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Sample records for sol-gel derived ferroelectric

  1. The Physics of Sol-Gel Derived Ferroelectric Thin Film PZT

    NASA Astrophysics Data System (ADS)

    Melnick, Bradley Michael

    Initial examination of a simple Auger depth profile reveals that thin film, pure lead zirconate titanate (PZT) is intrinsically a layered structure. Oxygen vacancies at the electrode interfaces create an n-type region in a normally p-type material by contributing electrons into the conduction band. Therefore, such measurable effects as the polarization versus applied field (hysteresis), and the dielectric constant versus applied field are all thickness dependent via a space charge effect on the surface of the material. M. E. Lines has suggested that the decay in switching polarization (fatigue) of barium titanate is linked to a build up of a space charge layer near the surface region. Although no specifics as to the source of the space charge layer (electronic or ionic) are given, it is implied that the space charge layer does inhibit switching due to an interaction with the domain nuclei. Therefore, it is plausible that degradation of the remnant polarization in PZT may also be connected with a surface layer. The implication from the above discussion is that thin film ferroelectric materials, such as sol-gel derived PZT, are intrinsically layered structures. This thesis involves the study of ferroelectric PZT synthesized via a solution-gelation technique (sol -gel). Using a reproducible and stable liquid solution, thin films are made by spinning droplets of the metalorganic liquid onto a substrate. The thin layers are then dried and annealed in order to form perovskite phase ferroelectric PZT capacitors for testing. A testing methodology is presented in order to test the capacitors unambiguous of artifacts due to the integration process. Capacitance versus voltage (CV), true DC leakage current, switching curve and hysteresis curve data is analyzed in order to examine the unique properties of the thin film ferroelectric. CV analysis indicates that a depletion region exists near the surface of the ferroelectric capacitor. The depletion region is found to dominate

  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 Hafnia Coatings

    NASA Technical Reports Server (NTRS)

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

    2002-01-01

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

  4. 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.

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

    SciTech Connect

    Shen Hongfang; Guo Qing; Zhao Zhiman; Cao Guozhong

    2009-11-15

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

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

    SciTech Connect

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

    2004-06-10

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

  7. Sol Gel-Derived SBA-16 Mesoporous Material

    PubMed Central

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

    2010-01-01

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

  8. 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.

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

    SciTech Connect

    Kueper, T.W.

    1992-05-01

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

  10. Granulation of sol-gel-derived nanostructured alumina

    SciTech Connect

    Deng, S.G.; Lin, Y.S.

    1997-02-01

    A sol-gel granulation process was developed to prepare porous nanostructured {gamma}-alumina granules as supports for catalysts and adsorbents. The process, which starts with an aqueous sol of gelatinous boehmite, involves droplet formation, gelation in paraffin oil, conditioning in ammonia solution, and drying and calcination in air under controlled conditions. The {gamma}-Al{sub 2}O{sub 3} granules prepared are 1--3 mm-dia. spherical particles with large surface area (380 m{sup 2}/g) and pore volume (0.5 cm{sup 3}/g), uniform pore-size distribution (20--60 {angstrom}), and controllable average pore size (35 {angstrom}). These sol-gel-derived granules have excellent mechanical properties with crush strength (>100 N per granule) and attrition resistance (<0.01 wt.%/h), much better than the commercial alumina and zeolite granules. Supported CuO sorbents were prepared on these granules for SO{sub 2} removal applications. The alumina-supported CuO sorbents contain higher loading of well-dispersed CuO and better sulfation properties than similar sorbents reported in the literature.

  11. Structure and electrical properties of Na0.5Bi0.5TiO3 ferroelectric thick films derived from a polymer modified sol-gel method.

    PubMed

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

    2011-10-01

    Lead-free NaBi(0.5)TiO(3) (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

  12. 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

  13. 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.

  14. Sol-gel-derived thick-film amperometric immunosensors.

    PubMed

    Wang, J; Pamidi, P V; Rogers, K R

    1998-03-15

    Sol-gel processing is used for the first time for the preparation of electrochemical immunosensors. One-step sensor fabrication, based on the coupling of sol-gel and screen-printing technologies, is employed. A low-temperature cured ink is prepared by dispersion of rabbit immunoglobulin G (RIgG), graphite powder, and a binder in the sol-gel solution. The enzyme-labeled antibody can readily diffuse toward the encapsulated antigen, which retains its binding properties, and the association reaction is easily detected at the dispersed graphite surface. Use of anti-RIgG labeled with alkaline phosphatase, naphthyl phosphate as the substrate, and amperometric detection at +400 mV (vs Ag/AgCl) results in a low detection limit of 5 ng/mL (32 pM) for the solution antigen. Tailoring the porosity of the ceramic-carbon matrix can be used for tuning the assay performance. The high sensitivity, low cost, durability, and simplicity of the new single-use immunosensors make them well suited for various on-site applications. PMID:9530007

  15. 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.

  16. 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.

  17. 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.

  18. 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. PMID:23171477

  19. Copper loaded on sol-gel-derived alumina adsorbents for phosphine removal.

    PubMed

    Hsu, Jung-Nan; Bai, Hsunling; Li, Shou-Nan; Tsai, Chuen-Jinn

    2010-05-01

    The hydride gas of phosphine (PH3) is commonly used for semiconductor and optoelectronic industries. The local scrubbers must immediately abate it because of its high toxicity. In this study, copper (Cu) loaded on the sol-gel-derived gamma-alumina (Al2O3) adsorbents are prepared and tested to investigate the possibility of PH3 removal and sorbent regeneration. Test results showed that during the breakthrough time of over 99% PH3 removal efficiency, the maximum adsorption capacity of Cu loaded on the sol-gel-derived gamma-Al2O3 adsorbent is 18 mg-PH3/g-adsorbent. This is much higher than that of Cu loaded on the commercial gamma-Al2O3 adsorbent--8.6 mg-PH3/g-adsorbent. The high specific surface area, narrow pore size distribution, and well dispersion of Cu loaded on the sol-gel-derived gamma-Al2O3 could be the reasons for its high PH3 adsorption capacity. The regeneration test shows that Cu loaded on the sol-gel-derived gamma-Al2O3 adsorbent can be regenerated after a simple air purging procedure. The cumulative adsorption capacity for five regeneration cycles is 65 mg-PH3/g-adsorbent, which is approximately double that of the Cu/zeolite adsorbent demonstrated in the literature. PMID:20480862

  20. 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. PMID:24189412

  1. A micron-size sol-gel-derived fiber-optic based chemical sensor

    SciTech Connect

    Ingersoll, C.M.; Narang, U.; Bright, F.V.

    1995-12-31

    The development of new chemical and biosensing schemes has been a topic of great interest. In our laboratory, a portion of our work has centered on the use of sol-gels doped with fluorescent dyes as materials for forming small optical fibers used for sensing. We are currently working with pyrene-doped fibers for oxygen sensing and fluorescein-doped fibers to detect changes in pH. These schemes have shown great promise, however, several factors (e.g., cost, size, rigidity, response time, sensitivity) are associated with building practical sensors. It is also critical to understand the actual sol-gel composite gelation process in order to quantitatively determine the appropriate conditions for forming microsensor tips from these sol-gel materials. This presentation will focus on the construction of an inexpensive, micron-size fiber-optic sensor as well as a small flow-cell apparatus for the detection of various analytes. Also, the actual preparation of these sol-gel derived optical fibers will be discussed.

  2. Synthesis and characterization of sol-gel-derived nanomaterials and nanocrystalline electroless metal coatings

    NASA Astrophysics Data System (ADS)

    Shukla, Satyajit Vishnu

    CuS (minimum size of 2.5 nm), Ag2S (minimum and average size of 2.5 nm and 26 nm respectively), and Au (with minimum size of <10 nm) nanoparticles dispersed within the sol-gel derived hydroxypropyl cellulose (HPC)-silica films are synthesized using the gas diffusion technique. The effectiveness of HPC polymer, as a 'compatibilizer', to synthesize semiconductor and metal nanoparticles distributed uniformly within the silica film is demonstrated. The sol-gel derived HPC-silica films containing dispersed nanoparticles are characterized using x-ray photoelectron spectroscopy (XPS) to understand the mechanism of formation of nanoparticles within the film. The XPS core-level binding energies (B.E.) for the nanoparticles are observed to be sensitive to the variation in the chemical composition at the surface and their size. The 'cluster size effect' is shown to be useful in predicting the average nanoparticle size. Nanocrystalline ZrO2 particles are successfully synthesized using sol-gel technique utilizing HPC polymer as a 'steric barrier'. The use of HPC polymer is demonstrated to synthesize submicron-sized, non-agglomerated, and spherical as well as nanocrystalline ZrO2 particles by adjusting the sol-gel synthesis parameters. The effect of sol-gel synthesis parameters on ZrO2 nanocrystallite size, its distribution, and the phase evolution behavior of ZrO2 is studied. The optimum sol-gel synthesis parameters for synthesizing nanocrystalline ZrO2 with 100% tetragonal phase are identified. Cu/CuO-ZrO2 composite powder is synthesized using the electroless metal deposition technique. The mechanism of electroless deposition of Cu over ZrO2 particle surface is investigated using XPS. On the basis of 'cluster size effect', it is suggested that, the electroless metal deposition process activates the non-catalytic ceramic substrate surface by depositing metallic Pd0 clusters and not by the accepted Pd-Sn alloy catalyst. Fly ash cenosphere particle surface is also activated by

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

    PubMed

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

    2004-08-01

    A firm bond between an implant and the surrounding soft tissue is important for the performance of many medical devices (e.g., stents, canyls, and dental implants). In this study, the performance of nonresorbable and reactive sol-gel-derived nano-porous titania (TiO(2)) coatings in a soft tissue environment was investigated. A direct attachment between the soft tissue and the sol-gel-derived titania coatings was found in vivo after 2 days of implantation, whereas the titanium control implants showed no evidence of soft tissue attachment. The coated implants were in immediate contact with the connective tissue, whereas the titanium controls formed a gap and a fibrous capsule on the implant-tissue interface. The good soft tissue attachment of titania coatings may result from their ability to initiate calcium phosphate nucleation and growth on their surfaces (although the formation of poorly crystalline bonelike apatite does not occur). Thus, the formation of a bonelike CaP layer is not crucial for their integration in soft tissue. The formation of bonelike apatite was hindered by the adsorption of proteins onto the initially formed amorphous calcium phosphate growth centers, thus preventing the dissolution/reprecipitation processes required for the formation of poorly crystalline bonelike apatite. These findings might open novel application areas for sol-gel-derived titania-based coatings. PMID:15227661

  4. 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. PMID:17037853

  5. 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.

  6. Formation and prevention of fractures in sol-gel-derived thin films.

    PubMed

    Kappert, Emiel J; Pavlenko, Denys; Malzbender, Jürgen; Nijmeijer, Arian; Benes, Nieck E; Tsai, Peichun Amy

    2015-02-01

    Sol-gel-derived thin films play an important role as the functional coatings for various applications that require crack-free films to fully function. However, the fast drying process of a standard sol-gel coating often induces mechanical stresses, which may fracture the thin films. An experimental study on the crack formation in sol-gel-derived silica and organosilica ultrathin (submicron) films is presented. The relationships among the crack density, inter-crack spacing, and film thickness were investigated by combining direct micrograph analysis with spectroscopic ellipsometry. It is found that silica thin films are more prone to fracturing than organosilica films and have a critical film thickness of 300 nm, above which the film fractures. In contrast, the organosilica films can be formed without cracks in the experimentally explored regime of film thickness up to at least 1250 nm. These results confirm that ultrathin organosilica coatings are a robust silica substitute for a wide range of applications. PMID:25466584

  7. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

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

  9. Fluorescence depolarization studies of sol-gel-derived glasses using a rigidochromic probe

    NASA Astrophysics Data System (ADS)

    McKiernan, John; Zink, Jeffrey I.; Dunn, Bruce S.

    1992-12-01

    The rigidochromic molecule rhenium(I)chlorotricarbonyl-2,2'-bipyridine was used in fluorescence depolarization experiments to probe the gelation, aging, and drying of silica and aluminosilicate sol-gel derived materials. These studies indicate that the local environment of the probe is fluid until well after gelation has occurred. Aluminosilicate gels show an increase in local viscosity after gelation while silica gels show no increase until the drying stage is begun. These results are compared to previous studies in which the shift of the emission band was used to indicate the rigidity in the local environment of the probe.

  10. Tunable Bragg stacks from sol-gel derived Ta2O5 and MEL zeolite films

    NASA Astrophysics Data System (ADS)

    Gospodinov, B.; Dikova, J.; Mintova, S.; Babeva, T.

    2012-12-01

    In this paper we investigated sol-gel derived Ta2O5 and nanosized MEL zeolite films obtained by spin coating of Tantalum sol and colloidal zeolite solution, respectively. Refractive index and thickness of the films were determined using non-linear curve fitting of measured reflectance spectra. The influence of the post deposition annealing on the optical properties and thickness of the films was studied. Besides tunable Bragg stacks were designed and prepared by layer-by-layer deposition of Ta2O5 and MEL suspensions with quarter-wave thicknesses. The influence of water, acetone and methanol on the optical behavior of Bragg stacks was discussed.

  11. 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.

  12. Temperature- and Frequency-Dependent Dielectric Properties of Sol-Gel-Derived BaTiO3-NaNbO3 Solid Solutions

    NASA Astrophysics Data System (ADS)

    Kwon, Do-Kyun; Goh, Yumin; Son, Dongsu; Kim, Baek-Hyun; Bae, Hyunjeong; Perini, Steve; Lanagan, Michael

    2016-01-01

    A sol-gel-derived powder synthesis method has been used to prepare BaTiO3-NaNbO3 (BT-NN) solid-solution ceramic samples with various compositions. Fine and homogeneous complex perovskite ceramics were obtained at lower processing temperatures than used in conventional solid-state processing. The ferroelectric and relaxor ferroelectric properties of the sol-gel-synthesized (1 - x)BaTiO3- xNaNbO3 [(1 - x)BT- xNN] ceramics in the wide composition range of 0 < x ≤ 0.7 were extensively studied. Structural and dielectric characterization results revealed that a low level of NN addition ( x = 0.04) to BT is sufficient to cause a continuous relaxor-to-ferroelectric transition, and the relaxor behavior was consistently observed at compositions with high NN content up to x = 0.7. A number of relaxor parameters including the Curie temperature, Burns temperature, freezing temperature, γ, diffuseness parameter ( δ), and activation energy were determined from the temperature and frequency dependency of the real part of the dielectric permittivity for various BT-NN compositions using the Curie-Weiss law and Vögel-Fulcher relationship. The systematic changes of these parameters with respect to composition indicate that a continuous crossover between BT-based relaxor and NN-based relaxor occurs at a composition near x = 0.4.

  13. 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

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

    PubMed Central

    Helka, Blake-Joseph; Brennan, John D.

    2013-01-01

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

  15. Biocompatibility of sol-gel-derived titania-silica coated intramedullary NiTi nails.

    PubMed

    Muhonen, V; Kujala, S; Vuotikka, A; Aäritalo, V; Peltola, T; Areva, S; Närhi, T; Tuukkanen, J

    2009-02-01

    We investigated bone response to sol-gel-derived titania-silica coated functional intramedullary NiTi nails that applied a continuous bending force. Nails 26 mm in length, either straight or with a radius of curvature of 28 or 15 mm, were implanted in the cooled martensite form from a proximal to distal direction into the medullary cavity of the right femur in 40 Sprague-Dawley rats. Body temperature restored the austenite form, causing the curved implants to generate a bending force on the bone. The femurs were examined after 24 weeks. Bone length measurements did not reveal any bowing or shortening of the bone in the experimental groups. The results from histomorphometry demonstrated that the stronger bending force, together with sol-gel surface treatment, resulted in more bone deposition around the implant and the formation of significantly less fibrous tissue. Straight intramedullary nails, even those with a titania-silica coating, were poorly attached when compared to the implants with a curved austenite structure. PMID:18838349

  16. Nonvolatile memory devices prepared from sol-gel derived niobium pentoxide films.

    PubMed

    Baek, Hyunhee; Lee, Chanwoo; Choi, Jungkyu; Cho, Jinhan

    2013-01-01

    We report on the resistive switching nonvolatile memory (RSNM) properties of niobium pentoxide (Nb(2)O(5)) films prepared using sol-gel chemistry. A sol-gel derived solution of niobium ethoxide, a precursor to Nb(2)O(5), was spin-coated on to a platinum (Pt)-coated silicon substrate, and was then annealed at approximately 620 and 450 °C to form a Nb(2)O(5) film of polycrystalline and amorphous structure, respectively. A top electrode consisting of Ag, W, Au, or Pt was then coated onto the Nb(2)O(5) films to complete the fabrication. After a forming process of limited current compliance up to 10 mA, known as "electroforming", a resistive switching phenomenon, independent of voltage polarity (unipolar switching), was observed at low operating voltages (0.59 ± 0.05 V(RESET) and 1.03 ± 0.06 V(SET)) with a high ON/OFF current ratio above 10(8). The reported approach offers opportunities for preparing Nb(2)O(5)-based resistive switching memory devices from solution process. PMID:23210494

  17. 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.

