by steady-state evaporation. The long-range order and microstructural orientation in these films suggest that the propagation of a critical-micelle-concentration transition front, with large physico-chemical gradients, promotes oriented self assembly of surfactant aggregates. This steep-gradient view is supported by results from unsteady evaporation of aerosols of similar solutions, in which internally well-ordered but complex particles are formed.

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

    NASA Technical Reports Server (NTRS)

    1982-01-01

    Containerless melting of glasses in space for the preparation of ultrapure homogeneous glass for optical waveguides is discussed. The homogenization of the glass using conventional raw materials is normally achieved on Earth either by the gravity induced convection currents or by the mechanical stirring of the melt. Because of the absence of gravity induced convection currents, the homogenization of glass using convectional raw materials is difficult in the space environment. Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation.

  19. Sol-gel technologies in thin film fabrication for integrated optics lasers and amplifiers

    NASA Astrophysics Data System (ADS)

    Almeida, Rui M.; Vasconcelos, H. C.

    1997-07-01

    There is a strong need for the development of cheap component technologies for optical functions such as switching, demultiplexing and amplification. Silica-on- silicon integrated optics using sol-gel processing is probably the best technology for such low cost applications. This review focuses on the sol-gel based thin film fabrication technologies for integrated optics (IO) lasers and amplifiers, using Nd3+ and Er3+ as the active species. Special emphasis is given to the work performed under the European Union sponsored projects NODES (ESPRIT) and CAPITAL (ACTS), in particular to the processing and characterization of Nd3+ and Er3+-doped silica-titania planar waveguides for IO lasers and amplifiers.

  20. Versatile technique to functionalize optical microfibers via a modified sol-gel dip-coating method.

    PubMed

    Xu, Z Y; Li, Y H; Wang, L J

    2014-01-01

    We present a convenient and versatile technique to functionalize microfibers by depositing sol-gel jackets via a modified dip-coating method. This was elucidated by gain-functionalizing microfibers with erbium-ytterbium codoped silica sol-gel jackets. For a 4.5-cm-long coated microfiber, an internal gain of 1.8 dB and a net gain of 0.8 dB for a 1550 nm signal were observed, when combing together the gain of the doped jackets and low loss of microfibers. With benefits of convenience and versatility, this technique can be used for functionalizing microfibers with jackets showing gains in other spectral ranges, high nonlinearity, high sensitivity, and many other functions.

  1. Relaxation dynamics near the sol-gel transition: From cluster approach to mode-coupling theory

    NASA Astrophysics Data System (ADS)

    Coniglio, A.; Arenzon, J. J.; Fierro, A.; Sellitto, M.

    2014-10-01

    A long standing problem in glassy dynamics is the geometrical interpretation of clusters and the role they play in the observed scaling laws. In this context, the mode-coupling theory (MCT) of type-A transition and the sol-gel transition are both characterized by a structural arrest to a disordered state in which the long-time limit of the correlator continuously approaches zero at the transition point. In this paper, we describe a cluster approach to the sol-gel transition and explore its predictions, including universal scaling laws and a new stretched relaxation regime close to criticality. We show that while MCT consistently describes gelation at mean-field level, the percolation approach elucidates the geometrical character underlying MCT scaling laws.

  2. Pulsed electric field assisted sol-gel preparation of TiO2 nanoparticles

    NASA Astrophysics Data System (ADS)

    Mani, Rajaboopathi; Han, Bing; Louhi-Kultanen, Marjatta

    2016-10-01

    This work studies the effect of a pulsed electric field (PEF) on the precipitation and properties of TiO2 nanoparticles. TiO2 nanoparticles were prepared using pulsed DC electric field assisted sol-gel method. The duration of the PEF treatment was varied to investigate its effect on the particle size of TiO2 nanoparticles. The nanoparticles were characterized by X-ray powder diffraction (XRD), Raman spectroscopy, UV diffuse reflectance spectroscopy (UV-DRS) and transmission electron microscopy (TEM). It was found that TiO2 particles prepared with pulsed electric field assisted sol-gel method had enhanced average crystallite size due to the effect of the pulsed electric field on primary nucleation. The effect of electric field on nanoparticle preparation is interesting which can be used to control the grain and crystallite size of nanoparticle.

  3. Photochemical reduction of methyl viologen in silicate xerogels obtained by the sol gel process

    NASA Astrophysics Data System (ADS)

    Maruszewski, Krzysztof; Jasiorski, Marek; Hreniak, Dariusz; Stręk, Wiesław

    2001-10-01

    Mixture of ruthenium (II) tris-bipyridine complex (Ru(bpy) 32+ — photosensitizer), methyl viologen (MV 2+ — electron acceptor) and EDTA (sacrificial electron donor) has been immobilized in silicate xerogels obtained by the sol-gel technique. Mixtures of Ru(bpy) 32+, MV 2+ and EDTA are capable of formation of the blue photoreduced MV rad + cation radical in aqueous solutions upon UV (around 280 nm) or visible (around 450 nm) excitations. However, when entrapped in silicate xerogels they do not exhibit blue coloration at all. On the other hand, UV excitation of xerogels doped only with MV 2+ results in appearance of blue color indicative of the paraquat photoreduction. It has been shown that in the case of the xerogel-entrapped methyl viologen the source of the reducing photoelectron is ethanol. The alcohol molecules are produced during the tetraethoxysilane (precursor) hydrolysis step of the silicate matrix production occurring via the sol-gel process.

  4. The role of temperature in forming sol-gel biocomposites containing polydopamine

    PubMed Central

    Dyke, Jason Christopher; Hu, Huamin; Lee, Dong Joon; Ko, Ching-Chang; You, Wei

    2014-01-01

    To further improve the physical strength and biomedical applicability of bioceramicsbuilt on hydroxyapatite-gelatin (HAp-Gel) and siloxane sol-gel reactions, we incorporated mussel adhesive inspired polydopamine (PD) into our original composite based on HAp-Gel cross-linked with siloxane. Surprisingly, with the addition of PD, we observed that the processing conditions and temperatures play an important role in the structure and performance of these materials. A systematic study to investigate this temperature dependence behavior discloses that the rate of crosslinking of silane during the sol-gel process is significantly influenced by the temperature, whereas the polymerization of the dopamine only shows minor temperature dependence. With this discovery, we report an innovative thermal process for the design and application of these biocomposites. PMID:25485111

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

    NASA Astrophysics Data System (ADS)

    Walcarius, Alain; Collinson, Maryanne M.

