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Sample records for alkoxide-based sol-gel route

  1. The effect of refluxing on the alkoxide-based sodium potassium niobate sol-gel system: Thermal and spectroscopic studies

    SciTech Connect

    Chowdhury, Anirban; Bould, Jonathan; Londesborough, Michael G.S.; Milne, Steven J.

    2011-02-15

    A study on the effects of prolonged heating under reflux conditions of up to 70 h on alkoxides of sodium, potassium and niobium dissolved in 2-methoxyethanol for the synthesis of sols of composition Na{sub 0.5}K{sub 0.5}NbO{sub 3} (NKN) has been carried out using combined thermogravimetric-Fourier transform infrared spectroscopic analyses. Extended refluxing increases the homogeneity of the Na{sub 0.5}K{sub 0.5}NbO{sub 3} (NKN) system. Spectroscopic analyses on the non-refluxed and 70 h refluxed NKN gels reveal the existence of inorganic hydrated carbonates and bicarbonates, which we propose arise from the hydration and carbonation of the samples on standing in air. The X-ray diffraction patterns of these two types of gels show orthorhombic NKN phase evolutions at higher temperatures. -- Graphical abstract: Total organic evolution plots over time for NKN dried gels obtained under different refluxing times show different thermochemical behaviours and these were investigated by thermal and spectroscopic analysis tools to find a correlation between the extent of -M-O-M- chain link formation and the amount of solvent vapour (methoxyethanol) evolution. Display Omitted Research highlights: > Prolonged refluxing of sol-gel NKN precursor solutions improves final properties of an NKN system. > An NKN process thermo-chemistry with thermal and spectroscopic analysis tools was explored. > An FTIR of NKN gels reveals tendency of NKN systems for rehydration and recarbonation on standing.

  2. Synthesis of Carbon Nanotubes Using Sol Gel Route

    NASA Astrophysics Data System (ADS)

    Abdel-Fattah, Tarek

    2002-12-01

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

  3. 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.

  4. Synthesis of nano-titanium dioxide by sol-gel route

    NASA Astrophysics Data System (ADS)

    Kaler, Vandana; Duchaniya, R. K.; Pandel, U.

    2016-04-01

    Nanosized titanium dioxide powder was synthesised via sol-gel route by hydrolysis of titanium tetraisopropoxide with ethanol and water mixture in high acidic medium. The synthesized nanopowder was further characterized by X-ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and Ultraviolet Visible Spectroscopy in order to determine size, morphology and crystalline structure of the material. The synthesis of nano-TiO2 powder in anatase phase was realized by XRD. The optical studies of nano-TiO2 powder was carried out by UV-Vis spectroscopy and band gap was calculated as 3.5eV, The SEM results with EDAX confirmed that prepared nano-TiO2 particles were in nanometer range with irregular morphology. The FTIR analysis showed that only desired functional groups were present in sample. These nano-TiO2 particles have applications in solar cells, chemical sensors and paints, which are thrust areas these days.

  5. A new synthesis route to high surface area sol gel bioactive glass through alcohol washing

    PubMed Central

    M. Mukundan, Lakshmi; Nirmal, Remya; Vaikkath, Dhanesh; Nair, Prabha D.

    2013-01-01

    Bioactive glass is one of the widely used bone repair material due to its unique properties like osteoconductivity, osteoinductivity and biodegradability. In this study bioactive glass is prepared by the sol gel process and stabilized by a novel method that involves a solvent instead of the conventional calcinations process. This study represents the first attempt to use this method for the stabilization of bioactive glass. The bioactive glass stabilized by this ethanol washing process was characterized for its physicochemical and biomimetic property in comparison with similar composition of calcined bioactive glass. The compositional similarity of the two stabilized glass powders was confirmed by spectroscopic and thermogravimetric analysis. Other physicochemical characterizations together with the cell culture studies with L929 fibroblast cells and bone marrow mesenchymal stem cells proved that the stabilization was achieved with the retention of its inherent bioactive potential. However an increase in the surface area of the glass powder was obtained as a result of this ethanol washing process and this add up to the success of the study. Hence the present study exhibits a promising route for high surface area bioactive glass for increasing biomimicity. PMID:23512012

  6. Porous titania films fabricated via sol gel rout - Optical and AFM characterization

    NASA Astrophysics Data System (ADS)

    Karasiński, Paweł; Gondek, Ewa; Drewniak, Sabina; Kajzer, Anita; Waczyńska-Niemiec, Natalia; Basiaga, Marcin; Izydorczyk, Weronika; Kouari, Youssef E. L.

    2016-06-01

    Mesoporous titania films of low refractive index ∼1.72 and thickness within the range of 57-96 nm were fabricated via sol-gel rout and dip-coating technique on a soda-lime glass substrate. Tetrabutylorthotitanate Ti(OBu)4 was used as a titania precursor. High porosity and consequently low refractive index were achieved using the polyethylene glycol (PEG 1100) as a template. Based on transmittance, using Tauc's relations, the optical energy band gaps and the Urbach energy were determined. The research shows that in the fabricated titania films there are two types of optical energy band gaps, connected with direct and indirect electron transitions and brought about by the presence of amorphous and crystalline phase respectively. Based on the quantum size effect, the diameters of nanocrystals versus film thickness were determined. AFM studies of the titania films have demonstrated that there are changes of surface morphology taking place with the change of thickness. We have demonstrated that the surface morphology of titania films has influence on wettability.

  7. Production and characterization of spodumene dosimetric pellets prepared by a sol-gel route

    NASA Astrophysics Data System (ADS)

    Lima, H. R. B. R.; Nascimento, D. S.; Bispo, G. F. C.; Teixeira, V. C.; Valério, M. E. G.; Souza, S. O.

    2014-11-01

    Spodumene is an aluminosilicate that has shown good results for high-dose TL dosimetry for beta or gamma rays. Due to its chemical composition (LiAlSi2O6) it has potential to be used as a neutron dosimeter. The synthetic spodumene is usually produced by solid state reaction and conventional sol-gel, whose shortcomings arise from the need to employ high temperatures and high cost reagents, respectively. Proteic sol-gel method is promising, because it can reduce production costs and the possibility of environmental contamination. This work reports the production of the spodumene by the proteic sol-gel method using edible unflavored gelatin as a precursor. The product is characterized physically and morphologically, and investigated its applicability as a TL dosimeter. Two sets of samples were prepared using different sources of silicon, one with TEOS (Si(OC3H5)4) and one with SILICA (SiO2). The materials produced were characterized by X-ray diffraction, differential thermal analysis and thermogravimetry in order to evaluate the structural properties, as well as possible changes in physical or chemical properties depending on the temperature. The production of spodumene was successful, with generation of the crystals in the β-phase with tetragonal structure. Sintered pellets produced from these crystals were irradiated with a 90Sr-90Y source and their TL glow curves were evaluated. Although the samples prepared by the proteic sol-gel method with TEOS presented a lower forming temperature, the samples produced with SILICA showed higher sensitivity to radiation.

  8. Low-temperature deposition of the high-performance anatase-titania optical films via a modified sol gel route

    NASA Astrophysics Data System (ADS)

    Sheng, Yonggang; Liang, Liping; Xu, Yao; Wu, Dong; Sun, Yuhan

    2008-04-01

    Anatase-titania films with high optical performances have been deposited via a modified sol-gel route. This involved several precisely controlled processes including a sufficient hydrolysis of titanium tetraisopropoxide (TTIP) with excessive water, a peptization at pH value of 1-2, a restrained condensation under the hydrothermal conditions at 373 K, and finally a spin-coating process at 293 K. A full characterization of the sols and films indicated that such a well-controlled hydrolysis and condensation of TTIP enabled the formation of high-quality precursor sols consisting of anatase-titania colloidal particles with the mean hydrodynamic diameter of about 17.2 nm, and then endowed the as-deposited films with nanocrystalline structure and the corresponding high refractive index of 1.92 (at 632.8 nm). Moreover, the prepared films exhibited large optical bandgap of 3.38 eV and high laser-induced damage threshold of 16.3 J/cm 2 (at 1064 nm, 3 ns pulse duration and R/1 testing mode), which must be closely related to their homogeneous and nearly defect-free network structures derived from the low-temperature sol-gel deposition route.

  9. New sol-gel synthetic route to transition and main-group metal oxide aerogels using inorganic salt precursors

    SciTech Connect

    Gash, A E; Tillotson, T M; Satcher Jr, J H; Hrubesh, L W; Simpson, R L

    2000-09-12

    We have developed a new sol-gel route to synthesize several transition and main-group metal oxide aerogels. The approach is straightforward, inexpensive, versatile, and it produces monolithic microporous materials with high surface areas. Specifically, we report the use of epoxides as gelation agents for the sol-gel synthesis of chromia aerogels and xerogels from simple Cr(III) inorganic salts. The dependence of both gel formation and its rate was studied by varying the solvent used, the Cr(III) precursor salt, the epoxide/Cr(III) ratio, as well as the type of epoxide employed. All of these variables were shown to affect the rate of gel formation and provide a convenient control of this parameter. Dried chromia aerogels were characterized by high-resolution transmission electron microscopy (HRTEM) and nitrogen adsorption/desorption analyses, results of which will be presented. Our studies have shown that rigid monolithic gels can be prepared from many different metal ions salts, provided the formal oxidation state of the metal ion is greater than or equal to +3. Conversely, when di-valent transition metal salts are used precipitated solids are the products.

  10. Effect of the sol-gel route on the textural characteristics of silica imprinted with Rhodamine B.

    PubMed

    de Coelho Escobar, Cícero; dos Santos, João Henrique Zimnoch

    2014-04-01

    A series of silica xerogels that support Rhodamine B as a template were synthesized using distinct sol-gel routes, namely, acid-catalyzed routes, a base-catalyzed route, acid-catalyzed with base-catalyzed (two steps) hydrolytic routes, and a FeCl3 -catalyzed nonhydrolytic route. The extraction methods (thermal, Soxhlet, water washing, and ultrasound) were also evaluated. The resulting xerogels were characterized through porosimetry using nitrogen adsorption/desorption. The samples were further analyzed through small-angle X-ray scattering, Fourier transform infrared spectroscopy, and SEM. The preparation route affected the materials' textural properties. Extraction was optimized using acid and two-step routes. The acid route from Rhodamine B to Rhodamine 6G generated the highest selectivity factor (2.5). The nonhydrolytic route produced the best imprinting factor. Competitive adsorption was also used, from which the approximate imprinting factor was 2. The cavity shape generated during the production of the imprinted silica dictates the adsorption behavior, not the magnitude of the surface area. PMID:24478149

  11. Formation of bimodal porous silica-titania monoliths by sol-gel route

    NASA Astrophysics Data System (ADS)

    Ruzimuradov, O. N.

    2011-10-01

    Silica-titania monoliths with micrometer-scale macroporous and nanometer-scale mesoporous structure and high titania contents are prepared by sol-gel process and phase separation. Titanium alkoxide precursor was not effective in the preparation of high titania content composites because of strong decrease in phase separation tendency. Bimodal porous gels with high titania content were obtained by using inorganic salt precursors such as titanium sulfate and titanium chloride. Various characterization techniques, including SEM, XRD, Hg porosimetry and N2 adsorption have been carried out to investigate the formation process and physical-chemical properties of silica-titania monoliths. The characterization results show that the silica-titania monoliths possess a bimodal porous structure with well-dispersed titania inside silica network. The addition of titania in silica improves the thermal stability of both macroporous and mesoporous structures.

  12. Thermo-optic characterization of neodymium/nickel doped silica glasses prepared via sol-gel route.

    PubMed

    Manuel, Ancy; Kumar, B Rajesh; Basheer, N Shemeena; Kumari, B Syamala; Paulose, P I; Kurian, Achamma; George, Sajan D

    2012-12-01

    Intrinsic as well as rare earth (Neodymium) doped silica glasses with various molar ratio of dopant and a metallic (Nickel) co-dopant is prepared via sol-gel route. The structural characterization of the sample is carried out using X-ray diffraction and Fourier Transform Infrared Spectroscopy. The influence of dopant and doping concentration on the optical properties of silica matrix is investigated via UV-VIS absorption spectroscopy. Effect of dopant on thermal effusivity value of the host matrix is carried out by laser induced open cell photoacoustic technique. Analysis of the results showed that doping affect the thermal effusivity value and results are interpreted in terms of structural modification of the lattice and phonon assisted heat transport mechanism.

  13. Influence of transition metals on the surface acidic properties of titania prepared by sol-gel route

    SciTech Connect

    Shali, N.B.; Sugunan, S. . E-mail: ssg@cusat.ac.in

    2007-09-04

    A series of titania catalysts containing chromium, molybdenum as well as tungsten has been prepared by colloidal sol-gel route using metatitanic acid as the precursor. Structural characterization of the prepared catalysts was done with Energy dispersive X-ray analysis, X-ray diffraction, BET surface area and pore volume measurements. The influence of different transition metals like chromium, molybdenum and tungsten on the surface acidic properties of titania is investigated in detail. Two independent methods have been used to study the surface acidity of these catalyst systems: temperature programmed desorption of ammonia which is a measure of total acidity and thermodesorption studies using 2,6-dimethyl pyridine which is a measure of Bronsted acidity. Cumene cracking reaction is carried out over the prepared systems for further characterizing the acidity of the prepared catalysts. Remarkable enhancement in the surface acidity is observed after transition metal incorporation. The catalytic activity of the prepared catalysts was tested towards the dehydrogenation of cyclohexane.

  14. Aluminosilicates with varying alumina-silica ratios: synthesis via a hybrid sol-gel route and structural characterisation.

    PubMed

    Nampi, Padmaja Parameswaran; Moothetty, Padmanabhan; Berry, Frank John; Mortimer, Michael; Warrier, Krishna Gopakumar

    2010-06-01

    Aluminosilicates with varying Al2O3:SiO2 molar ratios (3:1, 3:2, 3:3 and 3:4) have been synthesized using a hybrid sol-gel route using boehmite sol as the precursor for alumina and tetraethyl orthosilicate (TEOS) as the precursor for silica. The synthesis of boehmite sol from aluminium nitrate, and its use as the alumina precursor, is cost effective compared to alkoxide precursors. Structural aspects, including bonding and coordination, are studied in detail for samples calcined in the temperature range 400-1400 °C using both NMR and FTIR spectroscopy: the results are correlated with phase formation data (spinel and high temperature phases) obtained from XRD and thermal analysis. FTIR results show a broadening of peaks at 800 °C indicating a disordered distribution of octahedral sites caused by crosslinking between AlO6 octahedral and SiO4 tetrahedral units prior to the formation of mullite. (27)Al MAS NMR spectra are consistent with a progressive decrease in the number of AlO6 polyhedra with increasing temperature corresponding to Al in these units being forced to adopt a tetrahedral coordination due to the increasing presence of similarly coordinated Si species. XRD results confirm the formation of pure mullite at 1250 °C for a 3Al2O3:2SiO2 system. At 1400 °C, phase pure mullite is observed for all compositions except 3Al2O3:SiO2 where α-Al2O3 is the major phase with traces of mullite. The synthesis of aluminosilicates through a hybrid sol-gel route and the detailed insight into structural features gained from spectroscopic and diffraction techniques contributes further to the development of these materials in applications ranging from nanocatalysts to high-temperature ceramics.

  15. Synthesis of Yttria-Stabilized Zirconia Aerogels by a Non-Alkoxide Sol-Gel Route

    SciTech Connect

    Chervin, C N; Clapsaddle, B J; Chiu, H W; Gash, A E; Satcher, Jr., J H; Kauzlarich, S M

    2005-02-11

    Homogeneous, nanocrystalline powders of yttria-stabilized zirconia were prepared using a nonalkoxide sol-gel method. Monolithic gels, free of precipitation, were prepared by addition of propylene oxide to aqueous solutions of Zr{sup 4+} and Y{sup 3+} chlorides at room temperature. The gels were dried with supercritical CO{sub 2}(l), resulting in amorphous aerogels that crystallized into cubic stabilized ZrO{sub 2} following calcination at 500 C. The aerogels and resulting crystalline products were characterized using in-situ temperature profile X-ray diffraction, thermal analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and nitrogen adsorption/desorption analysis. TEM and N{sub 2} adsorption/desorption analysis of an aerogel indicated a porous network structure with a high surface area (409 m{sup 2}/g). The crystallized yttria-stabilized zirconia maintained high surface area (159 m{sup 2}/g) upon formation of homogeneous, nanoparticles ({approx}10 nm). Ionic conductivity at 1000 C of sintered YSZ (1500 C, 3 hours) prepared by this method, was 0.13 {+-} 0.02 {Omega}{sup -1} cm{sup -1}. Activation energies for the conduction processes from 1000-550 C and 550-400 C, were 0.95 {+-} 0.09 and 1.12 {+-} 0.05 eV, respectively. This is the first reported synthesis and characterization of yttria-stabilized zirconia via an aerogel precursor.

  16. Physical properties of NxTiO2 prepared by sol-gel route

    NASA Astrophysics Data System (ADS)

    Brahimi, Razika; Bessekhouad, Yassine; Trari, Mohamed

    2012-09-01

    The compounds NxTiO2(x=0, 0.05, 0.1, 0.2) with the anatase structure have been synthesized by Sol-Gel method using Tri-ethyl Amine as nitrogen source and their optical, electrical and electrochemical properties are investigated. The electrical conductivity and thermoelectric power are measured in the temperature rang 300-600 K. The samples exhibit p-type behavior in contrast to TiO2. The doped-samples exhibit two optical transitions (2.35≤Eh-Vis(eV)≤2.55; 1.97≤El-Vis (eV)≤2.06) directly allowed in the visible region, while only one transition is observed in UV region (EUV∼3.00 eV). Pure TiO2 shows direct band gap transition of 3.17 eV. The results confirm experimentally the calculations of Di. Valentin et al. [42]. The transitions Eh-Vis and El-Vis are attributed respectively to the promotion of electrons from the localized N 2p and π* N-O bond to the conduction band. In all cases, EUV is associated to the forbidden band energy. Though that the conductivity is generally improved by doping process, only N0.05TiO2 and N0.1TiO2 shows an enhanced mobility. The mechanism of conduction takes place by small polaron hopping. The band edge positions of NxTiO2 (x=0, 0.05, 0.1, 0.2) at room temperature is predicted from the obtained physical properties. This study proves experimentally the principal role of nitrogen in doping process and permits the electronic states localization associated with N-impurities in TiO2 anatase.

  17. Improved electrical characteristics of Pr-doped BiFeO3 ceramics prepared by sol-gel route

    NASA Astrophysics Data System (ADS)

    Madolappa, Shivanand; Kundu, Swarup; Bhimireddi, Rajasekhar; Varma, K. B. R.

    2016-06-01

    Ceramics of Bi1-x Pr x FeO3 (x = 0-0.1) were fabricated using the nanocrystalline powders obtained via sol-gel route. X-ray powder diffraction studies confirmed that these belonged to rhombohedral perovskite structure associated with R3c space group. The dielectric properties of the ceramic samples as a function of frequency (100 Hz-10 MHz) and temperature (30 °C-250 °C) were studied. The dielectric constant increased while the loss decreased with the increase of Pr content. Dielectric dispersion in these samples was found to be poly dispersive Debye type relaxation as confirmed by invoking Cole-Cole relation. Impedance spectroscopy was employed to determine the electrical parameters associated with the grain and grain boundaries. Grain and grain boundary resistances were found to decrease with the increase of temperature for all the samples under study. The activation energies for the dielectric relaxation were evaluated by electric modulus spectra and these increase with the increase of Pr dopant level. The frequency dependent conductivity at various temperatures demonstrated the involvement of correlated barrier hopping conduction mechanism. The electrical conduction in these ceramics was ascribed to long and short range migration of oxygen ion vacancies as demonstrated by temperature dependent ac conductivity studies.

  18. Tailored synthesis of ZnO:Er(III) nanosystems by a hybrid rf-sputtering/sol-gel route

    SciTech Connect

    Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Gasparotto, Alberto; Leonarduzzi, Daniele; Maragno, Cinzia; Tondello, Eugenio; Sada, Cinzia

    2006-09-15

    The rational design of rare-earth doped materials represents one of the major goals of current research in the field of optoelectronics. In this study, ZnO:Er(III) nanosystems were synthesized by means of a hybrid rf-sputtering/sol-gel (SG) route, consisting of the erbium (guest) rf-sputtering on porous zinc oxide xerogels (host) obtained by the SG method, followed by ex situ thermal treatments in air (300-600 deg. C, 1-5 h). Particular attention was focused on tailoring the erbium content and distribution in the resulting systems by optimization of the processing conditions. The structural, morphological, and compositional characteristics and their interplay with the synthesis procedure were investigated by glancing incidence x-ray diffraction, x-ray photoelectron spectroscopy, x-ray excited Auger electron spectroscopy, secondary ion mass spectrometry, UV-visible-near IR absorption spectroscopy, and atomic force microscopy. The obtained results highlight the advantages and versatility of the adopted preparation strategy in tailoring the amount and distribution of Er(III) species in high purity ZnO matrices, resulting in nanosystems endowed with compositional and morphological homogeneity at nanoscale level.

  19. Gravure-Printed Sol-Gels on Flexible Glass: A Scalable Route to Additively Patterned Transparent Conductors.

    PubMed

    Scheideler, William J; Jang, Jaewon; Ul Karim, Muhammed Ahosan; Kitsomboonloha, Rungrot; Zeumault, Andre; Subramanian, Vivek

    2015-06-17

    Gravure printing is an attractive technique for patterning high-resolution features (<5 μm) at high speeds (>1 m/s), but its electronic applications have largely been limited to depositing nanoparticle inks and polymer solutions on plastic. Here, we extend the scope of gravure to a new class of materials and on to new substrates by developing viscous sol-gel precursors for printing fine lines and films of leading transparent conducting oxides (TCOs) on flexible glass. We explore two strategies for controlling sol-gel rheology: tuning the precursor concentration and tuning the content of viscous stabilizing agents. The sol-gel chemistries studied yield printable inks with viscosities of 20-160 cP. The morphology of printed lines of antimony-doped tin oxide (ATO) and tin-doped indium oxide (ITO) is studied as a function of ink formulation for lines as narrow as 35 μm, showing that concentrated inks form thicker lines with smoother edge morphologies. The electrical and optical properties of printed TCOs are characterized as a function of ink formulation and printed film thickness. XRD studies were also performed to understand the dependence of electrical performance on ink composition. Printed ITO lines and films achieve sheet resistance (Rs) as low as 200 and 100 Ω/□, respectively (ρ≈2×10(-3) Ω-cm) for single layers. Similarly, ATO lines and films have Rs as low as 700 and 400 Ω/□ with ρ≈7×10(-3) Ω-cm. High visible range transparency is observed for ITO (86-88%) and ATO (86-89%). Finally, the influence of moderate bending stress on ATO films is investigated, showing the potential for this work to scale to roll-to-roll (R2R) systems.

  20. Structural investigation of nanomixed xSnO2-Al2O3 synthesized by sol-gel route

    NASA Astrophysics Data System (ADS)

    Kumar, C.; Mishra, N. K.; Kumar, A.; Bhatt, M.; Chaudhary, P.; Singh, R.

    2016-10-01

    Nanomixed SnO2-Al2O3 with variable composition has been synthesized by sol-gel technique using aluminium dichloride and stannous chloride as precursors. Synthesized nanocomposites have been characterized using various techniques such as X-ray diffraction (XRD), Fourier transform infrared, scanning electron microscopy and Energy-dispersive X-ray spectroscopy (EDX), Brunauer-Emmett-Teller (BET). XRD shows decrease in crystallinity as alumina component increases in following series of nanomixed oxides. The specific surface area calculated by Brunauer-Emmett-Teller (BET) method was about 191 m2/g and average pore diameter of 158 Å.

  1. Optical properties of undoped and Mg doped CuCrO{sub 2} powders synthesized by sol-gel route

    SciTech Connect

    Srinivasan, Radhakrishnan; Bolloju, Satish

    2014-01-28

    In this work, CuCrO{sub 2} was synthesized by sol-gel method using citric acid as a gelling agent. The different parameters like ratio of citric acid to metal ions, calcination temperature, and duration were studied. A green colored powder with particle size around 300 nm was formed at the calcination temperature of 800 °C for four hours duration. The increase in temperature has a profound impact on crystallite size and in turn effected the optical properties. Band gap of the obtained CuCrO{sub 2} has varied from 2.3 to 1.7 eV by increasing the temperature from 800 °C to 900 °C. Doping studies were performed by introducing Mg{sup 2+} ion to substitute Cr{sup 3+} in CuCrO{sub 2}. X-ray powder diffraction and SEM studies on 2% Mg doped samples indicated a clear formation of side phases. According to the X-ray powder patterns, the reflections from side phases were increasing with the increase in doping concentrations of Mg from 2 to 5%. The side phases were found to be MgCr{sub 2}O{sub 4} spinel and CuO. The band gap has decreased for doped samples in comparison to undoped one. In this paper, sol-gel synthesis and characterization by Xray powder diffraction, SEM studies and UV-Vis-Diffuse Reflectance spectra are presented.

  2. Structural, Optical and Magnetic Properties of Nickel-Silica Nanocomposite Prepared by a Sol-Gel Route

    NASA Astrophysics Data System (ADS)

    Saha, Mrinal; Soumya Mukherjee; Gayen, Arup; Siddhartha Mukherjee

    2015-10-01

    Nickel-silica nanocomposites have been synthesized by a sol-gel method using dextrose (C6H12O6) as the reducing agent. The dried gel is heat treated at 850 and 900 °C for 30 min in an inert atmosphere by N2 purging to obtain the composite material. The samples have been characterized by powder X-ray diffraction, field emission scanning electron microscopy, atomic force microscopy, transmission electron microscopy and selected area electron diffraction. Pure polycrystalline nickel granular particle has been found to form with face-centered cubic structure and is entrapped in amorphous silica matrix with particle sizes in between 10 and 30 nm and is almost spherical in shape. The strong ferromagnetic nature of Ni-SiO2 composite became evident from the M-H curve which is quite different from the bulk nickel. The band gap of the synthesized Ni-SiO2 nanocomposite is found to be 2.35 eV. The reported sol-gel technique is a convenient and effective method to prepare high purity nanopowders with uniform size distribution.

  3. Rh6G released from solid and nanoporous SiO2 spheres prepared by sol-gel route

    NASA Astrophysics Data System (ADS)

    García-Macedo, J. A.; Francisco S., P.; Franco, A.

    2015-10-01

    Porous silica nanoparticles are considering good systems for drug cargo and liquid separation. In this work we studied the release of rhodamine 6G (Rh6G) from solid and porous silica nanoparticles. Solid and porous SiO2 spheres were prepared by sol-gel method. Nanoporous channels were produced by using a surfactant that was removed by chemical procedure. Rh6G was incorporated into the channels by impregnation. The hexagonal structure of the pores was detected by XRD and confirmed by HRTEM micrographs. Rh6G released from the particles by stirring them in water at controlled speed was studied as function of time by photoluminescence. Released ratio was faster in the solid nanoparticles than in the porous ones. In the last case, a second release mechanism was observed. It was related with rhodamine coming out from the porous.

  4. Superconductivity in Ru-BASED Cuprate Ru(Sr1.5Ca0.5)PbCu2O8 Prepared by Sol-Gel Route

    NASA Astrophysics Data System (ADS)

    Yeoh, L. M.; Ahmad, M.; Abd-Shukor, R.

    Pb containing ruthenium-based superconducting cuprates Ru(Sr1.5Ca0.5)PbCu2O8 (Ru-1212 type) have been successfully synthesized through the sol-gel route. The optimum annealing temperature for the ruthenium-based cuprate superconductor was found to be 890°C. The crystal structure determined by X-ray powder diffraction method showed a single Ru-1212 type phase with tetragonal symmetry with lattice parameters a = b = 3.920 Å, and c = 11.76 Å. The Ru(Sr1.5Ca0.5)PbCu2O8 material showed onset temperature, Tc-onset at 35 K and zero resistant temperature, Tc-zero at 20 K. Pb together with the partial substitution of Sr with Ca lowered the formation temperature of the Ru-1212 type phase.