  18. 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

  19. 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.

  20. 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

  1. 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.

  2. Structure and Properties of Laser-Fired Sol-Gel Derived Tungsten Oxide Films

    NASA Astrophysics Data System (ADS)

    Taylor, Douglas John

    1995-01-01

    This investigation focuses on the use of laser radiation to fire sol-gel derived oxide films. The main emphasis of this work was to make high quality tungsten oxide films with good electrochromic properties. Laser firing was done with a carbon dioxide laser operated in continuous mode. The laser-fired tungsten oxide films were measured for density, composition, crystallinity and electrochromic behavior. Analytical tools included multi -angle ellipsometry, FTIR, TEM, XRD, spectrophotometry and electrochemistry. The effect of process variables (laser power, spot size and translation speed) on the extent of film densification and microstructural evolution was investigated. Thermal modeling of laser-heated sol-gel films was studied to further understand the laser firing process and to estimate firing temperatures. Temperature calculations were based on laser parameters, sample geometry and target materials. Properties characteristic of firing temperature were used to verify the thermal modeling. For laser-fired films, the properties at the calculated temperatures agreed well with the properties of similar furnace-fired films. The modeling also provided the thermal profiles seen by the laser heated materials. Laser firing was shown to be a feasible technique to make good quality electrochromic films. By precisely controlling the irradiation, the microstructure of tungsten oxide films was tailored to produce the desired electrochromic properties. Transmission electron microscopy showed film microstructures that varied from completely amorphous to fully crystalline. Corresponding optoelectrochemical measurements indicated a decrease in electrochromism with increasing crystallinity. The effects of density/porosity and coating composition are also discussed. It is proposed that laser firing of sol-gel derived films can be used for optics, sensors, graded index materials, and electrochromic windows. The ability to heat localized regions afforded by laser firing is

  3. Sol-gel derived titania coating with immobilized bisphosphonate enhances screw fixation in rat tibia.

    PubMed

    Linderbäck, Paula; Areva, Sami; Aspenberg, Per; Tengvall, Pentti

    2010-08-01

    A variety of surface modifications have been tested for the enhancement of screw fixation in bone, and locally delivered anti-osteoporosis drugs such as bisphosphonates (BP) are then of interest. In this in vivo study, the impact of surface immobilized BP was compared with systemic BP delivery and screws with no BP. After due in vitro characterization, differently treated stainless steel (SS) screws were divided into four groups with 10 rats each. Three of the groups received screws coated with sol-gel derived TiO(2) and calcium phosphate (SS+TiO(2)+CaP). One of these had no further treatment, one had alendronate (BP) adsorbed to calcium phosphate mineral, and one received systemic BP treatment. The fourth group received uncoated SS screws and no BP (control). The screw pullout force was measured after 4 weeks of implantation in rat tibiae. The immobilized amount and release rate of alendronate could be controlled by different immersion times. The SS+TiO(2)+CaP coating did not increase the pullout force compared to SS alone. Surface delivered alendronate enhanced the pullout force by 93% [p = 0.000; 95% Confidence Interval (CI): 67-118%] compared to SS, and by 39% (p = 0.044; 95% CI: 7-71%) compared to systemic alendronate delivery. Both surface immobilized and systemically delivered alendronate improved implant fixation. Also, locally delivered, that is, surface immobilized alendronate showed a better fixation than systemically delivered. Using sol-gel derived TiO(2) as a platform, it is possible to administer controllable amounts of a variety of BPs. PMID:20186735

  4. 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.

  5. 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.

  6. Influence of calcium precursors on the morphology and crystallinity of sol gel-derived hydroxyapatite nanoparticles

    NASA Astrophysics Data System (ADS)

    Vijayalakshmi Natarajan, U.; Rajeswari, S.

    2008-10-01

    Nanosized hydroxyapatite (HAP) particles were prepared by sol-gel method from the water-based solution of calcium and phosphorus precursor. In this study, two calcium precursors such as calcium nitrate tetrahydrate and calcium acetate were chosen as calcium precursors. The influence of aging period, pH, viscosity and sintering temperature on crystallinity and morphology of the HAP particles were investigated for the two calcium precursors with triethyl phosphate precursor. The morphology of nano-HAP towards phosphorous precursor was dependent on the type of calcium precursor used. The HAP prepared from calcium nitrate and triethyl phosphate was spherically shaped whereas the one from calcium acetate was found to be fibrous in structure. Both HAPs were stable up to 1200 °C and their crystallinity increased with respect to the sintering temperature. The obtained sample was characterized through X-ray diffraction (XRD), P 31 nuclear magnetic resonance (NMR), scanning electronic microscopy (SEM) and TEM analysis. The sol derived from the optimized aging period for the two different calcium precursors was coated on 316L stainless-steel (SS) implant and its corrosion resistivity during long-term implantation was studied by cyclic polarization in Ringer's solution. Both HAPs have their own desirable qualities and were found to be corrosion resistive.

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

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

    Sol-gel derived organic-inorganic hybrid materials doped with rare earth metal ions (Pr 3+) and small amounts of lithium ions (˜0.1-0.2 wt.%) were produced from the tetraethyl orthosilicate (TEOS), AlCl 3·6H 2O (about 10 mol%), ethyl methacrylate, butyl methacrylate and some other organic additions (ca. 35-40 wt.% of organics in the fresh gels) to obtain hybrid organic-inorganic hosts. The gel and hybrid materials obtained were aged at room temperature for three weeks, then heated in an electric drier for 3 h at temperature of 125 °C and investigated for morphology, structure and luminescence properties by X-ray diffraction (XRD), scanning electron microscopy equipped with energy dispersive X-ray spectroscopy (SEM/EDS), Fourier transform infrared spectroscopy (FTIR), 29Si and 27Al MAS nuclear magnetic resonance and fluorescence spectroscopy. An influence of the organic additions and inorganic dopants on microstructure of the materials obtained and their luminescence properties has been examined. Under excitation with UV radiation in a range of ˜210-350 nm, the sharp and relatively intense luminescence emission lines due to 3P 0 → 3H 4 (blue) and 3P 0 → 3F 3 (red) transitions of Pr 3+ ions were observed in the luminescence spectra of gel and hybrid materials of SA-series.

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

    PubMed

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

    2014-09-01

    Silica-based sol-gel coatings have gained attention in bone therapies and orthopedic applications, due to the biocompatibility and bioactivity, including a high potential for the controlled release both in vitro and in vivo. Bioactive materials are created to facilitate the biocompatibility of orthopedic implants. One of the promising alternatives is biomaterials with immobilized drugs. In this study we demonstrated for the first time novel sol-gel-derived silica coatings with active amino groups (SiO2(NH2)) functionalized with a steroid drug-betamethasone, applied to a substrate 316 L using dip coating technique. The presence of betamethasone in functionalized coatings was directly confirmed by Raman spectroscopy and energy-dispersive X-ray spectroscopic analysis. The wettability was evaluated by the sessile drop method, while the surface free energy was estimated based on the contact angles measured. Our results showed a shift in surface properties from hydrophobic to hydrophilic after application of the coatings. We have investigated the morphology, proliferation factor, and the population doubling time of adipose-derived stem cells for biological purposes. Moreover, the analysis of the distribution and localization of cellular microvesicles was performed to evaluate the influence of functionalized surfaces on cellular cytophysiological activity. Increased proliferation and activation of cells, determined by the observations of microvesicles shedding processes, provided evidence of the availability of the drug. Therefore, we conclude that the sol-gel synthesis proposed here allows to improve the metal substrates and can be successfully used for immobilization of betamethasone. This in turn enables the direct delivery of the drug with implanted material into the wound site, and to stimulate the activity of cells to enhance tissue regeneration. PMID:24825759

  9. Development of residual stress in sol-gel derived Pb(Zr ,Ti)O3 films: An experimental study

    NASA Astrophysics Data System (ADS)

    Corkovic, S.; Whatmore, R. W.; Zhang, Q.

    2008-04-01

    Residual stresses develop in the sol-gel-derived ferroelectric thin films during the transformation of the metal-organic gel to the metal oxide upon thermal treatment and due to the thermal and elastic mismatch between the Pb(Zrx,Ti1-x)O3 (PZT) film and the substrate materials during cooling. In this study, residual stresses were determined using the wafer curvature method after the deposition of multilayer PZT film on platinized (100) silicon wafers. A multilayer model for stress analysis was used to calculate the residual stress in PZT films of three different compositions: x =0.4, x =0.52, and x =0.6. Orientation dependent residual stresses were found in compositions containing the tetragonal phase, with x =0.4 and x =0.52. Depending on the fraction of (100) orientated domains low compressive or low tensile stress was found in Pb(Zr0.4Ti0.6)O3 (PZT 40/60). Higher residual stress was found in PZT films consisting of only rhombohedral crystallographic structure (PZT 60/40) while the residual stress in PZT films with morphotropic boundary composition (PZT 52/48) was significantly dependent on the film orientation and the phase composition and could range from 17to90MPa. The effect of the film orientation on residual stress was found to be a function of the anisotropic thermal expansion coefficient of PZT. The contribution of the thermal and elastic properties of materials to the total wafer curvature was investigated and discussed. Finally, the residual stress results calculated with the four layer model were compared to the results calculated using the Stoney equation.

  10. 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

  11. Investigation of correlation between the microstructure and electrical properties of sol-gel derived ZnO based thin films

    NASA Astrophysics Data System (ADS)

    Zhu, M. W.; Gong, J.; Sun, C.; Xia, J. H.; Jiang, X.

    2008-10-01

    Pure ZnO and aluminum doped ZnO films (ZAO) were prepared by sol-gel method and the effect of Al doping on the microstructure and electrical properties of the films was investigated. The results showed that the transformation from granular to columnar structure could be observed in pure ZnO films with the increase in heating time while in aluminum doped films little structural changes occurred even after a prolonged heating time. Additionally, measurements of electrical properties showed that both microstructural evolution and doping could significantly improve the conductivity of the films, which could be assigned to an increase both in Hall mobility and carrier concentration. The relationship between microstructure and the electrical properties of the films was discussed, and various scattering mechanisms were proposed for sol-gel derived ZnO and ZAO films as a function of the carrier concentration.

  12. 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

  13. 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

  14. 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.

  15. Preparation and characterization of protein-doped sol-gel derived nanocomposite films for biosensor development

    NASA Astrophysics Data System (ADS)

    Goring, Gillian Louise Grace

    The entrapment of biomolecules within TEOS-based sol-gel derived organic/inorganic nanocomposite materials has proven to be a viable platform for the development of biosensors and solid-phase biocatalysts. In this thesis, a series of organically modified silica materials were prepared by a two-step aqueous processing method that was suitable for biomolecule entrapment, and were formed as submicron thick films by dipcasting. Dispersed additives, such as polymers (Class I materials) and covalently bound additives, such as organically modified silanes (Class II materials), were used to modify the internal environment compared to the undoped matrices and to correlate the properties of entrapped enzymes. The morphology of organically modified silica materials could be modified through the use of either separate or co-hydrolysis of the silane precursors, with the later method generating optically transparent materials. Fluorescence microscopy revealed chemical heterogeneity in materials that appeared to be homogeneous by brightfield or SEM. Fluorescence emission studies of a solvatochromic dye entrapped within the film continued that the internal chemical environment of the films was strongly affected by doping with polymers and organosilanes. The films showed a rapid initial change in chemical properties owing to solvent evaporation, followed by a much slower evolution over several months owing to continued condensation reactions within the film. A reagentless biosensor was designed based on co-entrapment of an enzyme and a fluorescently labeled polymer. The enzymes urease and lipase were selected for this study as both catalyze reactions that alter the local pH. By co-entrapping pH sensitive fluorophores (SNARF-1 and fluorescein) bound to a high molecular weight polymer, it was possible to detect the analytes urea and glyceryl tributyrate using changes in the fluorescence intensity (fluorescein) or emission ratio (SNARF-1). By tuning the polarity of the matrix it was

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

    PubMed

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

    2013-02-01

    α-Fe(2)O(3) (hematite) photoanodes for the oxygen evolution reaction (OER) were prepared by a cost-efficient sol-gel procedure. Due to low active photoelectrochemical properties observed, it is assumed that the sol-gel procedure leads to hematite films with defects and surface states on which generated charge carriers are recombined or immobilized in trap processes. Electrochemical activation was proven to diminish unfavourable surface groups to some extent. More efficiently, a plasma treatment improves significantly the photoelectrochemical properties of the OER. X-ray photoelectron spectroscopy (XPS) analysis reveals an oxygen enriched surface layer with new oxygen species which may be responsible for the improved electrochemical activity. Due to surface photovoltage an increased fraction of transferred charge carriers from these newly produced surface defects are identified. PMID:23247669

  17. Optical sensors based on sol-gel derived, laminate planar waveguide structures

    SciTech Connect

    Yang, Lin; Armstrong, N.R.; Dunphy, D.R.; Saavedra, S.S.

    1995-12-31

    A new optical sensing platform based on a combination of planar and sol-gel processing technologies is described. The sensing element is a planar integrated optical waveguide (IOW) composed of two, submicron thick glass layers coated on glass substrate; both layers are fabricated via the sol-gel method. The lower layer is a densified titania-silica composite. The upper layer is an undensified silica doped with an optical indicator that is physically entrapped yet sterically accessible to dissolved analytes that can diffuse into the pore network. Formation of an analyte-indicator complex is detected via attenuated total reflection (ATR) of light guided in the IOW. The sensor response is both sensitive and rapid, features that are difficult to achieve simultaneously in monolithic sol-gel glass sensors. In the IOW-ATR geometry, these features are realized simultaneously because the primary axes of light propagation and analyte diffusion are orthogonal. The overall approach is technically simple, inexpensive, and applicable to a wide variety of indicator chemistries.

  18. Chemical sensing using sol-gel derived planar waveguides and indicator phases

    SciTech Connect

    Yang, L.; Saavedra, S.S.

    1995-04-15

    A new optical sensing platform based on a combination of planar waveguiding and sol-gel processing technologies is described. The sensing element consists of two, submicrometer thick glass layers supported on an optically thick glass substrate; both layers were fabricated using a sol-gel coating method. The lower layer is a densified glass that functions as a planar integrated optical waveguide (IOW). The upper layer is an undensified glass of lower index doped with an optical indicator that is immobilized, yet remains sterically accessible to analytes that diffuse into the pore network. Formation of a complex between the analyte and indicator is detected via attenuated total reflection (ATR) of light guided in the IOW. Feasibility was evaluated by constructing IOW-ATR sensors for Pb{sup 2+} and pH, based on immobilized xylenol orange and bromocresol purple, respectively. The response of both sensors was sensitive and rapid, features that are difficult to achieve simultaneously in monolithic sol-gel glass sensors. In the IOW-ATR geometry, these features are realized simultaneously because the primary axes of light propagation and analyte diffusion are orthogonal. The overall approach is technically simple, inexpensive, and applicable to a wide variety of indicator chemistries. 48 refs., 8 figs.

  19. Low-temperature sol-gel-derived nanosilver-embedded silane coating as biofilm inhibitor

    NASA Astrophysics Data System (ADS)

    Babapour, A.; Yang, B.; Bahang, S.; Cao, W.

    2011-04-01

    Silver nanocomposite coatings are prepared by the sol-gel method for the prevention of biofilm formation on the surface of medical implanted devices. High-temperature processing of such coatings can lead to diffusion of nanosilver and reduce the amount of available silver particles for long-term effects. Using a low-temperature sol-gel method, we have successfully prepared silane-based matrices, phenyltriethoxysilane (PhTEOS), containing different amounts of Ag nanoparticles. The incorporation of a silver salt into the sol-gel matrix resulted in a desired silver release rate, i.e. high initial release rate followed by a lower sustained release for more than 15 days, as determined by inductively coupled plasma mass spectrometry (ICP-MS). Scanning electron microscopy (SEM) has been employed to investigate the morphology of the film surfaces before and after immersion in a nutrient-rich bacterial suspension of approximately 108 CFU ml - 1, which was incubated for up to 30 days at 37 °C. It was found that thin films containing 35 nm particles could prevent the formation of biofilm for over 30 days. The presence of surface silver before and after 3, 9 and 15 days immersion was confirmed by x-ray photoelectron spectroscopy (XPS).

  20. The effect of lithiation on the electrochromism of sol-gel derived niobium oxide films

    SciTech Connect

    Macek, M.; Orel, B.; Krasovec, U.O.

