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Sample records for sol-gel derived ferroelectric

  1. Antiferroelectric-ferroelectric switching and induced strains for sol-gel derived lead zirconate thin layers

    SciTech Connect

    Tani, T.; Li, J.; Viehland, D.; Payne, D.A.

    1994-03-15

    Lead zirconate (PZ) thin layers were formed by a sol-gel method and crystallized with a pseudocubic (111) or (100) preferred orientation. The field-forced antiferroelectric (AFE)-to-ferroelectric (FE) phase transformation behavior was examined by Sawyer--Tower measurements. Dielectric properties were measured as a function of temperature and frequency, and the field-induced transformational strain was measured by interferometry. Both the high-field hysteresis behavior and the temperature-dependent weak-field dielectric properties were found to be strongly dependent on preferred orientation. An increase in the remanent polarization and dielectric constant was observed under high electric field strengths at room temperature, or for lower field strengths at higher temperature. Strains as large as 0.7% were determined for the field-forced AFE-to-FE transformation. AFE-to-FE switching was demonstrated with full saturation at room temperature for high dielectric strength (100 MV/m) thin layers (300 nm).

  2. 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.

  3. Sol-gel derived ? thin films on GaAs

    NASA Astrophysics Data System (ADS)

    Arscott, S.; Smith, N.; Kurchania, R.; Milne, S. J.; Miles, R. E.

    1998-02-01

    Sol-gel derived thin films of lead zirconate titanate (PZT) have been fabricated on a platinized GaAs substrate using a propane-1,3-diol based sol-gel route. PZT can be used as the piezoelectric component in bulk acoustic wave devices for monolithic microwave integrated circuit applications. A 100 nm silicon nitride buffer layer was deposited onto the GaAs by plasma-enhanced chemical vapour deposition in order to prevent gallium and arsenic outdiffusion during film fabrication. Rapid thermal processing (RTP) techniques were employed to decompose thermally the sol-gel layer to PZT in a further effort to minimize problems of gallium and arsenic outdiffusion. Adhesion between the bottom electrode and substrate was found to improve when an intermediate titanium layer deposited between the platinum and silicon nitride was oxidized prior to deposition of the platinum electrode. A crystalline PZT film was produced on the 0268-1242/13/2/016/img9 substrate configuration by firing the sol-gel coating at 0268-1242/13/2/016/img10C for 10 s using RTP. A single deposition of sol resulted in a film having a thickness of 0268-1242/13/2/016/img11. Ferroelectric hysteresis measurements yielded average values of remanant polarization and coercive field of 0268-1242/13/2/016/img12 and 0268-1242/13/2/016/img13 respectively.

  4. 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.

  5. 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.

  6. Highly reliable bipolar resistive switching in sol-gel derived lanthanum-doped PbTiO3 thin film: Coupling with ferroelectricity?

    NASA Astrophysics Data System (ADS)

    Wang, Ying; Chen, Wei-Jin; Zhang, Xiao-Yue; Ma, Wen-Jing; Wang, Biao; Zheng, Yue

    2014-08-01

    Nanoscale Pb x La1- x Ti1- x/4O3 (PLT) thin film has been fabricated on PtTiSiO2Si substrates by chemical solution deposition (CSD) method. Ferroelectricity of the fresh-made PLT thin film has been clearly detected through piezoelectric force microscopy (PFM) by writing reversible ferroelectric domains. However, PLT thin film also shows off-standard ferroelectric hysteresis loops highly dependent on frequency, indicating large amount of mobile space charges in the film. Subsequent current-voltage (C-V) studies show that sandwich-like PtPLTPt structure exhibits notable bipolar resistive switching (BRS) characteristics with high stability (> 103 switching cycles). It is found that the C-V curves of both high- and low-resistance states have the feature of space-charge-limited current (SCLC) conduction, indicating important roles of defects in the conduction. X-ray photoelectron spectroscopy measurement further verifies that oxygen vacancies based conductive filament mechanism is likely responsible for the observed RS effect. Our demonstration of stable RS effect in the PLT thin film and its possible coupling with ferroelectricity is promising in device development and applications, such as development of ferroelectric-tunable RS memories.

  7. Phase purity of sol-gel-derived hydroxyapatite ceramic.

    PubMed

    Hsieh, M F; Perng, L H; Chin, T S; Perng, H G

    2001-10-01

    Calcium oxide was reported in the sol-gel-derived hydroxyapatite (HA) as an unavoidable major impurity. In this study phase purity of HA synthesized by sol-gel route was explored using precursors of calcium nitrate tetrahydrate and triethyl phosphate. Two different drying methods, the fast drying of as-prepared precursors and the slow drying of aged precursors were adopted as major processing variables. The dried gels were subsequently calcined up to 600 degrees C. In the calcined powder from fast-dried gel, X-ray diffraction (XRD) patterns revealed an intense CaO peak. For the slow-dried gel, thermogravimetric analysis revealed a 2-step weight-loss behavior during heating. XRD analysis of the calcined powder, corresponding to the second weight-loss step, showed major peaks of hydroxyapatite and a very weak CaO peak. P-31 NMR analysis indicated formation of calcium phosphate complex during aging. Complete incorporation of Ca(NO3)2 into the complex due to proper aging therefore diminishes CaO formation. It was also found that the minor CaO derived in the slow drying method can be easily and completely washed out just by distilled water.

  8. 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.

  9. 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

  10. Sol-gel-derived waterproof coating for laser glass

    NASA Astrophysics Data System (ADS)

    Jiang, Zhonghong; Hu, Lili; Song, Xiuyu

    1997-12-01

    A two layer coating was deposited by sol-gel dip-coating method on phosphate laser glass. First silica film was coated from SiO2 colloidal suspension derived from ammonia catalyzed hydrolysis of tetraethoxysilane in ethanol. Then a methyl containing silicate film was covered. It was fabricated from a solution prepared by the hydrolysis of methyltriethoxysilane in the presence of hydrogen chloride catalyst. A 130 degree(s)C, 16h heat-treatment was done after coating process. It is confirmed by optical microscope that the two layer coating improves obviously the chemical durability of phosphate laser glass. The laser damage threshold of this coating is measured to be 31 J/cm2 at 1060 nm wavelength of 10 ns pulse duration. It is found that silica film contributes to the improvement on both film adhesion to phosphate glass substrate and laser damage threshold of film. The methyl containing silicate single film has only 18 J/cm2 laser damage threshold and can be easily dissolved in ethanol solution when it was coated on the phosphate laser glass substrate.

  11. 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.

  12. Optical activation of Si nanowires using Er-doped, sol-gel derived silica

    SciTech Connect

    Suh, Kiseok; Shin, Jung H.; Park, Oun-Ho; Bae, Byeong-Soo; Lee, Jung-Chul; Choi, Heon-Jin

    2005-01-31

    Optical activation of Si nanowires (Si-NWs) using sol-gel derived Er-doped silica is investigated. Si-NWs of about 100 nm diameter were grown on Si substrates by the vapor-liquid-solid method using Au catalysts and H{sub 2} diluted SiCl{sub 4}. Afterwards, Er-doped silica sol-gel solution was spin-coated, and annealed at 950 deg. C in flowing N{sub 2}/O{sub 2} environment. Such Er-doped silica/Si-NWs nanocomposite is found to combine the advantages of crystalline Si and silica to simultaneously achieve both high carrier-mediated excitation efficiency and high Er{sup 3+} luminescence efficiency while at the same time providing high areal density of Er{sup 3+} and easy current injection, indicating the possibility of developing sol-gel activated Si-NWs as a material platform for Si-based photonics.

  13. Citrate complexing sol-gel process of lead-free (K,Na)NbO3 ferroelectric films

    NASA Astrophysics Data System (ADS)

    Yao, Linlin; Zhu, Kongjun

    2016-05-01

    The citrate complexing sol-gel process to fabricate lead-free (K,Na)NbO3 ferroelectric thin films was studied. Soluble niobium source of niobium-citric acid (Nb-CA) solution was utilized as a raw material to synthesize (K,Na)NbO3 thin films, by pyrolyzing at 450-550∘C and annealing at 650∘C. The film pyrolyzed at 450∘C shows poor crystallization with porous morphology, whereas the film pyrolyzed at 550∘C appear to be well-crystallized and denser, and the ferroelectricity was also proved by the P-E hysteresis loop measurement.

  14. 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.

  15. Sol-gel-derived silicate nano-hybrids for biomedical applications.

    PubMed

    Tsuru, Kanji; Shirosaki, Yuki; Hayakawa, Satoshi; Osaka, Akiyoshi

    2013-01-01

    Organic-inorganic hybrids of poly(dimethyl siloxane), gelatin, and chitosan with such silanes as tetraethoxysilane and 3-glycidoxytriethoxysilane are derived via the sol-gel routes. Their biomedical applications are discussed from biomimetic deposition of bone-like apatite, cell culture, and in vivo behavior.

  16. 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.

  17. Sealing of pores in sol-gel-derived tritium permeation barrier coating by electrochemical technique

    NASA Astrophysics Data System (ADS)

    Zhang, Kun; Hatano, Yuji

    2011-10-01

    An electrolytic deposition technique was applied to seal open pores in sol-gel derived ZrO 2 coating and to improve barrier effects against permeation of hydrogen isotopes. Disk-type specimens of type 430 ferritic stainless steel were first covered by thin ZrO 2 films (50 nm) with a conventional sol-gel technique. Then, pores in the ZrO 2 film was sealed with ZrO 2 or Al 2O 3 by cathodic processes in ethanol solution of Zr or Al nitrate and subsequent heat treatments in air. The permeation rate of hydrogen was measured at 300-600 °C. The sol-gel derived ZrO 2 coatings showed only limited barrier effects; the permeation reduction factor (PRF) was about 6-800. Nevertheless, the treatments by electrolytic deposition technique resulted in considerable improvement in the barrier effects, especially at high temperature region (>500 °C), and the PRF increased to 100-1000.

  18. Studies of ferroelectric and dielectric properties of pure and doped barium titanate prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Bisen, Supriya; Mishra, Ashutosh; Jarabana, Kanaka M.

    2016-05-01

    In this work, Barium Titanate (BaTiO3) powders were synthesized via Sol-Gel auto combustion method using citric acid as a chelating agent. We study the behavior of ferroelectric and dielectric properties of pure and doped BaTiO3 on different concentration. To understand the phase and structure of the powder calcined at 900°C were characterized by X-ray Diffraction shows that tetragonal phase is dominant for pure and doped BTO and data fitted by Rietveld Refinement. Electric and Dielectric properties were characterized by P-E Hysteresis and Dielectric measurement. In P-E measurement ferroelectric loop tracer applied for different voltage. The temperature dependant dielectric constant behavior was observed as a function of frequency recorded on hp-Hewlett Packard 4192A, LF impedance, 5Hz-13Hz analyzer.

  19. Dielectric and magnetic properties of sol-gel-derived lead iron niobate ceramics

    SciTech Connect

    Majumder, S.B.; Bhattacharyya, S.; Katiyar, R.S.; Manivannan, A.; Dutta, P.; Seehra, M.S.

    2006-01-15

    In this work, we report the synthesis of sol-gel-derived lead iron niobate [Pb{sub 1.10}(Fe{sub 0.5}Nb{sub 0.5})O{sub 3}] (PFN) powders and sintered ceramics. The PFN powders were calcined at (T{sub a}), 973, 1073, 1173, 1273, and 1373 K for 3 h in air. As envisaged from x-ray-diffraction analyses, PFN powder calcined at 1173 K was crystallized into pure monoclinic perovskite phase whereas powders calcined at all other temperatures had varied amounts of retained pyrochlore (Pb{sub 3}Nb{sub 4}O{sub 13}) phase coexisted with dominant monoclinic perovskite phase. The PFN pellet (prepared using the phase pure powder calcined at 1173 K) sintered at 1373 K for 4 h in air also had a minute quantity of retained pyrochlore phase coexisting with desired perovskite phase. From the temperature dependence of measured capacitance and loss tangent at different frequencies, the ferroelectric to paraelectric phase-transition temperature of PFN ceramics was observed at T{sub c}{approx_equal}370 K. The diffused nature of this transition and high dielectric constant of PFN is related to the cation disorder at the B site of A(B{sub I}{sup +3}B{sub II}{sup +5})O{sub 3} lattice. For PFN powders, calcined at different temperatures, the temperature dependence of the magnetic susceptibility ({chi}) was measured in a temperature range of 2-360 K, whereas the magnetic hysteresis loops and electron magnetic resonance (EMR) spectra were measured at room temperature. Room-temperature ferromagnetism is observed in all the calcined powder samples and it was found that the magnetization increases with the increase in calcination temperature (T{sub a}). The symmetric EMR line shape with g{approx_equal}2.01 observed in all calcined samples was identified to be due to Fe{sup 3+} ions. It is suggested that the observed weak ferromagnetism, which increases with an increase in T{sub a}, may be due to canting of the Fe{sup 3+} spins. These observations suggest PFN to be a very attractive single

  20. Sol-gel technique for the preparation of beta-cyclodextrin derivative stationary phase in open-tubular capillary electrochromatography.

    PubMed

    Wang, Y; Zeng, Z; Guan, N; Cheng, J

    2001-07-01

    A novel open-tubular capillary electrochromatography (OT-CEC) column coated with 2,6-dibutyl-beta-cyclodextrin (DB-beta-CD) was prepared using sol-gel technique. In the sol-gel approach, owing to the three-dimensional 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. We achieved high efficiencies of 5-14 x 10(4) plates/m for the isomeric nitrophenols using the sol-gel-derived DB-beta-CD columns. The migration time reproducibility of the separation of the isomeric nitrophenols was better than 2.2% over five runs and 4.5% from column to column. These sol-gel-coated DB-beta-CD columns have shown improved separations of isomeric aminophenols, isomeric dihydroxybenzenes and isomeric nitrophenols, in comparison with the sol-gel matrix capillary column. The influences of buffer pH and methanol solvent on separation were investigated. The chiral resolution of enantiomers such as ibuprofen and binaphthol was explored primarily.

  1. Copper oxide and selenide nanoparticles embedded into sol-gel-derived silica glasses doped with europium

    NASA Astrophysics Data System (ADS)

    Gurin, Valerij S.; Yumashev, Konstantin V.; Prokoshin, P. V.; Zolotovskaya, S. A.; Alexeenko, A. A.

    2002-11-01

    The silica sol-gel derived glasses co-doped with CuxO and CuxSe nanoparticles and Eu3+ ions have been fabricated. The analysis of luminescence spectra of a series of glasses with different composition allows us to suppose the direct energy transfer between copper oxide nanoparticle and Eu3+ ion. A luminescence signal of europium ions occurs as the result of excitation of the complex active centres (SiO2:Cu2O:Eu3+) in the absorption range of copper oxide.

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

    NASA Astrophysics Data System (ADS)

    Haruvy, Yair; Liedtke, Volker

    2003-09-01

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

  3. Fabrication and optical properties of sol-gel-derived interference coating for high power laser applications

    NASA Astrophysics Data System (ADS)

    Zhang, Qinyuan; Pita, Kantisara; Xu, Chang-Qing; Que, Wenxiu; Hinooda, S.; Thilakan, Periyasamy

    2001-10-01

    A single layer sol-gel derived TiO2 thin films and 6 periods SiO2/TiO2 multilayer coating were designed and prepared on GaAs substrates as anti-reflection coating or near-IR-reflective coating for high power semiconductor laser applications. Crack free TiO2 thin films having thickness of 80-150 nm, and refractive indices of 1.8-2.1 have been obtained by simply sol-gel method upon heating at different temperatures. The obtained TiO2 thin films on GaAs substrates have shown reflectance of

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

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

  5. Ferroelectric, Dielectric, Ferromagnetic, and Magnetoelectric Properties of BNF-NZF Bilayer Nanofilms Prepared via Sol-Gel Process

    NASA Astrophysics Data System (ADS)

    Guo, Kaixin; Zhang, Rongfen; Mou, Qingfeng; Cui, Ruirui; Deng, Chaoyong

    2016-09-01

    Bilayer magnetoelectric (ME) nanofilms composed of Bi0.9Nd0.1FeO3 (BNF) and Ni0.55Zn0.45Fe2O4 (NZF) were fabricated on the Pt(111)/Ti/SiO2/Si(100) substrates via sol-gel and a subsequent rapid thermal process with different growth sequences of BNF and NZF forming the following layered structures: BNF/NZF and NZF/BNF. The phase composition, microstructure, and ferroelectric, dielectric, ferromagnetic, and ME coupling properties of the composites were investigated at room temperature. Structural characterization by X-ray diffraction and scanning electron microscopy showed that there are no other impurity phases but BNF and NZF, and the nucleation barrier caused that it is easier for NZF and BNF to grow on each other rather than on the surface of Pt/Ti/SiO2/Si. The tests of the physical properties indicated that such heterostructures present both good ferroelectric, ferromagnetic, and dielectric properties and the in-plane ME coupling coefficient α E at room temperature but some discrepancies also exist, which can be attributed to an interfacial effect, in other words, the deposition sequences of the constituent phases have a great influence on the properties of bilayer films.

  6. Ferroelectric, Dielectric, Ferromagnetic, and Magnetoelectric Properties of BNF-NZF Bilayer Nanofilms Prepared via Sol-Gel Process.

    PubMed

    Guo, Kaixin; Zhang, Rongfen; Mou, Qingfeng; Cui, Ruirui; Deng, Chaoyong

    2016-12-01

    Bilayer magnetoelectric (ME) nanofilms composed of Bi0.9Nd0.1FeO3 (BNF) and Ni0.55Zn0.45Fe2O4 (NZF) were fabricated on the Pt(111)/Ti/SiO2/Si(100) substrates via sol-gel and a subsequent rapid thermal process with different growth sequences of BNF and NZF forming the following layered structures: BNF/NZF and NZF/BNF. The phase composition, microstructure, and ferroelectric, dielectric, ferromagnetic, and ME coupling properties of the composites were investigated at room temperature. Structural characterization by X-ray diffraction and scanning electron microscopy showed that there are no other impurity phases but BNF and NZF, and the nucleation barrier caused that it is easier for NZF and BNF to grow on each other rather than on the surface of Pt/Ti/SiO2/Si. The tests of the physical properties indicated that such heterostructures present both good ferroelectric, ferromagnetic, and dielectric properties and the in-plane ME coupling coefficient α E at room temperature but some discrepancies also exist, which can be attributed to an interfacial effect, in other words, the deposition sequences of the constituent phases have a great influence on the properties of bilayer films. PMID:27599718

  7. 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.

  8. 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. PMID:14599142

  9. 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.

  10. 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.

  11. Direct electrochemistry and electrocatalysis of horseradish peroxidase immobilized in sol-gel-derived ceramic-carbon nanotube nanocomposite film.

    PubMed

    Chen, Hongjun; Dong, Shaojun

    2007-03-15

    The sol-gel-derived ceramic-carbon nanotube (SGCCN) nanocomposite film fabricated by doping multiwall carbon nanotubes (MWNTs) into a silicate gel matrix was used to immobilize protein. The SGCCN film can provide a favorable microenvironment for horseradish peroxidase (HRP) to perform direct electron transfer (DET) at glassy carbon electrode. The HRP immobilized in the SGCCN film shows a pair of well-defined redox waves and retains its bioelectrocatalytic activity to the reduction of O2 and H2O2, which is superior to that immobilized in silica sol-gel film.

  12. In vitro characterization of polyvinyl alcohol assisted hydroxyapatite derived by sol-gel method.

    PubMed

    Kaygili, Omer; Keser, Serhat; Al Orainy, R H; Ates, Tankut; Yakuphanoglu, Fahrettin

    2014-02-01

    The synthesis and characterization of sol-gel derived hydroxyapatite (HAp) were investigated with the effects of the addition of polyvinyl alcohol (PVA) to the structural and material in vitro behavior. All samples were soaked in simulated body fluid (SBF) for 14 and 28 days. The characterization of bioceramics before and after immersing in SBF was carried out by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, differential thermal analysis (DTA), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM) techniques. After the simulated body fluid period, the crystal structure and phase of HAp samples did not change significantly. The characteristic bands of hydroxyl, phosphate and carbonate groups were detected. HAp exhibited a thermal stability of room temperature to 1000 °C. The surface morphologies of the samples show an evident change with the soaking period in SBF.

  13. Integrated optics structures on sol-gel derived organic-inorganic hybrids for optical communications

    NASA Astrophysics Data System (ADS)

    André, P. S.; Vicente, C. M. S.; Fernandes, V.; Marques, C. A. F.; Pecoraro, E.; Nogueira, R. N.; Wada, N.; Carlos, L. D.; Marques, P. G.; Ferreira, R. A. S.

    2011-05-01

    Organic-inorganic hybrid materials are a technologically key class of advanced multifunctional materials that fulfil the challenging strict requirements of the beginning of the century: higher levels of sophistication, miniaturisation, recyclability, reliability and low energy consumption with potential to be used as low-cost components in optical networks operating at high bit rates. In this work, high-rejection optical filters (19 dB) first-order Bragg gratings inscribed in channel waveguides written in thin films of sol-gel derived organic-inorganic hybrid based on methacrylic acid modified zirconium tetrapropoxide, Zr(OPrn)4, (so-called di-ureasils), using UV-laser direct-write method.

  14. 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.

  15. Evaluating sol-gel ceramic thin films for metal implant applications: III. In vitro aging of sol-gel-derived zirconia films on Ti-6Al-4V.

    PubMed

    Kirk, P B; Filiaggi, M J; Sodhi, R N; Pilliar, R M

    1999-01-01

    Sol-gel-derived zirconia films were deposited onto polished Ti-6Al-4V substrates by dip-coating from an alkoxide precursor solution. No change in morphology of the zirconia film was observed after aging at 37 degrees C for 4-12 weeks in pH 4.0 buffer solution or Hanks' balanced salt solution (HBSS), although a precipitate predominantly composed of calcium phosphate was formed on those films aged in HBSS. X-ray diffraction identified the phase of the zirconia film as either cubic or tetragonal, and revealed no degradation to the monoclinic phase after aging. By a substrate straining test, the fracture strain of the coating was revealed to be 1.5%, above the yield strain of the titanium alloy substrate. At this strain level, through-thickness cracks formed in the coating where slip bands emerged from the substrate. Qualitatively, the adhesion of the film was sufficient to prevent gross delamination of the film at high strain levels, although small regions of delamination were caused by compressive buckling of the film. This behavior indicates generally good adhesion. No change in this behavior was observed after aging.

  16. 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.

  17. 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. PMID:27661569

  18. Luminescence behavior of terbium sulphosalicylic acid complexes in sol-gel derived host materials

    SciTech Connect

    Fan, X.; Wang, M.; Wang, Z.; Hong, Z.

    1997-08-01

    The formation and luminescence behavior of terbium sulphosalicylic acid (TbSSA) complexes in sol-gel derived host materials have been investigated. The 5-sulphosalicylic acid (H{sub 3}SSA) was dissolved in ethanol in advance, and then the TbCl{sub 3} and ethanol containing H{sub 3}SSA were introduced into the initial precursor sol, respectively. The resulting sol exhibits intramolecular energy transfer from the coordinated sulphosalicylic acid to the terbium ion. The TbSSA complex has formed in the TbCl{sub 3} and H{sub 3}SSA codoped sol. The complexes were found to have notably higher fluorescence intensities than TbCl{sub 3} in both the sol and the gel. In the sol, the concentration quenching was a diffusion-controlled process due to aggregation and effective collision between molecules and the fluorescence was decreased with increase of H{sub 3}SSA concentration. On the other hand, the molecules in the gel were isolated in the pores of the silica network. The fluorescence intensities of TbSSA in the gel were increased with the increase of concentration ratio of H{sub 3}SSA/TbCl{sub 3}. Maximum fluorescence intensity was obtained at H{sub 3}SSA/TbCl{sub 3} = 2.

  19. Synthesis, consolidation and characterization of sol-gel derived tantalum-tungsten oxide thermite composites

    NASA Astrophysics Data System (ADS)

    Cervantes, Octavio

    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. The heat of combustion of two distinctly synthesized stoichiometric tantalum-tungsten oxide energetic composites was investigated by bomb calorimetry. One composite was synthesized using a sol-gel (SG) derived method in which micrometric-scale tantalum is immobilized in a tungsten oxide three-dimensional nanostructured network structure. The second energetic composite was made from the mixing of micrometric-scale tantalum and commercially available (CA) nanometric tungsten oxide powders. The energetic composites were consolidated using the spark plasma sintering (SPS) technique under a 300 MPa pressure and at temperatures of 25, 400, and 500°C. For samples consolidated at 25°C, the density of the CA composite is 61.65 +/- 1.07% in comparison to 56.41 +/- 1.19% for the SG derived composite. In contrast, the resulting densities of the SG composite are higher than the CA composite for samples consolidated at 400 and 500°C. The theoretical maximum density for the SG composite consolidated to 400 and 500°C are 81.30 +/- 0.58% and 84.42 +/- 0.62%, respectively. The theoretical

  20. 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

  1. 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.

  2. 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

    2015-01-01

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

  3. Synthesis and Conductometric Property of Sol-Gel-Derived ZnO/PVP Nano Hybrid Films

    NASA Astrophysics Data System (ADS)

    Ilegbusi, Olusegun J.; Trakhtenberg, Leonid

    2013-03-01

    ZnO nanoparticles immobilized in polyvinylpyrrolidone (PVP) were prepared using sol-gel dip-coating technique with varying Zn2+/PVP ratios. The films were characterized using atomic force microscopy, x-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy for chemical analysis. The size and concentration of ZnO particles decreased as the Zn/PVP ratio decreased. Under low Zn2+/PVP molar ratios, ZnO particles were clearly well separated and capped in the PVP polymer matrix. Electrical resistivity of 108 Ω cm was achieved under these deposition conditions.

  4. 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.

  5. Dielectric and ferroelectric properties of highly oriented (Pb,Nb)(Zr,Sn,Ti)O3 thin films grown by a sol-gel process

    NASA Astrophysics Data System (ADS)

    Jiwei, Zhai; Cheung, M. H.; Xu, Zheng Kui; Li, Xin; Chen, Haydn; Colla, Eugene V.; Wu, T. B.

    2002-11-01

    Antiferroelectric (Pb,Nb)(Zr,Sn,Ti)O3 thin films were deposited via a sol-gel process on LaNiO3-coated silicon substrates. Films showed a strong (001) preferred orientation upon annealing at 500-700 degC for 30 min. The dependence of electrical properties on film thickness has been studied, with the emphasis placed on field-induced phase switching from the antiferroelectric to the ferroelectric state. The decrease of film thickness led to an increase of the phase-switching field along with the appearance of remanent polarization. However, the dielectric constant and maximum polarization decreased with the reduction of film thickness. Saturation polarization was 35 muC/cm2, which is equal to that observed in bulk samples.

  6. 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. PMID:24575625

  7. 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

  8. Nile red synchronous scan fluorescence spectroscopy to follow matrix modification in sol-gel derived media and its effect on the peroxidase activity of cytochrome c.

    PubMed

    Rei, Ana; Ferreira, M Isabel C; Hungerford, Graham

    2008-11-01

    The highly solvatochromic dye Nile red is used in conjunction with synchronous scan fluorescence spectroscopy to elucidate changes in the internal environment of cytochrome c, upon incorporation into differently modified sol-gel derived media. Nile red was first studied in a variety of solvents in order to quantify changes in polarity. Matrix modifications involved the addition of several silanes, intended to interact with any unreacted hydroxyl entities left from the matrix forming reaction, while polymers were used to help reduce shrinkage and modify the internal pore environment. Slight unfolding of the protein was observed on incorporation into the sol-gel derived media. During the aging process further changes were monitored by using difference synchronous scan fluorescence spectra and complementary measurements of catalytic activity, expressed as the initial velocity. Combining Nile red synchronous scan fluorescence with cytochrome c activity data lead to a method to elucidate effects linked to protein conformation and those related to the sol-gel derived host.

  9. 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.

  10. Sol-gel-derived xerogel-doped nickel tetrasulfophthalocyanine and its optical properties

    NASA Astrophysics Data System (ADS)

    Zhan, Hongbing; Chen, Wengzhe; Lin, Chunying

    2002-09-01

    Metallophthalocyanines (MPc) exhibit, among many useful properties, the abilty to protect sensors against short, intense pulse deleterious to efficient sensor operation. For the successful application of this optical limiting property, an important issue is the incorporation of MPc molecules in a matrix to fabricate a solid state system. We report here the study of different concentrations of Nickle Tetrasulfophthalocyanine (NiTSPc) encapsulated in silica xerogel matrix obtained by sol-gel technique. The resulted composites were transparent and homogeneously with appropriate optical quality. The trapping effect was check by the characteristic absorption bands of NiTSPc in the UV/Vis spectra. The optical limiting properties of the composites were measured at 532nm with 8ns pulses.

  11. 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.

  12. Sol-gel derived optical waveguide films: technological platform for development of planar evanescent wave sensors

    NASA Astrophysics Data System (ADS)

    Karasiński, Paweł

    2015-12-01

    Plane evanescent wave sensors are being developed for over thirty years. However, their full development is somehow limited by the lack of relatively cheap and stable waveguide layers of high refractive index, low optical losses and at the same time resistance to the impact of chemical substances. The paper involves waveguide layers SiO2:TiO2 of high refractive index (˜1.81) satisfying these criteria, fabricated via sol-gel method and dip-coating technique. The parameters of the waveguide layers SiO2:TiO2 were determined using elipsometric and spectrophotometric methods. The presented waveguide layers have excellent optical properties and are suitable for the application in the planar evanescent wave sensors technology. For the best waveguide SiO2:TiO2 layers, the obtained level of optical loss was below 0.2 dB/cm.

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. 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.

  18. Sol-Gel Derived Zinc Oxide Films and Their Sensitivity to Humidity

    NASA Astrophysics Data System (ADS)

    Dixit, Shobhna; Srivastava, Anchal; Srivastava, Atul; Shukla, Rajesh Kumar

    2008-07-01

    In this study, the sensitivity of ZnO thin films to humidity is examined using an optical method. A precursor solution for ZnO film is prepared using the sol-gel process. Sensing elements were fabricated by spin coating different numbers of layers on separate prisms and subsequently annealing them. The sensing mechanism is the modulation of light intensity reflected from the glass-film interface as the relative humidity in the ambient air changes. The change in sensing with variation in number of layers is substantiated by theoretical calculations. Infrared studies, thermal gravimetric analysis, and differential thermal analysis of the precursor films was performed. The ZnO films are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and optical transmission. SEMs studies confirm the presence of pores which are instrumental in adsorbing water vapour, thereby influencing the refractive index of the films. In the present opto-electronic sensing configuration described herein, a change of 0.09 RH% per unit change in emergent light intensity can be detected.

  19. Electrical switching in sol-gel derived Ag -SiO2 nanocomposite thin films

    NASA Astrophysics Data System (ADS)

    Sarkar, D. K.; Cloutier, F.; El Khakani, M. A.

    2005-04-01

    The sol-gel technique has been used to produce Ag -SiO2 nanocomposite thin films consisting of silver nanoparticles embedded in a SiO2 matrix. The size of the silver nanoparticles is of about (4±0.2)nm when the firing temperature is in the (500-700°C ) range, as determined from ultraviolet-visible spectroscopy analysis. The increase of the firing temperature beyond 300°C, was found to lead to an outer diffusion of Ag toward the surface. As a consequence the surface atomic concentration of Ag is found to increase from 1.3% to 12% for the as-dried (at 120°C) and for those further fired at 600°C, respectively. On the other hand, it is shown that the electrical behavior of these Ag -SiO2 nanocomposite films can drastically change from highly insulating to conducting depending on the firing temperature used. In the intermediate firing temperature (300-400°C) range, the films were found to exhibit a reversible switching behavior with a resistivity transition of about 7 orders of magnitude between the insulating (OFF) and the conducting (ON) state. Such an electrical switching could be explained by a change in the predominant conduction mechanism of the films.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. Fabrications and characterizations of dye-sensitized solar cells (DSSCs) with sol-gel derived gel electrolytes

    NASA Astrophysics Data System (ADS)

    Sukmawati Arsyad, Wa Ode; Pujiarti, Herlin; Tola, Pardi Sampe; Herman, Hidayat, Rahmat

    2013-09-01

    Dye Sensitized Solar Cells (DSSCs) have been fabricated by using sol-gel derived polymer gel electrolytes incorporating imidazolium ionic liquid. Two kinds of polymer gel electrolytes have been prepared. The first one is composed of siloxane polymer only, while the second one is composed of blend of siloxane and ethylene glycol polymers. The fabricated DSSC have the same structure configuration, namely ITO/Ti:ZnO/TiO2/Ru-dye/gelelectrolyte/Pt/ITO. DSSCs with the second type of gel electrolyte were found to exhibit much better photovoltaic performance in comparison to those with the first type of gel electrolyte. This fact is in agreement with the results from impedance spectroscopy measurements, which indicate more facile charge transfer process and much smaller ionic polarizations in the cell with the second type of gel electrolyte.

  5. Investigation of bioactivity and cell effects of nano-porous sol-gel derived bioactive glass film

    NASA Astrophysics Data System (ADS)

    Ma, Zhijun; Ji, Huijiao; Hu, Xiaomeng; Teng, Yu; Zhao, Guiyun; Mo, Lijuan; Zhao, Xiaoli; Chen, Weibo; Qiu, Jianrong; Zhang, Ming

    2013-11-01

    In orthopedic surgery, bioactive glass film coating is extensively studied to improve the synthetic performance of orthopedic implants. A lot of investigations have confirmed that nano-porous structure in bioactive glasses can remarkably improve their bioactivity. Nevertheless, researches on preparation of nano-porous bioactive glasses in the form of film coating and their cell response activities are scarce. Herein, we report the preparation of nano-porous bioactive glass film on commercial glass slide based on a sol-gel technique, together with the evaluation of its in vitro bioactivity through immersion in simulated body fluid and monitoring the precipitation of apatite-like layer. Cell responses of the samples, including attachment, proliferation and osteogenic differentiation, were also investigated using BMSCS (bone marrow derived mesenchymal stem cells) as a model. The results presented here provide some basic information on structural influence of bioactive glass film on the improvement of bioactivity and cellular effects.

  6. Effects of pyrolysis conditions on dielectric properties of PLZT films derived from a polyvinylpyrrolidone-modified sol-gel process

    SciTech Connect

    Chao, Sheng; Ma, Beihai; Liu, Shanshan; Narayanan, Manoj; Balachandran, Uthamalingam

    2012-03-15

    Graphical abstract: SEM images showing the surface morphology of PLZT films derived from solutions with various PVP content and treated with either RTA (rapid thermal annealing) or SPT (step-wise preheat treatment) process. Highlights: Black-Right-Pointing-Pointer High-quality PLZT films were fabricated by using a polyvinylpyrrolidone-modified sol-gel method. Black-Right-Pointing-Pointer Improved film density and integrity was achieved by employing a novel step-wise preheat treatment (SPT) process. Black-Right-Pointing-Pointer Enhanced dielectric properties were correlated to the improved microstructures as a result of the SPT process. -- Abstract: Pb{sub 0.92}La{sub 0.08}Zr{sub 0.52}Ti{sub 0.48}O{sub 3} (PLZT) films were deposited on platinized silicon substrates (Pt/Si) using a polyvinylpyrrolidone (PVP) modified sol-gel method. Pyrolysis of the green films was conducted via two methods: rapid thermal annealing (RTA) and a step-wise preheat treatment (SPT). Microstructure analysis and dielectric property characterization were performed on samples treated by these two methods. Results showed that the SPT-pyrolyzed films exhibited much better dielectric properties when compared with the RTA-pyrolyzed films. The differences in dielectric properties were correlated to microstructural features caused by the different pyrolysis conditions. High-quality PLZT films with high dielectric constant ( Almost-Equal-To 860 at zero bias) and high breakdown strength ( Almost-Equal-To 2.1 MV/cm) were fabricated under controlled pyrolysis conditions. This work demonstrated the potential application of this material for power electronics in electric drive vehicles.