    2009-07-01

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

  6. Nonlinear optical properties of sol-gel-type glasses containing oxidized Cu2Se nanoparticles

    NASA Astrophysics Data System (ADS)

    Yumashev, K. V.

    2000-03-01

    Nonlinear absorption of sol-gel-type glasses containing oxidized Cu2Se nanoparticles (25 nm in radius) is investigated with the aid of the picosecond excitation-probing technique. The oxidation of Cu2Se nanoparticles leads to the appearance of a wide absorption band, which has a maximum roughly at 1 µm and which is bleached on exposure to laser pulses. The time of relaxation of the bleached state approaches 300 psec, and the cross section for absorption at 1.06 µm is equal to about 1.3·10-16 cm2, as evaluated from the measured absorption saturation curve. The regime of Q-switching is obtained for a number of solid-state lasers with generation wavelengths 1.06, 1.34, and 1.54 µm, when sol-gel-type glasses containing oxidized Cu2Se nanoparticles were used as passive shutters.

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

    PubMed Central

    Tseng, Ting Ke; Lin, Yi Shing; Chen, Yi Ju; Chu, Hsin

    2010-01-01

    The sol-gel process is a wet-chemical technique (chemical solution deposition), which has been widely used in the fields of materials science, ceramic engineering, and especially in the preparation of photocatalysts. Volatile organic compounds (VOCs) are prevalent components of indoor air pollution. Among the approaches to remove VOCs from indoor air, photocatalytic oxidation (PCO) is regarded as a promising method. This paper is a review of the status of research on the sol-gel method for photocatalyst preparation and for the PCO purification of VOCs. The review and discussion will focus on the preparation and coating of various photocatalysts, operational parameters, and will provide an overview of general PCO models described in the literature. PMID:20640156

  8. Reversible Sol-Gel Transitions in Aqueous Solutions of N-Isopropylacrylamide Ionic Copolymers

    SciTech Connect

    Krzyminski, Karol J.; Jasionowski, Marek; Gutowska, Anna

    2008-04-01

    Ionic copolymers of N-isopropylacrylamide (NIPA) exhibiting sol-gel transitions in aqueous solutions were investigated. The studies were aimed at understanding of the structure-property relationship in design of injectable, in situ forming gels for potential biomedical applications in delivery of therapeutics and tissue engineering. Aqueous solutions of NIPA ionic copolymers were found to flow freely at ambient temperatures and formed soft gels with controlled syneresis above 32°C, the lower critical solution temperature of NIPA. The sol-gel transitions and temperature dependent properties of the resulting gels were analyzed using dynamic rheometry, UV and IR spectrometry, and were found to be controlled by the molecular weight and composition of copolymers, ionization state of comonomers, and composition of aqueous solvent.

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

    SciTech Connect

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

    1996-12-19

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

  10. Luminescent characteristics of sol-gel produced zinc sulphide display structures

    NASA Astrophysics Data System (ADS)

    Kavanagh, Yvonne M.; Cameron, David C.; Ryan, Brendan; Tobin, Ger

    2003-03-01

    Thin film electroluminescent (TFEL) display structures have been produced by sol-gel technology, with the active layer comprising doped zinc sulphide films produced by the sulphidation of sol-gel deposited zinc oxide thin films. The luminescent properties of display structures using manganese-doped zinc sulphide, which has a strong orange emission due to the Mn2+4 T1(4G) 6A1(6S) transitions have been investigated using photoluminescence (PL), cathodoluminescence (CL), and electroluminescence (EL) and the correlation between the luminescence produced by the various methods has been studied. A comparison of the spectra using PL, CL and EL has shown how these excitation methods can be used to quantify the electroluminescence produced by the zinc sulphide. The effects of the interaction between the insulating layer and the emission layer have also been studied.

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

    SciTech Connect

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

    2010-12-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

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

  13. Synthesis and Characterization of Al doped ZnO (AZO) by Sol-gel Method

    NASA Astrophysics Data System (ADS)

    Munawaroh, H.; Wahyuningsih, S.; Ramelan, A. H.

    2017-02-01

    Al doped ZnO (AZO) nanoparticles have been successfully synthesized by the simple sol-gel method. The starting materials of Al doped ZnO were Zn(CH3COO)2·2H2O and Al(OH)(CH3COO)2. Preparation of AZO using polyethylene glycol as a surfactant. The solution of precursors was stirred at 60 °C for 2 hour in the conditions of Al contents are 0%, 2%, 3% and 4% (g/mL), respectivelly. In the last step reaction, gelation occurred from solution to sol gel. The sol gel then were dried at 60 °C following by annealing process for crystalization. By this simple sol gel method, the nanoparticles have been produced. The characterizations were conducted X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Fourrier Transform Infra-Red (FTIR) and X-Ray Fluorescence (XRF). XRD analysis reveals that all samples has crystallizes in polycrystalline nature and exhibit no other impurity phase. The variation of Al doped ZnO slighly affect the crystallinity and crystal size. Both crystallinity and crystal size decrease with increasing of Al content in AZO. Morphology of AZO shown the particle distribution more equitable with increased Al content. The synthesized AZO gaved shift peak absorption of asymetric and symetric vibrations of Zn-O-Zn around wavelengths of 680 cm-1 and 1630 cm-1 atributed of the uptake of the Al-O-Al bond instead Zn-O-Zn. XRF analysis shown that the increase ratio of Al entering into Zn influenced the Al dopant concentration.

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

    SciTech Connect

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

    1993-10-01

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

  15. The detection of hexavalent chromium by organically doped sol-gels

    SciTech Connect

    Wong, P.W.; Mackenzie, J.D.

    1994-12-31

    The sol-gel process can be used to produce porous inorganic matrices that are doped with organic molecules. These doped gels can be used as a quantitative method for the spectrophotometric determination of trace concentrations of metallic ions. For the detection of hexavalent chromium, malachite green was used as the dopant. Preliminary results indicate concentrations on the order of 5 ppb are detectable using this method.