    1997-09-01

    Niobium oxide films are promising cathodic electrochromic materials that in certain aspects can compete with the more frequently studied WO{sub 3} films. The films reported here were prepared using the sol-gel route from a NbCl{sub 5} precursor. The electrochromic properties were pronounced for crystalline films heat-treated at 500 C exhibiting transmittance changes between the colored and bleached states of 60% in the ultraviolet (UV) and 80% in the visible and near-infrared spectral regions. The reversibility of electrochromic changes of thick niobium oxide films (d > 250 nm) was enhanced by lithiation.

  1. 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.

  2. Growth of vertically aligned one-dimensional ZnO nanowire arrays on sol-gel derived ZnO thin films

    NASA Astrophysics Data System (ADS)

    Kitazawa, Nobuaki; Aono, Masami; Watanabe, Yoshihisa

    2014-11-01

    Vertically aligned one-dimensional ZnO nanowire arrays have been synthesized by a hydrothermal method on sol-gel derived ZnO films. Sol-gel derived ZnO films and corresponding ZnO nanowire arrays have been characterized by X-ray diffraction and field-emission scanning electron microscopy. The effect of sol-gel derived ZnO film surface on the morphology of ZnO nanowire arrays has been investigated. The authors suggest from our investigation that sol-gel derived ZnO films affect the growth of one-dimensional ZnO nanostructures. Not only crystalline ZnO films but also amorphous ones can act as a scaffold for ZnO nucleus. Tilted ZnO micro-rods are grown on ZnO gel films, whereas vertically aligned ZnO nanowire arrays are grown on nanometer-sized ZnO grains. The average diameter of ZnO nanowire arrays are correlated strongly with the grain size of sol-gel derived ZnO films.

  3. Effects of ion irradiation on the surface mechanical behavior of hybrid sol-gel derived silicate thin films

    NASA Astrophysics Data System (ADS)

    Ghisleni, Rudy

    A study on the effects of ion irradiation on the surface mechanical behavior of hybrid sol-gel derived thin films has been performed. Hybrid organic/inorganic modified silicate thin films were synthesized by sol-gel processing from tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES) precursors and spin-coated onto (100) Si substrates. The synthesized films were investigated by nanoindentation, photoluminescence spectroscopy, and Raman spectroscopy. Hybrid TEOS/MTES sol-gel films modified by ion irradiation with deposited electronic energies of 1.87 x 1025 eV/cm3 or higher showed higher values of reduced elastic modulus and hardness than 800°C heat treated films. Thus, ion irradiation was found to be an effective means in converting the polymer sol into ceramic type coatings. The ions used in this study were Cu2+, N2+, Si+, O+, N+, He+, and H+, with incident energies ranging from 100 keV to 2 MeV, and fluences ranging from 1 x 1014 to 1 x 1017 ions/cm2. Both the reduced elastic modulus and hardness were seen to increase monotonically with the increase in ion fluence, with an observed maximum hardness of 7.7 GPa (an unirradiated film hardness was 0.4 GPa) and a maximum reduced elastic modulus of 84.0 GPa (an unirradiated film reduced elastic modulus was 7.1 GPa) for 250 keV N2+ irradiation with a 5 x 1016 ions/cm2 fluence. The electronic stopping power was found to be principally responsible for the film hardening, while the role of nuclear stopping power was minimal. A monotonic increase in hardness with increase in electronic energy deposited to the film surface was found. A model describing the hardening of ion irradiated films was developed. This model characterizes the hardening effectiveness of the ion species considered by two parameters: the constant hardening cross-section and the hardening coefficient. Where the hardening cross-section represents the cross-sectional area hardened by the interaction of an incident ion with the target, and the

  4. Sol-gel derived ZnO thin films: Effect of amino-additives

    NASA Astrophysics Data System (ADS)

    Hosseini Vajargah, P.; Abdizadeh, H.; Ebrahimifard, R.; Golobostanfard, M. R.

    2013-11-01

    Zinc oxide thin films were dip-coated from an alcoholic sol of zinc acetate with different amino-additives including monoethanolamine, diethanolamine, triethanolamine, triethylamine, and ethylenediamine. Sol-gel behavior, crystal structure, optoelectronic and morphological properties of thin films were investigated with focus on the effects of different amines and drying conditions. Investigations explicate the role of chemical and physical properties of amines such as organic chains, polarity, and boiling point as the main factors that cause distinct sol-gel behavior and film properties. It is shown that different amines in different molar ratios together with drying temperature cause dramatic impacts on sol transparency, stability, and consequently on structural, optoelectronic, and morphological properties of films. Notably, monoethanolamine and triethylamine films demonstrate a preferred orientation stimulated by increased molar ratio of amines. Further investigations indicated the positive effect of elevated drying temperature particularly on those films prepared from sols with high-boiling-point stabilizers. The variation of film optoelectronics seems to depend mainly on heat treatment, whereas sol chemistry influences the optical properties indirectly through the structural alteration. Peculiar morphologies in the ethylenediamine films disappeared with adjusting the drying conditions. The size of ZnO grains were approximately independent of amine types and primarily affected by the heat treatment

  5. Sol gel derived hydroxyapatite coatings on titanium and its alloy Ti6Al4V

    NASA Astrophysics Data System (ADS)

    Stoch, A.; Jastrzebski, W.; Długoń, E.; Lejda, W.; Trybalska, B.; Stoch, G. J.; Adamczyk, A.

    2005-06-01

    Titanium has been used for many medical and dental applications; however, its joining to a living bone is not satisfactorily good or the implant integration with bone tissue takes several months.The aim of this work is to produce hydroxyapatite (HAP) coatings on titanium and its alloy for facilitating and shortening the processes towards osseointegration. HAP coatings were obtained by sol-gel method with sol solutions prepared from calcium nitrate tetrahydrate and triammonium phosphate trihydrate as the calcium and phosphorous sources. Two types of gelatine were added to the sol: agar-agar or animals gelatine. Both were found to enhance the formation and stability of amorphous HAP using soluble salts as the sources of calcium and phosphate. HAP coatings were deposited from HAP-GEL sol using dip-withdrawal technique, then the plates were dried and annealed at temperatures 460-750 °C. FTIR spectroscopy and XRD analysis were used to study the phase composition of phosphate coatings. Morphology and chemical analysis of HAP layers was performed using a scanning electron microscope equipped with an energy dispersive X-ray analyser (SEM+EDX). The biological activity of sol-gel phosphate coatings was observed during thermostatic held in simulated body fluid (SBF). It was found that chemical composition and structure of HAP coatings depends on pH and final thermal treatment of the layer.

  6. Sol-gel-derived composite antimony-doped, tin oxide-coated clay-silicate semitransparent and conductive electrodes.

    PubMed

    Sadeh, A; Sladkevich, S; Gelman, F; Prikhodchenko, P; Baumberg, I; Berezin, O; Lev, O

    2007-07-15

    A new form of conductive and transparent porous composite electrode is introduced. The electrode material is composed of antimony-doped, tin oxide (ATO)-coated mica platelets imbedded in sol-gel-derived silicate or methyl silicate network. The platelet clays self-align in a layered structure within the silicate film, an anisotropic construction that minimizes the ATO loading required to achieve electric percolation. Transparency and resistance as a function of clay loading is reported with typical values of 100 k Omega/square and 1.5 OD for a 20-microm-thick film. The transparency is lower as compared to sputtered ATO glasses, but this is, as far as we know, the best method for the low-temperature preparation of transparent, porous, and electrically conductive (as opposed to the amply reported ionically conductive) electrode materials. Permselectivity induced by the silicate and clay ingredients is demonstrated by permeation of positively charged methyl viologen compared to negatively charged ferricyanide. Prussian blue-modified ATO-coated platelets dispersed in sol-gel-derived silicate were used to demonstrate feasibility of a transparent and electrically conductive porous electrochromic material. PMID:17555295

  7. 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

  8. 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

  9. Spectroellipsometric studies of sol-gel derived Sr0.6Ba0.4Nb2O6 films

    NASA Astrophysics Data System (ADS)

    Ho, Melanie M. T.; Tang, T. B.; Mak, C. L.; Pang, G. K. H.; Chan, K. Y.; Wong, K. H.

    2006-10-01

    Sr0.6Ba0.4Nb2O6 (SBN) films have been fabricated on (001)Si substrates by a sol-gel technique. The annealing process was carried out in air at various temperatures ranging from 200to700°C. Studies using x-ray diffractometry, high resolution transmission electron microscopy, and scanning electron microscopy showed that polycrystalline films, with a grain size of about 100nm, were obtained only for annealing temperatures ⩾600°C. The optical properties of these sol-gel derived SBN films were studied by spectroscopic ellipsometry (SE). In the analysis of the measured SE spectra, a triple-layer Lorentz model has been developed and used to deduce the optical properties of the SBN films. Our systematic SE measurements revealed that the refractive indices of the SBN films increase with the annealing temperature. This increase is more pronounced at around the crystallization temperature, i.e., between 500 and 600°C. The extinction coefficients of the films also exhibit a similar trend, showing a zero value for amorphous films and larger values for films annealed at above 600°C. Our results demonstrate that while crystallization helps to raise the refractive index of the film due to film densification, it also promotes scattering by grain boundary, resulting in a larger extinction coefficient.

  10. Second-harmonic generation in metal oxide/ormosils nanocomposites derived from sol-gel processing

    NASA Astrophysics Data System (ADS)

    Cheng, Chih-Hsing; Xu, Yuhuan; Mackenzie, John D.; Chee, Joseph K.; Liu, Jia-ming

    1992-12-01

    Nanocomposites of Ormosis containing metal oxides, such as niobates, titanates and zirconates, were prepared by sol-gel processing. The materials were hydrolyzed partially and were dried in air atmosphere for appropriate periods. Afterwards, the materials were heat- treated between 200 degree(s) and 450 degree(s)C for 2 days in pure oxygen. The final bulk samples are transparent in infrared and visible ranges. X-ray diffraction patterns showed that these samples did not have any crystalline phases after heating up to 200 degree(s)C. Using a Nd:YAG laser of 1.064 micrometers wavelength, second harmonic generation, of green light (0.532 micrometers ), was observed in these metal oxides/Ormosils nanocomposites. The refractive index and other optical properties of the metal oxides/Ormosils were also measured. The microstructures of these samples were examined by transmission electron microscopy.

  11. 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.

  12. A new type of a sol-gel-derived inorganic-organic nanocomposite

    SciTech Connect

    Kasemann, R.; Schmidt, H.K.; Wintrich, E.

    1994-12-31

    A new type of sol-gel-based transparent inorganic-organic nano composites has been developed by increasing the inorganic phase dimension to values just below the point, where scattering can be neglected. For this purpose, nanosized boehmite particles {le} < 50 nm are homogeneously incorporated in a sol based on tetraethoxysilane and an epoxysilane. The nanoscale boehmite particles act as catalysts for the polymerization of the epoxy silane to polyethylene oxide, as proved by {sup 13}C NMR, and are linked to the matrix by Si-O-Al bridges, as proven by {sup 27}Al-NMR spectroscopy. The synthesized sols can be applied by standard coating techniques on transparent polymers and are cured thermally. The mechanical properties (scratch resistance, hardness) have been substantially improved compared to systems with molecular dimensions of the inorganic phase. The effect is attributed to the special structure of flexibly suspended nano-scale boehmite particles in an inorganic-organic network by a tailored interface.

  13. 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.

  14. 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.

  15. Sol-gel kinetics by NMR

    SciTech Connect

    Assink, R.A.; Kay, B.D.

    1991-01-01

    The chemical synthesis of advanced ceramic and glass materials by the sol-gel process has become an area of increasing activity in the field of material science. The sol-gel process provides a means to prepare homogeneous, high purity materials with tailored chemical and physical properties. This paper surveyed the nuclear magnetic resonance (NMR) studies of silicon-based sol-gel kinetics. A review of the various models which have been used to analyze the chemical kinetics of various sol-gel systems was presented. The utility of NMR spectroscopy was demonstrated in investigating the influence that various reaction conditions have on the reaction pathways by which sol-gel derived materials are synthesized. By observing in a direct fashion the chemical pathway of the sol-gel, it is often possible to relate the final properties of the material to the formulation and reaction conditions of the sol-gel. The study of reaction kinetics by NMR is expected to play an increasingly important role in understanding sol-gel processing and material properties. 15 refs. (DP)

  16. Role of spinodal-like wrinkling as a prenucleation process in crystallization of sol-gel derived thin films

    NASA Astrophysics Data System (ADS)

    Valant, Matjaz; Fanetti, Mattia; Luin, Uros

    2016-04-01

    Studies of crystallization of a sol-gel derived alumina thin film showed on a critical role of spinodal-like wrinkling. The wrinkling that depends on a humidity gradient in the film provides nucleation sites with high supersaturation located at the top of topological islands that occur as a result of the wrinkling. Nucleation of crystal nuclei takes place at these sites at a significantly lower temperature as it would be the case for homogenous nucleation. The crystal growth continues through different supersaturation regimes that are defined by the wrinkling topology. We showed how the crystallization can be efficiently suppressed to higher temperatures by minimizing the humidity gradient in the dip-coated film by controlled drying.

  17. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-04-01

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

  19. Optical fibers from sol-gel-derived germania-silica glasses

    NASA Astrophysics Data System (ADS)

    Kirkbir, Fikret; Chaudhuri, S. R.

    1992-12-01

    Step index multimode optical fibers were successfully drawn from germania doped silica rods prepared by sol-gel process. The fiber, drawn using rod-in-tube technique, had a 100 micron core with a pure silica cladding of 140 micron. The numerical aperture of the fiber was 0.21. Initial experimental results indicate an attenuation of 20 dB/km at 850 nm wavelength. Precursors used for sol preparation were tetraethyl orthosilicate, Si(OC2H5)4 and tetraethyl orthogermanate, Ge(OC2H5)4. Clear wet gels were routinely produced without any problem of premature precipitation of germanium dioxide even at high dopant concentration levels. The gels were dried by supercritical drying technique. Dry gels were consolidated to clear glass samples routinely at a temperature of 1300 degree(s)C. Fiber was drawn from these rods at a temperature of 1800 degree(s)C. The sintering parameters, i.e., type of gas flow at different steps of the sintering operation, duration of such steps and temperature were optimized to eliminate reboil of the glass above 1800 degree(s)C, resulting in bubble-free glass fibers.

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

    NASA Astrophysics Data System (ADS)

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

    2012-06-01

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

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

    PubMed Central

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

    2012-01-01

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

  2. 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.

  3. The analysis of the electrical properties of BLT ceramics fabricated from sol-gel derived powders

    NASA Astrophysics Data System (ADS)

    Wodecka-Dus, Beata; Adamczyk, Malgorzata; Dzik, Jolanta; Osinska, Katarzyna

    2016-02-01

    The (Ba x La1- x )Ti1- x/4O3 (BLT, 0.001 ≤ x ≤ 0.005) amorphous gel was prepared by sol-gel process. The electrical properties of obtained materials has been investigated by impedance spectroscopy. Detailed analysis of impedance spectra allowed to propose an adequate equivalent circuit, which described the electric properties of discussed materials very well. Basing on the obtained circuits and the fitting procedure the grain and grain boundary resistivity was determined as a function of temperature and La concentration. With increase of La admixture the contribution of grain and grains impedance to the bulk impedance changes. It was found that the small amount of La additive decreases the blocking factor of the grain boundary in the temperature range 600-850 K, whereas the amount of La on the level of 0.4-0.5 mol.% causes the sharp increase of the mentioned factor. The fact may be attributed to a decrease of grain activation energy and increase of the grain boundary one.