  5. Structural and cyclic volta metric investigations on BIPBVOX solid electrolyte synthesized by ethylene glycol-citric acid sol-gel route

    NASA Astrophysics Data System (ADS)

    Naqvi, Faria K.; Beg, Saba; Al-Areqi, Niyazi A. S.

    2016-05-01

    Samples of BIPBVOX.x (Bi2V1-xPbxO5.5-x/2) in the composition range 0.05 ≤ x ≤ 0.20 were prepared by ethylene glycol- citric acid sol-gel synthesis route. Structural investigations were carried out by X-ray diffraction, DTA. The highly conducting γ'- phase was effectively stabilized at room temperature for compositions with x ≥ 0.17. Cyclic voltammetric measurements showed reversible redox reactions of vanadium and irreversible redox reaction of Bi3+ in the BIPBVOX system during the first cathodic and anodic sweep. However, a higher stability against the reduction of Bi3+ to metallic bismuth was seen for x=0.20.

  6. Synthesis of CdS/CdSe core/shell ultra small nanostructures using new microwave assisted ultrasonic sol gel route

    SciTech Connect

    Goswami, Y. C. Kumar, Vijay; Sharma, Ranjana; Singh, Rajeev

    2014-04-24

    Core-shell CdS/CdSe nanostructures have been synthesized by new microwave assisted ultrasonic sol gel route. The solution was obtained by dissolving cadmium acetate and Thiourea in the molar ratio 1:1 in Triethlioamine. The solution was Ultrasonically irradiated by Ultrasonic crystal at 40 Hz for 3 hours at 70°C. The sol was kept for another 24 hours for gel formation. Selenium dioxide was used as a selenium source and added separately. The gel was spin coated on Quartz and Glass slides followed by microwave heat treatment. The samples were characterized by structural morphological and optical characterization. XRD studies confirm the zinc blende phase of the CdS nanoparticles. The mean nanocrystal sizes calculated using Scherrer equation is ∼1.2nm. Optical studies show the strong blue shift in the spectra due to very small size of the nanocrystals. TEM and HRTEM confirm the formation of core shell structures.

  7. Synthesis and Luminescent Properties of CaSnO3:Eu Nanopowder Prepared by a Sol-Gel Route.

    PubMed

    Fu, Xiaoyan; Zhao, Tuyuan; Zhang, Yan; Chen, Yibin; Zhang, Hongwu

    2016-04-01

    Luminescent properties of nanocrystalline CaSnO3:1%Eu have been investigated in order to develop novel red phosphors. The results indicate that high-quality nanoparticles with controlled stoichiometry and microstructure were prepared by a sol-gel method using citric acid and EDTA as complexes. There are two broad excitation bands located at 240 and 270 nm existing in the excitation spectrum in addition to the characteristic excitation peaks of Eu3+. Further investigations show that the excitation band located at 240 nm can be assigned to the host absorption while the Eu-O charge transfer is responsible for the 270 nm excitation band. These results indicate that the host can efficiently transfer energy to the Eu3+ ions. The more important is that since the symmetry of Eu3+ ions is lower, the pure red emission (5D9 --> 7F2 transition located at 618 nm) is predominant over all the emission. This means CaSnO3:Eu is a potential candidate for red luminescent materials. PMID:27451726

  8. Structural, optical and morphological analyses of pristine titanium di-oxide nanoparticles - Synthesized via sol-gel route

    NASA Astrophysics Data System (ADS)

    Praveen, P.; Viruthagiri, G.; Mugundan, S.; Shanmugam, N.

    2014-01-01

    Pure titanium di-oxide nanoparticles (TiO2) were synthesized by sol-gel technique at room temperature with appropriate reactants. The synthesis of anatase phase TiO2 nanoparticles was achieved by tetraisopropyl orthotitanate and 2-propanol as common starting materials and the product was annealed at 450 °C for 4 h. The synthesized product was characterized by X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR), UV-VIS-Diffuse reflectance spectroscopy (DRS), Photoluminescence (PL) spectroscopy and Scanning electron microscopy (SEM) with Energy dispersive X-ray (EDX) analysis. XRD pattern confirmed the crystalline nature and tetragonal structure of synthesized composition. Average grain size was determined from X-ray line broadening, using the Debye-Scherrer relation. The functional groups present in the sample were identified by FTIR spectroscopy. Diffuse reflectance measurement indicated an absorption band edge on UV-region. The allowed direct and indirect band gap energies, as well as the crystallite size of pure TiO2 nanoparticles are calculated from DRS analysis. The microstructure and elemental identification were done by SEM with EDX analysis.

  9. Structural, optical and morphological analyses of pristine titanium di-oxide nanoparticles--synthesized via sol-gel route.

    PubMed

    Praveen, P; Viruthagiri, G; Mugundan, S; Shanmugam, N

    2014-01-01

    Pure titanium di-oxide nanoparticles (TiO2) were synthesized by sol-gel technique at room temperature with appropriate reactants. The synthesis of anatase phase TiO2 nanoparticles was achieved by tetraisopropyl orthotitanate and 2-propanol as common starting materials and the product was annealed at 450 °C for 4 h. The synthesized product was characterized by X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR), UV-VIS-Diffuse reflectance spectroscopy (DRS), Photoluminescence (PL) spectroscopy and Scanning electron microscopy (SEM) with Energy dispersive X-ray (EDX) analysis. XRD pattern confirmed the crystalline nature and tetragonal structure of synthesized composition. Average grain size was determined from X-ray line broadening, using the Debye-Scherrer relation. The functional groups present in the sample were identified by FTIR spectroscopy. Diffuse reflectance measurement indicated an absorption band edge on UV-region. The allowed direct and indirect band gap energies, as well as the crystallite size of pure TiO2 nanoparticles are calculated from DRS analysis. The microstructure and elemental identification were done by SEM with EDX analysis.

  10. A New Route to Liposil Formation by an Interfacial Sol-Gel Process Confined by Lipid Bilayer.

    PubMed

    Shen, Shukun; Yang, Lu; Lu, Yaxing; Chen, Jian-Gang; Song, Shaofei; Hu, Daodao; Parikh, Atul

    2015-11-18

    We report a new and simple approach to prepare a class of silica-reinforced liposomes with hybrid core-shell nanostructures. The amphiphilic natural structure of lipids was exploited to sequester hydrophobic molecules, namely precursor TEOS and pyrene, in the hydrophobic midplane of liposomal bilayer assemblies in the aqueous phase. Subsequent interfacial hydrolysis of TEOS at the bilayer/water interface and ensuing condensation within the hydrophobic interstices of the lipid bilayer drives silica formation in situ, producing a novel class of silica-lipid hybrid liposils. Structural characterization by scanning- and transmission electron microscopy confirm that the liposils so generated preserve closed topologies and size-monodipersity of the parent lecithin liposomes, and DSC-TGA and XRD measurements provide evidence for the silica coating. Monitoring fluorescence measurements using embedded pyrene yield detailed information on microenvironment changes, which occur during sol-gel process and shed light on the structural evolution during silica formation. We envisage that liposils formed by this simple, new approach, exploiting the hydrophobic core of the lipid bilayer to spatially localize silica-forming precursors enables preparation of stable liposils exhibiting capacity for cargo encapsulation, bicompatibility, and fluorescence monitoring, more generally opening a window for construction of stable, functional hybrid materials. PMID:26197062

  11. Sol-gel synthesis and characterization of nanocrystalline (Bi0.5Na0.5)TiO3 powders from the poly vinyl alcohol evaporation route

    NASA Astrophysics Data System (ADS)

    Haitao, Liu; xiaohui, Wang; Longtu, Li

    2009-09-01

    Nanocrystalline pure perovskite phase bismuth sodium titanate (Bi0.5Na0.5)TiO3(BNT) powders have been prepared by a sol-gel method from the poly vinyl alcohol evaporation route, bismuth nitrate [Bi(NO3)3], tetra-butyl titanate [Ti(OC4H9)4] and sodium acetate(CH3COONa) were used as raw materials and poly vinyl alcohol(PVA) as the sol-gel forming solvent. Stoichiometric amounts of the individual raw materials were thoroughly mixed in accordance with the BNT composition to form the stock solution. The pH of the stock was adjusted to 1-3 by adding acetate. Aqueous solution of PVA[10%(w/v)] was then added to the cationic mixture with thorough stirring. The weight ratio of the cationic mixture to the PVA aqueous solution was maintained at 2:1. The resulting viscous liquid was then heated over a hot crucible up to form a fluffy dry gel. The fluffy dry gels were calcined at different temperatures and times and then cooled to room temperature naturally. The X-ray powder diffraction(XRD) patterns of the heat-treated powders were obtained using a Bruker D8 Advance X-ray diffractometer with Cu Kα radiation and nickel filter. Scanning electron microscope (SEM) studies of the NBT powders were performed using a JSM-6700F electron microscope. Phase-pure BNT powders were obtained at 550°C for 2-2.5h which is relatively lower calcination temperature than other reports. The BNT powders consists of phase-pure perovskite nanocrystals with an average size of 100-200nm.

  12. Crystallization behaviors and electric properties of (Pb0.8Ca0.2)TiO3 thin films prepared by a sol-gel route

    NASA Astrophysics Data System (ADS)

    Chi, Q. G.; Zhu, H. F.; Lin, J. Q.; Chen, C. T.; Wang, X.; Chen, Y.; Lei, Q. Q.

    2013-05-01

    The pure tetragonal perovskite (Pb0.8Ca0.2)TiO3 (PCT) thin films deposited on (1 1 1)Pt/Ti/SiO2/Si substrate were successfully achieved by a sol-gel route, and the influence of pyrolysis temperature on crystallization behaviors and electric properties of the PCT films was investigated. It was found that the film pyrolyzed at 450 °C could be crystallized at temperature as low as 450 °C, while the film pyrolyzed at 350 °C is amorphous under the same crystallization temperature. It was also found that the PCT films pyrolyzed at different temperatures could be fully crystallized when the crystallization temperature was raised to 600 °C, and compared to the film pyrolyzed at 350 °C, the film pyrolyzed at 450 °C exhibited higher (1 0 0) orientation and possessed enhanced electric properties (remanent polarization ∼19.5 μC/cm2, piezoelectric constant ∼125 pm/v, pyroelectric coefficient ∼310 μC/m2K).

  13. Effect of annealing on the structural and optical properties of TiO2 powder prepared by sol-gel route

    NASA Astrophysics Data System (ADS)

    Halder, Nilanjan; Misra, Kamakhya Prakash

    2016-05-01

    Using titanium isopropoxide as the precursor, Titanium dioxide (TiO2) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO2 samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increase with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO2 nano powder samples.

  14. A novel synthetic route for magnesium aluminate (MgAl2O4) nanoparticles using sol-gel auto combustion method and their photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Nassar, Mostafa Y.; Ahmed, Ibrahim S.; Samir, Ihab

    2014-10-01

    In this paper a novel and inexpensive route for the preparation of spinel magnesium aluminate nanoparticles (MgAl2O4) is proposed. Magnesium aluminate photocatalyst was synthesized via sol-gel auto combustion method using oxalic acid, urea, and citric acid fuels at 350 °C. Subsequently, the burnt samples were calcined at different temperatures. The pure spinel MgAl2O4 with average crystallite size 27.7, 14.6 and 15.65 nm was obtained at 800 °C calcinations using the aforementioned fuels, respectively. The obtained samples were characterized by powder X-ray diffraction, Fourier transform infrared, UV-Vis spectroscopy, transmission electron microscope, scanning electron microscope. The photo catalytic activity of MgAl2O4 product was studied by performing the decomposition of Reactive Red Me 4BL dye under UV illumination or sunlight irradiation. The dye considerably photocatalytically degraded by 90.0% and 95.45% under UV and sunlight irradiation, respectively, within ca. 5 h with pseudo first order rate constants of 5.85 × 10-3 and 8.38 × 10-3 min-1, respectively.

  15. 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

  16. 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.

  17. Structural and optical properties of ZnO: K synthesized by sol-gel auto-combustion route

    SciTech Connect

    Krithiga, R. Sankar, S.; Subhashree, G.; Bharathi, R. Niruban

    2015-06-24

    The structural and optical behavior of ZnO and ZnO doped with K synthesized by solution combustion route is reported in this article. The XRD patterns confirm the substitution of K atoms into ZnO lattice. There are no secondary peaks observed in the XRD patterns. The band gap of the K doped samples show a red shift on comparison with the bandgap of ZnO. The photoluminescence spectral study discloses the quenching behavior of UV emission and the aggrandizing blue emission when K content increases. The rich presence of defects is confirmed from the optical analysis and a practical mechanism, involving Zn{sub i} for the origin of the blue emission in ZnO is discussed here.

  18. The Microscopic Magnetic Properties of W-type Hexaferrite Powder Prepared by A Sol-Gel Route

    SciTech Connect

    Jotania, Rajshree; Chauhan, Chetna; Sharma, Pooja

    2010-12-01

    Magnetic particles of W-type barium-calcium hexaferrite (BaCa{sub 2}Fe{sub 16}O{sub 27}) have been synthesized using a Stearic acid gel route. The gel precursors were dried at 100 deg. C for 2 hrs and then calcinated at 650 deg. C, 750 deg. C, 850 deg. C and 950 deg. C for 4 hrs in a furnace and slowly cooled to room temperature in order to obtain barium-calcium hexaferrite particles. The microscopic magnetic properties of prepared samples studying using Moessbauer spectroscopy. Moessbauer spectra of all samples were recorded at room temperature. Mossbauer parameters like Isomer shift, Quadruple splitting etc. were calculated with respect to iron foil. Barium calcium hexaferrite samples heated at 650 deg. C, 750 deg. C, 850 deg. C show relaxation type Moessbauer spectra along with paramagnetic doublet. The intensity of paramagnetic doublet increases with temperature confirm the presence of ferrous ions in the samples, where as sample calcinated at 950 deg. C confirm the presence of ferrimagnetic phase with partial super paramagnetic nature of prepared hexaferrite sample.

  19. 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.

  20. Nanocrystal/sol-gel nanocomposites

    DOEpatents

    Klimov, Victor L.; Petruska, Melissa A.

    2010-05-25

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

  1. Structural, magnetic and Mössbauer studies of (BiFeO3)0.7-(SrFe12O19)0.3 nanocomposite prepared by a sol-gel route

    NASA Astrophysics Data System (ADS)

    Das, A.; Roychowdhury, A.; Pati, S. P.; Bandyopadhyay, S.; Das, D.

    2014-04-01

    The nanocomposite (BiFeO3)0.7-(SrFe12O19)0.3 has been prepared by a sol-gel route and characterized by XRD, TEM, TGA/DTA, dc magnetization and 57Fe Mössbauer spectroscopy. The hyperfine parameters obtained from Mössbauer spectroscopy indicate formation of pure hexaferrite phase of SrFe12O19 (SRF) in the nanocomposite (NC). The NC exhibits typical hysteresis loops with significantly altered magnetization parameters (saturation magnetization, coercivity and remnant magnetization) in comparison with that of the pristine SRF and BiFeO3 (BFO) nanoparticles (NPs). The ZFC-FC curves show a divergence in low temperature region which confirms the irreversible character of magnetization.

  2. 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.

  3. Sol-gel route of synthesis of nanoparticles of MgFe 2O 4 and XRD, FTIR and VSM study

    NASA Astrophysics Data System (ADS)

    Pradeep, A.; Priyadharsini, P.; Chandrasekaran, G.

    Nanoparticles of MgFe 2O 4 are synthesized using sol-gel autocombustion method. Structural studies are carried out using X-ray diffraction (XRD). The XRD pattern of MgFe 2O 4 provides information about single-phase formation of spinel structure with cubic symmetry. The grain size and lattice constant are obtained using XRD data. The cation distribution is also proposed theoretically. The change in site preference of cations in nano-MgFe 2O 4 is compared with its bulk counterpart. The structural morphology of the nanoparticles is studied using Scanning Electron Microscopy (SEM). Formation of spinel structure is conformed using Fourier transform infrared spectroscopy (FTIR), which also lends support for the cation distribution proposed using XRD data. The effect of nanoregime on parameters such as bond length, vibration frequency and force constant are discussed with the help of FTIR data. The M- H loop of MgFe 2O 4 has been traced using the Vibrating Sample Magnetometer (VSM) and magnetic parameters such as saturation magnetization ( MS), coercivity ( HC) and retentivity ( MR) are obtained from VSM data.

  4. A novel non-aqueous sol-gel route for the in situ synthesis of high loaded silica-rubber nanocomposites.

    PubMed

    Wahba, Laura; D'Arienzo, Massimiliano; Dirè, Sandra; Donetti, Raffaella; Hanel, Thomas; Morazzoni, Franca; Niederberger, Markus; Santo, Nadia; Tadiello, Luciano; Scotti, Roberto

    2014-04-01

    Silica-natural rubber nanocomposites were obtained through a novel non-aqueous in situ sol-gel synthesis, producing the amount of water necessary to induce the hydrolysis and condensation of a tetraethoxysilane precursor by esterification of formic acid with ethanol. The method allows the synthesis of low hydrophilic silica nanoparticles with ethoxy groups linked to the silica surface which enable the filler to be more dispersible in the hydrophobic rubber. Thus, high loaded silica composites (75 phr, parts per hundred rubber) were obtained without using any coupling agent. Transmission Electron Microscopy (TEM) showed that the silica nanoparticles are surrounded by rubber layers, which lower the direct interparticle contact in the filler-filler interaction. At the lowest silica loading (up to 30 phr) silica particles are isolated in rubber and only at a large amount of filler (>60 phr) the interparticle distances decrease and a continuous percolative network, connected by thin polymer films, forms throughout the matrix. The dynamic-mechanical properties confirm that the strong reinforcement of the rubber composites is related to the network formation at high loading. Both the improvement of the particle dispersion and the enhancement of the silica loading are peculiar to the non-aqueous synthesis approach, making the method potentially interesting for the production of high-loaded silica-polymer nanocomposites. PMID:24651692

  5. Structural, magnetic and hyperfine properties of single-phase SrFe12O19 nanoparticles prepared by a sol-gel route

    NASA Astrophysics Data System (ADS)

    Das, A.; Roychowdhury, A.; Pati, S. P.; Bandyopadhyay, S.; Das, D.

    2015-02-01

    Single-phase nanocrystalline strontium hexaferrite (SrFe12O19) powders have been synthesized by a sol-gel method and their structural, magnetic and hyperfine properties are discussed. The optimum annealing temperature of the as-prepared gel for formation of the single-phase SrFe12O19 structure has been found to be 800 °C. X-ray diffraction and Fourier transform infrared studies confirmed formation of the hexaferrite phase. The cation distribution at crystallographic inequivalent sites of the hexaferrite structure has been examined by 57Fe Mössbauer spectroscopy and found to be identical to that reported earlier. Single-phase SrFe12O19 nanoparticles (NPs) showed a magnetic hysteresis loop with high coercivity and saturation magnetization denoting an irreversible magnetization character. The temperature dependent magnetization measurements reveal a difference between the zero-field-cooled and field-cooled curves throughout the measurement range 5-300 K that is attributed to superparamagnetic relaxation of finer hexaferrite particles and disordered spins at the surface of the NPs. Both hyperfine and magnetic studies confirm that magnetic anisotropy plays a crucial role in hexaferrite NPs.

  6. Microstructures and phase evolution in YBa 2Cu 3O 7- x films grown on various substrates fabricated via a non-fluorine sol-gel route

    NASA Astrophysics Data System (ADS)

    Li, A. H.; Ionescu, M.; Liu, H. K.; Shi, D. L.; Wang, X. L.; Peng, X.; Collings, E. W.

    2005-10-01

    YBa2Cu3O7-x films were grown on polycrystalline Ag and single crystalline YSZ, SrTiO3, and MgO substrates using non-fluorine sol-gel and spin coating methods. The effects of heat treatment conditions on the phase evolution and microstructures were investigated using optical microscope, X-ray diffraction, and atomic force microscope. For Ag substrates, Y123 phase started to form at 750 °C and higher sintering temperatures improved the degree of (0 0 1) texture. Mirror-like surfaces without any cracks were achieved for sintering at 750-900 °C. However, voids were observed for films grown on the Ag substrates at temperatures higher than 810 °C and their size and density increased as the temperature increased. For the films grown on single crystal substrates sintered at 800 °C, numerous microcracks with large crack widths were observed, while cracking is less of a problem for films grown on Ag substrates. Epitaxial films without any cracks were achieved for films grown on single crystalline substrates under optimized conditions. Possible mechanism for the formation of cracks is discussed.

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

    PubMed

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

    2000-01-01

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

  8. Effect of Ni-Zr codoping on dielectric and magnetic properties of SrFe12O19 via sol-gel route

    NASA Astrophysics Data System (ADS)

    Kuruva, Praveena; Reddy Matli, Penchal; Mohammad, Bououdina; Reddigari, Sandhya; Katlakunta, Sadhana

    2015-05-01

    Nanocrystalline strontium hexaferrites [SrFe12-2x (Ni2+-Zr4+)xO19] nanoparticles were successfully synthesized by sol-gel process. For densification the powders were sintered at 950 °C/4 h. The sintered samples were characterized by X-ray diffraction (XRD), surface area measurement, and field emission scanning electron microscope (FESEM). The lattice parameter a is almost constant but c increased with x upto 0.8 and then decreased. The frequency dependent complex permittivity (ε‧ and ε″) and permeability (μ‧ and μ″) and magnetic properties such as saturation magnetization (Ms), coercive field (Hc) were studied. It is observed that saturation magnetization increased gradually from 57.82 emu/g to 67.2 emu/g as x increased from 0.2 to 0.4 and then decreased from 67.2 emu/g to 31.63 emu/g for x=1.0. In present study, x=0.4 shows high value of Ms 67.2 emu/g. The real part of permittivity (ε‧) remains constant upto a frequency 1 GHz and increases further with an increase of frequency, a resonance and anti-resonance peak was observed above 1 GHz for all the samples. In real part of permeability (μ‧) the relaxation frequency is observed above 1 GHz for all the samples and it is attributed to the domain wall motion. It is well known that the permeability for polycrystalline ferrites can be described as the superposition of two different magnetizing mechanisms: spin rotation and domain wall motion. These low coercive strontium hexaferrites are suitable for magnetic recording applications in hard disks, floppy disks, video tapes, etc.

  9. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

  11. Preparation of nanostructured La0.7Ca0.3-xBaxMnO3 ceramics by a combined sol-gel and spark plasma sintering route and resulting magnetocaloric properties

    NASA Astrophysics Data System (ADS)

    Ayadi, F.; Regaieg, Y.; Cheikhrouhou-Koubaa, W.; Koubaa, M.; Cheikhrouhou, A.; Lecoq, H.; Nowak, S.; Ammar, S.; Sicard, L.

    2015-05-01

    This work proposes an original, easy to achieve and inexpensive route to synthesize manganite ceramics for magnetic refrigeration, combining sol-gel chemistry to Spark Plasma Sintering (SPS). The target La0.7Ca0.3-xBaxMnO3 (x=0, 0.1, 0.2) compounds are obtained as single phases which crystallize in the orthorhombic structure (Pnma space group). SPS allows a quick sintering at a relatively low temperature (700 °C in this work) compared to the conventional solid state method (≥1100 °C), leading to densified ultrafine grained pellets (85% of compactness). Magnetic studies show that Ba substitution does not affect significantly the relative cooling power (RCP) of these manganites, while it increases their Curie temperature (TC) by several tens of degrees. Typically, RCP values ranging between 267 and 270 J/kg (for a magnetic field change of 5 T) and TC between 205 and 245 K were measured when x was increased from 0 to 0.2, respectively. These results combined to the fact that the synthesis route is economically advantageous makes the obtained ceramics interesting as active refrigerants for magnetic refrigeration technology below room temperature.

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

    SciTech Connect

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

    1992-03-01

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

  13. Nanostructured energetic materials using sol-gel methodologies

    SciTech Connect

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

    2000-09-27

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

  14. Sol-gel antireflective coating on plastics

    DOEpatents

    Ashley, Carol S.; Reed, Scott T.

    1990-01-01

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

  15. Sol-gel 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].

  16. 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.

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

    PubMed

    Zolkov, Chen; Avnir, David; Armon, Robert

    2009-02-01

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

  18. Sol/gel transition of chitosan solutions.

    PubMed

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

    2005-01-01

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

  19. Sol-gel entrapped cobalt complex

    SciTech Connect

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

    2003-03-15

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

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

    NASA Technical Reports Server (NTRS)

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

    2000-01-01

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

  1. Chemical modification of TiO2 by H2PO{4/-}/HPO{4/2-} anions using the sol-gel route with controlled precipitation and hydrolysis: enhancing thermal stability

    NASA Astrophysics Data System (ADS)

    Elghniji, Kais; Saad, Mohamed El Khames; Araissi, Manel; Elaloui, Elimame; Moussaoui, Younes

    2014-12-01

    Two titanium phosphate materials (T p P and T h P) have been successfully synthesized by sol-gel route with controlled precipitation and hydrolysis. The T p P material was obtained from the reaction between precipitated titania and phosphate buffer solution H2PO{4/-} /HPO{4/2-} (pH = 7.3). The T p P material was prepared through hydrolysis of titanium in the presence of H2PO{4/-}/HPO{4/2}. The probable state of the phosphate anions in titania framework and their effect on the anatase-to-rutile transformation were characterized by ICP-AES, DTA-TG, 31P NMR, FT-IR, and Raman analysis HRTEM/SEM. FT-IR and 31P NMR analyses of titanium phosphate T p P calcined at low temperature showed that the phosphate species existed not only as Ti-O-P in the bulk TiO2 but also as amorphous titanium phosphates, including bidentate Ti(HPO4)2 and monodentate Ti(H2PO4)4. Increased calcination temperature only gave an enrichment of bidentate structure on the titania surface. For the T p P material, H2PO{4/-}/HPO{4/2-} anions were introduced into the initial solution, before precipitation, what promoted their lattice localization. At high temperatures, all the phosphorus inside the bulk of TiO2 migrated to the surface. The Raman analysis of both samples showed that the bidentate phosphates increased the temperature of the anatase-to-rutile phase transformation to more than 1000 °C with the formation of well crystalline TiP2O7 phase. This phenomenon was more evident for T p P sample.

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

    NASA Astrophysics Data System (ADS)

    Hales, Matthew; Martens, Wayde; Steinberg, Theodore

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

  3. Sol-gel based biofuel cell architectures

    NASA Astrophysics Data System (ADS)

    Lim, James Robert

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

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Tailoring red-green-blue emission from Er3+, Eu3+ and Tb3+ doped Y2O3 nanocrystals produced via PVA-assisted sol-gel route

    NASA Astrophysics Data System (ADS)

    Sobral, G. A.; Gomes, M. A.; Avila, J. F. M.; Rodrigues, J. J.; Macedo, Z. S.; Hickmann, J. M.; Alencar, M. A. R. C.

    2016-11-01

    Y2O3 luminescent nanoparticles were synthesized via PVA-assisted sol-gel method and their structural and optical properties were investigated. Effects of rare earth (Er3+, Eu3+ and Tb3+) doping on luminescence properties of the produced nanophosphors have been investigated under NIR (800 nm) and UV (240-300 nm) excitation. Intense infrared to red and green emissions were observed and a weak blue upconverted luminescence was also detected. Moreover, it was observed that changing the doping ions, the color emitted by the samples could be modified and different combinations of UV excitation and doping produced effective white light emissions. The obtained results demonstrate that PVA-assisted sol-gel is an effective methodology for the synthesis of rare-earth doped Y2O3 nanophosphors.