  7. In vitro bioactivity and structural features of mildly heat-treated sol-gel-derived silica fibers.

    PubMed

    Peltola, T; Jokinen, M; Veittola, S; Simola, J; Yli-Urpo, A

    2001-03-15

    The ability of sol-gel-derived silica fibers heat treated at a low temperature to induce formation of bone-like calcium phosphate (HCA) on their surfaces provides alternatives for the design of novel biomaterials, for example as implants used in tissue guiding or bone repairs. In this study, dry spinning was used to prepare the sol-gel fibers, which were heat-treated at 175 degrees and 250 degrees C. In addition, the differences in the surface topography (in a nanometer scale) of different fibers with respect to their in vitro bioactivity were studied. The structure of the fibers was varied using three different factors: (1) spinnable sols having varying structures and sizes of silica polymers to establish varying viscosity levels; (2) aging of green-state fibers; and (3) heat treatment of fibers. The in vitro bioactivity and solubility tests were done in simulated body fluid (SBF). To monitor surface topography and roughness of the heat-treated silica fibers, a scanning probe microscopy (SPM) with tapping mode AFM was used. Different fibers obtained clearly different properties. The fibers spun at about eta > 3.0 Pas had the best properties with respect to bioactivity, especially when they were heat-treated at 175 degrees C. It was found that surface structure in a nanometer scale was the most important factor controlling the in vitro bioactivity of heat-treated silica fibers. The correct proportions between the peaks and peak distances at the surfaces are suggested to be important with respect to in vitro bioactivity. The results indicate that peak distance distribution between 5-50 nm, especially between 5-20 nm, together with a peak height > or = 1 nm is most favorable for calcium phosphate formation.

  8. Drastic selectivity reversal on crown-ether based ion-sensing membranes made of ordered mesoporous silica and conventional sol-gel derived one.

    PubMed

    Yajima, Setsuko; Nakajima, Takahito; Higashi, Mariko; Kimura, Keiichi

    2010-03-21

    A crown-ether based ion sensor, in which ordered mesoporous silica was used as a membrane material, was fabricated for the first time, and drastic selectivity reversal was attained in comparison with conventional sol-gel derived membrane based on the same crown ether.

  9. Surface modification of surface sol-gel derived titanium oxide films by self-assembled monolayers (SAMs) and non-specific protein adsorption studies.

    PubMed

    Advincula, Maria; Fan, Xiaowu; Lemons, Jack; Advincula, Rigoberto

    2005-04-25

    Biological events occurring at the implant-host interface, including protein adsorption are mainly influenced by surface properties of the implant. Titanium alloys, one of the most widely used implants, has shown good biocompatibility primarily through its surface oxide. In this study, a surface sol-gel process based on the surface reaction of metal alkoxides with a hydroxylated surface was used to prepare ultrathin titanium oxide (TiOx) coatings on silicon wafers. The oxide deposited on the surface was then modified by self-assembled monolayers (SAMs) of silanes with different functional groups. Interesting surface morphology trends and protein adhesion properties of the modified titanium oxide surfaces were observed as studied by non-specific protein binding of serum albumin. The surface properties were investigated systematically using water contact angle, ellipsometry, X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM) measurements. Results showed that the surface sol-gel process predominantly formed homogeneous, but rough and porous titanium oxide layers. The protein adsorption was dependent primarily on the silane chemistry, packing of the alkyl chains (extent of van der Waals interaction), morphology (porosity and roughness), and wettability of the sol-gel oxide. Comparison was made with a thermally evaporated TiOx-Ti/Si-wafer substrate (control). This method further extends the functionalization of surface sol-gel derived TiOx layers for possible titanium alloy bioimplant surface modification.

  10. The osteogenic properties of multipotent mesenchymal stromal cells in cultures on TiO₂ sol-gel-derived biomaterial.

    PubMed

    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. 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.

  12. Temperature and Oxygen Sensing Properties of Ru(II) Covalently-Grafted Sol-Gel Derived Ormosil Hybrid Materials.

    PubMed

    Zhang, Haoran; Lei, Bingfu; Dong, Hanwu; Liu, Yingliang; Zheng, Mingtao; Xiao, Yong

    2016-04-01

    In this article, oxygen and temperature-sensing hybrid materials consisting of [Ru(Phen)3]2+ portions covalently-grafted onto the sol-gel derived ormosil network were prepared by co-condensation of tetraethoxysilane (TEOS) using n-octyltriethoxysilane as the network modifier. For comparison purposes, the hybrid materials in which [Ru(Phen)3]2+ were conventionally physically-incorporated into the matrix were also prepared. The obtained hybrid materials were characterized by Fourier transform infrared (FT-IR), luminescence intensity oxygen quenching Stern-Volmer plots, temperature quenching plots and excited-state lifetime. The near linear Stern-Volmer plots can be attributed to the approximate heterogeneous environment of the luminophore within the ormosil materials. The results reveal that the. covalently-grafted sample is more sensitive to 02, and has a higher sensing sensitivity and a higher thermal activation energy compared to the physically-incorporated one, since these Ru(II) molecules are strongly covalently-grafted onto the Si-O network via the CH2-Si bonds and less -OH group. PMID:27451760

  13. The incorporation of calix[6]arene and cyclodextrin derivatives into sol-gels for the preparation of stationary phases for gas chromatography.

    PubMed

    Delahousse, Guillaume; Peulon-Agasse, Valérie; Debray, Jean-Christophe; Vaccaro, Marie; Cravotto, Giancarlo; Jabin, Ivan; Cardinael, Pascal

    2013-11-29

    New polyethylene-glycol-based sol-gels containing cyclodextrin or calix[6]arene derivatives have been synthesized. An original method for sol-gel preparation and capillary column coating, which consumes smaller quantities of selectors and allows for control of their amounts in the stationary phase, is reported herein. The new stationary phases exhibited excellent column efficiencies over a large range of temperatures and thermal stability up to 280°C. The cyclodextrin derivative generally showed the best separation factors for aromatic positional isomers. The calix[6]arene derivative exhibited the best selectivity for the polychlorobiphenyl congeners and some polycyclic aromatic hydrocarbon isomers. The relationship between the structure and the chromatographic properties of the selectors is discussed. The tert-butyl groups on the upper rim of the calix[6]arene were found to possibly play an important role in the recognition of solutes. The incorporation of the cyclodextrin derivative into the sol-gel matrix did not affect its enantioselective recognition capabilities.

  14. The effect of heating rate on the structural and electrical properties of sol-gel derived Al-doped ZnO films

    NASA Astrophysics Data System (ADS)

    Gao, Meizhen; Wu, Xiaonan; Liu, Jing; Liu, Wenbao

    2011-05-01

    Al-doped ZnO (AZO) films are prepared by sol-gel method with a proper annealing procedure. For the first time, we find that the heating rate which is normally neglected during the post annealing process plays a significant role in improving AZO properties. The AZO film with nanorod structure is obtained by using a rapid heating rate. The AZO nanorods can provide a faster conduction pathway for charge transport due to the high crystal quality and thus enhance the conductivity of the film significantly. After hydrogen treatment, the AZO nanorod film exhibits a minimum resistivity of 1.4 × 10 -3 Ω cm. This approach to the preparation of AZO nanorods by a simple rapid annealing process may be helpful for the development of sol-gel-derived TCO films.

  15. The effect of post annealing treatment on the citrate sol-gel derived nanocrystalline BaFe12O19 powder: structural, morphological, optical and magnetic properties

    NASA Astrophysics Data System (ADS)

    Brightlin, B. C.; Balamurugan, S.

    2016-05-01

    The nanocrystalline BaFe12O19 powders were obtained from citrate sol-gel combustion-derived powder upon annealing at 800-1100 °C, and explored their structural, micro-structural, optical and magnetic properties. The thermal decomposition of citrate sol-gel combustion product was verified by means of thermogravimetric and differential thermal analysis. Structural identification of the citrate sol-gel combustion powder and annealed samples were investigated by powder X-ray diffraction. Though the combustion product exhibits cubic spinel phase material, the annealed powder yields good quality nanocrystalline hexagonal BaFe12O19 phase materials. The thin plate-like flakes morphology with random particle sizes of ~100-200 nm with slightly agglomerated particles of BaFe12O19 phase is analyzed by high resolution scanning electron microscopy for the good quality annealed sample. Photoluminescence emission spectrum of BaFe12O19 material reveals broad emission peak at ~360 nm under the excitation wavelength of 270 nm. Interestingly, the near infrared relative reflectivity of the nanocrystalline BaFe12O19 materials obtained by citrate sol-gel synthesis method is higher than the nanocrystalline BaFe12O19 materials obtained by mechano-thermal and co-precipitation method. The present dark brown colored BaFe12O19 materials can be applied as a ceramic color pigment which includes several applications. The room temperature magnetic hysteresis loop of the annealed BaFe12O19 sample exhibits a ferromagnetic saturation magnetization, M s of 55.774 emu/g at 15 kOe.

  16. 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.

  17. Voltammetric sensor for barbituric acid based on a sol-gel derivated molecularly imprinted polymer brush grafted to graphite electrode.

    PubMed

    Patel, Amit Kumar; Sharma, Piyush Sindhu; Prasad, Bhim Bali

    2009-04-17

    A voltammetric sensor based on a molecularly imprinted polymer (MIP) brush grafted to sol-gel film on graphite electrode is reported for the selective and sensitive analysis of barbituric acid (BA) in aqueous, blood plasma, and urine samples. The modified electrode was preanodised at +1.6 V (vs. saturated calomel electrode), where encapsulated BA involved hydrophobically induced hydrogen bondings, in MIP cavities exposed at the film/solution interface, at pH 7.0. Scanning electron microscopy (SEM) was employed to characterise the surface morphology of the resultant imprinted film of MIP brush. The differential pulse, cathodic stripping voltammetry (DPCSV) technique was employed to investigate the binding performance of the sol-gel-modified imprinted polymer brush, which yielded a linear response in the range of 4.95-100.00 microg mL(-1) of BA with a detection limit of 1.6 microg mL(-1) (S/N=3). PMID:19135515

  18. Evaluating interface strength of calcium phosphate sol-gel-derived thin films to Ti6Al4V substrate.

    PubMed

    Gan, Lu; Wang, Jian; Pilliar, Robert M

    2005-01-01

    The interface shear strength of Ca-P thin films applied to Ti6Al4V substrates have been evaluated in this study using a substrate straining method--a shear lag model. The Ca-P films were synthesized using sol-gel methods from either an inorganic or organic precursor solution. Strong interface bonding was demonstrated for both film types. The films were identified as non-stoichiometric hydroxyapatite but with different Ca/P ratios. The Ca-P films were 1-1.5 microm thick and testing and analysis using the shear lag approach revealed a shear strength of approximately 347 and 280 MPa for Inorganic and Organic Route-formed films, respectively. Overall, the exceptional mechanical properties of Ca-P/Ti6Al4V system along with the inherent advantages of sol-gel processing support continued studies to utilize this technology for bone-interfacing implant surface modification. PMID:15207465

  19. 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.

  20. 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.

  1. Examination of the haemolytic activity of sol-gel materials

    NASA Astrophysics Data System (ADS)

    Ulatowska-Jarza, Agnieszka; Podbielska, Halina; Holowacz, Iwona; Lechna-Marczynska, Monika I.; Szymonowicz, Maria; Staniszewska-Kus, Jolanta; Paluch, Danuta

    2001-10-01

    Recently, the sol-gel based biomaterials are extendedly investigated with emphasis on theirs various applications, including medical ones. In this respect it is important to investigate the influence of sol-gel matrices on biological systems. The results of laboratory and biological testing of aqueous extracts of sol-gels are presented in this work. It was proved that it is possible to produce the sol-gel derived materials that will be non-haemolytic. This can be achieved by heating the materials in elevated temperatures. This effect can also be reached by suitably long aging (minimum 6 months).

  2. 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

  3. In situ real-time investigation of kinetics of nucleation and growth of sol-gel-derived functional oxide thin films

    NASA Astrophysics Data System (ADS)

    Sun, Tao; Hu, Hao; Pan, Zixiao; Li, Xuefa; Wang, Jin; Dravid, Vinayak P.

    2008-05-01

    Early-stage nucleation and growth kinetics of sol-gel-derived multiferroic BiFeO3 thin films were investigated in situ and in real time by combining transmission electron microscopy and grazing-incidence small-angle x-ray scattering (GISAXS). While the initial phase of the nuclei was identified to be Bi2O2CO3 , the quantitative GISAXS analysis unambiguously revealed that the early-stage kinetic nucleation growth in the thin films was dominated by an oriented-attachment mechanism as opposed to the conventional Ostwald ripening in metallic and ceramic systems.

  4. 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.

  5. 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.

  6. Nanocrystal/sol-gel nanocomposites

    DOEpatents

    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

  7. 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.

  8. 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.

  9. 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. PMID:26364089

  10. In situ formation of silver nanostructures produced via laser irradiation within sol-gel derived films and their interaction with a fluorescence tagged protein.

    PubMed

    Hungerford, Graham; Toury, Marion; McLoskey, David; Finnigan, Scott; Gellie, Shaun; Holmes-Smith, A Sheila

    2010-11-28

    The presence of a conducting metal surface is known to affect the emission of a fluorophore in its proximity. This can lead to an enhancement in its fluorescence intensity along with a decrease in the fluorescence lifetime. This phenomenon, sometimes known as metal enhanced fluorescence, has implications in the area of sensing and "lab on a chip" applications. Here controlled, localised use of metallic structures can be advantageous in enhancing the detection of a fluorescent signal. The sol-gel technique has been demonstrated as a useful method by which to produce a biocompatible material. The versatility of the reaction allows for the inclusion of metal ions, which can form metallic nanostructures permitting the potential enhancement of fluorescence to be exhibited. In this work we incorporate silver nitrate within silica sol-gel derived films produced using a simple procedure at relative low temperatures (close to ambient). A compact time-resolved fluorescence microscope equipped with a semiconductor laser was used to photoactivate the silver ions to form localised metallic structures within the films. Patterning was achieved by computer control of the microscope stage and using the laser in CW mode. The films were characterised using AFM and UV-vis spectroscopy to ascertain the presence of the photoactivated silver nanostructures. The effect of the presence of these structures was elucidated by studying the time-resolved fluorescence of FITC labelled bovine serum albumin adsorbed to the films, where a decrease in the lifetime of the FITC label was observed in the location of the nanostructures.

  11. Room-temperature sol-gel derived molybdenum oxide thin films for efficient and stable solution-processed organic light-emitting diodes.

    PubMed

    Fu, Qiang; Chen, Jiangshan; Shi, Changsheng; Ma, Dongge

    2013-07-10

    Molybdenum oxide (MoO3) thin films were prepared by sol-gel methods at room temperature from the precursors of MoO3 powder mixing into NH3 or H2O2 solution and then directly treated by UV-ozone instead of widely used high-temperature annealing. Atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and ultraviolet photoelectron spectroscopy (UPS) characteristics demonstrated that the room-temperature sol-gel derived MoO3 thin films exhibited excellent uniformity, unchanged chemical structure, and high work function. For the first time, the novel solution-processed MoO3 thin films were successfully applied as the hole injection layers (HILs) for solution-processed organic light-emitting diodes (OLEDs). The efficiencies of the resulting OLEDs were comparable or even higher than that of the device using PEDOT:PSS as the HIL. More importantly, the lifetimes of the solution-processed OLEDs are improved by nearly 2 orders of magnitude. This study should provide a potential approach to develop low-cost, high-performance, and long-lifetime OLEDs for practical applications. PMID:23692351

  12. 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.

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

    SciTech Connect

    Shanmugham, S.; Liaw, P.K.

    1996-10-01

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

  14. Electroassisted codeposition of sol-gel derived silica nanocomposite directs the fabrication of coral-like nanostructured porous gold.

    PubMed

    Farghaly, Ahmed A; Collinson, Maryanne M

    2014-05-13

    Herein, we report on a one-step coelectrodeposition method to form gold-silica nanocomposite materials from which high surface area nanostructured gold electrodes can be produced. The as-prepared Au-SiO2 films possess an interconnected three-dimensional porous framework with different silica-gold ratios depending on the deposition solutions and parameters. Chemical etching of the nanocomposite films using hydrofluoric acid resulted in the formation of nanostructured porous gold films with coral-like structures and pores in the nanometer range. The cross-linkage of the gold coral branches resulted in the generation of a porous framework. X-ray photoelectron spectroscopy confirms the complete removal of silica. Well-controlled surface area enhancement, film thickness, and morphology were achieved by manipulating the deposition parameters, such as potential, time, and gold ion and sol-gel monomer concentrations in the deposition solution. An enhancement in the surface area of the electrode up to 57 times relative to the geometric area has been achieved. The thickness of the as-prepared Au-SiO2 nanocomposite films is relatively high and varied from 8 to 15 μm by varying the applied deposition potential while the thickness of the coral-like nanostructured porous gold films ranged from 0.22 to 2.25 μm. A critical sol-gel monomer concentration (CSGC) was determined at which the deposited silica around the gold coral was able to stabilize the coral-like gold nanostructures, while below the CSGC, the coral-like gold nanostructures were unstable and the surface area of the nanostructured porous gold electrodes decreased. PMID:24766096

  15. Field-induced phase switching and electrically driven strains in sol-gel derived antiferroelectric (Pb,Nb)(Zr,Sn,Ti)O{sub 3} thin layers

    SciTech Connect

    Sengupta, S.S.; Roberts, D.; Li, J.; Kim, M.C.; Payne, D.A.

    1995-07-15

    Tin-modified lead zirconate titanate thin layers were prepared by a sol-gel method. A room- temperature antiferroelectric (AFE) phase composition Pb{sub 0.99}Nb{sub 0.02}[(Zr{sub 0.58}Sn{sub 0.42}){sub 0.96}Ti{sub 0.04}] {sub 0.98}O{sub 3} was prepared and examined for weak- and high-field dielectric properties as a function of temperature, with emphasis on field-induced AFE-ferroelectric (FE) switching characteristics. Thin layers processed with a lead oxide cover coat were found to be free of any secondary phases and showed improved properties. Room-temperature values of dielectric constant {ital K}{prime}=390 and saturation polarization {ital P}{sub {ital s}}=20 {mu}C/cm{sup 2} were obtained with field-induced strains up to 0.15% in submicron grain structures. {copyright} {ital 1995} {ital American} {ital Institute} {ital of} {ital Physics}.

  16. 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. PMID:26369040

  17. 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.

  18. Structural characterization and magnetic properties of sol-gel derived ZnxFe3-xO4 nanoparticles

    NASA Astrophysics Data System (ADS)

    Petrova, E.; Kotsikau, D.; Pankov, V.

    2015-03-01

    Nanocrystalline ZnxFe3-xO4 solid solutions (with x=0, 0.18, 0.45, 1) with crystallite sizes of 5-10 nm, specific surface of about 180 m2/g were synthesized via an inorganic variant of the sol-gel approach. The composition and structure of the formed nanoparticles were examined with the help of powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma atomic emission spectrometry and Fourier transform infrared spectroscopy. Hysteresis loops recorded for the samples indicate their ferromagnetic behavior at 5 K and superparamagnetic behavior at 300 K. The highest maximum magnetization of 59 emu/g at room temperature corresponds to Zn0.18Fe2.82O4 composition, and at 5 K to Zn0.45Fe2.55O4 (86 emu/g). The saturation magnetization of the pure magnetite was measured to be respectively 62 and 49 emu/g.

  19. Sol-gel derived Al-Ga co-doped transparent conducting oxide ZnO thin films

    NASA Astrophysics Data System (ADS)

    Serrao, Felcy Jyothi; Sandeep, K. M.; Bhat, Shreesha; Dharmaprakash, S. M.

    2016-05-01

    Transparent conducting ZnO doped with Al, Ga and co-doped Al and Ga (1:1) (AGZO) thin films were grown on glass substrates by cost effective sol-gel spin coating method. The XRD results showed that all the films are polycrystalline in nature and highly textured along the (002) plane. Enhanced grain size was observed in the case of AGZO thin films. The transmittance of all the films was more than 83% in the visible region of light. The electrical properties such as carrier concentration and mobility values are increased in case of AGZO compared to that of Al and Ga doped ZnO thin films. The minimum resistivity of 2.54 × 10-3 Ω cm was observed in AGZO thin film. The co-doped AGZO thin films exhibited minimum resistivity and high optical transmittance, indicate that co-doped ZnO thin films could be used in transparent electronics mainly in display applications.

  20. 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.

  1. Photocatalytic reduction of carbon dioxide using sol-gel derived titania-supported CoPc catalysts.

    PubMed

    Liu, Shaohua; Zhao, Zhihuan; Wang, Zhizhong

    2007-06-01

    CoPc loaded titania was synthesized by an improved sol-gel method using a homogeneous hydrolysis technique. The grain size of TiO2 and CoPc-TiO2 was uniform and average diameters were less than 20 nm. Both catalysts had two crystal phases, of which rutile accounted for about 28%. When they were used for the photoreduction of CO2 in NaOH solution under ambient conditions, the formate yield was significantly higher than that of the others, such as formaldehyde, methanol and so on. In order to increase the activity of the photocatalysts some factors were optimized, including the quantity of CoPc-TiO2 catalyst, concentration of Na(2)SO(3) hole scavenger, concentration of the NaOH solution and irradiation time. Under the optimal conditions, the gross photocatalytic reduction of CO2 was 1032 micromol (g cat)(-1). Furthermore, the yield of CH4 did not increase in the presence of CH(3)OH or HCHO, showing that the generation of CH4 from CO2 did not proceed via methanol as an intermediate under these conditions.

  2. Nano-quantum size effect in sol-gel derived mesoporous titania layers deposited on soda-lime glass substrate

    NASA Astrophysics Data System (ADS)

    Gondek, Ewa; Karasiński, Paweł; Drewniak, Sabina

    2014-08-01

    The TiO2 nanolayers were fabricated on soda-lime glass substrates with the application of sol-gel method and dip-coating technique. In the fabricated TiO2 layers, the quantum size effect can be observed. For the sake of comparison, we investigated also the TiO2 nanolayers fabricated on soda-lime glass substrates with a buffer silica layer. The fabricated layers were investigated with the application of optical measurement techniques and atomic force microscopy. The widths of energy gap and Urbach energy were determined. The diffusion of sodium ions Na+ from the glass substrate to the TiO2 layer brings about the non-monotonic dependence of the energy band gap on the thickness of TiO2 layer. In the TiO2 layers fabricated on soda-lime glass substrates pre-coated with a SiO2 layer, the influence of silicon ions on the direct energy band gap was found.

  3. 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. PMID:27612779

  4. Effect of the excimer laser irradiation on sol-gel derived tungsten-titanium dioxide thin films

    NASA Astrophysics Data System (ADS)

    Joya, Yasir F.; Liu, Zhu

    2011-01-01

    A novel technique based on the excimer laser induced crystallization and modification of TiO2 thin films is being reported. W+6 ions loaded TiO2 (WTO) precursor films were prepared by a modified sol-gel method and spin-coated onto microscopic glass slides. Pulsed KrF (248 nm, 13 ns) excimer laser was used to irradiate the WTO amorphous films at various laser parameters. Mesoporous and nanostructured films consisting of anatase and rutile were obtained after laser irradiation at room temperature. The effect of varying W+6 ions concentrations on structural and optical properties the WTO films was analyzed by X-ray diffraction, field-emission scanning electron microscope, UV-Vis spectrophotometer and transmission electron microscope before and after laser treatment. Films irradiated for 10 pulses at 65-75 mJ/cm2 laser fluence, exhibited anatase whereas higher parameters promoted the formation of rutile. XPS results revealed WO3 along with minor proportion of WO2 compounds after laser irradiation. Photo-absorbance of the WTO films was increased with increase in W+6 ions concentration in the film. TEM results exhibited a crystallite size of 15 nm which was confirmed from SEM results as well.

  5. Design and Simulation of 2×2 MMI Coupler and Thermo-optic Switch Using Sol-Gel Derived Organic-Inorganic Hybrid Material

    NASA Astrophysics Data System (ADS)

    Samah, M. Firdaus A.; Nawabjan, Amirjan; Abdullah, Ahmad Sharmi; Ibrahim, Mohd Haniff; Kassim, Norazan Mohd; Mohamad, Abu Bakar

    2011-05-01

    A new design of Multimode Interference (MMI) thermo-optic switch with improved crosstalk figure is demonstrated in this paper. The device is designed and simulated using BeamProp 3D from Rsoft and 3D BPM CAD softwares. The devices are designed based on sol-gel derived organic-inorganic hybrid material, vinyltriethoxysilane (VTES), tetraethoxysilane (TEOS) and tetrabutoxytitanate (TTBu) or VTT with refractive index of 1.47 as a core and surrounded by silica with refractive index of 1.45 at 1550 nm wavelength. The switching power is 164mW and the simulation result show that the propagation loss of the MMI device is 1.8 dB and zero crosstalk.

  6. 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.

  7. Influence of sol and stage of spinnability on in vitro bioactivity and dissolution of sol-gel-derived SiO2 fibers.

    PubMed

    Peltola, T; Jokinen, M; Veittola, S; Rahiala, H; Yli-Urpo, A

    2001-03-01

    The ability of the sol-gel-derived green state silica fibers to induce the formation of bone-like calcium phosphate (HCA) on their surfaces has not been studied earlier. Bioactive silica fibers provide alternatives for the design of novel products, e.g., as implants used in tissue guiding or bone repairs. In this study, dry spinning was used to prepare the sol-gel fibers. Different fibers with different bulk structures were prepared by changing the composition and controlling the stage of spinnability. Additionally, the influence of the aging time of the fibers on the bulk structure of the samples was investigated. Furthermore, the ability to form calcium phosphate was investigated in vitro in the simulated body fluid (SBF). Transmission electron microscopy was used to illustrate the bulk structure of the green state fibers and scanning electron microscopy to illustrate the formed calcium phosphate layer on the fibers. The fibers were additionally characterized by measuring the dissolution of the silica in the SBF. In vitro bioactive silica fibers were successfully prepared. The calcium phosphate layer was formed within 1-5 days in the best case. The structural stability and the in vitro bioactivity varied with the aging time expect in one case where practically stable fibers could be prepared. The concentration of silica released in the SBF had no direct connection with the HCA formation. The silica-rich gel layer was not observed on the fibers, but the structure of the fibers was suggested to have an important role in the HCA formation.

  8. 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.

  9. Dielectric and ferroelectric properties of Ba(Sn{sub 0.15}Ti{sub 0.85})O{sub 3} thin films grown by a sol-gel process

    SciTech Connect

    Zhai Jiwei; Shen Bo; Yao Xi; Zhang Liangying

    2004-09-01

    Ferroelectric Ba(Sn{sub 0.15}Ti{sub 0.85})O{sub 3} (BTS) thin films were deposited on LaNiO{sub 3}-coated silicon substrates via a sol-gel process. Films showed a strong (1 0 0) preferred orientation depending upon annealing temperature and concentration of the precursor solution. The dependence of dielectric and ferroelectric properties on film orientation has been studied. The leakage current density of thin films at 100 kV/cm was 7 x 10{sup -7} A/cm{sup 2} and 5 x 10{sup -5} A/cm{sup 2} and their capacitor tunability was 54 and 25% at an applied field of 200 kV/cm (measurement frequency of 1 MHz) for the thin films deposited with 0.1 and 0.4 M spin-on solution, respectively. This work clearly reveals the highly promising potential of BTS compared with BST films for application in tunable microwave devices.

  10. 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

  11. 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

  12. Novel carboxy functionalized sol-gel precursors

    SciTech Connect

    Wolter, H.; Storch, W.; Gellermann, C.

    1996-12-31

    A novel family of inorganic-organic copolymers (ORMOCER`s) derived from urethane- and thioether(meth)acrylate alkoxysilanes has been successfully exploited for a variety of diverse applications. In order to widen the range of applications an additional functionality (carboxy group) has been incorporated int his silane type. Conventional sol-gel processing facilitates the formation of an inorganic Si-O-Si-network via hydrolysis and polycondensation reactions of alkoxysilyl moieties and in addition, the (meth)acrylate groups are available for radically induced polymerization to obtain a complementary organic polymer structure. The presence of a carboxy group would appear to have great potential for a range of diverse areas of application, such as an internal catalyst for the sol-gel process, complexation of elements such as Zr and Ti, increasing the adhesion to various substrates and modification of solubility. A number of novel silanes and their syntheses will be described in this paper.

  13. Sol-gel derived bioactive glasses with low tendency to crystallize: synthesis, post-sintering bioactivity and possible application for the production of porous scaffolds.

    PubMed

    Bellucci, Devis; Sola, Antonella; Salvatori, Roberta; Anesi, Alexandre; Chiarini, Luigi; Cannillo, Valeria

    2014-10-01

    A new sol-gel (SG) method is proposed to produce special bioactive glasses (BG_Ca family) characterized by a low tendency to devitrify. These formulations, derived from 45S5 Bioglass®, are characterized by a high content of CaO (45.6 mol%) and by a partial or complete substitution of sodium oxide with potassium oxide (total amount of alkaline oxides: 4.6 mol%), which increases the crystallization temperature up to 900°C. In this way, it is possible to produce them by SG preserving their amorphous nature, in spite of the calcination at 850°C. The sintering behavior of the obtained SG powders is thoroughly investigated and the properties of the sintered bodies are compared to those of the melt-derived (M) counterparts. Furthermore, the SG glass powders are successfully used to produce scaffolds by means of a modified replication technique based on the combined use of polyurethane sponges and polyethylene particles. Finally, in the view of a potential application for bone tissue engineering, the cytotoxicity of the produced materials is evaluated in vitro. PMID:25175252

  14. 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.

  15. Self-reinforcement and hydrolytic degradation of amorphous lactic acid based poly(ester-amide), and of its composite with sol-gel derived fibers.

    PubMed

    Haltia, Anna-Maija; Lähteenkorva, Kimmo; Törmälä, Pertti; Helminen, Antti; Tuominen, Jukka; Seppälä, Jukka; Veittola, Sinikka; Ahvenlammi, Jarno

    2002-10-01

    The self-reinforcing and hydrolytic degradation of an amorphous poly(ester-amide) (PEA) based on lactic acid have been studied and compared with those of poly-L-lactide (PLLA). The studied PEA-rods were self-reinforced (SR) by solid-state die drawing resulting double shear strength. The hydrolytic degradation of PEA was studied during exposure to phosphate buffered saline at pH 7.4 and at 37 degrees C for 18 weeks. The degradation and mechanical properties of PEA were also followed in a self-reinforced composite structure consisting of PEA and sol-gel derived SiO(2)-fibers (SGF, 8 wt %). The hydrolytic degradation of the SR-PEA-rods with and without SG-fibers was significantly faster than that of SR-PLLA-rods. The weight average molecular weight (Mw) of PEA decreased by 90% from the initial Mw during the first 6 weeks in hydrolysis, when the Mw of the PLLA decreased by 10%. PMID:15348182

  16. 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.

  17. Effect of sol-gel pH on XRD peak broadening, lattice strain, ferroelectric domain orientation, and optical bandgap of nanocrystalline Pb1.1(Zr0.52Ti0.48)O3

    NASA Astrophysics Data System (ADS)

    Pakizeh, E.; Moradi, M.; Ahmadi, A.

    2014-02-01

    Nanocrystalline Pb1.1(Zr0.52Ti0.48)O3 (PZT) samples were prepared using a citrate-nitrate sol-gel process near the morphotropic phase boundary. The effect of pH on the lattice parameters (tetragonality and lattice constants), crystal structure [strain broadening, relative phase content, ferroelectric domain (FD) orientation and nanocrystallite size], microstructure (grain size and particle morphology) and optical bandgap was investigated. The samples were characterized using X-ray diffraction (XRD), the size strain plot (SSP) method, Fourier-transform infrared spectroscopy, and the classical Tauc relation. The particle morphology was investigated using field-emission scanning electron microscopy. The XRD results revealed a perovskite structure and coexisting tetragonal and rhombohedral phases for all PZT samples. Lattice strain and peak broadening were determined from SSP and XRD results. The behavior of these parameters was in agreement for all pH values. The optical bandgap for PZT was estimated from UV-vis absorption spectra. We found that for PZT the maximum relative tetragonal phase content, c/a ratio, and FD orientation along the a-axis occurred at pH 4.

  18. Residual stress development and effect on the piezoelectric performance of sol-gel derived lead zirconate titanate (PZT) thin films

    NASA Astrophysics Data System (ADS)

    Berfield, Thomas A.

    Ferroelectric thin films have higher energy densities, larger strain capabilities and more rapid response times than their bulk counterparts. Typical applications include micro-actuators, micro-sensors and ultrasonic motors for MEMs applications, as well as, nonvolatile computer memories and switching capacitors for integrated circuitry. The electro-mechanical performance of ceramic thin films is greatly influenced by many factors, including grain size, orientation, film thickness, and residual stress level. Residual stresses which arise during the various processing phases of thin film manufacturing can be quite high due to substantial mismatches in substrate-film thermal properties, intrinsic sources (such as grain boundary interactions, etc.), and other external factors. This dissertation examines the relationship between field-induced displacement response and residual stress level for lead zirconate-titanate (PZT) thin films. The film piezoelectric properties are characterized via interferometric measurements for two different loading cases, while the residual stress is determined experimentally from wafer curvature measurements. Additionally two patterning methods, traditional chemical wet-etching and a novel soft lithographic technique, are explored as a means to reduce residual stress within film features. For the soft lithographic technique, film features are created by selective film cracking, a result of poor substrate adhesion promoted by a mediated, self-assembled monolayer. Wafer curvature stress measurements and DIC-based strain measurements of mediated monolayer patterned features reveal that the in-plane stress/strain development is reduced compared to the blanket film case. Critical in-plane strains at crack initiation are also measured using a new digital image correlation technique, in which fluorescent nanoparticles (c.a. 140 nm) provide the speckle pattern. A corresponding increase in the field induced displacements is observed for the film

  19. Comparisons between surfactant-templated mesoporous and conventional sol-gel-derived CaO-B{sub 2}O{sub 3}-SiO{sub 2} glasses: Compositional, textural and in vitro bioactive properties

    SciTech Connect

    Xiu Tongping; Liu Qian Wang Jiacheng

    2008-04-15

    Compositional, textural and in vitro bioactive comparisons between surfactant-templated mesoporous (MCBS) and conventional sol-gel-derived CaO-B{sub 2}O{sub 3}-SiO{sub 2} (CBS) glasses are studied in this paper. CBS glasses are heterogeneous in composition. Due to the heterogeneity, melting boron oxide that formed during the heat treatment will fill in the pores that should have been generated by decomposition of calcium species. So, unlike other conventional sol-gel-derived bioactive glasses that have disordered and widely distributed mesopores, the CBS glasses are almost nonporous. MCBS glasses are more homogeneous in composition than CBS glasses, mainly ascribed to the effect of the surfactant. MCBS glasses of different compositions possess wormhole-like mesoporous structure and have similar pore size. In vitro bioactive tests show that wormhole-like MCBS glasses are more bioactive than CBS glasses, due to their high porosity. - Graphical abstract: Surfactant-templated mesoporous CaO-B{sub 2}O{sub 3}-SiO{sub 2} glasses (MCBS) are superior to conventional sol-gel-derived CaO-B{sub 2}O{sub 3}-SiO{sub 2} glasses (CBS) in compositional homogeneity, textural properties and in vitro bioactivity. Display Omitted.