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

    PubMed

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

    2012-01-01

    In this paper, hydroxyapatite-carbon nanotube/titania (HA-CNT/TiO(2)) double layer coatings were successfully developed on titanium (Ti) substrates intended for biomedical applications. A TiO(2) coating was firstly developed by anodization to improve bonding between HA and Ti, and then the layer of HA and CNTs was coated on the surface by the sol-gel process to improve the biocompatibility and mechanical properties of Ti. The surfaces of double layer coatings were uniform and crack-free with a thickness of about 7 μm. The bonding strength of the HA-CNT/TiO(2) coating was higher than that of the pure HA and HA-CNT coatings. Additionally, in vitro cell experiments showed that CNTs promoted the adhesion of preosteoblasts on the HA-CNT/TiO(2) double layer coatings. These unique surfaces combined with the osteoconductive properties of HA exhibited the excellent mechanical properties of CNTs. Therefore, the developed HA-CNT/TiO(2) coatings on Ti substrates might be a promising material for bone replacement. PMID:22606041

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

    PubMed

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

    2016-10-01

    Sol-gel derived bioactive glass (BG) holds great potential in the application of skin repair. However, the specific regulation of BG on skin cells is still unclear and demands more investigation. Herein, we synthesized sol-gel derived BGs with different compositions (60S, 70S, 80S, and 90S) and found 90S BGs (90 mol % SiO2 , 6 mol % CaO, 4 mol % P2 O5 ) exhibited the best supportiveness for the proliferation of normal human foreskin fibroblasts. Thus, 90S BG particles were used as a model to systematically study the wound healing related cellular response of fibroblasts to BGs. Time-lapse imaging revealed a promoted fibroblast motility stimulated by 90S BG particles. Results on the expression of extracellular matrix (ECM) related genes illustrated that 90S BG particles modulated the synthesis capacity for critical ECM molecules including type I collagen, type III collagen, fibronectin, and tenascin-C. Moreover, the myofibroblastic differentiation of fibroblasts was greatly inhibited by 90S BG particles. Further analysis on the intracellular signaling pathways demonstrated that 90S BG particles down-regulated the collagen synthesis and fibroblast-to-myofibroblast differentiation via TGF-β1-Smad2 signaling, evidenced by the decreased expression levels of TGF-β receptor I and its downstream effector Smad2. Our study provided a further understanding of the specific regulation of 90S BG particles on fibroblasts, which may guide the future design of BG based wound dressing and benefit the clinical application of BG particles in skin repair. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 2420-2429, 2016. PMID:27177533

  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. Structural characterization of sol-gel derived oxide nanostuctures using synchrotron x-ray techniques

    NASA Astrophysics Data System (ADS)

    Sun, Tao

    Ceramic oxides possess extraordinarily rich functionalities. With the advent of nanofabrication techniques, it is now possible to grow nanostructured oxides with precise control of composition, morphology, and microstructure, which has re-vitalized the research in the field of traditional ceramics. The unexpected behavior and enhanced properties of oxide nanostructures have been extensively reported. However, knowledge about the underlying mechanisms as well as structural implications is still quite limited. Therefore, it is imperative to develop and employ sophisticated characterization tools for unraveling the structure-property relationships for oxide nanostructures. The present thesis work aims at addressing the critical issues associated with fabrication, and more importantly, structural characterization of functional oxide nanostructures. The dissertation starts with introducing the strategy for synthesizing phase-pure and highly controlled oxide nanostructures using sol-gel deposition and an innovative approach called "soft" electron beam lithography. Some specific oxides are chosen for the present study, such as BiFeO3, CoFe2O4, and SnO2, because of their scientific and technological significance. Subsequent to fabrication of tailored oxide nanostructures, advanced synchrotron x-ray scattering techniques have been applied for structural characterization. The nucleation and growth behavior of BiFeO3 thin film was investigated using in situ grazing-incidence small-angle x-ray scattering (GISAXS) technique. The results reveal that the kinetics for early-stage nuclei growth are governed by the oriented-attachment model. Moreover, the porous structures of undoped and Pd-doped semiconducting SnOx thin films were quantitatively characterized using GISAXS. By correlating the structural parameters with H2 sensitivity of SnOx films, it is found out that the microstructure of doped film is favorable for gas sensing, but it is not the major reason for the overall

  8. Calcium phosphate sol-gel-derived coatings on titanium-aluminum-vanadium substrate for biomedical applications

    NASA Astrophysics Data System (ADS)

    Gan, Lu

    Osseointegration of implants to host bone is a necessary requirement for dental and orthopaedic implants. The rate and quality of osseointegration were enhanced through the use of calcium phosphate (Ca-P) films on metallic substrates. The present study investigates the characteristics of Ca-P films applied using sol-gel dip coating methods to sintered porous-surfaced implants. Ca-P films have been formed using Inorganic Route and Organic Route processes. It has been shown that both approaches resulted in the formation of carbonated hydroxyapatite but with different Ca/P ratios as well as different surface textures and film structures, the Inorganic Route-formed film being more porous at its outermost surface, and having a more irregular topography. An interfacial reaction product (calcium titanium oxide) was detected for the Inorganic Route-formed coatings while this interfacial phase was not detectable in the Organic Route-formed coatings. The interface tensile and shear adhesion strength properties of Ca-P films have been evaluated using an improved direct pull-off testing (ASTM C633) and a substrate straining method, respectively. For both Ca-P films, the adhesive tensile strength was higher than the failure stress of ˜38 MPa occurring between the Ca-P films and the glue or in the glue. A shear lag approach revealed a shear strength of 347 +/- 64MPa and 280 +/- 28MPa for the Inorganic Route and the Organic Route Ca-P films, respectively. In vivo animal model studies have been performed to compare the effect on early bone formation of sintered porous-surfaced implants that had been modified through the addition of Ca-P film. In Group I study (i.e. Inorganic Route-formed Ca-P-coated implants vs. non-coated implants), it has been found that the Inorganic Route-formed Ca-P film significantly enhances the early rate of bone ingrowth for sintered porous-surfaced implants. However, in Group II study (i.e. Organic Route-formed Ca-P-coated implants vs. non

  9. Structural and pyroelectric properties of sol-gel derived multiferroic BFO thin films

    SciTech Connect

    Jo, Seo-Hyeon; Lee, Sung-Gap; Lee, Seung-Hwan

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer We fabricated multiferroic BFO/PZT multilayer films by spin-coating method. Black-Right-Pointing-Pointer The trap centers of carriers were formed at the interfaces between BFO and PZT films. Black-Right-Pointing-Pointer The ferroelectric properties were superior to those of single composition BFO film. -- Abstract: Multiferroic BFO/PZT multilayer films were fabricated by spin-coating method on the (1 1 1)Pt/Ti/SiO{sub 2}/Si substrate alternately using PZT(30/70), PZT(70/30) and BFO alkoxide solutions. The structural and ferroelectric properties were investigated for uncooled infrared detector applications. The coating and heating procedure was repeated six times to form BFO/PZT multilayer films. All films showed the typical XRD patterns of the perovskite polycrystalline structure without presence of the second phase such as Bi{sub 2}Fe{sub 4}O{sub 3}. The thickness of BFO/PZT multilayer film was about 200-220 nm. The ferroelectric properties such as dielectric constant, remnant polarization and pyroelectric coefficient were superior to those of single composition BFO film, and those values for BFO/PZT(70/30) multilayer film were 288, 15.7 {mu}C/cm{sup 2} and 9.1 Multiplication-Sign 10{sup -9} C/cm{sup 2} K at room temperature, respectively. Leakage current density of the BFO/PZT(30/70) multilayer film was 3.3 Multiplication-Sign 10{sup -9} A/cm{sup 2} at 150 kV/cm. The figures of merit, F{sub V} for the voltage responsivity and F{sub D} for the specific detectivity, of the BFO/PZT(70/30) multilayer film were 6.17 Multiplication-Sign 10{sup -11} Ccm/J and 6.45 Multiplication-Sign 10{sup -9} Ccm/J, respectively.

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

    PubMed

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

    2006-09-12

    Heterogeneous nucleation and growth of calcium phosphate (CaP) on sol-gel derived TiO(2) coatings was investigated in terms of surface topography and surface energy. The topography of the coatings was derived from AFM measurements, while the surface energy was determined with contact angle measurements. The degree of precipitation was examined with scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The precipitation of CaP was found to be dependent on both topography and surface energy. A high roughness value when combining the RMS roughness parameter S(q) with the number of local maxima per unit area parameter S(ds) enhances CaP formation. The hydrophilicity of the coating was also found to be of importance for CaP formation. We suggest that the water contact angle, which is a direct measure of the hydrophilicity of the surface, may be used to evaluate the surface energy dependent precipitation kinetics rather than using the often applied Lewis base parameter. PMID:16952264

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

    PubMed Central

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

    2015-01-01

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

  13. Sol-Gels for Optical Sensors

    NASA Astrophysics Data System (ADS)

    Podbielska, Halina; Ulatowska-Jarża, Agnieszka; Müller, Gerhard; Eichler, Hans J.

    Sol-gel process allows for formation of glassy and ceramics materials in temperatures much lower than offered by conventional melting techniques. The first paper on sol-gels was published over 150 years ago by Ebelmen, however, the rapid development of this technology and applications occurred in the last few years. There is a broad range of possible applications of solgel derived materials, what marked this technology as one of the most promising fields of contemporary material sciences

  14. Sol-gel derived copper-doped silica glass as a sensitive material for X-ray beam dosimetry

    NASA Astrophysics Data System (ADS)

    Capoen, Bruno; Hamzaoui, Hicham El; Bouazaoui, Mohamed; Ouerdane, Youcef; Boukenter, Aziz; Girard, Sylvain; Marcandella, Claude; Duhamel, Olivier

    2016-01-01

    The light emission from a sol-gel-derived Cu-doped silica glass was studied under 10 keV X-ray irradiation using a fibered setup. Both radioluminescence (RL) and optically stimulated luminescence (OSL) were analyzed at different high dose rates up to 50 Gy/s and for different exposure times, yielding accumulated doses up to 50 kGy (in SiO2). Even if a darkening effect appears at this dose level, the material remains X-sensitive after exposure to several kGy. At low dose rate, the scintillation mechanisms are similar to photoluminescence, involving the Cu+ ions electronic levels, contrary to the nonlinear domain (for dose rates higher than 30 Gy/s). This RL, as well as the OSL, could be exploited in their linear domain to measure doses as high as 3 kGy. A thorough study of the OSL signal has shown that it must be employed with caution in order to take the fading phenomenon and the response dependency on stimulation source intensity into consideration.

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

    NASA Astrophysics Data System (ADS)

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

    2011-03-01

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

  16. A case study of optical properties and structure of sol gel derived nanocrystalline electrochromic WO3 films

    NASA Astrophysics Data System (ADS)

    Deepa, M.; Srivastava, A. K.; Kar, M.; Agnihotry, S. A.

    2006-05-01

    Sol-gel derived, as-deposited amorphous tungsten oxide (WO3) films become nanocrystalline with a pseudocubic triclinic structure upon annealing at 600 °C. The annealed films are constituted of nanorods along with interconnected nanoparticles and pores. While the high transmission modulation and colouration efficiency in the visible region and the fast bleaching kinetics as shown by the nanostructured film were typical of amorphous WO3, the absorption coefficient spread in the 300-2000 nm wavelength range, the reflectance modulation and the colouration efficiency peak in the NIR region were reminiscent of crystalline WO3. The larger magnitude of the indirect band gap shift to blue than the direct gap shift for the same level of lithium intercalation (18 mC cm-2) and the irreversibility of the direct gap shift upon bleaching are characteristic of the nanocrystalline structure of the film. The moderate decline in the anodic peak current maximum, the diffusion coefficient for lithium and the optical modulation at 632.8 nm upon repetitive switching between the coloured and bleached states ratified that nanostructured films sustain 1000 cycles without much deterioration.

  17. Sol gel processes. (Latest citations from the NTIS bibliographic database). Published Search

    SciTech Connect

    Not Available

    1993-09-01

    The bibliography contains citations concerning the development and utilization of sol-gel processes and techniques. Topics include antireflective coatings, studies of sol-gel transitions, sol-gel synthesis and polymerization, sol-gel derived thin films and glasses, and sol-gel production of microspheres. Applications in nuclear waste management, nuclear fuel manufacturing, glass optical waveguide development, and solar energy collection are presented. (Contains 250 citations and includes a subject term index and title list.)

  18. Structural, morphology and electrical studies on ferroelectric bismuth titanate thin films prepared by sol?gel technique

    NASA Astrophysics Data System (ADS)

    Giridharan, N. V.; Madeswaran, S.; Jayavel, R.

    2002-04-01

    Crystal structure, surface morphology, compositional homogeneity and electrical properties of layered perovskite bismuth titanate (BTO) thin films have been investigated. BTO thin films were deposited on silicon and platinum-coated silicon substrates by spin coating. X-ray diffraction analysis confirms that the crystallinity of the films increases with increasing annealing temperature and the optimum temperature is found to be 600°C. Morphology studies by AFM showed that the surface of the films were smooth, dense and crack free. Composition analysis on the surface and in-depth confirms the stoichiometry of the films. C- V measurements show a counter-clockwise dielectric hysteresis, indicating that the ferroelectric property sufficiently controls the silicon potential with a memory width of 2 V. The leakage current density of the films is measured to be 2×10 -7 A/cm 2 from I- V characteristics at an applied voltage of 1 V.

  19. Application feasibility of Pb(Zr,Ti)O{sub 3} ceramics fabricated from sol-gel derived powders using titanium and zirconium alkoxides

    SciTech Connect

    Huang, C.L.; Chen, B.H.; Wu, L

    2004-04-02

    It is believed that what may be termed the 'Nanoscaled Century' will lead to a new industrial revolution, particularly in terms of sol-gel methods of assembly for nanostructure devices. A propyl alcohol (1-Pro) based sol-gel chemical has been developed to replace 2-methoxyethanol (MOE), 1,1,1-tris(hydroxymethyl)ethane (THOME) for the fabrication of PbZr{sub 0.53}Ti{sub 0.47}O{sub 3} (PZT) piezoelectric ceramics. This chemical is prepared from sol-gel derived powders that are near to the morphotropic phase boundary (MPB). The pyrochlore phase was still apparent when calcining at 900 deg. C with a shorter calcining time, such as 30 min. However, it disappeared for longer calcining times, for example 3 h or more. From the results of the analysis, PZT ceramics calcinations at 900 deg. C for 4 h, and sintering at 1100 deg. C for 2 h could reach a pyrochlore-free crystal phase with relative density of approximately 7.9 g/cm{sup 3}--close to 98% of the theoretical value. The P-E hysteresis loop, measured by the Sawyer-Tower circuit, revealed that the remanent polarization (P{sub r}) and coercive field (E{sub c}) were 8.54 {mu}C/cm{sup 2} and 15.6 kV/cm, respectively. The vibration modes of the PZT ceramics were between 150 and 1.5 MHz. Morevoer, under such processing conditions the PZT piezoceramics had uniform grain size distribution less than 1 {mu}m and zero temperature coefficient of resonant frequency (TCF). In summary, the PZT ceramics derived from the sol-gel method were confirmed to possess excellent piezoelectric properties. Furthermore, the processing temperatures were scaled down by 100-200 deg. C, compared to conventional oxide reaction. Finally, from an energy-saving viewpoint, this experiment can potentially make a very positive contribution.

  20. Low cost sol-gel derived SiC-SiO2 nanocomposite as anti reflection layer for enhanced performance of crystalline silicon solar cells

    NASA Astrophysics Data System (ADS)

    Jannat, Azmira; Lee, Woojin; Akhtar, M. Shaheer; Li, Zhen Yu; Yang, O.-Bong

    2016-04-01

    This paper describes the preparation, characterizations and the antireflection (AR) coating application in crystalline silicon solar cells of sol-gel derived SiC-SiO2 nanocomposite. The prepared SiC-SiO2 nanocomposite was effectively applied as AR layer on p-type Si-wafer via two step processes, where the sol-gel of precursor solution was first coated on p-type Si-wafer using spin coating at 2000 rpm and then subjected to annealing at 450 °C for 1 h. The crystalline, and structural observations revealed the existence of SiC and SiO2 phases, which noticeably confirmed the formation of SiC-SiO2 nanocomposite. The SiC-SiO2 layer on Si solar cells was found to be an excellent AR coating, exhibiting the low reflectance of 7.08% at wavelengths ranging from 400 to 1000 nm. The fabricated crystalline Si solar cell with SiC-SiO2 nanocomposite AR coating showed comparable power conversion efficiency of 16.99% to the conventional SixNx AR coated Si solar cell. New and effective sol-gel derived SiC-SiO2 AR layer would offer a promising technique to produce high performance Si solar cells with low-cost.

  1. 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.

  2. 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. PMID:27137982

  3. Analysis of lipid phase behavior and protein conformational changes in nanolipoprotein particles upon entrapment in sol-gel-derived silica.