  9. High specific surface area nickel mixed oxide powders LaNiO{sub 3} (perovskite) and NiCo{sub 2}O{sub 4} (spinel) via sol-gel type routes for oxygen electrocatalysis in alkaline media

    SciTech Connect

    El Baydi, M.; Chartier, P.; Koenig, J.F.; Poillerat, G.; Tiwari, S.K. |; Singh, R.N.; Rehspringer, J.L.

    1995-04-01

    A novel sol-gel process of preparation of oxide electrocatalysts is investigated to prepare Ni-containing mixed oxides LaNiO{sub 3} and NiCo{sub 2}O{sub 4} at moderate temperatures. High surface area (20-55 m{sup 2} g{sup {minus}1}) powders and high roughness electrodes (30-1500) were obtained. Apparent and real electrocatalytical activity are compared and discussed.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

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

    PubMed

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

    2001-10-01

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

  16. 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

  17. 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.

  18. Encapsulation of protein molecules in transparent porous silica matrices via an aqueous colloidal sol-gel process

    SciTech Connect

    Liu, D.M.; Chen, I.W.

    1999-12-10

    Encapsulation of several biologically important proteins, cytochrome c, catalase, myoglobin, and hemoglobin, into transparent porous silica matrices by an aqueous colloidal sol-gel process that requires no alcohol is reported. Optical characterization indicates a successful retention of protein conformation after encapsulation. The conformation retention is strongly correlated to both the rate of gelation and the subsequent drying speed. Using hemoglobin as a model protein, a higher colloidal solid concentration and a lower synthesis pH were found, both causing faster gelation, resulting in a better retention of conformation. Hemoglobin encapsulated in a thin film, which dries faster, also showed a better retention than in the bulk. This is attributed to the fact that when a protein is isolated, and especially when it is confined to a space close to its own dimensions, conformational changes are sterically hindered, hence the structural stability. Enzymatic activity of bovine liver catalase was also monitored and showed a remarkable improvement when encapsulated using the aqueous colloidal process, compared to using the conventional alkoxide-based process. Thus, the aqueous colloidal sol-gel process offers a promising alternative to the conventional sol-gel process for encapsulating biomolecules into transparent, porous matrices.

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

    NASA Astrophysics Data System (ADS)

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

    2001-10-01

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

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

    SciTech Connect

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

    2000-05-09

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

  1. Er3+-activated photonic structures fabricated by sol-gel and rf-sputtering techniques

    NASA Astrophysics Data System (ADS)

    Ferrari, M.; Alombert-Goget, G.; Armellini, C.; Berneschi, S.; Bhaktha, S. N. B.; Boulard, B.; Brenci, M.; Chiappini, A.; Chiasera, A.; Duverger-Arfuso, C.; Féron, P.; Gonçalves, R. R.; Jestin, Y.; Minati, L.; Moser, E.; Nunzi Conti, G.; Pelli, S.; Rao, D. N.; Retoux, R.; Righini, G. C.; Speranza, G.

    2009-05-01

    The realization of photonic structures operating at visible and near infrared frequencies is a highly attractive scientific and technological challenge. Since optical fiber innovation, a huge of activity has been performed leading to interesting results, such as optical waveguides and planar lightwave circuits, microphotonic devices, optical microcavities, nanowires, plasmonic structures, and photonic crystals. These systems have opened new possibilities in the field of both basic and applied physics, in a large area covering Information Communication Technologies, Health and Biology, Structural Engineering, and Environment Monitoring Systems. Several materials and techniques are employed to successfully fabricate photonic structures. Concerning materials, Er3+-activated silica-based glasses still play an important role, although recently interesting results have been published about fluoride glass-ceramic waveguides. As far as regards the fabrication methods sol-gel route and rf sputtering have proved to be versatile and reliable techniques. In this article we will present a review of some Er3+-activated photonic structures fabricated by sol gel route and rf sputtering deposition. In the discussion on the sol-gel approach we focus our attention on the silica-hafnia binary system presenting an overview concerning fabrication protocols and structural, optical and spectroscopic assessment of SiO2-HfO2 waveguides activated by Er3+ ions. In order to put in evidence the reliability and versatility of the sol-gel route for photonics applications four different confined structures are briefly presented: amorphous waveguides, coated microspheres, monolithic waveguide laser, and core-shell nanospheres. As examples of rf sputtering technique, we will discuss Er3+-activated silica-hafnia and silica-germania waveguides, the latter system allowing fabrication of integrated optics structures by UV photo-imprinting. Finally, two examples of photonic crystal structures, one

  2. 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.

  3. Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

    ERIC Educational Resources Information Center

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

    2010-01-01

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

  4. Schiff base mediated sol-gel polymerization

    SciTech Connect

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

    1996-12-31

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

  5. Sol-gel processing of energetic materials

    SciTech Connect

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

    1997-08-18

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

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

    SciTech Connect

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

    2009-02-01

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

  7. Solid-state NMR study of geopolymer prepared by sol-gel chemistry

    SciTech Connect

    Tsai, Yi-Ling; Hanna, John V.; Lee, Yuan-Ling; Smith, Mark E.; Chan, Jerry C.C.

    2010-12-15

    Geopolymers are a new class of materials formed by the condensation of aluminosilicates and silicates obtained from natural minerals or industrial wastes. In this work, the sol-gel method is used to synthesize precursor materials for the preparation of geopolymers. The geopolymer samples prepared by our synthetic route have been characterized by a series of physical techniques, including Fourier-transform infrared, X-ray diffraction, and multinuclear solid-state NMR. The results are very similar to those obtained for the geopolymers prepared from natural kaolinite. We believe that our synthetic approach can offer a good opportunity for the medical applications of geopolymer. -- Graphical abstract: Geopolymer prepared by the sol-gel route has the same spectroscopic properties as the sample prepared from the natural kaolinite. Display Omitted

  8. Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: Structural and optical studies by DRS, FT-IR, XRD, FESEM investigations

    NASA Astrophysics Data System (ADS)

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-01

    Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400 °C and 500 °C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm-1 can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm-1 are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide.

  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. Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: structural and optical studies by DRS, FT-IR, XRD, FESEM investigations.

    PubMed

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-25

    Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400°C and 500°C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm(-1) can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm(-1) are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide.

  11. Functionalized sol-gel coatings for optical applications.

    PubMed

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

    2007-09-01

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

  12. Soluble polymers in sol-gel silica

    NASA Astrophysics Data System (ADS)

    Beaudry, Christopher Laurent

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

  13. Structural properties and application in lithium cells of Li(Ni0.5Co0.5)1-yFeyO2 (0 ≤ y ≤ 0.25) prepared by sol-gel route: Doping optimization

    NASA Astrophysics Data System (ADS)

    Abdel-Ghany, A. E.; Hashem, A. M.; Elzahany, E. A.; Abuzeid, H. A.; Indris, S.; Nikolowski, K.; Ehrenberg, H.; Zaghib, K.; Mauger, A.; Julien, C. M.

    2016-07-01

    Layered Li(Co0.5Ni0.5)1-yFeyO2 (0.0 ≤ y ≤ 0.25) oxides were prepared by citric-acid assisted sol-gel method. Elemental and structural properties were investigated by energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman scattering (RS) and Mössbauer spectroscopy, and magnetometry. EDX images show a homogeneous distribution of Fe ions. XRD and RS spectroscopy reveal that the materials crystallize as a LiNiO2sbnd LiCoO2sbnd LiFeO2 solid solution with the typical rhombohedral α-NaFeO2 structure (R 3 bar m S.G.) up to y = 0.2 at which composition a secondary phase was observed. For y > 0.2 the XRD results show the appearance of the α-LiFeO2 phase with the cubic structure (Fm3m S.G.). The degree of cation mixing investigated by XRD analysis and magnetic measurements is z < 0.04, for y < 0.2. Electrochemical tests of Li(Co0.5Ni0.5)1-yFeyO2 (0.0 ≤ y ≤ 0.1) oxides in lithium cells show the influence of iron substitution. The best results have been obtained for the composition y(Fe) = 0.05, where the electrical conductivity is maximum. A specific capacity 32 mAh g-1 is maintained at 8C rate.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

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

    PubMed

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

    2015-01-01

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

  19. Mechanisms of silk fibroin sol-gel transitions.

    PubMed

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

    2006-11-01

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

  20. Crack formation during post-treatment of nano- and microfibres prepared by sol-gel technique.

    PubMed

    Tätte, T; Kolesnikova, A L; Hussainov, M; Talviste, R; Lõhmus, R; Romanov, A E; Hussainova, I; Part, M; Lõhmus, A

    2010-09-01

    We report on the method of TiO2 nano- and microfibres preparation and their cracking during processing and post-treatment. Nano- and microfibres were fabricated by drawing from viscous alkoxide based oligomeric concentrate precursors with the following exposure into an atmosphere of 30-50% humidity. The fibres microstructure was analyzed with TEM, solid state NMR, X-ray diffraction tools, and AFM. Experiments on crack formation in TiO2 microfibres proved that fibres with diameter larger than 10 micron are fractured for chosen post-treatment regimes. In theoretical considerations sol-gel produced and thermally treated microfibres are modeled as core/shell structures. It is suggested that the formation of fibres starts via solidification of liquid jet through the appearance of a rigid solid shell, which reveals tensile mechanical stresses because of material shrinkage. The effect of post-treatment is taken into account by additional densification of the fibre surface layer. The stress intensity factor K(I) is calculated for the model core/shell structures and the dependence of K(I) on the fibre diameter is demonstrated. The results of modeling qualitatively confirm experimental data of microfibre cracking above a certain threshold diameter.

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

    NASA Astrophysics Data System (ADS)

    Vinogradov, Vladimir V.; Avnir, David

    2015-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

    The sensitivities of metallophthalocyanine to vapor phase electron donors has gained significance in many areas and disciplines due to their sensing properties and ease of operation. In the present study the interaction mechanism of organic vapors in Copper Phthalocyanine (CuPc) sol-gel glass has been studied. The interaction mechanism is affected by many factors like morphology, electrical or optical properties of film. CuPc sol-gel glass has been synthesized using chemical route sol-gel method. Its structural characterization was conducted using XRD and the amorphous nature of the silicate glass was observed with characteristic α polymorph phase of CuPc at around 6.64˚ with 13.30Å interplanar spacing. The size of the particle as determined using Debbye Scherre's formula comes out around 15.5 nm. The presence of α phase of CuPc was confirmed using FTIR with the appearance of crystal parameter marker band at 787 cm-1. Apart from this A2u and Eu symmetry bands of CuPc have also been observed. The UV absorption spectrum of CuPc exhibits absorption peaks owing to π→ π* and n→ π* transitions. A blue shift in the prepared CuPc glass has been observed as compared to the dopant CuPc salt indicating increase of band gap. A split in B (Soret) band and Q band appears as observed with the help of Lorentzian fitting. CuPc sol gel glass has been exposed with chemical vapors of Methanol, Benzene and Bromine individually and the electrical measurements have been carried out. These measurements show the variation in conductivity and the interaction mechanism has been analyzed.

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

    SciTech Connect

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

    2015-05-15

    The sensitivities of metallophthalocyanine to vapor phase electron donors has gained significance in many areas and disciplines due to their sensing properties and ease of operation. In the present study the interaction mechanism of organic vapors in Copper Phthalocyanine (CuPc) sol-gel glass has been studied. The interaction mechanism is affected by many factors like morphology, electrical or optical properties of film. CuPc sol-gel glass has been synthesized using chemical route sol-gel method. Its structural characterization was conducted using XRD and the amorphous nature of the silicate glass was observed with characteristic α polymorph phase of CuPc at around 6.64° with 13.30Å interplanar spacing. The size of the particle as determined using Debbye Scherre’s formula comes out around 15.5 nm. The presence of α phase of CuPc was confirmed using FTIR with the appearance of crystal parameter marker band at 787 cm-1. Apart from this A2u and Eu symmetry bands of CuPc have also been observed. The UV absorption spectrum of CuPc exhibits absorption peaks owing to π→ π* and n→ π* transitions. A blue shift in the prepared CuPc glass has been observed as compared to the dopant CuPc salt indicating increase of band gap. A split in B (Soret) band and Q band appears as observed with the help of Lorentzian fitting. CuPc sol gel glass has been exposed with chemical vapors of Methanol, Benzene and Bromine individually and the electrical measurements have been carried out. These measurements show the variation in conductivity and the interaction mechanism has been analyzed.

  4. 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

  5. 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.

  6. 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.

  7. Passive and active sol-gel materials and devices

    NASA Astrophysics Data System (ADS)

    Andrews, Mark P.; Najafi, S. Iraj

    1997-07-01

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

  8. Investigations into the structural and down-shifting and up-conversion luminescence properties of Ba2Na1-3x Er x Nb5O15 (0 ≤ x ≤ 0.06) nanocrystalline phosphor synthesized via sol-gel route

    NASA Astrophysics Data System (ADS)

    Kundu, Swarup; Bhimireddi, Rajasekhar; Mishra, Kavita; Rai, S. B.; Varma, K. B. R.

    2015-10-01

    The present work deals with the structural and efficient down-shifting (DS) and up-conversion (UC) luminescence properties of erbium ion (Er3+) doped nanocrystalline barium sodium niobate (Ba2Na1-3x Er x Nb5O15, where x = 0, 0.02, 0.04 and 0.06) powders synthesized via novel citrate-based sol-gel route. The monophasic nature of the title compound was confirmed via x-ray powder diffraction followed by FT-IR studies. High-resolution transmission electron microscopy (HRTEM) facilitated the establishment of the nanocrystalline phase and the morphology of the crystallites. The Kubelka-Munk function, based on diffused reflectance studies and carried out on nano-sized crystallites, was employed to obtain the optical band-gap. The synthesized nanophosphor showed efficient DS/PL-photoluminescence and UC luminescence properties, which have not yet been reported so far in this material. The material emits intense DS green emission on excitation with 378 nm radiation. Interestingly, the material gives intense UC emission in the visible region dominated by green emission and relatively weak red emission on 976 nm excitation (NIR laser excitation). Such a dual-mode emitting nanophosphor could be very useful in display devices and for many other applications.

  9. 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.

  10. 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

  11. 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.

  12. 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.

  13. 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.

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

    SciTech Connect

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

    2011-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2008-08-01

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

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

    NASA Astrophysics Data System (ADS)

    Kaur, Rajvinder

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

  17. 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...

  18. 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.

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

    DOEpatents

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

    2000-01-01

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

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

    DOEpatents

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

    2002-11-26

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

  1. 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.

  2. A new approach to prepare nanoscopic rare earth metal fluorides: the fluorolytic sol-gel synthesis of ytterbium fluoride.

    PubMed

    Schmidt, L; Dimitrov, A; Kemnitz, E

    2014-06-25

    A new approach for the preparation of approx. 5 nm sized ytterbium fluoride nanoparticles based on the fluorolytic sol-gel route is reported. DLS, TEM, IR and XRD were used to characterize the particles as well as the aging behavior of the sols. Furthermore, a new Yb(III) complex was isolated from the precursor solution and characterized by X-ray single crystal structure determination.

  3. Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

    NASA Technical Reports Server (NTRS)

    Sibille, L.; Gavira-Gallardo, J. A.; Hourlier-Bahloul, D.

    2003-01-01

    Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SiO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2,7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil simular in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. The elemental composition and structure of the precursor molecules were characterized. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors.

  4. Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

    NASA Technical Reports Server (NTRS)

    Sibille, L.; Gavira-Gallardo, J. A.; Hourlier-Bahloul, D.

    2004-01-01

    Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil similar JSC-1 in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. Characterization of the precursor molecules and efforts to further concentrate and hydrolyze the products to obtain gel materials will be presented for evaluation as ceramic precursors.

  5. Sol-gel coating of lithium zinc ferrite powders

    SciTech Connect

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

    1991-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1994-10-01

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

  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. Tunable Optical Properties of Metal Nanoparticle Sol-Gel Composites

    NASA Technical Reports Server (NTRS)

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

    2001-01-01

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

  9. Polymer modified sol-gel materials for photochromic applications

    NASA Astrophysics Data System (ADS)

    Janik, Ryszard; Kucharski, Stanislaw

    2006-08-01

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

  10. Nanostructured Energetci Matreials with sol-gel Chemistry

    SciTech Connect

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

    2003-11-18

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

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

    NASA Astrophysics Data System (ADS)

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

    1999-09-01

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

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

    SciTech Connect

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

    2013-11-27

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

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

    SciTech Connect

    Hurd, A.J.

    1995-03-01

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

  14. Sol-Gel Thin Films for Plasmonic Gas Sensors

    PubMed Central

    Della Gaspera, Enrico; Martucci, Alessandro

    2015-01-01

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

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

    PubMed

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

    2005-01-01

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

  16. 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.

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

    PubMed

    Kaneko, Tsukasa; Iwata, Kazuki; Kobayashi, Makiko

    2015-09-01

    Piezoelectric films using sol-gel composites could be useful as ultrasonic transducers in various industrial fields. For sol-gel composite film fabrication, the spray coating technique has been used often because of its adaptability for various substrates. However, the spray technique requires multiple spray coating processes and heating processes and this is an issue of concern, especially for on-site fabrication in controlled areas. Stencil printing has been developed to solve this issue because this method can be used to fabricate thick sol-gel composite films with one coating process. In this study, PbTiO3 (PT)/Pb(Zr,Ti)O3 (PZT) films, PZT/PZT films, and Bi4Ti3O12 (BiT)/PZT films were fabricated by stencil printing, and PT/ PZT films were also fabricated using the spray technique. After fabrication, a thermal cycle test was performed for the samples to compare their ultrasonic performance. The sensitivity and signal-to-noise-ratio (SNR) of the ultrasonic response of PT/PZT fabricated by stencil printing were equivalent to those of PT/PZT fabricated by the spray technique, and better than those of other samples between room temperature and 300°C. Therefore, PT/PZT films fabricated by stencil printing could be a good candidate for nondestructive testing (NDT) ultrasonic transducers from room temperature to 300°C. PMID:26688872

  18. Sol-gel thin films for photonic application

    NASA Astrophysics Data System (ADS)

    Jasieniak, Jacek J.; Martucci, Alessandro

    2012-06-01

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

  19. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  1. Synthesis of phthalocyanine doped sol-gel materials

    NASA Technical Reports Server (NTRS)

    Dunn, Bruce

    1993-01-01

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

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

    DOEpatents

    Liu, Dean-Mo; Chen, I-Wei

    2001-01-01

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

  3. New insights in the structural and morphological properties of sol-gel deposited ZnO multilayer films

    NASA Astrophysics Data System (ADS)

    Demes, T.; Ternon, C.; Riassetto, D.; Roussel, H.; Rapenne, L.; Gélard, I.; Jimenez, C.; Stambouli, V.; Langlet, M.

    2016-08-01

    This study shows how the structural and morphological properties of sol-gel deposited ZnO films can be precisely tuned and selectively controlled. For that purpose, ZnO films have been deposited through a multilayer sol-gel route using solutions of zinc acetate dihydrate (ZAD) diluted in 1-butanol. The opto-geometrical, morphological, and structural properties of these films have been thoroughly studied in relation to the ZAD concentration in butanol, number of deposited single-layers, and heat-treatment conditions. On this basis, different physical processes occurring over the multilayer deposition procedure have been discussed to explain how the experimental parameters influence the film properties and enable to tune the grain size, texture coefficient, and surface coverage rate in a wide range of values. This work is a first step toward the optimized growth of ZnO nanowires on sol-gel films and their subsequent integration in 2D or 3D nanowire-based biosensors.

  4. Effect of chromophore-chromophore electrostatic interactions in the NLO response of functionalized organic-inorganic sol-gel materials

    NASA Astrophysics Data System (ADS)

    Reyes-Esqueda, J.; Darracq, B.; García-Macedo, J.; Canva, M.; Blanchard-Desce, M.; Chaput, F.; Lahlil, K.; Boilot, J. P.; Brun, A.; Lévy, Y.

    2001-10-01

    In the last years, important non-linear optical (NLO) results on sol-gel and polymeric materials have been reported, with values comparable to those found in crystals. These new materials contain push-pull chromophores either incorporated as guest in a high Tg polymeric matrix (doped polymers) or grafted onto the polymeric matrix. These systems present several advantages, however they require significant improvement at the molecular level—by designing optimized chromophores with very large molecular figure of merit, specific to each application targeted. Besides, it was recently stated in polymers that the chromophore-chromophore electrostatic interactions, which are dependent of chromophore concentration, have a strong effect into their NLO properties. This has not been explored at all in sol-gel systems. In this work, the sol-gel route was used to prepare hybrid organic-inorganic thin films with different NLO chromophores grafted into the skeleton matrix. Combining a molecular engineering strategy for getting a larger molecular figure of merit and by controlling the intermolecular dipole-dipole interactions through both: the tuning of the push-pull chromophore concentration and the control of tetraethoxysilane concentration, we have obtained a r33 coefficient around 15 pm/V at 633 nm for the classical DR1 azo-chromophore and a r33 around 50 pm/V at 831 nm for a new optimized chromophore structure.

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

    PubMed

    Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan

    2014-12-01

    Magnesium is one of the most critical elements in hard tissues regeneration and therefore causes speeding up the restoration of harmed bones, while high deterioration rate of magnesium in body fluid restricts it to be used as biodegradable implants. Alloying magnesium with some relatively nobler metals such as aluminium, zinc, rare earth elements, magnesium-bioceramics composites, and surface modification techniques are some of the routes to control magnesium corrosion rate. In this study AZ91 magnesium alloy had been coated by nanostructured hydroxyapatite via sol-gel dip coating and electrophoretical methods to survey the final barricade properties of the obtained coatings. In order to perform electrophoretic coating, powders were prepared by sol-gel method, and then the powders deposited on substrates utilizing direct current electricity. Zeta potentials of the electrophoresis suspensions were measured to determine a best mode for good quality coatings. Transmission Electron Microscopy (TEM), and Scanning Electron Microscopy (SEM) were used to confirm nanoscale dimension, and the uniformity of the nanostructured hydroxyapatite coating, respectively. Fourier Transform-Infrared and X-ray diffraction analysis were utilized for functional group and phase structure evaluation of the prepared coatings, correspondingly. Electrochemical corrosion tests were performed in SBF at 37±1 (°)C which revealed considerable increase in corrosion protection resistivity and corrosion current density for electrophoretic coated specimens versus sol-gel coated specimens. Results showed that both sol-gel and electrophoretical techniques seem to be suitable to coat magnesium alloys for biomedical applications but electrophoretic coating technique is a better choice due to the more homogeneity and more crystalline structure of the coating. PMID:25095258

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

  7. Green synthesis of magnetic chitosan nanocomposites by a new sol-gel auto-combustion method

    NASA Astrophysics Data System (ADS)

    Ansari, Fatemeh; Sobhani, Azam; Salavati-Niasari, Masoud

    2016-07-01

    The Fe2O3/CuFe2O4/chitosan nanocomposites have been successfully synthesized via a new sol-gel auto-combustion route. To prepare the nanocomposites, copper ferrite (CuFe2O4) and iron (II) oxide (Fe2O3) nanostructures were first prepared utilizing onion as a green reductant for the first time, and characterized by SEM, TEM, XRD, IR and VSM. Then chitosan was added into the nanostructures dispersed in water. Chitosan was used to functionalize and modify the nanostructures and also to improve surface properties. The nanocomposites were also characterized by several techniques including SEM, TEM, XRD, IR and VSM. The effects of amount of onion and chitosan on the morphology and particle size of nanocomposites were evaluated.

  8. Cerium-activated sol-gel silica glasses for radiation dosimetry in harsh environment

    NASA Astrophysics Data System (ADS)

    El Hamzaoui, Hicham; Capoen, Bruno; Helou, Nissrine Al; Bouwmans, Géraud; Ouerdane, Youcef; Boukenter, Aziz; Girard, Sylvain; Marcandella, Claude; Duhamel, Olivier; Chadeyron, Geneviève; Mahiou, Rachid; Bouazaoui, Mohamed

    2016-04-01

    Cerium-doped silica glass has been prepared for ionizing radiation dosimetry applications, using the sol-gel route and densification under different atmospheres. In comparison with the glass densified under air atmosphere, the one obtained after sintering the xerogel under helium gas presents improved optical properties, with an enhancement of the photoluminescence quantum yield up to 33%, which is attributed to a higher Ce3+ ions concentration. Such a glassy rod has been jacketed in a quartz tube and then drawn at high temperature to a cane, which has been used as active material in a fibered remote x-ray radiation dosimeter. The sample exhibited a reversible linear radioluminescence intensity response versus the dose rate up to 30 Gy s-1. These results confirm the potentialities of this material for in vivo or high rate dose remote dosimetry measurements.

  9. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

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

  11. 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.

  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. Sol-gel based sensor for selective formaldehyde determination.

    PubMed

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

    2010-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1995-09-01

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

  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. Nanostructured Energetic Materials with Sol-Gel Methods

    SciTech Connect

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

    2003-11-25

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

  17. Exact kinetics of the sol-gel transition

    NASA Astrophysics Data System (ADS)

    Lushnikov, A. A.

    2005-04-01

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

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

    NASA Astrophysics Data System (ADS)

    Barhoum, Moussa

    Single molecule trajectories of 1,1'-dioctadecyl-3,3,3'3'-tetramethylindocarbo - cyanine perchlorate (DiI) fluorophores diffusing on planar supported 1,2-dimyristoyl-snglycero- 3-phosphocholine (DMPC) lipid bilayers imaged through total internal reflection fluorescence (TIRF) microscopy at different temperatures are investigated. The spatial resolution limit for detecting molecular motion is evaluated by characterizing the apparent motion which arises from the limited signal-to-noise ratio (S/N) of imaged and simulated stationary DiI molecules. Statistical criteria for reliably distinguishing molecular motion from stationary molecules using F-test statistics, including the computation of local signal-to-noise ratios are then established and used for reliably detecting subdiffraction motion of DiI molecules on DMPC. The same single molecule tracking concept is used in investigating the temperature dependence of subdiffraction diffusional confinement of single Rhodamine 6G molecules in polymer brushes of poly (N-isopropylacrylamide), pNIPAAm, above and below its lower critical solution temperature (LCST) of 32°C. Reliably distinguishing subdiffraction molecular motion from stationary events is crucial in validating the application of single molecule tracking experiment in probing nanometersized hydrophobic environments of polymer structure. A versatile and rapid sol-gel technique for the fabrication of high quality one-dimensional photonic bandgap materials was developed. Silica/titania multilayer materials are fabricated by a sol-gel chemistry route combined with dip-coating onto planar or curved substrate. A shock-cooling step immediately following the thin film heat-treatment process is introduced. The versatility of this sol-gel method is demonstrated by the fabrication of various Bragg stack-type materials with fine-tuned optical properties. Measured optical properties show good agreement with theoretical simulations confirming the high quality of these sol-gel

  19. 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.

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

    PubMed

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

    2014-08-01

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

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

    PubMed

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

    2010-10-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2010-01-01

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

  3. 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.

  4. Sol-Gel Precursors for Ceramics from Minerals Simulating Soils from the Moon and Mars

    NASA Technical Reports Server (NTRS)

    Sibille, Laurent; Gavira-Gallardo, Jose-Antonio; Hourlier-Bahloul, Djamila

    2003-01-01

    Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report some preliminary results on the production of sol-gel precursors for ceramic products using mineral resources available in Martian or Lunar soil. The presence of SiO2, TiO2, and A12O3 in both Martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and Lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from Lunar and Martian simulant soils. Clear sol-gel precursors have been obtained by dissolution of silica from Lunar simulant soil in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Thermogravimetric Analysis and X-ray Photoelectron Spectroscopy were used to characterize the elemental composition and structure of the precursor molecules. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors. In the second set of experiments, we used the same starting materials to synthesize silicate esters in acidified alcohol mixtures. Preliminary results indicate the presence of silicon alkoxides in the product of distillation.

