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Sample records for sol-gel derived ceramic

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    NARCIS (Netherlands)

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

    1995-01-01

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

  3. Sol-gel derived multiwalled carbon nanotubes ceramic electrode modified with molecularly imprinted polymer for ultra trace sensing of dopamine in real samples

    Energy Technology Data Exchange (ETDEWEB)

    Prasad, Bhim Bali, E-mail: prof.bbpd@yahoo.com [Department of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi 221 005 (India); Kumar, Deepak; Madhuri, Rashmi; Tiwari, Mahavir Prasad [Department of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi 221 005 (India)

    2011-08-01

    Highlights: > MWCNTs-CE was prepared by silane acrylate which provides a nanometer thin MIP film. > The sensor was modified by iniferter and MIP using 'surface grafting-from approach'. > A comparative study was performed between differentially designed ceramic electrodes. > The sensor can detect dopamine in real samples with LODs (0.143-0.154 ng mL{sup -1}). - Abstract: A new class of composite electrodes made of sol-gel derived ceramic-multiwalled carbon nanotubes is used for the growth of a nanometer thin film adopting 'surface grafting-from approach'. For this the multiwalled carbon nanotubes-ceramic electrode surface is first modified with an iniferter (benzyl N,N-diethyldithiocarbamate) and then dopamine imprinted polymer, under UV irradiation, for differential pulse anodic stripping voltammetric sensing of dopamine in aqueous, blood serum, cerebrospinal fluid, and pharmaceutical samples (detection limit 0.143-0.154 ng mL{sup -1}, 3{sigma}), without any cross reactivity, interferences and false-positive contributions. Such composite electrodes offer higher stability, electron kinetics, and renewable porous surface of larger electroactive area (with insignificant capacitance) than carbon ceramic electrodes. Additional cyclic voltammetry (stripping mode) and chronocoulometry experiments were performed to explore electrodics and kinetics of electro-oxidation of dopamine.

  4. A new sol-gel process for producing Na(2)O-containing bioactive glass ceramics.

    Science.gov (United States)

    Chen, Qi-Zhi; Li, Yuan; Jin, Li-Yu; Quinn, Julian M W; Komesaroff, Paul A

    2010-10-01

    The sol-gel process of producing SiO(2)-CaO bioactive glasses is well established, but problems remain with the poor mechanical properties of the amorphous form and the bioinertness of its crystalline counterpart. These properties may be improved by incorporating Na(2)O into bioactive glasses, which can result in the formation of a hard yet biodegradable crystalline phase from bioactive glasses when sintered. However, production of Na(2)O-containing bioactive glasses by sol-gel methods has proved to be difficult. This work reports a new sol-gel process for the production of Na(2)O-containing bioactive glass ceramics, potentially enabling their use as medical implantation materials. Fine powders of 45S5 (a Na(2)O-containing composition) glass ceramic have for the first time been successfully synthesized using the sol-gel technique in aqueous solution under ambient conditions, with the mean particle size being approximately 5 microm. A comparative study of sol-gel derived S70C30 (a Na(2)O-free composition) and 45S5 glass ceramic materials revealed that the latter possesses a number of features desirable in biomaterials used for bone tissue engineering, including (i) the crystalline phase Na(2)Ca(2)Si(3)O(9) that couples good mechanical strength with satisfactory biodegradability, (ii) formation of hydroxyapatite, which may promote good bone bonding and (iii) cytocompatibility. In contrast, the sol-gel derived S70C30 glass ceramic consisted of a virtually inert crystalline phase CaSiO(3). Moreover, amorphous S70C30 largely transited to CaCO(3) with minor hydroxyapatite when immersed in simulated body fluid under standard tissue culture conditions. In conclusion, sol-gel derived Na(2)O-containing glass ceramics have significant advantages over related Na(2)O-free materials, having a greatly improved combination of mechanical capability and biological absorbability. 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  5. Eu3+ probe ion for rare-earth dopant site structure in sol-gel derived LiYF4 oxyfluoride glass-ceramic

    Science.gov (United States)

    Secu, C. E.; Negrea, R. F.; Secu, M.

    2013-10-01

    Sol-gel route using metal alkoxides and trifluoroacetic acid as precursors has been used to prepare oxyfluoride glass-ceramic containing Eu3+-doped LiYF4 nanocrystals of about tens of nm size embedded in a silica matrix through controlled crystallization at higher temperatures of the xerogel. Photoluminescence spectra and decay curves recorded in the Eu3+-doped LiYF4 polycrystalline pellet and glass ceramic have been discussed using group-theoretical arguments. In the glass-ceramic Eu3+ ions are embedded dominantly inside the LiYF4 nanocrystals most probably as Eu-O center and/or dimer centers in low symmetry (C2v) sites; oxygen ions were incorporated in their neighborhood during the glass ceramization.

  6. Site-selective spectroscopy in Sm{sup 3+}-doped sol-gel-derived nano-glass-ceramics containing SnO{sub 2} quantum dots

    Energy Technology Data Exchange (ETDEWEB)

    Yanes, A C; Castillo, J del [Departamento de Fisica Basica, Universidad de La Laguna, E-38206 La Laguna, Tenerife (Spain); Velazquez, J J; Mendez-Ramos, J; RodrIguez, V D [Departamento de Fisica Fund. y Experimental, Universidade La Laguna, E-38206 La Laguna, Tenerife (Spain)], E-mail: ayanesh@ull.es, E-mail: vrguez@ull.es

    2008-07-23

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

  7. Sol-gel synthesis of carbon based materials reinforced ultra high temperature ceramic composites

    OpenAIRE

    Wang, Xiaojing

    2017-01-01

    This Ph.D. research is based on the development of novel sol-gel techniques for synthesis of nanostructured ultra high temperature ceramics (UHTCs) and subsequent spark plasma sintering (SPS) for densifying the UHTC composites. The liquid nature of the sol-gel process offers advantages such as high purity and ability for mixing and infiltration, and thus it can overcome some shortcomings of the conventional power processing of ceramics. SPS delivers microstructures with good density and fine ...

  8. White phosphor using Yb3+-sensitized Er3+-and Tm3+-doped sol-gel derived lead-fluorosilicate transparent glass ceramic excited at 980 nm

    Science.gov (United States)

    Tavares, M. C. P.; da Costa, E. B.; Bueno, L. A.; Gouveia-Neto, A. S.

    2018-01-01

    Generation of primary colors and white light through frequency upconversion using sol-gel derived 80SiO2:20PbF2 vitroceramic phosphors doped with Er3+, Er3+/Yb3+, Tm3+/Yb3+, and Er3+/Tm3+/Yb3+ excited at 980 nm is demonstrated. For Er3+ and Er3+/Yb3+ doped samples emissions were obtained in the blue (410 nm), green (530, and 550 nm) and red (670 nm) regions, corresponding to the 2H9/2 → 4I15/2,2H11/2 → 4I15/2, 4S3/2 → 4I152 and 4F9/2 → 4I15/2 transitions of Er3+, respectively. The codoping with Yb3+ ions altered the spectral profile of most of the emissions compared to the single doped samples, resulting in changes in the emitted color, in addition to a significant increase in the emission intensity. In Tm3+/Yb3+ co-doped samples visible emissions in the blue (480 nm), and red (650 nm), corresponding to transitions 1G4 → 3H6 and 1G4 → 3F4 of Tm3+, respectively, were obtained. The emission intensity around 480 nm overcome the red emission, and luminescence showed a predominantly blue tone. White light with CIE-1931 coordinates (0.36; 0.34) was produced by homogeneously mixing up powders of heat treated at 400 °C co-doped samples 5.0Er3+/5.0Yb3+ and 0.5Tm3+/2.5Yb3+ in the mass ratio of 13%, and 87%, respectively. The measured emission spectrum for a sample resulting from the mixture showed a profile with very good agreement with the spectrum found from the superimposition of the spectra of the co-doped samples.