    PubMed

    Zeno, Wade F; Hilt, Silvia; Aravagiri, Kannan K; Risbud, Subhash H; Voss, John C; Parikh, Atul N; Longo, Marjorie L

    2014-08-19

    The entrapment of nanolipoprotein particles (NLPs) and liposomes in transparent, nanoporous silica gel derived from the precursor tetramethylorthosilicate was investigated. NLPs are discoidal patches of lipid bilayer that are belted by amphiphilic scaffold proteins and have an average thickness of 5 nm. The NLPs in this work had a diameter of roughly 15 nm and utilized membrane scaffold protein (MSP), a genetically altered variant of apolipoprotein A-I. Liposomes have previously been examined inside of silica sol-gels and have been shown to exhibit instability. This is attributed to their size (∼150 nm) and altered structure and constrained lipid dynamics upon entrapment within the nanometer-scale pores (5-50 nm) of the silica gel. By contrast, the dimensional match of NLPs with the intrinsic pore sizes of silica gel opens the possibility for their entrapment without disruption. Here we demonstrate that NLPs are more compatible with the nanometer-scale size of the porous environment by analysis of lipid phase behavior via fluorescence anisotropy and analysis of scaffold protein secondary structure via circular dichroism spectroscopy. Our results showed that the lipid phase behavior of NLPs entrapped inside of silica gel display closer resemblance to its solution behavior, more so than liposomes, and that the MSP in the NLPs maintain the high degree of α-helix secondary structure associated with functional protein-lipid interactions after entrapment. We also examined the effects of residual methanol on lipid phase behavior and the size of NLPs and found that it exerts different influences in solution and in silica gel; unlike in free solution, silica entrapment may be inhibiting NLP size increase and/or aggregation. These findings set precedence for a bioinorganic hybrid nanomaterial that could incorporate functional integral membrane proteins. PMID:25062385

  4. Sol gels. (Latest citations from Materials Business file). Published Search

    SciTech Connect

    1996-01-01

    The bibliography contains citations concerning sol gel derived materials. The citations examine research conducted by universities, corporations and government agencies for the development of novel sol gel processes, and commercial applications of these techniques. Uses of sol gels in the production of glass, ceramics, composites, protective coatings, and hybrid organic/inorganic materials are described. Other topics include new products, expanding markets for sol gel derived materials, and profit potential. (Contains 50-250 citations and includes a subject term index and title list.) (Copyright NERAC, Inc. 1995)

  5. Structural and electrical properties of ferroelectric Na0.5 (Bi1-xPrx )0.5TiO3 (x=0.00 and 0.10) ceramics synthesized by Sol-Gel method

    NASA Astrophysics Data System (ADS)

    Shalini, K.; Muneeswaran, M.; Giridharan, N. V.

    2016-05-01

    Ferroelectric Na0.5(Bi1-xPrx)0.5TiO3 (x=0.00, 0.10) ceramics have been synthesized through sol-gel method. The phase formation has been confirmed by X-ray diffraction analysis of ceramics annealed at 800°C. The relaxation mechanism is observed from variation of dielectric constant with respect to temperature and frequency. Substitution of Pr reduces vacancies and defects identified from leakage current measurements. Further, the polarization Vs electricfield (P-E) measurements have been performed at room temperature.

  6. Optical spectroscopy of trivalent chromium in sol-gel lithium niobate

    SciTech Connect

    Krebs, J.K.; Happek, U.

    2005-12-19

    We report on the characterization of sol-gel derived lithium niobate via trivalent chromium probe ions, a study that is motivated by recent reports on the synthesis of high quality sol-gel lithium niobate (LiNbO{sub 3}). In order to assess the quality of sol-gel derived LiNbO{sub 3}, we incorporate Cr{sup 3+} during the hydrolysis stage of the sol-gel process. A comparison of the Cr{sup 3+} emission and photoexcitation data on both sol-gel and melt-grown LiNbO{sub 3} shows that the sol-gel derived material is highly stoichiometric.

  7. Toward sol-gel-based sensors

    SciTech Connect

    Jordan, J.D.; Ingersoll, C.M.; Dunbar, R.A.

    1995-12-31

    Advances in biotechnology have produced a variety of antibodies and other biomolecules that possess selective recognition capabilities. Current techniques for the immobilization of these biomolecules typically involve multistep derivatization of a primary substrate, which is labor intensive and often requires large volumes of costly reagents. Further, these immobilization chemistries often adversely affect the characteristic properties of the protein (e.g., the binding affinity). As a result, the need for fast, accurate, inexpensive, and simple to operate diagnostic assays escalates. Because of their room temperature processing, transparency, inertness, and tunable pore structure, sol-gel-derived composites represent promising chemical and biosensing platforms. To date, many researchers have entrapped proteins and enzymes in sol-gel monoliths, and found that they retain some of their native properties. Our group first reported on the affinity of a sol-gel entrapped antibody. However, although these biogel monoliths were promising, analyte diffusion through the monolith matrix is slow, resulting in long response times. Thus, it is clear that the next level of sol-gel-derived biosensor must depend on thin film technology. In the current work, the affinity of fluorescein entrapped within a sol-gel derived thin film for the anti fluorescent hapten, 5- (and 6-)-carboxy 4{prime}, 5{prime}-dimethylfluorescein, is investigated. A novel film preparation technique will be introduced, and the response and response times of these films as a function of processing and storage conditions will be discussed.

  8. 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.

  9. Improved performance by plasma-treated silicate phosphor particles with a sol-gel derived protective coating of indium oxide

    NASA Astrophysics Data System (ADS)

    Kim, Hyeon; Yun, Changhun; Jeon, Sie Wook; Lee, June Key; Kim, Jae Pil

    2016-03-01

    The optical properties and reliability of silicate phosphor was fairly improved by an amorphous In2O3 protective coating on plasma-treated phosphor particles. The In2O3 layers were coated using a conventional sol-gel method with alkoxide precursor in N2 gas. The surface morphology of silicate particles was smoother after Ar-plasma surface modification. When plasma surface treatment of the phosphor was applied before sol-gel coating, the In2O3 coating was almost 3-times thicker, and the surface of the phosphor particles was smoother, than could be obtained when sol-gel coating was not preceded by plasma treatment. This was because the treatment caused the surface to become hydrophilic. The light absorption rate and quantum efficiency were increased from 75.3% and 93.8%, to 79.2% and 95.7%, after plasma-treated In2O3 coating. Bare silicate phosphor used in 450-nm vertical-type LEDs, displayed 10% decreased optical output, whereas In2O3-coated phosphor showed just 3% decreased optical output after 1000 h of input current at 350 mA; under conditions of high humidity and high temperature.

  10. 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.

  11. 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.

  12. Sol-Gel-derived TiO2-SiO2 implant coatings for direct tissue attachment. Part II: Evaluation of cell response.

    PubMed

    Areva, Sami; Aäritalo, Virpi; Tuusa, Sari; Jokinen, Mika; Lindén, Mika; Peltola, Timo

    2007-08-01

    Silica-releasing sol-gel derived TiO2-SiO2 coatings with tailored nanostructure were evaluated in fibroblast and osteoblast cell cultures. The adhesion of both fibroblasts and osteoblasts proceeded within two hours. The highest fibroblast proliferation activities were observed on the TiO2-SiO2 (70:30) and (30:70) coatings. However, the cell layer on TiO2-SiO2 (30:70) coating was disordered. Prolonged osteoblast activity was observed on the coatings as a function of increased amount of released silica. At day 21 the surfaces were fully covered by the calcified nodules and extracellular matrix except for the coatings TiO2-SiO2 (10:90) i.e. having the highest SiO2 amount. The results suggested that TiO2-SiO2 (70:30) was the best for fibroblasts and TiO2-SiO2 (30:70) for osteoblasts. The applicability of the sol-gel derived TiO2 and TiO2-SiO2 coatings as an alternative for the calcium phosphate based implant coatings are discussed. PMID:17483880

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

    SciTech Connect

    Not Available

    1989-09-01

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

  14. Sol-gel processes. January 1970-September 1988 (Citations from the NTIS database). Report for January 1970-September 1988

    SciTech Connect

    Not Available

    1988-09-01

    This bibliography contains citations concerning the development and utilization of sol-gel processes and techniques. Topics include antireflective coatings, studies of sol-gel transitions, sol-gel synthesis and polymerization, sol-gel derived thin films and glasses, and sol-gel production of microspheres. Applications in nuclear waste management, nuclear fuel manufacturing, glass optical waveguide development, and solar energy collection are presented. (This updated bibliography contains 140 citations, 28 of which are new entries to the previous edition.)

  15. 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.

  16. 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

  17. 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

  18. 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.

  19. Resistive Switching Properties of Sol-Gel-Derived V-Doped SrTiO3 Thin Films

    NASA Astrophysics Data System (ADS)

    Tang, Zhen Hua; Xiong, Ying; Xu, Ding Lin; Tang, Ming Hua; Wang, Zi Ping; Xiao, Yong Guang; Zeng, Bo Wen; Gu, Xiao Chen; Li, Jian Cheng; Wang, Long Hai

    2013-08-01

    V-doped and undoped SrTiO3 (V:STO and STO) thin films on Pt/Ti/SiO2/Si substrates were synthesized using a sol-gel method to form metal-insulator-metal (MIM) structures. Coexistence of the bipolar and unipolar resistive switching (BRS and URS) modes in Pt/STO/Pt and Pt/V:STO/Pt structures was observed as a irreversible transition from BRS to URS on adjustment of the compliance current ( I comp). Both states were stable and reproducible over 60 cycles, and the maximum operating voltage of the Pt/STO/Pt was reduced from 10 V to 2 V by doping with V. Linear fitting of current-voltage curves suggests that space-charge-limited leakage was the limiting leakage mechanism for these two devices. Based on these results, a switching mechanism based on filament theory is proposed to explain both resistive switching modes.

  20. 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.

  1. 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

  2. Alkoxy sol-gel derived Y{sub 3{minus}x}Al{sub 5}O{sub 12}:Tb{sub x} thin films as efficient cathodoluminescent phosphors

    SciTech Connect

    Choe, Jae Young; Ravichandran, D.; Blomquist, S. M.; Morton, D. C.; Kirchner, K. W.; Ervin, M. H.; Lee, Unchul

    2001-06-11

    Thin-film Y{sub 3{minus}x}Al{sub 5}O{sub 12}:Tb{sub x}{sup 3+} (YAG:Tb) phosphor derived from a sol-gel chemistry is analyzed by x-ray diffraction, scanning electron microscopy, photoluminescence (PL) and cathodoluminescence (CL). The metal alkoxides organic precursors were chosen as the starting materials to form the sol-gel. This liquid sol-gel was spin coated on sapphire and silicon substrates to form the uniform thin films, then crystallized by annealing. The PL intensity of the crystallized film at 545 nm green emission was 15 times higher than that of the as-coated noncrystalline film. CL measurements show that luminance and efficiency are comparable to the films deposited by other techniques. {copyright} 2001 American Institute of Physics.

  3. Third-order optical nonlinearities of sol-gel silica coating films containing metal porphyrin derivatives measured by resonant femtosecond degenerate four-wave mixing technique

    NASA Astrophysics Data System (ADS)

    Kasatani, Kazuo; Okamoto, Hiroaki; Takenaka, Shunsuke

    2003-11-01

    Third-order optical nonlinearities of sol-gel silica coating films containing metal porphyrin derivatives were measured under resonant conditions by the femtosecond degenerate four-wave mixing (DFWM) technique. Temporal profiles of the DFWM signal were measured with a time resolution of 0.3 ps, and were found to consist of two components, the coherent instantaneous nonlinear response and the delayed response with a decay time constant of several to several hundred ps. The latter can be attributed to population grating of an excited state, and contribution of slow component was very little for a zinc porphyrin derivative. The values of electronic component of the optical nonlinear susceptibility, χ(3) xxxx, for these films were ca. 2 x 10-10 esu.

  4. 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.

  5. 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.

  6. Structural investigations of sol-gel-derived LiYF 4 and LiGdF 4 powders

    NASA Astrophysics Data System (ADS)

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

    2007-11-01

    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 19F nuclear magnetic resonance (NMR) studies showed that samples heat treated at 300 °C are already crystallized but for a full crystallization in LiGdF 4 and LiYF 4 a thermal treatment at 550 °C is needed. Temperature dependence of powder morphology was analyzed by scanning electron microscopy (SEM).

  7. Photophysical properties of sol-gel derived luminescent silicone hybrids synthesized via facile amino-ene reaction.

    PubMed

    Yue, Yuanzhi; Liang, Yan; Wang, Hua; Feng, Linglong; Feng, Shengyu; Lu, Haifeng

    2013-01-01

    Novel luminescent silicone hybrids (LSHs) containing lanthanide ions were prepared via different sol-gel processes. The precursor, dimethyl ester-functionalized silane, was synthesized via a facile amino-ene reaction. The coordinated assembly of the ester ligands and lanthanide ions (Eu(3+), Tb(3+) and Dy(3+)) occurred. The ester ligands were immobilized onto the Si-O network backbone during the preparation of the silicone hybrid materials. The particle size can be controlled to ca 50 nm by adjusting the solvent ratio. The obtained materials were characterized by Fourier transform infrared, (1)H nuclear magnetic resonance spectroscopy (NMR), (13)C NMR, (28)Si NMR, X-ray diffraction, X-ray photoelectron spectroscopy, thermogravimetric analysis, high-resolution scanning electronic microscopy and luminescent (excitation and emission) spectroscopy. The coordination state and photophysical performance of the compounds were studied in detail. The terbium- and europium-containing materials show sharp green and red emissions, respectively, which indicate that efficient intramolecular energy transfer took place in these LSHs. PMID:22774939

  8. 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.

  9. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2011-01-01

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

  11. Influence of annealing temperature on microstructure and optical properties of sol-gel derived tungsten oxide films

    NASA Astrophysics Data System (ADS)

    Sun, Xilian; Cao, Hongtao; Liu, Zhimin; Li, Jianzhong

    2009-07-01

    Tungsten oxide (WO 3) thin films have been extensively studied for their interesting physical properties and a variety of potential applications in electrochromic devices. In order to explore the possibility of using these in electrochromic devices, a preliminary and thorough study of the optical properties of the host materials is an important step. Based on this, the influence of annealing temperature on the structural, surface morphological, optical and electrochromic properties has been investigated in the present work. The host material, WO 3 films, has been prepared from an ethanolic acetylated peroxotungstic acid sol containing 5 wt.% oxalic acid dehydrate (OAD) by sol-gel technique. The monoclinic structure and textured nature change of the films with the temperature increasing have been investigated by X-ray diffraction analysis. The surface morphology evolution of the films has been characterized by SEM. The shift in absorption edge towards the higher wavelength region observed from optical studies may be due to the electron scattering effects and the optical band filling effect that reveals the crystallization of the film. The amorphous film shows better optical modulation (Δ T = 76.9% at λ = 610 nm), fast color-bleach kinetics ( tc ˜ 4 s and tb ˜ 9 s) and good reversibility ( Qb/ Qc = 90%), thereby rendering it suitable for smart window applications.

  12. In situ SAXS observation on metal-salt-derived alumina sol-gel system accompanied by phase separation.

    PubMed

    Tokudome, Yasuaki; Nakanishi, Kazuki; Kanamori, Kazuyoshi; Hanada, Teiichi

    2010-12-15

    The structure formation process of hierarchically porous alumina gels has been investigated by in situ small angle X-ray scattering (SAXS). The measurement was performed on the sol-gel solution containing aluminum chloride hexahydrate (AlCl(3)·6H(2)O), poly(ethylene oxide) (PEO), and propylene oxide (PO). The temporal divergence of scattering intensity in the low q regime was observed in the early stage of reaction, indicating that the occurrence of spinodal-decomposition-type phase separation. Detailed analysis of the SAXS profiles revealed that phase separation occurs between weakly branched polymerizing aluminum hydroxide (AH) and PEO. Further progress of the condensation reaction forms phase-separated two phases, that is, AH-rich phase and PEO-rich phase with the micrometer-range heterogeneity. The growth and aggregation of primary particles occurs in the phase-separated AH-rich domain, and therefore, the addition of PEO influences on the structure in nanometer regime as well as micrometer regime. The moderate stability of oligomeric species allows homogeneous condensation reaction parallel to phase separation and successful formation of hierarchically porous alumina gel. PMID:20822775

  13. Preparation and characterization of bioactive sol-gel-derived Na2Ca2Si3(O)9.

    PubMed

    Du, Ruilin; Chang, Jiang

    2004-12-01

    In this study, pure Na2Ca2Si3(O)9 was synthesized by a sol-gel method, and Na2Ca2Si3(O)9 cuboids and disks were prepared by uniaxial pressing and calcining at 700 degrees C. The porosity and mechanical strength of the Na2Ca2Si3(O)9 cuboids were measured, and the results showed that the Na2Ca2Si3(O)9 cuboids were porous with an average porosity of 44%, and the 3-point bending strength of the cuboids was 6.08 MPa. The in vitro bioactivity of Na2Ca2Si3(O)9 was carried out by soaking Na2Ca2Si3(O)9 disks in simulated body fluid (SBF). The results showed that hydroxyapatite (HA) formed on the surface of Na2Ca2Si3(O)9 samples after soaking for 1 day, which indicated good bioactivity of Na2Ca2Si3(O)9. PMID:15747180

  14. 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.

  15. 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

  16. Molecular host sol-gel films for chemical sensing applications

    SciTech Connect

    Shi, J.; Johnson, S.; Yang, X.; Swanson, B.