  16. Synthetic implant surfaces. 1. The formation and characterization of sol-gel titania films.

    PubMed

    Haddow, D B; Kothari, S; James, P F; Short, R D; Hatton, P V; van Noort, R

    1996-03-01

    Sol-gel has been used to prepare thin titania films. We have investigated the effects of dip rate, sintering temperature and time on the chemical composition of the films, their physical structure and thickness, and adherence to a silica substrate. Our aim has been to produce films that mimic as closely as possible the natural oxide layer that is found on titanium. These films are to be used as substrates in an in vitro model of osseointegration.

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

    NASA Technical Reports Server (NTRS)

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

    1983-01-01

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

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

    SciTech Connect

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

    2015-05-15

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

  19. Novel Sol-Gel Deposition for Repair of Conducting Paths in Polyceramic Systems

    DTIC Science & Technology

    1994-02-24

    and spectroelectroanalytical techniques. Based on elemental analysis results, the doping level of chemically synthesized polyaniline and poly...at 60C until the gel was formed. The resulting sol-gel composites ( polyaniline /poly(MMA-MSNA)-S0 2 ) were doped with HC1 aqueous solution to convert...MSMA (10%) was found to be soluble in m-cresol. Doped polyaniline or blends of emeraldine base and camphorsulfonic acid were dissolved in m-cresol and

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

    DTIC Science & Technology

    2015-10-19

    Catalysts in Sol-Gel Matrices 5a. CONTRACT NUMBER 5b. GRANT NUMBER N00014-09-1-0217 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Detty, Michael R. 5d...SUPPLEMENTARY NOTES 14. ABSTRACT We have developed new xerogel coatings with organochalcogenide or metal oxide catalysts for the activation of...hydrogen peroxide as anti-fouling, fouling-release surfaces. The catalysts perform more efficiently when covalently attached to the xerogel framework

  1. Sensor layers and waveguide layers produced in sol-gel technology

    NASA Astrophysics Data System (ADS)

    Karasinski, Pawel; Zielonka, Iwona

    2003-04-01

    The paper presents the results of investigation studies on the application of sol-gel technology for the production of sensor layers and waveguide layers for the system of planar waveguide sensors. The sensor layers are made up by silica SiO2, which is playing the role of a matrix fixing bromocresol purpole. These layers are sensitive to ammonia. The waveguide layers are produced in a two-component system SiO2:TiO2.

  2. Secondary Crystal Growth on a Cracked Hydrotalcite-Based Film Synthesized by the Sol-Gel Method.

    PubMed

    Lee, Wooyoung; Lee, Chan Hyun; Lee, Ki Bong

    2016-05-02

    The sol-gel synthesis method is an attractive technology for the fabrication of ceramic films due to its preparation simplicity and ease of varying the metal composition. However, this technique presents some limitations in relation to the film thickness. Notably, when the film thickness exceeds the critical limit, large tensile stresses occur, resulting in a cracked morphology. In this study, a secondary crystal growth method was introduced as a post-treatment process for Mg/Al hydrotalcite-based films synthesized by the sol-gel method, which typically present a cracked morphology. The cracked hydrotalcite-based film was hydrothermally treated for the secondary growth of hydrotalcite crystals. In the resulting film, hydrotalcite grew with a vertical orientation, and the gaps formed during the sol-gel synthesis were filled with hydrotalcite after the crystal growth. The secondary crystal growth method provides a new solution for cracked ceramic films synthesized by the sol-gel method.

  3. Photoresist-Free Fully Self-Patterned Transparent Amorphous Oxide Thin-Film Transistors Obtained by Sol-Gel Process

    NASA Astrophysics Data System (ADS)

    Lim, Hyun Soo; Rim, You Seung; Kim, Hyun Jae

    2014-04-01

    We demonstrated self-patterned solution-processed amorphous oxide semiconductor thin-film transistors (TFTs) using photosensitive sol-gels. The photosensitive sol-gels were synthesized by adding β-diketone compounds, i.e., benzoylacetone and acetylacetone, to sol-gels. The chemically modified photosensitive sol-gels showed a high optical absorption at specific wavelengths due to the formation of metal chelate bonds. Photoreactions of the modified solutions enabled a photoresist-free process. Moreover, Zn-Sn-O with a high Sn ratio, which is hard to wet-etch using conventional photolithography due to its chemical durability, was easily patterned via the self-patterning process. Finally, we fabricated a solution-processed oxide TFT that included fully self-patterned electrodes and an active layer.

  4. Thermodynamic analysis of sol-gel transition of gelatin in terms of water activity in various solutions.

    PubMed

    Miyawaki, Osato; Omote, Chiaki; Matsuhira, Keiko

    2015-12-01

    Sol-gel transition of gelatin was analyzed as a multisite stoichiometric reaction of a gelatin molecule with water and solute molecules. The equilibrium sol-gel transition temperature, Tt , was estimated from the average of gelation and melting temperature measured by differential scanning calorimetry. From Tt and the melting enthalpy, ΔHsol , the equilibrium sol-to-gel ratio was estimated by the van't Hoff equation. The reciprocal form of the Wyman-Tanford equation, which describes the sol-to-gel ratio as a function of water activity, was successfully applied to obtain a good linear relationship. From this analysis, the role of water activity on the sol-gel transition of gelatin was clearly explained and the contributions of hydration and solute binding to gelatin molecules were separately discussed in sol-gel transition. The general solution for the free energy for gel-stabilization in various solutions was obtained as a simple function of solute concentration.

  5. Research of materials for porous matrices in sol-gel systems based on silicon dioxide and metallic oxides

    NASA Astrophysics Data System (ADS)

    Maraeva, E. V.; Bobkov, A. A.; Maximov, A. I.; Moshnikov, V. A.; Nalimova, S. S.

    2015-11-01

    In this study silicon dioxide - stannic oxide and silicon dioxide - zinc nanomaterials oxide were obtained through sol-gel technology. The results of nitrogen thermal desorption measurements, atomic force microscopy measurements and particle sizes measurements are discussed.