  20. 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.

  1. Effect of aging time of sol on structure and in vitro calcium phosphate formation of sol-gel-derived titania films.

    PubMed

    Peltola, T; Jokinen, M; Rahiala, H; Pätsi, M; Heikkilä, J; Kangasniemi, I; Yli-Urpo, A

    2000-08-01

    Titanium and its alloys have been used successfully in the manufacture of orthopedic and dental implants to replace damaged bone tissue. In this study, different sol-gel-derived TiO(2) coatings were produced on titanium substrates using different aging times (5, 10, 24, or 48 h) of the sol before dipping the coatings and varying numbers (one, three, or five) of coating layers. The influence of the aging time of the sol on the structure of the titania coatings with respect to in vitro bioactivity was investigated. The in vitro bioactivity tests were done in a simulated body fluid (SBF). The sol properties were monitored using a capillary viscometer and dynamic light scattering to determine the viscosity and particle size, respectively. The topography of the films was characterized using atomic force microscopy. The various sol aging times and numbers of layers produced differences in the topography of the titania films. For the coatings with one and three layers, the aging of the sols had an influence on the height of the peaks (lower with longer aging times) although the peak distance was about the same. The number of coating layers had a stronger influence. The distribution of the peak distances became narrower with an increasing number of coating layers. The coating with three layers (top coating prepared after 24 h of sol aging) and the coatings with five layers had a similar distribution of peak distances (15-50 nm), which was favorable for calcium phosphate formation. On these substrates, calcium phosphate formation started within 3-6 days of immersion in SBF. The aging time of the titania sol and the number of coating layers were found to have a strong influence on the surface topography in the nanometer scale of the titania films. The results indicate that the topography of the outermost surface is of importance for in vitro bioactivity.

  2. 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.

  3. 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.

  4. 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.

  5. Passive and active sol-gel materials and devices

    NASA Astrophysics Data System (ADS)

    Andrews, Mark P.; Najafi, S. Iraj

    1997-07-01

    This paper examines sol-gel materials for photonics in terms of partnerships with other material contenders for processing optical devices. The discussion in four sections identifies semiconductors, amorphous and crystalline inorganic dielectrics, and amorphous and crystalline organic dielectrics as strategic agents in the rapidly evolving area of materials and devices for data communications and telecommunications. With Zyss, we trace the hierarchical lineage that connects molecular hybridization (chemical functionality), through supramolecular hybridization (collective properties and responses), to functional hybridization (device and system level constructs). These three concepts thread their way through discussions of the roles sol-gel glasses might be anticipated to assume in a photonics marketplace. We assign a special place to glass integrated optics and show how high temperature consolidated sol-gel derived glasses fit into competitive glass fabrication technologies. Low temperature hybrid sol-gel glasses that combine attractive features of organic polymers and inorganic glasses are considered by drawing on examples of our own new processes for fabricating couplers, power splitters, waveguides and gratings by combining chemical synthesis and sol-gel processing with simple photomask techniques.

  6. Ferroelectricity in corundum derivatives

    NASA Astrophysics Data System (ADS)

    Ye, Meng; Vanderbilt, David

    2016-04-01

    The search for new ferroelectric (FE) materials holds promise for broadening our understanding of FE mechanisms and extending the range of application of FE materials. Here we investigate a class of A B O3 and A2B B'O6 materials that can be derived from the X2O3 corundum structure by mixing two or three ordered cations on the X site. Most such corundum derivatives have a polar structure, but it is unclear whether the polarization is reversible, which is a requirement for a FE material. In this paper, we propose a method to study the FE reversal path of materials in the corundum derivative family. We first categorize the corundum derivatives into four classes and show that only two of these allow for the possibility of FE reversal. We then calculate the energy profile and energy barrier of the FE reversal path using first-principles density functional methods with a structural constraint. Furthermore, we identify several empirical measures that can provide a rule of thumb for estimating the energy barriers. Finally, the conditions under which the magnetic ordering is compatible with ferroelectricity are determined. These results lead us to predict several potentially new FE materials.

  7. Strong magnetoelectric coupling in sol-gel derived multiferroic (Pb0.76Ca0.24)TiO3-CoFe2O4 composite films

    NASA Astrophysics Data System (ADS)

    Cheng, T. D.; Tang, X. G.; Wang, Yu; Chan, H. L. W.

    2012-10-01

    A multilayer heterostructure composite thin films consisting of alternating layers (Pb0.76Ca0.24)TiO3 (PCT) and CoFe2O4 (CFO) were grown on Pt/Ti/SiO2/Si(100) substrate by a sol-gel process. X-ray measurements indicated high quality of crystallization of both PCT and CFO layers. The magnetic and ferroelectric properties of the composite were investigated. Well-defined polarization vs. electric field (P-E) and magnetic hysteresis (M-H) loops were obtained. A strong magnetoelectric (ME) response was observed in the sample which was subjected to an alternating magnetic field, and a high ME voltage coefficient αE = 870 mV/Oe cm was obtained for the composite thin films when applied magnetic field parallel to the sample plane.

  8. [Biological tests of sol-gel biomaterials].

    PubMed

    Ulatowska-Jarza, A; Podbielska, H; Szymonowicz, M; Staniszewska-Kuś, J; Paluch, D

    2000-01-01

    Recently, the sol-gel based biomaterials are extendedly investigated in emphasis on theirs medical applications. In this respect it is important to investigate the influence of sol-gel matrices on biological systems. The results of laboratory and biological testing of water extracts of sol-gels are presented in this work. It was proved that it is possible to construct the sol-gels that are not cytotoxic for which the haemolytic reactions fulfils the foreseen norms. This can be achieved by heating the materials in certain temperatures (higher than 350 degrees C). This effect can also be reached by suitably long aging (minimum 6 months).

  9. 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.

  10. 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.

  11. 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.

  12. Enhanced self-repairing capability of sol-gel derived SrTiO3/nano Al2O3 composite films

    NASA Astrophysics Data System (ADS)

    Yao, Manwen; Peng, Yong; Xiao, Ruihua; Li, Qiuxia; Yao, Xi

    2016-08-01

    SrTiO3/nano Al2O3 inorganic nanocomposites were prepared by using a conventional sol-gel spin coating process. For comparison, SrTiO3 films doped by equivalent amount of sol-Al2O3 have also been investigated. Aluminum deposited by using vacuum evaporation was used as the top electrode. The nanocomposites exhibited a significantly enhanced dielectric strength of 506.9 MV/m, which was increased by 97.4% as compared with the SrTiO3 films doped with sol-Al2O3. The leakage current maintained of the same order of microampere until the ultimate breakdown of the nanocomposites. The excellent electrical performances are ascribed to the anodic oxidation reaction in origin, which can repair the internal and/or surface defects of the films.

  13. 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.

  14. 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. PMID:26373362

  15. 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.

  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. 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.

  18. Sol-gel-based poliovirus-1 detector.

    PubMed

    Zolkov, Chen; Avnir, David; Armon, Robert

    2009-02-01

    Hybrid sol-gel films were used to grow Buffalo Green Monkey kidney cell tissues, which were used for poliovirus-1 detection. It is shown that the sol-gel approach allows cutting the standard EPA procedure from 48 to 24h of detection time; that better visualization of the plaques is obtained; that a variety of stains, including fluorescence, can be used; and that the shelf life of the resulting plaques system is well over a year.

  19. Sol/gel transition of chitosan solutions.

    PubMed

    Rwei, S P; Chen, T Y; Cheng, Y Y

    2005-01-01

    This work studies the occurrence of sol/gel transition and the gel rheology for chitosan solution under various conditions. Experiments were conducted in an oscillatory shear apparatus with small amplitude, using a Rheometrics SR-5 rheometer, with Couette and parallel plate geometries. The experimental results demonstrate that the sol/gel transition concentration and the elastic modulus (G') for CS gel decrease as the pH value and the molecular weight (Mw) increase. However, the sol/gel transition concentration and G' became independent of Mw when Mw exceeded a threshold. The higher ionization constant, Kp, is responsible for the higher sol/gel transition concentration in a formic acid solution than in an acetic acid solution with equivalent molar concentration. The elastic modulus G' of a CS gel increases with temperature, which relationship differs from that for many polysaccharides, and can be understood through classical rubber elastic theory. Finally, a gel whose concentration was barely above the sol/gel point exhibited aging, and its G' and G" declined rather than increase with time, accompanied by a reversal from the sol/gel state back to the sol state. This is an uncommon aging behavior for a polysaccharide and a detailed explanation is provided.

  20. 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.

  1. 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

  2. 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

  3. 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.

  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. Microwave sol-gel derived NaCaGd(MoO4)3:Er3+/Yb3+ phosphors and their upconversion photoluminescence properties

    NASA Astrophysics Data System (ADS)

    Lim, Chang Sung

    2016-05-01

    Ternary molybdate NaCaGd1-x(MoO4)3:Er3+/Yb3+ phosphors with the proper doping concentrations of Er3+ and Yb3+ (x = Er3+ + Yb3+, Er3+ = 0, 0.05, 0.1, 0.2 and Yb3+ = 0, 0.2, 0.45) were successfully synthesized by microwave sol-gel method for the first time. Well-crystallized particles formed after heat-treatment at 900 °C for 16 h showed a fine and homogeneous morphology with particle sizes of 3-5 μm. The optical properties were examined comparatively using photoluminescence emission and Raman spectroscopy. Under excitation at 980 nm, the doped particles exhibited a strong 525-nm emission band, a weak 550-nm emission band in the green region, which correspond to the 2H11/2 → 4I15/2 and 4S3/2 → 4I15/2 transitions, and a very weak 655-nm emission band in the red region, which corresponds to the 4F9/2 → 4I15/2 transition. The optimal Yb3+:Er3+ ratio was obtained to be 9:1, as indicated by the composition-dependent quenching effect of Er3+ ions. The pump power dependence of upconversion emission intensity and Commission Internationale de L'Eclairage chromaticity coordinates of the phosphors were evaluated in detail.

  6. 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.

  7. 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.

  8. Investigation of the surface reactivity of a sol-gel derived glass in the ternary system SiO 2-CaO-P 2O 5

    NASA Astrophysics Data System (ADS)

    Mami, Mohamed; Lucas-Girot, Anita; Oudadesse, Hassane; Dorbez-Sridi, Rachida; Mezahi, Fatima; Dietrich, Elodie

    2008-09-01

    A new glass formulation, with the molar composition 60% SiO 2-35% CaO-5% P 2O 5, was synthesized using the sol-gel process, for applications as biomaterial in orthopaedic or maxillo facial surgery. Pellets, made of glass powder, were uniaxially compacted and soaked in simulated body fluid (SBF) for up to 7 days at 37 °C to evaluate glass bioactivity. Ionic exchanges at the interface glass-SBF were evaluated by studying evolutions of calcium, phosphorus and silicon concentrations in SBF using ICP-OES. Changes in glass surface, and the formation of crystalline phases were analyzed using XRD, SEM, EDS and FTIR methods. Results form ICP-OES showed a high reactivity of the glass surface with a very high and continuous release of calcium, a limited glass dissolution and an uptake of phosphorous from SBF. Results from both FTIR and XRD analysis indicated that the glass surface was progressively covered by two different phases: CaCO 3 as calcite and a carbonated apatite layer. The formation of these phases, following two different schemas, was observed after 2 h of immersion and confirmed after 7 days. SEM micrographs and EDS analysis demonstrated that the main phase, a carbonated apatite, was present as micro-spheroids and the secondary phase, calcite, was materialized by agglomerates which have diameters up to 10-15 μm. These results are in accordance with a bioactive feature of the glass studied.

  9. 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.

  10. 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. PMID:25728582

  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. AOTF-based remote sensor with sol-gel probe

    SciTech Connect

    Volkan, M.; Lee, Y.; Vo-Dinh, T.

    1999-11-01

    The authors report the development and application of a sensor using acousto-optic tunable filter (AOTF) and sol-gel probe technology. A pH-sensitive probe is used as a model sensing system with dextran derivatives of pH sensitive dyes doped into sol-gel thin films. They used a unique combination of pH-sensitive and pH-insensitive dual-label dye system. For optimization studies, the performance of these films as a pH sensing probe was evaluated using synchronous fluorescence detection. The performance of the prototype AOTF-based monitor using a low-power argon laser as an ion excitation source was evaluated.

  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. Effect of calcination temperature on phase transformation, structural and optical properties of sol-gel derived ZrO2 nanostructures

    NASA Astrophysics Data System (ADS)

    Kumar, Sachin; Bhunia, Snehasis; Ojha, Animesh K.

    2015-02-01

    Zirconia (ZrO2) nanostructures of various sizes have been synthesized using sol-gel method followed by calcination of the samples from 500 to 700 °C. The calcined ZrO2 powder samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infra-red spectroscopy (FT-IR), UV-visible spectroscopy (UV-vis.), Raman spectroscopy (RS) and thermogravimetric analysis (TGA). The phase transformation from tetragonal (t) to monoclinic (m) was observed. The average diameter of the ZrO2 nanostructures calcined at 500, 600 and 700 °C was calculated to be 8, 17 and 10 nm, respectively. The ZrO2 sample calcined at 500 °C with tetragonal phase shows a direct optical band gap of 5.1 eV. The value of optical band gap is decreased to 4.3 eV for the ZrO2 calcined at 600 °C, which contains both tetragonal (73%) and monoclinic (27%) phases. On further calcination at 700 °C, where the ZrO2 nanostructures have 36% tetragonal and 64% monoclinic phases, the optical band gap is calculated to be 4.8 eV. The enhancement in optical band gap for ZrO2 calcined at 700 °C may be due to the rod like shape of ZrO2 nanostructures. The tetragonal to monoclinic phase transformation was also confirmed by analyzing Raman spectroscopic data. The TG analysis revealed that the ZrO2 nanostructure with dominance of monoclinic phase is found to be more stable over the tetragonal phase. In order to confirm the phase stability of the two phases of ZrO2, single point energy is calculated corresponding to its monoclinic and tetragonal structures using density functional theory (DFT) calculations. The results obtained by theoretical calculations are in good agreement with the experimental findings.

  15. Sol-gel based biofuel cell architectures

    NASA Astrophysics Data System (ADS)

    Lim, James Robert

    Sol-gel based biofuel cell architectures were investigated and quantified for electrochemical performance. The flexible solution chemistry of the sol-gel process has been used to synthesize bio-hybrid materials in which a wide variety of biomolecules are encapsulated in a transparent, inorganic matrix. These biomolecules retain their characteristic reactivities and spectroscopic properties despite being immobilized in the pores of the inorganic matrix. Stability of the biomolecules is also improved because of the confinement in the rigid inorganic network. Sol-gel immobilization serves as the basis for the electrode architecture used in enzymatic biofuel cells. In this dissertation, the fabrication and characterization of an enzymatic glucoseoxygen biofuel cell that incorporates nanostructured silica sol-gel/carbon nanotube composite electrodes was evaluated. These novel electrodes combine the benefits of sol-gel encapsulation with the use of carbon nanotubes which provide enhanced electronic conduction pathways and increase the effective surface area of the electrode. With this immobilization approach, the silica sol-gel is sufficiently porous that both glucose and oxygen have access to enzymes and yet provide a protective cage that preserves biological structure and function, offers long-term stability and perhaps enables operation at elevated temperatures. In addition, direct electron transfer was exhibited by a nanostructured cathode. More notably, these nanostructured composites were developed for power generation. Analysis of electron transfer rates and enzyme kinetics were used to quantify encapsulation properties and explore potential opportunities for optimization. Another topic for biofuel cells is miniaturization. Through miniaturization, biofuel cell design and integration are major considerations for increasing power density and performance.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. Sol-Gel derived Sb-doped SnO II/SiO II nano-composite thin films for gas sensors

    NASA Astrophysics Data System (ADS)

    Gu, Zhengtian; Liang, Peihui; Zhang, Weiqing

    2006-05-01

    Sb-doped SnO II/SiO II nano-composite thin films prepared by sol-gel dip-coating method have been studied. By using X-ray diffraction (XRD), atomic force microscopy (AFM) and Fourier transform infrared (FTIR) spectroscopy, detailed investigation on the structure and morphology of the films has shown the crystalline grain size of Sb-doped SnO II/SiO II thin films is about 34nm, with larger specific surface area and duty porosity, which is fit for gas-sensing materials. The adulteration of SiO II particles leads to the condensation of Sn-OH and the strengthening of gel network, and improve the adhesion of the films. In addition, the optical properties of the thin films were studied by UV-Vis spectra and p-polarized light reflectance angular spectrum. The results showthat the optical transmissivity of Sb-doped SnO II/SiO II thin films is higher, near 95% in visible spectrum range, the measured optical gap is found equal to 3.67eV, also the films take on smaller refractive index and extinction coefficient compared with those of the SnO II and Sb:SnO II films, which is compatible with the semiconductor substrate in the solar cell. Further, the gas-sensing test was made to three kinds of gas C 3H 8, C IIH 5OH and NH 3 in our novel high sensitive scheme for optical film sensors. The results indicate that Sb doping to SnO II films greatly improves the gas sensitivity to C IIH 5OH, and the gas sensitivity of Sb:SnO II/SiO II nano-composite thin films are higher than that of Sb:SnO II thin films. The detection sensitivity of this optical film sensor is available to 10 -1ppm provided that the resolution of reflectance ratio is 10 -2.

  1. Fabrication and Characterization of Lead Zirconate Titanate (PZT) Thin Films by Sol-Gel Technique

    NASA Astrophysics Data System (ADS)

    Rahman, M. F.; Miglioli, L.

    2016-02-01

    In this work, thin lead zirconate titanate, Pb[Zr0.52Ti0.48]O3 (PZT) films have been developed from a novel sol-gel route. The sol-gel films were deposited by spin coating method. Isopropanol-based solution was used for its less toxic property. Gold (Au), platinum (Pt) and indium tin oxide (ITO) were used as substrates. Homogeneous polycrystalline films with (110) preferred orientation were obtained from all the films. The films behaved as ferroelectric material where dielectric constant at 0V for the films obtained from Au, Pt and ITO substrates were 484, 770 and 655, respectively. The coercive field values were around 10-15KV/cm which revealed that the films were soft ferroelectric.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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

  7. Biological effects of sol-gel derived ZrO2 and SiO2/ZrO2 coatings on stainless steel surface--In vitro model using mesenchymal stem cells.

    PubMed

    Smieszek, Agnieszka; Donesz-Sikorska, Anna; Grzesiak, Jakub; Krzak, Justyna; Marycz, Krzysztof

    2014-11-01

    The objective of this study was to determine biocompatibility of zirconia-based coatings obtained by the sol-gel method. Two matrices, ZrO2 and SiO2/ZrO2, were created and applied on stainless steel type 316L with dip-coating technique. The morphology and topography of biomaterials' surface were characterized using energy-dispersive X-ray spectroscopy and atomic force microscopy, while chemical composition was analyzed by Raman spectroscopy. Additionally, wettability and surface free energy were characterized. Biocompatibility of obtained biomaterials was evaluated using an in vitro model employing mesenchymal stem cells (MSCs) of adipose and bone marrow origin. Biological analysis included determination of proliferation activity and morphology of MSCs in cultures on synthesized biomaterials. Osteoinductive properties of biomaterials were determined both in non-osteogenic, as well as osteogenic conditions. The results showed that investigated biomaterials exerted different impact on MSCs. Biomaterial with ZrO2 layer was more biocompatible for adipose-derived MSCs, while SiO2/ZrO2 layer promoted proliferation of bone marrow derived MSCs. Moreover, hybrid coating exhibited greater osteoinductive properties than ZrO2 coating, both on cultures with adipose-derived stromal (stem) cells and bone marrow stromal cells. Observed biological effects may result not only from different chemical composition, but also from diverse wettability. The ZrO2 coating was characterized as hydrophobic layer, while SiO2/ZrO2 exhibited hydrophilic properties. The results obtained suggest that behavior of MSCs in response to the biomaterial may vary depending on their origin, therefore we postulate, that screening analysis of implants' biocompatibility, should incorporate model applying both adipose- and bone marrow derived MSCs.

  8. 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.

  9. 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.

  10. Sol-gel-derived magnetic SiO2/TiO2 nanocomposite reinforced hollow fiber-solid phase microextraction for enrichment of non-steroidal anti-inflammatory drugs from human hair prior to high performance liquid chromatography.

    PubMed

    Es'haghi, Zarrin; Esmaeili-Shahri, Effat

    2014-10-01

    Hollow fiber-solid phase micro-extraction (HF-SPME) technique containing sol-gel-derived Fe3O4/SiO2/TiO2 core-double shell nanocomposite as a novel high efficiency sorbent, coupled with high performance liquid chromatography was used to extraction and determination of six non-steroidal anti-inflammatory drugs; acetylsalicylic acid, naproxen, piroxicam, diclofenac, indomethacin and mefenamic acid, in hair samples. First, magnetite nanoparticles (Fe3O4-NPs) were synthesized by chemical co-precipitation of Fe(II) and Fe(III) ions (where the ratio of Fe(II) to Fe(III) is 1:2 and a non-oxidizing environment), in alkaline medium to produce magnetite particles. Subsequently, surface of Fe3O4-NPs was modified with SiO2 and TiO2 using layer-by-layer chemical technique. A core-shell structure of Fe3O4/SiO2/TiO2 composite was prepared by coating magnetite core particles with silica and titania layers. In the proposed method, NSAIDs were extracted by the synthesized nanocomposite and analyzed by HPLC. The parameters affecting the efficiency of magnetic nanoparticle (MNPs) assisted HF-SPME were investigated and optimized. The method validation was included and satisfying results with high pre-concentration factors (405 up to 2450) were obtained. It owes large surface area and porosity of the nano-adsorbent. Under the optimal conditions, the method detection limits (S/N=3) were in the range of 0.01-0.10μgml(-1) and the limits of quantification (S/N=10) between 0.04 and 0.30μgml(-1). Relative standard deviations were 3.09-6.61%. Eventually, the method was successfully applied to human hair after administration of NSAIDs.

  11. Spontaneous Pattern Formation Induced by Bénard-Marangoni Convection for Sol-Gel-Derived Titania Dip-Coating Films: Effect of Co-solvents with a High Surface Tension and Low Volatility.

    PubMed

    Uchiyama, Hiroaki; Matsui, Tadayuki; Kozuka, Hiromitsu

    2015-11-17

    Evaporation-driven surface tension gradient in the liquid layer often causes the convective flow, i.e., Bénard-Marangoni convection, resulting in the formation of cell-like patterns on the surface. Here, we prepared sol-gel-derived titania films from Ti(OC3H7(i))4 solutions by dip coating and discussed the effect of the addition of co-solvents with a high surface tension and low volatility on the spontaneous pattern formation induced by Bénard-Marangoni convection. Propylene glycol (PG, with a surface tension of 38.6 mN m(-1)) and dipropylene glycol (DPG, with a surface tension of 33.9 mN m(-1)) were added to the coating solutions containing 2-propanol (2-Pr, with a surface tension of 22.9 mN m(-1)) for controlling the evaporation-driven surface tension gradient in the coating layer on a substrate. During dip coating at a substrate withdrawal speed of 50 cm min(-1) in a thermostatic oven at 60 °C, linearly arranged cell-like patterns on a micrometer scale were spontaneously formed on the titania gel films, irrespective of the composition of coating solutions. Such surface patterns remained even after the heat treatment at 200 and 600 °C, where the densification and crystallization of the titania films progressed. The width and height of the cell-like patterns increased with increasing PG and DPG contents in the coating solutions, where the addition of PG resulted in the formation of cells with a larger height than DPG.

  12. 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. PMID:27040248

  13. 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.

  14. 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…

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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. PMID:24397288

  20. Solution chemistry optimization of sol-gel processed PZT thin films

    SciTech Connect

    Lockwood, S.J. Schwartz, R.W.; Tuttle, B.A.; Thomas, E.V.

    1992-12-31

    We have optimized the ferroelectric properties and microstructural characteristics of sol-gel PZT thin films used in a CMOS-integrated, 256 bit ferroelectric non-volatile memory. The sol-gel process utilized in our work involved the reaction of Zr n-butoxide, Ti isopropoxide, and Pb (IV) acetate in a methanol/acetic acid solvent system. A 10-factor screening experiment identified solution concentration, acetic acid addition, and water volume as the solution chemistry factors having the most significant effects on the remanent polarization, coercive field, ferroelectric loop quality, and microstructural quality. The optimal values for these factors were determined by running a 3-factor uniform shell design, modeling the responses, and testing the models at the predicted optimal conditions. The optimized solution chemistry generated 3-layer, 300--400 nm thick films on RuO{sub 2} coated silicon substrates with coercive fields of less than 25 kv/cm (a 40--50% improvement over the original solution chemistry), a remanent polarization of 25--30 {mu}C/cm, and a reduction in the pyrochlore phase content below observable levels.

  1. Nanocrystalline multiferroic BiFeO3 ultrafine fibers by sol-gel based electrospinning

    NASA Astrophysics Data System (ADS)

    Xie, S. H.; Li, J. Y.; Proksch, Roger; Liu, Y. M.; Zhou, Y. C.; Liu, Y. Y.; Ou, Y.; Lan, L. N.; Qiao, Y.

    2008-12-01

    Novel nanocrystalline BiFeO3 ultrafine fibers have been synthesized by sol-gel based electrospinning, with fiber diameter in the range of 100-300 nm and grain size of around 20 nm. Phase pure perovskite BiFeO3 can be obtained if the fibers are fired in Ar atmosphere, eliminating impurity phases often observed when fired in air or N2 atmosphere. Excellent piezoelectricity and clear ferroelectric domain structure of the ultrafine fibers are characterized by high voltage piezoresponse force microscopy. Enhanced weak ferromagnetism arising from the nanocrystalline structure of ultrafine fibers is also observed.

  2. 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.

  3. Functionalized sol-gel coatings for optical applications.

    PubMed

    Pénard, Anne-Laure; Gacoin, Thierry; Boilot, Jean-Pierre

    2007-09-01

    Sol-gel processing is well-known to be a powerful technique for designing materials for optical applications. Here, some recent applications of functionalized sol-gel coatings in optics are briefly reviewed. Lanthanide-doped oxide nanocrystals form a new promising class of nanophosphors allowing the easy sol-gel preparation of transparent and luminescent films for the development of light-emitting devices. Recent experiments on organized mesoporous films show their potential applications in optics, such as stable low-index layers in interferential antireflective devices or as silica binders in TiO 2-photocatalytic devices. PMID:17330964

  4. Soluble polymers in sol-gel silica

    NASA Astrophysics Data System (ADS)

    Beaudry, Christopher Laurent

    In the last few years, the inherent versatility of sol-gel processing has led to a significant research effort on inorganic/organic materials. One method of incorporating an organic phase into sol-gel silica is dissolving an organic polymer in a tetraethylorthosilicate (TEOS) solution, followed by in situ polymerization of silica in the presence of organic polymer. The first part of the study involved the development of a two-step (acid-base) synthesis procedure to allow systematic control of acidity in TEOS solutions. With this procedure, it was possible to increase the pH of the TEOS solution while correlating the acidity and properties. The properties were the gelation time, syneresis rate, drying behavior, and xerogel pore structure, as determined by nitrogen sorption. Furthermore, controlling the acidity was shown to control the silica xerogel pore structure. In the second part of the study, the two-step procedure was used to synthesize silica/poly(ethylene glycol) (PEG), and silica/poly(vinyl acetate) (PVAc) composite materials. The content of organic polymer and the molecular weight were varied. The gelation time, the syneresis rate, the drying behavior, and the pore structure were determined for compositions with 10% PEG (M.W. 2,000), 5, 10, and 15% PEG (M.W. 3,400), and 10 and 25% PVAc (M.W. 83,000). Other compositions and molecular weights of PEG lead to sedimentation. In the PEG compositions, the tendency to phase separate was correlated with the effects of the processing variables on the segregation strength and polymerization rate. The PVAc compositions did not show any visible phase separation during processing, giving the composite xerogels an appearance similar to pure silica. The property differences between gels with PEG and gels with PVAc show the relative strength of the interactions with silica. Both polymers exhibit hydrogen bonding between the phases. In the case of PEG, hydrogen bonding between the ether oxygens of the polymer and silanol

  5. 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.

  6. Sol-gel entrapped cobalt complex

    SciTech Connect

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

    2003-03-15

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

  7. Organofunctional Sol-Gel Materials for Toxic Metal Separation

    SciTech Connect

    Im, Hee-Jung; Yost, Terry L.; Yang, Yihui; Bramlett, J. Morris; Yu, Xiang-Hua; Fagan, Bryan C.; Allain, Leonardo R.; Chen, Tianniu; Xue, Ziling; Barnes, Craig E.; Dai, Sheng; Rocker, Lee E.; Sepaniak, Michael J.

    2003-09-10

    Inorganic-organic silica sol-gels grafted or encapsulated with organic ligands were prepared and found to selectively and reversibly remove target metal ions such as Cu2+, Cd2+, and Sr2+. These organofunctional sol-gel materials, which were easily prepared from off-the-shelf chemicals, were hydrophilic and showed fast kinetics of metal uptake. The sol-gels were easily regenerated and used in multi-cycle metal removal. In our search for new ligands for metal removal, we found that the reactions of thioacetal ligands with Hg2+ gave Hg(SCH2COOH)2. Our studies of organofunctional sol-gel materials for metal separation will be discussed.

  8. 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.

  9. 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.

  10. 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. PMID:26470065

  11. 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.

  12. 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.

  13. Preparation and Characterisation of Hydroxyapatite Coatings on Nanotubular TiO2 Surface Obtained by Sol-Gel Process.

    PubMed

    Shin, Jin-Ho; Kim, Jung-Hwa; Koh, Jeong-Tae; Lim, Hyun-Pil; Oh, Gye-Jeong; Lee, Seok-Woo; Lee, Kwang-Min; Yun, Kwi-Dug; Park, Sang-Won

    2015-08-01

    Hydroxyapatite (HA) coating on titanium dioxide (TiO2) nanotubular surface has been developed to complement the defects of both TiO2 and HA. A sol-gel processing technique was used to coat HA on TiO2 nanotubular surface. All the titanium discs were blasted with resorbable blast media (RBM). RBM-blasted Ti surface, anodized Ti surface, and sol-gel HA coating on the anodized Ti surface were prepared. The characteristics of samples were observed using scanning electron microscopy and X-ray photoemission spectroscopy. Biologic responses were evaluated with human osteosarcoma MG63 cells in vitro. The top of the TiO2 nanotubes was not completely covered by HA particles when the coating time was less than 60 sec. It was demonstrated the sol-gel derived HA film was well-crystallized and this enhanced biologic responses in early stage cell response.

  14. 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}.

  15. 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. PMID:12392950

  16. Luminescence properties of Cr-doped silica sol gel glasses

    NASA Astrophysics Data System (ADS)

    Strek, Wieslaw; Lukowiak, Edward; Deren, Przemyslaw J.; Maruszewski, K.; Trabjerg, Ib; Koepke, Czeslaw; Malashkevich, G. E.; Gaishun, Vladimir E.

    1997-11-01

    The emission of Cr-doped silica glass obtained by the sol- gel method is characterized by an orange broad band with a maximum at 610 nm. Its nature is examined by the absorption, excited state absorption, emission, excitation and lifetime measurements over a wide range of temperature and for different concentration of Cr ions. Our measurement show that in spite of fact that the absorption properties of Cr- doped silica sol-gel glass are predominantly associated with Cr4+ centers, the observed in visible range emission can be assigned neither to Cr3+ nor to Cr4+ ions. The discussion of the nature of observed emission was carried out for all possible valencies of the Cr ions. In conclusion is suggested that it may be ascribed to the transitions on the monovalent Cr1+ ion. The reducing agents occurring during the sol-gel process and leading to lowering the Cr valency are discussed.

  17. Characterization of Sol-gel Encapsulated Proteins using Small-angle Neutron Scattering

    SciTech Connect

    Luo, Guangming; Zhang, Qiu; Del Castillo, Alexis Rae; Urban, Volker S; O'Neill, Hugh Michael

    2009-01-01

    Entrapment of biomolecules in silica-derived sol-gels has grown into a vibrant area of research since it was originally demonstrated. However, accessing the consequences of entrapment on biomolecules and the gel structure remains a major challenge in characterizing these biohybrid materials. We present the first demonstration that it is possible with small-angle neutron scattering (SANS) to study the conformation of dilute proteins that are entrapped in transparent and dense sol-gels. Using deuterium-labeled green fluorescent protein (GFP) and SANS with contrast variation, we demonstrate that the scattering signatures of the sol-gel and the protein can be separated. Analysis of the scattering curves of the sol-gels using a mass-fractal model shows that the size of the colloidal silica particles and the fractal dimensions of the gels were similar in the absence and presence of protein, demonstrating that GFP did not influence the reaction pathway for the formation of the gel. The major structural difference in the gels was that the pore size was increased 2-fold in the presence of the protein. At the contrast match point for silica, the scattering signal from GFP inside the gel became distinguishable over a wide q range. Simulated scattering curves representing a monomer, end-to-end dimer, and parallel dimer of the protein were calculated and compared to the experimental data. Our results show that the most likely structure of GFP is that of an end-to-end dimer. This approach can be readily applied and holds great potential for the structural characterization of complex biohybrid and other materials.

  18. 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

  19. Synthesis of Sol-Gel Matrices for Encapsulation of Enzymes Using an Aqueous Route

    SciTech Connect

    Ashley, C.S.; Bhatia, R.B.; Brinker, C.J.; Harris, T.M.

    1998-11-23

    Sol-gel matrices are promising host materials for potential chemical and biosensor applications. Previous studies have focused on modified sol-gel routes using alkoxides for encapsulation of enzymes. However the formation of alcohol as a byproduct during hydrolysis and condensation reactions poses limitations. We report the immobilization of glucose oxidase and peroxidase in silica prepared by an aqueous route which may provide a more favorable environment for the biomolecules. A two step aqueous sol-gel procedure using sodium silicate as the precursor was developed to encapsulate the enzymes and the dye precursor, o-dianisidine. Glucose oxidase catalyzes the oxidation of glucose to give gluconic acid and hydrogen peroxide. Peroxidase then catalyzes the reaction of the dye precursor with hydrogen peroxide to produce a colored product. The kinetics of the coupled enzymatic reactions were monitored by optical spectroscopy and compared to those occurring in tetramethyl orthosilicate (TMOS) derived silica matrices developed by Yamanaka. Enhanced kinetics in the aqueous silicate matrices were related to differences in the host microstructure as elucidated by microstructural comparisons of the corresponding aerogels.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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}).