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

    Science.gov (United States)

    Shankhwar, Nisha; Srinivasan, A

    2016-05-01

    Multicomponent oxide powders with nominal compositions of (45-x)·SiO2·24.5CaO·24.5Na2O·6P2O5xFe2O3 (in wt.%) were prepared by a modified sol-gel procedure. X-ray diffraction (XRD) patterns and high resolution transmission electron microscope images of the sol-gel products show fully amorphous structure for Fe2O3 substitutions up to 2 wt.%. Sol-gel derived 43SiO2·24.5CaO·24.5Na2O·6P2O5·2Fe2O3 glass (or bioglass 45S5 with SiO2 substituted with 2 wt.% Fe2O3), exhibited magnetic behavior with a coercive field of 21 Oe, hysteresis loop area of 33.25 erg/g and saturation magnetization of 0.66 emu/g at an applied field of 15 kOe at room temperature. XRD pattern of this glass annealed at 850 °C for 1h revealed the formation of a glass-ceramic containing sodium calcium silicate and magnetite phases in nanocrystalline form. Temperature dependent magnetization and room temperature electron spin resonance data have been used to obtain information on the magnetic phase and distribution of iron ions in the sol-gel glass and glass-ceramic samples. Sol-gel derived glass and glass-ceramic exhibit in-vitro bioactivity by forming a hydroxyapatite surface layer under simulated physiological conditions and their bio-response is superior to their melt quenched bulk counterparts. This new form of magnetic bioglass and bioglass ceramics opens up new and more effective biomedical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, A.J., E-mail: antoniojulio.lopez@urjc.es [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain); Rico, A.; Rodriguez, J.; Rams, J. [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain)

    2010-08-15

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

  11. Sol-Gel Derived, Nanostructured Oxide Lubricant Coatings

    National Research Council Canada - National Science Library

    Taylor, Douglas

    2000-01-01

    In this program, we deposited oxide coatings of titanium and nickel by wet-chemical deposition methods, also referred to as sol-gel, which showed excellent tribological properties in previous investigations...

  12. Wide colour gamut generated in triply lanthanide doped sol-gel nano-glass-ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Castillo, J. del, E-mail: fjvargas@ull.e [Universidad de La Laguna, Dpto. Fisica Basica (Spain); Mendez-Ramos, J. [Universidad de La Laguna, Dpto. Fisica Fundamental y Experimental, Electronica y Sistemas (Spain); Yanes, A. C. [Universidad de La Laguna, Dpto. Fisica Basica (Spain); Rodriguez, V. D. [Universidad de La Laguna, Dpto. Fisica Fundamental y Experimental, Electronica y Sistemas (Spain)

    2009-05-15

    The generation of a wide colour gamut, based on up-conversion of cheap near-infrared photons into the visible range, is of great importance for general lighting appliances and integrated optical devices. Here, we report for the first time on up-conversion luminescence under infrared excitation at 980 nm in Yb{sup 3+}-Er{sup 3+}-Tm{sup 3+} triply doped sol-gel derived SiO{sub 2}-LaF{sub 3} based nano-glass-ceramics (SOL-YET), containing LaF{sub 3} nanocrystals with a size about 13 nm. Efficient simultaneous up-conversion emission of the three primary colours (blue, green and red) gives rise to a balanced white overall emission. The ratio between up-conversion emission bands can be varied by changing pump power intensity resulting in colour tuneable up-conversion phosphor.

  13. Sol-gel route to functional and hierarchical ceramic matrix composites

    Science.gov (United States)

    Colomban, Ph.

    1996-04-01

    The use of sol-gel technique to fabricate functionally graded ceramic matrix composites reinforced with woven fibers is illustrated with composites made by alternating dielectric and conducting layers (microwave absorbent) or by alternating materials that have high hardness and good corrosion resistance. Emphasis on the preparation of multiscale reinforced composites is given according to the idea of biomimetic materials.

  14. Iron Oxide Silica Derived from Sol-Gel Synthesis

    Directory of Open Access Journals (Sweden)

    João Carlos Diniz da Costa

    2011-02-01

    Full Text Available In this work we investigate the effect of iron oxide embedded in silica matrices as a function of Fe/Si molar ratio and sol pH. To achieve homogeneous dispersion of iron oxide particles, iron nitrate nonahydrate was dissolved in hydrogen peroxide and was mixed with tetraethyl orthosilicate and ethanol in a sol-gel synthesis method. Increasing the calcination temperature led to a reduction in surface area, although the average pore radius remained almost constant at about 10 Å, independent of the Fe/Si molar ratio or sol pH. Hence, the densification of the matrix was accompanied by similar reduction in pore volume. However, calcination at 700 °C resulted in samples with similar surface area though the iron oxide content increased from 5% to 50% Fe/Si molar ratio. As metal oxide particles have lower surface area than polymeric silica structures, these results strongly suggest that the iron oxides opposed the silica structure collapse. The effect of sol pH was found to be less significant than the Fe/Si molar ratio in the formation of molecular sieve structures derived from iron oxide silica.

  15. Up-conversion in nanostructured Yb{sup 3+}-Tm{sup 3+} co-doped sol-gel derived SiO{sub 2}-LaF{sub 3} transparent glass-ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Mendez-Ramos, J.; Velazquez, J.J. [Departamento de Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Yanes, A.C.; Del-Castillo, J. [Departamento de Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Rodriguez, V.D.

    2008-02-15

    Nanostructured transparent glass-ceramics with composition of 95SiO{sub 2}-5LaF{sub 3} doped with 0.1 mol% of Tm{sup 3+} or co-doped with 0.1 mol% of Tm{sup 3+} and 0.3 mol% of Yb{sup 3+} were synthesized by thermal treatment of precursor sol-gel derived glasses. A comparative luminescence analysis in terms of different temperatures of thermal treatments has been carried out. Segregation of LaF{sub 3} nanocrystals in the matrix was confirmed by X-ray diffraction. Blue and red efficient up-conversion emissions were observed under 980 nm excitation at room temperature. These results indicate partition of a significant fraction of co-dopants into the precipitated LaF{sub 3} nanocrystals. The mechanisms involved in the up-conversion emissions have been analyzed and can be ascribed to processes with two, three and four photons. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  16. Sol-Gel Derived Mg-Based Ceramic Scaffolds Doped with Zinc or Copper Ions: Preliminary Results on Their Synthesis, Characterization, and Biocompatibility

    National Research Council Canada - National Science Library

    Theodorou, Georgios S; Kontonasaki, Eleana; Theocharidou, Anna; Bakopoulou, Athina; Bousnaki, Maria; Hadjichristou, Christina; Papachristou, Eleni; Papadopoulou, Lambrini; Kantiranis, Nikolaos A; Chrissafis, Konstantinos; Paraskevopoulos, Konstantinos M; Koidis, Petros T

    2016-01-01

      Glass-ceramic scaffolds containing Mg have shown recently the potential to enhance the proliferation, differentiation, and biomineralization of stem cells in vitro, property that makes them promising...