  6. Silica sol-gel matrix doped with Photolon molecules for sensing and medical therapy purposes.

    PubMed

    Podbielska, Halina; Ulatowska-Jarza, Agnieszka; Müller, Gerhard; Holowacz, Iwona; Bauer, Joanna; Bindig, Uwe

    2007-11-01

    Photolon is one of the new photosensitisers that has found application in photodynamic therapy (PDT). Its chemical structure has a partially reduced porphyrin moiety and its molecular structure is comparable to chlorin e(6), which can be isolated after hydrolysis of the 5-membered exocyclic beta-ketoester moiety of pheophorbide a. For this study, a Photolon doped sol-gel matrix was produced in the form of coatings deposited on silica fibers cores. The material was produced from sols prepared from the silicate precursor TEOS mixed with ethyl alcohol. The sol-gel films were prepared with factor R=20, where R denotes the solvent-to-precursor molar ratio. Hydrochloric acid was added as a catalyst in the correct proportion to ensure acid hydrolysis (pH approximately 2). The mixture was stirred at room temperature for 4h using a magnetic stirrer (speed 400 rpm). The coated fibers were examined in different environments, liquid and gaseous, at different pH values and with various zinc cation concentrations. The chemical reactions were studied by means of spectroscopic methods, whereby the fluorescence response was studied. It was demonstrated that Photolon immobilized in a sol-gel matrix is accessible for the environment and shows visible response to the external changes. Furthermore, it was observed that these reactions are reversible. These biomaterials are also examined as carriers for PDT. It was also proved that a toxic effect is observed an environment with microorganisms, meaning that doped coatings have photodynamic activity.

  7. Disinfection studies on TiO2 thin films prepared by a sol-gel method.

    PubMed

    Kambala, Venkata Subba Rao; Naidu, Ravi

    2009-02-01

    Transparent anatase TiO2 nanometer thin films were prepared by dip-coating on soda-lime glass plates via the sol-gel method. The un-calcined and the calcined films were characterized by X-ray diffraction (XRD), AFM, Nano-indentation (hardness and Young's modulus), UV-vis spectrometry, thickness and hydrophilicity (contact angle measurements). The photocatalytic activity of the thin films was evaluated by performing disinfection studies on the Gram-negative microorganisms like Escherichia coli, and Staphylococcus Aureus, a Gram-positive organism. The photocatalytic activity for both groups of organisms was studied in saline and nutrient broth. The leakage of potassium from the bacteria was observed parallel to cell viability. The activity of the sol-gel prepared TiO2 thin films were compared under UV lamps and natural day light (ND) lamps with Degussa P-25 TiO2 thin films prepared on soda-lime glass using a polymer support and the commercial self-cleaning glass (SC). The sol-gel prepared thin films which were annealed at 450 degrees C, show highest photocatalytic activity, the slowest conversion rate from hydrophilic to a hydrophobic state, light-induced hydrophilicity, and also higher disinfection activities compared to P-25 films and commercial self-cleaning glass. The films also show excellent activities when continuously reused for more than a month.

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

    PubMed

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

    2015-07-27

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

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

    PubMed

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

    2016-08-01

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

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

    PubMed

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

    2017-05-01

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

  11. Direct test of the critical exponents at the sol-gel transition

    NASA Astrophysics Data System (ADS)

    Kaya, Demet; Pekcan, Önder; Yılmaz, Yaşar

    2004-01-01

    The steady state fluorescence technique was used to study the sol-gel transition for the solution-free radical cross-linking polymerization of acrylamide (AAm), with N,N'-methylenebis (acrylamide) as cross linker in the presence of ammonium persulfate as an initiator. Pyranine (8-hydroxypyrene-1, 3,6-trisulfonic acid, trisodium salt) is used as a fluoroprobe for monitoring the polymerization. Pyranine molecules start to bind to acrylamide polymer chains upon the initiation of the polymerization, thus the spectra of the bonded pyranines shift to the shorter wavelengths. Fluorescence spectra from the bonded pyranines allows one to monitor the sol-gel transition, without disturbing the system mechanically, and to test the universality of the sol-gel transition as a function of some kinetic parameters such as polymer concentration, cross-linker concentration, and temperature. Observations around the critical point show that there are three regimes for AAm concentration in which the exponents differ drastically. The gel fraction exponent β and the weight average degree of polymerization exponent γ agree best with the static percolation results for higher acrylamide concentrations above 1M, but they cross over from percolation to mean-field (Flory-Stockmayer) values when the AAm concentration is lower than 2M. For very low polymer concentrations, below which the system can not form the gel, the exponents differ considerably from both the percolation and the mean-field values.

  12. Thin-film silica sol-gels doped with ion-responsive fluorescent lipid bilayers

    NASA Astrophysics Data System (ADS)

    Sasaki, Darryl Y.; Shea, Lauren E.; Sinclair, Michael B.

    1999-05-01

    A metal ion sensitive, fluorescent lipid-bilayer material (5% PSIDA/DSPC) was successfully immobilized in a silica matrix using a tetramethoxysilane (TMOS) sol-gel procedure. The sol- gel immobilization method was quantitative in the entrapment of self-assembled lipid-bilayers and yielded thin films for facile configuration to optical fiber platforms. The silica matrix was compatible with the solvent sensitive lipid bilayers and provided physical stabilization as well as biological protection. Immobilization in the silica sol-gel produced an added benefit of improving the bilayer's metal ion sensitivity by up to two orders of magnitude. This enhanced performance was attributed to a preconcentrator effect from the anionic surface of the silica matrix. Thin gels (193 micron thickness) were coupled to a bifurcated fiber optic bundle to produce a metal ion sensor probe. Response times of 10 - 15 minutes to 0.1 M CuCl2 were realized with complete regeneration of the sensor using an ethylenediaminetetraacetic acid (EDTA) solution.