  5. Micro-PIXE-RBS methods highlighting the influence of phosphorus on the in vitro bioactivity of sol-gel derived glass particles in the SiO 2-CaO-P 2O 5 system

    NASA Astrophysics Data System (ADS)

    Lao, J.; Nedelec, J. M.; Moretto, Ph.; Jallot, E.

    2008-05-01

    Ion beam analysis methods were used to characterize the interface of bioactive glasses with surrounding biological fluids. Glass particles in the SiO2-CaO and SiO2-CaO-P2O5 compositions were made by sol-gel processing and soaked in biological fluids for periods up to 4 days. The surface changes were characterized using PIXE-RBS, which are efficient methods for multielemental analysis and accurate trace elements quantification. Elemental maps of major and trace elements were obtained at a micrometer scale and revealed the bone bonding ability of the materials. Glass particles are quickly coated with a thin calcium phosphate-rich layer containing traces of magnesium. After a few days, SiO2-CaO-P2O5 glass particles are entirely changed into calcium phosphates, whereas SiO2-CaO particles exhibit a different behavior: the previously Ca-P enriched periphery has been dissolved and glass particles consist of a silicate network. Calculation of the Ca-P atomic ratios at the glass/biological fluids interface provides us with an explanation for this: an enduring apatitic phase seems to be formed at the periphery of SiO2-CaO-P2O5 glass particles. Presence of phosphorus in the glass matrix thus has an influence on the amplitude and the kinetics of reaction of the bioactivity process. It might result in an improved chemical bond with living tissues.

  6. 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...

  7. 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.

  8. 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.

  9. 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.

  10. Intrinsically tunable bulk acoustic wave resonators based on sol-gel grown PMN-PT films

    NASA Astrophysics Data System (ADS)

    Vorobiev, A.; Spreitzer, M.; Veber, A.; Suvorov, D.; Gevorgian, S.

    2014-08-01

    Intrinsically tunable bulk acoustic wave resonators, based on sol-gel 0.70Pb(Mg1/3Nb2/3)O3-0.30PbTiO3 (PMN-PT) thin films, with high effective electromechanical coupling coefficient of 13% and tunability of the series resonance frequency up to 4.0% are fabricated and characterized. The enhanced electroacoustic properties of the PMN-PT resonators are attributed to the mechanism of polarization rotation occurring in the region of the morphotropic phase boundary. Electroacoustic performance of the PMN-PT resonators is analyzed using the theory of dc field-induced piezoelectric effect in ferroelectrics. Extrinsic acoustic loss in the PMN-PT resonators is analyzed using the model of the wave scattering at reflections from rough interfaces. Mechanical Q-factor of the resonators is up to 70 at 4.1 GHz and limited mainly by losses in the PMN-PT film.

  11. 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.

  12. 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. PMID:26952414

  13. Synthesis and properties of nanostructured sol-gel sorbents for simultaneous removal of sulfur dioxide and nitrogen oxides from flue gas

    NASA Astrophysics Data System (ADS)

    Buelna Quijada, Genoveva

    2001-07-01

    Regenerative, alumina-supported, copper-based sorbent/catalysts provide a promising technique for simultaneous removal of SO2 and NO x from flue gas. These sorbents can remove over 90% of SO2 and 70+% of NOx while generating no wastes, reducing energy consumption, and producing valuable by-products. The lack of a cost-effective sorbent with low attrition rate and good reactivity has been the main hurdle to commercialization of this copper oxide process. Developing such a sorbent is the focus of this dissertation. This work examines using sol-gel techniques rather than traditional processes to produce gamma-alumina and copper coated 7-alumina granular sorbents. Important modifications to the established sol-gel synthesis process were made, which minimized generated wastes and reduced preparation time and sorbent cost. A laboratory scale semi-continuous process providing a basis for large-scale synthesis was developed. The effect of the copper content on the surface area and dispersion of the active species on sol-gel-derived sorbents coated by the one step and wet-impregnation methods was studied. The sol-gel-derived sorbents showed superior sulfation and regeneration properties than the existing commercial sorbents used in the copper oxide process in terms of sulfation capacity, fast regeneration, recovery of sorption capacity, and SO2 concentration in the regenerated effluent. The optimum temperature for NO reduction by NH3 over sol-gel-derived CuO/gamma-Al2O3 was found to be 350°C for both fresh and sulfated catalysts. This was also the optimum operating temperature for simultaneous removal of SO2 and NOx from simulated flue gas. At 350°C, the adsorption capacity of the sol-gel sorbent/catalyst was higher than UOP's sorbent, and very close to the capacity of ALCOA's sorbent, while the catalytic activity for NO reduction of the sol-gel-derived CuO/gamma-Al 2O3 sorbent fell between the commercial sorbents. The new mesoporous sol-gel-derived materials showed

  14. Sol-gel coating of lithium zinc ferrite powders

    SciTech Connect

    Brooks, K.G.; Amarakoon, V.R.W. )

    1991-04-01

    This paper reports on lithium zinc ferrite powders of composition Li{sub 0 {minus} 3} Zn{sup 0 {minus}4}Mn{sub 0.05}Fe{sub 2.25}O{sub 4} were prepared by solid-state synthesis. Liquid-phase borosilicate sintering additives were applied to the ferrite particle surfaces at room temperature via a sol-gel coating technique. Calcined and comminuted ferrite powder was dispersed in methanol with predetermined quantities of tetraethyl orthosilicate and triethyl borate. Hydrofluoric acid was used to catalyze the sol-gel reactions. Amorphous coatings of 10 to 20 nm thickness were observed on particle surfaces by TEM. Chemical bonding in the coatings was studied using diffuse reflectance FTIR spectroscopy.

  15. Nanostructured energetic materials using sol-gel methodologies

    SciTech Connect

    Tillotson, T M; Simpson, R L; Hrubesh, L W; Gash, A E; Thomas, I M; Poco, J F

    2000-09-27

    The fundamental differences between energetic composites and energetic materials made from a monomolecular approach are the energy density attainable and the energy release rates. For the past 4 years, we have been exploiting sol-gel chemistry as a route to process energetic materials on a microstructural scale. At the last ISA conference, we described four specific sol-gel approaches to fabricating energetic materials and presented our early work and results on two methods - solution crystallization and powder addition. Here, we detail our work on a third approach, energetic nanocomposites. Synthesis of thermitic types of energetic nanocomposites are presented using transition and main group metal-oxide skeletons. Results on characterization of structure and performance will also be given.

  16. 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.

  17. 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.

  18. Polymer modified sol-gel materials for photochromic applications

    NASA Astrophysics Data System (ADS)

    Janik, Ryszard; Kucharski, Stanislaw

    2006-08-01

    The chromophoric materials were prepared by copolymerization of various methacrylic monomers. The incorporation of the chromophore groups was done by coupling reaction of diazonium salts of the sulfonamide such as: sulfomethazine or sulfisomidine). The copolymers having free OH groups were able to react with 3-triethoxypropyl isocyanate forming intermediates used to prepare hybrid transparent films by sol-gel technique. The films of both copolymers as well as of hybrid sol-gel structures showed photochromic properties via trans-cis isomerization of the diazo groups. The absorption maximum of the trans form was ca. 435-445 nm depending on chemical composition of the material. Illumination of the films with coherent laser beams (two-beam coupling) resulted in formation of diffraction grating. The diffraction efficiency reached 4-5 % and refractive index modulation was in the range up to 0.0032.

  19. 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.

  20. Inhomogeneous distribution of organic molecules adsorbed in sol gel glasses

    NASA Astrophysics Data System (ADS)

    Meneses-Nava, M. A.; Chávez-Cerda, S.; Sánchez-Villicaña, V.; Sánchez-Mondragón, J. J.; King, T. A.

    1999-09-01

    The effects of the porous matrix upon the radiative characteristics of quinine sulphate doped sol-gel glasses are investigated. The broadenings of the absorption and fluorescence spectra are explained by the attachment of the molecules on distorted sites or in a non-planar fashion, creating an inhomogeneous distribution of adsorbed molecules. For this reason, each emitting center relaxes with its own characteristics. This inhomogeneous distribution is also supported by the non-exponential and the wavelength dependence of the fluorescence decay.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. 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. PMID:26688872

  6. Sol-gel thin films for photonic application

    NASA Astrophysics Data System (ADS)

    Jasieniak, Jacek J.; Martucci, Alessandro

    2012-06-01

    For the fabrication of photonic devices the sol-gel technique is a potentially lucrative alternative to methods such as physical vapor or chemical vapor deposition because of its solution-processability, low cost and relative ease of production. In this work we harness this potential by developing based photonic devices which incorporate highly luminescent CdSe@ZnS core-shell semiconductor quantum dots (QDs) doped within inorganic (TiO2, ZrO2) or hybrid organic-inorganic sol-gel films. As a pre-requisite to the formation of such devices, luminescent waveguides emitting between green and red have been obtained and their optical properties have been characterized. The photochemical stability of these waveguides was found to highly dependent on the exact sol-gel material used. QDs:Titania based composites were found to be inherently photo-unstable due to photoelectron injection into the bulk matrix and subsequent nanocrystal oxidation. In comparison, zirconia composites were significantly more robust with high photoluminescence retained up to annealing temperatures of 300 °C. Despite this difference in photo-chemical stability, both titania and zirconia composite waveguides exhibited amplified stimulated emission (ASE) with one-photon and two-photon optical pumping, however only zirconia based waveguides exhibited long term photostability. This Zirconia based films have been used for the realization of distributed feedback lasers and Bragg micro-cavities.

  7. 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.

  8. 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

  9. Integrated optical components using hybrid organic-inorganic materials prepared by sol-gel technology

    NASA Astrophysics Data System (ADS)

    Mishechkin, Oleg Viktorovich

    2003-10-01

    A technological platform based on low-temperature hybrid sol-gel method for fabrication of optical waveguides and integrated optical components has been developed. The developed chemistry for doping incorporation in the host network provides a range of refractive indexes (1.444--1.51) critical for device optimization. A passivation method for improving long-term stability of organic-inorganic sol-gel material is reported. The degradation of waveguide loss over time due to moisture adsorption from the atmosphere is drastically suppressed by coating the material with a protective thin SiO2 film. The results indicate a long-term optical loss below 0.3 dB/cm for protected waveguides. The theory of multimode interference couplers employing self-imaging effect is described. A novel approach for design of high-performance MMI devices in low-contrast material is proposed. The design method is based on optimization of refractive index contrast and width of a multimode waveguide (the body of MMI couplers) to achieve a maximum number of constructively interfering modes resulting to the best self-imaging. This optimization is carried out using 3D BPM simulations. This method was applied to design 1 x 4, 1 x 12, and 4 x 4 MMI couplers and led to a superior performance in excess loss, power imbalance in output ports, and polarization sensitivity. Taking advantage of the inherent input-output phase relations in a 4 x 4 MMI coupler, an optical 90° hybrid is realized by incorporation a Y-junction to coherently excite two ports of the coupler. A series of MMI couplers were fabricated and characterized. The experimental results are in good agreement with the design. Measured performance of the sol-gel derived MMI components was compared to analogues fabricated by other technologies. The comparison demonstrates the superior performance of the sol-gel devices. The polarization sensitivity of all fabricated couplers is below 0.05 dB.

  10. 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

  11. Preparation and characteristics of sol-gel-coated calix[4]arene fiber for solid-phase microextraction.

    PubMed

    Li, Xiujuan; Zeng, Zhaorui; Gao, Shengzhe; Li, Haibing

    2004-01-01

    5,11,17,23-Tetra-tert-butyl-25,27-diethoxy-26,28-dihydroxycalix[4]arene/hydroxy-terminated silicone oil coated fiber was first prepared and applied for solid-phase microextraction (SPME) with sol-gel technology. The possible sol-gel mechanism was discussed and confirmed by IR spectra. It showed wonderful selectivity and sensitivity to polar (aromatic amines), nonpolar (benzene derivatives, polycyclic aromatic hydrocarbons) and high boiling point compounds (phthalates) and the extraction equilibria were reached quite fast. The coating has high thermal stability (380 degrees C) and solvent stability (organic and inorganic), thus its lifetime is longer than conventional fibers. In addition, it has surprising fiber-to-fiber and batch-to-batch reproducibility. The detection limits were quite low and the linear ranges were pretty broad for all analytes.

  12. 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.

  13. Sol-gel based sensor for selective formaldehyde determination.

    PubMed

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

    2010-02-01

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

  14. 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

  15. Fluorescent sol-gel layer for optical cryogenic temperature sensor

    NASA Astrophysics Data System (ADS)

    Bertrand, S.; Bresson, F.; Tribillon, Gilbert M.; Audebert, Patrick

    1995-09-01

    The expansion of optical sensors and the interest of the sol-gel process for the working out of new materials, have led us to develop a sensor applied to cryogenic temperature measurement in harsh environments. The measurement technique uses the decay-time of the luminescence emitted by doped crystals, in response to a short duration excitation pulse. The principle of the measurement has already been demonstrated by a prototype with crystals under bulk shape, and we present here a non contact version of the sensor, using fluorescent layers deposited on mechanical parts. These layers are composed of photoluminescent crystals reduced to powder and mixed to a binder. The originality of this work is that the binder is a silica-based hybrid gel. Such a gel has a good adherence to metallic substrates in cryogenic mediums and it can be used in chemically oxidizing environments. The fluorescence decay-time technique associated with the sol-gel process can then provide an interesting alternative in the development of new noncontact optical fiber sensors, working in hostile conditions.

  16. 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.

  17. Exact kinetics of the sol-gel transition

    NASA Astrophysics Data System (ADS)

    Lushnikov, A. A.

    2005-04-01

    The formation of a gel in a disperse system wherein binary coagulation alone governs the temporal changes of particle mass spectra is studied under the assumption that the coagulation kernel is proportional to the product of masses of coalescing particles. This model is known to reveal the sol-gel transition, i.e., the formation of one giant cluster with the mass comparable to the total mass of the whole system. This paper reports on the exact solution of this model for a finite total mass of the coagulating system. The evolution equation for the generating functional defining all properties of coagulating systems is solved exactly for this particular kernel. The final output is the exact expression for the single-particle mass spectrum as a function of time. The analysis of the spectrum in the thermodynamic limit shows that after a critical time a giant single particle (the gel) appears. Although the concentration of this giant gel particle is zero in the thermodynamic limit, it actively interacts with smaller particles “eating” them and thus growing in mass. Special attention is given to the transition point, where the gel is appearing. It is demonstrated that the sol-gel transition reminds the second-order phase transition. The time dependencies of the gel mass, the number concentration, and the second moment of the particle mass spectrum are found.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. Polymer sol-gel composite inverse opal structures.

    PubMed

    Zhang, Xiaoran; Blanchard, G J

    2015-03-25

    We report on the formation of composite inverse opal structures where the matrix used to form the inverse opal contains both silica, formed using sol-gel chemistry, and poly(ethylene glycol), PEG. We find that the morphology of the inverse opal structure depends on both the amount of PEG incorporated into the matrix and its molecular weight. The extent of organization in the inverse opal structure, which is characterized by scanning electron microscopy and optical reflectance data, is mediated by the chemical bonding interactions between the silica and PEG constituents in the hybrid matrix. Both polymer chain terminus Si-O-C bonding and hydrogen bonding between the polymer backbone oxygens and silanol functionalities can contribute, with the polymer mediating the extent to which Si-O-Si bonds can form within the silica regions of the matrix due to hydrogen-bonding interactions. PMID:25734614

  3. Polymer sol-gel composite inverse opal structures.

    PubMed

    Zhang, Xiaoran; Blanchard, G J

    2015-03-25

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

  4. 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.

  5. Sol-gel synthesis and characterization of mesoporous manganese oxide

    SciTech Connect

    Hong Xinlin; Zhang Gaoyong; Zhu Yinyan; Yang Hengquan

    2003-10-30

    Mesoporous manganese oxide (MPMO) from reduction of KMnO{sub 4} with maleic acid, was obtained and characterized in detail. The characterization of the material was confirmed by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffractometry (XRD) and N{sub 2} sorptometry. The results showed that MPMO is a pseudo-crystalline material with complex network pore structure, of which BET specific surface area is 297 m{sup 2}/g and pore size distribution is approximately in the range of 0.7-6.0 nm. The MPMO material turns to cryptomelane when the calcinating temperature rises to 400 deg. C. The optimum sol-gel reaction conditions are KMnO{sub 4}/C{sub 4}H{sub 4}O{sub 4} molar ratio=3, pH=7 and gelation time>6 h.

  6. 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.

  7. 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.

  8. 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

    2014-11-01

    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. PMID:25466691

  9. Mayenite Synthesized Using the Citrate Sol-Gel Method

    SciTech Connect

    Ude, Sabina N; Rawn, Claudia J; Meisner, Roberta A; Kirkham, Melanie J; Jones, Gregory L.; Payzant, E Andrew

    2014-01-01

    A citrate sol-gel method has been used to synthesize mayenite (Ca12Al14O33). X-ray powder diffraction data show that the samples synthesized using the citrate sol-gel method contained CaAl2O4 and CaCO3 along with mayenite when fired ex-situ in air at 800 C but were single phase when fired at 900 C and above. Using high temperature x-ray diffraction, data collected in-situ in air at temperatures of 600 C and below showed only amorphous content; however, data collected at higher temperatures indicated the first phase to crystallize is CaCO3. High temperature x-ray diffraction data collected in 4% H2/96% N2 does not show the presence of CaCO3, and Ca12Al14O33 starts to form around 850 C. In comparison, x-ray powder diffraction data collected ex-situ on samples synthesized using traditional solid-state synthesis shows that single phase was not reached until samples were fired at 1350 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method suggest the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is very different depending on the environment. Brunauer-Emmett-Teller (BET) measurements showed a slightly higher surface area of 7.4 0.1 m2/g in the citrate gel synthesized samples compared to solid-state synthesized sample with a surface area of 1.61 0.02 m2/g. SEM images show a larger particle size for samples synthesized using the solid-state method compared to those synthesized using the citrate gel method.

  10. 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.

  11. 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

  12. 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.

  13. Thermal strain measurement in sol-gel lead zirconate titanate thin films

    NASA Astrophysics Data System (ADS)

    Berfield, T. A.; Carroll, J. F.; Payne, D. A.; Sottos, N. R.

    2009-12-01

    A fluorescence-based digital image correlation (DIC) technique is used to characterize the in-plane strain development of blanket sol-gel derived lead zirconate titanate thin films deposited on platinized silicon substrates. The in-plane strain is also measured within film line features patterned via a mediated octadecyltrichlorosilane (ODS) monolayer. The results indicate that the selective film failure induced by the mediated ODS layer succeeds in slightly reducing the in-plane strain transverse to the line feature direction (˜25% lower), while remaining nearly the same as the blanket film case in the direction parallel to the line direction. Additional in-plane stress estimates from wafer curvature measurements for the two film configurations (blanket and ODS patterned) were consistent with the DIC measured strain results.

  14. 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.

  15. 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.

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

    NASA Astrophysics Data System (ADS)

    Huang, Z.; Donohue, P. P.; Zhang, Q.; Williams, D. J.; Anthony, C. J.; Whatmore, R. W.; Todd, M. A.

    2003-02-01

    Lead scandium tantalate (PST) thin films for uncooled infrared (IR) detector applications have been deposited by liquid delivery chemical vapour deposition (LDCVD), sputtering and sol-gel techniques. The sol-gel and sputtered films were deposited at low temperature into a non-ferroelectric phase with the required perovskite structure being formed using a high temperature rapid thermal anneal (RTA). In contrast to this, the LDCVD films were deposited at high temperature directly into the perovskite phase but were found to still require a high temperature RTA step to optimize their merit for IR detection. Detailed structural and electrical characterization of the PST films deposited by these different methods have revealed that there is no simple relationship between microstructure and electrical properties. The sol-gel and LDCVD techniques produce thin films with excellent microstructures, as determined by x-ray diffraction analysis and transmission electron microscopy, but inferior electrical properties and relatively low merit figures. By contrast, the sputtered and then rapid thermal annealed films have inferior microstructures, characterized by extensive voiding, but excellent electrical properties and high merit figures.

  17. Polyester-inorganic nanocomposite materials via sol-gel reactions: Synthesis and characterization of fundamental properties

    NASA Astrophysics Data System (ADS)

    Lambert, Alexander Adam, III

    A scheme was developed for producing poly(ethylene terephthalate (PET) ionomer)/silicate hybrid materials via polymer-in situ sol-gel reactions for tetraethylorthosilicate (TEOS) using different solvents. Scanning electron microscopy/EDAX studies revealed that silicate structures can be grown deep within PET ionomer films that were melt pressed from silicate-incorporated resin pellets. 29Si solid-state NMR spectroscopy revealed considerable, successful Si-O-Si bond formation, but also a significant fraction of uncondensed SiOH groups. 23Na solid-state NMR spectra suggested the presence of ionic aggregates within the unfilled PET ionomer and that these aggregates do not suffer major structural re-arrangements by silicate incorporation. For an ionomer treated with TEOS using MeCl2 solvent, Na + ions are less self-associated than in the unfilled control, suggesting silicate intrusion between PET-SO3- Na + ion pair associations. The ionomer treated with TEOS + tetrachloroethane had more poorly formed ionic aggregates, which illustrates the influence of solvent type on ionic aggregation. First-scan DSC thermograms for the ionomers demonstrate an increase in crystallinity after the incorporation of silicates, but solvent induced crystallization also appears to be operative. Second-scan DSC thermograms also suggest that the addition of silicate particles is not the only factor implicated in re-crystallization, and that solvent type is important even in second scan behavior. Silicate incorporation does not profoundly affect the second scan Tg vs. solvent type, i.e., chain mobility in the amorphous regions is not severely restricted by silicate incorporation. Re-crystallization and melting in these hybrids appears to be due to an interplay between a solvent induced crystallization that strongly depends on solvent type, and interactions between PET chains and in situ-grown, sol-gel-derived silicate particles. Isothermal studies confirmed that the crystallization rate and

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

    NASA Astrophysics Data System (ADS)

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

    2010-07-01

    Hydroxyapatite (HAp) forms the main mineral component of bone and teeth. This naturally occurring HAp is in the form of nano-metre sized crystallites of Ca10(PO4)6(OH)2 that contain a number of cation and anion impurities, for example CO32-, F-, Na+, Mg2+ and Sr2+. Synthetic nano-sized HAp particles exhibit favourable biocompatibility and bioactivity and in order to better match the composition to natural HAp there is great interest in producing a range of chemically modified powders. In this study, two HAp powders have been synthesised via a water-based low-temperature sol-gel method and a third, commercial powder from Sigma-Aldrich have been analysed. Subsequent powder calcination has been carried out within the temperature range of 500-700 °C and the products characterised by bulk chemical analysis, X-ray diffraction and electron microscopy. Energy dispersive X-ray spectroscopy (EDX) in the TEM has been used to assess the composition of individual HAp particles. In order to do this accurately it is first necessary to account for the sensitivity of the HAp structure and composition to irradiation by the high energy electron beam of the TEM. This was done by monitoring the estimated Ca/P ratio derived from TEM-EDX of stoichiometric HAp under increasing levels of electron fluence. A fluence threshold (at a given beam energy) was established below which the measured Ca/P ratio can be considered to be stable. Subsequent elemental analysis at or below this threshold has enabled the variation in composition between particles both within and between synthesis batches to be accurately assessed. Compositional variability between particles is also evident, even in the commercial powder, but is far greater in the powders prepared by the sol-gel method.

  19. The controlled release of drugs from emulsified, sol gel processed silica microspheres.

    PubMed

    Radin, Shula; Chen, Tiffany; Ducheyne, Paul

    2009-02-01

    Controlled release silica sol gels are room temperature processed, porous, resorbable materials with generally good compatibility. Many molecules including drugs, proteins and growth factors can be released from sol gels and the quantity and duration of the release can vary widely. Processing parameters render these release properties exquisitely versatile. The synthesis of controlled release sol gels typically includes acid catalyzed hydrolysis to form a sol with the molecules included. This is then followed by casting, aging and drying. Additional steps such as grinding and sieving are required to produce sol gel granules of a desirable size. In this study, we focus on the synthesis of sol gel microspheres by using a novel process with only two steps. The novelty is related to acid-base catalysis of the sol prior to emulsification. Sol gel microspheres containing either vancomycin (antibiotic) or bupivacaine (analgesic) were successfully synthesized using this method. Both drugs showed controlled, load dependent and time dependent release from the microspheres. The in vitro release properties of sol gel microspheres were remarkably different from those of sol gel granules produced by grinding and sieving. In contrast to a fast, short-term release from granules, the release from microspheres was slower and of longer duration. In addition, the degradation rate of microspheres was significantly slower than that of the granules. Using various mathematical models, the data reveal that the release from sol gel powder is governed by two distinct phases of release. In addition, the release from emulsified microspheres is delayed, a finding that can be attributed to differences in surface properties of the particles produced by emulsification and those produced by casting and grinding. The presented results represent an excellent data set for designing and implementing preclinical studies.

  20. 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.

  1. Processing of patterned ferroelectric capacitors

    NASA Astrophysics Data System (ADS)

    Rod, Bernard J.

    1992-09-01

    Processing steps are described in detail for a procedure to fabricate sol-gel-derived lead-zirconate-titanate (PZT) ferroelectric thin-film capacitors in a manner compatible with processed complementary metal-oxide-semiconductor (CMOS) integrated-circuit wafers. The intended purpose of this work is to fabricate nonvolatile-element memory test structures for electrical and radiation characterization studies. A number of critical processing issues dealing with the etching of the PZT films and the deposition and definition of the top and bottom platinum electrodes were addressed and suitable solutions found during the course of this work. Using the procedures described herein, we fabricated working PZT capacitors and evaluated them electrically.

  2. 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.

  3. Application of sol-gel-developed integrated optic devices to biochemical fiber optic sensors based on polarimetric interferometry

    NASA Astrophysics Data System (ADS)

    Gnyba, Marcin; Wierzba, Pawel; Plucinski, Jerzy

    2004-07-01

    Principles of integrated optical sensors based on polarimetric interferometry are presented in the paper. A wide area of their applications in biochemistry includes monitoring of protein concentration in solutions, detection of antibodies as well as indirect investigation of chemical reactions, based on precise measurement of complex refractive index. In order to address a problem of irreversibility of wide group of biological processes and chemical reactions as well as to decrease cost of the sensors, authors propose to develop disposable measurement converters and to use optical components made from sol-gel derived hybrid polymers. The technology of hybrid materials synthesis and subsequent planar waveguides manufacturing as well as their properties are shown.

  4. "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.

  5. 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.

  6. Synthesis of Carbon Nanotubes Using Sol Gel Route

    NASA Astrophysics Data System (ADS)

    Abdel-Fattah, Tarek

    2002-12-01

    Since 1990, carbon nanotubes were discovered and they have been the object of intense scientific study ever since. A carbon nanotube is a honeycomb lattice rolled into a cylinder. The diameter of a carbon nanotube is of nanometer size and the length is in the range of micrometer. Many of the extraordinary properties attributed to nanotubes, such as tensile strength and thermal stability, have inspired predictions of microscopic robots, dent-resistant car bodies and earthquake-resistant buildings. The first products to use nanotubes were electrical. Some General Motors cars already include plastic parts to which nanotubes were added; such plastic can be electrified during painting so that the paint will stick more readily. Two nanotube-based lighting and display products are well on their way to market. In the long term, perhaps the most valuable applications will take further advantage of nanotubes' unique electronic properties. Carbon nanotubes can in principle play the same role as silicon does in electronic circuits, but at a molecular scale where silicon and other standard semiconductors cease to work. There are several routes to synthesize carbon nanotubes; laser vaporization, carbon arc and vapor growth. We have applied a different route using sol gel chemistry to obtain carbon nanotubes. This work is patent-pending.

  7. Mechanisms of silk fibroin sol-gel transitions.

    PubMed

    Matsumoto, Akira; Chen, Jingsong; Collette, Adam L; Kim, Ung-Jin; Altman, Gregory H; Cebe, Peggy; Kaplan, David L

    2006-11-01

    Silk fibroin sol-gel transitions were studied by monitoring the process under various physicochemical conditions with optical spectroscopy at 550 nm. The secondary structural change of the fibroin from a disordered state in solution to a beta-sheet-rich conformation in the gel state was assessed by FTIR and CD over a range of fibroin concentrations, temperatures, and pH values. The structural changes were correlated to the degree of gelation based on changes in optical density at 550 nm. No detectable changes in the protein secondary structure (FTIR, CD) were found up to about 15% gelation (at 550 nm), indicating that these early stages of gelation are not accompanied by the formation of beta-sheets. Above 15%, the fraction of beta-sheet linearly increased with the degree of gelation. A pH dependency of gelation time was found with correlation to the predominant acidic side chains in the silk. Electrostatic interactions were related to the rate of gelation above neutral pH. The overall independencies of processing parameters including concentration, temperature, and pH on gel formation and protein structure can be related to primary sequence-specific features in the molecular organization of the fibroin protein. These findings clarify aspects of the self-assembly of this unique family of proteins as a route to gain control of material properties, as well as for new insight into the design of synthetic silk-biomimetic polymers with predictable solution and assembly properties.

  8. /dopamine films prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  9. Sol-gel template synthesis of semiconductor nanostructures

    SciTech Connect

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

    1997-03-01

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

  10. Functionalization of ceramic tile surface by sol-gel technique.

    PubMed

    Bondioli, F; Taurino, R; Ferrari, A M

    2009-06-15

    The aim of this investigation was the surface functionalization of industrial ceramic tiles by sol-gel technique to improve at the same time the cleanability of unglazed surfaces. This objective was pursued through the design and preparation of nanostructured coating that was deposited on polished unglazed tiles by air-brushing. In particular TiO(2)-SiO(2) binary film with 1, 2 or 5wt% of titania were prepared by using tetraethoxysilane and titania nanoparticles as precursors. The obtained films were characterized by scratch tests to verify the adhesion of the coatings to the polished tiles. To mainly evaluate the effect of the thermal treatment (temperature range 100-600 degrees C) on the photocatalicity of the coatings, the films were studied under UV exposure by contact angle measurements and cleanability test. Particular attention has been paid to preserve the aesthetical aspect of the final product and the obtained hue variation was evaluated by means of UV-visible spectroscopy and colorimetric analysis.

  11. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-09-01

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

  13. 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.

  14. 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. PMID:23798771

  15. New low temperature multiphase ferroelectric films

    NASA Astrophysics Data System (ADS)

    Bescher, Eric; Xu, Yuhuan; Mackenzie, J. D.

    2001-06-01

    This article describes the low-temperature synthesis of new multiphase ferroelectrics containing an inorganic ferroelectric phase entrapped in amorphous silica or in an organically modified silicate (ormosil). Sol gel derived LiNbO3 and BaTiO3 crystals were grown in SiO2 and in RSiO1.5 glass where R contains a chromophore (TDP) insensitive to hydrolysis and condensation reactions. The LiNbO3-SiO2 and BaTiO3-SiO2 compositions as well as the TDP-LiNbO3-SiO2 and TDP-BaTiO3-SiO2 ormosils exhibit ferroelectric-like properties. This unusual characteristic is due to the presence of small, partially ordered crystallites of the ferroelectric, dispersed in the amorphous matrix. In addition to their ferroelectric properties, the ormosils also exhibit interesting optical characteristics: the TDP-BaTiO3-SiO2 materials are red, whereas the TDP-LiNbO3-SiO2 are yellow. The materials described in this article are representative of two new classes of weak ferroelectrics. In the first class, a ferroelectric is dispersed in an amorphous matrix. The second class may be called "organically-modified crystals": small ferroelectric crystals embedded in an organically modified matrix. The fabrication of such materials is possible for inorganic crystalline phases forming at temperatures below the decomposition temperature of the organic (about 250 °C). This article also contains some theoretical considerations explaining why these materials, although amorphous by x-ray diffraction, exhibit ferroelectric-like properties.

  16. 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.

  17. Solid-state tunable lasers based on dye-doped sol-gel materials

    SciTech Connect

    Dunn, B.; Mackenzie, J.D.; Zink, J.I.; Stafsudd, O.M.

    1992-03-01

    The sol-gel process is a solution synthesis technique which provides a low temperature chemical route for the preparation of rigid transparent matrix materials. The luminescent organic dye molecules, rhodamine 6G and coumarin 540A have been incorporated, via the sol-gel method, into aluminosilicate and organically modified silicate host matrices. Synthesis, laser oscillation and photostability for these systems are reported. The improved photostability of these materials with respect to comparable polymeric host materials is discussed.

  18. 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.

  19. 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.

  20. 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.

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

    PubMed

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

    2016-03-01

    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.

  2. Characterizing the hierarchical structures of bioactive sol-gel silicate glass and hybrid scaffolds for bone regeneration.

    PubMed

    Martin, R A; Yue, S; Hanna, J V; Lee, P D; Newport, R J; Smith, M E; Jones, J R

    2012-03-28

    Bone is the second most widely transplanted tissue after blood. Synthetic alternatives are needed that can reduce the need for transplants and regenerate bone by acting as active temporary templates for bone growth. Bioactive glasses are one of the most promising bone replacement/regeneration materials because they bond to existing bone, are degradable and stimulate new bone growth by the action of their dissolution products on cells. Sol-gel-derived bioactive glasses can be foamed to produce interconnected macropores suitable for tissue ingrowth, particularly cell migration and vascularization and cell penetration. The scaffolds fulfil many of the criteria of an ideal synthetic bone graft, but are not suitable for all bone defect sites because they are brittle. One strategy for improving toughness of the scaffolds without losing their other beneficial properties is to synthesize inorganic/organic hybrids. These hybrids have polymers introduced into the sol-gel process so that the organic and inorganic components interact at the molecular level, providing control over mechanical properties and degradation rates. However, a full understanding of how each feature or property of the glass and hybrid scaffolds affects cellular response is needed to optimize the materials and ensure long-term success and clinical products. This review focuses on the techniques that have been developed for characterizing the hierarchical structures of sol-gel glasses and hybrids, from atomic-scale amorphous networks, through the covalent bonding between components in hybrids and nanoporosity, to quantifying open macroporous networks of the scaffolds. Methods for non-destructive in situ monitoring of degradation and bioactivity mechanisms of the materials are also included.

  3. 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.

  4. Characterization of Hafnia Powder Prepared from an Oxychloride Sol Gel

    SciTech Connect

    McGilvery, Catriona M.; De Gendt, S; Payzant, E Andrew; MacKenzie, M; Craven, A J; McComb, D W

    2011-01-01

    Hafnium containing compounds are of great importance to the semiconductor industry as a replacement for Si(O,N) with a high- gate dielectric. Whilst Hf is already being incorporated into working devices1, much is still to be understood about it. Here we investigate the crystallisation processes and chemistry of bulk HfO2 powders which will aid in interpretation of reactions and crystallisation events occurring in thin films used as gate dielectrics. Amorphous HfO2 powder was prepared via a sol-gel route using hafnium oxychloride (HfOCl2 xH2O) as a precursor. The powders were subjected to various heat treatments and analysed using x-ray diffraction (XRD) and thermal analysis techniques. It was found that a large change in the crystallisation pathway occurred when the sample was heated in an inert environment compared with in air. Instead of the expected monoclinic phase (m-HfO2), tetragonal HfO2 (t-HfO2) also formed under these conditions and was observed up to temperatures of ~760 C. The t-HfO2 particles, which are less than 30nm in size, eventually transform into m-HfO2 on further heating. Possible mechanisms for the crystallisation of t-HfO2 are discussed. It is proposed that within this temperature range t-HfO2 is stabilised due to the presence of oxygen vacancies in the inert environment, forming by the reduction of HfIV to HfIII. As the crystal grows in size as the temperature increases there are too few oxygen vacancies left in the structure to continue stabilising the t-HfO2 phase and so transformation to m-HfO2 occurs.