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

    Science.gov (United States)

    Han, Kuo

    Sol-gel process is a simple chemistry to convert the small precursor molecules into an inorganic polymer, which could be applied to synthesize inorganic materials, modify the interface of materials, bridge the organic and inorganic materials, etc. In this dissertation, novel sol-gel derived composites have been developed for high dielectric breakdown capacitors, low high frequency loss capacitors and flexible piezoelectrics. Numerous efforts have been made in the past decades to improve the energy storage capability of composite materials by incorporating nanometer scale ceramic addictives with high dielectric permittivity into dielectric polymers with high breakdown strength. However, most composites suffer from the low breakdown strength and make the potential gain in energy density small. Here, a new chemical strategy is proposed that, through sol-gel reactions between ceramic precursors and functional groups at the end of the functionalized Poly(vinylidene fluoride -co-chlorotrifluoroethylene) chains, amorphous low permittivity ceramics was in-situ generated in the polymer matrix and cross-linked the polymer chains simultaneously. By carefully tuning precursors, the polymer/precursors feeding ratios, a series of nanocomposites were systematically designed. All the samples are comprehensively characterized and the structure-property correlations are well investigated. The optimal samples exhibit higher breakdown strength than the pristine polymer. The enhanced breakdown strength ascribed to low contrast in permittivity, great dispersion and improved electrical and mechanical properties. This newly developed approach has shown great promise for new composite capacitors. The percolative polymer composites have recently exhibited great potential in energy storage due to their high dielectric permittivities at the neighborhood of the percolation threshold. Yet high energy dissipation and poor voltage endurance of the percolative composites resulted from electrical

  18. Oxide Ceramic Fibers by the Sol-Gel Methods

    Science.gov (United States)

    1989-02-10

    improved fuel efficiency, reduced weight and greater thrust -to -weight ratio. Using ceramic materials also decreases the dependence on strategic...heating element by Archimedes method. Sample Bulk Apparent Percent Density Density Porosity (g/cc) O (%) End Sample 4.72 6.48 27.1 (High Ca) Middle

  19. Sol-gel synthesis and structure of cordierite/tialite glass-ceramics

    Directory of Open Access Journals (Sweden)

    Lachezar Radev

    2009-09-01

    Full Text Available In the present work the results of the research on the sol-gel synthesis and structure of cordierite (2MgO·2Al2O3·5SiO2, tialite (Al2O3·TiO2 and cordierite/tialite glass-ceramics as well cordierite containing 2 wt.% of Co and Co+Cu have been described and discussed. The sol-gel synthesis was carried out using different kind of precursors as follows: Al(NO3×9H2O, Si(OC2H54 , Ti(OC4H94 , Mg(NO32×6H2O, chlorides or nitrates of corresponding metals, H2O, C2H5OH, Aqua Regia, NH4F and PEG. The synthesized gels were dried and thermally treated in the temperature range from 800°C to 1200°C. The sol-gel processes and structure of the cordierite, tialite and cordierite/tialite glass-ceramics have been investigated by means of XRD, FTIR, TEM, SEM and EPMA.

  20. Sol-Gel Derived Mg-Based Ceramic Scaffolds Doped with Zinc or Copper Ions: Preliminary Results on Their Synthesis, Characterization, and Biocompatibility

    Directory of Open Access Journals (Sweden)

    Georgios S. Theodorou

    2016-01-01

    Full Text Available Glass-ceramic scaffolds containing Mg have shown recently the potential to enhance the proliferation, differentiation, and biomineralization of stem cells in vitro, property that makes them promising candidates for dental tissue regeneration. An additional property of a scaffold aimed at dental tissue regeneration is to protect the regeneration process against oral bacteria penetration. In this respect, novel bioactive scaffolds containing Mg2+ and Cu2+ or Zn2+, ions known for their antimicrobial properties, were synthesized by the foam replica technique and tested regarding their bioactive response in SBF, mechanical properties, degradation, and porosity. Finally their ability to support the attachment and long-term proliferation of Dental Pulp Stem Cells (DPSCs was also evaluated. The results showed that conversely to their bioactive response in SBF solution, Zn-doped scaffolds proved to respond adequately regarding their mechanical strength and to be efficient regarding their biological response, in comparison to Cu-doped scaffolds, which makes them promising candidates for targeted dental stem cell odontogenic differentiation and calcified dental tissue engineering.

  1. White light up-conversion in transparent sol-gel derived glass-ceramics containing Yb{sup 3+}-Er{sup 3+}-Tm{sup 3+} triply-doped YF{sub 3} nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Santana-Alonso, A. [Departamento Fisica Basica, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Mendez-Ramos, J. [Departamento Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Yanes, A.C., E-mail: ayanesh@ull.es [Departamento Fisica Basica, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Castillo, J. del [Departamento Fisica Basica, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Rodriguez, V.D. [Departamento Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain)

    2010-11-01

    Transparent glass-ceramics containing YF{sub 3} nanocrystals triply-doped with Yb{sup 3+}-Er{sup 3+}-Tm{sup 3+} ions have been successfully obtained under adequate thermal treatment of precursor sol-gel glasses for the first time to our knowledge. X-ray diffraction and high resolution transmission electron microscopy analysis pointed out the precipitation of YF{sub 3} nanocrystals. Up-conversion luminescence features confirm the effective partition of luminescent ions into precipitated nanocrystals. Corresponding energy transfer up-conversion mechanisms and the dependence of the overall emitting colour have been analyzed as a function of doping ions, with varying concentration. In particular, very bright and efficient up-conversion emission, almost matching the standard equal energy white light illumination point of the standard chromaticity diagram, has been achieved showing up as promising candidate material for potential applications in photonic integrated devices and infrared tuneable phosphors.

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

    Energy Technology Data Exchange (ETDEWEB)

    Petcu, Cristian; Purcar, Violeta [National Research-Development Institute for Chemistry and Petrochemistry-ICECHIM, Polymer Department, Splaiul Independentei 202, 6th district, 060021, Bucharest (Romania); Ianchiş, Raluca, E-mail: ralumoc@yahoo.com [National Research-Development Institute for Chemistry and Petrochemistry-ICECHIM, Polymer Department, Splaiul Independentei 202, 6th district, 060021, Bucharest (Romania); Spătaru, Cătălin-Ilie; Ghiurea, Marius; Nicolae, Cristian Andi [National Research-Development Institute for Chemistry and Petrochemistry-ICECHIM, Polymer Department, Splaiul Independentei 202, 6th district, 060021, Bucharest (Romania); Stroescu, Hermine [Institute of Physical Chemistry “Ilie Murgulescu” of the Romanian Academy, Splaiul Independentei 202, 060021, Bucharest (Romania); Atanase, Leonard-Ionuţ [University Apollonia, “Acad. Ioan Haulica” Research Institute, Iasi (Romania); Frone, Adriana Nicoleta; Trică, Bogdan; Donescu, Dan [National Research-Development Institute for Chemistry and Petrochemistry-ICECHIM, Polymer Department, Splaiul Independentei 202, 6th district, 060021, Bucharest (Romania)

    2016-12-15

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

  3. Residual stress fields in sol-gel-derived thin TiO2 layers

    NARCIS (Netherlands)

    Teeuw, D.H.J.; Haas, M. de; Hosson, J.Th.M. De

    1999-01-01

    This paper discusses the induction of residual stresses during the curing process of thin titania layers, which are derived using a sol-gel process. During this process, stresses may build up in the spinning stage, the drying stage, and the consolidation stage. The magnitude and character of these

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

    NARCIS (Netherlands)

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

    1999-01-01

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

  5. Sulfur dioxide removal by sol-gel sorbent derived CuO/Alumina sorbents in fixed bed adsorber

    Directory of Open Access Journals (Sweden)

    Zhong-Min Wang

    2017-02-01

    Full Text Available Nanostructured alumina supported copper oxide granular sorbents were prepared by the sol-gel method. The properties of the sol-gel derived sorbents were compared with a similar commercial sorbent which has been used in the pilot scale moving-bed copper oxide process for flue gas treatment. The crushing strength of the sol-gel derived sorbents is about 6–7 times that of the commercial samples, while the attrition rate of the former is at least 3 times smaller. At temperatures below 400 °C, SO2 sorption capacity of the sol-gel derived sorbent is about 3 times that of the commercial sorbent with a similar amount of CuO loading (7–9 wt%. The better mechanical properties and higher sulfation capacity of the sol-gel derived alumina supported copper oxide sorbents are due to their unique microstructure and the coating method for CuO.