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

    NASA Astrophysics Data System (ADS)

    Yadav, Reeta

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

  14. Aqueous sol-gel encapsulation of genetically engineered Moraxella spp. cells for the detection of organophosphates.

    PubMed

    Yu, Diana; Volponi, Joanne; Chhabra, Swapnil; Brinker, C Jeffrey; Mulchandani, Ashok; Singh, Anup K

    2005-01-15

    An all-aqueous sol-gel method for encapsulation of bacterial cells in porous silicate matrices towards the development of a biosensor is described. The sol-gel encapsulation of cells is achieved at room temperature and neutral pH. Furthermore, use of sodium silicate as precursor avoids generation of alcohol that can be detrimental to cells in contrast to the traditional alkoxide sol-gel encapsulation process. Moraxella spp. cells engineered to express recombinant organophosphorus hydrolase (OPH) on the cell surface were encapsulated and OPH enzymatic activity was measured for paraoxon hydrolysis. Kinetic parameters (Km and Vmax) as well as pH behavior of surface-expressed OPH were determined to evaluate the effect of encapsulation. Cells encapsulated by the sodium silicate method displayed higher activity retention compared to those by the traditional alkoxide process. Time-course studies over a 2-month period indicate that immobilization through the sodium silicate process led to a reduction in activity of approximately 5% as compared to approximately 30% activity reduction in case of free cells in buffer indicating that immobilization leads to stabilization, a key parameter in biosensor development.

  15. Qualification of Target Chamber Vacuum Systems Cleanliness using Sol-Gel Coatings

    SciTech Connect

    Miller, P; Stowers, I F; Ertel, J R

    2006-01-03

    This document defines the procedure necessary to qualify the airborne molecular cleanliness (AMC) of vacuum systems (enclosures or large components) that are placed within the National Ignition Facility (NIF) target chamber or are attached to it and communicate with it during vacuum operation. This test is specific to the NIF target chamber because the allowable time dependent rate of rise in the pore filling of a sol-gel coated SAW sensor is based on some nominal change-out time for the disposable debris shields. These debris shields will be sol-gel coated and thus they represent a means of ''pumping'' AMCs from the target chamber. The debris shield pumping rate sets the allowable change in pore filling with time specified in the test procedure. This document describes a two-part procedure that provides both a static measurement of sol-gel pore filling at the end of a 48-hour test period and a dynamic record of pore-filling measured throughout the test period. Successful qualification of a vacuum system requires that both the static and dynamic measurements meet the criteria set forth in Section 7 of this document.

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

    NASA Astrophysics Data System (ADS)

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

    2012-02-01

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

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

    PubMed Central

    Vinogradov, Vladimir V.; Avnir, David

    2015-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Vinogradov, Vladimir V.; Avnir, David

    2015-09-01

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

  19. Thin-film silica sol-gels doped with ion responsive fluorescent lipid bilayers

    SciTech Connect

    Sasaki, D.Y.; Shea, L.E.; Sinclair, M.B.

    1999-01-12

    A metal ion sensitive, fluorescent lipid-b i layer material (5oA PSIDA/DSPC) was successfully immobilized in a silica matrix using a tetramethoxysilane (TMOS) sol-gel procedure. The sol-gel immobilization method was quantitative in the entrapment of seif-assembled Iipid-bilayers and yielded thin films for facile configuration to optical fiber piatforms. The silica matrix was compatible with the solvent sensitive lipid bilayers and provided physical stabilization as well as biological protection. Immobilization in the silica sol-gel produced an added benefit of improving the bilayer's metal ion sensitivity by up to two orders of magnitude. This enhanced performance was attributed to a preconcentrator effect from the anionic surface of the silica matrix. Thin gels (193 micron thickness) were coupled to a bifurcated fiber optic bundle to produce a metal ion sensor probe. Response times of 10 - 15 minutes to 0.1 M CUCIZ were realized with complete regeneration of the sensor using an ethylenediarninetetraacetic acid (EDTA) solution.

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

    PubMed Central

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

    2015-01-01

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

  1. Synthesis of polymeric fluorinated sol-gel precursor for fabrication of superhydrophobic coating

    NASA Astrophysics Data System (ADS)

    Li, Qianqian; Yan, Yuheng; Yu, Miao; Song, Botao; Shi, Suqing; Gong, Yongkuan

    2016-03-01

    A fluorinated polymeric sol-gel precursor (PFT) is synthesized by copolymerization of 2,3,4,5,5,5-hexafluoro-2,4-bis(trifluorinated methyl)pentyl methacrylate (FMA) and 3-methacryloxypropyltrimethoxysilane (TSMA) to replace the expensive long chain fluorinated alkylsilanes. The fluorinated silica sol is prepared by introducing PFT as co-precursor of tetraethyl orthosilicate (TEOS) in the sol-gel process with ammonium hydroxide as catalyst, which is then used to fabricate superhydrophobic coating on glass substrate through a simple dip-coating method. The effects of PFT concentrations on the chemical structure of the formed fluorinated silica, the surface chemical composition, surface morphology, wetting and self-cleaning properties of the resultant fluorinated silica coatings were studied by using X-ray powder diffraction (XRD), Fourier transform infrared spectrometer (FTIR), X-ray photoelectron spectrophotometer (XPS), scanning electron microscopy (SEM) and water contact angle measurements (WCA). The results show that the fluorinated silica sols are successfully obtained. The size and size distribution of the fluorinated silica particles are found greatly dependent on the concentration of PFT, which play a crucial role in the surface morphology of the corresponding fluorinated silica coatings. The suitable PFT concentration added in the sol-gel stage, i.e. for F-sol-1 and F-sol-2, is helpful to achieve both the low surface energy and multi-scaled microstructures, leading to the formation of the superhydrophobic coatings with bio-mimicking self-cleaning property similar to lotus leaves.

  2. Preparation and characterisation of a sol-gel process α-Al₂O₃ polycrystalline detector.

    PubMed

    Ferreira, H R; Santos, A

    2015-02-01

    This article presents the dosimetric characteristics of α-Al2O3 detectors prepared through the sol-gel process, disc pressing and sintering in a highly reducing atmosphere. Comparative tests between the sol-gel process α-Al2O3 polycrystalline and anion-defective α-Al2O3:C single-crystal detectors indicate that the ones prepared through this approach present good dosimetric characteristics similar to those found in single-crystal detectors, such as a simple glow curve with the main peak at ∼198 °C (2 °C s(-1)), high sensitivity, a detection threshold of 1.7 µGy, linearity of response, low fading, relatively low photon energy dependence, reusability without annealing and good reproducibility. However, the undesirable feature of heating rate dependence of the thermoluminescence (TL) output in α-Al2O3:C single crystal is practically non-existent in the sol-gel process α-Al2O3 polycrystalline detector. This characteristic renders it useful for the routine processing of large numbers of personal and environmental dosemeters at higher heating rates and also when it comes to the proposal for new approaches to thermal quenching investigation.