  5. Densification and crystallization of zirconia thin films prepared by sol-gel processing

    SciTech Connect

    Schwartz, R.W.; Voigt, J.A.; Buchheit, C.D.; Boyle, T.J.

    1993-12-31

    We have investigated the effects of precursor nature and heat treatment schedule on the densification and crystallization behavior of sol-gel derived zirconia thin films. Precursor solutions were prepared from n-propanol, zirconium (IV) n-propoxide, and either acetic acid, or 2,4-pentanedione (acac) and water additions. By controlling the ligand type and ligand-to-metal ratio, we were able to prepare films which displayed significant differences in densification behavior. We attribute the dissimilarity in densification to variations in the nature of the as-deposited films, as influenced by ligand type and concentration. While the acac- derived film was a physical gel, (i.e., a physical aggregation of the oligomeric species), the acetic acid-derived film, which exhibited less consolidation, was a chemical gel that could not be redissolved in the parent solvent. Films prepared with large acac/metal ratios and small water additions exhibited minimal crosslinking at 25{degree}C, displayed the greatest consolidation ({approximately}86% shrinkage) and the highest refractive index (n = 2.071) when heat treated. These results indicate the importance that M-O-M bonds (crosslinks) formed at low temperature can have on densification behavior. We also report on the effects of heat-treatment schedules and ramp rates on densification behavior. All of the films of the present study crystallized into the cubic phase, at temperatures ranging from {approximately}400{degree}C to greater than 700{degree}C, depending on the heating rate.

  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. Dynamics of Proteins Encapsulated in Silica Sol-gel Glasses Studied with IR Vibrational Echo Spectroscopy

    PubMed Central

    Massari, Aaron M.; Finkelstein, Ilya J.; Fayer, Michael D.

    2008-01-01

    Spectrally-resolved infrared stimulated vibrational echo spectroscopy is used to measure the fast dynamics of heme-bound CO in carbonmonoxy-myoglobin (MbCO) and hemoglobin (HbCO) embedded in silica sol-gel glasses. On the time scale of ~100 fs to several ps, the vibrational dephasing of the heme-bound CO is measurably slower for both MbCO and HbCO relative to aqueous protein solutions. The fast structural dynamics of MbCO, as sensed by the heme-bound CO, are influenced more by the sol-gel environment than those of HbCO. Longer time scale structural dynamics (tens of ps), as measured by the extent of spectral diffusion, are the same for both proteins encapsulated in sol-gel glasses compared to aqueous solutions. A comparison of the sol-gel experimental results to viscosity dependent vibrational echo data taken on various mixtures of water and fructose shows that the sol-gel encapsulated MbCO exhibits dynamics that are the equivalent to the protein in a solution that is nearly 20 times more viscous than bulk water. In contrast, the HbCO dephasing in the sol-gel reflects only a 2-fold increase in viscosity. Attempts to alter the encapsulating pore size by varying the molar ratio of silane precursor to water (R-value) used to prepare the sol-gel glasses were found to have no effect on the fast or steady-state spectroscopic results. The vibrational echo data are discussed in the context of solvent confinement and protein-pore wall interactions to provide insights into the influence of a confined environment on the fast structural dynamics experienced by a biomolecule. PMID:16551107

  8. Non-hydrolytic Sol-gel Synthesis of Tin Sulfides

    NASA Astrophysics Data System (ADS)

    Kaur, Rajvinder

    The non-hydrolytic sol-gel (NHSG) process is an effective low temperature route well known for preparing homogeneous metal oxides. Thermodynamically as well as kinetically favored products, which cannot be prepared with the traditional solid-state routes, can be produced using NHSG. This project is focused on the exploration of NHSG synthesis of binary tin sulfides. In the past few years, metal sulfides have been the subject of significant interest. Much effort has been devoted to understand these materials because of their potential applications in electronic, optical, and superconductor devices.4 Among these materials, tin sulfides are materials of technological importance, which are being explored as semiconductors, anode materials for Li ion batteries, photoconductors, photocatalysts and absorber layer materials in photovoltaic solar cell devices. All of these applications depend upon features like homogeneity, oxidation state, high surface area and purity of the materials. These properties can be difficult to achieve by employing traditional synthetic routes, which require high temperatures due to slow diffusion, limiting the products to thermodynamically stable phases and prohibiting control over properties like particle size and surface area. A variety of low temperature methods are being explored due to the increased demand for such advanced materials. This project is focused on exploring the NHSG approach to synthesize binary tin sulfides, with the main goal of establishing conditions for the targeted synthesis of different tin sulfide polymorphs with controlled particle size. Being non-oxide materials, tin sulfides can be air sensitive, which requires special attention in handling. All reactions were carried out in absence of oxygen. This project explores the reaction of tin halides with thioethers in a dry solvent medium, leading to the formation of tin sulfides. There are a number of synthetic parameters that can be varied for the NHSG approach. A

  9. 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.

  10. 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.

  11. Asymmetric bioreduction of acetophenones by Baker's yeast and its cell-free extract encapsulated in sol-gel silica materials

    NASA Astrophysics Data System (ADS)

    Kato, Katsuya; Nakamura, Hitomi; Nakanishi, Kazuma

    2014-02-01

    Baker's yeast (BY) encapsulated in silica materials was synthesized using a yeast cell suspension and its cell-free extract during a sol-gel reaction of tetramethoxysilane with nitric acid as a catalyst. The synthesized samples were fully characterized using various methods, such as scanning electron microscopy, nitrogen adsorption-desorption, Fourier transform infrared spectroscopy, thermogravimetry, and differential thermal analysis. The BY cells were easily encapsulated inside silica-gel networks, and the ratio of the cells in the silica gel was approximately 75 wt%, which indicated that a large volume of BY was trapped with a small amount of silica. The enzyme activity (asymmetric reduction of prochiral ketones) of BY and its cell-free extract encapsulated in silica gel was investigated in detail. The activities and enantioselectivities of free and encapsulated BY were similar to those of acetophenone and its fluorine derivatives, which indicated that the conformation structure of BY enzymes inside silica-gel networks did not change. In addition, the encapsulated BY exhibited considerably better solvent (methanol) stability and recyclability compared to free BY solution. We expect that the development of BY encapsulated in sol-gel silica materials will significantly impact the industrial-scale advancement of high-efficiency and low-cost biocatalysts for the synthesis of valuable chiral alcohols.

  12. 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.

  13. 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.

  14. 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.

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

    PubMed

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

    2004-02-01

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

  16. 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.

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

    PubMed

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

    2004-02-01

    The effects of various salts on the sol-gel transition of aqueous methylcellulose (MC) solutions have been studied systematically by means of a micro differential scanning calorimeter. It was found that the heating process was endothermic while the cooling process was exothermic for both MC solutions with and without salts. The addition of salts did not change the patterns of gelation and degelation of MC. However, the salts could shift the sol-gel transition and the gel-sol transition to lower or higher temperatures from a pure MC solution, depending on the salt type. These opposite effects were termed the salt-assisted and salt-suppressed sol-gel transitions. Either the salt-assisted transition or the salt-suppressed sol-gel transition was a function of salt concentration. In addition, each salt was found to have its own concentration limit for producing a stable aqueous solution of MC at a given concentration of MC, which was related to the anionic charge density of the salt. Cations were proved to have weaker effects than anions. The "salt-out strength", defined as the salt effect per mole of anion, was obtained for each anion studied. The thermodynamic mechanisms involved in the salt-assisted and salt-suppressed sol-gel transitions are discussed. PMID:15773087

  18. From inulin to fructose syrups using sol-gel immobilized inulinase.

    PubMed

    Santa, Gonçalo L M; Bernardino, Susana M S A; Magalhães, Salomé; Mendes, Vanessa; Marques, Marco P C; Fonseca, Luís P; Fernandes, Pedro

    2011-09-01

    The present work aims to provide the basic characterization of sol-gel immobilized inulinase, a biocatalyst configuration yet unexploited, using as model system the hydrolysis of inulin to fructose. Porous xerogel particles with dimensions in slight excess of 10 μm were obtained, yielding an immobilization efficiency of roughly 80%. The temperature- and pH-activity profiles displayed a broader bell-shaped pattern as a result of immobilization. In the latter case, a shift of the optimal pH of 0.5 pH units was observed towards a less acidic environment. The kinetic parameters estimated from the typical Michaelis-Menten kinetics suggest that immobilization in sol-gel did not tamper with the native enzyme conformation, but on the other hand, entrapment brought along mass transfer limitations. The sol-gel biocatalyst displayed a promising operational stability, since it was used in more than 20 consecutive 24-hour batch runs without noticeable decay in product yield. The performance of sol-gel biocatalyst particles doped with magnetite roughly matched the performance of simple sol-gel particles in a single batch run. However, the operational stability of the former proved poorer, since activity decay was evident after four consecutive 24-hour batch runs. PMID:21445597

  19. Sol-gel prepared glass for micro-optical elements and arrays

    NASA Astrophysics Data System (ADS)

    Haruvy, Yair; Gilath, Irith; Maniewictz, M.; Eisenberg, Naftali P.

    1997-09-01

    Sol-gel processes of metal alkoxides involve hydrolysis of the alkoxy groups and condensation to a 3-D oxide glass network. Volume reduction of the drying gel typically results in cracking, unless sufficient relaxation is allowed to take place. Further, the common shrinkage by a factor of 2.5 and higher imposes great difficulty to obtain dimensional accuracy in thus prepared micro-optical elements. The new fast sol-gel method enables facile preparation of siloxane-based glassy materials in which polymerization is completed within minutes and curing within a few hours. The optical quality of thin films obtained by the fast sol-gel method and the ease of preparation makes this method technologically and economically attractive for micro-lenses and micro-optical arrays by replication. Micro-optical arrays are highly patterned, including sharp curvatures of small radii. This necessitates to study primarily two aspects of the sol-gel replication process: (1) the chemical constitution of the sol-gel and the reaction pathway that ensures prompt adhesion to the template during the process. (2) the surface chemical adaptation of the template that allows timing of adhesion and release of the produced elements. The adaptation of this process to the desired replication is described. Thence, the results of preliminary fabrication of micro-optical elements and arrays by this method are shown and their features discussed.

  20. 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.

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

    SciTech Connect

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

    2006-11-20

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

  2. High quality factor Er-doped Fabry-Perot microcavities by sol-gel processing

    NASA Astrophysics Data System (ADS)

    Li, Yigang; Fortes, Luís M.; Chiappini, Andrea; Ferrari, Maurizio; Almeida, Rui M.

    2009-10-01

    An optimized sol-gel process was developed to fabricate 1D photonic bandgap structures. Several erbium-doped Fabry-Perot microcavities were prepared and characterized. The thickest sample contained two Bragg mirrors, each having 12 distributed Bragg reflector periods of alternating silicate glass and titania layers. The total thickness of this sample reached ~12 µm. The Er3+ photoluminescence spectra at 1.5 µm were measured for the microcavities. A quality factor of 250 and an Er3+ photoluminescence enhancement of 96 times at 1.5 µm have been reached. The sol-gel processing details, the crystallization of the titania films and the refractive index of the deposited materials are discussed in detail. The simulated optical spectra of the microcavities were found to agree well with the actually measured curves. These results demonstrate that the present sol-gel processing technique is of potential interest for low cost fabrication of 1D photonic bandgap devices.

  3. Crown ether-doped sol-gel materials for strontium(II) separation

    PubMed

    Yost; Fagan; Allain; Barnes; Dai; Sepaniak; Xue

    2000-11-01

    Hybrid organic/inorganic sol-gel materials containing an encapsulated crown ether ligand were found to selectively remove 91.4 +/- 1.3% of Sr2+ from a solution containing excess of competing ions such as Ca2+. The crown ether ligand, 1,4,10,13-tetraoxa-7,16-diazacyclooctadecane-7,16-bis(malonate) ligand (Na4oddm), with known high affinity for Sr2+ was encapsulated in hydrophilic SiO2 through a simple sol-gel process. Washing the Sr(2+)-loaded gel with acid or ethylenediaminetetraacetic acid disodium salt recovered the Sr2+ from the sol-gel sorbent and regenerated the doped gel for subsequent Sr2+ intake. The approach reported here is a new alternative to the use of crown ethers in metal ion separation through, for example, solvent extraction or the use of sorbents containing chemically grafted crown ether ligands. PMID:11080909

  4. Size selected silicon particles in sol-gel glass by centrifugal processing

    NASA Astrophysics Data System (ADS)

    Duval, David J.; McCoy, Benjamin J.; Risbud, Subhash H.; Munir, Zuhair A.

    1998-02-01

    Centrifugal processing was used to induce size selectivity in Si particles suspended in a silica sol-gel precursor solution. A model was developed to describe Stokes settling of the silicon particles in the sol-gel medium whose viscosity increases exponentially with time eventually leading to hardening to a solid glassy material. An empirical modification to the theoretical model accounts for settling of particle agglomerates. Experimental results for polydisperse silicon particulates centrifuged in a sol-gel of tetraethyl orthosilicate catalyzed by phosphoric acid are reported; the particle size and spatial distribution in the gelled matrix are explained by the model. The utility of centrifugal processing to produce functionally graded materials and semiconductor nanostructures is discussed.

  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. Direct Patterning on Sol-Gel Low-k Porous Silica by Thermal Nanoimprinting

    NASA Astrophysics Data System (ADS)

    Makoto Okada,; Takahiro Nakayama,; Yuji Kang,; Yuichi Haruyama,; Kazuhiro Kanda,; Shinji Matsui,

    2010-06-01

    The direct patterning of low-dielectric constant (low-k) materials via nanoimprint lithography (NIL) has the potential to simplify fabrication processes and significantly reduce the manufacturing costs of semiconductor devices. It is known that a low k is realized by introducing a large number of nanoscale pores into a material. We demonstrated nanoimprinting on a sol-gel low-k material (k˜ 2.0) formed using methyl silicate as a siloxane oligomer source and surfactants as a pore template. As a result, 200-nm-linewidth mold patterns were successfully transferred onto the sol-gel low-k material by thermal nanoimprinting at 200 °C. However, pattern shrinkage was observed. The imprinted pattern linewidth was 180 nm. We assumed from the Fourier transform infrared spectroscopy (FT-IR) spectra of the sol-gel film before and after baking that the pattern shrinkage was induced by the condensation reaction.

  7. Direct Patterning on Sol-Gel Low-k Porous Silica by Thermal Nanoimprinting

    NASA Astrophysics Data System (ADS)

    Okada, Makoto; Nakayama, Takahiro; Kang, Yuji; Haruyama, Yuichi; Kanda, Kazuhiro; Matsui, Shinji

    2010-06-01

    The direct patterning of low-dielectric constant (low-k) materials via nanoimprint lithography (NIL) has the potential to simplify fabrication processes and significantly reduce the manufacturing costs of semiconductor devices. It is known that a low k is realized by introducing a large number of nanoscale pores into a material. We demonstrated nanoimprinting on a sol-gel low-k material (k˜2.0) formed using methyl silicate as a siloxane oligomer source and surfactants as a pore template. As a result, 200-nm-linewidth mold patterns were successfully transferred onto the sol-gel low-k material by thermal nanoimprinting at 200 °C. However, pattern shrinkage was observed. The imprinted pattern linewidth was 180 nm. We assumed from the Fourier transform infrared spectroscopy (FT-IR) spectra of the sol-gel film before and after baking that the pattern shrinkage was induced by the condensation reaction.

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

    SciTech Connect

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

    1996-08-01

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

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

    SciTech Connect

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

    1992-11-03

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

  10. 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.

  11. The sol-gel entrapment of noble metals in hybrid silicas: a molecular insight

    PubMed Central

    2013-01-01

    Background Why are metal nanoparticles sol-gel entrapped in ORMOSIL so active and stable? In other words, why ORMOSIL-entrapped metal nanoparticles are more active and selective than many heterogenized counterparts, including silica-entrapped noble metals? Results Unveiling specific interactions between MNPs and the molecular structure of ORMOSIL, this work investigates subtle structural aspects through DRIFT spectroscopy. Conclusions The results point to interactions between entrapped Pd and Pt nanocrystallites with the organosilica sol-gel cages similar to those taking place in enzymes. PMID:24079552

  12. 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.

  13. 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.

  14. 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.

  15. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2013-11-01

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

  17. 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...

  18. 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.

  19. Optical and dielectric properties of BiMn1-xAExO3 (AE=Cr, Fe, Co, and Zn; x=0, 0.1) nanoparticles synthesized by sol-gel technique

    NASA Astrophysics Data System (ADS)

    Bhardwaj, Neha; Gaur, Anurag; Yadav, Kamlesh

    2015-08-01

    BiMnO3 is a multiferroic material which means that it shows both the ferroelectricity and ferromagnetism. Present study deals about the study of optical and dielectric properties of BiMnO3 and doped BiMnO3. The magnetic and non magnetic ions are introduced as dopants in place of Mn sublattice, BiMn1-xAExO3 (where x=0.1 and AE= Cr, Fe, Co, and Zn). We have synthesized nanoparticles of BiMnO3 and BiMn1-xAExO3 (where x=0.1 and AE= Cr, Fe, Co, and Zn) by sol-gel technique. Optical properties have been studied by using FTIR (Fourier Transform Infrared) spectroscopy. FTIR (Fourier Transform Infrared Spectroscopy) analysis showed that there is an increase in the band gap of BiMn1-xAExO3 (where x=0.1 and AE= Cr, Fe, Co, and Zn) than pure BiMnO3 for the samples synthesized by sol-gel technique. The increase in band gap on doping is due to the radius to charge ratio. Ferroelectric hysteresis loop confirms the presence of ferroelectricity in BiMnO3. From the ferroelectric hysteresis loop the parameters like coericivity, saturation polarization and remanant polarization has been calculated. Nanoparticles of BiMnO3 have applications in memory storage devices.

  20. 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.

  1. 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.

  2. 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. PMID:26322304

  3. 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.

  4. 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

  5. Two substrate-confined sol-gel coassembled ordered macroporous silica structures with an open surface.

    PubMed

    Guo, Wenhua; Wang, Ming; Xia, Wei; Dai, Lihua

    2013-05-21

    A sol-gel cooperative assembly method was demonstrated for the fabrication of inverse opal films with an open surface. In this method, a sol-gel silicate precursor was cooperatively assembled into the interstitial spaces of microspheres at the same time when polystyrene templates formed in between two desired substrates. Silica inverse opals with a three-dimensional ordered macroporous (3DOM) structure were obtained after selective removing the colloidal templates by calcination. The open surfaces with a high degree of interconnected porosity and extremely uniform pore size were characterized by scanning electron microscope (SEM). Optical transmission spectra reveals the existence of considerable deep band gaps of up to 70% and steep band edges of up to 6%/nm in the [111] directions of the 3DOM silica samples. A little shrinkage confirmed by transmission spectra is not larger than 3%, in consistent with the results measured by SEM, which revealing the sufficient and compact infiltration into the interstitial spaces by our confined sol-gel coassembly method. With different incidence angles, the positions of pseudogaps can be easily tuned in the wide range from 720 nm to 887 nm, agreed well with the calculated values by the Bragg law. All the results prove that the sol-gel coassembly method with two substrates confinement is a simple, low cost, convenient and versatile method for the fabrication of silica inverse opals without overlayers in large domains. PMID:23614663

  6. Sol-gel coating of inorganic nanostructures with resorcinol-formaldehyde resin.

    PubMed

    Li, Na; Zhang, Qiao; Liu, Jian; Joo, Jibong; Lee, Austin; Gan, Yang; Yin, Yadong

    2013-06-01

    A general sol-gel process has been developed to form a coating of resorcinol-formaldehyde (RF) resin on inorganic nanostructures of various compositions and morphologies. The RF shell can be conveniently converted into carbon through high temperature carbonization under an inert atmosphere.

  7. Sol-gel optics: Proceedings SPIE-The International Society for Optical Engineering

    NASA Astrophysics Data System (ADS)

    MacKenzie, John D.; Ulrich, Donald R.

    1992-03-01

    This conference produced the first proceedings on sol-gel optics. The proceedings include reports on the attempts to fabricate semiconductor-in-glass quantum-well confinement lenses. The successful preparation of organic dyes-in-oxides laser elements is discussed, as well as research on the fabrication of grooved glass discs through the mechanical patterning of the soft gels.

  8. 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

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. The influence of surfactants on the roughness of titania sol-gel films

    SciTech Connect

    Medina-Valtierra, Jorge . E-mail: jormeval@yahoo.com; Frausto-Reyes, Claudio . E-mail: cfraus@cio.mx; Calixto, Sergio . E-mail: scalixto@cio.mx; Bosch, Pedro . E-mail: lacv@xanum.uam.mx

    2007-03-15

    Substrate dipping in a composite sol-gel solution was used to prepare both smooth and rough thin films of titanium dioxide (TiO{sub 2}) on commercial fiberglass. The deposition of a composite film was done in a beaker using a solution of titanium (IV) isopropoxide as the sol-gel precursor and cetyltrimethyl ammonium bromide as the surfactant. In order to establish a correlation between experimental conditions and the titanium oxide produced, as well as the film quality, the calcined samples were characterized using Raman spectroscopy, UV-vis spectrophotometry, scanning electron microscopy and atomic force microscopy. One of the most important results is that a 61-nm TiO{sub 2} film was obtained with a short immersion of fiberglass into the sol-gel without surfactant. In other cases, the deposited film consisted of a titanium precursor gel encapsulating micelles of surfactant. The gel films were converted to only the anatase phase by calcining them at 500 deg. C. The resulting films were crystalline and exhibited a uniform surface topography. In the present paper, it was found that the TiO{sub 2} films prepared from the sol-gel with a surfactant showed a granular microstructure, and are composed of irregular particles between 1.5 and 3 {mu}m. Smooth TiO{sub 2} films could have useful optical and corrosion-protective properties and, on other hand, roughness on the TiO{sub 2} films can enhance the inherent photocatalytic activity.

  16. Sol-gel fabrication of one-dimensional photonic crystals with predicted transmission spectra

    NASA Astrophysics Data System (ADS)

    Ilinykh, V. A.; Matyushkin, L. B.

    2016-08-01

    One-dimensional multilayer structures of periodically alternating low refractive index (silica) and high refractive index (titania) materials have been deposited by sol-gel spincoating. Experimental spectra of the structures are in agreement with spectra calculated by transfer matrix technique. As an example, theoretical and experimental spectra with a stop band corresponding 600 nm-reflection are shown.

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

    SciTech Connect

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

    2009-02-01

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

  18. Gilded nanoparticles for plasmonically enhanced fluorescence in TiO2:Sm3+ sol-gel films

    NASA Astrophysics Data System (ADS)

    Pikker, Siim; Dolgov, Leonid; Heinsalu, Siim; Mamykin, Sergii; Kiisk, Valter; Kopanchuk, Sergei; Lõhmus, Rünno; Sildos, Ilmo

    2014-03-01

    Silica-gold core-shell nanoparticles were used for plasmonic enhancement of rare earth fluorescence in sol-gel-derived TiO2:Sm3+ films. Local enhancement of Sm3+ fluorescence in the vicinity of separate gilded nanoparticles was revealed by a combination of dark field microscopy and fluorescence spectroscopy techniques. An intensity enhancement of Sm3+ fluorescence varies from 2.5 to 10 times depending on the used direct (visible) or indirect (ultraviolet) excitations. Analysis of fluorescence lifetimes suggests that the locally stronger fluorescence occurs because of higher plasmon-coupled direct absorption of exciting light by the Sm3+ ions or due to plasmon-assisted non-radiative energy transfer from the excitons of TiO2 host to the rare earth ions.

  19. 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

  20. 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

  1. 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.

  2. 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.

  3. Stable ferroelectric liquid crystals derived from salicylaldimine-core.

    PubMed

    Veerabhadraswamy, Bhyranalyar N; Rao, D S Shankar; Yelamaggad, Channabasaveshwar V

    2015-03-26

    Five pairs of enantiomers derived from salicylaldimine-core have been prepared by condensing (R)- or (S)-4-(octan-2-yloxy)anilines with 4-formyl-3-hydroxyphenyl 4-(n-alkoxy)benzoates. They have been designed to probe the correlation between molecular structure and mesomorphism, and especially to provide stable mesogens having potential for applications in ferroelectric liquid crystal devices. Thus, they have been substituted with a chiral tail at one end and by n-alkoxy chains of varying length at the other terminal. A detailed study confirms an indistinguishable behavior of all ten mesogens exhibiting an enantiotropic chiral smectic C (SmC*) phase besides blue phase (BP) and chiral nematic (N*) phase. The SmC* phase occurring over a 50-70 °C thermal width shows ferroelectric switching with spontaneous polarization (Ps) value crossing over 100 nC/cm(2). Circular dichroism spectroscopic study of the mesophases confirms the chromophores of the molecules being in the macroscopic chiral (helical) environment.

  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. Effect of PMMA impregnation on the fluorescence quantum yield of sol-gel glasses doped with quinine sulfate

    NASA Astrophysics Data System (ADS)

    Meneses-Nava, M. A.; Barbosa-García, O.; Díaz-Torres, L. A.; Chávez-Cerda, S.; Torres-Cisneros, M.; King, T. A.

    2001-08-01

    The fluorescence quantum yield of quinine sulfate in sol-gel and PMMA impregnated glasses is measured. The observed quantum yield improvement in the sol-gel matrix, compared to ethanol, is interpreted as a reduction of non-radiative relaxation channels by isolation of the molecules by the cage of the glass. PMMA impregnated sol-gel glasses show an extra improvement of the fluorescence yield, which is interpreted as a reduction of the free space and the rigid fixation of the molecules to the matrix.

  6. Ferroelectric properties of PZT/BFO multilayer thin films prepared using the sol-gel method

    PubMed Central

    2012-01-01

    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. PMID:22221519

  7. 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.

  8. 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.

  9. Sol-gel co-assembly of hollow cylindrical inverse opals and inverse opal columns.

    PubMed

    Haibin, Ni; Ming, Wang; Wei, Chen

    2011-12-19

    A facile approach of fabricating hollow cylindrical inverse opals and inverse opal columns by sol-gel co-assembly method was proposed. Polystyrene (PS) colloidal suspension added with hydrolyzed silicate precursor solution was used to self-assemble composite colloidal crystals which consist of PS colloidal crystal template and infiltrated silica gel in the interstitial of microspheres. Continuous hollow cylindrical composite colloidal crystal films have been produced on capillaries' outside and internal surface. Composite colloidal crystal columns which filling up the interior of a capillary were fabricated by pressure assisted sol-gel co-assembly method. Hollow cylindrical inverse opals and inverse opal columns were obtained after removing PS colloidal crystal from the composite colloidal crystal. Optical properties of the silica hollow cylindrical inverse opals were characterized by transmission spectrum and a stop band was observed. Structure and optical properties of the inverse opal columns were investigated. PMID:22274178

  10. High-efficiency sol-gel antireflection coatings for astronomical optics

    NASA Astrophysics Data System (ADS)

    Stilburn, James R.

    2000-08-01

    The antireflective properties of silica sol-gel coatings have been known for some time, and such coatings have bene used to reduce losses in the optical elements of high- powered lasers used in fusion experiments. Research at DAO has developed the technology to the pont where optical elements in three 4-meter class telescopes at CFHT, KPNO, and CTIO have benefitted from coatings made form high- efficiency sol-gel films. The process is attractive because it is simple to apply, is inexpensive, and is as effective as multi-layer vacuum-deposited coatings which it can replace. A description is given of the basic chemistry involved and the techniques used to apply the coatings. Techniques used to improve the durability of the films by hardening and waterproofing are described, as well as a two- layer coating in combination with magnesium fluoride.

  11. 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

  12. Effect of sol-gel modifications on formation and morphology of nanocrystalline lanthanum aluminate

    SciTech Connect

    Koc, S. Naci . E-mail: nacik@istanbul.edu.tr; Oksuzomer, Faruk; Yasar, Erdem; Akturk, Selcuk; Gurkaynak, M. Ali

    2006-12-14

    LaAlO{sub 3} powders are prepared by sol-gel method. The effect of preparation conditions on morphological properties and crystal formations are investigated. iso-Propanol/tert-butanol and ethyl acetoacetate/ethylene glycol monomethylether are used solvents and complexing agents, respectively. Samples are dried with conventional and freeze-drying methods and calcined between 600 and 1000 deg. C. TGA, DTA, XRD, SEM and TEM methods are used for characterization. It is observed that freeze-dried sample prepared with tert-butanol has the lowest LaAlO{sub 3} formation temperature and uniform rhombohedral crystals. But conventionally dried sample, prepared with iso-propanol has smallest agglomerates at 1000 deg. C and does not show clear crystallization temperature in DTA analysis. The XRD peaks of LaAlO{sub 3} crystal are observed at 600 deg. C for all samples prepared by various sol-gel conditions.

  13. 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.

  14. Chitosan-silane sol-gel hybrid thin films with controllable layer thickness and morphology.

    PubMed

    Spirk, Stefan; Findenig, Gerald; Doliska, Ales; Reichel, Victoria E; Swanson, Nicole L; Kargl, Rupert; Ribitsch, Volker; Stana-Kleinschek, Karin

    2013-03-01

    The preparation of thin films of chitosan-silane hybrid materials by combining sol-gel processing and spin coating is reported. A variety of silanes can be used as starting materials for the preparation of such thin films, namely tetraethoxysilane, tri-tert-butoxysilanol, trimethylethoxysilane, p-trifluoromethyltetra-fluorophenyltriethoxysilane, trivinylmethoxysilane, (methoxymethyl)trimethyl-silane, and hexamethoxydisilane. These silanes are subjected to a sol-gel process before they are added to acidic chitosan solutions. The chitosan:silane ratio is kept constant at 6:1 (w/w) and dilutions with ethanol are prepared and spin coated. Depending on the degree of dilution, film thickness can be controlled in a range between 5 and 70 nm. For the determination of additional surface properties, static water contact angle measurements and atomic force microscopy have been employed.

  15. 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

  16. 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.

  17. 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.

  18. Three-phase microemulsion/sol-gel system for aqueous catalysis with hydrophobic chemicals.

    PubMed

    Abu-Reziq, Raed; Blum, Jochanan; Avnir, David

    2004-02-20

    A facile three-phase transport process is described that allows to carry out catalytic reactions in water, whereby all components are hydrophobic. According to this process a hydrophobic substrate is microemulsified in water and subjected to an organometallic catalyst, which is entrapped within a partially hydrophobized sol-gel matrix. The surfactant molecules, which carry the hydrophobic substrate, adsorb/desorb reversibly on the surface of the sol-gel matrix breaking the micellar structure, spilling their substrate load into the porous medium that contains the catalyst. A catalytic reaction then takes place within the ceramic material to form the desired products that are extracted by the desorbing surfactant, carrying the emulsified product back into the solution. The method is general and versatile and has been demonstrated with the catalytic hydrogenations of alkenes, alkynes, aromatic C=C bonds, and nitro and cyano groups.

  19. 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.

  20. 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.

  1. 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

  2. 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.

  3. 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.

  4. 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.

  5. Chemically active organically doped sol-gel materials: enzymatic sensors, chemical sensors, and photoactive materials

    NASA Astrophysics Data System (ADS)

    Avnir, David; Braun, S.; Lev, Ovadia; Ottolenghi, M.

    1992-12-01

    Organically-doped porous sol-gel matrices of optical grade have evolved in recent years into a wide class of materials with diverse applications. We review recent progress made in our laboratories in three domains of applications: the trapping of enzymes with the consequent design of (e.g. glucose) sensors; the development of chemical sensors; and the design of photoactive material for (solar) light energy conversion.

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

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

    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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Secondary Crystal Growth on a Cracked Hydrotalcite-Based Film Synthesized by the Sol-Gel Method.

    PubMed

    Lee, Wooyoung; Lee, Chan Hyun; Lee, Ki Bong

    2016-05-01

    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.

  13. 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.

  14. Controllable synthesis of hollow mesoporous silica particles by a facile one-pot sol-gel method.

    PubMed

    Song, Jing-Chuan; Xue, Fei-Fei; Lu, Zhong-Yuan; Sun, Zhao-Yan

    2015-07-01

    A simple and facile one-pot sol-gel method is proposed for the fabrication of hollow mesoporous silica particles. Both the particle size and the shell thickness can be well controlled by moderately tuning some experimental parameters.

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

    NASA Astrophysics Data System (ADS)

    Vinogradov, Vladimir V.; Avnir, David

    2015-09-01

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

  16. Synthesization of Nanostructured Titanium Dioxide at Low Molarity of Sol-Gel Process

    NASA Astrophysics Data System (ADS)

    Maarof, S. K. M.; Abdullah, S.; Rusop, M.

    2013-06-01

    Titanium dioxide, TiO2 is one of the semiconductor materials. The aim of this paper is to determine the production of TiO2 by sol-gel method. The sol-gel method used because this method is quite simple compare to other methods such as dip-coated and refractive sputtering. The parameter will be used in this paper is the concentration. The sol-gel TiO2 solution then spin coated on the glass substrate to form homogenous and transparent thin film. The thin film was coated at 8 layers to adjust the refractive index characteristics and to get the clear images during characterize by spin coating technique. Other than that, this work also to get the band gap energy similar to the standard bandgap for TiO2. The optical properties such as absorption and transmittance of TiO2 can be done by Ultraviolet-visible Spectroscopy (UV-Vis). The changes on the surface morphology were observed using Atomic Force Microscopy (AFM), Field Emission Scanning Electron Microscopy (FESEM). Based on the result, higher the molarity of TiO2, the uniformity of the surface morphology, and the energy bandgap is much better. Higher the molarity, the bandgap will be lower with 0.1M (3.78 eV) and its too large compare to the standard value (3.2 eV).

  17. 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.

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

    PubMed

    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

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. Single element high frequency (<50 MHz) PZT sol gel composite ultrasound transducers.