    1997-12-31

    Sol-gel cyclodextrin coatings on surface acoustic wave (SAW) device as VOC sensors have been studied. The sol-gel approach to thin films efficiently yields uniform coatings on SAW devices. The films were characterized by ATR-FT-IR, ellipsometry and SEM. The incorporation of molecular host reagents (cyclodextins and their derivatives) into thin films greatly enhance the sensitivity and selectivity of SAW sensors. It is believed that molecular recognition (selective sorption) occurs at the gas-solid interface. From the SAW data, it is possible to calculate the binding constants of sol-gel films towards a variety VOCs. The identification of VOCs based on SAW sensor arrays is discussed.

  17. 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.

  18. 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.

  19. 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

  20. 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

  1. 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.

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

    SciTech Connect

    Not Available

    1988-08-01

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

  3. Novel sol-gel bioactive fibers.

    PubMed

    Oréfice, R L; Hench, L L; Clark, A E; Brennan, A B

    2001-06-15

    Bioactive fibers were produced using a sol-gel method. The rheological properties of two different sol compositions prepared from a mixture of TEOS, phosphorous alkoxide and calcium nitrate, or calcium chloride in a water-ethanol solution, are reported. The sols were extruded through a spinneret to produce continuous 10 microm-diameter fibers. Discontinuous fibers and fibrous mats were prepared by air-spraying the multicomponent sols. The sol-gel fibers were converted to the bioactive fibers by three different thermal treatments at either 600 degrees, 700 degrees, or 900 degrees C for 3 h. SEM, BET, EDX, and FTIR were used to characterize the morphology and structure of the fibers. The BET measured surface area of the fibers sintered at 900 degrees C was 0 m(2)/gm compared to a value of 200 m(2)/gm for a typical sol-gel-derived particle of similar composition. Both the continuous and discontinuous fibers exhibited in vitro bioactivity in a simulated body fluid. PMID:11288073

  4. 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

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

    PubMed

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

    2012-12-01

    A novel material, sol-gel derived La(OH)(3) nanorods (La(OH)(3)NRs) with excellent film forming ability was prepared, and it was first designed to incorporate with carbon nanotubes (CNTs) to modify glassy carbon electrode (GCE) to simultaneously voltammetric determine ascorbic acid (AA), dopamine (DA), uric acid (UA), and nitrite (NO(2)(-)). Cyclic voltammetry (CV), transmission electron microscopy (TEM), and X-ray diffraction (XRD) were employed to characterize the sensor. Under optimal conditions, the linear response range for AA, DA, UA, and NO(2)(-) were 0.5 μmol L(-1) to 1.46 mmol L(-1), 50 nmol L(-1) to 35.36 μmol L(-1), 50 nmol L(-1) to 0.79 mmol L(-1), and 0.55 μmol L(-1) to 0.72 mmol L(-1), respectively and the detection limits were 1.67 μmol L(-1), 1.67 nmol L(-1), 1.67 nmol L(-1), and 0.18 μmol L(-1). The sensor demonstrated well stability, high selectivity and sensitivity. More importance, this material can be extended to construct other electrochemical sensors by the immobilization of enzymes and antibodies. PMID:22766296

  6. Grafting of organosilane derived from 3-glycidoxypropyltrimethoxysilane and thiourea onto magnesium phyllosilicate by sol-gel process and investigation of metal adsorption properties

    NASA Astrophysics Data System (ADS)

    Dey, R. K.; Oliveira, Andrea S.; Patnaik, Tanushree; Singh, V. K.; Tiwary, D.; Airoldi, Claudio

    2009-08-01

    A layered inorganic-organic magnesium silicate (Mg-GTPS-TU) has been successfully synthesized by using sol-gel based precursor under mild temperature conditions and a new silylaing agent (GTPS-TU) derived from 3-glycidoxypropyltrimethoxysilane (GTPS) and thiourea (TU) as the silicon source. The hybrid material was characterized through elemental analysis, infrared spectroscopy, X-ray diffractometry, thermogravimetry, and carbon and silicon solid-state nuclear magnetic resonance spectroscopy. The result confirmed the attachment of organic functionality to the inorganic silicon network. The inter-lamellar distance for the hybrid material was found to be 18.8 Å. Metal adsorption characteristics follows Cr(III) >Mn(II)>Zn(II) with more affinity towards Cr(III) in dilute aqueous solution. Evaluation of thermodynamic parameters ΔH and ΔS for Cr(III) were found to be 25.44 J mol -1 and 79.9 J mol -1 K -1, respectively, indicating adsorption process to be endothermic in nature. The negative value of Δ G indicated the feasibility and spontaneity of ongoing adsorption process at relatively higher temperature. The presence of multiple coordination sites in the attached organic functionality expresses the potentiality of the hybrid material containing new silylating agent for heavy cation removal from eco-system.

  7. Study of the surface modification with oleic acid of nanosized HfO2 synthesized by the polymerized complex derived sol-gel method

    NASA Astrophysics Data System (ADS)

    Ramos-González, R.; García-Cerda, L. A.; Quevedo-López, M. A.

    2012-06-01

    The synthesis of nanosized hafnium oxide by the polymerized complex derived sol-gel method is reported. The structural and morphological characterization of the HfO2 was carried out by X-ray diffraction and scanning electron microscopy. The surface of hafnium oxide nanoparticles was modified by capping with oleic acid. The nanoparticle surface area was measured by the gas adsorption technique in order to determine the minimal amount of oleic acid needed to obtain a uniform coverage of the hafnium oxide. The existence of organic layer can be confirmed by Fourier transform spectroscopy, solid state nuclear magnetic resonance spectroscopy, thermal gravimetric analysis and transmission electron microscopy. The FTIR and solid state NMR results reveal that oleic acid is chemisorbed as a carboxylate onto the HfO2 nanoparticle surface and confirm the formation of a monomolecular layer of oleic acid surrounding the HfO2. The cover density of oleic acid on the HfO2 increases with the amount of oleic acid used to modify the nanoparticles and the surface properties of HfO2 nanoparticles modified with oleic acid change from hydrophilic to hydrophobic.

  8. Sol-gel-derived TiO(2)-SiO (2) implant coatings for direct tissue attachment. Part I: design, preparation and characterization.

    PubMed

    Aäritalo, Virpi; Areva, Sami; Jokinen, Mika; Lindén, Mika; Peltola, Timo

    2007-09-01

    A series of sol-gel derived TiO(2)-SiO(2) mixed oxide coatings were prepared by carefully controlling the process parameters to obtain silica-releasing coatings consisting of nanoparticles. These features are of paramount importance for enhanced cell adhesion and activation. To achieve both these goals the Ti-alkoxide and Si-alkoxide were first separately hydrolysed and the titania-silica mixed sol was further reacted before the dipping process to obtain the desired particle sizes resulting to the biologically favourable topographical features. Silica release was observed from all the prepared coatings and it was dependent on SiO(2) amount added to the sols, i.e., the higher the added amount the higher the release. In addition, calcium phosphate was able to nucleate on the coatings. From the obtained SiO(2) dissolution data, together with the detailed XPS peak analysis, the mixed oxide coatings are concluded to be chemically heterogeneous, consisting of TiO(2) and SiO(2) species most likely linked together by Ti-O-Si bonds. TiO(2) is chemically stable making long-term implant coating possible and the desired nanoscale dimensions were well preserved although the composition was changed as a consequence of SiO(2) dissolution under in vitro conditions. PMID:17508132

  9. 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.

  10. 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.

  11. Grafting of organosilane derived from 3-glycidoxypropyltrimethoxysilane and thiourea onto magnesium phyllosilicate by sol-gel process and investigation of metal adsorption properties

    SciTech Connect

    Dey, R.K.; Oliveira, Andrea S.; Patnaik, Tanushree; Singh, V.K.; Tiwary, D.; Airoldi, Claudio

    2009-08-15

    A layered inorganic-organic magnesium silicate (Mg-GTPS-TU) has been successfully synthesized by using sol-gel based precursor under mild temperature conditions and a new silylaing agent (GTPS-TU) derived from 3-glycidoxypropyltrimethoxysilane (GTPS) and thiourea (TU) as the silicon source. The hybrid material was characterized through elemental analysis, infrared spectroscopy, X-ray diffractometry, thermogravimetry, and carbon and silicon solid-state nuclear magnetic resonance spectroscopy. The result confirmed the attachment of organic functionality to the inorganic silicon network. The inter-lamellar distance for the hybrid material was found to be 18.8 A. Metal adsorption characteristics follows Cr(III) >Mn(II)>Zn(II) with more affinity towards Cr(III) in dilute aqueous solution. Evaluation of thermodynamic parameters DELTAH and DELTAS for Cr(III) were found to be 25.44 J mol{sup -1} and 79.9 J mol{sup -1} K{sup -1}, respectively, indicating adsorption process to be endothermic in nature. The negative value of DELTAG indicated the feasibility and spontaneity of ongoing adsorption process at relatively higher temperature. The presence of multiple coordination sites in the attached organic functionality expresses the potentiality of the hybrid material containing new silylating agent for heavy cation removal from eco-system. - Abstract: We report the synthesis and adsorption properties of a layered inorganic-organic magnesium silicate (Mg-GTPS-TU) derived from a new silylaing agent from 3-glycidoxypropyltrimethoxysilane (GTPS) and thiourea (TU) as the silicon source. Display Omitted

  12. Kinetics and structure of silicate sol-gels

    SciTech Connect

    Assink, R.A.; Brinker, C.J.; Kay, B.D.

    1990-01-01

    The structure of a silicate sol-gel derived material depends on the nature of its reaction kinetics. The chemical state of the silicate sol-gel is characterized by both the functional group concentrations and the distribution of the functional groups about a single silicon atom. {sup 29}Si nuclear magnetic resonance (NMR) spectroscopy provides a way to quantitatively determine these concentrations and distributions as a function of time during the reaction. During the early stages of the sol-gel reaction, the distribution of hydrolyzed species enables one to calculate the relative rates of hydrolysis. During the intermediate stages of the reaction, the rate of formation of various condensed species enables one to determine the reaction rate constants for both water-producing and alcohol-producing condensation. The chemical bonding of sol-gel derived solid materials can be determined by direct polarization NMR combined with magic angle spinning techniques. These capabilities provide a valuable tool for studying the relationships between the reaction conditions, the chemical kinetics and the resulting structure of the sol-gel derived material. 8 refs., 4 figs.

  13. Nanocrystal/sol-gel nanocomposites

    DOEpatents

    Klimov, Victor L.; Petruska, Melissa A.

    2010-05-25

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

  14. Ferroelectricity in corundum derivatives

    NASA Astrophysics Data System (ADS)

    Ye, Meng; Vanderbilt, David

    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. The known FE materials LiNbO3 can be regarded as derived from the A2O3 corundum structure with cation ordering. Here we consider more general binary (AB O3) and ternary (A2 BB' O6) corundum derivatives as an extended class of potential FE materials, motivated by the fact that some members of this class have recently been synthesized. There are four structure types for these corundum derivatives, and the number of cation combinations is enormous, but in many cases the energy barriers for polarization reversal may be too large to allow FE behavior. Here we present a first-principles study of the polar structure, coherent FE barrier, and domain-wall switching barrier for a representative set of polar corundum derivatives, allowing us to identify several potentially new FE materials. We also discuss the conditions under which ferroelectricity is compatible with magnetic ordering. Finally, we identify several empirical measures that can provide a rule of thumb for estimating the barrier energies. Our results should assist in the experimental search for new FE materials in the corundum derivative family. This work is supported by ONR Grant No. N-00014-12-1-1035.

  15. Comparison of formats for the development of fiber-optic biosensors utilizing sol-gel derived materials entrapping fluorescently-labelled protein.

    PubMed

    Flora, K; Brennan, J D

    1999-10-01

    The development of fiber-optic biosensors requires that a biorecognition element and a fluorescent reporter group be immobilized at or near the surface of an optical element such as a planar waveguide or optical fiber. In this study, we examined a model biorecognition element-reporter group couple consisting of human serum albumin that was site-selectively labelled at Cys 34 with iodoacetoxy-nitrobenzoxadiazole (HSA-NBD). The labelled protein was encapsulated into sol-gel derived materials that were prepared either as monoliths, as beads that were formed at the distal tip of a fused silica optical fiber, or as thin films that were dipcast along the length of a glass slide or optical fiber. For fiber-based studies, the entrapped protein was excited using a helium-cadmium laser that was launched into a single optical fiber, and emission was separated from the incident radiation using a perforated mirror beam-splitter, and detected using a monochromator-photomultiplier tube assembly. Changes in fluorescence intensity were generated by denaturant-induced conformational changes in the protein or by iodide quenching. The analytical parameters of merit for the different encapsulation formats, including minimum protein loading level, response time and limit-of-detection, were examined, as were factors such as protein accessibility, leaching and photobleaching. Overall, the results indicated that both beads and films were suitable for biosensor development. In both formats, a substantial fraction of the entrapped protein remained accessible, and the entrapped protein retained a large degree of conformational flexibility. Thin films showed the most rapid response times, and provided good detection limits for a model analyte. However, the entrapment of proteins into beads at the distal tip of fibers provided better signal-to-noise and signal-to-background ratios, and required less protein for preparation. Hence, beads appear to be the most viable method for interfacing of

  16. Sol-gel processes and materials. (Latest citations from the US Patent bibliographic file with exemplary claims). Published Search

    SciTech Connect

    1995-12-01

    The bibliography contains citations of selected patents concerning sol-gel processes and sol-gel derived materials and products. Selected patents include sol-gel compositions, ceramic and refractory materials, fabrication of silica glass, sol-gel thin films and coatings, transparent inorganic oxide glass, luminescent quartz glass, catalysts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, sol-gel production of microspheres, alumina composites, photographic materials, and dental materials. (Contains 50-250 citations and includes a subject term index and title list.) (Copyright NERAC, Inc. 1995)

  17. 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.

  18. 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.

  19. Structural, optical, vibrational, and magnetic properties of sol-gel derived Ni doped ZnO nanoparticles

    NASA Astrophysics Data System (ADS)

    Srinet, Gunjan; Kumar, Ravindra; Sajal, Vivek

    2013-07-01

    With a view to study structural, optical, vibrational, and magnetic properties of solgel derived Zn1-xNixO (x = 0.02, 0.04, and 0.06) nanoparticles, systematic investigations have been carried out. The Rietveld refinement of X-ray powder diffraction data revealed a single hexagonal phase with space group P63mc. The secondary phase of NiO appeared only in 6% Ni doped sample. Phonon modes in Ni doped ZnO nanoparticles were studied through Fourier transform infrared measurements. Furthermore, the enhancement in optical band gap with Ni doping from 3.29 to 3.32 eV has been observed through UV-visible spectroscopic analysis. Photoluminescence spectra of Zn1-xNixO show the UV-emission peak showing the blue shift with increase in doping concentration followed by broad visible (blue) emission corresponding to the defect emission whose intensity decreased with increasing Ni concentration. A clear room temperature ferromagnetism is observed in all samples but saturation magnetization decreased with increasing Ni content. The suitability of bound magnetic polarons (BMP) model is checked and numbers of BMPs are found to be of the order 1015 per cm3, which is very small for the percolation in ZnO. In the present case, oxygen rich stoichiometry with enhanced Zn-O bonding favours the indirect Ni-O-Ni ferromagnetic exchange coupling and reduction of oxygen vacancies leading to strong hybridization of Ni in ZnO host matrix responsible for room temperature ferromagnetism.

  20. 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.

  1. 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.

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

    NASA Technical Reports Server (NTRS)

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

    1995-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Zhang, Weiwei; Zhang, Junying; Li, Yuan; Chen, Ziyu; Wang, Tianmin

    2010-05-01

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

  4. Bipolar and unipolar resistive switching behaviors of sol-gel-derived SrTiO3 thin films with different compliance currents

    NASA Astrophysics Data System (ADS)

    Tang, M. H.; Wang, Z. P.; Li, J. C.; Zeng, Z. Q.; Xu, X. L.; Wang, G. Y.; Zhang, L. B.; Xiao, Y. G.; Yang, S. B.; Jiang, B.; He, J.

    2011-07-01

    The SrTiO3 (STO) thin films on a Pt/Ti/SiO2/Si substrate were synthesized using a sol-gel method to form a metal-insulator-metal structure. This device shows the bipolar resistance switching (BRS) behavior for a compliance current Icc of less than 0.1 mA but exhibits soft breakdown at a higher level of compliance current. A transition from the BRS behavior to the stable unipolar resistive switching behavior (URS) was also observed. We found that the BRS behavior may be controlled by the structure interface while the URS behavior is likely bulk controlled. Our study indicates that the external compliance current is a key factor in resistance switching phenomenon of STO thin films.