  5. 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.

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

    DOEpatents

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

    2006-06-06

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

  7. Polymer sol-gel composite inverse opal structures.

    PubMed

    Zhang, Xiaoran; Blanchard, G J

    2015-03-25

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

  8. Polymer sol-gel composite inverse opal structures.

    PubMed

    Zhang, Xiaoran; Blanchard, G J

    2015-03-25

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

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

    SciTech Connect

    Hong Xinlin; Zhang Gaoyong; Zhu Yinyan; Yang Hengquan

    2003-10-30

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

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

    NASA Astrophysics Data System (ADS)

    Kucharski, Stanisław; Janik, Ryszard

    2005-09-01

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

  11. Manufacture of Regularly Shaped Sol-Gel Pellets

    NASA Technical Reports Server (NTRS)

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

    2006-01-01

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

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

    PubMed

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

    2014-11-01

    Recently, silica nanoparticles (SNPs) have drawn widespread attention due to their applications in many emerging areas because of their tailorable morphology. During the last decade, remarkable efforts have been made on the investigations for novel processing methodologies to prepare SNPs, resulting in better control of the size, shape, porosity and significant improvements in the physio-chemical properties. A number of techniques available for preparing SNPs namely, flame spray pyrolysis, chemical vapour deposition, micro-emulsion, ball milling, sol-gel etc. have resulted, a number of publications. Among these, preparation by sol-gel has been the focus of research as the synthesis is straightforward, scalable and controllable. Therefore, this review focuses on the recent progress in the field of synthesis of SNPs exhibiting ordered mesoporous structure, their distribution pattern, morphological attributes and applications. The mesoporous silica nanoparticles (MSNPs) with good dispersion, varying morphology, narrow size distribution and homogeneous porous structure have been successfully prepared using organic and inorganic templates. The soft template assisted synthesis using surfactants for obtaining desirable shapes, pores, morphology and mechanisms proposed has been reviewed. Apart from single template, double and mixed surfactants, electrolytes, polymers etc. as templates have also been intensively discussed. The influence of reaction conditions such as temperature, pH, concentration of reagents, drying techniques, solvents, precursor, aging time etc. have also been deliberated. These MSNPs are suitable for a variety of applications viz., in the drug delivery systems, high performance liquid chromatography (HPLC), biosensors, cosmetics as well as construction materials. The applications of these SNPs have also been briefly summarized. PMID:25466691

  13. Mayenite Synthesized Using the Citrate Sol-Gel Method

    SciTech Connect

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

    2014-01-01

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

  14. Sol-Gel Glass Holographic Light-Shaping Diffusers

    NASA Technical Reports Server (NTRS)

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

    2005-01-01

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

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

    PubMed

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

    2012-03-18

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

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

    PubMed

    Radin, Shula; Chen, Tiffany; Ducheyne, Paul

    2009-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2006-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

  20. /dopamine films prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  1. Sol-gel template synthesis of semiconductor nanostructures

    SciTech Connect

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

    1997-03-01

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

  2. 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.

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

    PubMed

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

    2009-06-15

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

  4. Molecular receptors in metal oxide sol-gel materials prepared via molecular imprinting

    DOEpatents

    Sasaki, Darryl Y.; Brinker, C. Jeffrey; Ashley, Carol S.; Daitch, Charles E.; Shea, Kenneth J.; Rush, Daniel J.

    2000-01-01

    A method is provided for molecularly imprinting the surface of a sol-gel material, by forming a solution comprised of a sol-gel material, a solvent, an imprinting molecule, and a functionalizing siloxane monomer of the form Si(OR).sub.3-n X.sub.n, wherein n is an integer between zero and three and X is a functional group capable of reacting with the imprinting molecule, evaporating the solvent, and removing the imprinting molecule to form the molecularly imprinted metal oxide sol-gel material. The use of metal oxide sol-gels allows the material porosity, pore size, density, surface area, hardness, electrostatic charge, polarity, optical density, and surface hydrophobicity to be tailored and be employed as sensors and in catalytic and separations operations.

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

    NASA Astrophysics Data System (ADS)

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

    2012-09-01

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

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

    NASA Technical Reports Server (NTRS)

    Kamiya, K.; Yoko, T.; Sakka, S.

    1987-01-01

    An investigation is carried out on the types of siloxane polymers produced in the course of the hydrolysis of silicon tetraethoxide, as well as the preparation of oxide glasses from metal alkoxides by the sol-gel method.

  7. Enhanced piezoelectric performance of composite sol-gel thick films evaluated using piezoresponse force microscopy.

    PubMed

    Liu, Yuanming; Lam, Kwok Ho; Kirk Shung, K; Li, Jiangyu; Zhou, Qifa

    2013-05-14

    Conventional composite sol-gel method has been modified to enhance the piezoelectric performance of ceramic thick films. Lead zirconate titanate (PZT) and lead magnesium niobate-lead titanate (PMN-PT) thick films were fabricated using the modified sol-gel method for ultrasonic transducer applications. In this work, piezoresponse force microscopy was employed to evaluate the piezoelectric characteristics of PZT and PMN-PT composite sol-gel thick films. The images of the piezoelectric response and the strain-electric field hysteresis loop behavior were measured. The effective piezoelectric coefficient (d33,eff) of the films was determined from the measured loop data. It was found that the effective local piezoelectric coefficient of both PZT and PMN-PT composite films is comparable to that of their bulk ceramics. The promising results suggest that the modified composite sol-gel method is a promising way to prepare the high-quality, crack-free ceramic thick films. PMID:23798771

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

    PubMed

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

    2011-02-21

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

  9. Sol-gel hybrid materials for aerospace applications: Chemical characterization and comparative investigation of the magnetic properties

    NASA Astrophysics Data System (ADS)

    Catauro, Michelina; Mozzati, Maria Cristina; Bollino, Flavia

    2015-12-01

    In the material science field, weightless conditions can be successfully used to understand the relationship between manufacturing process, structure and properties of the obtained materials. Aerogels with controlled microstructure could be obtained by sol-gel methods in microgravity environment, simulated using magnetic levitation if they are diamagnetic. In the present work, a sol-gel route was used to synthesize class I, organic-inorganic nanocomposite materials. Two different formulations were prepared: the former consisted in a SiO2 matrix in which different percentages of polyethylene glycol (PEG) were incorporated, the latter was a ZrO2 matrix entrapping different amounts of poly (ε-caprolactone) (PCL). Fourier Transform Infrared Spectroscopy (FT-IR) detected that the organic and the inorganic components in both the formulation interact by means of hydrogen bonds. X-ray diffraction (XRD) analysis highlighted the amorphous nature of the synthesized materials and Scanning Electron Microscope (SEM) showed that they have homogeneous morphology and are nanocomposites. Superconducting Quantum Interference Device (SQUID) magnetometry confirmed the expected diamagnetic character of those hybrid systems. The obtained results were compared to those achieved in previous studies regarding the influence of the polymer amount on the magnetic properties of SiO2/PCL and ZiO2/PEG hybrids, in order to understand how the diamagnetic susceptibility is influenced by variation of both the inorganic matrix and organic component.

  10. Vapor-Diffusion-Controlled Sol-Gel Synthesis of Flaky Lithium Vanadium Oxide and Its Electrochemical Behavior

    SciTech Connect

    Zhang, Hong-Li; Neilson, James R.; Morse, Daniel E.

    2010-10-28

    Effectively modifying an existing synthesis method for materials can prove as useful as developing a new one. In this work, we revisited a conventional sol-gel synthesis of lithium vanadium oxide, a promising electrode material for rechargeable lithium batteries. Employing a kinetically controlled, vapor diffusion strategy (in which ammonia vapor was slowly diffused into the solution), we modified the conventional method to obtain a thin, flaky, lithium vanadium oxide with an average thickness of ~120 nm. In comparison, material prepared by the conventional sol-gel route (in which aqueous ammonia was dropwise added to the solution) exhibited an agglomeration of irregular particles with a typical size of ~10 μm. When evaluated as cathode material for rechargeable lithium batteries, this flaky material displayed a stable, reversible capacity of ~250 and ~115 mAh/g at discharge rates of 0.1 C and 2 C, respectively, considerably better than the agglomerated sample. The reasons for this improved performance were investigated by evaluating the electrochemical reaction kinetics, morphological and structural stability using cyclic voltammetry, scanning electron microscopy, and X-ray diffraction.

  11. Preparation and antioxidant capacity of element selenium nanoparticles sol-gel compounds.

    PubMed

    Bai, Yan; Qin, Biyin; Zhou, Yanhui; Wang, Yudong; Wang, Zi; Zheng, Wenjie

    2011-06-01

    This paper reported the preparation and antioxidant capacities of element selenium nanoparticles (nanoSe(0))-ascorbic acid (Vc) sol and nanSe(0)/Vc/selenocystine (SeCys) sol-gel compounds. NanoSe(0)-Vc sol was prepared by reduction of selenious dioxide (SeO2) with Vc. In the nanoSe(0)-Vc sol, highly concentrated Vc was also used as a modifier to modulate the diameter of Se(0) nanoparticles in the liquid phase. Then excellent nanoSe(0) sol-gel compounds were obtained by adding SeCys into the nanoSe(0)-Vc sol. The structure of the nanoSe(0)/Vc/SeCys sol-gel compounds was defined, which was constructed via C-Se, Se-H and O=C-Se valences and by interaction between SeCys and Vc via peptide bonds, esterification and dehydration. The antioxidant capacities of the nanoSe(0)-Vc sol and the nanoSe(0)Vc/SeCys sol-gel compounds were estimated by oxygen radical absorption capacity (ORAC) assay. The nanoSe(0)/Vc/SeCys sol-gel compounds possessed a strong antioxidant capacity due to forming the perfect three-dimensional (3D) frameworks structure. The results suggested that the nanoSe(0)-Vc sol and the nanoSe(0)Vc/SeCys sol-gel compounds might be potential medicine, especially antioxidant.

  12. Robust aptamer sol-gel solid phase microextraction of very polar adenosine from human plasma.

    PubMed

    Mu, Li; Hu, Xiangang; Wen, Jianping; Zhou, Qixing

    2013-03-01

    Conventional solid phase microextraction (SPME) has a limited capacity to extract very polar analytes, such as adenosine. To solve this problem, aptamer conjugating sol-gel methodology was coupled with an SPME fiber. According to the authors' knowledge, this is the first reported use of aptamer SPME. The fiber of aptamer sol-gel SPME with a mesoporous structure has high porosity, large surface area, and small water contact angle. Rather than employing direct entrapment, covalent immobilization was the dominant method of aptamer loading in sol-gel. Aptamer sol-gel fiber captured a specified analyte from among the analog molecules, thereby, exhibiting an excellent selective property. Compared with commercial SPME fibers, this aptamer fiber was suitable for extracting adenosine, presenting an extraction efficiency higher than 20-fold. The values of repeatability and reproducibility expressed by relative standard deviation were low (9.4%). Interestingly, the sol-gel network enhanced the resistance of aptamer SPME to both nuclease and nonspecific proteins. Furthermore, the aptamer sol-gel fiber was applied in human plasma with LOQ 1.5 μg/L, which is an acceptable level. This fiber also demonstrates durability and regeneration over 20-cycles without significant loss of efficiency. Given the various targets (from metal ions to biomacromolecules and cells) of aptamers, this methodology will extend the multi-domain applications of SPME.

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

    PubMed

    Allhusen, John S; Conboy, John C

    2013-11-27

    RuO2 conductive thin films were synthesized using the sol-gel method and deposited onto transparent insulating substrates. The optical transmission, film thickness, surface morphology and composition, resistivity, and spectroelectrochemical performance have been characterized. The optical transmission values of these films ranged from 70 to 89% in the visible region and from 56 to 88% in the infrared region. Resistivity values of the RuO2 sol-gel films varied from 1.02 × 10(-3) to 1.13 Ω cm and are highly dependent on the initial solution concentration of RuO2 in the sol-gel. The RuO2 sol-gel films were used as electrodes for the electrochemical oxidation and reduction of ferrocenemethanol. The electrochemical behavior of our novel RuO2 sol-gel films was compared to that of a standard platinum disk electrode and showed no appreciable differences in the half-wave potential (E1/2). The mechanical and chemical stability of the coatings was tested by physical abrasion and exposure to highly acidic, oxidizing Piranha solution. Repeated exposure to these extreme conditions did not result in any appreciable decline in electrochemical performance. Finally, the use of the novel RuO2 sol-gel conductive and transparent films was demonstrated in a spectroelectrochemistry experiment in which the oxidation and reduction of ferrocenemethanol was monitored via UV-vis spectroscopy as the applied potential was cycled.

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

    PubMed

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

    2016-03-01

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

  15. Synthesis and Characterization of Sol-Gel Prepared Silver Nanoparticles

    NASA Astrophysics Data System (ADS)

    Ahlawat, Dharamvir Singh; Kumari, Rekha; Rachna; Yadav, Indu

    2014-03-01

    Silver nanoparticles (SNPs) have been successfully prepared using sol-gel method by annealing the sample at 550°C for 30 min. The SNPs were not confirmed by X-ray diffraction (XRD) analysis when the annealing temperature was considered at 450°C. They were also not confirmed without calcination of the sample. The physical mechanism of silver clusters formation in the densified silica matrix with respect to thermal treatment has been understood. The presence of silver metal in the silica matrix was confirmed by XRD analysis and TEM image of the samples. The average size of nanoparticles dispersed in silica matrix was determined as 10.2 nm by the XRD technique. The synthesized nanocomposites were also characterized by UV-Visible spectroscopy with a peak in the absorption spectra at around 375 nm. The distribution of particle size has been reported here in the range from 8 nm to 25 nm by TEM observations of the sample prepared at 550°C. The spherically smaller size (≈10 nm) SNPs have reported the surface plasmons resonance (SPR) peak less than or near to 400 nm due to blue-shifting and effect of local refractive index. Without annealing the silica samples the absorption spectra does not show any peak around 375 nm. The FTIR spectroscopy of the three types of samples prepared at different temperatures (room temperature, 450°C and 550°C) has also been reported. This spectra have provided the identification of different chemical groups in the prepared samples. It has been predicted that the size of SNPs by XRD, UV-Visible and TEM results have agreed well with each other. It may be concluded that formation of SNPs is a function of annealing temperature.

  16. Large-area sol-gel highly-reflective coatings processed by the dipping technique

    SciTech Connect

    Belleville, P.; Pegon, P.

    1997-12-01

    The Centre d`Etudes de Limeil-Valenton is currently involved in a project which consists of the construction of a 2 MJ/500TW (351-nm) pulsed Nd:glass laser devoted to Inertial Confinement Fusion (ICF) research. With 240 laser beams, the proposed megajoule-class laser conceptual design necessitates 44-cm x 2 44-cm x 6-cm cavity-end mirrors (1053-nm) representing more than 50-m{sup 2} of coated area. These dielectric mirrors are made of quaterwave stacks of SiO{sub 2} and ZrO{sub 2}-PVP (PolyVinylPyrrolidone) and are prepared from colloidal suspensions (sols) using the sol-gel route. After a sustained search effort. we have prepared (SiO{sub 2}/ZrO{sub 2}-PVP){sup 10} mirrored coatings with up to 99% reflection at 1053-nm and for different incidence use. Adequate laser-conditioned damage thresholds ranging 14 - 15 J/cm{sup 2} at 1053-nm wavelength and with 3-ns pulse duration were achieved. Large-area mirrors with good coating uniformity and weak edge-effect were produced by dip-coating at room temperature and atmospheric pressure.

  17. Glass-based confined structures fabricated by sol-gel and radio frequency sputtering

    NASA Astrophysics Data System (ADS)

    Chiappini, Andrea; Armellini, Cristina; Carpentiero, Alessandro; Vasilchenko, Iustyna; Lukowiak, Anna; Ristić, Davor; Varas, Stefano; Normani, Simone; Mazzola, Maurizio; Chiasera, Alessandro

    2014-07-01

    Some of the main results obtained in the field of glass-based photonic crystal (PC) systems using complementary techniques, such as radio frequency (RF) sputtering and sol-gel route, are presented. Initially, rare earth-activated one-dimensional PCs fabricated by RF-sputtering technique will be discussed, specifically the cavity is constituted by an Er-doped SiO active layer inserted between two Bragg reflectors consisting of 10 pairs of SiO2/TiO2 layers. Moreover, from near infrared, transmittance and variable angle reflectance spectra have verified the presence of a stop band from 1500 to 2000 nm with a cavity resonance centered at 1749 nm at 0 deg and quality factor of 890. In the second case, a composite system based on polystyrene colloidal nanoparticles assembled and embedded in an elastomeric matrix will be presented in detail. This system has been designed as a structure that displays an iridescent green color that can be attributed to the PC effect. This feature has been exploited to create a chemical sensor; in fact optical measurements have evidenced that this system presents a different optical response as a function of the solvent applied on the surface, showing: (1) high sensitivity, (2) fast response, and (3) reversibility of the signal change.

  18. Antibacterial modification of an injectable, biodegradable, non-cytotoxic block copolymer-based physical gel with body temperature-stimulated sol-gel transition and controlled drug release.

    PubMed

    Wang, Xiaowen; Hu, Huawen; Wang, Wenyi; Lee, Ka I; Gao, Chang; He, Liang; Wang, Yuanfeng; Lai, Chuilin; Fei, Bin; Xin, John H

    2016-07-01

    Biomaterials are being extensively used in various biomedical fields; however, they are readily infected with microorganisms, thus posing a serious threat to the public health care. We herein presented a facile route to the antibacterial modification of an important A-B-A type biomaterial using poly (ethylene glycol) methyl ether (mPEG)- poly(ε-caprolactone) (PCL)-mPEG as a typical model. Inexpensive, commercial bis(2-hydroxyethyl) methylammonium chloride (DMA) was adopted as an antibacterial unit. The effective synthesis of the antibacterial copolymer mPEG-PCL-∼∼∼-PCL-mPEG (where ∼∼∼ denotes the segment with DMA units) was well confirmed by FTIR and (1)H NMR spectra. At an appropriate modification extent, the DMA unit could render the copolymer mPEG-PCL-∼∼∼-PCL-mPEG highly antibacterial, but did not largely alter its fascinating intrinsic properties including the thermosensitivity (e.g., the body temperature-induced sol-gel transition), non-cytotoxicity, and controlled drug release. A detailed study on the sol-gel-sol transition behavior of different copolymers showed that an appropriate extent of modification with DMA retained a sol-gel-sol transition, despite the fact that a too high extent caused a loss of sol-gel-sol transition. The hydrophilic and hydrophobic balance between mPEG and PCL was most likely broken upon a high extent of quaternization due to a large disturbance effect of DMA units at a large quantity (as evidenced by the heavily depressed PCL segment crystallinity), and thus the micelle aggregation mechanism for the gel formation could not work anymore, along with the loss of the thermosensitivity. The work presented here is highly expected to be generalized for synthesis of various block copolymers with immunity to microorganisms. Light may also be shed on understanding the phase transition behavior of various multiblock copolymers.

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

    PubMed

    Regina, Viduthalai Rasheedkhan; Søhoel, Helmer; Lokanathan, Arcot Raghupathi; Bischoff, Claus; Kingshott, Peter; Revsbech, Niels Peter; Meyer, Rikke Louise

    2012-11-01

    Enzymes with antifouling properties are of great interest in developing nontoxic antifouling coatings. A bottleneck in developing enzyme-based antifouling coatings is to immobilize the enzyme in a suitable coating matrix without compromising its activity and stability. Entrapment of enzymes in ceramics using the sol-gel method is known to have several advantages over other immobilization methods. The sol-gel method can be used to make robust coatings, and the aim of this study was to explore if sol-gel technology can be used to develop robust coatings harboring active enzymes for antifouling applications. We successfully entrapped a protease, subtilisin (Savinase, Novozymes), in a ceramic coating using a sol-gel method. The sol-gel formulation, when coated on a stainless steel surface, adhered strongly and cured at room temperature in less than 8 h. The resultant coating was smoother and less hydrophobic than stainless steel. Changes in the coating's surface structure, thickness and chemistry indicate that the coating undergoes gradual erosion in aqueous medium, which results in release of subtilisin. Subtilisin activity in the coating increased initially, and then gradually decreased. After 9 months, 13% of the initial enzyme activity remained. Compared to stainless steel, the sol-gel-coated surfaces with active subtilisin were able to reduce bacterial attachment of both Gram positive and Gram negative bacteria by 2 orders of magnitude. Together, our results demonstrate that the sol-gel method is a promising coating technology for entrapping active enzymes, presenting an interesting avenue for enzyme-based antifouling solutions.

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

    PubMed Central

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

    2008-01-01

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

  1. Growth of epitaxial LaAlO{sub 3} and CeO{sub 2} films using sol-gel precursors

    SciTech Connect

    Shoup, S.S.; Paranthaman, M.; Beach, D.B.

    1996-04-01

    LaAlO{sub 3} and CeO{sub 2} films have been successfully grown using sol-gel precursors. LaAlO{sub 3} precursor solution has been prepared from a metal alkoxide route and spun-cast on a SrTiO{sub 3} (100) single crystal to yield an epitaxial film following pyrolysis at 800{degrees}C in a rapid thermal annealer. A CeO{sub 2} precursor solution has been made using both an aqueous and an alkoxide route.

  2. Quasi-one-dimensional nanostructured cobalt (Co) intercalated vanadium oxide (V{sub 2}O{sub 5}): Peroxovanadate sol gel synthesis and structural study

    SciTech Connect

    Langie da Silva, Douglas; Moreira, Eduardo Ceretta; Dias, Fábio Teixeira; Neves Vieira, Valdemar das; Brandt, Iuri Stefani; Cas Viegas, Alexandre da; Pasa, André Avelino

    2015-01-15

    Nanostructured cobalt vanadium oxide (V{sub 2}O{sub 5}) xerogels spread onto crystalline Si substrates were synthesized via peroxovanadate sol gel route. The resulting products were characterized by distinct experimental techniques. The surface morphology and the nanostructure of xerogels correlate with Co concentration. The decrease of the structural coherence length is followed by the formation of a loose network of nanopores when the concentration of intercalated species was greater than 4 at% of Co. The efficiency of the synthesis route also drops with the increase of Co concentration. The interaction between the Co(OH{sub 2}){sub 6}{sup 2+} cations and the (H{sub 2}V{sub 10}O{sub 28}){sup 4−} anions during the synthesis was suggested as a possible explanation for the incomplete condensation of the V{sub 2}O{sub 5} gel. Finally the experimental results points for the intercalation of Co between the bilayers of the V{sub 2}O{sub 5}. In this scenario two possible preferential occupation sites for the metallic atoms in the framework of the xerogel were proposed. - Graphical abstract: Quasi-one-dimensional nanostructured cobalt (Co) intercalated vanadium oxide (V{sub 2}O{sub 5}) nanoribbons synthesized by peroxovanadate sol gel route. - Highlights: • Nanostructured cobalt V{sub 2}O{sub 5} gel spread onto c{sub S}i were synthesized via peroxovanadate sol gel route. • The micro and nanostructure correlates with the cobalt content. • The efficiency of the synthesis route shows to be also dependent of Co content. • The experimental results points for the intercalation of Co between the bilayers of the V{sub 2}O{sub 5} xerogel.

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

    PubMed

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

    2004-02-01

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

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

    PubMed

    Greer, Andrew I M; Lim, Teoh S; Brydone, Alistair S; Gadegaard, Nikolaj

    2016-01-01

    Sol-gel processing is an attractive method for large-scale surface coating due to its facile and inexpensive preparation, even with the inclusion of precision nanotopographies. These are desirable traits for metal orthopaedic prostheses where ceramic coatings are known to be osteoinductive and the effects may be amplified through nanotexturing. However there are a few concerns associated with the application of sol-gel technology to orthopaedics. Primarily, the annealing stage required to transform the sol-gel into a ceramic may compromise the physical integrity of the underlying metal. Secondly, loose particles on medical implants can be carcinogenic and cause inflammation so the coating needs to be strongly bonded to the implant. These concerns are addressed in this paper. Titanium, the dominant material for orthopaedics at present, is examined before and after sol-gel processing for changes in hardness and flexural modulus. Wear resistance, bending and pull tests are also performed to evaluate the ceramic coating. The findings suggest that sol-gel coatings will be compatible with titanium implants for an optimum temperature of 500 °C.

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

    PubMed

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

    2016-09-20

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

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

    PubMed

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

    2004-02-01

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

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

    PubMed

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

    2011-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1997-09-01

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

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

    PubMed

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

    2016-09-20

    The impact of fictive temperature (Tf) on the evolution of point defects and optical attenuation in non-doped and Er3+-doped sol-gel silica glasses was studied and compared to Suprasil F300 and Infrasil 301 glasses before and after γ-irradiation. To this aim, sol-gel optical fiber preforms have been fabricated by the densification of erbium salt-soaked nanoporous silica xerogels through the polymeric sol-gel technique. These γ-irradiated fiber preforms have been characterized by FTIR, UV-vis-NIR absorption spectroscopy, electron paramagnetic resonance, and photoluminescence measurements. We showed that a decrease in the glass fictive temperature leads to a decrease in the glass disorder and strained bonds. This mainly results in a lower defect generation rate and thus less radiation-induced attenuation in the UV-vis range. Furthermore, it was found that γ-radiation "hardness" is higher in Er3+-doped sol-gel silica compared to un-doped sol-gel silica and standard synthetic silica glasses. The present work demonstrates an effective strategy to improve the radiation resistance of optical fiber preforms and glasses through glass fictive temperature reduction. PMID:27661569

  10. Ionic conductivity of Bi{sub 2}Ni{sub x}V{sub 1−x}O{sub 5.5−3x/2} (0.1 ≤ x ≤ 0.2) oxides prepared by a low temperature sol-gel route

    SciTech Connect

    Rusli, Rolan; Patah, Aep Prijamboedi, Bambang Ismunandar; Abrahams, Isaac

    2014-03-24

    Solid oxides fuel cells (SOFCs) is one technology that could contribute toward future sustainable energy. One of the most important components of an SOFC is the electrolyte, which must have high ionic conductivity. Cation substitution of vanadium in Bi{sub 4}V{sub 2}O{sub 11} yields a family of fast oxide ion conducting solids known collectively as the BIMEVOXes (bismuth metal vanadium oxide), which have the potential to be applied as electrolytes in SOFCs. The purpose of this work is to study the effect of Ni concentration, when used as a dopant, on the ionic conductivity of Bi{sub 2}Ni{sub x}V{sub 1−x}O{sub 5.5−3x/2} (BINIVOX) oxides (0.1 ≤ x ≤ 0.2) when prepared by a sol gel method. The gels were calcined at 600 °C for 24 h to produce pure BINIVOX. These oxides were found to exhibit the γ-phase structure with tetragonal symmetry in space group I4/mmm. Ionic conductivity of BINIVOX at 300 °C were 6.9 × 10{sup −3} S cm{sup −1}, 1.2 × 10{sup −3} S cm{sup −1}, and 8.2 × 10{sup −4} S cm{sup −1}, for x = 0.1; 0.15; and 0.2; respectively; and at 600 °C were 1.1 × 10{sup −1} S cm{sup −1}, 5.3 × 10{sup −2} S cm{sup −1}, and 2.8 ×10{sup −2} S cm{sup −1}, for x = 0.1; 0.15; and 0.2; respectively.