    PubMed

    Lukacs, M; Sayer, M; Foster, S

    2000-01-01

    A sol gel composite process has been used to produce lead zirconate titanate coatings in the thickness range of 3 to 100 microm on aluminum substrates. The complex permittivity (epsilon(33)(S )), elastic stiffness (c(33)(D)), and the piezoelectric constant (h(33)) of the coating and the complex elastic stiffness (c(33)(D)) of the substrate have been determined using impedance measurements and a commercially available software program [Piezoelectric Resonance Analysis Program PRAP 2.0, TASI Technical Software, Kingston, Ontario, Canada]. The complex components of the material parameters account for the losses within the film and the substrate. Sol gel composite films on aluminum have a dielectric constant of 220 with an imaginary component of 1% and an electromechanical coupling coefficient of up to 0.24 with an imaginary component of 3%. These films are applied to the fabrication of a high frequency transducers suitable for ultrasound biomicroscopy (UBM). By combining the sol gel composite material with existing transducer fabrication techniques, single-element focusing transducers have been produced that operate in the frequency range of 70 to 160 MHz. Devices have -6-dB bandwidths up to 52% and minimum insertion losses ranging from -47 to -58 dB. Real-time images of phantom materials and ex vivo biological samples are shown. PMID:18238526

  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. Hydrophobicity-induced selective covering of carbon nanotubes with sol gel sheaths achieved by ultrasound assistance

    NASA Astrophysics Data System (ADS)

    Park, Ki Chul; Mahiko, Tomoaki; Morimoto, Shingo; Takeuchi, Kenji; Endo, Morinobu

    2008-09-01

    A simple construction of sol-gel sheaths onto the surface of multi-walled carbon nanotubes (MWCNTs) has been carried out in water by a hydrophobicity-induced covering with the assistance of ultrasound. The ultrasound assistance prevents in water an unregulated agglomeration induced by the hydrophobicity of MWCNTs and phenyl-containing sols, leading to a selective construction of sol-gel sheaths on the nanotube surface. The phenyl groups of the resulting sol-gel sheaths were successfully removed by air-oxidation to provide the MWCNTs covered with amorphous SiO 2 sheaths. The effect of the SiO 2 sheaths on the electrical and thermal properties of the SiO 2-MWCNT nanocomposites was evaluated from the electrical resistivities of the nanocomposites with two different SiO 2 concentrations and the thermal conductivities of their phenol-resin composites. The results indicate that the small increase of the SiO 2 concentration remarkably increases the electrical resistivity of the SiO 2-MWCNT nanocomposites. Furthermore, the SiO 2 sheaths have more directly influenced the thermal property of the polymer composites than the inside nanotubes.

  7. 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

  8. 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. PMID:27157742

  9. 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.

  10. Art and practice to emboss gratings into sol-gel waveguides

    NASA Astrophysics Data System (ADS)

    Szendro, Istvan

    2001-05-01

    Recent interest in optical sensors, especially optical biosensors, has led to the introduction of commercially available instrumentation and sensor schemes for label free, real time monitoring of intermolecular interactions. One of the promising optical structure is the grating coupler planar waveguide sensor, where high precision surface relief grating is used and a low cost manufacturing is needed. A practical method to mass-produce gratings with limited lateral dimension is to emboss master grating into a sol-gel waveguide film. With proper optimization of the sol-gel process, a wide time window is available to perform embossing and highly reproducible, cost effective grating structures can be replicated. In our practice SiO2, TiO2, SiO2/TiO2, Ta2O5 and a mixture of these sol-gel thin films are proved to be good candidates for low optical loss waveguide materials in which grating with 2400 line/mm periodicity could be directly embossed. The relatively wide time window for optimal embossing opens the possibility to develop grating structures with more than one grating. Producing multiple gratings separated laterally and/or vertically from each other is demonstrated.

  11. A study on the effect factors of sol-gel synthesis of yttrium aluminum garnet nanopowders

    NASA Astrophysics Data System (ADS)

    Yang, Lin; Lu, Tiecheng; Xu, Hui; Zhang, Wei; Ma, Benyuan

    2010-03-01

    Yttrium aluminum garnet (YAG) nanopowders were synthesized by sol-gel method using aluminum nitrate, yttrium nitrate, and citric acid as starting materials, de-ionized water, ethanol, and ethylene glycol as solvents, respectively. The phase formation process, state of particle size distribution (PSD), compositions, morphological characteristics, and thermal behavior of the powders were investigated by means of x-ray diffractometry, PSD, Fourier transform infrared, transmission electronic microscope, and thermogravimetry-differential scanning calorimetry. Results indicate that the formation and characteristics of precursor gel and YAG powder, such as the rate of gelation, average particle size, and powder agglomerate state, strongly depend on the stoichiometric amount of citric acid, the solvent composition, and the precalcination process. Highly crystalline, well-dispersed YAG nanopowder was obtained by calcining at 800 °C for 2 h in the presence of citric acid to nitrate ratio of 3, ethanol solvent, and precalcination process. According to the analysis of experimental results, sol-gel chemistry, DLVO theory, and steric effect, the effects of stoichiometric amount of citric acid, solvent composition, and precalcination process on the formation and characteristics of precursor gel and YAG powder have been discussed. Meanwhile, the overall synthesis mechanism in sol-gel method has been suggested.

  12. 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

  13. 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

  14. 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

  15. Novel hybrid organic-inorganic sol-gel materials based on highly efficient heterocyclic push-pull chromophores

    NASA Astrophysics Data System (ADS)

    Abbotto, Alessandro; Bozio, Renato; Brusatin, Giovanna; Facchetti, Antonio; Guglielmi, Massimo; Innocenzi, Plinio; Meneghetti, Moreno; Pagani, Giorgio A.; Signorini, Raffaella

    1999-10-01

    We report the synthesis of sol-gel materials based on highly efficient heterocycle-based push-pull chromophores showing second- and third-order nonlinear optical activity. We show the proper functionalization of the best performing chromophores and their incorporation into a hybrid organic- inorganic sol-gel matrix. Different types of functionalization of the active molecule have been considered, including hydroxyl and alkoxysilyl end-groups. The functionalization strategy responded to different criteria such as stability and synthetic availability of the final molecular precursors, their solubility, and the used synthetic approach to the sol-gel material. The synthesis of the sol-gel materials has been tuned in order to preserve molecular properties and control important factors such as final concentration of the active dye in the matrix. Both acid- and base-catalyzed sol-gel synthesis has been taken into account. 3-Glycidoxypropyltrimethoxysilane and 3- aminopropyltriethoxysilane have been used as the organically modified alkoxides to prepare the hybrid organic-inorganic matrix. Characterization of the spectroscopic properties of the sol-gel materials is presented.

  16. Solid oxide fuel cells developed by the sol-gel process for oxygen generation

    NASA Astrophysics Data System (ADS)

    Finch, Joshua S.

    Electrochemical fuel cells convert chemical energy directly to electrical energy through the reaction of a fuel and an oxidant. Solid oxide fuel cells (SOFC) are solid-state devices that operate at temperatures around 800°C, using a solid oxygen electrolyte. The goal of this thesis is to prepare a defect-free solid oxygen electrolyte by a sol-gel process that is capable of (a) functioning in a fuel cell; and (b) producing measurable oxygen when operated as an oxygen generator. Sol-gel processing was chosen for membrane development because it offers a means of applying high-purity layers with controlled doping and a variety of geometries. In this study, the sol-gel process was used to produce yttria-stabilized zirconia (YSZ) electrolyte membranes as well as the electrodes required for an operational fuel cell. Zirconium oxychloride (ZOC) was used as the precursor material for the electrolyte. The YSZ solution was prepared by mixing yttrium nitrate and ZOC in a 50/50 ETOH and water solvent. The reaction was catalyzed with 1.5M NH4OH. Viscosity and solution application techniques were varied to monitor the effect on membrane development. The YSZ layer was sintered to full density. The sol-gel process was used to synthesize supported lanthanum strontium manganate (LSM) electrodes separated by a YSZ electrolyte. The LSM solution was made by mixing strontium nitrate, lanthanum chloride, and manganese acetate solutions. The LSM layers were sintered but were porous. After the membranes were assembled by successive layering and sintering, the membranes and completed fuel cells were characterized using TGA, XRD, FE-SEM, a gas pressurization technique, and electrochemical testing. The YSZ membrane exhibited a stable tetragonal crystal phase and formed a triple phase boundary (TPB) with the cathode. The three phases are the electrode, the electrolyte, and air. Electrochemical testing showed successful membrane development. Although oxygen production was not measured

  17. Investigation of the peroxovanadate sol-gel process and characterization of the gels

    NASA Astrophysics Data System (ADS)

    Fontenot, Craig Joseph

    Vanadium oxide gels derived from aqueous solution of V2O 5 and H2O2 have been investigated using in situ 51V NMR and laser Raman spectroscopic techniques. On the basis of this characterization, a pathway for peroxovanadate decomposition has been proposed, including the presence of two peroxovanadate dieters. New Raman bands and assignments for these species are reported. Experimental 51V NMR evidence suggested the VO2+ species was directly involved in the formation of the gel. The vanadia xerogels were studied using 51V and 17O MAS NMR, 17 O 3QMAS NMR, TGA, DSC, XRD, SEM and laser Raman spectroscopy. Based primarily on the 51V MAS NMR and TGA results, the coordination of five distinct vanadia sites has been detailed, which possibly include a previously unreported dieter. The relative concentration of these sites changed as dehydration progressed, and a model of this process has been proposed based on the numerical analysis of the NMR MAS spectra. Depending on sample treatment, it was possible to synthesize both layered and non-layered materials. The laser Raman spectra revealed differences between layered and non-layered materials. These differences have been attributed to the interaction of coordinated water molecules, which were trapped between layers and held firmly in place, thus restricting or altering certain Raman-active vibrations. The environments of oxygen sites in crystalline V2O5 and in vanadia produced via sol-gel synthesis were also investigated using 17O MAS and 3QMAS NMR. For crystalline V2O5, three sites were observed: V=O (vanadyl), V2O (bridging), and V 3O (corner sharing). Line shape parameters for these sites were determined from numerical simulation of the MAS spectrum. For the vanadia gel, assignments have been proposed for several oxygen sites including bridging and corner sharing oxygen, along with several vanadyl sites. Based on the 17O MQMAS NMR results, the coordination of the water sites has been detailed. Upon re-hydration of the

  18. 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

  19. 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.

  20. 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.

  1. Effect of the condensation of hybrid organic-inorganic sol-gel materials on the optical properties of tripan blue

    NASA Astrophysics Data System (ADS)

    Hicks, Craig; Morshed, Muhammad; Melia, Garrett; Barton, Killian; Duffy, Brendan; Oubaha, Mohamed

    2015-09-01

    The work reported in this paper highlights the effect of sol-gel structures on the optical properties of a typical organic dye (Trypan Blue, TB). Three transition-metal-based hybrid sol-gel materials with different structures and morphologies were developed and characterised by TEM. The optical properties of TB were investigated by incorporating it in the different sol-gel materials and the UV-Visible spectra recorded in both liquid and solid state, in thin-coatings cured at temperatures in the range 100-150 °C. These studies revealed two relevant results. First, the sol-gel morphology plays a critical role in the optical properties of the dye. The effect of the sol-gel host matrix on the optical properties of the dye is attributed to the steric hindrance of the nanostructures, themselves intimately dependant on the reactivity of the transition metal. For instance, the less condensed system showed the highest reactivity with the dye, while the more condensed system exhibited limited interaction with the dye, symbolised by a significant change or quasi-unchanged UV-Visible spectra, respectively. It is also shown that the increase of the condensation degree of the sol-gel coatings by heat-curing can dramatically alter the optical properties of the dye especially for the most condensed sol-gel systems. This has been attributed to proximity effects enabled by the further increase of the materials densities. The results reported here aim to provide a better understanding of how material formulations can influence the optical properties of organic dyes and suggest that the structure of the host matrix along with the applied curing process have to be fully considered and assessed in the choice of organic dyes for a given application.

  2. Structural Characterization and Corrosion Behavior of Stainless Steel Coated With Sol-Gel Titania

    NASA Astrophysics Data System (ADS)

    Vasconcelos, Daniela C. L.; Nunes, Eduardo H. M.; Sabioni, Antônio Claret S.; da Costa, João C. Diniz; Vasconcelos, Wander L.

    2012-03-01

    Sol-gel titania films were prepared from hydrolysis and condensation of titanium (IV) isopropoxide. Diethanolamine was used as chelant agent in titania synthesis. 316L stainless steel substrates were dip-coated at three different withdrawal speeds (6, 30, and 60 mm/min) and heated up to 400 °C. Thermogravimetry and differential thermal analyses of the titania gel solution evinced a continuous mass loss for temperatures up to 800 °C. The transition of anatase to the rutile phase begins at 610-650 °C, being the rutile transformation completed at 900 °C. The thicknesses of the films were determined as a function of the heat treatment and withdrawal speed. It was observed that their thicknesses varied from 130 to 770 nm. Scanning electron microscopy images of the composites revealed the glass-like microstructure of the films. The obtained sol-gel films were also characterized by energy dispersive spectroscopy. The chemical evolution of the films as a function of the heating temperature was evaluated by Fourier transform infrared spectroscopy (specular reflectance method). After performing the adhesion tests, the adherence of the titania films to the stainless steel substrate was excellent, rated 5B according to ASTM 3359. The hardness of the ceramic films obtained was measured by the Knoop microindentation hardness test with a 10 g load. We observed that the titania film became harder than the steel substrate when it was heated above 400 °C. The corrosion rates of the titania/steel composites, determined from potentiodynamic curves, were two orders of magnitude lower than that of the bare stainless steel. The presence of the sol-gel titania film contributed to the increase of the corrosion potential in ca. 650 mV and the passivation potential in ca. 720 mV.

  3. Preparation and mechanical properties of silicon oxycarbide fibers from electrospinning/sol-gel process

    SciTech Connect

    Wang, Xiaofei; Gong, Cairong; Fan, Guoliang

    2011-12-15

    Graphical abstract: Ceramic fibers, silicon oxycarbide (SiOC) fibers were demonstrated and showed higher mechanical properties from electrospinning/sol-gel process at 1000 Degree-Sign C. Highlights: Black-Right-Pointing-Pointer SiOC fibers with low cost are promising to substitute the non-oxide fibers. Black-Right-Pointing-Pointer Successful preparation of SiOC fibers by electrospinning/sol-gel process. Black-Right-Pointing-Pointer Confirmation of the designed product using material characterization methods. Black-Right-Pointing-Pointer The SiOC fibers prepared at 1000 Degree-Sign C possess higher strength (967 MPa). -- Abstract: Silicon oxycarbide (SiOC) fibers were produced through the electrospinning of the solution containing vinyltrimethoxysilane and tetraethoxysilane in the course of sol-gel reaction with pyrolysis to ceramic. The effect of the amount of spinning agent Polyvinylpyrrolidone (PVP) on the dope spinnability was investigated. At a mass ratio of PVP/alkoxides = 0.05, the spinning sol exhibited an optimal spinnable time of 50 min and generated a large quantity of fibers. Electrospun fibers were characterized by Fourier transform infrared spectroscopy (FTIR), thermo gravimetric analysis-differential scanning calorimetry (TGA-DSC), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The SEM results revealed that the SiOC fibers had a smooth surface and dense cross-section, free of residue pores and cracks. The XPS results gave high content of SiC (13.99%) in SiOC fibers. The SiOC fibers prepared at 1000 Degree-Sign C had a high tensile strength of 967 MPa and Young's modulus of 58 GPa.

  4. 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.

  5. 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.

  6. 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.

  7. Thermal Infrared Reflective Metal Oxide Sol-Gel Coatings for Carbon Fiber Reinforced Composite Structures

    NASA Astrophysics Data System (ADS)

    Richard, Brandon Demar

    Recent trends in composite research include the development of structural materials with multiple functionalities. In new studies, novel materials are being designed, developed, modified, and implemented into composite designs. Typically, an increase in functionality requires additional material phases within one system. The presence of excessive phases can result in deterioration of individual or overall properties. True multi-functional materials must maintain all properties at or above the minimum operating limit. In this project, samples of antimony and cobalt-doped tin oxide (ATO(Co2O 3)) sol-gel solutions are used to coat carbon fibers and are heat treated at a temperature range of 200 - 500 °C. Results from this research are used to model the implementation of sol-gel coatings into carbon fiber reinforced multifunctional composite systems. This research presents a novel thermo-responsive sol-gel/ (dopant) combination and evaluation of the actuating responses (reflectivity and surface heat dissipation) due to various heat treatment temperatures. While ATO is a well-known transparent conductive material, the implementation of ATO on carbon fibers for infrared thermal reflectivity has not been examined. These coatings serve as actuators capable of reflecting thermal infrared radiation in the near infrared wavelengths of 0.7-1.2 μm. By altering the level of Co2O3 and heat treatment temperatures, optimal optical properties are obtained. While scanning electron microscopy (SEM) is used for imaging, electron diffraction spectroscopy (EDS) is used to verify the compounds present in the coatings. Fourier transform infrared (FT-IR) spectroscopy was performed to analyze the chemical bonds and reflectivity in the infrared spectra after the heat treatments. Total reflection and angle-dependent reflectivity measurements were performed on the coatings in the wavelengths of 0.7-2 μm. Laser induced damage threshold testing was done to investigate the dielectric breakdown

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

    DOEpatents

    Panitz, J.K.; Reed, S.T.; Ashley, C.S.; Neiser, R.A.; Moffatt, W.C.

    1999-07-20

    Electrophoretically active sol-gel processes to fill, seal, and/or density porous, flawed, and/or cracked coatings on electrically conductive substrates. Such coatings may be dielectrics, ceramics, or semiconductors and, by the present invention, may have deposited onto and into them sol-gel ceramic precursor compounds which are subsequently converted to sol-gel ceramics to yield composite materials with various tailored properties. 6 figs.

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

    DOEpatents

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

    1999-01-01

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

  10. 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

  11. Synthesis and luminescence properties of encapsulated sol-gel glass samarium complexes

    NASA Astrophysics Data System (ADS)

    Zaitoun, M. A.; Momani, K.; Jaradat, Q.; Qurashi, I. M.

    2013-11-01

    Luminescence efficiency of lanthanide complexes generally largely depend on the choice of the organic ligand and the host matrix in which these complexes are doped. Two Sm(III) complexes, namely: Sm(III) dithicarbamate - Sm(L1)3B [L1 = (R)2NCS2B, R = C2H5 and B = 1,10-phenanthroline] and Sm(III) complex with the polytonic ligand L2 = N‧, N‧2-bis[(1E)-1-(2-pyridyl)ethylidene]ethanedihydrazide {Sm2-L2-(CH3COO)2; L2 = C16H16N6O2} are synthesized, these complexes are then trapped in sol-gel glass. Room temperature luminescence of Sm(L1)3B and {Sm2-L2-(CH3COO)2} complexes encapsulated in sol-gel glass are studied using a spectrofluorometer. Up on excitation by a UV light, ligand L1B absorbs this light and transfers it into the Sm(III) ions and emission bands were observed in the visible region and were attributed to f-f transitions of Sm(III). The observed emission indicated an efficient L1B ligand as a sensitizer, while ligand L2 shows no ability to work as a sensitizer. The branching ratio I4G5/2→6H9/2/I4G5/2→6H7/2) of electric dipole transition to magnetic dipole transition was used as an effective spectroscopic probe to predict symmetry of the site in which Sm(III) is located. The encapsulation of the Samaium complexes was performed for three reasons: (i) before rare earth (RE)-doped sol-gel glasses can be used in applications such as laser materials, several fluorescence quenching mechanisms must be overcome, we show in this work that lanthanide fluorescence is greatly enhanced by chelation and selecting a suitable host matrix (sol-gel) to accommodate the lanthanide complex, (ii) to improve the stability of the phosphor with efficient and high color-purity characteristics under ultraviolet excitation and (iii) this work provides a framework for preparing transparent composite glasses that are robust hosts to study the fundamental interactions between nano-materials and light.

  12. Free volume effects on the fluorescence characteristics of sol-gel glasses doped with quinine sulphate

    NASA Astrophysics Data System (ADS)

    Meneses-Nava, M. A.; Barbosa-García, O.; Díaz-Torres, L. A.; Chávez-Cerda, S.; King, T. A.

    1999-12-01

    The broadening of the absorption and fluorescence spectra and the red shift of the fluorescence maximum of quinine sulfate doped sol-gel glasses, before and after PMMA polymer impregnation, are investigated at different concentrations. The fluorescence decay of the quinine sulfate doped samples does not fit to a single exponential, as it does in ethanol solutions. We found that a double exponential gives a good fit to the obtained results. Introduction of solvent to fill the pores of the matrix does not only have the same effect as the polymer, but also reveals the strong attachment of the molecules to the pore walls and the influence of the interaction with the cage.

  13. Synthesis and luminescence properties of encapsulated sol-gel glass samarium complexes.

    PubMed

    Zaitoun, M A; Momani, K; Jaradat, Q; Qurashi, I M

    2013-11-01

    Luminescence efficiency of lanthanide complexes generally largely depend on the choice of the organic ligand and the host matrix in which these complexes are doped. Two Sm(III) complexes, namely: Sm(III) dithicarbamate - Sm(L1)3B [L1=(R)2NCS2B, R=C2H5 and B=1,10-phenanthroline] and Sm(III) complex with the polytonic ligand L2=N', N'(2)-bis[(1E)-1-(2-pyridyl)ethylidene]ethanedihydrazide {Sm2-L2-(CH3COO)2; L2=C16H16N6O2} are synthesized, these complexes are then trapped in sol-gel glass. Room temperature luminescence of Sm(L1)3B and {Sm2-L2-(CH3COO)2} complexes encapsulated in sol-gel glass are studied using a spectrofluorometer. Up on excitation by a UV light, ligand L1B absorbs this light and transfers it into the Sm(III) ions and emission bands were observed in the visible region and were attributed to f-f transitions of Sm(III). The observed emission indicated an efficient L1B ligand as a sensitizer, while ligand L2 shows no ability to work as a sensitizer. The branching ratio I4G5/2→6H9/2/I4G5/2→6H7/2) of electric dipole transition to magnetic dipole transition was used as an effective spectroscopic probe to predict symmetry of the site in which Sm(III) is located. The encapsulation of the Samaium complexes was performed for three reasons: (i) before rare earth (RE)-doped sol-gel glasses can be used in applications such as laser materials, several fluorescence quenching mechanisms must be overcome, we show in this work that lanthanide fluorescence is greatly enhanced by chelation and selecting a suitable host matrix (sol-gel) to accommodate the lanthanide complex, (ii) to improve the stability of the phosphor with efficient and high color-purity characteristics under ultraviolet excitation and (iii) this work provides a framework for preparing transparent composite glasses that are robust hosts to study the fundamental interactions between nano-materials and light.

  14. Electroanalytical applications of screen-printable surfactant-induced sol-gel graphite composites

    DOEpatents

    Guadalupe, Ana R.; Guo, Yizhu

    2001-05-15

    A process for preparing sol-gel graphite composite electrodes is presented. This process preferably uses the surfactant bis(2-ethylhexyl) sulfosuccinate (AOT) and eliminates the need for a cosolvent, an acidic catalyst, a cellulose binder and a thermal curing step from prior art processes. Fabrication of screen-printed electrodes by this process provides a simple approach for electroanalytical applications in aqueous and nonaqueous solvents. Examples of applications for such composite electrodes produced from this process include biochemical sensors such as disposable, single-use glucose sensors and ligand modified composite sensors for metal ion sensitive sensors.

  15. Barium hydroxyapatite nanoparticles synthesized by citric acid sol-gel combustion method

    SciTech Connect

    Xiu Zhiliang; Lue Mengkai . E-mail: mklu@icm.sdu.edu.cn; Liu Suwen; Zhou Guangjun; Su Benyu; Zhang Haiping

    2005-09-01

    Barium hydroxyapatite (BaHAP) nanoparticles have been synthesized by citric acid sol-gel combustion method using citric acid as a reductant/fuel and nitrate as an oxidant at a relatively low temperature of 600 deg. C. The thermal decomposition of nitrate-citrate xerogel was investigated by thermogravimetric/differential thermal analysis (TG/DTA) technique. The yielding powders calcined at 600 deg. C have been characterized by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), and transmission electron microscope (TEM). The possible combustion process was presented.

  16. Synthesis and sintering of nanocrystalline hydroxyapatite powders by citric acid sol-gel combustion method

    SciTech Connect

    Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

    2004-01-03

    The citric acid sol-gel combustion method has been used for the synthesis of nanocrystalline hydroxyapatite (HAP) powder from calcium nitrate, diammonium hydrogen phosphate and citric acid. The phase composition of HAP powder was characterized by X-ray powder diffraction analysis (XRD). The morphology of HAP powder was observed by transmission electron microscope (TEM). The HAP powder has been sintered into microporous ceramic in air at 1200 deg. C with 3 h soaking time. The microstructure and phase composition of the resulting HAP ceramic were characterized by scanning electron microscope (SEM) and XRD, respectively. The physical characterization of open porosity and flexural strength have also been carried out.

  17. Surface and catalytic properties of acid metal carbons prepared by the sol gel method

    NASA Astrophysics Data System (ADS)

    Aguado-Serrano, J.; Rojas-Cervantes, M. L.; Martín-Aranda, R. M.; López-Peinado, A. J.; Gómez-Serrano, V.

    2006-06-01

    The sol-gel method has been applied for the synthesis of a series of acid metal-carbon xerogels (with M = V, Cr, Mo and Ni) by polymerisation of resorcinol with formaldehyde in the presence of metallic precursors. A blank sample was also prepared without any metal addition. The xerogels were heated in nitrogen at 1000 °C to obtain the pyrolysed products. The samples were characterised by different techniques such as thermal-mass spectrometry analysis, gas physisorption, and mercury porosimetry. In addition, the acid character of the pyrolysed products was tested by the Claisen-Schmidt condensation between benzaldehyde and acetophenone for the formation of chalcones.

  18. Controlling the porosity of microporous silica by sol-gel processing using an organic template approach

    SciTech Connect

    Lu, Y.; Cao, G.Z.; Kale, R.P.; Delattre, L.; Lopez, G.P.; Brinker, C.J. |

    1996-12-31

    The authors use an organic template approach to prepare microporous silica with controlled pore size and narrow pore size distributions. This was accomplished by fabricating relatively dense hybrid silica matrices incorporating organic template ligands by sol-gel synthesis and then removing the organic ligands to create a microporous silica network. Comparison of computer simulation results and experimental data indicated that using this fugitive template approach, pore volume can be controlled by the amount of organic template added to the system, and pore size can be controlled by the size of the organic ligands.

  19. Development of an efficient large-aperture high damage-threshold sol-gel diffraction grating.

    SciTech Connect

    Ashley, Carol S.; Rambo, Patrick K.; Schwarz, Jens; Dunphy, Darren Robert; Branson, Eric D.; Smith, Ian Craig; Johnson, William Arthur; Reed, Scott T.; Cook, Adam W.

    2005-03-01

    In order to develop the next generation of high peak intensity lasers, new grating technology providing higher damage thresholds and large apertures is required. The current assumption is that this technical innovation will be multilayer dielectric gratings, wherein the uppermost layer of a thin film mirror is etched to create the desired binary phase grating. A variant of this is explored with the upper grating layer being a lower density gelatin-based volume phase grating in either sol-gel or dichromated gelatin. One key benefit is the elimination of the etching step.

  20. Sol-gel based anti-reflection coatings on wedged laser rods using a spin coater

    NASA Astrophysics Data System (ADS)

    Pareek, R.; Joshi, A. S.; Gupta, P. D.; Biswas, P. K.; Das, S.

    2005-07-01

    Anti-reflection (AR) sol-gel coatings are deposited on wedge glass optics for high-power lasers using spin coating technique. Characterization of these coatings on BK-7 glass substrates is carried out in terms of thickness profile across the surface, thickness variation w.r.t. wedge angle, and its effect on AR coating reflectivity, at different wedge angles from 1° to 7°. Results of the study are used to deposit AR coatings on inclined end faces of Nd:phosphate glass laser rods.

  1. Switching of lasing wavelength in a sol-gel laser with dynamic distributed feedback

    SciTech Connect

    Balenko, V G; Trufanov, A N; Umanskii, B A; Dolotov, S M; Petukhov, V A

    2011-09-30

    A scheme of switching the lasing wavelength of active centres in a sol-gel matrix excited by external laser radiation is proposed. A distributed feedback is formed during pumping by using a right-angle prism due to the interference of the direct and reflected pump beams. The lasing wavelength is determined by the period of the interference pattern, which depends on the convergence angle of interfering beams. Control is performed by a liquid-crystal cell, which changes the pump radiation polarisation, and a birefringent prism. As a result, the convergence angle of interfering beams changes, leading to a change in the interference pattern period and the excited radiation wavelength.

  2. Influence of POST Annealing on Sol-Gel Deposited ZnO Thin Films

    NASA Astrophysics Data System (ADS)

    Bhadane, Hemalata; Samuel, Edmund; Gautam, Dinesh Kumar

    2014-05-01

    The effect of annealing temperature on sol-gel deposited ZnO thin films have been studied. The average crystallite size determined from XRD shows that the deposited films are nanocrystalline. FTIR confirms deposition of ZnO thin films. The transmittance of annealed ZnO thin films is greater than 80% in visible region with bandgap ranging from 3.25-3.19 eV. The films annealed at 450°C temperature shows lower resistivity value of 527.241 Ωm. The deposited nanocrystalline films are suitable for biosensing applications due to its higher surface area.

  3. YAG:Ce3+ Nanophosphor Synthesized with the Salted Sol-Gel Method

    SciTech Connect

    D. Jia; C. V. Shaffer; J. E. Weyant; A. Goonewardene; X. Guo; Y. Wang; X. Z. Guo; K. K. Li; Y. K. Zou; W. Jia

    2006-05-01

    Nano-phosphors of Y3Al5O12:Ce3+ (YAG:Ce) were synthesized with a novel salted sol-gel method, in which aqueous solution of inorganic salts (yttrium/cerium nitrates) were used along with the metal alkoxide precursor, aluminum sec-butoxide, Al(OC4H9)3. YAG single phase was formed at temperature as low as 800 C. Luminescence of YAG:Ce reached the maximum intensity when calcined above 1350C. The SEM image reveals that the grain sizes of the nano-phosphors calcined at 1100 C are in a range of 50-150 nm.

  4. Sol-gel synthesis and characterization of SiO2/PCL hybrid materials containing quercetin as new materials for antioxidant implants.

    PubMed

    Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando; Piccolella, Simona; Pacifico, Severina

    2016-01-01

    The development of biomaterials with intrinsic antioxidant properties could represent a valuable strategy for preventing peri-implant disease onset. In this context quercetin, a naturally occurring flavonoid, has been entrapped, at different weight percentages in a silica/poly(ε-caprolactone)-based hybrid material by a sol-gel route. FT-IR and UV spectroscopic techniques were employed in order to characterize the hybrids. FT-IR analysis indicated changes in stretching frequencies of the quercetin dienonic moiety, suggesting that a flavonol oxidized derivative was formed during the sol-gel process. The establishment of hydrogen-bonded interactions between quercetin and silica and polymer matrices,was strongly affected by the amount of polymer. Poly(ε-caprolactone) did not interact with quercetin when it was loaded at high doses (50 wt.%). The morphology of the synthesized materials was observed by using SEM. The obtained images proved that the materials are hybrid nanocomposites. Their bioactivity was shown by the formation of a hydroxyapatite layer on samples' surface soaked in a fluid simulating the composition of the human plasma. The antiradical properties of the investigated systems were evaluated by DPPH and ABTS methods and their cytotoxicity by the MTT assay. Data obtained revealed that the synthesized materials are biocompatible and that the hybrid system,with 6 wt.% of PCL and 15 wt.% of quercetin, produced the strongest antiradical efficacy. PMID:26478390

  5. Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

    NASA Astrophysics Data System (ADS)

    Ouyang, Xin; Cao, Peng; Huang, Saifang; Zhang, Weijun; Huang, Zhaohui; Gao, Wei

    2015-07-01

    CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.

  6. Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: dissolution behaviour and biological properties after crystallisation.

    PubMed

    Tredwin, Christopher J; Young, Anne M; Abou Neel, Ensanya A; Georgiou, George; Knowles, Jonathan C

    2014-01-01

    Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) were synthesised by the sol-gel method as possible implant coating or bone-grafting materials. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride were incorporated for the preparation of the FHA and FA sol-gels. After heating and powdering the sol-gels, dissolution behaviour was assessed using ion chromatography to measure Ca(2+) and PO4 (3-) ion release. Biological behaviour was assessed using cellular proliferation with human osteosarcoma cells and alamarBlue™ assay. Statistical analysis was performed with a two way analysis of variance and post hoc testing with a Bonferroni correction. Increasing fluoride substitution into an apatite structure decreased the dissolution rate. Increasing the firing temperature of the HA, FHA and FA sol-gels up to 1,000 °C decreased the dissolution rate. There was significantly higher cellular proliferation on highly substituted FHA and FA than on HA or Titanium. The properties of an implant coating or bone grafting material can be tailored to meet specific requirements by altering the amount of fluoride that is incorporated into the original apatite structure. The dissolution behaviour can further be altered by the temperature at which the sol-gel is fired.

  7. Novel multifunctional titania-silica-lanthanum phosphate nanocomposite coatings through an all aqueous sol-gel process.

    PubMed

    Smitha, Venu Sreekala; Jyothi, Chembolli Kunhatta; Peer, Mohamed A; Pillai, Saju; Warrier, Krishna Gopakumar

    2013-04-01

    A novel nanocomposite coating containing titania, silica and lanthanum phosphate prepared through an all aqueous sol-gel route exhibits excellent self-cleaning ability arising from the synergistic effect of the constituents in the nanocomposite. A highly stable titania-silica-lanthanum phosphate nanocomposite sol having particle size in the range of 30-50 nm has been synthesized starting from a titanyl sulphate precursor, which was further used for the development of photocatalytically active composite coatings on glass. The coatings prepared by the dip coating technique as well as the nanocomposite powders are heat treated and characterized further for their morphology and multifunctionality. The nanocomposite containing 1.5 wt% LaPO4 has shown a surface area as high as 138 m(2) g(-1) and a methylene blue degradation efficiency of 94% in two hours of UV exposure. The composite coating has shown very good homogeneity evidenced by transparency as high as 99.5% and low wetting behaviour. The present novel approach for energy conserving, aqueous derived, self-cleaning coatings may be suitable for large scale industrial applications.

  8. Application of a nanostructured platform and imprinted sol-gel film for determination of chlorogenic acid in food samples.

    PubMed

    Ribeiro, Carla M; Miguel, Eliane M; Silva, Jonadab Dos S; Silva, Cristian B da; Goulart, Marília O F; Kubota, Lauro T; Gonzaga, Fabiano B; Santos, Wilney J R; Lima, Phabyanno R

    2016-08-15

    Chlorogenic acid (CGA) is a polyphenol derivative that widely exists in higher plants like fruits, vegetables, black teas, and some traditional Chinese medicines. In this work, we have proposed a sensitive and selective electrochemical sensor for detection of CGA. The sensor was based on a glassy carbon electrode (GCE) modified with a functional platform by grafting vinyltrimethoxysilane (VTMS) in multi-walled carbon nanotubes (MWCNTs) and covered by a molecularly imprinted siloxane (MIS) film prepared using the sol-gel process. The VTMS was grafted onto the surface of the MWCNTs via in situ free radical polymerization. The MIS was obtained from the acid-catalyzed hydrolysis/condensation of a solution consisting of tetraethoxysilane (TEOS), phenyltriethoxysilane (PTEOS), (3-aminopropyl)trimethoxysilane (APTMS), and CGA as a template molecule. The modification procedure was evaluated by differential pulse voltammetry (DPV) and scanning electron microscopy (SEM). Under optimized operational conditions, a linear response was obtained covering a concentration ranging from 0.08μmolL(-1) to 500μmolL(-1) with a detection limit (LOD) of 0.032μmolL(-1). The proposed sensor was applied to CGA determination in coffee, tomato, and apple samples with recoveries ranging from 99.3% to 108.6%, showing a promising potential application in food samples. Additionally, the imprinted sensor showed a significantly higher affinity for target CGA than the non-imprinted siloxane (NIS) sensor. PMID:27260443

  9. Ultrathin phenyl-functionalized solid phase microextraction fiber coating developed by sol-gel deposition.

    PubMed

    Azenha, Manuel; Malheiro, Catarina; Silva, A Fernando

    2005-04-01

    A new sol-gel application for the development of SPME fibers is described. Phenyltrimethoxysilane (PTMOS) and methyltrimethoxysilane (MTMOS) were the sol-gel precursors used at different proportions, together with different water contents, catalyst and reaction time. It was observed that obtaining a good film quality was determinant for a good extracting fiber performance. The film thickness ranged 0.2-1 microm and could not be increased by multi-coating processes. Apparently, a dense, non-porous microstructure was obtained. These coatings exhibited a strong hydrophobic character, as shown by the capability of extraction of long chain and apolar aromatic compounds, which, was comparable to that of the 100 microm polydimethylsiloxane (PDMS) and 65 microm carbowax-divinylbenzene (CW-DVB). The developed fiber has shown high thermal (350 degrees C) and organic solvent stability (ethanol, toluene and dichloromethane), thus bearing adequate characteristics to be associated to GC and potentialities that may also envisage suitability for HPLC. The new fibers may be useful for the microextraction of non-polar compounds, although at trace levels and in simple matrixes only, due to the susceptibility to competition.