  3. Effect of two-step sol-gel reaction on the mesoporous silica structure.

    PubMed

    Choi, Dae-Geun; Yang, Seung-Man

    2003-05-01

    In the present study, we investigated the effects of two-step sol-gel reaction by abrupt pH change on the SBA-15 and mesocellular silica foams (MCF). Mesoporous silica was fabricated by using triblock copolymer templates (poly(ethylene oxide) and poly(propylene oxide)). The prepared silica structure was characterized by X-ray diffraction, transmission electron microscopy, and N(2) sorption experiment. Specifically, we prepared SBA-15 with long-range two-dimensional hexagonal arrangement of 3 to 6-nm feature spacing and MCF with larger pores of a few tens of nanometers. The pore size and ordering were influenced by pH change in a two-step sol-gel reaction and the concentration of organic solvent. Although well-ordered hexagonal arrangement of mesopores was prevalent in acidic conditions, the materials synthesized by a single-step reaction in neutral or basic conditions possessed gel-like structure without mesopores. However, the present two-step reaction (low pH sol-gel reaction followed by high pH reaction) not only produced mesoporous materials but also provided controllability of the pore size. In particular, mesoporous structures with pore sizes as large as those of MCF were successfully fabricated by the two-step reaction without using organic swelling agents. As expected, when xylene was added as a swelling agent, the pore size increased with the xylene/copolymer weight ratio.

  4. Hybrid sol-gel technology for fast prototyping in astronomical interferometry

    NASA Astrophysics Data System (ADS)

    Ghasempour, A.; Leite, A. M. P.; Alexandre, D.; Reynaud, F.; Marques, P. V. S.; Garcia, P. J. V.

    2010-07-01

    Hybrid sol-gel technology was used for fabrication of prototypes of coaxial two, three and four telescopes beam combiners for astronomical applications. These devices were designed for the astronomical J-band and have been characterized using an optical source with emission centered at 1265 nm and with a spectral FWHM of 50 nm. Interferometric characterization of the two, three and four beam combiners, showed average contrasts respectively higher than 98%, 96% and 95%. Interferometric spectral analysis of the beam combiners revealed that the chromatic differential dispersion is the main contributor to the observed contrast decay in the latter cases. The laser direct writing technique was used for fabrication of a coaxial two beam combiner on sol-gel material; it showed a contrast of 95%. The measured high contrast fringes confirm that the procedures used lead to performant IO beam combiners. These results demonstrate the capabilities of the hybrid sol-gel technology for fast prototyping of complex chip designs for astronomical applications.

  5. Nanoscale morphology for high hydrophobicity of a hard sol gel thin film

    NASA Astrophysics Data System (ADS)

    Wu, Y. L.; Chen, Z.; Zeng, X. T.

    2008-08-01

    It is challenging to obtain a hydrophobic smooth coating with high optical and mechanical properties at the same time because the hydrophobic additives are soft in nature resulting in reduced hardness and durability. This paper reports a durable hydrophobic transparent coating on glass fabricated by sol-gel technology and a low volume medium pressure (LVMP) spray process. The sol-gel formula consists of a pre-linked hydrophobic nano-cluster from hydroxyl-terminated polydimethylsiloxane, titanium tetraisopropoxide and a silica-based sol-gel matrix with silica hard fillers. Polydimethylsiloxane (PDMS) is uniformly distributed throughout the coating layer providing durable hydrophobic property. Mechanical properties are achieved by the hard matrix and hard fillers with the nano-structures. Due to the surface nano-morphology, a high degree of hydrophobicity was maintained with only 10 vol.% PDMS, while the hardness and abrasion resistance of the coatings were not significantly compromised. Chemical analyses by FTIR confirmed the uniform distribution of the PDMS and surface morphology analyses by atomic force microscopy (AFM) displayed the nano-surface structures that enhanced the hydrophobicity. The special surface nanostructures can be quantified using surface Kurtosis and ratio between asperity peak height to distance between peaks. The LVMP process influences the spray droplet size resulting in different surface structures.

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

    NASA Astrophysics Data System (ADS)

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

    2014-05-01

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

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

    PubMed

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

    2016-03-31

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

  8. Spectroscopic studies of trimetoxypropylsilane and bis(trimethoxysilyl)ethane sol-gel coatings on aluminum and copper

    NASA Astrophysics Data System (ADS)

    Li, Ying-Sing; Tran, Tuan; Xu, Yue; Vecchio, Nicolas E.

    2006-11-01

    Trimethoxypropylsilane (TMPS) and bis(trimethoxysilyl)ethane (BTMSE) were used as surface modifiers of metal vie the sol-gel process and dip coating. In addition to the single coating of Al, Cu and Sn, double treatments of Al were also conducted by combining coatings with these sol-gels in different sequences. Reflection and absorption infrared spectroscopy (RAIR) was employed to characterize and to trace the proceeding of the sol-gel process of the films. It was found that the silanol condensation occurs in the coating films on Al and the covalent linkage exists between the TMPS film and copper surface. From the assigned vibration modes, two conformers were identified in pure TMPS, TMPS sol-gel and coated film. A series of dip coating experiments with different concentrations of TMPS sol-gel was conducted, and the results from the collected RAIR spectra of the coated samples suggested that the coated Cu consistently has a better RAIR spectrum than that of the coated Al. The TMPS sol-gel appeared to have a better affinity to Cu than to Al. The temperature effect and the aging effect in the coating films were studied. X-ray photoelectronic spectroscopy (XPS) was employed to characterize the coated film, and the XPS data confirm the formation of the siloxane film from the silane coupling agents (SCA). Electrochemical impedance spectra (EIS) have been collected for bare Al and Cu, BTMSE sol-gel coated Al, and TMPS sol-gel coated Cu in 0.15 M NaCl solution. The corresponding electronic circuit parameters have been determined to match the experimental EIS data.