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

    Energy Technology Data Exchange (ETDEWEB)

    Brinkman, K

    2009-01-08

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

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

    Science.gov (United States)

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

    2017-11-01

    The purpose of this study was to evaluate the effect of sol-gel derived bioactive coatings on the biaxial flexural strength and fibroblast proliferation of zirconia, aimed to be used as an implant abutment material. Yttrium stabilized zirconia disc-shaped specimens were cut, ground, sintered, and finally cleansed ultrasonically in each of acetone and ethanol for 5 minutes. Three experimental groups (n = 15) were fabricated, zirconia with sol-gel derived titania (TiO2 ) coating, zirconia with sol-gel derived zirconia (ZrO2 ) coating, and non-coated zirconia as a control. The surfaces of the specimens were analyzed through images taken using a scanning electron microscope (SEM), and a non-contact tapping mode atomic force microscope (AFM) was used to record the surface topography and roughness of the coated specimens. Biaxial flexural strength values were determined using the piston-on-three ball technique. Human gingival fibroblast proliferation on the surface of the specimens was evaluated using AlamarBlue assay™. Data were analyzed using a one-way analysis of variance (ANOVA) followed by Tukey's post-hoc test. Additionally, the biaxial flexural strength data was also statistically analyzed with the Weibull distribution. The biaxial flexural strength of zirconia specimens was unaffected (p > 0.05). Weibull modulus of TiO2 coated and ZrO2 coated groups (5.7 and 5.4, respectively) were lower than the control (8.0). Specimens coated with ZrO2 showed significantly lower fibroblast proliferation compared to other groups (p sol-gel derived coatings have no influence on the flexural strength of zirconia. ZrO2 coated specimens showed significantly lower cell proliferation after 12 days than TiO2 coated or non-coated control. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 2401-2407, 2017. © 2016 Wiley Periodicals, Inc.

  8. Densification and properties of Sol-Gel derived PZT-fibers for 1-3 composites

    Energy Technology Data Exchange (ETDEWEB)

    Scholz, H.; Sporn, D.; Ullrich, A. [Fraunhofer-Institut fuer Silicatforschung, Wuerzburg (Germany)

    1995-09-01

    The microstructural evolution of sol-gel derived PZT-fibers is strongly dependent on the atmosphere and the T/t-schedule of drying, pyrolysis and sintering. The PbO-partial pressure during sintering plays a key role for grain growth and densification of the PZT-fibers. Fiber density, grain size and the fiber load in the polymer matrix affect the dielectric and ferroelectric properties of the 1-3 composite.

  9. Residual stress fields in sol-gel-derived thin TiO2 layers

    OpenAIRE

    Teeuw, D.H.J.; Haas, M.; De Hosson, J.Th.M.

    1999-01-01

    This paper discusses the induction of residual stresses during the curing process of thin titania layers, which are derived using a sol-gel process. During this process, stresses may build up in the spinning stage, the drying stage, and the consolidation stage. The magnitude and character of these stresses depend heavily on the morphology of the layers in the various stages and the processing conditions. Dried layers are densified using two different processes, conventional furnace heating an...

  10. Effects of sol-gel processed silica coating on bond strength of resin cements to glass-infiltrated alumina ceramic.

    Science.gov (United States)

    Xie, Haifeng; Wang, Xiaozu; Wang, Yu; Zhang, Feimin; Chen, Chen; Xia, Yang

    2009-02-01

    The aim of this study was to verify the effects of sol-gel processed silica coating on the bond strength between resin cement and glass-infiltrated aluminum oxide ceramic. Silica coatings were prepared on glass-infiltrated aluminum oxide ceramic surface via the sol-gel process. Atomic Force Microscope (AFM), Fourier Transmission Infrared spectrum (FTIR), and Energy Dispersive X-ray Spectroscopy (EDS) were used for coating characterization. Forty-eight blocks of glass-infiltrated aluminum oxide ceramic were fabricated. The ceramic surfaces were polished following sandblasting. Three groups of specimens (16 for each group) with different surface treatment were prepared. Group P: no treatment; group PO: treated with silane solution; group PTO: silica coating via sol-gel process, followed by silane application. Composite cylinders were luted with resin cement to the test specimens. Half of the specimens in each group were stored in distilled water for 24 h and the other half were stored in distilled water for 30 days before shear loading in a universal testing machine until failure. Selected ceramic surfaces were analyzed to identify the failure mode using a scanning electron microscopy (SEM). Nanostructured silica coatings were prepared on glass-infiltrated aluminum oxide ceramic surfaces by the sol-gel process. The silicon element on the ceramic surface increased significantly after the coating process. The mean shear bond strength values (standard deviation) before artificial aging were: group P: 1.882 +/- 0.156 MPa; group PO: 2.177 +/- 0.226 MPa; group PTO: 3.574 +/- 0.671 MPa. Statistically significant differences existed between group PTO and group P, and group PTO and groups PO. The failure mode for group P and group PO was adhesive, while group PTO was mixed. The mean shear bond strength values (standard deviation) after artificial aging were: group P: 1.594 +/- 0.111 MPa; group PO: 2.120 +/- 0.339 MPa; group PTO: 2.955 +/- 0.113 MPa. Statistically significant

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

    Directory of Open Access Journals (Sweden)

    Woobin Lee

    2015-12-01

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

  12. Application of the Sol-Gel Method at the Fabrication of PLZT:Yb3+ Ceramics

    Directory of Open Access Journals (Sweden)

    Osińska K.

    2016-09-01

    Full Text Available The aim of presented study was to obtain the PLZT:Yb3+ ceramics. Nanopowders of itterbium doped PLZT materials were synthesized by the sol-gel method from high quality metaloorganic precursors, as lead (II acetate, lanthanum acetate, ytterbium acetate, zirconium (IV propoxide and titanium (IV propoxide. Anhydrous acetic acid and n-propyl alcohol were used as solvents, while acetyloacetone was added as stabilizer of hydrolysis reactions. Thermal evolution of the dried gels, before and after calcination, was studied by the simultaneous thermal analysis. The amorphous PLZT:Yb3+ gels were first calcined in the furnace at T = 850°C, and then mixed in the planetary ball mill. Additionally, the mean particle sizes were calculated by means of powder specific surface area measurements, based on the BET physical adsorption isotherm. Such obtained powders were subsequently pressed into pellets, and sintered by the free sintering method at temperature T = 1250°C / 6h. The morphology of fabricated PLZT:Yb3+ ceramic powders and samples was studied using Scanning Electron Microscopy. Chemical characterization of samples was carried on using the Energy-dispersive X-ray spectroscopy - EDS system. Studies provided detailed data concerning the relationships between doping and preparing conditions on the basic physical and chemical properties of obtained ceramic materials.

  13. Life Cycle Assessment for Proton Conducting Ceramics Synthesized by the Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Soo-Sun Lee

    2014-09-01

    Full Text Available In this report, the environmental aspects of producing proton conducting ceramics are investigated by means of the environmental Life Cycle Assessment (LCA method. The proton conducting ceramics BaZr0.8Y0.2O3-δ (BZY, BaCe0.9Y0.1O2.95 (BCY10, and Sr(Ce0.9Zr0.10.95Yb0.05O3-δ (SCZY were prepared by the sol-gel process. Their material requirements and environmental emissions were inventoried, and their energy requirements were determined, based on actual production data. This latter point makes the present LCA especially worthy of attention as a preliminary indication of future environmental impact. The analysis was performed according to the recommendations of ISO norms 14040 and obtained using the Gabi 6 software. The performance of the analyzed samples was also compared with each other. The LCA results for these proton conducting ceramics production processes indicated that the marine aquatic ecotoxicity potential (MAETP made up the largest part, followed by fresh-water aquatic ecotoxicity potential (FAETP and Human Toxicity Potential (HTP. The largest contribution was from energy consumption during annealing and calcinations steps.

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

    Science.gov (United States)

    Kapusuz, Derya; Durucan, Caner

    2017-07-01

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

  15. Review on Development of Ceramic Membrane From Sol-Gel Route: Parameters Affecting Characteristics of the Membrane

    Directory of Open Access Journals (Sweden)

    M. R. Othman and H. Mukhtar

    2012-08-01

    Full Text Available The importance of laboratory scale ceramic membrane preparation using sol-gel technique with pore sizes in the range of 1-10nm is reviewed. Parameters affecting the characteristics of membrane during membrane development are highlighted and discussed in detail. Experimental results from literatures have shown that the correct amount of acid, water, PVA, appropriate membrane thickness, proper control of drying rate, and appropriate temperature profile selection during sintering process are necessary in order to acquire sufficient strength and reduce the formation of crack in the membrane. The different temperature setting during sintering process also influences the size of pore formed.Key Words: Sol-Gel, Inorganic Membrane, Ceramic Membrane, Gas Permeation, Sintering, Sol Properties, Membrane Morphologies, Pore Size Distribution.