  11. Synthesis of TiO(2) (Anatase) by Sol-Gel Process Performed in Metal Chlorides Saturated Aqueous Solutions.

    PubMed

    de Farias, Robson Fernandes

    2001-07-15

    Titania powders were synthesized by a sol-gel process using titanium tetrabutoxide as a precursor. The syntheses were performed in water or in saturated aqueous solutions of KCl, CaCl(2), NiCl(2), CoCl(2), and MnCl(2). It is demonstrated, by X-ray diffraction patterns of the synthesized powders that the samples obtained in saturated aqueous solutions of metal chlorides are crystalline (anatase phase) with some minor amount of brookite phase, whereas the sample synthesized in water is amorphous in nature. Thus, it is shown that the anatase phase can be obtained independently on any previous or further treatment of the synthesized powder, such as hydrothermal or heat treatment, providing a new, simple, quick, and inexpensive route to synthesize anatase powders. Copyright 2001 Academic Press.

  12. Recycling of chemicals from alkaline waste generated during preparation of UO 3 microspheres by sol-gel process

    NASA Astrophysics Data System (ADS)

    Kumar, Ashok; Vittal Rao, T. V.; Mukerjee, S. K.; Vaidya, V. N.

    2006-05-01

    Internal gelation process, one of the sol-gel processes for nuclear fuel fabrication, offers many advantages over conventional powder pellet route. However, one of the limitation of the process is generation of large volume of alkaline liquid waste containing hexamethylenetetramine, urea, ammonium nitrate, ammonium hydroxide etc. Presence of ammonium nitrate with hexamethylenetetramine and urea presents a fire hazard which prevents direct disposal of the waste as well as its recycle by evaporation. The paper describes the studies carried out to suitably process the waste. Nitrate was removed from the waste by passing through Dowex 1 × 4 anion exchange resin in OH - form. 1.0 M NaOH was used to regenerate the resin. The nitrate-free waste was further treated to recover and recycle hexamethylenetetramine, urea and ammonium hydroxide for preparation of UO 3 microspheres. The quality of the microspheres obtained was satisfactory. An optimized flow sheet for processing of the waste solution has been suggested.

  13. 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.

  14. Preparation and characterization of indium tin oxide films by sol-gel method

    NASA Astrophysics Data System (ADS)

    Ciuciumis, Alina; Cernica, Ileana

    2007-05-01

    Sol-gel technology is a relatively simple and cheap process to deposit oxides under thin film form out of a sol. The experiments were developed in order to obtain nanomaterials by sol-gel method; nanomaterials that mixed with resin and additives can be deposited in thin and uniform films by spraying on different lignocellulosic composite surfaces. This method assures a functional finishing of the nanomaterials. These films are transparent and the surfaces are flat with no cracks. The influence of substrate type, morphology of the films and of the substrates before and after deposition was studied by means of optical microscopy, scanning electron microscopy (SEM) and atomic force microscopy (AFM). The sol-gel deposit on the lignocellulosic composite substrates lowered the sorption rates of water and water vapours.

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

    SciTech Connect

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

    2006-11-20

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-10-01

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

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

    PubMed

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

    2000-11-01

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

  18. 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.

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

    NASA Astrophysics Data System (ADS)

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

    1998-02-01

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

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

    NASA Technical Reports Server (NTRS)

    Mukherjee, S. P.; Holman, R. A.

    1981-01-01

    Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process referred to here is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation. The use of gels offers several advantages such as high purity and lower melting times and temperatures. The sol-gel process is studied for utilization in the preparation of multicomponent ultrapure glass batches for subsequent containerless melting of the batches in space to prepare glass blanks for optical waveguides.

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

    NASA Astrophysics Data System (ADS)

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

    2010-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2010-06-01

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

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

    SciTech Connect

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

    1996-08-01

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

  4. 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.

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

    SciTech Connect

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

    1992-11-03

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

  6. Novel Sol-Gel Based Pt Nanocluster Catalysts for Propane Dehydrogenation

    SciTech Connect

    Boespflug, Elaine; Kawola, Jeffrey S.; Martino, Anthony; Sault, Allen G.

    1999-08-09

    We report propane dehydrogenation behavior of catalysts prepared using two novel synthesis strategies that combine inverse micelle Pt nanocluster technology with silica and alumina sol-gel processing. Unlike some other sol-gel catalyst preparations. Pt particles in these catalysts are not encapsulated in the support structure and the entire Pt particle surface is accessible for reaction. Turnover frequencies (TOF) for these catalysts are comparable to those obtained over Pt catalysts prepared by traditional techniques such as impregnation, yet the resistance to deactivation by carbon poisoning is much greater in our catalysts. The deactivation behavior is more typical of traditionally prepared PtSn catalysts than of pure Pt catalysts.

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

    PubMed Central

    2013-01-01

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

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

    NASA Technical Reports Server (NTRS)

    Stiegman, Albert E.

    1995-01-01

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

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

    DOEpatents

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

    2016-09-27

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

  10. Transparent poly(vinyl acetate)-silica gels by a sol-gel process

    NASA Astrophysics Data System (ADS)

    Wojcik, Anna B.; Klein, Lisa C.

    1993-12-01

    Rod shaped silica-poly(vinyl acetate) (PVAc) gels have been prepared by a sol gel process. In situ polymerization of tetraethoxysilane (TEOS) was accomplished in the presence of low molecular weight PVAc by dissolving various amounts of PVAc in a mixture of TEOS, ethanol, water and hydrochloric acid (HCl). Gelation of this mixture was carried out between room temperature and slightly above. Silica-PVAc rods recovered from cylindrical molds were homogeneous and transparent. Gels with weight percents of PVAc ranging from 2% to 50% were prepared. Silica-PVAc gels have higher flexure strengths, less brittle character and improved water durability in comparison with pure sol- gel silica.

  11. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    SciTech Connect

    Figus, Cristiana Quochi, Francesco Piana, Giacomo; Saba, Michele; Mura, Andrea; Bongiovanni, Giovanni; Artizzu, Flavia; Mercuri, Maria Laura; Serpe, Angela; Deplano, Paola

    2014-10-21

    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ{sub 4}) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ{sub 4} are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution.

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

    NASA Astrophysics Data System (ADS)

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

    2013-11-01

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

  13. A comparative synthesis and physicochemical characterizations of Ni/Al2O3-MgO nanocatalyst via sequential impregnation and sol-gel methods used for CO2 reforming of methane.

    PubMed

    Aghamohammadi, Sogand; Haghighi, Mohammad; Karimipour, Samira

    2013-07-01

    Carbon dioxide reforming of methane is an interesting route for synthesis gas production especially over nano-sized catalysts. The present research deals with catalyst development for dry reforming of methane with the aim of reaching the most stable catalyst. Effect of preparation method, one of the most significant variables, on the properties of the catalysts was taken in to account. The Ni/Al2O3-MgO catalysts were prepared via sol-gel and sequential impregnation methods and characterized with XRD, FESEM, EDAX, BET and FTIR techniques. The reforming reactions were carried out using different feed ratios, gas hourly space velocities (GHSV) and reaction temperatures to identify the influence of operational variables. FESEM images indicate uniform particle size distribution for the sample synthesized with sol-gel method. It has been found that the sol-gel method has the potential to improve catalyst desired properties especially metal surface enrichment resulting in catalytic performance enhancement. The highest yield of products was obtained at 850 degrees C for both of the catalysts. During the 10 h stability test, CH4 and CO2 conversions gained higher values in the case of sol-gel made catalyst compared to impregnated one.

  14. Silica/quercetin sol-gel hybrids as antioxidant dental implant materials

    NASA Astrophysics Data System (ADS)

    Catauro, Michelina; Papale, Ferdinando; Bollino, Flavia; Piccolella, Simona; Marciano, Sabina; Nocera, Paola; Pacifico, Severina

    2015-06-01

    The development of biomaterials with intrinsic antioxidant properties could represent a valuable strategy for preventing the onset of peri-implant diseases. In this context, quercetin, a naturally occurring flavonoid, has been entrapped at different weight percentages in a silica-based inorganic material by a sol-gel route. The establishment of hydrogen bond interactions between the flavonol and the solid matrix was ascertained by Fourier transform infrared spectroscopy. This technique also evidenced changes in the stretching frequencies of the quercetin dienonic moiety, suggesting that the formation of a secondary product occurs. Scanning electron microscopy was applied to detect the morphology of the synthesized materials. Their bioactivity was shown by the formation of a hydroxyapatite layer on sample surface soaked in a fluid that simulates the composition of human blood plasma. When the potential release of flavonol was determined by liquid chromatography coupled with ultraviolet and electrospray ionization tandem mass spectrometry techniques, the eluates displayed a retention time that was 0.5 min less than quercetin. Collision-activated dissociation mass spectrometry and untraviolet-visible spectroscopy were in accordance with the release of a quercetin derivative. The antiradical properties of the investigated systems were evaluated by DPPH and ABTS methods, whereas the 2,7-dichlorofluorescein diacetate assay highlighted their ability to inhibit the H2O2-induced intracellular production of reactive oxygen species in NIH-3T3 mouse fibroblast cells. Data obtained, along with data gathered from the MTT cytotoxicity test, revealed that the materials that entrapped the highest amount of quercetin showed notable antioxidant effectiveness.

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

    PubMed

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

    2014-02-18

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

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

    PubMed

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

    2014-02-18

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

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

    EPA Science Inventory

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

  18. Electrochemical and In Vitro Behavior of Nanostructure Sol-Gel Coated 316L Stainless Steel Incorporated with Rosemary Extract

    NASA Astrophysics Data System (ADS)

    Motalebi, Abolfazl; Nasr-Esfahani, Mojtaba

    2013-06-01

    The corrosion resistance of AISI 316L stainless steel for biomedical applications, was significantly enhanced by means of hybrid organic-inorganic sol-gel thin films deposited by spin-coating. Thin films of less than 100 nm with different hybrid characters were obtained by incorporating rosemary extract as green corrosion inhibitor. The morphology, composition, and adhesion of hybrid sol-gel coatings have been examined by SEM, EDX, and pull-off test, respectively. Addition of high additive concentrations (0.1%) did not disorganize the sol-gel network. Direct pull-off test recorded a mean coating-substrate bonding strength larger than 21.2 MPa for the hybrid sol-gel coating. The effect of rosemary extract, with various added concentrations from 0.012 to 0.1%, on the anticorrosion properties of sol-gel films have been characterized by electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization tests in simulated body fluid (SBF) solution and has been compared to the bare metal. Rosemary extract additions (0.05%) have significantly increased the corrosion protection of the sol-gel thin film to higher than 90%. The in vitro bioactivity of prepared films indicates that hydroxyapatite nuclei can form and grow on the surface of the doped sol-gel thin films. The present study shows that due to their excellent anticorrosion properties, bioactivity and bonding strength to substrate, doped sol-gel thin films are practical hybrid films in biomedical applications.

  19. Increasing the activity and enantioselectivity of lipases by sol-gel immobilization: further advancements of practical interest.

    PubMed

    Tielmann, Patrick; Kierkels, Hans; Zonta, Albin; Ilie, Adriana; Reetz, Manfred T

    2014-06-21

    The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of the sol-gel approach.

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

    PubMed

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

    2015-01-01

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

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

    PubMed

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

    2015-01-01

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

  2. Effectiveness of silica based Sol-gel microencapsulation Method for odorants and flavours leading to sustainable Environment

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

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

    PubMed Central

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

    2015-01-01

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

  4. 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

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

    PubMed

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

    2013-05-21

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

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

    PubMed

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

    2013-06-01

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

  7. 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.

  8. 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.

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

    NASA Astrophysics Data System (ADS)

    MacKenzie, John D.; Ulrich, Donald R.

    1992-03-01

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

  10. Foldable and Cytocompatible Sol-gel TiO2 Photonics

    PubMed Central

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

    2015-01-01

    Integrated photonics provides a miniaturized and potentially implantable platform to manipulate and enhance the interactions between light and biological molecules or tissues in in-vitro and in-vivo settings, and is thus being increasingly adopted in a wide cross-section of biomedical applications ranging from disease diagnosis to optogenetic neuromodulation. However, the mechanical rigidity of substrates traditionally used for photonic integration is fundamentally incompatible with soft biological tissues. Cytotoxicity of materials and chemicals used in photonic device processing imposes another constraint towards these biophotonic applications. Here we present thin film TiO2 as a viable material for biocompatible and flexible integrated photonics. Amorphous TiO2 films were deposited using a low temperature (<250 °C) sol-gel process fully compatible with monolithic integration on plastic substrates. High-index-contrast flexible optical waveguides and resonators were fabricated using the sol-gel TiO2 material, and resonator quality factors up to 20,000 were measured. Following a multi-neutral-axis mechanical design, these devices exhibit remarkable mechanical flexibility, and can sustain repeated folding without compromising their optical performance. Finally, we validated the low cytotoxicity of the sol-gel TiO2 devices through in-vitro cell culture tests. These results demonstrate the potential of sol-gel TiO2 as a promising material platform for novel biophotonic devices. PMID:26344823

  11. Foldable and Cytocompatible Sol-gel TiO2 Photonics.

    PubMed

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

    2015-09-07

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

  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. Foldable and Cytocompatible Sol-gel TiO2 Photonics

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

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

    DOEpatents

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

    2000-01-01

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

  15. Auto-organisation of hybrid organic-inorganic materials prepared by sol-gel process.

    PubMed

    Boury, Bruno; Corriu, Robert J P

    2002-04-21

    Silica-based hybrid organic-inorganic materials prepared by sol-gel chemistry exhibit chemical and physical properties revealing their anisotropic organisation. Besides the opportunities that this phenomenon opens for the preparation of new materials, it also provides arguments to the chemist looking for a better comprehension and control of the organisation of solids.

  16. A Sol-Gel-Modified Poly(methyl methacrylate) Electrophoresis Microchip with a Hydrophilic Channel Wall

    SciTech Connect

    Chen, Gang; Xu, Xuejiao; Lin, Yuehe; Wang, Joseph

    2007-07-27

    A sol-gel method was employed to fabricate a poly(methyl methacrylate) (PMMA) electrophoresis microchip that contains a hydrophilic channel wall. To fabricate such a device, tetraethoxysilane (TEOS) was injected into the PMMA channel and was allowed to diffuse into the surface layer for 24 h. After removing the excess TEOS, the channel was filled with an acidic solution for 3 h. Subsequently, the channel was flushed with water and was pretreated in an oven to obtain a sol-gel-modified PMMA microchip. The water contact angle for the sol-gel-modified PMMA was 27.4° compared with 66.3° for the pure PMMA. In addition, the electro-osmotic flow increased from 2.13×10-4 cm2 V-1 s-1 for the native-PMMA channel to 4.86×10-4 cm2 V-1 s-1 for the modified one. The analytical performance of the sol-gel-modified PMMA microchip was demonstrated for the electrophoretic separation of several purines, coupled with amperometric detection. The separation efficiency of uric acid increased to 74 882.3 m-1 compared with 14 730.5 m-1 for native-PMMA microchips. The result of this simple modification is a significant improvement in the performance of PMMA for microchip electrophoresis and microfluidic applications.

  17. Investigation of optical properties of anthocyanin doped into sol-gel based matrix

    NASA Astrophysics Data System (ADS)

    Hashim, Hasrina; Abdul Aziz, Nik Mohd Azmi Nik; Isnin, Aishah

    2012-06-01

    Anthocyanin dye was extracted from petal of Hibiscus rosasinensis (Bunga Raya) and doped into sol-gel based matrix to investigate an effect of pH change on its optical properties. Sol-gel matrix based on Vinyl triethoxysilene (VTES) as a precursor was prepared through Sol-gel process at pH 7. The sol was doped with 0.1% of Anthocyanin and the same amount of dye was also dissolved in ethanol as a comparative sample. Hydrochloric Acid, HCl and Tetramethylammonium Hydroxide, TMAH were used to change the pH value by adding them at various concentrations into each sample. The emission spectra and chemical structures of the samples were measured by Spectrofluorometer and Fourier Transform Infrared (FTIR) respectively. When excited at 410 nm, two emission peaks at about 492 and 574 nm were observed for Anthocyanin in acidic environment both in ethanol and VTES sol. In base environment however, only Anthocyanin dissolved in ethanol produced emission peak with a single peak at about 539 nm. The sensitivity of Anthocyanin dye toward pH changes in VTES open a possibility to use it as sensing element in which sol-gel based matrix are known to have higher mechanical strength and thermal stability.

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

    SciTech Connect

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

    2007-03-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

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

    PubMed Central

    2011-01-01

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

  1. Sol-gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

    NASA Astrophysics Data System (ADS)

    Kareiva, Simonas; Klimavicius, Vytautas; Momot, Aleksandr; Kausteklis, Jonas; Prichodko, Aleksandra; Dagys, Laurynas; Ivanauskas, Feliksas; Sakirzanovas, Simas; Balevicius, Vytautas; Kareiva, Aivaras

    2016-09-01

    Aqueous sol-gel chemistry route based on ammonium-hydrogen phosphate as the phosphorus precursor, calcium acetate monohydrate as source of calcium ions, and 1,2-ethylendiaminetetraacetic acid (EDTA), or 1,2-diaminocyclohexanetetracetic acid (DCTA), or tartaric acid (TA), or ethylene glycol (EG), or glycerol (GL) as complexing agents have been used to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, CHAp). The phase transformations, composition, and structural changes in the polycrystalline samples were studied by infrared spectroscopy (FTIR), X-ray powder diffraction analysis (XRD), and scanning electron microscopy (SEM). The local short-range (nano- and mezo-) scale effects in CHAp were studied using solid-state NMR spectroscopy. The spatial 3D data from the SEM images of CHAp samples obtained by TA, EG and GL sol-gel routes were recovered for the first time to our knowledge.

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

    PubMed

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

    2014-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2001-08-01

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

  4. The Physics of Evaporation-Induced Assembly of Sol-Gel Materials

    SciTech Connect

    HURD,ALAN J.; STEINBERG,LEV

    2000-07-24

    Remarkable materials ordered at the nanoscale emerge when a sol-gel solution becomes co-organized with a surfactant. At sufficiently high concentration, the surfactant forms crystalline or liquid-crystalline arrays of micelles in the presence of the sol-gel, and as gelation proceeds the arrays become locked into the gel. Recent experiments demonstrate that the degree of order in the resulting mesoporous ceramic phase can be enhanced and controlled by continuous dip coating in which the solution, initially dilute, evolves through the critical micelle concentration by steady-state evaporation. The long-range order and microstructural orientation in these films suggest that the propagation of a critical-micelle-concentration transition front, with large physico-chemical gradients, promotes oriented self assembly of surfactant aggregates. This steep-gradient view is supported by results from unsteady evaporation of aerosols of similar solutions, in which internally well-ordered but complex particles are formed.

  5. Nonlinear optical properties of sol-gel-type glasses containing oxidized Cu2Se nanoparticles

    NASA Astrophysics Data System (ADS)

    Yumashev, K. V.

    2000-03-01

    Nonlinear absorption of sol-gel-type glasses containing oxidized Cu2Se nanoparticles (25 nm in radius) is investigated with the aid of the picosecond excitation-probing technique. The oxidation of Cu2Se nanoparticles leads to the appearance of a wide absorption band, which has a maximum roughly at 1 µm and which is bleached on exposure to laser pulses. The time of relaxation of the bleached state approaches 300 psec, and the cross section for absorption at 1.06 µm is equal to about 1.3·10-16 cm2, as evaluated from the measured absorption saturation curve. The regime of Q-switching is obtained for a number of solid-state lasers with generation wavelengths 1.06, 1.34, and 1.54 µm, when sol-gel-type glasses containing oxidized Cu2Se nanoparticles were used as passive shutters.

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

    PubMed

    Haibin, Ni; Ming, Wang; Wei, Chen

    2011-12-19

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

  7. 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

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

    NASA Astrophysics Data System (ADS)

    Stilburn, James R.

    2000-08-01

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

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

    PubMed Central

    Tseng, Ting Ke; Lin, Yi Shing; Chen, Yi Ju; Chu, Hsin

    2010-01-01

    The sol-gel process is a wet-chemical technique (chemical solution deposition), which has been widely used in the fields of materials science, ceramic engineering, and especially in the preparation of photocatalysts. Volatile organic compounds (VOCs) are prevalent components of indoor air pollution. Among the approaches to remove VOCs from indoor air, photocatalytic oxidation (PCO) is regarded as a promising method. This paper is a review of the status of research on the sol-gel method for photocatalyst preparation and for the PCO purification of VOCs. The review and discussion will focus on the preparation and coating of various photocatalysts, operational parameters, and will provide an overview of general PCO models described in the literature. PMID:20640156

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

    SciTech Connect

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

    2006-12-14

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

  11. Cotton Fabric Surface Modification by Sol-Gel Deposition of ZnO Thin Films

    NASA Astrophysics Data System (ADS)

    Vihodceva, S.; Kukle, S.

    2012-08-01

    One of the main tasks of research is to impact the additional value on natural textiles by adding to them ultraviolet (UV) absorption and antimicrobial protection properties with ZnO nano-level coatings. ZnO shows high absorption in the UV region of the light spectrum, in comparison with organic absorbers conventionally used in the textile industry shows no significant degradation, is stable and classified as non-toxic material. Nanosols were prepared by using the sol-gel process. In this work comparison of samples coated by nanosols with zinc acetate (Zn (CH3COO)2-2H2O) and zinc sulphate (ZnSO4) was made. Scanning electron microscopy (SEM) was used to examine the nature of the surface modification with ZnO coating by the sol-gel technique as also after exploitation of samples; energy dispersive X-ray spectroscopy was used for the analysis of elemental composition of coated fabric samples.

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

    PubMed

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

    2013-03-01

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

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

    DOEpatents

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

    2006-05-02

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

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

    NASA Astrophysics Data System (ADS)

    Raghu, P.; Naveen, C. S.; Shailaja, J.; Mahesh, H. M.

    2016-05-01

    Transparent ZnO thin films were prepared using different molar concentration (0.1 M, 0.2 M & 0.8 M) of zinc acetate on soda lime glass substrates by the sol-gel spin coating technique. The optical properties revealed that the transmittance found to decrease with increase in molar concentration. Absorption edge showed that the higher concentration film has increasingly red shifted. An increased band gap energy of the thin films was found to be direct allowed transition of ˜3.9 eV exhibiting their relevance for photovoltaic applications. The extinction coefficient analysis revealed maximum transmittance with negligible absorption coefficient in the respective wavelengths. The results of ZnO thin film prepared by sol-gel technique reveal its suitability for optoelectronics and as a window layer in solar cell applications.

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

    PubMed

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

    2004-02-20

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

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

    NASA Technical Reports Server (NTRS)

    1982-01-01

    Containerless melting of glasses in space for the preparation of ultrapure homogeneous glass for optical waveguides is discussed. The homogenization of the glass using conventional raw materials is normally achieved on Earth either by the gravity induced convection currents or by the mechanical stirring of the melt. Because of the absence of gravity induced convection currents, the homogenization of glass using convectional raw materials is difficult in the space environment. Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation.

  17. Pulsed electric field assisted sol-gel preparation of TiO2 nanoparticles

    NASA Astrophysics Data System (ADS)

    Mani, Rajaboopathi; Han, Bing; Louhi-Kultanen, Marjatta

    2016-10-01

    This work studies the effect of a pulsed electric field (PEF) on the precipitation and properties of TiO2 nanoparticles. TiO2 nanoparticles were prepared using pulsed DC electric field assisted sol-gel method. The duration of the PEF treatment was varied to investigate its effect on the particle size of TiO2 nanoparticles. The nanoparticles were characterized by X-ray powder diffraction (XRD), Raman spectroscopy, UV diffuse reflectance spectroscopy (UV-DRS) and transmission electron microscopy (TEM). It was found that TiO2 particles prepared with pulsed electric field assisted sol-gel method had enhanced average crystallite size due to the effect of the pulsed electric field on primary nucleation. The effect of electric field on nanoparticle preparation is interesting which can be used to control the grain and crystallite size of nanoparticle.

  18. The role of temperature in forming sol-gel biocomposites containing polydopamine

    PubMed Central

    Dyke, Jason Christopher; Hu, Huamin; Lee, Dong Joon; Ko, Ching-Chang; You, Wei

    2014-01-01

    To further improve the physical strength and biomedical applicability of bioceramicsbuilt on hydroxyapatite-gelatin (HAp-Gel) and siloxane sol-gel reactions, we incorporated mussel adhesive inspired polydopamine (PD) into our original composite based on HAp-Gel cross-linked with siloxane. Surprisingly, with the addition of PD, we observed that the processing conditions and temperatures play an important role in the structure and performance of these materials. A systematic study to investigate this temperature dependence behavior discloses that the rate of crosslinking of silane during the sol-gel process is significantly influenced by the temperature, whereas the polymerization of the dopamine only shows minor temperature dependence. With this discovery, we report an innovative thermal process for the design and application of these biocomposites. PMID:25485111

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

    PubMed

    Haibin, Ni; Ming, Wang; Wei, Chen

    2011-12-19

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

  20. Fluor-hydroxyapatite sol-gel coating on titanium substrate for hard tissue implants.

    PubMed

    Kim, Hae-Won; Kim, Hyoun-Ee; Knowles, Jonathan C

    2004-08-01

    Hydroxyapatite (HA) and fluor-hydroxyapatite (FHA) films were deposited on a titanium substrate using a sol-gel technique. Different concentrations of F- were incorporated into the apatite structure during the sol preparation. Typical apatite structures were obtained for all coatings after dipping and subsequent heat treatment at 500 degrees C. The films obtained were uniform and dense, with a thickness of approximately 5 microm. The dissolution rate of the coating layer decreased with increasing F- incorporation within the apatite structure, which demonstrates the possibility of tailoring the solubility by a functional gradient coating of HA and FHA. The cell proliferation rate on the coating layer decreased slightly with increasing F- incorporation. The alkaline phosphatase (ALP) activity of the cells on all the HA and FHA coated samples showed much higher expression levels compared to pure Ti. This confirmed the improved activity of cell functions on the substrates with the sol-gel coating treatment.

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

    SciTech Connect

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

    1993-10-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1992-12-01

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

  3. 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.

  4. The detection of hexavalent chromium by organically doped sol-gels

    SciTech Connect

    Wong, P.W.; Mackenzie, J.D.

    1994-12-31

    The sol-gel process can be used to produce porous inorganic matrices that are doped with organic molecules. These doped gels can be used as a quantitative method for the spectrophotometric determination of trace concentrations of metallic ions. For the detection of hexavalent chromium, malachite green was used as the dopant. Preliminary results indicate concentrations on the order of 5 ppb are detectable using this method.

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

    NASA Technical Reports Server (NTRS)

    Mukherjee, S. P.; Debsikdar, J. C.; Beam, T.

    1983-01-01

    The sol-gel process for the preparation of homogeneous gels in three binary oxide systems was investigated. The glass forming ability of certain compositions in the selected oxide systems (SiO-GeO2, GeO2-PbO, and SiO2-TiO2) were studied based on their potential importance in the design of optical waveguide at longer wavelengths.

  6. Thermodynamic analysis of sol-gel transition of gelatin in terms of water activity in various solutions.

    PubMed

    Miyawaki, Osato; Omote, Chiaki; Matsuhira, Keiko

    2015-12-01

    Sol-gel transition of gelatin was analyzed as a multisite stoichiometric reaction of a gelatin molecule with water and solute molecules. The equilibrium sol-gel transition temperature, Tt , was estimated from the average of gelation and melting temperature measured by differential scanning calorimetry. From Tt and the melting enthalpy, ΔHsol , the equilibrium sol-to-gel ratio was estimated by the van't Hoff equation. The reciprocal form of the Wyman-Tanford equation, which describes the sol-to-gel ratio as a function of water activity, was successfully applied to obtain a good linear relationship. From this analysis, the role of water activity on the sol-gel transition of gelatin was clearly explained and the contributions of hydration and solute binding to gelatin molecules were separately discussed in sol-gel transition. The general solution for the free energy for gel-stabilization in various solutions was obtained as a simple function of solute concentration.