  9. Synthesis of an imprinted hybrid organic-inorganic polymeric sol-gel matrix toward the specific binding and isotherm kinetics investigation of creatinine.

    PubMed

    Chang, Yong-Sheun; Ko, Ting-Hsien; Hsu, Ting-Jung; Syu, Mei-Jywan

    2009-03-15

    Hybrid organic-inorganic polymeric sol-gel materials imprinted with creatinine template molecules were synthesized for the specific binding of creatinine. Creatinine is a metabolite from creatine and is the final product from kidney metabolism. Therefore, creatinine can be an important index to estimate the function of the kidney. It was then chosen as the target molecule in this work. To achieve the specific binding toward creatinine, molecular imprinting was used to create a polymeric matrix for the regarding purpose. Sol-gel was further added to create a rigid network structure for the absorption of creatinine. An inorganic precursor, tetraethoxysilane (TEOS), was mixed with an organic functional monomer, 2-acrylamido-2-methylpropane-sulfonic acid (AMPS), and the creatinine template to form a hybrid organic-inorganic imprinted polymer. The chemical functionality was achieved as well as a confined matrix via the polymerization and the hydrolysis-condensation of the sol-gel. The imprinting effect from the hybrid materials against the corresponding nonimprinted was investigated. BET (Brunauer-Emmett-Teller) analysis was carried out for the imprinted and the nonimprinted materials. The specificity of the hybrid materials was further examined by capping the surface silanol groups with chloro-trimethylsilane (CTMS) and 1,1,1,3,3,3-hexamethyldisilazane (HMDS), respectively. The capping effect was compared and discussed from the binding results. Selectivity of the materials toward creatinine was obtained using mixture solutions in the presence of creatinine and its analogues. Reutilization and storage stability of the hybrid organic-inorganic imprinted material were also studied. Additionally, the affinity distribution of the hybrid imprinted materials derived from the allosteric model was also analyzed from the adsorption isotherm data.

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

    NASA Astrophysics Data System (ADS)

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

    2011-03-01

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

  11. Processing and properties of lead zirconate titanate thin films on gallium nitride and ruthenium by sol-gel and chemical vapor deposition

    NASA Astrophysics Data System (ADS)

    Cao, Wei

    The Pb(ZrxTi1-x)O3 (PZT) thin films are potential candidates for ferroelectric random access memory (FeRAM) devices and components for microelectromechanical systems (MEMS). For example, the PZT/GaN system is being explored as RF MEMS devices for insertion in RF communication systems. A reproducible sol-gel process was developed for the deposition of PZT films on wurtzite (0001) GaN/sapphire substrates. The composition, crystallography, and interfacial nanochemistry were evaluated by various characterization techniques. The PZT/GaN heterostructure exhibited a chemically sharp interface with insignificant interdiffusion between PZT and GaN layers. However, PZT in metal -ferroelectric -semiconductor (MFS) configuration showed lower capacitance and asymmetrical polarization hysteresis compared to PZT in metal-ferroelectric-metal configuration. Such a deviation was attributed to the high depolarization field (Edepol) within PZT. To mitigate this issue, a two-pronged approach was used. First, the calculated spatial distribution of the electric field and potential, which stem from all the charge densities within the MFS configuration, demonstrated that by adjusting controllable parameters, one can minimize Edepol and maximize polarization. Second, a robust metal-organic chemical vapor deposition (MOCVD) process was developed to fabricate high quality PZT thin films on GaN. In this experimental approach, phase-pure and highly (111) oriented PZT films were deposited on GaN/sapphire substrates by MOCVD. The orientation relationships of PZT/GaN system were determined using x-ray pole figure and high-resolution transmission electron microscopy (TEM). The nanochemistry of the PZT/GaN interface, studied using analytical TEM, indicated a chemically sharp interface with interdiffusion limited to a region below 5 nm. The properties of MOCVD-PZT on GaN are briefly compared with PZT by sol-gel processing, rf sputtering, and pulsed laser deposition. Additionally, a preliminary study

  12. Study on polarization characteristics of BiFeO3 thin films prepared by sol-gel spin-coating technology

    NASA Astrophysics Data System (ADS)

    Jia, Ze; Wu, Xiao; Zhang, Mingming; Xu, Jianlong; Zhang, Naiwen; Liou, Juin J.

    2015-07-01

    The ferroelectric polarization properties of bismuth ferrite (BFO) thin films deposited on Pt(111)/TiO2/SiO2/Si(100) substrates by sol-gel spin-coating technology affected by the processes and dopants have been studied and analyzed tentatively. The results indicate BFO thin film should be introduced to a rapid thermal annealing (RTA) process at N2 atmosphere. The enhanced ferroelectric polarization properties were observed in Mn and La doped BFO thin films, because ion substitution may improve the inherent volatility of Bi atoms, valence fluctuation of Fe ions and magnetic spin structures, reducing the formation of oxygen vacancies. The increased remnant polarization observed in the BFO thin film with a lead zirconate titanate (PZT) seeding layer has also been analyzed as the probable results of small changes of lattice parameters caused by constraint stress, reduced defects and decreased leakage current density, which are contributed by the PZT seeding layer possibly. Moreover, the remnant polarization approximately 79 μC/cm2 is observed in (Bi0.95La0.05)FeO3 (BLFO) thin film with a PZT seeding layer, which is twice and treble the values of BFO thin films with and without a PZT seeding layer, indicating PZT seeding layer is much more effective for BLFO thin film which has a substitution at A site.

  13. Modification of the sensitivity and selectivity of thin porous layers coated by the sol-gel method on silica optical fibers to gases

    NASA Astrophysics Data System (ADS)

    Matejec, Vlastimil; Berkova, Daniela; Chomat, Miroslav; Kuncova, Gabriela

    1999-12-01

    It has been found that thin layers of aerogels applied by the sol-gel method on silica optical fibers change their optical properties due to the interaction with gases such as hydrocarbons. This paper deals with modification of the sensitivity and selectivity to vapors of hydrocarbons and chlorinated hydrocarbons of siloxane aerogel layers based on their doping with TiOTi chains and/or immobilizing in them Cu-ephedrine and Cu-phthalocyanine. The sensing fibers were prepared by the sol-gel application of porous siloxane and doped-siloxane layers on bare cores of PCS fibers. By using the excitation of the fiber with inclined laser beams it is experimentally shown that there are positive or negative changes of the output optical power from the fibers due to bringing the prepared layers into contact with vapors of aliphatic, aromatic and chlorinated hydrocarbons in nitrogen. These effects may be related to a difference between the refractive index of the layer and refractive index of liquid hydrocarbon or hydrocarbon its derivative. It is shown experimentally that doping porous siloxane layers with copper complexes changes their refractive index and optical losses changing thus their sensitivity and selectivity to hydrocarbons and hydrocarbon derivatives.