  16. Sol-gel dip coating of yttria-stabilized tetragonal zirconia dental ceramic by aluminosilicate nanocomposite as a novel technique to improve the bonding of veneering porcelain

    National Research Council Canada - National Science Library

    Madani, Azamsadat; Nakhaei, Mohammadreza; Karami, Parisa; Rajabzadeh, Ghadir; Salehi, Sahar; Bagheri, Hossein

    2016-01-01

    The aim of this in vitro study was to evaluate the effect of silica and aluminosilicate nanocomposite coating of zirconia-based dental ceramic by a sol-gel dip-coating technique on the bond strength...

  17. Fe-Doped Sol-Gel Glasses and Glass-Ceramics for Magnetic Hyperthermia.

    Science.gov (United States)

    Baino, Francesco; Fiume, Elisa; Miola, Marta; Leone, Federica; Onida, Barbara; Laviano, Francesco; Gerbaldo, Roberto; Verné, Enrica

    2018-01-22

    This work deals with the synthesis and characterization of novel Fe-containing sol-gel materials obtained by modifying the composition of a binary SiO₂-CaO parent glass with the addition of Fe₂O₃. The effect of different processing conditions (calcination in air vs. argon flowing) on the formation of magnetic crystalline phases was investigated. The produced materials were analyzed from thermal (hot-stage microscopy, differential thermal analysis, and differential thermal calorimetry) and microstructural (X-ray diffraction) viewpoints to assess both the behavior upon heating and the development of crystalline phases. N₂ adsorption-desorption measurements allowed determining that these materials have high surface area (40-120 m²/g) and mesoporous texture with mesopore size in the range of 18 to 30 nm. It was assessed that the magnetic properties can actually be tailored by controlling the Fe content and the environmental conditions (oxidant vs. inert atmosphere) during calcination. The glasses and glass-ceramics developed in this work show promise for applications in bone tissue healing which require the use of biocompatible magnetic implants able to elicit therapeutic actions, such as hyperthermia for bone cancer treatment.

  18. Fe-Doped Sol-Gel Glasses and Glass-Ceramics for Magnetic Hyperthermia

    Directory of Open Access Journals (Sweden)

    Francesco Baino

    2018-01-01

    Full Text Available This work deals with the synthesis and characterization of novel Fe-containing sol-gel materials obtained by modifying the composition of a binary SiO2-CaO parent glass with the addition of Fe2O3. The effect of different processing conditions (calcination in air vs. argon flowing on the formation of magnetic crystalline phases was investigated. The produced materials were analyzed from thermal (hot-stage microscopy, differential thermal analysis, and differential thermal calorimetry and microstructural (X-ray diffraction viewpoints to assess both the behavior upon heating and the development of crystalline phases. N2 adsorption–desorption measurements allowed determining that these materials have high surface area (40–120 m2/g and mesoporous texture with mesopore size in the range of 18 to 30 nm. It was assessed that the magnetic properties can actually be tailored by controlling the Fe content and the environmental conditions (oxidant vs. inert atmosphere during calcination. The glasses and glass-ceramics developed in this work show promise for applications in bone tissue healing which require the use of biocompatible magnetic implants able to elicit therapeutic actions, such as hyperthermia for bone cancer treatment.

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

    Science.gov (United States)

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

    2012-12-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

  1. Sol-gel derived zinc oxide films alloyed with cobalt and aluminium

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Mamta [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India); Mehra, R.M., E-mail: rammehra2003@yahoo.co [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India)

    2010-05-03

    ZnO films codoped with 5 at.% Co and 1 at.% Al were prepared by sol-gel technique on corning glass and silicon substrates with precursor sols of different pH values. The pH was varied from 5.4 to 11 by adding varying amounts of monoethanolamine to the sol. Since pH plays an important role in controlling the properties of films, we discuss in detail the effect of pH value on the structural, morphological and optical properties of the grown films. X-ray diffraction and atomic force microscopy images reveal that the size of crystallites increases with pH of the sol. The variation of pH in the reaction system influences the density of homogeneous nucleation and the crystal growth along the c-axis. High quality Co and Al codoped ZnO films annealed at 600 {sup o}C have been obtained using a sol with pH = 9. These sol-gel derived films find their suitability to be used as dilute magnetic semiconductors.

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

    Science.gov (United States)

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

    2009-02-01

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

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

    Science.gov (United States)

    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.

  4. Sol-Gel Derived Eu3+-Doped Gd2Ti2O7 Pyrochlore Nanopowders

    Directory of Open Access Journals (Sweden)

    Sanja Ćulubrk

    2015-01-01

    Full Text Available Herein we presented hydrolytic sol-gel synthesis and photoluminescent properties of Eu3+-doped Gd2Ti2O7 pyrochlore nanopowders. According to Gd2Ti2O7 precursor gel thermal analysis a temperature of 840°C is identified for the formation of the crystalline pyrochlore phase. Obtained samples were systematically characterized by powder X-ray diffraction, scanning and transmission electron microscopy, and photoluminescence spectroscopy. The powders consist of well-crystalline cubic nanocrystallites of approximately 20 nm in size as evidenced from X-ray diffraction. The scanning and transmission electron microscopy shows that investigated Eu3+-doped Gd2Ti2O7 nanopowders consist of compact, dense aggregates composed entirely of nanoparticles with variable both shape and dimension. The influence of Eu3+ ions concentration on the optical properties, namely, photoluminescence emission and decay time, is measured and discussed. Emission intensity as a function of Eu3+ ions concentration shows that Gd2Ti2O7 host can accept Eu3+ ions in concentrations up to 10 at.%. On the other hand, lifetime values are similar up to 3 at.% (~2.7 ms and experience decrease at higher concentrations (2.4 ms for 10 at.% Eu3+. Moreover, photoluminescent spectra and lifetime values clearly revealed presence of structural defects in sol-gel derived materials proposing photoluminescent spectroscopy as a sensitive tool for monitoring structural changes in both steady state and lifetime domains.

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

    Energy Technology Data Exchange (ETDEWEB)

    Cervantes, O [Univ. of California, Davis, CA (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Hari Babu, B., E-mail: hariphy2012@gmail.com, E-mail: matthieu.lancry@u-psud.fr; León Pichel, Mónica [Laboratoire des Solides Irradiés, UMR CEA-CNRS 7642, Ecole Polytechnique, Université Paris Saclay, 91128 Palaiseau (France); Institut de Chimie Moléculaire et des Matériaux d' Orsay, UMR CNRS-UPSud 8182, Université Paris Sud, 91405 Orsay (France); Ollier, Nadège [Laboratoire des Solides Irradiés, UMR CEA-CNRS 7642, Ecole Polytechnique, Université Paris Saclay, 91128 Palaiseau (France); El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed [Laboratoire PhLAM (UMR CNRS 8523), IRCICA (USR CNRS 3380), CERLA - FR CNRS 2416, Université Lille 1, Villeneuve d' Ascq Cedex F-59655 (France); Poumellec, Bertrand; Lancry, Matthieu, E-mail: hariphy2012@gmail.com, E-mail: matthieu.lancry@u-psud.fr [Institut de Chimie Moléculaire et des Matériaux d' Orsay, UMR CNRS-UPSud 8182, Université Paris Sud, 91405 Orsay (France); Ibarra, Angel [National Fusion Laboratory, CIEMAT, Avda Complutense 40, 28040 Madrid (Spain)

    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.