  10. Folding Myoglobin within a Sol-Gel Glass: Protein Folding Constrained to a Small Volume

    PubMed Central

    Peterson, Eric S.; Leonard, Emma F.; Foulke, Jocelyn A.; Oliff, Matthew C.; Salisbury, Rosanne D.; Kim, David Y.

    2008-01-01

    The unfolding and refolding reaction of myoglobin was examined in solution and within a porous silica sol-gel glass. The sol-gel pores constrain the protein to a volume that is the same size and shape as the folded native state accompanied by a few layers of water solvation. Denaturants such as low pH buffers can be diffused through the gel pores to the protein to initiate unfolding and refolding. Acid-induced unfolding was hindered by the steric constraints imposed by the gel pores such that more denaturing conditions were required within the gel than in solution to create the unfolded state. No new folding intermediates were observed. Refolding of myoglobin was not complete in millimolar pH 7 buffer alone. Addition of 25% glycerol to the pH 7 buffer resulted in nearly complete refolding, and the use of 1 M phosphate buffer resulted in complete refolding. The role of this cosolvent and salt in disrupting the ordered water surrounding the protein within the gel is discussed in light of the Hofmeister series and entropic trapping via a diminished hydrophobic effect within the gel. These results are consistent with the premises of folding models in which secondary and tertiary structures are considered to form within a compact conformation of the protein backbone. PMID:18339762

  11. Phospholipid fatty acids as physiological indicators of Paracoccus denitrificans encapsulated in silica sol-gel hydrogels.

    PubMed

    Trögl, Josef; Jirková, Ivana; Kuráň, Pavel; Akhmetshina, Elmira; Brovdyová, Taťjána; Sirotkin, Alexander; Kirilina, Tatiana

    2015-01-01

    The phospholipid fatty acid (PLFA) content was determined in samples of Paracoccus denitrificans encapsulated in silica hydrogel films prepared from prepolymerized tetramethoxysilane (TMOS). Immediately after encapsulation the total PLFA concentration was linearly proportional to the optical density (600 nm) of the input microbial suspension (R2 = 0.99). After 7 days this relationship remained linear, but with significantly decreased slope, indicating a higher extinction of bacteria in suspensions of input concentration 108 cells/mL and higher. trans-Fatty acids, indicators of cytoplasmatic membrane disturbances, were below the detection limit. The cy/pre ratio (i.e., ratio of cyclopropylated fatty acids (cy17:0 + cy19:0) to their metabolic precursors (16:1ω7 + 18:1ω7)), an indicator of the transition of the culture to a stationary growth-phase, decreased depending on co-immobilization of nutrients in the order phosphate buffer > mineral medium > Luria Broth rich medium. The ratio, too, was logarithmically proportional to cell concentration. These results confirm the applicability of total PLFA as an indicator for the determination of living biomass and cy/pre ratio for determination of nutrient limitation of microorganisms encapsulated in sol-gel matrices. This may be of interest for monitoring of sol-gel encapsulated bacteria proposed as optical recognition elements in biosensor construction, as well as other biotechnological applications. PMID:25690547

  12. Band gap and FTIR studies for copper-zinc sol-gel glasses

    NASA Astrophysics Data System (ADS)

    Kaur, G.; Kaur, Navneet; Rawat, Mohit; Singh, K.; Kumar, Vishal

    2016-05-01

    Sol-gel technique was used for synthesis of Calcium phosphorous Borosilicate (CaO-SiO2-B2O3-P2O5-CuO-ZnO) glasses by varying composition of Copper oxide and Zinc oxide. Sol-gel route uses organic precursors which provide better homogeneity and uniform particle size compared to melt quenched glass. Four different glass stoichiometries were characterised using UV-visible spectroscopy and Fourier transforms infra-red spectroscopy (FTIR). Infra-red spectrum of transmittance of powdered glass samples is obtained by FTIR which measure the transmittance of wavelength in them and it also determines the presence of different functional group. Band gap has been obtained using UV-visible spectroscopy for all the glasses so as to study the effect of increasing ZnO content in glass composition. The change in band gap with ZnO content is indication of the change in number of non-bridging oxygen's (NBO).

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

    NASA Astrophysics Data System (ADS)

    Lau, L. N.; Ibrahim, N. B.

    2015-09-01

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

  14. Oxide and organic nano-porous sol-gel materials synthesized for lipid bilayer formation

    NASA Astrophysics Data System (ADS)

    Nellis, Barbara

    Sol-gel synthesized materials have many applications and in this thesis, different sol-gel films have been investigated as a scaffolding substrate for vesicle-fused lipid bilayers. Oxide, organic, and phosphate-based xerogels have been characterized using methods such as scanning electron microscopy (SEM), x-ray diffraction (XRD), atomic force micrsocopy (AFM) and contact angle goniometry to determine their viability as lipid membrane supports. Membranes containing 1,2-Dioleoyl-Glycero-3-Phosphocholine (DOPC) and two-phase lipid bilayer membranes containing DOPC and 1,2-Distearoyl-Glycero-3-Phosphocholine (DSPC) have been successfully assembled on these surfaces and characterized using fluorescence microscopy and fluorescence recovery after photobleaching (FRAP) to determine the lateral mobility and diffusion coefficients of these unique systems. It was found that xerogel films with rough surface topography lead to slower lipid diffusion due to obstruction of the membrane. Further work is needed to determine if more complexities, which are found in real cell membranes, can be accommodated by these new substrate chemistries. Additionally, sugar-based aerogel and xerogel materials were synthesized for catalytic applications. These unique materials were characterized with SEM and BET surface area and pore size analysis and it was found that sucrose aerogels, with high surface area and smaller pore diameters, are the most promising sugar-based material studied for further catalysis research.

  15. Responsive hydrogels produced via organic sol-gel chemistry for cell culture applications.

    PubMed

    Patil, Smruti; Chaudhury, Pulkit; Clarizia, Lisa; McDonald, Melisenda; Reynaud, Emmanuelle; Gaines, Peter; Schmidt, Daniel F

    2012-08-01

    In this study, we report the synthesis of novel environmentally responsive polyurea hydrogel networks prepared via organic sol-gel chemistry and demonstrate that the networks can stabilize pH while releasing glucose both in simple aqueous media and in mammalian cell culture settings. Hydrogel formulations have been developed based on the combination of an aliphatic triisocyanate with pH-insensitive amine functional polyether and pH-sensitive poly(ethyleneimine) segments in a minimally toxic solvent suitable for the sol-gel reaction. The polyether component of the polyurea network is sufficiently hydrophilic to give rise to some level of swelling independent of environmental pH, while the poly(ethyleneimine) component contains tertiary amine groups providing pH sensitivity to the network in the form of enhanced swelling and release under acidic conditions. The reaction of these materials to form a network is rapid and requires no catalyst. The resultant material exhibits the desired pH-responsive swelling behavior and demonstrates its ability to simultaneously neutralize lactic acid and release glucose in both cell-free culture media and mammalian cell culture, with no detectable evidence of cytotoxicity or changes in cell behavior, in the case of either SA-13 human hybridomas or mouse embryonic stem cells. Furthermore, pH is observed to have a clear effect on the rate at which glucose is released from the hydrogel network. Such characteristics promise to maintain a favorable cell culture environment in the absence of human intervention. PMID:22561670

  16. Phospholipid Fatty Acids as Physiological Indicators of Paracoccus denitrificans Encapsulated in Silica Sol-Gel Hydrogels

    PubMed Central

    Trögl, Josef; Jirková, Ivana; Kuráň, Pavel; Akhmetshina, Elmira; Brovdyová, Tat′jána; Sirotkin, Alexander; Kirilina, Tatiana

    2015-01-01

    The phospholipid fatty acid (PLFA) content was determined in samples of Paracoccus denitrificans encapsulated in silica hydrogel films prepared from prepolymerized tetramethoxysilane (TMOS). Immediately after encapsulation the total PLFA concentration was linearly proportional to the optical density (600 nm) of the input microbial suspension (R2 = 0.99). After 7 days this relationship remained linear, but with significantly decreased slope, indicating a higher extinction of bacteria in suspensions of input concentration 108 cells/mL and higher. trans-Fatty acids, indicators of cytoplasmatic membrane disturbances, were below the detection limit. The cy/pre ratio (i.e., ratio of cyclopropylated fatty acids (cy17:0 + cy19:0) to their metabolic precursors (16:1ω7 + 18:1ω7)), an indicator of the transition of the culture to a stationary growth-phase, decreased depending on co-immobilization of nutrients in the order phosphate buffer > mineral medium > Luria Broth rich medium. The ratio, too, was logarithmically proportional to cell concentration. These results confirm the applicability of total PLFA as an indicator for the determination of living biomass and cy/pre ratio for determination of nutrient limitation of microorganisms encapsulated in sol-gel matrices. This may be of interest for monitoring of sol-gel encapsulated bacteria proposed as optical recognition elements in biosensor construction, as well as other biotechnological applications. PMID:25690547

  17. Responsive hydrogels produced via organic sol-gel chemistry for cell culture applications.

    PubMed

    Patil, Smruti; Chaudhury, Pulkit; Clarizia, Lisa; McDonald, Melisenda; Reynaud, Emmanuelle; Gaines, Peter; Schmidt, Daniel F

    2012-08-01

    In this study, we report the synthesis of novel environmentally responsive polyurea hydrogel networks prepared via organic sol-gel chemistry and demonstrate that the networks can stabilize pH while releasing glucose both in simple aqueous media and in mammalian cell culture settings. Hydrogel formulations have been developed based on the combination of an aliphatic triisocyanate with pH-insensitive amine functional polyether and pH-sensitive poly(ethyleneimine) segments in a minimally toxic solvent suitable for the sol-gel reaction. The polyether component of the polyurea network is sufficiently hydrophilic to give rise to some level of swelling independent of environmental pH, while the poly(ethyleneimine) component contains tertiary amine groups providing pH sensitivity to the network in the form of enhanced swelling and release under acidic conditions. The reaction of these materials to form a network is rapid and requires no catalyst. The resultant material exhibits the desired pH-responsive swelling behavior and demonstrates its ability to simultaneously neutralize lactic acid and release glucose in both cell-free culture media and mammalian cell culture, with no detectable evidence of cytotoxicity or changes in cell behavior, in the case of either SA-13 human hybridomas or mouse embryonic stem cells. Furthermore, pH is observed to have a clear effect on the rate at which glucose is released from the hydrogel network. Such characteristics promise to maintain a favorable cell culture environment in the absence of human intervention.

  18. Synthesis and characterization of NiO nanopowder by sol-gel process

    SciTech Connect

    Ningsih, Sherly Kasuma Warda

    2015-09-30

    Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms were produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.

  19. Synthesis and nonlinear optical properties of sol-gel materials containing phthalocyanines

    NASA Astrophysics Data System (ADS)

    Fuqua, Peter D.; Mansour, Kamjou; Alvarez, Daniel, Jr.; Marder, Seth R.; Perry, Joseph W.; Dunn, Bruce S.

    1992-12-01

    Optical limiters are devices that have the ability to limit the intensity of light that passes through them. They function like 'optical surge protectors,' blocking a greater fraction of photons when the incident light intensity is very high than when the incident intensity is low. This might allow an electronic sensor or a human eye to function under ambient lighting conditions and yet be protected from being blinded by direct laser illumination. Phthalocyanine (Pc) dyes which exhibit nonlinear optical behavior known as reverse saturable absorption (RSA) have been demonstrated to be effective in solution-based optical limiters. There is considerable interest in the possibility of fabricating optical limiters based on solid-state materials containing phthalocyanine dyes. Sol-gel processing is a solution based technique for preparing porous metal oxide monoliths at low temperatures. By adding an organic dye to the precursor solution, one can trap these organic molecules in the pores of a silica host. These potentially thermally stable materials are of interest for the fabrication of monolithic lens/limiter optical components. Our study of sol-gel synthetic approaches to phthalocyanine doped glassy materials show that phthalocyanine dyes in silica hosts are stable and exhibit optical nonlinearities comparable to those of the corresponding dye solutions.

  20. Surface acoustic wave characterization of optical sol-gel thin layers.

    PubMed

    Fall, Dame; Compoint, François; Duquennoy, Marc; Piombini, Hervé; Ouaftouh, Mohammadi; Jenot, Frédéric; Piwakowski, Bogdan; Belleville, Philippe; Ambard, Chrystel

    2016-05-01

    Controlling the thin film deposition and mechanical properties of materials is a major challenge in several fields of application. We are more particularly interested in the characterization of optical thin layers produced using sol-gel processes to reduce laser-induced damage. The mechanical properties of these coatings must be known to control and maintain optimal performance under various solicitations during their lifetime. It is therefore necessary to have means of characterization adapted to the scale and nature of the deposited materials. In this context, the dispersion of ultrasonic surface waves induced by a micrometric layer was studied on an amorphous substrate (fused silica) coated with a layer of ormosil using a sol-gel process. Our ormosil material is a silica-PDMS mixture with a variable polydimethylsiloxane (PDMS) content. The design and implementation of Surface Acoustic Wave InterDigital Transducers (SAW-IDT) have enabled quasi-monochromatic Rayleigh-type SAW to be generated and the dispersion phenomenon to be studied over a wide frequency range. Young's modulus and Poisson's ratio of coatings were estimated using an inverse method.

  1. Laser Surface Treatment of Silica Sol-gel Coating to Produce Nanocrystalline Structure

    NASA Astrophysics Data System (ADS)

    Razavi, R. Shoja; Gordani, Gh.; Hojjati, A.

    2011-12-01

    In this study two methods of laser and furnace sintering are used to prepare nanocrystalline structure of silica sol-gel coating on glass substrate. In laser sintering method, an Nd:YAG pulsed laser with a laser pulse energy of 1 J used to sinter the silica sol-gel coating. To evaluate the surface morphology and microstructural analysis, XRD and SEM were used. The optical properties of coatings were examined by UV/VIS spectroscopy. The results indicated that the laser sintered coating was denser than the furnace sintered coating. No porosity and cracks were detected on the surface of laser sintered coating. Using Scherer mathematical equation, it was shown that the grain size of laser sintered coating is well within nano size range. The uniformity of nanocrystalline structure clearly improved the reflection of incident beam from the laser sintered coating. This was mainly due to increase in grain boundary regions which in turn can cause some the wavelength of the incident beam to be transmitted from silica coatings.

  2. Frequency control of sol-gel composite films fabricated by stencil printing for nondestructive testing applications

    NASA Astrophysics Data System (ADS)

    Kaneko, Tsukasa; Kibe, Taiga; Kimoto, Keisuke; Nishimura, Ryota; Kobayashi, Makiko

    2016-07-01

    Ultrasonic transducers made of sol-gel composites have been developed for nondestructive testing (NDT) applications in various industrial fields. Stencil printing of sol-gel composite films has been developed for the reduction of fabrication time and cost. However, it was necessary to develop low frequency (<10 MHz) ultrasonic transducers for inspecting industrial structures under severe high-temperature conditions, because high-frequency components suffer attenuation effect caused by high temperature. To realize this, increasing the thickness of Pb(Zr,Ti)O3 (PZT)/PZT films fabricated by stencil printing was attempted in this study. The samples were fabricated by single-layer stencil printing with a thick stencil mask and multilayer pure stencil printing with prespraying and postspraying. The film thicknesses were 150-185 µm, and the center frequencies of ultrasonic responses were 6.0-6.4 MHz. Throughout three thermal cycles of up to 370 K, the ultrasonic performance was stable, and the frequency characteristics were not markedly different from the beginning to the end of the test. Therefore, low-frequency ultrasonic transducers were successfully manufactured using a stencil-printing-based technique.

  3. Conventional E-glass fibre light guides: self-sensing composite based on sol gel cladding

    NASA Astrophysics Data System (ADS)

    Wang, L.; Kister, G.; Ralph, B.; Talbot, J. D. R.; Fernando, G. F.

    2004-02-01

    The aim of this study was to modify conventional reinforcing E-glass fibres to enable them to act as optical waveguides and subsequently as sensor devices. This required the glass fibres to be coated with a relatively homogeneous coating with a corresponding refractive index that was lower than the E-glass fibre (1.56). Although a range of coating materials are available, this study focused on using materials that are generally used as sizing agents for glass fibres to improve the adhesion to the matrix. Two different methods based on conventional sol gel processing were used to obtain crack-free coatings. In the first method, tetraethoxysilane (TEOS) and polyvinyl alcohol were used as precursors. In the second method, acid-catalysed solutions of TEOS mixed with 3-glycidoxypropyltrimethoxysilane were used as precursors. UV visible transmission results showed that the films had low absorption and high transparency in the visible range. The refractive indices of the films were found to be a function of the molar fractions of the major chemical components. A simple impregnation procedure was used to apply the coating to the E-glass fibre bundles. The light transmission characteristics of the coated fibres along with their mechanical properties were evaluated. The sol gel coatings were shown to be effective in converting the conventional E-glass fibres into light guides.

  4. TiO2/PCL hybrid materials synthesized via sol-gel technique for biomedical applications.

    PubMed

    Catauro, M; Bollino, F; Papale, F; Marciano, S; Pacifico, S

    2015-02-01

    The aim of the present work has been the synthesis of organic/inorganic hybrid materials based on titanium dioxide and poly(ε-caprolactone) (PCL) to be used in the biomedical field. Several materials have been synthesized using sol-gel methods by adding different amounts of polymer to the inorganic sol. The obtained gels have been characterized using Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and atomic force microscopy (AFM). The FT-IR data allowed us to hypothesize that the structure formed was that of an interpenetrating network, realized by hydrogen bonds between TiOH groups in the sol-gel intermediate species and carbonyl groups in the polymer repeating units. SEM and AFM analyses highlighted that the obtained materials were nanostructurated hybrids. To evaluate the biological properties of the hybrids, their bioactivity and cytotoxicity were investigated as a function of the PCL amount. The bioactivity of the synthesized systems was proven by the formation of a hydroxyapatite layer on the surface of samples soaked in a fluid simulating human blood plasma (SBF). MTT cytotoxicity tests and Trypan Blue dye exclusion tests were carried out exposing NIH-3T3 mouse embryonic fibroblasts for 24 and 48h to extracts from the investigated hybrid materials. The results showed that all the hybrids had a non-cytotoxic effect on target cells.

  5. "Beating speckles" via electrically-induced vibrations of Au nanorods embedded in sol-gel.

    PubMed

    Ritenberg, Margarita; Beilis, Edith; Ilovitsh, Asaf; Barkai, Zehava; Shahmoon, Asaf; Richter, Shachar; Zalevsky, Zeev; Jelinek, Raz

    2014-01-01

    Generation of macroscopic phenomena through manipulating nano-scale properties of materials is among the most fundamental goals of nanotechnology research. We demonstrate cooperative "speckle beats" induced through electric-field modulation of gold (Au) nanorods embedded in a transparent sol-gel host. Specifically, we show that placing the Au nanorod/sol-gel matrix in an alternating current (AC) field gives rise to dramatic modulation of incident light scattered from the material. The speckle light patterns take form of "beats", for which the amplitude and frequency are directly correlated with the voltage and frequency, respectively, of the applied AC field. The data indicate that the speckle beats arise from localized vibrations of the gel-embedded Au nanorods, induced through the interactions between the AC field and the electrostatically-charged nanorods. This phenomenon opens the way for new means of investigating nanoparticles in constrained environments. Applications in electro-optical devices, such as optical modulators, movable lenses, and others are also envisaged. PMID:24413086

  6. Use of sol-gel systems for solid/liquid separation.

    SciTech Connect

    Chaiko, D. J.; Kopasz, J. P.; Elison, A. J. G.; Chemical Engineering

    1998-01-01

    A unique approach using sol-gel technology is presented for separating and recovering particulates and colloids from caustic waste slurries. The approach involves the addition of an alkali silicate and an organic gelling agent directly to the waste stream to immobilize particulates that range from macro sizes to submicron colloids. The particulates and colloids become trapped within a silica network that remains porous during the early stages of the sol-gel process. The freshly gelled monolith undergoes a process of syneresis, whereby the water and soluble salts are ejected from the monolith as it contracts. The approach has been illustrated by removal of ultrafine particulates from a Hanford Tank Waste simulant. Initial laboratory tests have shown that it is possible to produce silica monoliths in the presence of 4 M hydroxide. Analysis of the mother liquor produced during syneresis indicated quantitative recovery of the particulates within the monolith. The partitioning of ions between the silica gel and the mother liquor during syneresis correlates directly with the lyotropic series. Salt recoveries from the mother liquor in excess of 90% can be achieved. With a capability of recovering >99.999% of all particulates, including colloids, the process is more efficient than membrane filtration. This approach produces a rock-hard silica monolith that can be used directly as a feedstock to a glass melter or can be consolidated to near theoretical density by sintering.

  7. Finite element modeling of evaporation and condensation during sol-gel film and fiber formation

    SciTech Connect

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

    1993-07-01

    Free surfaces, multicomponent phase change, volume expansion and compression, and surface tension gradients make for challenging application of the finite element method to sol-gel (ceramic) film and fiber formation. The microstructure of the final product is largely controlled by the competition between the drying, curing, and underlying fluid mechanics of formation. Sol-gel materials are peculiar because they often contain more than one solvent, each solvent differing in volatility and surface tension. Hence, nonuniform evaporation can produce surface tension gradients that dramatically change the meniscus shape. These processes are complicated further by a volume change that accompanies evaporation and condensation, making for shock-like discontinuities in concentration and velocity at the free surface. Computer-aided predictions of film formation by dip coating and of fiber spinning (see Figure 1) are made for alcohol-water mixtures with one non-volatile species. The Navier-Stokes system is augmented with two convective-diffusion equations to track the concentration of alcohol and water, and an energy equation to monitor temperature changes. The equations are solved in both phases by discretizing them first with the Galerkin/finite element method. The resulting non-linear algebraic equation set is solved with Newton`s method. The subdomaining technique is based on elliptic grid generation and is designed to parameterize the moving meniscus. Special treatment of the functional representations of velocity and concentration within the elements lining the free surface are made to accommodate the volume change that accompanies mass exchange between phases.

  8. Fluorescent properties of Tb-doped borosilicate glass films prepared by a sol-gel method

    NASA Astrophysics Data System (ADS)

    Tonooka, Kazuhiko; Shimokawa, Katsuyoshi; Nishimura, Okio

    2001-04-01

    Rare earth elements have been used as optical dopants in glasses for many years. Boro-silicate glass films doped with rare-earths were deposited on glass substrates by using a simple sol-gel method. To avoid the undesirable precipitation due to the different hydrolysis rates between silicon and boron alkoxides, two solutions were used for dip-coating separately. One solution consisted of silicon tetraethoxide, ethanol, water and terbium nitrate as the Tb dopant. Another consisted of triethyl borate. Layer-by-layer deposition was applied by dipping into solutions containing metal alkoxides in sequence. The fluorescence properties of Tb3+ were investigated for the boro-silicate samples in relation to the firing effect. As-deposited silicate and boro-silicate samples showed similar fluorescence spectra under UV excitation. After firings at about 800 degrees C, a remarkable increase of the Tb3+-ion fluorescence was observed for the boro-silicate samples, while the silicate sample showed a little increase in fluorescence intensity. These experimental results suggested the formation of boro- silicate network and the incorporation of Tb3+ into the boro-silicate matrix. The multilayer process was found useful to fabricate multi-component sol-gel films.

  9. Nanocrystalline mesoporous SMO thin films prepared by sol gel process for MEMS-based hydrogen sensor

    NASA Astrophysics Data System (ADS)

    Gong, Jianwei; Fei, Weifeng; Seal, Sudipta; Chen, Quanfang

    2004-01-01

    MEMS based SnO2 gas sensor with sol gel synthesized mesoporous nanocrystalline (<10 nm) semiconductor thin (100~150 nm) film has been recently developed. The SnO2 nano film is fabricated with the combination of polymeric sol gel chemistry with block copolymers used for structure directing agents. The novel hydrogen sensor has a fast response time (1s) and quick recovery time (3s), as well as good sensitivity (about 90%), comparing to other hydrogen sensors developed. The improved capabilities are credited to the large surface to volume ratio of gas sensing thin film with nano sized porous surface topology, which can greatly increase the sensitivity even at relatively low working temperature. The gas sensing film is deposited onto a thin dielectric membrane of low thermal conductivity, which provides good thermal isolation between substrate and the gas-sensitive heated area on the membrane. In this way the power consumption can be kept very low. Since the fabrication process is completely compatible with IC industry, it makes mass production possible and greatly reduces the cost. The working temperature of the new sensor can be reduced as low as 100°C. The low working temperature posse advantages such as lower power consumption, lower thermal induced signal shift as well as safe detection in certain environments where temperature is strictly limited.

  10. Aging effect on the phase evolution of water-based sol-gel hydroxyapatite.

    PubMed

    Liu, Dean-Mo; Troczynski, T; Tseng, Wenjea J

    2002-02-01

    In a number of recent reports on the synthesis of sol-gel hydroxyapatite, aging of the precursor solution has been found to be critical in developing an apatitic phase. Critical aging time is required to complete reaction between Ca and P molecular precursors to form a desired intermediate complex that permits a further transformation to apatite phase under appropriate thermal treatment. In this investigation, we employed a water-based sol-gel process recently developed to fabricate hydroxyapatite at relatively low temperatures. The aging effect on apatite formation was systematically studied in terms of aging time and temperature. Experimental results show that the aging time is considerably reduced as aging temperature rises. Long-term thermal aging was unfavorable for apatite formation. The optimal aging parameters for apatite formation were experimentally determined, which was further consolidated into a phase evolution map. Aging kinetic was investigated by monitoring the variation of solution pH, following the determination of an apparent activation energy, which has a value as high as 10.35 kcal/mol, for the chemical reaction occurring upon aging. Optimal solution chemistry was elucidated based on the corresponding phase evolution map.

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

    PubMed

    Rashti, Ali; Yahyaei, Hossein; Firoozi, Saman; Ramezani, Sara; Rahiminejad, Ali; Karimi, Roya; Farzaneh, Khadijeh; Mohseni, Mohsen; Ghanbari, Hossein

    2016-12-01

    Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants. PMID:27612823

  12. Sol-gel replicated optics made from single point diamond turned masters exhibit fractal surface roughness

    SciTech Connect

    Bernacki, B.E.; Miller, A.C. Jr.; Evans, B.M. III; Moreshead, W.V.; Nogues, J.L.R.

    1996-05-01

    Deterministic optics manufacturing, notably single point diamond turning (SPDT) has matured such that the current generation of machines is capable of producing refractive and reflective optics for the visible wavelength region that are quite acceptable for many applications. However, spiral tool marks are still produced that result in unwanted diffractive scattering from grating-like features having a spatial frequency determined by the machine feed, tool radius, and other influences such as vibration and material removal effects. Such regular artifacts are the characteristic of deterministic manufacturing methods such as SPDT. The authors present some initial findings suggesting that fractal, or non-deterministic surfaces can be produced by SPDT through sol-gel replication. The key is the large isotropic shrinkage that occurs through monolithic sol-gel replication (a factor of 2.5) that results in all features, including tooling marks, being reduced by that amount. The large shrinkage itself would be a laudable-enough feature of the replication process. However, by an as-yet-not understood manner, the replication process itself seems to alter the roughness character of the replicated surface such that it appears to be fractal when analyzed using contact profilometry and the power spectrum approach.

  13. Spectroscopic studies of chemical reactions and dynamics in sol-gel matrices

    SciTech Connect

    Akbarian, F.; Dunn, B.; Fuqua, P.D.; McKiernan, J.; Simoni, E.; Zink, J.I.

    1994-12-31

    The synthesis of sol-gel glasses containing organic and organometallic molecular dopants has been well established as an approach for creating new optical materials. Some of these properties are dependent upon chemical reactions which occur in porous xerogel matrices during the sol-gel process or when encapsulated molecules are exposed to other molecules in solution. In this paper, the study of two different types of chemical reactions in the pores of xerogel matrices is reported. In one case copper phthalocyanine is used to characterize dimerization within the pores. The results show that dimer formation is most likely to occur towards the end of the drying stage as the dye concentration in the pores increases from solvent evaporation. A second example involves the use of a pump-probe technique to determine the rate of proton recombination inside the pores of silica monoliths. The behavior of sols and gels is similar to aqueous solution while recombination of protons in the xerogel seems to be affected by the walls of the pores.

  14. Epoxide opening versus silica condensation during sol-gel hybrid biomaterial synthesis.

    PubMed

    Gabrielli, Luca; Russo, Laura; Poveda, Ana; Jones, Julian R; Nicotra, Francesco; Jiménez-Barbero, Jesús; Cipolla, Laura

    2013-06-10

    Hybrid organic-inorganic solids represent an important class of engineering materials, usually prepared by sol-gel processes by cross-reaction between organic and inorganic precursors. The choice of the two components and control of the reaction conditions (especially pH value) allow the synthesis of hybrid materials with novel properties and functionalities. 3-Glycidoxypropyltrimethoxysilane (GPTMS) is one of the most commonly used organic silanes for hybrid-material fabrication. Herein, the reactivity of GPTMS in water at different pH values (pH 2-11) was deeply investigated for the first time by solution-state multinuclear NMR spectroscopic and mass spectrometric analysis. The extent of the different and competing reactions that take place as a function of the pH value was elucidated. The NMR spectroscopic and mass spectrometric data clearly indicate that the pH value determines the kinetics of epoxide hydrolysis versus silicon condensation. Under slighly acidic conditions, the epoxy-ring hydrolysis is kinetically more favourable than the formation of the silica network. In contrast, under basic conditions, silicon condensation is the main reaction that takes place. Full characterisation of the formed intermediates was carried out by using NMR spectroscopic and mass spectrometric analysis. These results indicate that strict control of the pH values allows tuning of the reactivity of the organic and inorganic moities, thus laying the foundations for the design and synthesis of sol-gel hybrid biomaterials with tuneable properties.

  15. Application of fluorinated compounds to cotton fabrics via sol-gel

    NASA Astrophysics Data System (ADS)

    Ferrero, Franco; Periolatto, Monica

    2013-06-01

    The aim of this work was the study of the surface modification of cotton fibers to confer hydro and oil repellency to the fabrics. A surface treatment not involving the bulk of the fibers was chosen, so fabrics can maintain comfort properties. Moreover the study focused on an economical and environmental friendly process, in order to obtain an effective treatment with good fastness to washing. A modified silica based film was applied on fibers surface by sol-gel, comparing laboratory grade reagents with a commercial product as precursors and optimizing process parameters. From obtained results sol-gel can be indicated as a promising process to confer an effective and durable finishing to cotton fibers with low add-ons. Long impregnation times can significantly improve the treatment fastness, while ironing the washed samples can restore, at least partially, hydro and oil repellency lost after the washing. Obtained results were supported by a deep surface characterization of untreated, treated and washed samples. The best results were obtained using the commercial product as the only precursor. This is interesting for an industrial application, due to the low cost of this product if compared with the laboratory grade reagents investigated. Some applications of finished textiles can be for household use, technical garments, umbrellas or outdoor textiles.

  16. The preparation of fluorine doped cadmium oxide thin film by sol-gel process.

    PubMed

    Kim, In Yea; Kim, Jong Sung

    2014-11-01

    During the several decades, CdO thin film has attracted many attentions as a candidate for the transparent conducting electrodes due to its high electrical conductivity and high optical transmittance. Various dopants such as F, In, Al, Sn, and Cr have been used to improve the optical and electrical properties of the film. Generally, the optical and electrical property of the thin film is dependent on its oxidation state, the amount of dopant materials, and the fabrication process. In this study, fluorine doped CdO thin films were prepared by using sol-gel process with various atomic ratios of Cd:F, and their electrical and optical properties were investigated. The precursor solution for sol-gel film was prepared with pH 5 and pH 8, and the film was annealed at 350 degrees C. X-ray diffraction pattern confirmed the cubic CdO:F phase formation, and the 10% fluorine doped film prepared with pH 8 precursor solution showed the lowest resistivity of 0.01574 Ω cm.

  17. NiO-silica based nanostructured materials obtained by microemulsion assisted sol-gel procedure

    SciTech Connect

    Mihaly, M.; Comanescu, A.F.; Rogozea, A.E.; Vasile, E.; Meghea, A.

    2011-10-15

    Graphical abstract: TEM micrograph of NiO/SiO{sub 2} nanoparticles. Highlights: {yields} Microemulsion assisted sol-gel procedure for NiO silica nanomaterials synthesis. {yields} Controlling the size and shape of nanoparticles and avoiding their aggregation. {yields} Narrow band-gap semiconductors (energies <3 eV) absorbing VIS or near-UV light biologically and chemically inert semiconductors entrapping/coating in silica network. {yields} Low cost as the microemulsion is firstly used in water metallic cation extraction. -- Abstract: NiO-silica based materials have been synthesized by microemulsion assisted sol-gel procedure. The versatility of these soft nanotechnology techniques has been exploited in order to obtain different types of nanostructures, such as NiO nanoparticles, NiO silica coated nanoparticles and NiO embedded in silica matrix. These materials have been characterized by adequate structural and morphology techniques: DLS, HR-TEM/SAED, BET, AFM. Optical and semiconducting properties (band-gap values) of the synthesized materials have been quantified by means of VIS-NIR diffuse reflectance spectra, thus demonstrating their applicative potential in various electron transfer phenomena such as photocatalysis, electrochromic thin films, solid oxide fuel cells.

  18. Lead magnesium niobate-lead titanate fibres by a modified sol-gel method

    SciTech Connect

    Lam, K.-H. . E-mail: 02900857r@polyu.edu.hk; Li Kun; Chan, H.L.-W.

    2005-11-03

    Lead magnesium niobate-lead titanate (PMN-PT) ceramic fibres with the nominal composition of 0.65Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-0.35PbTiO{sub 3} have been fabricated by a modified sol-gel method. Due to the difficulty of dissolving the magnesium component, the mixed oxide method was used together with the traditional sol-gel method. To obtain crack-free fibres, pyrolysis was carried out at a very slow heating rate under specific atmosphere to control the organic burnout. The thermal and microstructural properties were investigated using thermogravimetric analysis, scanning electron microscopy and X-ray diffraction. The optimum sintering temperature is 1200 deg. C and yields a fibre with a final diameter of around 100 {mu}m. A single PMN-PT fibre has been poled and its electrical properties were measured. The properties of the fibre are found to be better than that of a ceramic disc.