  5. 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

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

    SciTech Connect

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

    2014-09-15

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

  7. Structural studies and impedance spectroscopy of sol-gel derived Bi0.9Pr0.1FeO3 nanoceramics

    NASA Astrophysics Data System (ADS)

    Mahato, Dev K.; Saha, Sujoy; Sinha, T. P.

    2016-05-01

    Nano-crystalline Bi0.9Pr0.1FeO3 (BPFO) ceramics have been synthesized by a sol-gel technique. The Rietveld refinement of the room temperature powder X-ray diffraction pattern confirms that the BPFO crystallizes in the rhombohedral R3c space group symmetry. SEM image of the sintered BPFO ceramic shows particles with same shape and fine grain morphology with the average grain size of 53±12 nm. The electrical properties of the ceramic are analysed by impedance spectroscopy. Grain and grain-boundary effect is observed in the material at lower temperature range which has been confirmed by electric modulus formalism. The ac conductivity spectrum obeys the Johnscher's power law. The activation energy calculated from dc conductivity is found to be 0.373 eV, which represents the conduction of small polaron over barrier between two sites of the lattice.

  8. : comparison between magnetron sputtering and sol-gel synthesis

    NASA Astrophysics Data System (ADS)

    Cosentino, S.; Knebel, S.; Mirabella, S.; Gibilisco, S.; Simone, F.; Bracht, H.; Wilde, G.; Terrasi, A.

    2014-07-01

    SiGeO films have been produced by a sol-gel derived approach and by magnetron sputtering deposition. Post-thermal annealing of SiGeO films in forming gas or nitrogen atmosphere between 600 and 900 °C ensured the phase separation of the SiGeO films and synthesis and growth of Ge nanoclusters (NCs) embedded in SiO2. Rutherford backscattering spectrometry analysis evidenced a similar Ge concentration (~12 %), but a different Ge out-diffusion after annealing between the two types of techniques with the formation of a pure SiO2 surface layer (~30 nm thick) in sol-gel samples. The thermal evolution of Ge NCs has been followed by transmission electron microscopy and Raman analysis. In both samples, Ge NCs form with similar size increase (from ~3 up to ~7 nm) and with a concomitant amorphous to crystalline transition in the 600-800 °C temperature range. Despite a similar Ge concentration, a significant lower NCs density is observed in sol-gel samples attributed to an incomplete precipitation of Ge, which probably remains still dispersed in the matrix. The optical absorption of Ge NCs has been measured by spectrophotometry analyses. Ge NCs produced by the sol-gel method evidence an optical band gap of around 2 eV, larger than that of NCs produced by sputtering (~1.5 eV). These data are presented and discussed also considering the promising implications of a low-cost sol-gel based technique towards the fabrication of light harvesting devices based on Ge nanostructures.

  9. 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].

  10. 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.

  11. 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.

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

    SciTech Connect

    Not Available

    1990-01-01

    This bibliography contains citations of selected patents concerning sol-gel processes and sol-gel derived materials and products. Selected patents include sol-gel compositions, ceramic and refractory materials, fabrication of silica glass, sol-gel thin films and coatings, transparent inorganic oxide glass, luminescent quartz glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, sol-gel production of microspheres, alumina composites, photographic materials, and dental materials. (This updated bibliography contains 120 citations, 12 of which are new entries to the previous edition.)

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

    SciTech Connect

    Not Available

    1989-09-01

    This bibliography contains citations of selected patents concerning Sol-Gel processes and Sol-Gel derived materials and products. Selected patents include Sol-Gel compositions, ceramic and refractory materials, fabrication of silica glass, Sol-Gel thin films and coatings, transparent inorganic oxide glass, luminescent quartz glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, Sol-Gel production of microspheres, alumina composites, photographic materials, and dental materials. (This updated bibliography contains 108 citations, 37 of which are new entries to the previous edition.)

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

    NASA Astrophysics Data System (ADS)

    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

    2012-05-01

    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.

  15. 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

  16. 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

  17. The morphology, proliferation rate, and population doubling time factor of adipose-derived mesenchymal stem cells cultured on to non-aqueous SiO2, TiO2, and hybrid sol-gel-derived oxide coatings.

    PubMed

    Marycz, Krzysztof; Krzak-Roś, Justyna; Donesz-Sikorska, Anna; Śmieszek, Agnieszka

    2014-11-01

    In recent years, much attention has been paid to the development of tissue engineering and regenerative medicine, especially when stem cells of various sources are concerned. In addition to the interest in mesenchymal stem cells isolated from bone marrow, recently more consideration has been given to stem cells isolated from adipose tissue (AdMSCs), due to their less invasive method of collection as well as their ease of isolation and culture. However, the development of regenerative medicine requires both the application of biocompatible material and the stem cells to accelerate the regeneration. In this study, we investigated the morphology, proliferation rate index (PRi), and population doubling time factor of adipose-derived mesenchymal stem cells cultured on non-aqueous sol-gel-derived SiO2, TiO2, and SiO2/TiO2 oxide coatings. The results indicated an increase in PRi of AdMSCs when cultured on to titanium dioxide, suggesting its high attractiveness for AdMSCs. In addition, the proper morphology and the shortest doubling time of AdMSCs were observed when cultured on titanium dioxide coating. PMID:24408867

  18. Effect of annealing temperature on the structural, photoluminescence and magnetic properties of sol-gel derived Magnetoplumbite-type (M-type) hexagonal strontium ferrite

    NASA Astrophysics Data System (ADS)

    Teh, Geok Bee; Wong, Yat Choy; Tilley, Richard D.

    2011-09-01

    Magnetoplumbite-type (M-type) hexagonal strontium ferrite particles were synthesized via sol-gel technique employing ethylene glycol as the gel precursor at two different calcination temperatures (800 and 1000 °C). Structural properties were systematically investigated via X-ray diffraction (XRD), field emission scanning electron microscopy, high resolution transmission electron microscopy (HRTEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), photoluminescence spectrophotometry and superconducting quantum interference device magnetometer. XRD results showed that the sample synthesized at 1000 °C was of single-phase with a space group of P6 3/mmc and lattice cell parameter values of a=5.882 Å and c=23.048 Å. EDS confirmed the composition of strontium ferrite calcined at 1000 °C being mainly of M-type SrFe 12O 19 with HRTEM micrographs confirming the ferrites exhibiting M-type long range ordering along the c-axis of the crystal structure. The photoluminescence (PL) property of strontium ferrite was examined at excitation wavelengths of 260 and 270 nm with significant PL emission peaks centered at 350 nm being detected. Strontium ferrite annealed at higher temperature (1000 °C) was found to have grown into larger particle size, having higher content of oxygen vacancies and exhibited 83-85% more intense PL. Both the as-prepared strontium ferrites exhibited significant oxygen vacancies defect structures, which were verified via TGA. Higher calcination temperature turned strontium ferrite into a softer ferrite.

  19. Sol-gel derived Zn1-xFexS diluted magnetic semiconductor thin films: Compositional dependent room or above room temperature ferromagnetism

    NASA Astrophysics Data System (ADS)

    Goktas, A.

    2015-06-01

    Zn1-xFexS (where x = 0.00, 0.01, 0.03, 0.05, 0.1 and 0.2) thin films were synthesized by sol-gel method. To investigate the origin of room or above room temperature ferromagnetism in these films several tools such as XRD, SEM, XPS, UV-Vis spectrophotometer and SQUİD magnetometer were used. The XRD studies showed that the phase singularity of ZnS zinc blende (hexagonal) structure. The SEM images indicated the homogeneous film surface with no cracking and increased particle size with increasing Fe-doping ratio except for 1 at.% Fe dopant. The presence of Zn, Fe, S, Si and O atoms in the films was observed in EDS spectrum. The XPS studies confirmed that the existence of Fe3+ ions in host ZnS thin films. In the UV-Vis measurements the band gap energy corresponding to the absorption edge was estimated to be approximately in the range of 3.59-2.08 eV, depending on the Fe doping level. The magnetization measurements revealed that the films had paramagnetic or ferromagnetic order depending on Fe doping ratio at 5, 100, 200, 300 and 350 K. The observed room or above room temperature ferromagnetism can be attributed to the strong p-d exchange interaction between Fe3+ d and anion (S2-) p orbitals as well as impurities.

  20. Evaluation of sol-gel derived Eu 2+ activated SrMgAl 2SiO 7 as a novel nanostructure luminescent pigment

    NASA Astrophysics Data System (ADS)

    Sameie, H.; Salimi, R.; Sabbagh Alvani, A. A.; Sarabi, A. A.; Moztarzadeh, F.; Tahriri, M.

    2010-12-01

    A novel nanostructure pigment of Eu 2+ doped SrMgAl 2SiO 7 was prepared via the sol-gel route. The phase composition and condition of crystallites during heating were characterized by X-ray diffraction (XRD) analysis. Investigation of optical properties by spectrophotometer illustrated that under short ultraviolet excitation wavelength, the main emission peak occurred at about 415-420 nm. Also, relatively pure purplish blue color was observed that can be ascribed to the 4f 65d 1( 2D) →4f 7( 8S 7/2) transition of Eu 2+. The effect of calcination temperature on the luminescence properties of the phosphors was evaluated and, also in this case, scanning electron microscope (SEM) was employed. From colorimetry results, color coordinations of phosphor shift towards the deep blue region as calcination temperature increases. Finally, grain size of products at optimum calcination temperature was estimated to be about 20-30 nm using Scherrer’s equation, which was consistent with transmission electron microscopy (TEM) observations.

  1. Synthesis characterization and luminescence studies of 100 MeV Si8+ ion irradiated sol gel derived nanocrystalline Y2O3

    NASA Astrophysics Data System (ADS)

    Lakshminarasappa, B. N.; Shivaramu, N. J.; Nagabhushana, K. R.; Singh, Fouran

    2014-06-01

    Nanoparticles of pure yttrium oxide (Y2O3) have been prepared by sol gel method. The powder X-ray diffraction (PXRD) pattern of as synthesized sample showed the amorphous nature. The as synthesized Y2O3 powders are annealed at 500, 600, 700, 800 and 900 °C for 2 h. Y2O3 powder heat treated for 600 °C showed cubic phase and the crystallite sizes are found to be ˜13 nm. Fourier transformed infrared spectroscopy (FTIR) revealed absorption with peaks at 3434, 1724, 1525, 1400, 847, 562 and 465 cm-1. Photoluminescence (PL) of 100 MeV Si8+ ion irradiated samples shows emission with peaks at 417, 432, 465 nm. It is found that PL intensity increases with increasing in ion fluence up to ˜3 × 1012 ions cm-2 and then decreases with further increase in ion fluence. A well resolved thermoluminescence (TL) glow with peak at ˜430 K (Tm1) and an unresolved TL glow with peak at ˜538 (Tm2), 584 K (Tm3) are observed in ion irradiated samples.

  2. Far-infrared properties of sol-gel derived PbZr0.52Ti0.48O3 thin films on Pt-coated substrates

    NASA Astrophysics Data System (ADS)

    Kafadaryan, E. A.; Hovsepyan, R. K.; Khachaturova, A. A.; Aghamalyan, N. R.; Shirinyan, G. O.; Manukyan, A. L.; Vardanyan, R. S.; Hayrapetyan, A. G.; Grigoryan, S. G.; Vardanyan, E. S.

    2003-02-01

    Polycrystalline tetragonal PbZr0.52Ti0.48O3 (PZT) thin films have been deposited on the nickel and (111) platinum coated (110) sapphire substrates by the sol-gel method. Optical properties of the PZT thin films were studied using far-infrared reflectivity spectroscopy in the 200-10 000 cm-1 frequency range at 300 K. The frequency dependence of the optical characteristics (sigma, varepsilon, -Im varepsilon-1) of the films were calculated by the Kramers-Kronig transformation of the reflectivity spectra and analysed by the Drude-Lorentz model. The frequency dependence of the optical conductivity, sigma(omega), of the PZT films deposited on platinum coated sapphire is well described by the free-carrier term and an overdamped mid-infrared component. Sapphire/Pt/PZT structures reveal semiconductor properties (effective carrier concentration N/mast is up to 1020 cm-3, plasma minimum is located near 3000 cm-1). This effect can be related to the favourable influence of the platinum electrode on the charge carrier density at Pt/PZT contact and formation of the interfacial conductive layer.

  3. 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

  4. Ion-induced secondary electron emission behavior of sol-gel-derived MgO thin films used for protective layers in alternating current plasma display panels

    NASA Astrophysics Data System (ADS)

    Jung, Hyun Suk; Lee, Jung-Kun; Hong, Kug Sun; Youn, Hyuk-Joon

    2002-09-01

    MgO thin films were prepared using two sols (hydrolyzed sol and stabilized sol) and the ion-induced secondary electron emission behavior of the resultant thin films was investigated. A severe fluctuation in the secondary electron emission current was found in MgO films from hydrolyzed sol. The instability of the ion-induced current was due to the nanosized pores, which were formed during the topotactic reaction of Mg(OH)2 to MgO. Nonhydrolyzed MgO films, however, showed a stable ion-induced current. The ion-induced secondary electron emission coefficients (gammai) of the MgO films had a maximum of 0.95plus-or-minus0.02 when the films were heat treated at 550 degC in O2. The change in gammai of nonhydrolyzed films was discussed from the viewpoint of crystallinity, residual organics, and surface roughness. The high gammai and low processing temperature of nonhydrolyzed MgO films revealed that the sol-gel process is suitable to prepare MgO films for use as a protective layer in ac plasma display panel cells.

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

    SciTech Connect

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

    2010-12-15

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

  7. 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.

  8. 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.

  9. In vitro response of human osteoblasts to multi-step sol-gel derived bioactive glass nanoparticles for bone tissue engineering.

    PubMed

    Fan, Jian Ping; Kalia, Priya; Di Silvio, Lucy; Huang, Jie

    2014-03-01

    A multi-step sol-gel process was employed to synthesize bioactive glass (BG) nanoparticles. Transmission electron microscopy (TEM) revealed that the BG nanoparticles were spherical and ranged from 30 to 60 nm in diameter. In vitro reactivity of the BG nanoparticles was tested in phosphate buffer saline (PBS), Tris-buffer (TRIS), simulated body fluid (SBF), and Dulbecco's modified Eagle's medium (DMEM), in comparison with similar sized hydroxyapatite (HA) and silicon substituted HA (SiHA) nanoparticles. Bioactivity of the BG nanoparticles was confirmed through Fourier transform infrared spectroscopy (FTIR) analysis. It was found that bone-like apatite was formed after immersion in SBF at 7 days. Solutions containing BG nanoparticles were slightly more alkaline than HA and SiHA, suggesting that a more rapid apatite formation on BG was related to solution-mediated dissolution. Primary human osteoblast (HOB) cell model was used to evaluate biological responses to BG nanoparticles. Lactate dehydrogenase (LDH) cytotoxicity assay showed that HOB cells were not adversely affected by the BG nanoparticles throughout the 7day test period. Interestingly, MTS assay results showed an enhancement in cell proliferation in the presence of BG when compared to HA and SiHA nanoparticles. Particularly, statistically significant (p<0.05) alkaline phosphatase (ALP) activity of HOB cells was found on the culture containing BG nanoparticles, suggesting that the cell differentiation might be promoted by BG. Real-time quantitative PCR analysis (qPCR) further confirmed this finding, as a significantly higher level of RUNX2 gene expression was recorded on the cells cultured in the presence of BG nanoparticles when compared to those with HA and SiHA. PMID:24433905

  10. Temperature dependence of the optical band gap and electrical conductivity of sol-gel derived undoped and Li-doped ZnO films

    NASA Astrophysics Data System (ADS)

    Caglar, Mujdat; Caglar, Yasemin; Aksoy, Seval; Ilican, Saliha

    2010-06-01

    Undoped and lithium (Li)-doped ZnO films were prepared by sol-gel method using spin coating technique. The effects of Li content on the crystallinity and morphological properties of ZnO films were assessed by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). XRD patterns of the films showed the hexagonal wurtzite type polycrystalline structure and that the incorporation of lithium leads to substantial changes in the structural characteristics of ZnO films. The SEM and AFM measurements showed that the surface morphology of the films was affected from the lithium incorporation. The wrinkle network was observed on the surface from both SEM and AFM results for undoped ZnO. The wrinkle structure disappeared with increasing Li content. The absorption spectra of the ZnO and 5% Li-doped ZnO (LZO5) films were carried out between 140 and 400 K temperatures. The optical band gap of ZnO and LZO5 films (calculated at various temperatures) showed a linear dependence on the temperature. The absolute zero value optical band gap and the rate of change of the band gap with temperature of the ZnO and LZO5 films were found to be 3.339 and 3.322 eV, and 2.95 × 10 -4 and 1.60 × 10 -4 eV/K, respectively. The transport mechanisms in the ZnO and LZO5 films have been investigated by analyzing of the temperature (80-300 K) dependence of the conductivity. The activation energies of the ZnO film increased with Li content.