  7. Microwave assisted sol-gel synthesis of high dielectric constant CCTO and BFN ceramics for MLC applications

    Directory of Open Access Journals (Sweden)

    Sonia

    2017-06-01

    Full Text Available Ba(Fe1/2Nb1/2O3 (BFN and CaCu3Ti4O12 (CCTO ceramic powders were synthesized by microwave assisted sol-gel synthesis technique and sintered at 1100°C and 1000°C, respectively. Calcination and sintering processes were carried out in a microwave furnace. Dielectric constant (εr~2450 and dielectric loss (tan δ~0.5 at frequency of 1 kHz and 20°C were observed for the BFN ceramic samples. Higher value of εr ~ 3600 and lower value of tan δ ~ 0.07 at frequency of 1 kHz and in 20-60°C temperature range for the CCTO ceramic samples suggested its utility for MLC applications. Sharp decrease of εr and sharp increase of tan δ at higher frequencies of BFN ceramic samples indicated the presence of Debye like relaxation.

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

    Science.gov (United States)

    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. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Observation and manipulation of magnetic domains in sol gel derived thin films of spinel ferrites

    Science.gov (United States)

    Datar, Ashwini A.; Mathe, Vikas L.

    2017-12-01

    Thin films of spinel ferrites, namely zinc substituted nickel, cobalt ferrite, and manganese substituted cobalt ferrite, were synthesized using sol-gel derived spin-coating techniques. The films were characterized using x-ray diffraction, field emission scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy techniques for the analysis of structural, morphological and vibrational band transition properties, which confirm the spinel phase formation of the films. The magnetic force microscopy (MFM) technique was used to observe the magnetic domain structure present in the synthesized films. Further, the films were subjected to an external DC magnetic field of 2 kG to orient the magnetic domains and analyzed using an ex situ MFM technique.

  10. Influence of the intermediate layer on the hydrothermal stability of sol-gel derived hybrid silica membranes

    NARCIS (Netherlands)

    ten Hove, Marcel; Luiten-Olieman, Mieke W.J.; Huiskes, Cindy; Nijmeijer, Arian; Winnubst, Louis

    2017-01-01

    The hydrothermal stability of microporous silica hybrid sol-gel derived membranes is often only tested for either the mesoporous intermediate membrane layer or the microporous separation layer. In this work an investigation is done on the interaction between the intermediate γ-alumina layer and the

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

    Science.gov (United States)

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

    2011-11-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-08-26

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

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

    Science.gov (United States)

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

    2004-07-01

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

  14. A Comparative Study of Solvothermal and Sol-Gel-Derived Nanocrystalline Alumina Catalysts for Ethanol Dehydration

    Directory of Open Access Journals (Sweden)

    Mingkwan Wannaborworn

    2015-01-01

    Full Text Available The ethanol dehydration to ethylene over alumina catalysts prepared by solvothermal and sol-gel methods was investigated. Also, a commercial alumina was used for comparison purposes. The results showed that the catalytic activity depends on the properties of catalyst derived from different preparation methods and reaction temperature. The alumina synthesized by solvothermal method exhibited the highest activity. This can be attributed to the higher surface area and larger amount of acid site, especially the ratio of weak/strong acid strength as determined by N2 physisorption and NH3-TPD studies. The solvothermal-derived catalyst exhibited an excellent performance with complete ethanol conversion and 100% selectivity to ethylene at 350°C in comparison with other ones. In addition, we further studied the catalytic dehydration of alumina catalyst modified with Fe. The presence of 10 wt.% Fe decreased both conversion and ethylene selectivity. However, the acetaldehyde selectivity apparently increased. It was related to the dehydrogenation pathway that takes place on Fe species.

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

    Science.gov (United States)

    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.

  16. Sol-gel derived solid chiral materials and their optical activity

    Science.gov (United States)

    Xia, Haiping; Tao, Weidong; Wang, Jinhao; Zhang, Jianli; Nie, Qiuhua

    2004-11-01

    The chiral organic molecules glucose (C 6H 12O 6) and griseofulvin (C 17H 17ClO 6) were first uniformly incorporated in sol-gel derived materials. The polarity response, absorption spectra and thermal stability were measured and discussed. The DTA results indicated that the C 6H 12O 6 and C 17H 17ClO 6 in gels were stable in air at the temperature lower than 210 and 350 °C, respectively. An absorption band at about 1.4 μm due to OH - existed in the infrared absorption spectra of the gels. The similar behaviors of optical activity for the organic chiral molecules in solutions were hold in solid gels. The specific rotations for C 6H 12O 6 and C 17H 17ClO 6 in gels were -0.95 and -1.45°/cm, corresponding to the chiral parameter 1.55 × 10 -7 and 2.37 × 10 -7, respectively.

  17. Biosorption of uranium and copper by Bacillus Sphaericus JG-A12 cells, spores and S-layer proteins embedded in sol-gel ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Raff, J.; Soltmann, U.; Boettcher, H. [Arbeitsgruppe Funktionelle Schichten, GMBU e.V., Dresden (Germany); Matys, S.; Pompe, W. [Inst. fuer Materialwissenschaft, Technische Univ. Dresden (Germany); Selenska-Pobell, S.

    2002-05-01

    Vegetative cells, spores and stabilized S-layer sheets of B. sphaericus JG-A12 were embedded in SiO{sub 2} bulk particles using sol-gel techniques. In sorption experiments the metal binding capacity of the free biocomponents and the corresponding biological ceramics were compared. (orig.)

  18. Characterization and photoluminescence properties of sol-gel derived Bi2MoO6:Eu3+ phosphor

    Science.gov (United States)

    Zhang, Jie; Han, Bing; Li, Pengju; Li, Jianliang; Bian, Yang

    2015-05-01

    This work first reported the characterization and photoluminescence properties of Eu3+ doped Bi2MoO6 phosphor prepared by sol-gel method. The phosphor was characterized by X-ray diffraction, field emission scanning electron microscopic, fourier transform infrared spectrum, and fluorescence spectroscopy measurements in order to investigate the phase purity, surface morphology, and photoluminescence properties. The spectroscopic characteristics including excitation and emission spectrum, decay curve, and chromaticity coordinates were discussed. The as-prepared phosphor can be effectively excited with 345/465 nm light, and exhibit red emission belonging to the prevailing 5 D 0 → 7 F 2 transition of Eu3+ with decay time of milliseconds. The above spectral characteristics indicate sol-gel derived Bi2MoO6:Eu3+ phosphor could be regarded as a potential red phosphor for application in white light-emitting diodes (w-LEDs) based on ultraviolet (UV)/blue LED chips.

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

    Science.gov (United States)

    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.

  20. Synthesis, characterization and bioactivity of a calcium-phosphate glass-ceramics obtained by the sol-gel processing method.

    Science.gov (United States)

    Jmal, Nouha; Bouaziz, Jamel

    2017-02-01

    In this work, a calcium-phosphate glass-ceramics was successfully obtained by heat treatment of a mixture of 26.52 in wt.% of fluorapatite (Fap) and 73.48 in wt.% of 77S (77 SiO214 CaO9 P2O5 in wt.%) gel. The calcium phosphate-glass-ceramics was prepared by sol-gel process with tetraethyl orthosilicate (TEOS), triethyl phosphate (TEP), calcium nitrate and fluorapatite. The synthesized powders were characterized by some commonly used tools such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), 31P magic angle spinning nuclear magnetic resonance (MAS-NMR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and thin-film X-ray diffraction (TF-XRD). The obtained results seemed to confirm the nucleation and growth of hydroxyapatite (Hap) nano-phase in the glass. Moreover, an in-vitro evaluation of the glass-ceramic was performed. In addition, to assess its bioactive capacity, it was soaked in simulated body fluid (SBF) at different time intervals. The SEM, EDS and TF-XRD analyses showed the deposition of hydroxyapatite on the surface of the specimens after three days of immersion in SBF solution. The mechanical properties of the obtained material such as rupture strength, Vickers hardness and elastic modulus were measured. In addition, the friction coefficient of calcium phosphate-glass-ceramics was tested. The values of the composite of rupture strength (24MPa), Vickers hardness (214Hv), Young's modulus (52.3GPa), shear modulus (19GPa) and friction coefficient (0.327) were obtained. This glass-ceramics can have useful applications in dental prostheses. Indeed, this material may have promising applications for implants because of its content of fluorine, the effective protector against dental caries. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Mesoporous silica matrices derived from sol-gel process assisted by low power ultrasonic activation