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

    PubMed

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

    2016-05-01

    The sol-gel synthesis method is an attractive technology for the fabrication of ceramic films due to its preparation simplicity and ease of varying the metal composition. However, this technique presents some limitations in relation to the film thickness. Notably, when the film thickness exceeds the critical limit, large tensile stresses occur, resulting in a cracked morphology. In this study, a secondary crystal growth method was introduced as a post-treatment process for Mg/Al hydrotalcite-based films synthesized by the sol-gel method, which typically present a cracked morphology. The cracked hydrotalcite-based film was hydrothermally treated for the secondary growth of hydrotalcite crystals. In the resulting film, hydrotalcite grew with a vertical orientation, and the gaps formed during the sol-gel synthesis were filled with hydrotalcite after the crystal growth. The secondary crystal growth method provides a new solution for cracked ceramic films synthesized by the sol-gel method.

  8. Research of materials for porous matrices in sol-gel systems based on silicon dioxide and metallic oxides

    NASA Astrophysics Data System (ADS)

    Maraeva, E. V.; Bobkov, A. A.; Maximov, A. I.; Moshnikov, V. A.; Nalimova, S. S.

    2015-11-01

    In this study silicon dioxide - stannic oxide and silicon dioxide - zinc nanomaterials oxide were obtained through sol-gel technology. The results of nitrogen thermal desorption measurements, atomic force microscopy measurements and particle sizes measurements are discussed.

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

    PubMed

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

    2015-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

  11. Thin-film silica sol-gels doped with ion responsive fluorescent lipid bilayers

    SciTech Connect

    Sasaki, D.Y.; Shea, L.E.; Sinclair, M.B.

    1999-01-12

    A metal ion sensitive, fluorescent lipid-b i layer material (5oA PSIDA/DSPC) was successfully immobilized in a silica matrix using a tetramethoxysilane (TMOS) sol-gel procedure. The sol-gel immobilization method was quantitative in the entrapment of seif-assembled Iipid-bilayers and yielded thin films for facile configuration to optical fiber piatforms. The silica matrix was compatible with the solvent sensitive lipid bilayers and provided physical stabilization as well as biological protection. Immobilization in the silica sol-gel produced an added benefit of improving the bilayer's metal ion sensitivity by up to two orders of magnitude. This enhanced performance was attributed to a preconcentrator effect from the anionic surface of the silica matrix. Thin gels (193 micron thickness) were coupled to a bifurcated fiber optic bundle to produce a metal ion sensor probe. Response times of 10 - 15 minutes to 0.1 M CUCIZ were realized with complete regeneration of the sensor using an ethylenediarninetetraacetic acid (EDTA) solution.

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

    PubMed

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

    2015-01-01

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

  13. 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}.

  14. Synthesis of polymeric fluorinated sol-gel precursor for fabrication of superhydrophobic coating

    NASA Astrophysics Data System (ADS)

    Li, Qianqian; Yan, Yuheng; Yu, Miao; Song, Botao; Shi, Suqing; Gong, Yongkuan

    2016-03-01

    A fluorinated polymeric sol-gel precursor (PFT) is synthesized by copolymerization of 2,3,4,5,5,5-hexafluoro-2,4-bis(trifluorinated methyl)pentyl methacrylate (FMA) and 3-methacryloxypropyltrimethoxysilane (TSMA) to replace the expensive long chain fluorinated alkylsilanes. The fluorinated silica sol is prepared by introducing PFT as co-precursor of tetraethyl orthosilicate (TEOS) in the sol-gel process with ammonium hydroxide as catalyst, which is then used to fabricate superhydrophobic coating on glass substrate through a simple dip-coating method. The effects of PFT concentrations on the chemical structure of the formed fluorinated silica, the surface chemical composition, surface morphology, wetting and self-cleaning properties of the resultant fluorinated silica coatings were studied by using X-ray powder diffraction (XRD), Fourier transform infrared spectrometer (FTIR), X-ray photoelectron spectrophotometer (XPS), scanning electron microscopy (SEM) and water contact angle measurements (WCA). The results show that the fluorinated silica sols are successfully obtained. The size and size distribution of the fluorinated silica particles are found greatly dependent on the concentration of PFT, which play a crucial role in the surface morphology of the corresponding fluorinated silica coatings. The suitable PFT concentration added in the sol-gel stage, i.e. for F-sol-1 and F-sol-2, is helpful to achieve both the low surface energy and multi-scaled microstructures, leading to the formation of the superhydrophobic coatings with bio-mimicking self-cleaning property similar to lotus leaves.

  15. Qualification of Target Chamber Vacuum Systems Cleanliness using Sol-Gel Coatings

    SciTech Connect

    Miller, P; Stowers, I F; Ertel, J R

    2006-01-03

    This document defines the procedure necessary to qualify the airborne molecular cleanliness (AMC) of vacuum systems (enclosures or large components) that are placed within the National Ignition Facility (NIF) target chamber or are attached to it and communicate with it during vacuum operation. This test is specific to the NIF target chamber because the allowable time dependent rate of rise in the pore filling of a sol-gel coated SAW sensor is based on some nominal change-out time for the disposable debris shields. These debris shields will be sol-gel coated and thus they represent a means of ''pumping'' AMCs from the target chamber. The debris shield pumping rate sets the allowable change in pore filling with time specified in the test procedure. This document describes a two-part procedure that provides both a static measurement of sol-gel pore filling at the end of a 48-hour test period and a dynamic record of pore-filling measured throughout the test period. Successful qualification of a vacuum system requires that both the static and dynamic measurements meet the criteria set forth in Section 7 of this document.

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

    PubMed

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

    2015-07-27

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

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

    PubMed

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

    2016-08-01

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

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

    NASA Astrophysics Data System (ADS)

    Yadav, Reeta

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

  19. 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.

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

    PubMed

    Lukacs, M; Sayer, M; Foster, S

    2000-01-01

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

  1. Nanoscale morphology for high hydrophobicity of a hard sol gel thin film

    NASA Astrophysics Data System (ADS)

    Wu, Y. L.; Chen, Z.; Zeng, X. T.

    2008-08-01

    It is challenging to obtain a hydrophobic smooth coating with high optical and mechanical properties at the same time because the hydrophobic additives are soft in nature resulting in reduced hardness and durability. This paper reports a durable hydrophobic transparent coating on glass fabricated by sol-gel technology and a low volume medium pressure (LVMP) spray process. The sol-gel formula consists of a pre-linked hydrophobic nano-cluster from hydroxyl-terminated polydimethylsiloxane, titanium tetraisopropoxide and a silica-based sol-gel matrix with silica hard fillers. Polydimethylsiloxane (PDMS) is uniformly distributed throughout the coating layer providing durable hydrophobic property. Mechanical properties are achieved by the hard matrix and hard fillers with the nano-structures. Due to the surface nano-morphology, a high degree of hydrophobicity was maintained with only 10 vol.% PDMS, while the hardness and abrasion resistance of the coatings were not significantly compromised. Chemical analyses by FTIR confirmed the uniform distribution of the PDMS and surface morphology analyses by atomic force microscopy (AFM) displayed the nano-surface structures that enhanced the hydrophobicity. The special surface nanostructures can be quantified using surface Kurtosis and ratio between asperity peak height to distance between peaks. The LVMP process influences the spray droplet size resulting in different surface structures.

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

    NASA Astrophysics Data System (ADS)

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

    2008-09-01

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

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

    PubMed Central

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

    2015-01-01

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

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

    PubMed

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

    2016-08-01

    The objective of this work has been to develop low temperature sol-gel glass coatings to modify the substrate surface and to evaluate their bioactivity and biocompatibility. Glasses, based on SiO2·CaO·P2O5, were synthesized by the sol-gel technique using tetraethyl orthosilicate, calcium nitrate tetrahydrate and triethyl phosphate as precursors of SiO2, CaO and P2O5, respectively. Those materials, still in the sol phase, have been used to coat substrates by means of the dip-coating technique. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) has been used for characterize coatings and a microstructural analysis has been obtained using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated substrate was immersed in simulated body fluid (SBF) for 21days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. In order to study the cell behavior and response to our silica based materials, prepared via the sol-gel method, with various Ca/P ratio and coating substrate, we have used the human osteoblast-like U2OS cell line. PMID:27157742

  5. Direct test of the critical exponents at the sol-gel transition

    NASA Astrophysics Data System (ADS)

    Kaya, Demet; Pekcan, Önder; Yılmaz, Yaşar

    2004-01-01

    The steady state fluorescence technique was used to study the sol-gel transition for the solution-free radical cross-linking polymerization of acrylamide (AAm), with N,N'-methylenebis (acrylamide) as cross linker in the presence of ammonium persulfate as an initiator. Pyranine (8-hydroxypyrene-1, 3,6-trisulfonic acid, trisodium salt) is used as a fluoroprobe for monitoring the polymerization. Pyranine molecules start to bind to acrylamide polymer chains upon the initiation of the polymerization, thus the spectra of the bonded pyranines shift to the shorter wavelengths. Fluorescence spectra from the bonded pyranines allows one to monitor the sol-gel transition, without disturbing the system mechanically, and to test the universality of the sol-gel transition as a function of some kinetic parameters such as polymer concentration, cross-linker concentration, and temperature. Observations around the critical point show that there are three regimes for AAm concentration in which the exponents differ drastically. The gel fraction exponent β and the weight average degree of polymerization exponent γ agree best with the static percolation results for higher acrylamide concentrations above 1M, but they cross over from percolation to mean-field (Flory-Stockmayer) values when the AAm concentration is lower than 2M. For very low polymer concentrations, below which the system can not form the gel, the exponents differ considerably from both the percolation and the mean-field values.

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

    NASA Astrophysics Data System (ADS)

    Szendro, Istvan

    2001-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2010-03-01

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

  8. Increasing the activity and enantioselectivity of lipases by sol-gel immobilization: further advancements of practical interest

    NASA Astrophysics Data System (ADS)

    Tielmann, Patrick; Kierkels, Hans; Zonta, Albin; Ilie, Adriana; Reetz, Manfred T.

    2014-05-01

    The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of the sol-gel approach.The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of

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

    PubMed

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

    2016-03-31

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

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

    PubMed

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

    2016-03-31

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

  11. Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

    PubMed

    Catauro, M; Papale, F; Bollino, F

    2016-01-01

    The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0sol-gel route starting from tetraethyl orthosilicate and calcium nitrate tetrahydrate. Those materials, still in the sol phase, have been used to coat titanium substrates by means of the dip-coating technique. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) allowed the materials to be characterized and a microstructural analysis of the coatings obtained was performed using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated titanium was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. To investigate cell-material interactions, mouse embryonic fibroblast cells (3T3) were seeded onto the specimens and the cell viability was evaluated by a WST-8 assay.

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

    PubMed

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

    2016-01-01

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

  13. Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

    PubMed

    Catauro, M; Papale, F; Bollino, F

    2016-01-01

    The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0sol-gel route starting from tetraethyl orthosilicate and calcium nitrate tetrahydrate. Those materials, still in the sol phase, have been used to coat titanium substrates by means of the dip-coating technique. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) allowed the materials to be characterized and a microstructural analysis of the coatings obtained was performed using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated titanium was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. To investigate cell-material interactions, mouse embryonic fibroblast cells (3T3) were seeded onto the specimens and the cell viability was evaluated by a WST-8 assay. PMID:26478379

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

    PubMed

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

    2001-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1999-10-01

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

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

    NASA Astrophysics Data System (ADS)

    Finch, Joshua S.

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

  17. Stability High Salt Content Waste Using Sol Gel Process. Mixed Waste Focus Area. OST Reference Number 0236

    SciTech Connect

    None, None

    1999-09-01

    Mixed waste sludges, soils, and homogeneous solids containing high levels of salt ( ~ greater than 15% by weight ) have proven to be difficult to stabilize due to the soluble nature of the salts. The current stabilization technique for high salt waste, grouting with Portland cement, is limited to low waste loadings. The presence of salts interfere with the hydration and curing of the cement, cause waste form deteriorating mineral expansions, or result in an undesirable separate phase altogether. Improved technologies for the stabilization of salt waste must be able to accommodate higher salt loadings, while maintaining structural integrity, chemical durability, and leach resistance. In a joint collaboration supported by the Department of Energy’s (DOE’s) Mixed Waste Focus Area (MWFA), the Pacific Northwest National Laboratory (PNNL) and the Arizona Materials Laboratory (AML) at the University of Arizona have developed a sol-gel (wet-chemical) based, low-temperature-processing route for the stabilization of salt-containing mixed wastes. By blending and reacting liquid precursors at room temperature with salt waste, strong, impermeable “polyceram” matrices have been formed that encapsulate the environmentally hazardous waste components. As depicted by Figure 1, polycerams are hybrid organic/inorganic materials with unique properties derived from the chemical combination of polymer (organic) and ceramic (inorganic) components. For this application, the stabilizing polyceram matrices contain polybutadiene-based polymer components and silicon dioxide (SiO2) as the inorganic component. Polybutadiene (PBD) is a strong, tough, waterresistant plastic and its use in the polyceram promotes these same characteristics in the waste form. The PBD polymer component is modified to increase its reactivity with the SiO2 precursor during sol-gel processing. When combined, the polymer and SiO2 precursors react, gel, solidify, and encapsulate the

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

    PubMed

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

    2013-04-01

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

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

    NASA Astrophysics Data System (ADS)

    Lian, Xiaojuan; Yang, Xin; Liu, Shangjun; Xu, Ying; Jiang, Chunping; Chen, Jinwei; Wang, Ruilin

    2012-01-01

    Ti-doped α-Fe2O3 thin films were successfully prepared on FTO substrates by the sol-gel route. Hematite film was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy dispersive spectrometer (EDS). The XRD data showed α-Fe2O3 had a preferred (1 1 0) orientation which belonged to the rhombohedral system. Interestingly, the grains turned into worm-like shape after annealed at high temperature. The IPCE could reach 32.6% at 400 nm without any additional potential vs. SCE. Titanium in the lattice can affect the photo electro chemical performance positively by increasing the conductivity of the thin film. So the excited electrons and holes could live longer, rather than recombining with each other rapidly as undoped hematite. And the efficient carrier density on the Ti-doped anode surface was higher than the undoped anode, which contribute to the well PEC performance.

  20. High efficiency TiO2 photocatalysts by the sol-gel process. Final report, 1 April-30 September 1995

    SciTech Connect

    Huang, Y.; Chu, C.J.

    1995-10-25

    Objective of Phase I project is to demonstrate that the dye-sensitized and doped materials by sol-gel process can be used in the photocatalytic reaction for oxidation of chemical wastes under the simulated solar irradiation, and to develop innovative technologies to improve the efficiency of photodegradation of chemical waste. In Phase I research, the authors met the following goals: (1) Development of various technologies on fabrication of TiO2 materials including powders, and porous aerogels with much higher specific surface area comparing to commercial TiO2 anatase powder-Degussa P25 powder. (2) Characterization of crystallographic phase development, morphologies and surface area of materials using XRD, SEM and BET analyser. (3) Investigation on effects of various parameters, such as tungsten doping, dye-sensitization crystallographic phase, morphologies and specific surface area, on efficiency of photodegradation of chemical waste under the simulated solar radiation. (4) Improvements of photocatalytic efficiency by developing innovative technologies, such as using aerosol and aerogel routes with doping and sensitized dye.

  1. Surfactant based sol-gel approach to nanostructured LiFePO 4 for high rate Li-ion batteries

    NASA Astrophysics Data System (ADS)

    Choi, Daiwon; Kumta, Prashant N.

    Porous nanostructured LiFePO 4 powder with a narrow particle size distribution (100-300 nm) for high rate lithium-ion battery cathode application was obtained using an ethanol based sol-gel route employing lauric acid as a surfactant. The synthesized LiFePO 4 powders comprised of agglomerates of crystallites <65 nm in diameter exhibiting a specific surface area ranging from 8 m 2 g -1 to 36 m 2 g -1 depending on the absence or presence of the surfactant. The LiFePO 4 obtained using lauric acid resulted in a specific capacity of 123 mAh g -1 and 157 mAh g -1 at discharge rates of 10 C and 1 C with less than 0.08% fade per cycle, respectively. Structural and microstructural characterization were performed using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) with energy dispersive X-ray (EDX) analysis while electronic conductivity and specific surface area were determined using four-point probe and N 2 adsorption techniques.

  2. Magnetic properties of hard-soft SrFe10Al2O19/Co0.8Ni0.2Fe2O4 ferrite synthesized by one-pot sol-gel auto-combustion

    NASA Astrophysics Data System (ADS)

    Torkian, Shahab; Ghasemi, Ali; Razavi, Reza Shoja

    2016-10-01

    SrFe10Al2O19/Co0.8Ni0.2Fe2O4 hard/soft nanocomposite ferrites with different content of soft phase have been prepared by simple one-pot sol-gel auto-combustion route. X-ray diffraction (XRD), field emission scanning electron microscopy and vibrating ample magnetometer were employed to analysis of structural and magnetic features of synthesized samples. XRD patterns reflect the formation of hard/soft composites of ferrites without the existence of any kind of secondary phases. Narrow size distributions of particles were formed by sol-gel method. Single smooth hysteresis loops of nanocomposites show the presence of exchange coupling between hard and soft phases. Nanocomposite with 15 wt% of soft phase reaches the highest Mr/Ms ratio of 0.63. Compared to the physical mixing of hard/ soft nanocomposites, the one-pot sol-gel auto-combustion method could be considered as a suitable method for synthesizing exchange coupled magnet.

  3. 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.

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

    PubMed

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

    2015-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2012-03-01

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

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

    SciTech Connect

    Wang, Xiaofei; Gong, Cairong; Fan, Guoliang

    2011-12-15

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

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

    PubMed

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

    2013-08-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

    A coating with self-cleaning characteristics has been developed using a TiO2/SiO2 hybrid sol-gel, TiO2 nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO2 nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO2 nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO2 phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO2 NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

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

    NASA Astrophysics Data System (ADS)

    Richard, Brandon Demar

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

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

    DOEpatents

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

    1999-07-20

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

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

    DOEpatents

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

    1999-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2002-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2008-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1999-12-01

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

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

    PubMed

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

    2013-11-01

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

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

    DOEpatents

    Guadalupe, Ana R.; Guo, Yizhu

    2001-05-15

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

  19. 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.

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

    NASA Astrophysics Data System (ADS)

    Mishechkin, Oleg Viktorovich

    2003-10-01

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

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

    SciTech Connect

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

    2005-09-01

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

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

    SciTech Connect

    Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

    2004-01-03

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

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

    NASA Astrophysics Data System (ADS)

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

    2006-06-01

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

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

    SciTech Connect

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

    1996-12-31

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

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

    SciTech Connect

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

    2005-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2005-07-01

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

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

    SciTech Connect

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

    2011-09-30

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-05-01

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

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

    SciTech Connect

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

    2006-05-01

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

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

    PubMed

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

    2014-01-01

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

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

    PubMed

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

    2013-07-01

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

  12. Dielectric properties and alternating current conductivity of sol-gel made La0.8Ca0.2FeO3 compound

    NASA Astrophysics Data System (ADS)

    Benali, A.; Souissi, A.; Bejar, M.; Dhahri, E.; Graça, M. F. P.; Valente, M. A.

    2015-09-01

    In this work, single phase La0.8Ca0.2FeO3 nanomaterial has been synthesized by the sol-gel method using the citric acid route. By employing impedance spectroscopy, ac electrical properties have been measured over a temperature range from 300 to 673 K at various frequencies. With the analysis based on Debye's theory and a series of Arrhenius relations, the relaxation was argued to be associated with the hopping motions of charge carriers between Fe ions. The relaxation in the La0.8Ca0.2FeO3 compound was ascribed to be a polaronic relaxation. The ac electrical conduction was studied and associated to the non-overlapping small polaron tunneling (NSPT) model.

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

    PubMed

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

    2005-04-01

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

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

    PubMed Central

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

    2008-01-01

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

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

    PubMed

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

    2015-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

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

    NASA Astrophysics Data System (ADS)

    Nellis, Barbara

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

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

    PubMed

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

    2012-08-01

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

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

    PubMed Central

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

    2015-01-01

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

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

    PubMed

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

    2012-08-01

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

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

    SciTech Connect

    Ningsih, Sherly Kasuma Warda

    2015-09-30

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

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

    NASA Astrophysics Data System (ADS)

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

    1992-12-01

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

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

    PubMed

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

    2016-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2004-02-01

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

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

    PubMed

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

    2015-02-01

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

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

    PubMed

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

    2014-01-01

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

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

    SciTech Connect

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

    1998-01-01

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

  10. 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

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

    SciTech Connect

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

    1993-07-01

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

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

    NASA Astrophysics Data System (ADS)

    Tonooka, Kazuhiko; Shimokawa, Katsuyoshi; Nishimura, Okio

    2001-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2004-01-01

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

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

    PubMed

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

    2002-02-01

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

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

    PubMed

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

    2016-12-01

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

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

    SciTech Connect

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

    1996-05-01

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

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

    SciTech Connect

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

    1994-12-31

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

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

    PubMed

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

    2013-06-10

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

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

    NASA Astrophysics Data System (ADS)

    Ferrero, Franco; Periolatto, Monica

    2013-06-01

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

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

    PubMed

    Kim, In Yea; Kim, Jong Sung

    2014-11-01

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

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

    SciTech Connect

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

    2011-10-15

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

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

    SciTech Connect

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

    2005-11-03

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

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

    SciTech Connect

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

    1995-12-31

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

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

    SciTech Connect

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

    2007-09-15

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

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

    PubMed

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

    2015-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2006-05-01

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

  8. 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.

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

    PubMed

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

    2013-06-01

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

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

    SciTech Connect

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

    2015-09-25

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

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

    SciTech Connect

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

    2002-05-15

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

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

    SciTech Connect

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

    2002-06-05

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

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

    PubMed

    Hitrik, Maria; Lev, Ovadia; Mandler, Daniel

    2014-09-15

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

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

    SciTech Connect

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

    1999-04-21

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

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

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

    PubMed

    Yilmaz, Elvan; Bengisu, Murat

    2006-04-01

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

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

    PubMed

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

    2014-12-01

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

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

    PubMed

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

    2015-08-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1998-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Ullah Khan, Sajid; ten Elshof, Johan E.

    2012-04-01

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

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

    PubMed

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

    2015-01-01

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

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

    PubMed

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

    2015-09-01

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

  3. 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

  4. 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.

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

    PubMed

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

    1999-01-01

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

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

    PubMed

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

    2003-04-10

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

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

    NASA Astrophysics Data System (ADS)

    Lippincott, Hugh Walker

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

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

    PubMed

    Chen, Hongjun; Dong, Shaojun

    2007-03-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2002-05-01

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

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

    NASA Astrophysics Data System (ADS)

    Deetz, Joshua David

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

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

    NASA Astrophysics Data System (ADS)

    Rao, Sudeep Motupalli

    1998-12-01

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

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

    NASA Astrophysics Data System (ADS)

    Rodriguez Hernandez, Jose Carlos

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

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

    NASA Astrophysics Data System (ADS)

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

    2010-04-01

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

  15. Synthesis and Characterization of ZnO/Bi2O3 Core/Shell Nanoparticles by the Sol-Gel Method

    NASA Astrophysics Data System (ADS)

    Liu, Ting-Ting; Wang, Mao-hua; Zhang, Han-Ping

    2016-08-01

    In this work, a novel two-step synthesis of ZnO/Bi2O3 core/shell nanoparticles is presented. Spherical core particles of ZnO were first synthesized by a 95°C direct precipitation method with the assistance of polyethylene glycol (PEG-6000) surfactants, and then used as precursors to prepare ZnO/Bi2O3 core/shell particles via a 70°C low-temperature sol-gel method. Techniques including x-ray diffraction, Fourier-transform infrared spectroscopy, transmission electron microscopy, energy-dispersive x-ray spectroscopy and scanning electron microscopy were employed to characterize the as-synthesized samples. The ZnO nanoparticles were almost spherical in shape, with particle size ranging from 15 nm to 28 nm, and belonged to a hexagonal wurtzite crystal structure. Furthermore, the experimental result showed that ZnO nanoparticles were fully covered with Bi2O3. In addition, using ZnO/Bi2O3 core/shell nanoparticles (1 mol.% Bi2O3) via this sol-gel method, after sintering in air at 1100°C for 2 h, the varistors showed maximum relative density of 96.6%, with high breakdown voltage (2191 ± 0.72 V/cm), low leakage current (0.12 ± 0.07 μA) and nonlinear coefficient (6 ± 0.14), suggesting that nano-coating is a promising route for the preparation of ZnO varistors.

  16. Reaction mechanism and optimal conditions for preparation of high-quality vanadium oxide films by organic sol-gel for optoelectronic applications

    NASA Astrophysics Data System (ADS)

    Sun, Minghui; Wen, Yuejiang; Xu, Xiangdong; Wang, Meng; He, Qiong; Jiang, Yadong; Dai, Zelin; Gu, Yu; Chen, Zhegeng

    2016-03-01

    Although vanadium oxides (VO x ) are important functional materials for academic research and industrial applications, the reaction mechanism of VO x prepared by organic sol-gel remains unclear. In order to investigate this mechanism, VO x organic sols were reacted at different temperatures, by which various VO x thin films were prepared. The products were systematically characterized by infrared spectroscopy, Raman spectroscopy, UV-vis spectroscopy, thermogravimetric analysis, scanning electron microscopy, x-ray diffraction, and a high resistance meter. Results reveal that vanadium alkoxides are created through an alcoholysis reaction of V2O5 powder and isobutyl alcohol, and then a condensation reaction of the vanadium alkoxides leads to the formation of VO x networks. The as-prepared sols are strongly temperature-dependent, causing different chemical structures and physical properties for the resulting VO x films. Particularly, a moderate temperature of 110 °C prompts both alcoholysis and condensation reactions, and thus the VO x films that are produced by the sol reacted at 110 °C possess a low resistivity of 23 Ω cm, a high temperature coefficient resistance (TCR) of  -3.2% K-1, and a low average transmittance of 54% in 580-1100 nm, compared with those prepared by the sols reacted at lower or higher temperatures. Therefore, 110 °C is a desirable sol temperature for producing VO x films serving as high-quality bolometric materials for uncooled infrared detectors. This work discloses not only the reaction mechanism of VO x films prepared by organic sol-gel, but also the route to yield desirable VO x films for optoelectronic applications.

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

    SciTech Connect

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

    2014-04-24

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

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

    NASA Astrophysics Data System (ADS)

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

    1998-11-01

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

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

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey; Selvaduray, Guna; Leiser, Daniel

    1992-01-01

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

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

    PubMed

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

    2015-09-01

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

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

    SciTech Connect

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

    2003-01-02

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

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

    SciTech Connect

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

    2010-02-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2000-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-07-01

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

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

    NASA Astrophysics Data System (ADS)

    Shu-wen, Xue

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

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

    PubMed Central

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

    2013-01-01

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

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

    SciTech Connect

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

    2007-01-18

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

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

    DOEpatents

    Pekala, Richard W.

    1998-04-28

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

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

    DOEpatents

    Pekala, Richard W.

    1996-01-01

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

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

    DOEpatents

    Pekala, R.W.

    1995-12-19

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

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

    DOEpatents

    Pekala, R.W.

    1996-09-17

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

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

    DOEpatents

    Pekala, Richard W.

    1995-01-01

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

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

    DOEpatents

    Pekala, R.W.