  11. 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.

  12. 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.

  13. 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.

  14. Neutron detector using sol-gel absorber

    SciTech Connect

    Hiller, J.M.; Wallace, S.A.; Dai, S.

    1999-10-26

    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.

  15. 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.

  16. 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.

  17. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna

    1992-01-01

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

  18. 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.

  19. Sol-gel processing of metal sulfides

    NASA Astrophysics Data System (ADS)

    Stanic, Vesha

    Metal sulfides were synthesised via a sol-gel process using various metal alkoxides and hydrogen sulfide in toluene. Colloidal gels were prepared from germanium ethoxide, germanium isopropoxide, zinc tert-butoxide and tungsten (VI) ethoxide, whereas colloidal powder was produced from tungsten (V) dichloride ethoxide. Special precautions were necessary to protect the reaction mixture from water contamination which produced metal oxides. Results indicated that the main source of water is the hydrogen sulfide gas. In addition, synthesis of metal sulfides from a mixture of metal oxide and sulfide was demonstrated by the example of monoclinic germanium disulfide. It was produced by reaction of the sol-gel product with sulfur. Heat treatment of the sol-gel product and sulfur yielded single phase GeSsb2. The sol-gel prepared materials and their heat treated products were characterized by various methods. A chemical kinetics study of the functional groups -OR, -SH and Ssp{2-} was carried out for the sol-gel processing of GeSsb2 from of hydrogen sulfide and two different alkoxides, germanium ethoxide and germanium isopropoxide. The study was performed for different concentrations of precursors at different molar ratios and temperatures. The results indicate that the proposed reaction mechanism was simplified under appropriate reaction conditions. Experimentally determined rate constants of thiolysis and condensations demonstrate that thiolysis is slow and that condensations are fast steps, regardless of the studied reaction conditions. A study of the temperature effect on the reaction rate constant shows that it increases with temperature in accord with both Arrhenius law and transition-state theory. Activation energies, Esba, and activation parameters DeltaSsp{ddagger}, DeltaHsp{ddagger} and DeltaGsp{ddagger}, were determined for thiolysis and condensation reactions. The potentiometric tiration method was used for quantitative determination of germanium sulfide and

  20. Modified sol-gel coatings for biotechnological applications

    NASA Astrophysics Data System (ADS)

    Beganskiene, A.; Raudonis, R.; Zemljic Jokhadar, S.; Batista, U.; Kareiva, A.

    2007-12-01

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

  1. Droplet Spreading with Sol-Gel Transition

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

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

  2. Innovative materials based on sol gel technology

    NASA Astrophysics Data System (ADS)

    Reisfeld, Renata; Saraidarov, Tsiala

    2006-01-01

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

  3. 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.

  4. 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.

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

    PubMed

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

    1996-08-01

    Enzymes usually cannot withstand the high-temperature curing associated with the thick-film fabrication process and require a separate immobilization step in connection with the production of single-use biosensors. We report on the development of sol-gel-derived enzyme-containing carbon inks that display compatibility with the screen-printing process. Such coupling of sol-gel and thick-film technologies offers a one-step fabrication of disposable enzyme electrodes, as it obviates the need for thermal curing. The enzyme-containing sol-gel carbon ink, prepared by dispersing the biocatalyst, along with the graphite powder and a binder, within the sol-gel precursors, is cured very rapidly (10 min) at low temperature (4 °C). The influence of the ink preparation conditions is explored, and the sensor performance is evaluated in connection with the incorporation of glucose oxidase or horseradish peroxidase. The resulting strips are stable for at least 3 months. Such sol-gel-derived carbon inks should serve as hosts for other heat-sensitive biomaterials in connection with the microfabrication of various thick-film biosensors. PMID:21619216

  6. 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.

  7. Sol-gel manufactured energetic materials

    DOEpatents

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

    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.

  8. 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. PMID:25074359

  9. 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

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

    SciTech Connect

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

    2007-10-17

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

  11. 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.

  12. 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.

  13. Photochromic organic-inorganic composite materials prepared by sol-gel processing: Properties and potentials

    SciTech Connect

    Hou, L. |; Mennig, M.; Schmidt, H.

    1994-12-31

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

  14. 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. PMID:25464107

  15. 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. PMID:26539840

  16. Fluoride glasses from sol gels. Final report

    SciTech Connect

    Uhlmann, D.R.

    1986-09-15

    The use of sol-gel coatings to strengthen oxide glasses was demonstrated for the case of fused silica. Increases in strength to as much as 2.2 times the strength of uncoated glass were obtained. The strengthening does not involve the annealing of surface microcracks, but rather the filling-in of such flaws. The strengthening does not depend on coating thickness over the range 2000-10000 Angstroms, but does depend significantly upon the state of hydrolysis of the substrate surface.

  17. 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

  18. 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.

  19. OPTIMIZATION OF ALKYL ESTER PRODUCTION FROM GREASE USING A PHYLLOSILICATE SOL-GEL IMMOBILIZED LIPASE

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Simple alkyl ester derivatives of restaurant grease were prepared using a lipase from Pseudomonas cepacia immobilized within a phyllosilicate sol-gel matrix as biocatalyst. Alcoholysis reactions of grease were carried out in solvent-free media using a one step addition of alcohol to reaction mixtur...

  20. 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…

  1. 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. PMID:21132520

  2. 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

  3. Optical characterization of anti reflective sol-gel coatings fabricated using dip coating method

    NASA Astrophysics Data System (ADS)

    Melninkaitis, A.; Juškevičius, K.; Maciulevičius, M.; Sirutkaitis, V.; Beganskienė, A.; Kazadojev, I.; Kareiva, A.; Perednis, D.

    2007-01-01

    In recent years, there has been a growing interest in further development of sol-gel method which can produce ceramics and glasses using chemical precursors at relative low-temperatures. The applications for sol-gel derived products are numerous. Department of General and Inorganic Chemistry with Laser Research Center of Vilnius University and Institute of Physics continues an ongoing research effort on the synthesis, deposition and characterization of porous solgel. Our target is highly optically resistant anti-reflective (AR) coatings for general optics and nonlinear optical crystals. In order to produce AR coatings a silica (SiO II) sol-gel has been dip coated on the set of fused silica substrates. The optical properties and structure of AR-coatings deposited from hydrolysed tetraethylorthosilicate (TEOS) sol were characterized in detail in this study. The influence of different parameters on the formation of colloidal silica antireflective coatings by dip-coating technique has been investigated. All samples were characterized performing, transmission electron microscopy, UV-visible spectroscopy, atomic force microscopy, ellipsometric, total scattering and laser-induced damage threshold measurements. Herewith we present our recent results on synthesis of sol-gel solvents, coating fabrication and characterization of their optical properties.

  4. Composite sol-gel process for photocatalytic titanium dioxide

    NASA Astrophysics Data System (ADS)

    Keshmiri, Mehrdad

    Photocatalytic TiO2 decomposes organic and inorganic pollutants upon irradiation with UV light. TiO2 thin films and powder suspensions are used for purification treatments, but small surface area of TiO2 films, and difficult filtration of powders are the two major drawbacks in application of photocatalytic TiO2. The major objective of this work was to develop a novel process to combine the thin film coatings and the fine (sub-micron) powder anatase TiO2 to provide high photocatalytic efficiency thick films and self-supported membranes. The microstructural properties and photocatalytic efficiency of the developed materials were characterized and compared with that of the conventional TiO2 coatings and powders. Photocatalytic activity of CSG TiO 2 was measured through the ability to decompose organic compounds (trichloroethane, dioxane, toluene), as well as to destroy bacteria. The major achievement of this work is the development of a process wherein structurally sound, thick films and membranes of CSG anatase photocatalytic TiO2 can be produced in reproducible way. A novel method for the synthesis of monodispersed anatase TiO2 microspheres through colloidal precipitation has also been established. The microspheres were used as filler TiO2 in the composite microstructure, bonded with sot-gel derived TiO2, to produce the composite sol-gel (CSG) TiO2. A sol-gel-assisted sintering model for the CSG thick films and self-supported membranes was established and validated by experimental data. The model has the ability to predict the sintering behavior of the CSG-TiO2, in terms of the reduction of specific surface area versus the time of heating, particularly at the initial and intermediate stages of the sintering.

  5. 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.

  6. Energy migration of the local excitation at the Eu3+ site in a Eu-O chemical cluster in sol-gel derived SiO2:Eu3+ glasses

    NASA Astrophysics Data System (ADS)

    Hayakawa, Tomokatsu; Nogami, Masayuki

    2001-09-01

    By using the fluorescence line-narrowing technique, we observed a broad fluorescence band in the vicinity of a resonant line of the 5D0→7F0 transition in an Eu3+-doped SiO2 glass synthesized by a sol-gel process. The comparison with a similar line in an Al2O3-SiO2:Eu3+ sol-gel glass revealed the existence of a chemical cluster of Eu3+ and O2- in the tetrahedral SiO4 network. The broad fluorescence band was attributable to an energy migration among the Eu3+ ions for the site-selectively received excitation energy. Also, based on Yokota-Tanimoto's energy diffusion model, the fluorescence decay curves for the 5D0→7F2 transition were closely correlated with the energy migration and gel-glass transformation. The gel-shrinkage and reduced interatomic distance between Eu3+ ions due to a thermal treatment at higher temperature definitely resulted in a decrease in the associated lifetime of the initial decay.

  7. 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.

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

    NASA Technical Reports Server (NTRS)

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

    1990-01-01

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

  9. 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.

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

    SciTech Connect

    Singh, Satyendra; Krupanidhi, S. B.

    2012-01-15

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

  11. Dielectric anomaly in Li-doped zinc oxide thin films grown by sol gel route

    NASA Astrophysics Data System (ADS)

    Dhananjay; Singh, Satyendra; Nagaraju, J.; Krupanidhi, S. B.

    2007-08-01

    Sol gel route was employed to grow polycrystalline thin films of Li-doped ZnO thin films (Zn1-xLixO, x=0.15). Polycrystalline films were obtained at a growth temperature of 400 500 °C. Ferroelectricity in Zn0.85Li0.15O was verified by examining the temperature variation of the real and imaginary parts of dielectric constant, and from the C V measurements. The phase transition temperature was found to be 330 K. The room-temperature dielectric constant and dissipation factor were 15.5 and 0.09 respectively, at a frequency of 100 kHz. The films exhibited well-defined hysteresis loop, and the values of spontaneous polarization (Ps) and coercive field were 0.15 μC/cm2 and 20 kV/cm, respectively, confirming the presence of ferroelectricity.

  12. 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

  13. 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.

  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. Regioselective hydroaminomethylation of vinylarenes by a sol-gel immobilized rhodium catalyst.

    PubMed

    Nairoukh, Zackaria; Blum, Jochanan

    2014-03-21

    In the course of our studies toward the development of new heterogeneous conditions for better controlling regioselectivity in organic reactions, we investigated the application of sol-gel immobilized organometallic catalyst for regioselective hydroaminomethylation of vinylarenes with aniline or nitroarene derivatives in an aqueous microemulsion. By immobilization of 6 mol % [Rh(cod)Cl]2 within a hydrophobic silica sol-gel matrix we were able to perform efficient hydroaminomethylation under mild conditions and isolate 2-arylpropylamines with high regioselectivity. The regioselectivity of the reaction was found to be mainly dependent on the hydrophobicity of the catalyst support. It is also significantly affected by the electronic nature of the substrates, by the reaction temperature, and by syngas pressure. The heterogenized catalyst can be reused for several times. PMID:24528141

  17. Structural evolution and stability of sol gel biocatalysts

    NASA Astrophysics Data System (ADS)

    Rodgers, L. E.; Knott, R. B.; Holden, P. J.; Pike, K. J.; Hanna, J. V.; Foster, L. J. R.; Bartlett, J. R.

    2006-11-01

    Immobilisation strategies for catalytic enzymes are important as they allow recovery and reuse of the biocatalysts. In this work, sol-gel matrices have been used to immobilise Candida antarctica lipase B (CALB), a commonly used industrial enzyme. The sol-gel bioencapsulate is produced through fluoride-catalysed hydrolysis of mixtures of tetramethylorthosilicate (TMOS) and methyltrimethoxysilane (MTMS) in the presence of CALB, yielding materials with controlled pore sizes and surface chemistries. Sol-gel matrices prolong the catalytic life and enhance the activity of CALB, although the molecular basis for this effect has yet to be elucidated due to the limitations of analytical techniques applied to date. Small angle neutron scattering (SANS) allows such multi-component systems to be characterised through contrast matching. In the sol-gel bioencapsulate system at the contrast match point for silica, residual scattering intensity is due to the CALB and density fluctuations in the matrix. A SANS contrast variation series found the match point for the silica matrix, both with and without enzyme present, to be around 35%. The model presented here proposes a mechanism for the interaction between CALB and the surrounding sol-gel matrix, and the observed improvement in enzyme activity and matrix strength. Essentially, the inclusion of CALB modulates silicate speciation during evolution of the inorganic network, leading to associated variations in SANS contrast. The SANS protocol developed here may be applied more generally to other encapsulated enzyme systems.

  18. 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.

  19. Modification of sol-gel coatings by ion implantation

    NASA Astrophysics Data System (ADS)

    Hirashima, Hiroshi; Adachi, Kenji; Imai, Hiroaki

    1994-10-01

    In order to densify and to improve the physical properties, TiO2 sol-gel films, about 100 nm in thickness, on silica glass or silicon wafer were implanted with Ar+ or B+ ions. The refractive index of the as-dried films increased and the IR absorption band of OH disappeared after Ar+ implantation. Dehydration and densification of sol-gel films were enhanced by Ar+ implantation. On the other hand, the refractive index and the thickness of the films hardly changed by B+ implantation. However, IR absorption bands attributed to B-O bond were observed after B+ implantation. This suggests that sol-gel films could be chemically modified by ion implantation with reactive ion species.

  20. 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.

  1. Synthesis of garnet structure compounds using aqueous sol-gel processing

    NASA Astrophysics Data System (ADS)

    Leleckaite, A.; Kareiva, A.

    2004-07-01

    The sol-gel method based on metal chelates in aqueous solvents has been developed to prepare different oxides having garnet crystal structure. This synthetic approach has been used to prepare rare-earth doped yttrium aluminum garnet Y 3Al 5O 12:Ce, Y 3Al 5O 12:Nd, Y 3Al 5O 12:Ho, and Y 3Al 5O 12:Er samples (YAG:Ln). The polycrystalline powders sintered at 1000 °C are formed as single-phase garnet materials. The formation of pure and neodymium-doped lanthanum aluminum garnets (La 3Al 5O 12 (LAG), and La 3Al 5O 12:Nd (LAG:Nd)) at the same synthesis conditions, however, does not proceed. A systematic study of sol-gel technique synthesized Y 3Ga 5O 12 (YGG) is presented using six different complexing agents. These complexing agents were found to influence the characteristics of the end products, in particular the homogeneity. Finally, some specific features of sol-gel derived mixed-metal Y 3Sc xAl 5- x- yGa yO 12 (0⩽ x, y⩽5) (YSAGG) garnets are discussed in the present paper. The phase purity, composition and microstructural features in the polycrystalline samples were studied by XRD analysis, IR spectroscopy and scanning electron microscopy.

  2. 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.

  3. 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

  4. 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.

  5. 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.

  6. Investigations of sol gel-derived highly (100)-oriented Ba0.5Sr0.5TiO3 : MgO composite thin films for phase-shifter applications

    NASA Astrophysics Data System (ADS)

    Jain, M.; Majumder, S. B.; Katiyar, R. S.; Bhalla, A. S.; Miranda, F. A.; van Keuls, F. W.

    2005-02-01

    Sol gel deposition of highly oriented Ba0.5Sr0.5TiO3 : MgO composite thin films has shown desirable dielectric constant reduction and higher figure of merit for phase-shifter applications. In this multilayer configuration, MgO distributed homogeneously through the Ba0.5Sr0.5TiO3 (BST50) matrix, and it helped in tailoring the dielectric constant and reducing the loss tangent significantly. In the present study, the high-frequency dielectric behavior of the films has been evaluated by fabricating an eight-element coupled microstrip phase shifter and measuring the degree of phase shift and insertion loss as a function of applied voltage at room temperature. An increase in phase-shifter figure of merit (degree of phase shift per dB insertion loss) from 28°/dB for pure BST50 to 71°/dB for a BST50 : MgO film (at 14 GHz and 333 kV/cm) has been observed.

  7. 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}).

  8. Stoichiometric hydroxyapatite obtained by precipitation and sol gel processes

    NASA Astrophysics Data System (ADS)

    Vazquez, C. G.; Barba, C. P.; Munguia, N.

    2005-06-01

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

  9. 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.

  10. 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...