    Directory of Open Access Journals (Sweden)

    Václav Štengl

    2009-06-01

    Full Text Available The present work contributes to elucidating the differences between silica gels obtained by low doses ultrasonic activation, and those obtained by the conventional method, termed as classical sol gel. Silica matrices were produced by sol-gel synthesis process, assisted and non-assisted by an ultrasonic fi eld, and subsequently characterized by various methods. Nitrogen adsorption and small-angle neutron scattering (SANS measurements provided texture and microstructure of the dried gels. The adsorption results show that the sample sonicated for 2 hours presents the most ordered microstructure, characterized by pore shape close to spherical and the narrowest size distribution – about 90 % of the pores for this sample fall into the mesopore range (2–50 nm. SANS data reveal the formation of primary structural units of sizes around 1.5–2 nm which are small linear or branched polymeric species of roughly spherical shape and with rough surface. They are generated in the very early stage of sol gel process, as a result of hydrolysis and condensation reactions. The aggregated primary units form the secondary porous structure which can be described as a rough surface with fractal dimension above 2. The best porosity characteristics were obtained for the sample activated for 2 hours, indicating the optimal doses of sonication in the present conditions. Our results demonstrate the possibility of tailoring the pore size distribution using a low power ultrasonic bath.

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

    Science.gov (United States)

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

    2017-10-11

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

  3. Structural phase analysis of a sol-gel nano-crystalline lithium-mica glass-ceramic through different compositions

    Energy Technology Data Exchange (ETDEWEB)

    Tohidifar, M.R., E-mail: tohidifar@znu.ac.ir [Faculty of Engineering, University of Zanjan, P.O. Box 45371-38791, Zanjan (Iran, Islamic Republic of); Alizadeh, P. [Department of Materials Science and Engineering, Tarbiat Modares University, P.O. Box 14115-143, Tehran (Iran, Islamic Republic of)

    2016-08-15

    The current paper attempts to study the influence of chemical composition on the phase development of nano-crystalline lithium-mica glass-ceramic. For this purpose, aqueous sol-gel technique was employed to prepare the glass-ceramics. The synthesis process was accomplished using two chemical compositions of Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} and LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2} at different x values along with various mass% of MgF{sub 2} inclusion. It was found that considering an optimized amount of MgF{sub 2}, the specimens synthesized through a new formulation of LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2} composition are more appropriate for the sol-gel synthesis method, especially because of intensifying the lithium-mica precipitation and also omission of the secondary phase (i.e. lithium aluminum silicate). The results also indicated that any deviation from the optimized amount of MgF{sub 2} (8%) would cause degradation in the intensity of the precipitated lithium-mica, following the nucleation treatment. - Highlights: • Higher intensity of mica phase obtains through LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2} composition. • LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2} composition offers mica phase without applying excess MgF{sub 2}. • Applying LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2} composition leads to omission of minor phases. • Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} formula cannot be useful in mica nucleation process. • Optimum amount of MgF{sub 2} was obtained as 8% following the nucleation process.

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

    Energy Technology Data Exchange (ETDEWEB)

    Veinot, Jonathan G C; Henderson, Eric J; Hessel, Colin M, E-mail: jveinot@ualberta.ca [Department of Chemistry, University of Alberta, Edmonton, Alberta (Canada)

    2009-11-15

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

  5. Luminescence of nanostructured SnO2-SiO2 glass-ceramics prepared by sol-gel method.

    Science.gov (United States)

    del-Castillo, J; Yanesl, A C; Méndez-Ramos, J; Rodríguez, V D

    2008-04-01

    Nanostructured silica based glass-ceramics samples of composition (100 - x)SiO2-xSnO2, with x from 1 to 10, have been synthesized by thermal treatment of precursor sol-gel glasses. The average size of the obtained SnO2 nanocrystals, calculated by using the X-ray diffraction, can be predetermined by using well-controlled concentration of tin precursor. The mean radius ranging from 1.6 to 5.5 nm, is comparable to the exciton Bohr radius, corresponding to wide band-gap semiconductor quantum-dots in an insulator SiO2 glass. A spectroscopy study in terms of optical absorption and photoluminescence spectra has been carried out as a function of SnO2 concentration. Size-dependent red-shifts of excitation and emission bands, with increasing of tin precursor concentration, point to the quantum confinement effect. The nanocrystal sizes have been obtained and compared by using the Brus and Scherrer equations. The band gap increase is in agreement with results, based on the effective mass model. The recombination of conduction band electron with oxygen vacancies is proposed to explain the luminescence red-shift.

  6. Sol-gel Derived Warfarin - Silica Composites for Controlled Drug Release.

    Science.gov (United States)

    Dolinina, Ekaterina S; Parfenyuk, Elena V

    2017-01-01

    Warfarin, commonly used anticoagulant in clinic, has serious shortcomings due to its unsatisfactory pharmacodynamics. One of the efficient ways for the improvement of pharmacological and consumer properties of drugs is the development of optimal drug delivery systems. The aim of this work is to synthesize novel warfarin - silica composites and to study in vitro the drug release kinetics to obtain the composites with controlled release. The composites of warfarin with unmodified (UMS) and mercaptopropyl modified silica (MPMS) were synthesized by sol-gel method. The composite formation was confirmed by FTIR spectra. The concentrations of warfarin released to media with pH 1.6, 6.8 and 7.4 were measured using UV spectroscopy. The drug release profiles from the solid composites were described by a series of kinetic models which includes zero order kinetics, first order kinetics, the modified Korsmeyer-Peppas model and Hixson-Crowell model. The synthesized sol-gel composites have different kinetic behavior in the studied media. In contrast to the warfarin composite with unmodified silica, the drug release from the composite with mercaptopropyl modified silica follows zero order kinetics for 24 h irrespective to the release medium pH due to mixed mechanism (duffusion + degradation and/or disintegration of silica matrix). The obtained results showed that warfarin - silica sol-gel composites have a potential application for the development of novel oral formulation of the drug with controlled delivery. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  7. The Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Khalid Suliman Aboodh

    2015-02-01

    Full Text Available Abstract An increasingly important application of liquid jets is the disintegration of the jet to form droplets of liquid containing nuclear fuel. These droplets are then dried and sintered to form ceramic micro spheres for use in fuel elements in nuclear reactors. The total operations required to form the droplets convert them to solids and fire them to ceramic bodies comprise what are known as Sol-Gel processes Reference 13.

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

    Science.gov (United States)

    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.

  9. Exploitation of the Sol-Gel Route in Processing Ceramics and Composites

    Science.gov (United States)

    1985-05-01

    later able to over-ride this requirement of seeds by using higher pressure and no seeds (25). Similar results were obtained with a- spodumene and many...Alumionosilicates: Eucryptite, Spodumene and Petalite,’ J. Am.Ceram. Soc. V , 152-159 (1950). 27. James W. McCauley and Rustum Roy, ’Controlled Nucleation...Eucryptite, Spodumene and Petalite,’ J. Am. Ceram. Soc., 33, 152-159 (1950). 5 V.G. Hill, R. Roy and E.F. Osborn, ’The Systsem Alumina-Gallia-Water

  10. Laser sintering of doped strontium aluminate via modified sol-gel for use as a ceramic pigment; Sinterizacao a laser do aluminato de estroncio dopado via sol-gel modificado para aplicacao como pigmento ceramico

    Energy Technology Data Exchange (ETDEWEB)

    Soares, F.M. dos S.; Valerio, M.E.G. [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil)