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

    PubMed

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

    2015-02-01

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

  15. Synthesis of nano-bound microsphere Co3O4 by simple polymer-assisted sol-gel technique

    NASA Astrophysics Data System (ADS)

    Karthick, S. N.; Hemalatha, K. V.; Justin Raj, C.; Kim, Hee Je; Yi, Moonsuk

    2013-03-01

    Nano-bound Co3O4 microspheres and molten Co3O4 microspheres were synthesized for the first time by a simple polymer (poly-(vinylpyrrolidone))-assisted sol-gel and sol-gel technique, respectively. Thermal decomposition of the precursor samples of both polymer-assisted sol-gel and sol-gel technique were studied by thermogravimetric analysis. In both techniques, the material was calcined at different temperatures for the formation of phase pure Co3O4. X-ray diffraction confirmed the formation of phase pure cubic spinel structured Co3O4 at 400 and 500 °C for the polymer-assisted sol-gel and sol-gel technique, respectively. Fourier transform infrared spectroscopy revealed the vibrational assignments of functional groups associated with the cubic spinel structure of Co3O4. Scanning electron microscopy of all samples showed clear microsphere sizes ranging from 1 to 4 μm. Both techniques allowed the formation of spherical-shaped microspheres by a simple process. Nano-bound microspheres were observed from the polymer-assisted sol-gel technique because the decomposition of PVP at 400 °C is the main reason for the formation of nano-bound microspheres. The nanoparticle size of the nano-bound microsphere measured by transmission electron microscopy was 40 nm. Therefore, PVP is an essential compound for the formation of nano-bound microspheres. This very simple and inexpensive technique is suitable for the formation of spherical-shaped microspheres.

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

    A coating with self-cleaning characteristics has been developed using a TiO2/SiO2 hybrid sol-gel, TiO2 nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO2 nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO2 nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO2 phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO2 NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

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

    NASA Technical Reports Server (NTRS)

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

    2004-01-01

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

  18. Synthesis and characterization of sol gel silica films doped with size-selected gold nanoparticles

    NASA Astrophysics Data System (ADS)

    Ferrara, M. C.; Mirenghi, L.; Mevoli, A.; Tapfer, L.

    2008-09-01

    Homogeneous nanocomposite silica films uniformly doped with size-selected gold nanoparticles (AuNPs) have been prepared by a combined use of colloidal chemistry and the sol-gel process. For this purpose, stable thiol-functionalized AuNPs (DDT-AuNPs) were first synthesized by a two-phase aqueous/organic system and, subsequently, dispersed in an acid-catalysed sol-gel silica solution. The microstructural morphology of the samples was investigated by x-ray diffraction and field emission scanning electron microscopy. X-ray photoelectron spectroscopy (XPS) and UV-vis optical spectrophotometry were instead employed to investigate the elemental chemical behaviour and the evolution of the surface plasmon resonance (SPR) band of the AuNPs from their synthesis up to the formation of the Au-doped silica films. The results show that the size, shape and crystalline domains of the AuNPs remain unchanged during the entire preparation process, indicating that their aggregation or decomposition was prevented. XPS results show that the DDT-AuNPs lose the capping shells and oxidize themselves when dispersed in acid-catalysed sol-gel solutions, and that bare AuNPs are embedded in the SiO2 films. A large broadening of the SPR band, observed for systems with DDT-AuNPs, suggests the presence of interface effects which cause a surface electron density lowering. Thiol chain detachment from the AuNPs determines an increase of the SPR peak intensity while the oxidation of the Au surfaces causes a red shift of its position. The latter is no longer observed in doped films, suggesting that no interfacial effects between bare AuNPs and the host medium are present.

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

    NASA Technical Reports Server (NTRS)

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

    2003-01-01

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

  20. Stability High Salt Content Waste Using Sol Gel Process. Mixed Waste Focus Area. OST Reference Number 0236

    SciTech Connect

    None, None

    1999-09-01

    Mixed waste sludges, soils, and homogeneous solids containing high levels of salt ( ~ greater than 15% by weight ) have proven to be difficult to stabilize due to the soluble nature of the salts. The current stabilization technique for high salt waste, grouting with Portland cement, is limited to low waste loadings. The presence of salts interfere with the hydration and curing of the cement, cause waste form deteriorating mineral expansions, or result in an undesirable separate phase altogether. Improved technologies for the stabilization of salt waste must be able to accommodate higher salt loadings, while maintaining structural integrity, chemical durability, and leach resistance. In a joint collaboration supported by the Department of Energy’s (DOE’s) Mixed Waste Focus Area (MWFA), the Pacific Northwest National Laboratory (PNNL) and the Arizona Materials Laboratory (AML) at the University of Arizona have developed a sol-gel (wet-chemical) based, low-temperature-processing route for the stabilization of salt-containing mixed wastes. By blending and reacting liquid precursors at room temperature with salt waste, strong, impermeable “polyceram” matrices have been formed that encapsulate the environmentally hazardous waste components. As depicted by Figure 1, polycerams are hybrid organic/inorganic materials with unique properties derived from the chemical combination of polymer (organic) and ceramic (inorganic) components. For this application, the stabilizing polyceram matrices contain polybutadiene-based polymer components and silicon dioxide (SiO2) as the inorganic component. Polybutadiene (PBD) is a strong, tough, waterresistant plastic and its use in the polyceram promotes these same characteristics in the waste form. The PBD polymer component is modified to increase its reactivity with the SiO2 precursor during sol-gel processing. When combined, the polymer and SiO2 precursors react, gel, solidify, and encapsulate the