    1998-04-28

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

  15. Titania-based molecularly imprinted polymer for sulfonic acid dyes prepared by sol-gel method.

    PubMed

    Li, Man; Li, Rong; Tan, Jin; Jiang, Zi-Tao

    2013-03-30

    A novel titania-based molecularly imprinted polymer (MIP) was synthesized through sol-gel process with sunset yellow (Sun) as template, without use of functional monomer. MIP was used as a solid-phase extraction material for the isolation and enrichment of sulfonic acid dyes in beverages. The results showed that MIP exhibited better selectivity, higher recovery and adsorption capacity for the sulfonic acid dyes compared to the non-imprinted polymer (NIP). MIP presented highest extraction selectivity to Sun when pH less than or equal to 3. The adsorption capacity was 485.9 mg g(-1), which was larger than that of NIP (384.7 mg g(-1)). The better clean-up ability demonstrated the capability of MIP for the isolation and enrichment of sulfonic acid dyes in complicated food samples. The mean recoveries for the sulfonic acid dyes on MIP were from 81.9% to 97.2% in spiked soft drink.

  16. Structural properties and gas sensing behavior of sol-gel grown nanostructured zinc oxide

    NASA Astrophysics Data System (ADS)

    Rajyaguru, Bhargav; Gadani, Keval; Rathod, K. N.; Solanki, Sapana; Kansara, S. B.; Pandya, D. D.; Shah, N. A.; Solanki, P. S.

    2016-05-01

    In this communication, we report the results of the studies on structural properties and gas sensing behavior of nanostructured ZnO grown using acetone precursor based modified sol-gel technique. Final product of ZnO was sintered at different temperatures to vary the crystallite size while their structural properties have been studied using X-ray diffraction (XRD) measurement performed at room temperature. XRD results suggest the single phasic nature of all the samples and crystallite size increases from 11.53 to 20.96nm with increase in sintering temperature. Gas sensing behavior has been studied for acetone gas which indicates that lower sintered samples are more capable to sense the acetone gas and related mechanism has been discussed in the light of crystallite size, crystal boundary density, defect mechanism and possible chemical reaction between gas traces and various oxygen species.

  17. Deposition of Co-doped TiO2 Thin Films by sol-gel method

    NASA Astrophysics Data System (ADS)

    Boutlala, A.; Bourfaa, F.; Mahtili, M.; Bouaballou, A.

    2016-03-01

    Cobalt doped TiO2 thin films have been prepared by sol-gel method onto glass substrate at room temperature. in this present work, we are interesting to study the effect of Cobalt doped TiO2 thin films.the concentration of Co was varied from 0 to 6%at .The obtained films have been annealed at 500°C for 2 hours. X-ray diffraction patterns showed that Co: TiO2 films are polycrystalline with a tetragonal anatase and orthorhombic brookite types structures. The surface morphologies of the TiO2 doped with cobalt thin films were evaluated by Atomic Force Microscopy (AFM). The optical properties were studied by mean of UV-visible and near infrared spectroscopy.The calculated optical band gap decreases from 3.30 to 2.96 eV with increasing Co doping.

  18. Impact of temperature on zinc oxide particle size by using sol-gel process

    SciTech Connect

    Lee, Keanchuan Ching, Dennis Ling Chuan; Saipolbahri, Zulhilmi Akmal bin; Guan, Beh Hoe E-mail: hassan.soleimani@petronas.com.my; Soleimani, Hassan E-mail: hassan.soleimani@petronas.com.my

    2014-10-24

    Zinc oxide (ZnO) nanoparticles were prepared and synthesized via sol-gel method, by using citric acid as a precursor. The impact of annealing on the particle size was investigated. Based on the results from the Thermogravimetric Analysis (TGA), three different annealing temperature which is 500, 600 and 700 °C were chosen followed by the characterization of the ZnO nanoparticle by using Powder X-Ray Diffraction (PXRD), Transmission Electron Microscopy (TEM) and Field Emission Scanning Electron Microscopy (FESEM). Results showed that the crystallite size estimated from PXRD increased with the annealing temperature which was hexagonal structure for ZnO. TEM further revealed the same tendency which the Zn NPs size also increased with the annealing temperature.

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

    PubMed

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

    2014-02-01

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

  20. Dynamical transition of heat transport in a physical gel near the sol-gel transition

    NASA Astrophysics Data System (ADS)

    Kobayashi, Kazuya U.; Oikawa, Noriko; Kurita, Rei

    2015-12-01

    We experimentally study heat transport in a gelatin solution near a reversible sol-gel transition point where viscosity strongly depends on temperature. We visualize the temperature field and velocity field using thermochromic liquid crystals and polystyrene latex particles, respectively. During the initial stages of heating, we find that heat transport undergoes a dynamical transition from conductive to convective. Subsequently, during later stages, we observe that the transport dynamics are much more complex than conventional thermal convections. At the sample’s surface we observe the formation of stagnant domains, which lack fluid flow. Their formation is not due to the effects of local cooling. We determine that it is the dynamics of these stagnant domains that induce convective-conductive-convective transitions.

  1. Surfactant-assisted sol-gel synthesis of forsterite nanoparticles as a novel drug delivery system.

    PubMed

    Hassanzadeh-Tabrizi, S A; Bigham, Ashkan; Rafienia, Mohammad

    2016-01-01

    In the present study, forsterite nanoparticles were synthesized via surfactant-assisted sol-gel method using cetyltrimethyl ammonium bromide (CTAB) as a surfactant. The effects of CTAB contents and heat treatment on the textural properties and drug release from nanoparticles were investigated. The synthesized powders were studied by X-ray diffraction, Fourier transform infrared spectra, Brunauer-Emmett-Teller surface area analysis and transmission electron microscope images. Mg2SiO4 materials demonstrated mesoporous characteristics and large specific surface area ranging from 159 to 30 m(2)/g. The TEM results showed that forsterite nanorods had diameters about 4 nm and lengths ranging from 10 to 60 nm. It was found that the samples with 6g CTAB show slower drug release rate than the other specimens, which is due to smaller pore size. This study revealed that the drug delivery of forsterite can be tailored by changing the amount of surfactant.

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

    NASA Astrophysics Data System (ADS)

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

    2009-12-01

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

  3. Synthesis of hybrid sol-gel materials and their biological evaluation with human mesenchymal stem cells.

    PubMed

    Hernández-Escolano, M; Juan-Díaz, M J; Martínez-Ibáñez, M; Suay, J; Goñi, I; Gurruchaga, M

    2013-06-01

    Surface engineering of biomaterials could promote the osseointegration of implants. In this work, two types of hybrid sol-gel materials were developed to stimulate cell attachment, proliferation and differentiation of osteogenic cells. One type was synthesised from vinyl triethoxysilane (VTES) and tetraethyl-orthosilicate (TEOS) at different molar ratios, while the other from VTES and hydroxyapatite particles (HAp). Hybrid materials were systematically investigated using nuclear magnetic resonance, Fourier transform infrared spectroscopy and contact angle metrology. The biocompatibility and osseoinduction of the coatings were evaluated by measuring mesenchymal stem cell proliferation using MTT assays and analysing the mineralised extracellular matrix production by quantifying calcium-rich deposits. The results highlighted the versatility of these coatings in obtaining different properties by changing the molar ratio of the VTES:TEOS precursors. Thus, mineralisation was stimulated by increasing TEOS content, while the addition of HAp improved cell proliferation but worsened mineralisation. PMID:23475116

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

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

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

  5. Superparamagnetic calcium ferrite nanoparticles synthesized using a simple sol-gel method for targeted drug delivery.

    PubMed

    Sulaiman, N H; Ghazali, M J; Majlis, B Y; Yunas, J; Razali, M

    2015-01-01

    The calcium ferrite nano-particles (CaFe2O4 NPs) were synthesized using a sol-gel method for targeted drug delivery application. The proposed nano-particles were initially prepared by mixing calcium and iron nitrates that were added with citric acid in order to prevent agglomeration and subsequently calcined at a temperature of 550°C to obtain small particle size. The prepared nanoparticles were characterized by using an XRD (X-ray diffraction), which revealed the configuration of orthorhombic structures of the CaFe2O4 nano-particles. A crystallite size of ~13.59 nm was obtained using a Scherer's formula. Magnetic analysis using a VSM (Vibrating Sample Magnetometer analysis), revealed that the synthesized particles exhibited super-paramagnetic behavior having magnetization saturation of approximately 88.3emu/g. Detailed observation via the scanning electron microscopy (SEM) showed the calcium ferrite nano-particles were spherical in shape. PMID:26405858

  6. Physical Properties of Potassium Phosphate Glass Prepared by Sol Gel Method

    SciTech Connect

    Mat, Noorhidayah Che; Sahar, Md Rahim; Pauzi, Safwan Ahmad

    2010-07-07

    Series of glasses based on Al{sub 2}O{sub 3}-K{sub 2}O-P{sub 2}O{sub 5} have successfully been made by sol gel method. The amorphous state has been confirmed by X-ray diffraction (XRD) while the actual composition has been determined using Energy Dispersive X-ray (EDX) analysis. The glass density is determined using Archimedes method while the Vickers Micro hardness Test has been used to measure the hardness. It is found that all the samples are amorphous in nature with their actual composition contained phosphate in the range of 40-53% mol. It is also observed that the glass density is about 2.4 gcm{sup -3} while the hardness is in the range of 40-100 Hv, depending on composition.

  7. Sol-gel/rhodamine 6G composite films with tailored microstructures

    SciTech Connect

    Logan, D.L.; Ashley, C.S.; Assink, R.A.; Brinker, C.J. |

    1992-12-31

    A multi-step hydrolysis procedure was developed to prepare composite organic dye/sol-gel thin films with variable porosity for such as switches or sensors. Variation of acid and base catalyzed hydrolysis sequences of three sols prepared from tetraethoxysilane with identical H{sub 2}O/Si ratios, dilution factors, and pH resulted in considerably different silicate speciation. Under conditions where monomer was avoided, the refractive indices of as-deposited films could be varied by an again step prior to film deposition. This general strategy, which relies on the aggregation of fractal polymeric clusters, is compatible with the low temperature and near neutral pH requirements of both organic dyes and biologically active species such as enzymes.

  8. Titania sol-gel coatings with silver on non-porous titanium and titanium alloys

    NASA Astrophysics Data System (ADS)

    Horkavcova, D.; Cerny, M.; Sanda, L.; Novak, P.; Jablonska, E.; Zlamalova-Cflova, Z.; Helebrant, A.

    2016-04-01

    The objective of the work was to prepare and characterize titania sol-gel coatings on non-porous titanium and newly developed titanium alloys. Basic titania sol contained two forms of silver. Titania sol without silver was used as a reference sample. Coatings were prepared by dip-coating technique during stirring and fired. Coatings after firing were characterized by scanning electron microscopy. All titania coatings were measured to determine their adhesive and bactericidal properties. Adhesion of the coatings to the substrate was measured by tape test. Gram-negative bacteria E. coli was used for the bactericidal test. Coated substrates were immersed into suspension of E. coli in physiological solution for 24 hours. The in vitro cytotoxicity test was performed after one day. The bactericidal effect without toxicity was confirmed for selected coatings.

  9. Preparation of silver nanoparticles by a non-aqueous sol-gel process.

    PubMed

    Petit, Christophe T G; Alsulaiman, Muath S A; Lan, Rong; Mann, Gregory; Tao, Shanwen

    2013-08-01

    Using a non-aqueous sol-gel process with a direct calcination step in air after prior drying, silver nanoparticles with average size distribution ranging from 20 to 100 nm were synthesised. Studies in reduced atmosphere were also performed with mixed results, both in phase and particle size, as the samples were found to be mixed with an amorphous phase. In oxidising atmosphere, the temperature and dwelling time were found to be critical factors with the former playing a larger role than the latter. Optimally nanoparticles of silver are best prepared by direct calcination in air of the precursor gel at 250 degrees C for 1 hour. Compared to silver particles prepared by microemulsions, the particle size is larger due to the thermal treatment, which causes a growth of the silver particles. PMID:23882777

  10. TiO2 nanosized powders controlling by ultrasound sol-gel reaction.

    PubMed

    Latt, Kyaing Kyaing; Kobayashi, Takaomi

    2008-04-01

    We studied that anatase-TiO2 powders prepared from sol-gel process of titanium tetra-isopropoxide (TTIP) were developed under ultrasonic irradiation with different frequency of 28, 45 and 100 kHz. The irradiated ultrasound (US) was controlled by using semi-cylindrical reflection plate that was placed onto the vicinity of reaction vessel. The focused US influenced the reduction of particles size and increased the surface area of resultant nanosized TiO2 powders. We also examined photodegradation of rhodamine 640 dye (Rh-640) solution by the resultant TiO2 under UV light exposure. It was observed that low frequency for TiO2 photocatalyst preparation and low calcination temperature were more affected onto the photodegradation of the dye. PMID:17904404

  11. Optical properties of ZnO powder prepared by using a proteic sol-gel process

    NASA Astrophysics Data System (ADS)

    Kwon, Bong-Joon; Woo, Hyun-Joo; Park, Ji-Yeon; Jang, Kiwan; Lim, Seung-Hyuk; Cho, Yong-Hoon

    2013-03-01

    We have studied the optical properties of ZnO powder synthesized by using a proteic sol-gel process with coconut water as the precursor. The energy dispersive X-ray spectrometer and X-ray diffraction results show high purity of the synthesized ZnO powder. From the low-temperature (12 K) and power-dependent PL spectra, the donor-bound exciton, the acceptor-bound exciton, the donor-to-acceptor pair (DAP), and the phonon-replica of the DAP transition have been observed at 3.38, 3.34, 3.26, and 3.19 eV, respectively. The free exciton emission (˜3.3 eV) is also observed at 300 K in the temperature-dependent PL spectra.

  12. Weak localization in CdO thin films prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Wang, W. J.; Xie, X. J.; Liu, J. Y.; Gao, K. H.

    2016-07-01

    This paper reports the study of the magnetotransport properties of polycrystalline CdO thin films prepared by the sol-gel method. Both the sheet resistance and electron density as a function of temperature indicate that our samples are degenerate semiconductors. The weak localization (WL) effect is observed in the low temperature range. Applying the two-dimensional WL theory, we have extracted the dephasing length and a relatively large value (the maximum gets to 151 nm at 2 K) is obtained. The temperature dependence of the extracted dephasing length can be well described by the electron-electron scattering process, indicating that the electron-electron scattering is main dephasing mechanism for electrons.

  13. Effect of solvents on the preparation of lithium aluminate by sol-gel method

    SciTech Connect

    Oksuzomer, Faruk; Koc, S. Naci; Boz, Ismail; Gurkaynak, M. Ali

    2004-04-02

    {gamma}-Lithium aluminate was prepared by sol-gel method using lithium methoxide and aluminum-sec-butoxide precursors in i-propanol, n- and tert-butanol. Clear gels could be obtained due to the addition of ethylacetoacetate and the dried solids were calcined at 550 and 900 deg. C. The resulting solids were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), thermo-gravimetric analysis/differential thermal analysis (TGA/DTA). {gamma}-Lithium aluminate with the highest purity was obtained with t-butanol solvent and LiAl{sub 5}O{sub 8} was the second major phase.

  14. Sol-Gel-Prepared Nanoparticles of Mixed Praseodymium Cobaltites-Ferrites.

    PubMed

    Pekinchak, Olga; Vasylechko, Leonid; Lutsyuk, Iryna; Vakhula, Yaroslav; Prots, Yuri; Carrillo-Cabrera, Wilder

    2016-12-01

    Two series of nanocrystalline powders of PrCo1 - x Fe x O3 (x = 0.1, 0.3, 0.5, 0.7 and 0.9) of high purity were obtained by sol-gel citrate method at 700 and 800 °C. The formation of continuous solid solution with an orthorhombic perovskite structure (sp. group Pbnm) was observed. A peculiarity of the PrCo1 - x Fe x O3 solid solution is the lattice parameter crossovers, which occurred at certain compositions and revealed in the pseudo-tetragonal or pseudo-cubic metric. An average crystallite size of the PrCo1 - x Fe x O3 samples estimated from the analysis of the angular dependence of the X-ray diffraction (XRD) line broadening varies between 30 and 155 nm, depending on the composition and synthesis temperature.

  15. Encapsulation of nanoclusters in dried gel materials via an inverse micelle/sol gel synthesis

    DOEpatents

    Martino, Anthony; Yamanaka, Stacey A.; Kawola, Jeffrey S.; Showalter, Steven K.; Loy, Douglas A.

    1998-01-01

    A dried gel material sterically entrapping nanoclusters of a catalytically active material and a process to make the material via an inverse micelle/sol-gel synthesis. A surfactant is mixed with an apolar solvent to form an inverse micelle solution. A salt of a catalytically active material, such as gold chloride, is added along with a silica gel precursor to the solution to form a mixture. To the mixture are then added a reducing agent for the purpose of reducing the gold in the gold chloride to atomic gold to form the nanoclusters and a condensing agent to form the gel which sterically entraps the nanoclusters. The nanoclusters are normally in the average size range of from 5-10 nm in diameter with a monodisperse size distribution.

  16. Encapsulation of nanoclusters in dried gel materials via an inverse micelle/sol gel synthesis

    DOEpatents

    Martino, A.; Yamanaka, S.A.; Kawola, J.S.; Showalter, S.K.; Loy, D.A.

    1998-09-29

    A dried gel material sterically entrapping nanoclusters of a catalytically active material and a process to make the material via an inverse micelle/sol-gel synthesis are disclosed. A surfactant is mixed with an apolar solvent to form an inverse micelle solution. A salt of a catalytically active material, such as gold chloride, is added along with a silica gel precursor to the solution to form a mixture. To the mixture are then added a reducing agent for the purpose of reducing the gold in the gold chloride to atomic gold to form the nanoclusters and a condensing agent to form the gel which sterically entraps the nanoclusters. The nanoclusters are normally in the average size range of from 5--10 nm in diameter with a monodisperse size distribution. 1 fig.

  17. nanoflakes prepared via a two-step sol-gel-exfoliation method

    NASA Astrophysics Data System (ADS)

    Zhuiykov, Serge; Kats, Eugene

    2014-08-01

    The morphology and electrical properties of orthorhombic β-WO3 nanoflakes with thickness of ~7 to 9 nm were investigated at the nanoscale with a combination of scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), current sensing force spectroscopy atomic force microscopy (CSFS-AFM, or PeakForce TUNA™), Fourier transform infra-red absorption spectroscopy (FTIR), linear sweep voltammetry (LSV) and Raman spectroscopy techniques. CSFS-AFM analysis established good correlation between the topography of the developed nanostructures and various features of WO3 nanoflakes synthesized via a two-step sol-gel-exfoliation method. It was determined that β-WO3 nanoflakes annealed at 550°C possess distinguished and exceptional thickness-dependent properties in comparison with the bulk, micro and nanostructured WO3 synthesized at alternative temperatures.

  18. Investigation of the Peroxovanadate Sol-Gel Process and Characterization of the Gels

    SciTech Connect

    Craig Joseph Fontenot

    2001-12-31

    In general, the peroxovanadate solution sol-gel process can be thought of as consisting of two parts: (1) the decomposition of the peroxo species and (2) cation hydrolysis leading to gelation. By controlling the synthesis conditions, both layered and amorphous compounds can be created. However, the type of water coordination observed in these gels was found to be identical no matter what the long-range order. The current work clarified many of the discrepancies found in the literature and offered much new valuable information. Highlights include the types of vanadium environments present at various stages of hydration, the role of adsorbed water, oxygen exchange from adsorbed water into the gel sites, and the ability to create metastable VMoO solid solution phases. These results could have a variety of impacts on future catalysis research.

  19. Superabrasive cubic boron nitride-oxide composites prepared by sol-gel processing

    SciTech Connect

    Nazeri-Eshghi, A.

    1989-01-01

    Superabrasive cubic boron nitride (CBN) grains were incorporated in different oxide matrices prepared through sol-gel processing. CBN grains of different particle size from 0.5 to 25 microns were homogeneously dispersed in alumina, alumina-silicate and silica gels. Monolithic composites were achieved upon firing to higher temperatures either by sintering or hot-pressing. Densification of these composites versus temperature was monitored by continuous shrinkage measurements in a dilatometer. The effect of particle size and the volume content of CBN on densification of the gel matrix was investigated. Experimental results were compared with the theories on gel shrinkage and densification of heterogeneous ceramic powders. Reactions at the interface between the CBN particles and the gel matrix and some mechanical properties of the composites were studied.

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

    NASA Astrophysics Data System (ADS)

    Zhan, Hongbing; Chen, Wengzhe; Lin, Chunying

    2002-09-01

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

  1. Facile sol-gel synthesis of porous silicas using poly(propylene)imine dendrimers as templates

    SciTech Connect

    Larsen, Gustavo; Lotero, Edgar; Marquez, Manuel

    2000-08-01

    Commercially available poly(propylene)imine (DAB-Am-32 and DAB-Am-64) dendrimers were used as single-molecule templates to tailor the porosity of silicas via a nonacidic sol-gel method. X-ray diffraction on both the as-prepared (oven-dried at 373 K) and the calcined (833 K) materials revealed that modest contraction took place on template removal and that the cavities created did not achieve three-dimensional ordering under the current synthesis conditions. Transmission electron microscopy of ''Pt-stained'' samples supported this picture. A modified Horvath-Kawazoe analysis of the argon adsorption isotherms indicated that DAB-Am-64 is a much more effective template than DAB-Am-32. Pyrolysis and oxidation protocols for template removal are also presented. (c) 2000 Materials Research Society.

  2. Induced crystallization in CW laser-irradiated sol-gel deposited titania films

    SciTech Connect

    Exarhos, G.J.; Hess, N.J.

    1993-12-31

    Isothermal annealing of amorphous TiO{sub 2} films deposited from acidic sol-gel precursor solutions results in film densification and concomitant increase in refractive index. Subsequent heating above 300C leads to irreversible transformation to an anatase crystalline phase. Similar phenomena occur when such amorphous films are subjected to focused cw laser irradiation. Controlled variations in laser fluence are used to densify or crystallize selected regions of the film. Low fluence conditioning leads to the evolution of a subtle nanograin-size morphology, evident in AFM images, which appears to retard subsequent film crystallization when such regions are subjected to higher laser fluence. Time-resolved Raman spectroscopy has been used to characterize irradiated regions in order to follow the crystallization kinetics, assess phase homogeneity, and evaluate accompanying changes in residual film stress.

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

    PubMed

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

    2009-10-15

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

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

    NASA Astrophysics Data System (ADS)

    Karasiński, Paweł

    2015-12-01

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

  5. Synthesis of high-surface-area titanium dioxide by sol-gel process for DSSC

    NASA Astrophysics Data System (ADS)

    Wahyuningsih, S.; Ramelan, A. H.; Juliana, G.; Khoirunisa, A. R.; Rahardjo, S. B.; Pramono, E.; Suharyana, S.; Suryana, R.; Supriyanto, A.

    2014-05-01

    Mesoporous TiO2 material was synthesized from dissolution ilmenite as well as from titanium chloride precursor via a sol-gel process in acidic aqueous solution. The properties of these materials were characterized with several analytical techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), wide angle X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) analysis, and Barrett-Joyner-Halenda (BJH) analysis. The mesoporous TiO2 materials calcinated at various temperatures were found to have high value surface areas. The photovoltaic of photo-anode build from the mesoporous TiO2 was characterized with I-V Keitley Multimeter, and it was found that photovoltaics fabricated using the mesoporous TiO2 have a good performance. Such a high photovoltaic activity is explained with large surface area and small crystal size.

  6. Structural and Optical Characterization of Synthesized TiO2 Nanopowder Using Sol-Gel Technique

    NASA Astrophysics Data System (ADS)

    Lourduraj, S.; Williams, R. Victor

    2016-02-01

    The nanocrystalline TiO2 powder was synthesized by sol-gel method. The XRD analysis reveals that TiO2 powder was highly crystalline (anatase phase) and nanostructured with tetragonal system. The average crystallite size after calcined at 673K is found to be 7.7nm. The surface morphological studies using scanning electron microscopy (SEM) exhibit that the formation of nanosized TiO2 particles with less densification nature. Atomic force microscopy (AFM) topography exhibits the uniform distribution of spherical-shaped particles. The energy dispersive X-ray spectroscopy (EDX) confirms the presence of Titanium and Oxygen in synthesized TiO2 nanopowder. The value of optical bandgap of TiO2 nanopowder calculated from UV-Visible spectrum is 3.45eV. The presence of TiO2 particles is confirmed from the dominant fourier transform infrared (FTIR) peaks at 621cm-1 and 412cm-1.

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

    NASA Astrophysics Data System (ADS)

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

    2013-03-01

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

  8. 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.

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

    SciTech Connect

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

    1994-03-15

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

  10. Zirconium carbonitride pellets by internal sol gel and spark plasma sintering as inert matrix fuel material

    NASA Astrophysics Data System (ADS)

    Hedberg, Marcus; Cologna, Marco; Cambriani, Andrea; Somers, Joseph; Ekberg, Christian

    2016-10-01

    Inert matrix fuel is a fuel type where the fissile material is blended with a solid diluent material. In this work zirconium carbonitride microspheres have been produced by internal sol gel technique, followed by carbothermal reduction. Material nitride purities in the produced materials ranged from Zr(N0.45C0.55) to Zr(N0.74C0.26) as determined by X-ray diffraction and application of Vegard's law. The zirconium carbonitride microspheres have been pelletized by spark plasma sintering (SPS) and by conventional cold pressing and sintering. In all SPS experiments cohesive pellets were formed. Maximum final density reached by SPS at 1700 °C was 87% theoretical density (TD) compared to 53% TD in conventional sintering at 1700 °C. Pore sizes in all the produced pellets were in the μm scale and no density gradients could be observed by computer tomography.

  11. Structural, electrical and magnetic properties of Ni2+ substituted cobalt nanoferrite using sol-gel method

    NASA Astrophysics Data System (ADS)

    Blessington Selvadurai, A. Paul; Gazzali, P. M. Md.; Murugasen, C.; Pazhanivelu, V.; Murugaraj, R.; Chandrasekaran, G.

    2013-02-01

    Ni doped cobalt ferrite of chemical formula Ni(1-x)CoxFe2O4 with x values = 1, 0.5, 0 were prepared by using Poly Vinyl Alcohol (PVA) sol-gel method. The prepared samples were heat treated at 450°C for an hour and grounded to form fine powder. XRD of the powder sample confirms the formation of spinel ferrite phase. SEM and EDAX spectrum reveals the surface and chemical composition of the sample. FTIR spectra of the samples show the stretching vibration of the tetrahedral (ν1) and octahedral (ν2) bands of Fe-O bonds appearing at 600cm-1 and 424cm-1 respectively. Room temperature magnetic and electrical studies were done using VSM and LCZ meter to analyze their property respectively.

  12. A luminescence endotoxin biosensor prepared by the sol-gel method

    NASA Astrophysics Data System (ADS)

    Hreniak, A.; Maruszewski, K.; Rybka, J.; Gamian, A.; Czyżewski, J.

    2004-07-01

    Silicate thin films with terminal amino groups were prepared via the sol-gel technique and selected biological molecules labeled with luminophores were covalently attached to their surfaces. The obtained thin films with covalently bound Concanavalin-A (Con-A) labeled with fluorescein (FITC) were immersed in a buffer and polarized emission spectra were measured. In the next step, the samples were incubated with a lipopolysaccharide (LPS) isolated from Hafnia alvei PCM 1186 bacterial strain and the emission spectra were collected again. The influence of LPS binding to Con-A on the luminescence depolarization has been proven. The system based on the this effect can be employed as an optical sensor for detection of certain types of bacteria.

  13. Durable superhydrophobic and antireflective surfaces by trimethylsilanized silica nanoparticles-based sol-gel processing.