  19. Encapsulated metal nanocluster materials prepared by a novel inverse micelle/sol-gel technique

    SciTech Connect

    Yamanaka, S.A.; Martino, A.; Kawola, J.S.

    1995-12-31

    A wide variety of manometer sized metal and semiconductor particles (Au, Ag, Pd, Pt, Rh, Fe, Ni, CdS, MoS{sub 2} and FeS{sub 2}) can be prepared using an inverse micelle technique. Such materials are of great interest for their potential use in catalytic, photochemical, electrochemical and optical applications but their practicality is often hindered by the agglomeration of the particles. Agglomeration may be prevented by using a porous support matrix where the nanoclusters are sterically trapped within the pores. The sol-gel process results in the formation of such a porous support material. We have thus combined the technique of forming metal nanoclusters in inverse micelle solutions with the technique of forming sol-gel materials. Using our novel method, we have succeeded in preparing manometer sized metal colloids encapsulated in both xerogel and aerogel materials. Characterization of these materials has been carried out by TEM, SEM, UV/Vis, NMR and nitrogen sorption porosimetry.

  20. Sol-gel auto-combustion synthesis of zinc ferrite for moderate temperature desulfurization

    SciTech Connect

    Rongjun Zhang; Jiejie Huang; Jiantao Zhao; Zhiqiang Sun; Yang Wang

    2007-09-15

    Zinc ferrite as a desulfurization sorbent with an average crystallite size of about 36 nm was synthesized by a sol-gel auto-combustion method. The precursor for the sorbent was a gel obtained from metal nitrates and citric acid by a sol process. The nitrate-citrate gel exhibits a self-propagating combustion behavior, and after combustion, it can transform into a nanosized spinel structured zinc ferrite directly. The prepared sorbent has a larger specific surface area and higher reactivity when compared with the sorbent achieved by a solid mixing method, and it could efficiently reduce the H{sub 2}S concentration from 6000 ppm to less than 2 ppm at a moderate temperature range. The sulfur capacity at 400{sup o}C reaches about 38.5 g of sulfur/100 g of sorbent, which corresponds to 96.4% of the theoretical value. The temperature programmed oxidation test for the sulfided sorbent shows that the most sulfur is desorbed before 500{sup o}C. XRD results confirm that the sulfided sample after exposure to a 5% O{sub 2}/N{sub 2} gas mixture at 500{sup o}C can be regenerated completely, which indicates that the regeneration temperature of the sorbent prepared by the sol-gel auto-combustion method could be greatly reduced. 40 refs., 10 figs., 2 tabs.

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

    PubMed

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

    2015-01-01

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

  2. Evaporation induced self assembly and rheology change during sol-gel coating

    NASA Astrophysics Data System (ADS)

    Lee, Chang H.; Lu, Yunfeng; Shen, Amy Q.

    2006-05-01

    Thin films with self-assembled nanostructures are important in applications such as catalysis and biosensor technology. A major technique used to prepare such films is sol-gel processing. This technique involves depositing a complex fluid on a substrate by dip, spin, or spray coating, followed by allowing the film to evaporate and form self-assembled nanostructures. Since the composition of the film during coating is central to understanding how changing chemical and physical conditions affect the properties and microstructures of the films, we investigate the rheological properties of the entrained fluid film and its subsequent impact on the steady state film thickness during the evaporation-induced self-assembly process. We perform systematic experiments to measure the meniscus shape and film thickness during sol-gel dip coating. We observe that the experimental data of film thickness lie way below the Landau-Levich-Derjaguin prediction from the classic film-coating results. To explain this discrepancy, we present a thin film model based on the lubrication approximation with an evaporation effect. Our results show that evaporation-induced self-assembly leads to rheological variations in the entrained film and, consequently, alters the film thickness. The predicted film thickness based on the evaporation-induced rheology variation model compares well with the experiments.

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

    PubMed

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

    2013-06-01

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

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

    SciTech Connect

    Lau, L. N. Ibrahim, N. B.

    2015-09-25

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

  5. Energetic Nanocomposites with Sol-gel Chemistry: Synthesis, Safety and Characterization

    SciTech Connect

    Gash, A E; Simpson, R L; Satcher, J H

    2002-05-15

    The preparation and characterization of energetic composite materials containing nanometer-sized constituents is currently a very active and exciting area of research at laboratories around the world. Some of these efforts have produced materials that have shown very unique and important properties relative to traditional energetic materials. We have previously reported on the use of sol-gel chemical methods to prepare energetic nanocomposites. Primarily we reported on the sol-gel method to synthesize nanometer-sized ferric oxide that was combined with aluminum fuel to make pyrotechnic nanocomposites. Since then we have developed a synthetic approach that allows for the preparation of hybrid inorganic/organic energetic nanocomposites. This material has been characterized by thermal methods, energy-filtered transmission electron microscopy (EFTEM), N, adsorption/desorption methods, and Fourier-Transform (FT-IR) spectroscopy, results of which will be discussed. According to these characterization methods the organic polymer phase fills the nanopores of the composite material, providing superb mixing of the component phases in the energetic nanocomposite. The EFTEM results provide a convenient and effective way to evaluate the intimacy of mixing between these component phases. The safe handling and preparation of energetic nanocomposites is of paramount importance to this research and we will report on studies performed to ensure such.

  6. Energetic Nanocomposites with Sol-gel Chemistry: Synthesis, Safety, and Characterization

    SciTech Connect

    Gash, A E; Simpson, R L; Satcher, J H

    2002-06-05

    The preparation and characterization of energetic composite materials containing nanometer-sized constituents is currently a very active and exciting area of research at laboratories around the world. Some of these efforts have produced materials that have shown very unique and important properties relative to traditional energetic materials. We have previously reported on the use of sol-gel chemical methods to prepare energetic nanocomposites. Primarily we reported on the sol-gel method to synthesize nanometer-sized ferric oxide that was combined with aluminum fuel to make pyrotechnic nanocomposites. Since then we have developed a synthetic approach that allows for the preparation of hybrid inorganic/organic energetic nanocomposites. This material has been characterized by thermal methods, energy-filtered transmission electron microscopy (EFTEM), N{sub 2} adsorption/description methods, and Fourier-Transform (FT-IR) spectroscopy, results of which will be discussed. According to these characterization methods the organic polymer phase fills the nanopores of the composite material, providing superb mixing of the component phases in the energetic nanocomposite. The EFTEM results provide a convenient and effective way to evaluate the intimacy of mixing between these component phases. The safe handling and preparation of energetic nanocomposites is of paramount importance to this research and we will report on studies performed to ensure such.

  7. In situ electrodeposition of an asymmetric sol-gel membrane based on an octadecyltrimethoxysilane Langmuir film.

    PubMed

    Hitrik, Maria; Lev, Ovadia; Mandler, Daniel

    2014-09-15

    The unique properties of Langmuir film formation were utilized in assembling a thin skin of an asymmetric membrane. An octadecyltrimethoxysilane (ODTMS) Langmuir monolayer was formed at the air-water interface and served as the substrate for growing a bulky sol-gel polymer in situ. The latter was based on the electrochemical deposition of tetramethoxysilane dissolved in the water subphase by means of horizontal touch electrochemistry. The resultant asymmetric layer that consisted of a thin hydrophobic ODTMS Langmuir film connected to a bulk hydrophilic sol-gel network was studied in situ and ex situ by using various techniques, such as cyclic voltammetry, electrochemical impedance spectroscopy (EIS), scanning electron microscopy, transmission electron microscopy (TEM), and goniometry. We found that a porous hydrophilic film grew on top of a hydrophobic layer as was evident from TEM, contact angle, and EIS analyses. The film thickness and film permeability could be controlled by changing the deposition conditions such as the potential window applied and its duration. Hence, this method offers an alternative approach for assembling asymmetric films for various applications.

  8. Dialkylenecarbonate-Bridged Polysilsesquioxanes. Hybrid Organic Sol-Gels with a Thermally Labile Bridging Group

    SciTech Connect

    Loy, D.A.; Beach, J.V.; Baugher, B.M.; Assink, R.A.; Shea, K.J.; Tran, J.; Small, J.H.

    1999-04-21

    In this paper, we introduce a new approach for altering the properties of bridged polysilsesquioxane xerogels using post-processing modification of the polymeric network. The bridging organic group contains latent functionalities that can be liberated thermally, photochemically, or by chemical means after the gel has been processed to a xerogel. These modifications can produce changes in density, volubility, porosity, and or chemical properties of the material. Since every monomer possesses two latent functional groups, the technique allows for the introduction of high levels of functionality in hybrid organic-inorganic materials. Dialkylenecarbonate-bridged polysilsesquioxane gels were prepared by the sol-gel polymerization of bis(triethoxysilylpropyl)carbonate (1) and bis(triethoxysilylisobutyl)-carbonate (2). Thermal treatment of the resulting non-porous xerogels and aerogels at 300-350 C resulted in quantitative decarboxylation of the dialkylenecarbonate bridging groups to give new hydroxyalkyl and olefinic substituted polysilsesquioxane monolithic xerogels and aerogels that can not be directly prepared through direct sol-gel polymerization of organotrialkoxysilanes.

  9. Effect of chelating agent acetylacetone on corrosion protection properties of silane-zirconium sol-gel coatings

    NASA Astrophysics Data System (ADS)

    Yu, Mei; Liang, Min; Liu, Jianhua; Li, Songmei; Xue, Bing; Zhao, Hao

    2016-02-01

    The hybrid sol-gel coatings on AA2024-T3 were prepared with a silane coupling agent 3-glycidoxypropyltrimethoxysilane (GPTMS) and a metal alkoxide tetra-n-propoxyzirconium (TPOZ) as precursors. The effect of acetylacetone (AcAc) as a chelating agent on the corrosion protection properties of sol-gel coatings were evaluated and the optimal AcAc/TPOZ molar ratio was obtained. The sol-gel coatings were characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The corrosion protection properties of the coatings were evaluated by means of potentiodynamic polarization study (PDS) and electrochemical impedance spectroscopy (EIS). It is demonstrated that AcAc avoids fast hydrolysis of TPOZ and benefits to form stable sols. The coating with AcAc/TPOZ molar ratio of 3 shows the best corrosion protection performance in 0.05 M NaCl solution.

  10. Drug entrapment in silica microspheres through a single step sol-gel process and in vitro release behavior.

    PubMed

    Yilmaz, Elvan; Bengisu, Murat

    2006-04-01

    A single step sol-gel process was used to precipitate silica microspheres containing ibuprofen or naproxen for controlled drug delivery applications. The drug release behavior from these systems was analyzed in vitro. Pure ibuprofen and naproxen exhibited linear release with time, while sol-gel silica entrapped drugs were released with a logarithmic time dependence starting with an initial burst effect followed by a gradual decrease. Microscopic analysis combined with gravimety and infrared spectroscopy indicated that some of the drug is entrapped as large crystals attached to silica microspheres while the rest is encapsulated inside the microspheres. Drug-loaded silica microspheres with no open porosity and with a narrow particle size distribution were obtained. Both erosion of the microspheres and diffusion through them contributed to drug release. Sol-gel precipitation of silica microspheres is a promising method for drug entrapment and controlled release.

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

    PubMed

    Bakas, Idriss; Hayat, Akhtar; Piletsky, Sergey; Piletska, Elena; Chehimi, Mohamed M; Noguer, Thierry; Rouillon, Régis

    2014-12-01

    We report here a novel method to detect methidathion organophosphorous insecticides. The sensing platform was architected by the combination of molecularly imprinted polymers and sol-gel technique on inexpensive, portable and disposable screen printed carbon electrodes. Electrochemical impedimetric detection technique was employed to perform the label free detection of the target analyte on the designed MIP/sol-gel integrated platform. The selection of the target specific monomer by electrochemical impedimetric methods was consistent with the results obtained by the computational modelling method. The prepared electrochemical MIP/sol-gel based sensor exhibited a high recognition capability toward methidathion, as well as a broad linear range and a low detection limit under the optimized conditions. Satisfactory results were also obtained for the methidathion determination in waste water samples.

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

    NASA Technical Reports Server (NTRS)

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

    1998-01-01

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

  13. Patterning titania with the conventional and modified micromolding in capillaries technique from sol-gel and dispersion solutions

    NASA Astrophysics Data System (ADS)

    Ullah Khan, Sajid; ten Elshof, Johan E.

    2012-04-01

    We report TiO2 patterns obtained by a soft-lithographic technique called 'micromolding in capillaries' using sol-gel and dispersion solutions. A comparison between patterning with a sol-gel and dispersion solutions has been performed. The patterns obtained from sol-gel solutions showed good adhesion to the substrate and uniform shapes, but large shrinkage, whereas those obtained from dispersion solution had high solid content, but exhibited poor adhesion and non-uniform shapes. A fabrication method of a layer-by-layer structured pattern is also demonstrated. This type of pattern may find application in sensors, waveguides and other photonics elements. The occurrence of an undesirable residue layer, which hinders the fabrication of isolated patterns, is highlighted and a method of prevention is suggested.

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

    PubMed

    Kojarunchitt, Thunjiradasiree; Baldursdottir, Stefania; Dong, Yao-Da; Boyd, Ben J; Rades, Thomas; Hook, Sarah

    2015-01-01

    Thermoresponsive, particle-loaded, Poloxamer 407 (P407)-Pluronic-R® (25R4) or chitosan-methyl cellulose (MC) formulations were developed as single-dose, sustained release vaccines. The sol-gels, loaded either with a particulate vaccine (cubosomes) or soluble antigen (ovalbumin) and adjuvants (Quil A and monophosphoryl lipid A), were free-flowing liquids at room temperature and formed stable gels at physiological temperatures. Rheological results showed that both systems meet the criteria of being thermoresponsive gels. The P407-25R4 sol-gels did not significantly sustain the release of antigen in vivo while the chitosan-MC sol-gels sustained the release of antigen up to at least 14 days after administration. The chitosan-MC sol-gels stimulated both cellular and humoral responses. The inclusion of cubosomes in the sol-gels did not provide a definitive beneficial effect. Further analysis of the formulations with small-angle X-ray scattering (SAXS) revealed that while cubosomes were stable in chitosan-MC gels they were not stable in P407-25R4 formulations. The reason for the mixed response to cubosome-loaded vehicles requires more investigation, however it appears that the cubosomes did not facilitate synchronous vaccine release and may in fact retard release, reducing efficacy in some cases. From these results, chitosan-MC sol-gels show potential as sustained release vaccine delivery systems, as compared to the P407-25R4 system that had a limited ability to sustain antigen release.

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

    PubMed

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

    2015-09-01

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

  16. Silica-titania sol-gel hybrid materials: synthesis, characterization and potential application in solid phase extraction.

    PubMed

    de Moraes, Sandra V M; Passos, Joana B; Schossler, Patricia; Caramão, Elina B; Moro, Celso C; Costa, Tania M H; Benvenutti, Edilson V

    2003-04-10

    The biphenilaminepropylsilica and biphenilaminepropylsilicatitania were synthesized by sol-gel method, in two steps: (a) biphenylamine reacts with chloropropyltrimethoxysilane and (b) the product of reaction was polycondensed with tetraethylorthosilicate (TEOS) or TEOS and titanium isopropoxide. The sol-gel materials were characterized using infrared spectroscopy and N(2) adsorption-desorption isotherms and they were employed as sorbents for carcinogenic N-containing compound retention, in aqueous solution, using the SPE technique. The N-containing compounds adsorption was influenced by the titania presence and the sorption process seems to happen in the pores with higher organic density.

  17. Characterization of Nanostructured n-ZnO/p-Si Heterojunction Prepared by a Simple Sol-Gel Method

    NASA Astrophysics Data System (ADS)

    He, Bo; Xu, Jing; Ning, Huanpo; Xiong, Hao; Xing, Huaizhong; Qin, Yuming

    2016-03-01

    The nanostructured ZnO film was prepared on a texturized Si wafer by a simple sol-gel method to fabricate n-ZnO/p-Si heterojunction photoelectric device. The novel sol-gel method is cheap and convenient. The structural, optical and electrical properties of the nanostructured ZnO film were studied by XRD, SEM, XPS, PL, UV-Vis spectrophotometer and Hall effect measurement. The current-voltage (I-V) curve of nanostructured ZnO/p-Si heterojunction device shows good rectifying behavior. Good photoelectric behavior is obtained.

  18. Development and characterization of a family of shape memory, biocompatible, degradable, porous (co)-polyurethanes via sol-gel chemistry

    NASA Astrophysics Data System (ADS)

    Lippincott, Hugh Walker

    In support of the goal of a tissue engineering scaffold that is moldable, biodegradable and has shape-memory, this work explored the space of polyurethane sol-gel formulations and solvents to create a biocompatible, porous xerogel with potential to be such a porous scaffold. The work has resulted in both a process and a sol-gel formulation to effectively create a family of degradable, biocompatible, shape memory, porous, block copolyurethane xerogels from polycaprolactone and castor oil. Formulations of the sol-gel family of potential scaffolds were characterized for their biocompatibility, hydrolytic degradability, porosity, and shape memory. Of the scaffolds tested in this fashion, the most successful supported the attachment and growth of 3T3 fibroblast cells at 72% of the rate of attachment and growth in the standard tissue culture plastic Petri dishes. A method was developed and explained that selects the solvent for creation of a porous xerogel by controlling the phase separation of the polymerizing polyurethane from the reaction solution. This method uses standard polymer solvent swelling and extraction test data. Solvent solutions plotted in the 3-D space of Hansen solubility parameters were used to select solvents that produced porous xerogels from two different polyurethane sol-gel formulations. The process effectively combines a set of methods that search the sol-gel formulation spaces for both shape-memory and porosity. Easily produced dense xerogels from trial sol-gel formulations are sufficient for DSC and initial DMA shape-memory test data, as well as standard solvent swelling and extraction test data to support the search for shape memory and the computation of rankings to select solvent(s) that is most likely to produce a porous xerogel. Accelerated degradation tests on the dense xerogels also produced results useful to guide further testing of the sol-gel formulations. Standard shape-memory research testing only characterizes the free return to

  19. Deposition of YBCO thin films on silver substrate via a fluorine-free sol-gel synthesis

    NASA Astrophysics Data System (ADS)

    Xu, Yongli; Shi, Donglu; Lian, L.; Wang, M.; McClellan, Shaun M.

    2002-05-01

    To further develop grain-textured YBCO thin films for conductor development, we deposited, via a fluorine-free sol-gel synthesis, YBCO thin films on non-textured silver substrate. The interface structures were studied by both x-ray diffraction (XRD) and transmission electron microscopy (HRTEM). XRD data indicated that the YBCO films on silver substrate exhibited c-axis grain orientations. Experimental details are reported on the sol-gel synthesis chemistry and XRD and HRTEM characterization of the YBCO thin films.

  20. Reactive Molecular Dynamics Investigations of Alkoxysilane Sol-Gel and Surface Coating Processes

    NASA Astrophysics Data System (ADS)

    Deetz, Joshua David

    The ability to generate nanostructured materials with tailored morphology or chemistry is of great technological interest. One proven method of generating metal-oxide materials, and chemically modifying metal-oxide surfaces is through the reactions of molecular building blocks known as alkoxysilanes. Alkoxysilanes are a class of chemicals which contain one or more organic alkoxy groups bonded to silicon atoms. Alkoxysilane (Si-O-R) chemical groups can undergo reactions to form bridges (Si-O-M) with metal oxides. Due to their ability to "attach" to metal-oxides through condensation reactions, alkoxysilanes have a number of interesting applications, such as: the generation of synthetic siloxane materials through the sol-gel process, and the formation of functionalized surface coatings on metal-oxide surfaces. Despite widespread study of sol-gel and surface coatings processes, it is difficult to predict the morphology of the final products due to the large number of process variables involved, such as precursor molecule structure, solvent effects, solution composition, temperature, and pH. To determine the influence of these variables on the products of sol-gel and coatings processes reactive molecular dynamics simulations are used. A reactive force field was used (ReaxFF) to allow the chemical bonds in simulation to dynamically form and break. The force field parameters were optimized using a parallel optimization scheme with a combination of experimental information, and density functional theory calculations. Polycondensation of alkoxysilanes in mixtures of alcohol and water were studied. Steric effects were observed to influence the rates of hydrolysis and condensation in solutions containing different precursor monomers. By restricting the access of nucleophiles to the central silicon atom, the nucleation rate of siloxanes can be controlled. The influence of solution precursor, water, and methanol composition on reaction rates was explored. It was determined that

  1. Anti-weathering treatments to protect mineral surfaces: Hybrid sol-gel and biomimetic strategies

    NASA Astrophysics Data System (ADS)

    Rao, Sudeep Motupalli

    1998-12-01

    The natural weathering of stone is accelerated by the combined effects of acid rain, salt crystallization and the freeze-thaw cycles of water. This dissertation describes the development of two anti-weathering preservation treatments that are specific to limestone surfaces. The first strategy involves the application of a surface-specific, bifunctional, passivating, coupling agent that binds to both the limestone surface and to a consolidating inorganic polymeric silica matrix by a sol-gel process. The second strategy involves biomimetic process that converts the exposed limestone surface into a nonreactive calcium oxalate hydrate ceramic layer found in kidney stones and lichen deposits. The microreactor environment of a scanning probe microscope (SPM) fluid cell was used to simulate acid rain effects on treated and untreated calcite surfaces, seen as etch pits and crystal step movement. The treatment process was also monitored at near molecular scale resolution using the SPM. Calcite crystals treated with aminoethylaminopropyltrimethoxysilane (25% AEAPS) passivating coupling agent and a silica consolidating solution (50%w/w), are resistant to the leaching action of deionized water equilibriated with atmospheric COsb2 to pH 5. The aminoalkoxylsilane coupling agent catalyses the condensation reaction and also reacts with the surface to offer the coupling mechanism. Modulus of rupture strength tests on limestone cores treated with the AEAPS and silica-based consolidant showed a 25-35% increase in strength. Environmental scanning electron microscopy of treated limestone exposed to concentrated sulfuric acid showed degradation of the surface except in areas where thick layers of the consolidant were deposited. Powder leach tests using a pH-stat apparatus yielded quantitative proof of the efficacy of the biomimetic calcium oxalate process. The dissolution rates (2.14×10sp{-9} mmol/cmsp2/sec) of treated calcite were two orders of magnitude less than untreated calcium

  2. Encapsulation of fluorescence vegetable extracts within a templated sol-gel matrix

    NASA Astrophysics Data System (ADS)

    Lacatusu, Ioana; Badea, Nicoleta; Nita, Rodica; Murariu, Alina; Miculescu, Florin; Iosub, Ion; Meghea, Aurelia

    2010-04-01

    The sol-gel encapsulation of labile substances with specific properties and recognition functions within robust polymer matrices remains a challenging task, despite the considerable research that has been focused on this field. Numerous studies have been reported in the field of sol-gel processes regarding different physical and chemical packing of sensitive biomolecules encapsulated in silica matrix. In this paper the classical sol-gel synthesis has been used under mild conditions in order to minimize denaturizing effects on encapsulated active vegetable extracts from flavones class. The silica templated matrix was obtained by using two types of surfactants with different alkyl chain (didodecyldimethyl-ammonium bromide and trioctadecylmetilammonium bromide) as structure-directing agents for the silicon oxide framework. An organic precursor of silicic acid (triethoxymethylsilane) has been used and it was processed by competitive hydrolysis and polycondensation reactions under controlled directions assured by the presence of oriented template. Silica materials thus obtained are used for encapsulation of two flavonoid samples containing as active principles two sources: rutin and a vegetable extract from Begonia plant. The synthesis of encapsulated nanocompounds has been achieved taking into consideration the specific interaction between the colloidal gel precursors and molecular structures of selected biomolecules. The main objective was to improve the encapsulation conditions for specific biomolecules, searching for the highest stability and functionality without loosing the quality of the flavonoid properties, particularly optical properties like fluorescence. The structural properties of the encapsulated samples have been studied by FT-IR and UV-VIS spectroscopy, thermal analysis and SEM/EDX analysis. The fluorescence experiments showed that, in the case of all four encapsulated samples, the fluorescence spectra manifest a significant increase in intensity

  3. Thickness-Dependent Electrocaloric Effect in Pb0.9La0.1Zr0.65Ti0.35O3 Films Grown by Sol-Gel Process

    NASA Astrophysics Data System (ADS)

    Roh, Im-Jun; Kwon, Beomjin; Baek, Seung-Hyub; Kim, Seong Keun; Kim, Jin-Sang; Kang, Chong-Yun

    2016-02-01

    Unlike bulk materials, many physical properties of thin-film materials depend on film thickness due to extrinsic effects such as residual stress and the dead layer. In this work, the effect of thickness on the electrocaloric properties of Pb0.9La0.1(Zr0.65Ti0.35)O3(10/65/35) (PLZT) films grown by the sol-gel method was studied experimentally. In the sol-gel synthesis, the annealing process results in residual stress and the metal-dielectric contact generates a dead layer. These extrinsic effects influence the dielectric and ferroelectric properties of the thin films, and their roles are film thickness dependent. For PLZT of nanometer thickness (from 420 nm to 1080 nm), the permittivity and polarization, and their temperature dependences, showed strong dependence on film thickness. In particular, in the temperature range from 70°C to 350°C, the electrocaloric temperature change showed threefold improvement (from 0.2°C to 0.6°C) as the thickness was increased from 420 nm to 840 nm. This work will aid development of polycrystalline thin films including PLZT for electrocaloric applications.

  4. Structural and electrical properties of sol-gel spin coated indium doped cadmium oxide thin films

    SciTech Connect

    Rajammal, R.; Savarimuthu, E. Arumugam, S.

    2014-04-24

    The indium doped CdO thin films have been prepared by the sol-gel spin coating technique and the influence of indium doping concentration on the structural and electrical properties of the deposited films has been investigated. The indium doping concentration in the solution has been varied from 0-10 wt% insteps of 2wt%. A indium doping concentration of 6wt% has been found to be optimum for preparing the films and at this stage a minimum resistivity of 5.92×10{sup −4}Ω cm and a maximum carrier concentration of 1.20×10{sup 20}cm{sup −3} have been realized.

  5. Infrared spectroscopy analysis of the local atomic structure in silica prepared by sol-gel

    NASA Astrophysics Data System (ADS)

    Martínez, J. R.; Ruiz, F.; Vorobiev, Y. V.; Pérez-Robles, F.; González-Hernández, J.

    1998-11-01

    Infrared spectroscopy has been used to analyze the structural changes in samples prepared by the sol-gel method. Silica gels were prepared from alcoholic solutions of tetraethylorthosilicate (TEOS) with different H2O/TEOS molar ratios. The IR spectra of these gels, in the Si-O bond stretching region, shows that their structure strongly depends on the H2O/TEOS ratio. The relative change in intensity of the Si-O stretching modes, in samples prepared using different H2O/TEOS ratios, are interpreted in terms of different degrees of structural disorder. According to our infrared absorption data, a decrease in the H2O/TEOS ratio from about 7, the SiO2 structure evolves from a three-dimensional network toward a chainlike structure.

  6. Ice nucleation behaviour on sol-gel coatings with different surface energy and roughness.

    PubMed

    Fu, Q T; Liu, E J; Wilson, P; Chen, Z

    2015-09-01

    In this paper, the ice nucleation temperatures of 10 μL water droplets on a series of sol-gel coatings with different roughness and surface energies were obtained using a customized automatic measurement system. Classical nucleation theory was then employed to explain the different icing behaviour on the coatings. It was found that the wetting mode at low temperatures is strongly correlated with the icing behavior of the droplets on the surfaces. Ice-phobic coatings can lower the icing temperature of the droplet on the surface by up to 6.9 °C compared with non-icephobic ones. Using classical nucleation theory, our results support some recent observations that the dominant nucleation sites are along the substrate-water-vapour three-phase contact line rather than at the substrate-water interface. PMID:26220055

  7. Nanorods of Various Oxides and Hierarchically Structured Mesoporous Silica by Sol-Gel Electrophoresis

    SciTech Connect

    Limmer, Steven J.; Hubler, Timothy L.; Cao, Guozhong

    2003-01-02

    In this paper, we report the template-based growth of nanorods of oxides and hierarchically structured mesoporous silica, formed by means of a combination of sol-gel processing and elecrophoretic deposition. Both single metal oxides (TiO2) and complex oxides (Pb(Zr0.52Ti0.48)O3) have been grown by this method. This method has also been applied to the growth of nanorods of mesoporous silica having an ordered pore structure, where the pores are aligned parallel to the long axis of the nanorod. Uniformly sized nanorods of about 125-200 nm in diameter and 10 um in length were grown over large areas with near unidirectional alignment. Appropriate sol preparation yielded the desired stoichiometric chemical composition and crystal structure of the oxide nanorods, with a heat treatment (500-700 C for 15-30 min) for crystallization, densification and any necessary pyrolysis.

  8. Development of 3D photonic crystals using sol-gel process for high power laser applications

    NASA Astrophysics Data System (ADS)

    Benoit, F.; Dieudonné, E.; Bertussi, B.; Vallé, K.; Belleville, P.; Mallejac, N.; Enoch, S.; Sanchez, C.

    2015-08-01

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

  9. Stabilization of ZnMnO3 Phase from Sol-gel Synthesized Nitrate Precursors

    SciTech Connect

    Saraf, Laxmikant V.; Nachimuthu, Ponnusamy; Engelhard, Mark H.; Baer, Donald R.

    2010-02-01

    The stabilization and analysis of pure ZnMnO3 spinel phase may help to understand the solubility limits of Mn in ZnO in wurtzite and spinel cubic structures. In this report, synthesis and characterization of stable ZnMnO3 phase is discussed which is extracted from sol-gel synthesis of zinc and manganese nitrate precursors. The reflections at higher diffraction angles for this known cubic system with space group Fd3m were calculated with the help of JADE 8.0 program. High resolution X-ray photoelectron spectroscopy measurements of Mn3p position of ZnMnO3 compared with ZnMn2O4 showed a higher binding energy shift ~0.85 eV indicating Mn4+ valence state in ZnMnO3.

  10. Development of Metal Casting Molds By Sol-Gel Technology Using Planetary Resources

    NASA Technical Reports Server (NTRS)

    Sibille, L.; Sen, S.; Curreri, P.; Stefanescu, D.

    2000-01-01

    Metals extracted from planetary soils will eventually need to be casted and shaped in-situ to produce useful products. In response to this challenge, we propose to develop and demonstrate the manufacturing of a specific product using Lunar and Martian soil simulants, i.e. a mold for the casting of metal and alloy parts, which will be an indispensable tool for the survival of outposts on the Moon and Mars. Drawing from our combined knowledge of sol-gel and metal casting technologies, we set out to demonstrate the extraordinary potential of mesoporous materials such as aerogels to serve as efficient casting molds as well as fulfilling numerous other needs of an autonomous planetary outpost.

  11. The enhancement of benzotriazole on epoxy functionalized silica sol-gel coating for copper protection

    NASA Astrophysics Data System (ADS)

    Peng, Shusen; Zhao, Wenjie; Li, He; Zeng, Zhixiang; Xue, Qunji; Wu, Xuedong

    2013-07-01

    The influence of the amount of benzotriazole (BTA) on the wetting and anticorrosion ability of the epoxy functionalized silica sol-gel (ESol) coating was studied by various complementary methods. IR results demonstrate that BTA reacted with ESol through a 1:1 addition reaction of Nsbnd H to epoxy group. The water contact angle of the ESol coating increases with an increase in the amount of BTA. SEM and adhesion tests reveal that BTA could improve the adhesion of ESol to copper surface. Moreover, the best protection was achieved when the amount of BTA equals to the molar number of epoxy group in the ESol coating according to the results of electrochemical measurements and salt spray test.

  12. Study of ZnO:Zn Phosphors Prepared by Sol-gel and Ionimplantation Techniques

    NASA Astrophysics Data System (ADS)

    Shu-wen, Xue

    ZnO thin films were firstly deposited on glass substrates by the sol-gel process, and then Zn ions with energy of 56 keV were implanted into the ZnO films to a dose of 1×1017 cm-2. The effects of ion implantation on the structural and optical properties of the ZnO films were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), photoluminescence (PL) and optical transmittance measurements. The results showed that the as-deposited films had hexagonal wurtzite structure with high c-axis preferred orientation and (002) peak disappeared after ion implantation. Both the near band edge (NBE) excitonic UV emission at 390 nm and the defect related deep level emission (DLE) centered at 470 nm in the visible region were greatly decreased after Zn ion implantation. The optical band gap redshifted from 3.10 to 3.04 eV after ion implantation.

  13. Tailoring the oxidation state of cobalt through halide functionality in sol-gel silica

    PubMed Central

    Olguin, Gianni; Yacou, Christelle; Smart, Simon; Diniz da Costa, João C.

    2013-01-01

    The functionality or oxidation state of cobalt within a silica matrix can be tailored through the use of cationic surfactants and their halide counter ions during the sol-gel synthesis. Simply by adding surfactant we could significantly increase the amount of cobalt existing as Co3O4 within the silica from 44% to 77%, without varying the cobalt precursor concentration. However, once the surfactant to cobalt ratio exceeded 1, further addition resulted in an inhibitory mechanism whereby the altered pyrolysis of the surfactant decreased Co3O4 production. These findings have significant implications for the production of cobalt/silica composites where maximizing the functional Co3O4 phase remains the goal for a broad range of catalytic, sensing and materials applications. PMID:24022785

  14. Photoluminescence from terbium doped silica-titania prepared by a sol-gel method

    SciTech Connect

    Ismail, Adel Ali; Abboudi, Mostafa . E-mail: abboudi14@hotmail.com; Holloway, Paul; El-Shall, Hassan

    2007-01-18

    Terbium doped (0.5 at.%) TiO{sub 2}-SiO{sub 2} (30%/70%) was prepared by a sol-gel method. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the powder calcined at two different temperatures. At a low temperature of 550 deg. C an amorphous phase was obtained, but at a higher temperature of 1000 deg. C, the anatase TiO{sub 2} phase was crystallized in the amorphous SiO{sub 2} phase. Green photoluminescence from ultraviolet excitation was detected after heating to either temperature, but the amorphous sample heated to 550 deg. C exhibited a higher intensity. X-ray diffraction and photoluminescence excitation data are discussed to explain these observations.

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

    DOEpatents

    Pekala, Richard W.

    1998-04-28

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

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

    DOEpatents

    Pekala, Richard W.

    1996-01-01

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

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

    DOEpatents

    Pekala, R.W.

    1995-12-19

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

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

    DOEpatents

    Pekala, R.W.

    1996-09-17

    The sol-gel polymerization of a phenolic-furfural mixture in dilute solution leads to a highly cross-linked network that can be supercritically dried to form a high surface area foam. These porous materials have cell/pore sizes {<=}1,000{angstrom}, and although they are dark brown in color, they can be classified as a new type of aerogel. The phenolic-furfural aerogel can be pyrolyzed in an inert atmosphere at 1,050 C to produce carbon aerogels. This new aerogel may be used for thermal insulation, chromatographic packing, water filtration, ion-exchange, and carbon electrodes for energy storage devices, such as batteries and double-layer capacitors. 8 figs.

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

    DOEpatents

    Pekala, Richard W.

    1995-01-01

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

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

    DOEpatents

    Pekala, R.W.

    1998-04-28

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