    PubMed

    Manca, Michele; Cannavale, Alessandro; De Marco, Luisa; Aricò, Antonino S; Cingolani, Roberto; Gigli, Giuseppe

    2009-06-01

    We present a robust and cost-effective coating method to fabricate long-term durable superhydrophobic andsimultaneouslyantireflective surfaces by a double-layer coating comprising trimethylsiloxane (TMS) surface-functionalized silica nanoparticles partially embedded into an organosilica binder matrix produced through a sol-gel process. A dense and homogeneous organosilica gel layer was first coated onto a glass substrate, and then, a trimethylsilanized nanospheres-based superhydrophobic layer was deposited onto it. After thermal curing, the two layers turned into a monolithic film, and the hydrophobic nanoparticles were permanently fixed to the glass substrate. Such treated surfaces showed a tremendous water repellency (contact angle = 168 degrees ) and stable self-cleaning effect during 2000 h of outdoor exposure. Besides this, nanotextured topology generated by the self-assembled nanoparticles-based top layer produced a fair antireflection effect consisting of more than a 3% increase in optical transmittance. PMID:19466786

  14. Metal mediated sol-gel chemistry of 1,2-Bis(triethoxysilyl)-ethene

    SciTech Connect

    Carpenter, J.P.; Yamanaka, S.A.; McClain, M.D.

    1996-10-01

    Ethenyl-bridged polysilsesquioxane xerogels and aerogels were formed from the sol-gel polymerization of 1,2-bis(triethoxysilyl)ethene. Gels were synthesized from the cis- and trans-isomers by both acid and base catalysis. While the trans-monomer exhibited relatively fast gelation times, the cis-monomer depending on the conditions either formed no gel of had very long gelation times. The addition of a coordinating metal such as Pd to the cis-monomer sol results in dramatically decreased gelation times. The addition of salts with noncoordinating metals did not significantly shorten the gelation times indicating that a template effect may be directing the polymerization of the cis-monomer. The ethenyl-bridged polysilsesquioxanes were characterized by solid state {sup 29}Si and {sup 13}C NMR, nitrogen sorption porosimetry, and transmission electron microscopy.

  15. Synthesis and characterization of vinyl-bridged polysilsesquioxane sol-gel materials

    SciTech Connect

    Yamanaka, S.A.; Carpenter, J.P.; McClain, M.D.; Loy, D.A.

    1995-08-01

    Vinyl-bridged polysilsesquioxane gels were formed through the use of sol-gel polymerization methods. Acid- and base-catalyzed samples were prepared from both the pure cis-(l) and pure trans-(2) isomers of 1, 2-bis(triethoxysilyl)ethylene. Gelation times of the two isomers were compared. The trans monomer 2 formed gels within a week while the cis monomer I failed to gel-even after several months. Gelation of 1 could be promoted by the addition of a coordinating metal such as palladium. The resulting cis- and trans- vinyl-bridged polysilsesquioxane gels were then processed either by vacuum drying to afford xerogels or by extracting with supercritical carbon dioxide to afford aerogels. These vinylbridged polysilsesquioxanes were characterized by SEM, nitrogen sorption porosimetry, solid State {sub 29}Si and {sub 13}C NMR and x-ray powder diffraction.

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

    NASA Astrophysics Data System (ADS)

    Lambert, Alexander Adam, III

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

  17. Photopolymerized sol-gel monoliths for separations of glycosylated proteins and peptides in microfluidic chips.

    PubMed

    Levy, Miriam H; Plawsky, Joel; Cramer, Steven M

    2013-07-01

    Photopolymerized silica sol-gel monoliths, functionalized with boronic acid ligands, have been developed for protein and peptide separations in polydimethylsiloxane microfluidic devices. Pore size characterization of the monoliths was carried out with SEM, image analysis, and differential scanning calorimetry to evaluate both the micron-sized macropores and the nanometer-sized mesopores. Monoliths were functionalized with boronic acid using three different immobilization techniques. Batch experiments were conducted to determine the capacity of the monoliths and selectivity toward cis-diol-containing compounds. Conalbumin was used as a model glycoprotein, and a tryptic digest of the glycoprotein horseradish peroxidase was used as a peptide mixture to demonstrate proof-of-concept extraction of glycoproteins and glycopeptides by the monoliths formulated in polydimethylsiloxane microfluidic chips. For proteins, fluorescence detection was used, whereas the peptide separations employed off-line analysis using MALDI-MS. PMID:23703808

  18. Dynamical transition of heat transport in a physical gel near the sol-gel transition

    PubMed Central

    Kobayashi, Kazuya U.; Oikawa, Noriko; Kurita, Rei

    2015-01-01

    We experimentally study heat transport in a gelatin solution near a reversible sol-gel transition point where viscosity strongly depends on temperature. We visualize the temperature field and velocity field using thermochromic liquid crystals and polystyrene latex particles, respectively. During the initial stages of heating, we find that heat transport undergoes a dynamical transition from conductive to convective. Subsequently, during later stages, we observe that the transport dynamics are much more complex than conventional thermal convections. At the sample’s surface we observe the formation of stagnant domains, which lack fluid flow. Their formation is not due to the effects of local cooling. We determine that it is the dynamics of these stagnant domains that induce convective-conductive-convective transitions. PMID:26690696

  19. Microbicidal activity of TiO2 nanoparticles synthesised by sol-gel method.

    PubMed

    Priyanka, Karathan Parakkandi; Sukirtha, Thiruvangium Henry; Balakrishna, Kagalagodu Manjunthiah; Varghese, Thomas

    2016-04-01

    In this study, the authors investigated antimicrobial activity of TiO2 nanoparticles (NPs) synthesised by sol-gel method. As synthesised TiO2 NPs were characterised by X-ray diffraction, scanning electron microscopy and ultraviolet-visible absorption spectroscopy. The antimicrobial activity of calcined TiO2 nanoparticle samples was examined in day light on Gram positive bacteria (Staphylococcus aureus, Streptococcus pneumonia and Bacillus subtilis), Gram negative bacteria (Proteus vulgaris, Pseudomonas aeruginosa and Escherichia coli) and fungal test pathogen Candida albicans. The synthesised TiO2 NPs were found to be effective in visible light against Streptococcus pneumonia, Staphylococcus aureus, Proteus vulgaris, Pseudomonas aeruginosa and Candida albicans. PMID:27074858

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

    NASA Astrophysics Data System (ADS)

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

    2014-08-01

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

  1. Synthesis of nano-sized lithium cobalt oxide via a sol-gel method

    NASA Astrophysics Data System (ADS)

    Li, Guangfen; Zhang, Jing

    2012-07-01

    In this study, nano-structured LiCoO2 thin film were synthesized by coupling a sol-gel process with a spin-coating method using polyacrylic acid (PAA) as chelating agent. The optimized conditions for obtaining a better gel formulation and subsequent homogenous dense film were investigated by varying the calcination temperature, the molar mass of PAA, and the precursor's molar ratios of PAA, lithium, and cobalt ions. The gel films on the silicon substrate surfaces were deposited by multi-step spin-coating process for either increasing the density of the gel film or adjusting the quantity of PAA in the film. The gel film was calcined by an optimized two-step heating procedure in order to obtain regular nano-structured LiCoO2 materials. Both atomic force microscopy (AFM) and scanning electron microscopy (SEM) were utilized to analyze the crystalline and the morphology of the films, respectively.

  2. Recent developments in silica sol-gel anti-reflection (AR) coatings

    SciTech Connect

    Sermon, P.A.; Vong, M.S.W.; Bazin, N.; Badheka, R.; Spriggs, D.

    1995-12-31

    Silica sol-gel anti-reflective (AR) coatings have been investigated with particular reference to their laser induced damage threshold (LIDT) when subjected to irradiation from a Nd pulse laser at 1,064nm. Coatings (whose thickness was optimized for minimum reflection at 1,064nm) were deposited by spinning silica sols (average particle size 15nm) produced formed by the base (ammonium hydroxide) catalyzed hydrolysis/condensation of TEOS in ethanol. Addition of polyethylene glycols (PEGs) increased the size of the colloidal silica particles and also induced some particle aggregation in the sol, unlike a similar chain length diol. Increases in the LIDT of the coatings possibly depend upon the impurity levels, the wettability of the substrate and the presence of PEG. LIDT improvements may be obtained by control of substrate and coating surface wettability, hydrophilicity and surface chemistry.

  3. Durable superhydrophobic and antireflective surfaces by trimethylsilanized silica nanoparticles-based sol-gel processing.

    PubMed

    Manca, Michele; Cannavale, Alessandro; De Marco, Luisa; Aricò, Antonino S; Cingolani, Roberto; Gigli, Giuseppe

    2009-06-01

    We present a robust and cost-effective coating method to fabricate long-term durable superhydrophobic andsimultaneouslyantireflective surfaces by a double-layer coating comprising trimethylsiloxane (TMS) surface-functionalized silica nanoparticles partially embedded into an organosilica binder matrix produced through a sol-gel process. A dense and homogeneous organosilica gel layer was first coated onto a glass substrate, and then, a trimethylsilanized nanospheres-based superhydrophobic layer was deposited onto it. After thermal curing, the two layers turned into a monolithic film, and the hydrophobic nanoparticles were permanently fixed to the glass substrate. Such treated surfaces showed a tremendous water repellency (contact angle = 168 degrees ) and stable self-cleaning effect during 2000 h of outdoor exposure. Besides this, nanotextured topology generated by the self-assembled nanoparticles-based top layer produced a fair antireflection effect consisting of more than a 3% increase in optical transmittance.

  4. 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.

  5. Magneto-structural studies of sol-gel synthesized nanocrystalline manganese substituted nickel ferrites

    NASA Astrophysics Data System (ADS)

    Pandav, R. S.; Patil, R. P.; Chavan, S. S.; Mulla, I. S.; Hankare, P. P.

    2016-11-01

    Nanocrystalline NiFe2-xMnxO4 (2≥x≥0) ferrites were prepared by sol-gel method. X-ray diffraction patterns reveal that synthesized compounds are in single phase cubic spinel lattice for all the composition. The surface morphology of all the samples were studied by scanning electron microscopy. The particle size measured from transmission electron microscopy and X-ray diffraction patterns confirms the nanosized dimension of the as-prepared powder. The elemental analysis was carried out by energy dispersive X-ray analysis technique. Magnetic properties such as saturation magnetization, coercivity and remanence are studied as a function of increasing Mn concentration at room temperature. The saturation magnetization shows a decreasing trend with increase in Mn content. The substitution of manganese in the nickel ferrite affects the structural and magnetic properties of cubic spinels.

  6. Sol-gel processing of highly transparent conducting Cd2SnO4 thin films

    NASA Astrophysics Data System (ADS)

    Bel-Hadj-Tahar, Radhouane; Bel-Hadj-Tahar, Noureddine; Belhadj Mohamed, Abdellatif

    2015-03-01

    Polycrystalline thin films of cadmium stannate (Cd2SnO4) (CTO) were coated on corning glass substrates by sol-gel method. The films were fired at different temperatures and annealed in inert ambient (N2) at 680°C. The structural, optical, and electrical properties of dip-coated cadmium-tin-oxide (CTO) thin films are discussed. CTO layers with a Hall mobility of 30 cm2/Vs and a carrier density of 1.4 × 1021 cm-3 resulting in a resistivity of 5 × 10-4 Ω cm have been deposited. Dip-coating conditions must be carefully monitored to produce consistent films. The high electronic conductivity is due to two effective mechanisms of n-type doping: (i) stoichiometric deviation and (ii) self-doping.

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

    PubMed

    Kayili, H Mehmet; Salih, Bekir

    2016-08-01

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

  8. Synthesis and Characterization of Pure and Doped Ceria Films by Sol-Gel and Sputtering

    SciTech Connect

    Koch, K.T.; Saraf, L.

    2004-01-01

    Pure and doped Ceria are known for their ability to gain or lose Oxygen, which is of interest to the Solid Oxide Fuel Cell (SOFC) and catalyst community. Current efforts are focused in SOFCs to reduce the operating temperature of the cell while maintaining ionic conduction. Ceria is known for its high ionic conductivity in the intermediate temperature region. (600-800° C) We have prepared pure and doped Ceria films by Sol-gel and magnetron sputtering methods. Enhanced grain-boundary contribution in the conductivity can be studied in the Sol-gel process due to excellent control over the synthesis conditions, which enabled us to control the average grain size. Sputtered films were grown and investigated as a prelude to possible multi-layered CeO2 structures in the near future. These films were characterized by X-ray diffraction (XRD), nuclear reaction analysis (NRA), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and Oxygen conduction measurements. We have observed greater volume diffusion in nanocrystalline Ceria compared to bulk polycrystalline films as a result of low density. Near surface diffusion properties with increasing temperature indicate a decrease in the volume diffusion as a result of grain growth. However, a linear increase in O2 content at ~600nm depth was observed and can be correlated to the redistribution of O2 in the samples. Surface roughness of <111> and <200> oriented Ceria films on Al2O3 and YSZ was observed to be 0.13nm and 0.397nm, respectively. In the case of Ceria grown on YSZ, structural properties from XRD results showed a highly oriented structure with cube on cube growth. XRD results from Ceria grown on Al2O3 showed an oriented structure whose degree of orientation appeared to be partially dependent on substrate temperature. Preliminary XPS results indicate reduction in Ceria from the Ce4+ to Ce3+ state near the surface.

  9. Pr(III) luminescence enhancement by chelation in solution and in sol-gel glass

    NASA Astrophysics Data System (ADS)

    Zaitoun, M. A.; El-Qisairi, A. K.; Momani, K. A.; Qaseer, H. A.; Jaradat, Q. M.

    2015-02-01

    Due to the weak emission of lanthanide ions in solution, it is common practice to form complexes of the lanthanide ions with organic ligands that strongly absorbs light and transfers the energy to the lanthanide ion center via the antenna effect. The organic ligands 2-6-pyridinedicarboxylate (L1) and the polytonic diazine (N-N) ligand L2 (C22H16N12O2) were used to synthesize two Pr(III) complexes, namely: Pr-L1 (Na3[Pr(C7H3NO4)3]) and Pr-L2. The prepared complexes were further encapsulated in an optically transparent sol-gel glass. The synthesized ligands and complexes were characterized by FTIR and 1H NMR. Room temperature luminescence of Pr-L1 and Pr-L2 complexes in solution and in sol-gel glass were investigated using a spectrofluorometer. Excitation at the maximum absorption wavelength of the ligands (280 nm) resulted in the typical visible luminescence (centered at around 600 nm) resulting from the 1D2 → 3H4 transition of the Pr(III) ion, which contributes to the efficient energy transfer from the absorbing ligand L1 to the chelated Pr(III) ion (an antenna effect) while the Pr(III) luminescence is not efficiently sensitized by ligand L2. The obtained emission spectra indicated that the excitation energy level for the central Pr(III) is in a slightly lower location than ligand L1 excitation triplet (T1) level and can accept the energy transfer from T1 efficiently.

  10. Diffusion of dissolved ions from wet silica sol-gel monoliths: implications for biological encapsulation.

    PubMed

    Dickson, David J; Lassetter, Bethany; Glassy, Benjamin; Page, Catherine J; Yokochi, Alexandre F T; Ely, Roger L

    2013-02-01

    Divalent nickel (Ni(2+)), Cu(II)EDTA, methyl orange, and dichromate were used to investigate diffusion from hydrated silica sol-gel monoliths. The objective was to examine diffusion of compounds on a size regime relevant to supporting biological components encapsulated within silica gel prepared in a biologically compatible process space with no post-gelation treatments. With an initial sample set, gels prepared from tetraethoxysilane were explored in a factorial design with Ni(2+) as the tracer, varying water content during hydrolysis, acid catalyst present during hydrolysis, and the final concentration of silica. A second sample set explored diffusion of all four tracers in gels prepared with aqueous silica precursors and a variety of organically modified siloxanes. Excluding six outliers which displayed significant syneresis, the mean diffusion constant (D(gel)) across the entire process space of sample set 1 was 2.42×10(-10) m(2) s(-1); approximately 24% of the diffusion coefficient of Ni(2+) in unconfined aqueous solution. In sample set 2, the tracer size and not gel hydrophobicity was the primary determinant of changes in diffusion rates. A strong linear inverse correlation was found between tracer size and the magnitude of D(gel). Based on correlation with the tracers used in this investigation, the characteristic 1-h diffusion distance for carbonate species relevant to supporting active phototrophic organisms was approximately 1.5mm. These results support the notion that silica sol-gel formulations may be optimized for a given biological entity of interest with manageable impact to the diffusion of small ions and molecules.

  11. Fluorescence of Pentavalent Chromium in SiO2 Sol-Gel Glasses

    NASA Technical Reports Server (NTRS)

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

    1998-01-01

    Chromium ions are very attractive to optical spectroscopy and laser physics. It is well known that the first laser in the history is a ruby laser activated with Cr(3+). It was found in early nineties that Cr(4+) was also an interesting lasing ion in the near infrared, and various Cr(4+) lasers have been developed. Very recently, it was reported that Cr(2+) doped in CdSe crystals showed lasing action in the infrared. The above achievement have stimulated an interest in searching for Cr(5+) and investigating its optical properties. Cr(5+) is isoelectronic with Ti(3+) and V(4+), having electron configuration 3d1. Ti(3+) is the active center of commercial cw and femtosecond sapphire lasers, tunable in the range 680-1100 nm. V(4+) doped in YAlO3 and Al2O3 showed broad band emission near 635 nm. Although EPR results of Cr(5+) were reported, the optical properties were less studied. Herren et al. reported an observation of luminescence from Cr doped in SiO2 sol-gel glass. The luminescence spectrum was assigned to pentavalent ions in their first paper, and later it was identified to be the emission from the charge transfer transition of Cr(6+). The first observation of photoluminescence from octahedrally coordinated Cr(5+) in BaCaMg aluminate glasses was reported very recently. In this work, we report luminescence results of Cr doped SiO2 sol-gel glasses. The fluorescence spectra are very different from Herrens' results, and we believe it originates from pentavalent Cr.

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

    PubMed Central

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

    2015-01-01

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

  13. Nano rods for coloured glasses obtained by hybrid sol-gel coating.

    PubMed

    Veron, Olivier; Blondeau, Jean-Philippe; Moineau, Johanne; Aubert, Pierre-Henri; Vignolle, Caroline Andreazza; Banet, Philippe; Allam, Lévi

    2011-09-01

    Many new materials are now allowing new properties thanks to nanotechnology because this domain of physics gives possibilities to optimize targeted properties even if these materials react in very various influential parameters. Architectural, automotive, bone pathologies, environment, display applications are some concerned domains. The sol-gel process is a method allowing the realisation of coats at ambiant temperature, thus it is possible to realize Liquid Crystal Display (LCD), water-repellent coatings on privacy glass, antireflective coatings, hydrophobic or hydrophilic surfaces, bone tissue regeneration. In this study, the purpose is to show the thermal influence on a covered glass with a complex hybrid sol-gel solution. This coated glass is going to change color from red to orange under the heat influence. This color change effect comes from the evolution of various compounds organizations then/or from their loss during the degassing sequence. We show in spite of the complexity of the process that the responsible is mainly the organic dye. Thus the structure of the heated glass at 250 degrees C looks radically different than the heated one at 350 degrees C. SEM measurement allows to identify the surface compositions and to determine the elementary composition along the sample's cross section. TGA is used to justify a mass loss when samples are annealed. UV/Visible measurement is realized by two methods: in-line transmission to evaluate luminous flux and thus give colorimetric dot in the normalized CIE diagram and diffuse transmission to observe the size influence of the pigments. Infrared Reflectivity allows to evaluate the influence of species on the structure and to better target the nature of the lost compounds during annealing. TEM measurement proves that the obtained iron particles are nano rods for both samples.

  14. Nano rods for coloured glasses obtained by hybrid sol-gel coating.

    PubMed

    Veron, Olivier; Blondeau, Jean-Philippe; Moineau, Johanne; Aubert, Pierre-Henri; Vignolle, Caroline Andreazza; Banet, Philippe; Allam, Lévi

    2011-09-01

    Many new materials are now allowing new properties thanks to nanotechnology because this domain of physics gives possibilities to optimize targeted properties even if these materials react in very various influential parameters. Architectural, automotive, bone pathologies, environment, display applications are some concerned domains. The sol-gel process is a method allowing the realisation of coats at ambiant temperature, thus it is possible to realize Liquid Crystal Display (LCD), water-repellent coatings on privacy glass, antireflective coatings, hydrophobic or hydrophilic surfaces, bone tissue regeneration. In this study, the purpose is to show the thermal influence on a covered glass with a complex hybrid sol-gel solution. This coated glass is going to change color from red to orange under the heat influence. This color change effect comes from the evolution of various compounds organizations then/or from their loss during the degassing sequence. We show in spite of the complexity of the process that the responsible is mainly the organic dye. Thus the structure of the heated glass at 250 degrees C looks radically different than the heated one at 350 degrees C. SEM measurement allows to identify the surface compositions and to determine the elementary composition along the sample's cross section. TGA is used to justify a mass loss when samples are annealed. UV/Visible measurement is realized by two methods: in-line transmission to evaluate luminous flux and thus give colorimetric dot in the normalized CIE diagram and diffuse transmission to observe the size influence of the pigments. Infrared Reflectivity allows to evaluate the influence of species on the structure and to better target the nature of the lost compounds during annealing. TEM measurement proves that the obtained iron particles are nano rods for both samples. PMID:22097469

  15. Rare Earth based Sol-Gel Materials: An Intra- and Inter- Collegiate Collaborative Research Project

    NASA Astrophysics Data System (ADS)

    Silversmith, Ann

    2004-03-01

    Sol-gel glasses containing rare earth (RE) impurities form an exciting class of new optical materials with potential uses as phosphors and solid state laser media. The low temperature glass synthesis based on the liquid organic precursor tetramethoxysilane allows incorporation of higher RE concentrations than in traditional melt glasses without compromising the amorphous character of the material. The synthesis and spectroscopic characterization of these materials have together formed the basis for a fruitful interdisciplinary and multi-institutional research collaboration. All materials used in this project are made by Hamilton College chemistry students; spectroscopy experiments are performed by students and faculty in the physics departments at Hamilton, Franklin and Marshall, and Davidson Colleges. In this talk results from two ongoing spectroscopic investigations will be presented, both connected to the long-term goal of improving the low fluorescence efficiency of these materials. The first is the chelation of the RE metal to create an enhanced fluorescence excitation path and to physically separate the RE from the sol-gel matrix. Chelating molecules absorb strongly in the uv, and subsequent energy transfer can produce intense visible emission from the RE. Results are presented for the chelating agent 2,6-pyridine-dicarboxylic acid (PDC) bound to europium ions and incorporated into gels. Red emission from europium follows excitation into the PDC absorption band below 300nm. The second investigation focuses on fluorescence quenching of blue emission from trivalent terbium. Two separate mechanisms -energy transfer from terbium to residual hydroxide ions and among terbium ions - lead to reduced intensity of the blue emission lines relative to other longer wavelength signals.

  16. Pr(III) luminescence enhancement by chelation in solution and in sol-gel glass.

    PubMed

    Zaitoun, M A; El-Qisairi, A K; Momani, K A; Qaseer, H A; Jaradat, Q M

    2015-02-01

    Due to the weak emission of lanthanide ions in solution, it is common practice to form complexes of the lanthanide ions with organic ligands that strongly absorbs light and transfers the energy to the lanthanide ion center via the antenna effect. The organic ligands 2-6-pyridinedicarboxylate (L1) and the polytonic diazine (N-N) ligand L2 (C22H16N12O2) were used to synthesize two Pr(III) complexes, namely: Pr-L1 (Na3[Pr(C7H3NO4)3]) and Pr-L2. The prepared complexes were further encapsulated in an optically transparent sol-gel glass. The synthesized ligands and complexes were characterized by FTIR and (1)H NMR. Room temperature luminescence of Pr-L1 and Pr-L2 complexes in solution and in sol-gel glass were investigated using a spectrofluorometer. Excitation at the maximum absorption wavelength of the ligands (280nm) resulted in the typical visible luminescence (centered at around 600nm) resulting from the (1)D2→(3)H4 transition of the Pr(III) ion, which contributes to the efficient energy transfer from the absorbing ligand L1 to the chelated Pr(III) ion (an antenna effect) while the Pr(III) luminescence is not efficiently sensitized by ligand L2. The obtained emission spectra indicated that the excitation energy level for the central Pr(III) is in a slightly lower location than ligand L1 excitation triplet (T1) level and can accept the energy transfer from T1 efficiently. PMID:25467665

  17. Formulation and Performance of Novel Energetic Nanocomposites and Gas Generators Prepared by Sol-Gel Methods

    SciTech Connect

    Clapsaddle, B J; Zhao, L; Prentice, D; Pantoya, M L; Gash, A E; Satcher Jr., J H; Shea, K J; Simpson, R L

    2005-03-24

    In the field of composite energetic materials, properties such as ingredient distribution, particle size, and morphology affect both sensitivity and performance. Since the reaction kinetics of composite energetic materials are typically controlled by the mass transport rates between reactants, one would anticipate new and potentially exceptional performance from energetic nanocomposites. We have developed a new method of making nanostructured energetic materials, specifically explosives, propellants, and pyrotechnics, using sol-gel chemistry. A novel sol-gel approach has proven successful in preparing nanostructured metal oxide materials. By introducing a fuel metal, such as aluminum, into the nanostructured metal oxide matrix, energetic materials based on thermite reactions can be fabricated. Two of the metal oxides are tungsten trioxide and iron(III) oxide, both of which are of interest in the field of energetic materials. Due to the versatility of the preparation method, binary oxidizing phases can also be prepared, thus enabling a potential means of controlling the energetic properties of the subsequent nanocomposites. Furthermore, organic additives can also be easily introduced into the nanocomposites for the production of nanostructured gas generators. The resulting nanoscale distribution of all the ingredients displays energetic properties not seen in its micro-scale counterparts due to the expected increase of mass transport rates between the reactants. The unique synthesis methodology, formulations, and performance of these materials will be presented. The degree of control over the burning rate of these nanocomposites afforded by the compositional variation of a binary oxidizing phase will also be discussed. These energetic nanocomposites have the potential for releasing controlled amounts of energy at a controlled rate. Due to the versatility of the synthesis method, a large number of compositions and physical properties can be achieved, resulting in

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

    NASA Astrophysics Data System (ADS)

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

    2010-07-01

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

  19. Direct Evidence for Percolation of Immobilized Polymer Layer around Nanoparticles Accounting for Sol-Gel Transition in Fumed Silica Dispersions.

    PubMed

    Zheng, Zhong; Song, Yihu; Yang, Ruiquan; Zheng, Qiang

    2015-12-22

    Immobilized polymer fractions have been claimed to be of vital importance for sol-gel transitions generally observed in nanoparticle dispersions but remain a matter of debate regarding mechanism and difficulty for prediction. Here we investigate the immobilized layer structures of trifunctionality polyether polyol (PPG) near the surfaces of hydrophilic and hydrophobic fumed silica (FS) nanoparticles to reveal the role of surface chemistry on the molecular dynamics and sol-gel transitions of the dispersions. Using modulated differential scanning calorimetry, we measure the specific heat capacity during glass transition and the enthalpy during cold-crystallization. Comparing with hydrophobic FS that forms a fully immobilized (glassy) layer, we find that hydrophilic FS immobilizes more PPG, forming a partially immobilized outer layer being unable to crystallize next to the inner glassy layer. By correlating the thickness of the glassy layer with half of the minimum spacing between nanoparticles, we directly evidence the percolation of this layer along the nearest neighbor nanoparticles responsible for the sol-gel transition. Using effective volume fraction including the glassy layer, we successfully construct master curves of relative viscosity of both hydrophilic and hydrophobic FS dispersions, pointing to a common sol-gel transition mechanism mediated by the surface chemistry.

  20. ELISA AND SOL-GEL BASED IMMUNOAFFINITY PURIFICATION OF THE PYRETHROID BIOALLETHRIN IN FOOD AND ENVIRONMENTAL SAMPLES

    EPA Science Inventory

    The peer-reviewed article describes the development of a new sol-gel based immunoaffinity purification procedure and an immunoassay for the pyrethroid bioallethrin. The immunoaffinity chromatography procedure was applied to food samples providing an efficient cleanup prior to im...