    2017-01-15

    Powder of Dy{sup 3+} co-doped SrAl{sub 2}O{sub 4} :Eu{sup 3+} was produced via proteic sol-gel method, a modified sol-gel route which allows the formation of oxides at lower temperatures than other methods. CO{sub 2} laser sintering was used as a method for heat treatment, effective in reducing trivalent europium ions in doped samples. Thermal analysis of the precursors, performed by TG and DTA, revealed that the crystallization of SrAl{sub 2}O{sub 4} phase occurred at approximately 1060 °C. X-ray diffraction showed that the samples, before and after sintering, had monoclinic and hexagonal phases formation. DLS technique revealed the presence of nanosized and micrometric particles, and particle agglomerates, confirmed by SEM images. Micrographs of the fracture surface of a sintered pellet revealed a high degree of densification caused by heat treatment. Photoluminescence measurements showed that the samples after synthesis and before heat treatment with laser had reddish emission, composed of characteristic narrow emission lines from Eu{sup 3+} and more intense emission when the samples were excited at 265 nm. The laser treatment promoted the reduction of Eu{sup 3+} to Eu{sup 2+} and this effect was confirmed by the presence of a wide emission band in the green region of the spectrum with a maximum emission obtained after excitation at 350 nm. The luminescent decay time of the thermally treated sample was approximately 100 min. Via XRF measurements of acquired frit and DTA and TG of the frit, pigment and mixtures of both, it was noticed good compatibility in terms of thermal processes, that indicated that the pigment has a potential to be used in ceramic tiles. (author)

  11. Page 1 Alumina ceramics by sol-gel technique 103 shows the ...

    Indian Academy of Sciences (India)

    Cryst. Solids 10837. Pierre A C and Uhlman D R 1984 in Better ceramics through chemistry (ed.) CJ Brinker (North. Holland: Elsevier Sci. Pub.Co., Inc) p. 119. Yoldas B E 1975a Bull. An. Ceran. Soc. 3287. Yoldas B E 1975b J. Mater. Sci, 10 856.

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

    Energy Technology Data Exchange (ETDEWEB)

    Rau, J.V., E-mail: giulietta.rau@ism.cnr.it [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Teghil, R. [Universita della Basilicata, Dipartimento di Chimica ' A.M. Tamburro' , Via dell' Ateneo Lucano, 10-85100 Potenza (Italy); CNR-IMIP U.O.S. di Potenza, Zona Industriale di Tito scalo (PZ) (Italy); Fosca, M. [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Universita di Roma ' La Sapienza' , Dipartimento di Chimica, Piazzale Aldo Moro, 5-00185 Rome (Italy); De Bonis, A. [Universita della Basilicata, Dipartimento di Chimica ' A.M. Tamburro' , Via dell' Ateneo Lucano, 10-85100 Potenza (Italy); CNR-IMIP U.O.S. di Potenza, Zona Industriale di Tito scalo (PZ) (Italy); Cacciotti, I.; Bianco, A. [Universita di Roma ' Tor Vergata' , Dipartimento di Ingegneria Industriale, UR INSTM ' Roma Tor Vergata' , Via del Politecnico, 1-00133 Rome (Italy); Albertini, V. Rossi [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Caminiti, R. [Universita di Roma ' La Sapienza' , Dipartimento di Chimica, Piazzale Aldo Moro, 5-00185 Rome (Italy); Ravaglioli, A. [Parco Torricelli delle Arti e delle Scienze, Via Granarolo, 64-48018 Faenza (Ra) (Italy)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer Bioactive glass-ceramic coatings for bone tissue repair and regeneration. Black-Right-Pointing-Pointer Pulsed Lased Deposition allowed congruent transfer of target composition to coating. Black-Right-Pointing-Pointer Target was prepared by sol-gel process suitable for compositional tailoring. Black-Right-Pointing-Pointer Titanium, widely used for orthopaedics and dental implants, was used as substrate. Black-Right-Pointing-Pointer The physico-chemical properties of the prepared coatings are reported. -- Abstract: The deposition of innovative glass-ceramic composition (i.e. RKKP) coatings by Pulsed Lased Deposition (PLD) technique is reported. RKKP was synthesised following two methodologies: melt-processing and sol-gel, the latter being particularly suitable to tailor the compositional range. The PLD advantage with respect to other deposition techniques is the congruent transfer of the target composition to the coating. The physico-chemical properties of films were investigated by Scanning Electron and Atomic Force Microscopies, Fourier Transform Infrared Spectroscopy, Angular and Energy Dispersive X-ray Diffraction, and Vickers microhardness. The deposition performed at 12 J/cm{sup 2} and 500 Degree-Sign C allows to prepare crystalline films with the composition that replicates rather well that of the initial targets. The 0.6 {mu}m thin melt-processing RKKP films, possessing the hardness of 25 GPa, and the 4.3 {mu}m thick sol-gel films with the hardness of 17 GPa were obtained.

  13. Structural and electrochemical behavior of sol-gel ZrO{sub 2} ceramic film on chemically pre-treated AZ91D magnesium alloy

    Energy Technology Data Exchange (ETDEWEB)

    Li Qing [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)], E-mail: liqingd@swu.edu.cn; Chen Bo; Xu Shuqiang; Gao Hui; Zhang Liang; Liu Chao [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)

    2009-06-10

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

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

    Science.gov (United States)

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

    2013-04-01

    This study investigated the effect of the addition of sol-gel derived nanoscale bioactive glass (NBG) particles on the mechanical properties and biological performances of PCL polymer, in order to evaluate the potential applications of PCL/NBG composites for bone tissue regeneration. Regardless of the NBG contents (10, 20, and 30 wt.%), the NBG particles, which were synthesized through the sol-gel process using polyethylene glycol (PEG) polymer as a template, could be uniformly dispersed in the PCL matrix, while generating pores in the PCL/NBG composites. The elastic modulus of the PCL/NBG composites increased remarkably from 89±11 MPa to 383±50 MPa with increasing NBG content from 0 to 30 wt.%, while still showing good ultimate tensile strength in the range of 15-19 MPa. The hydrophilicity, water absorption and degradation behavior of the PCL/NBG composites were also enhanced by the addition of the NBG particles. Furthermore, the PCL/NBG composite with a NBG content of 30 wt.% showed significantly enhanced in vitro bioactivity and cellular response compared to those of the pure PCL. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Shiquan Tao

    2006-12-31

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

  16. Synthesis of 8YSZ-LSGM Composite Thick Film Ceramics for Solid Electrolyte From Nanopowder Utilizing Local Zircon Prepared Using Sol Gel Process

    Science.gov (United States)

    Syarif, Dani Gustaman; Soepriyanto, Syoni; Ismunandar, Korda, Akhmad

    2010-10-01

    Thick film ceramics of 8% mol Y2O3 doped-ZrO2 (8YSZ)-La0.8Sr0.2Ga0.2Mg0.8O3 (LSGM) composite for solid electrolyte have been synthesized from nanopowder. Concentration of LSGM was 0 and 10% weight. A paste for the thick films was made from 8YSZ nanopowder prepared using sol gel method and LSGM powder prepared by solid state reaction. Precursors for the 8YSZ nanopowder preparation were ZrOCl2ṡ8H2O derived from local zircon as byproduct of Tin processing at Bangka Island using caustic fussion method, and Y(NO3)3. The thick films were produced by screen printing technique on alumina substrates. The films were sintered at 1500° C for 2 hours in air. X-ray diffraction (XRD) data showed that the nanopowder of 8YSZ was well produced with broad peaks. The particle size of the 8YSZ powder was about 12 nm as calculated using Debye Scherrer method. The thick films of 8YSZ and 8YSZ-LSGM (90:10 in weight %) composite could be produced, however, the films still contain voids. The ionic conductance of the YSZ-10LSGM films was smaller than that of the YSZ films.

  17. Thermal stability of nanostructured titania and titania-ceria ceramic powders prepared by the sol-gel process

    NARCIS (Netherlands)

    Koebrugge, G.W.; Winnubst, Aloysius J.A.; Burggraaf, A.J.

    The preparation and characterisation of nanometre TiO2 powder materials, prepared by the sol-gel method, are described. Controlled hydrolysis of a titanium-2-methyl-2-butoxide precursor was applied to obtain alcosols with particles (in alcohol) smaller than 5 nm. Powders obtained from this sol were

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

    Science.gov (United States)

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

    2017-03-01

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

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

    Science.gov (United States)

    Joughehdoust, S.; Manafi, S.

    2012-03-01

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

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

    Science.gov (United States)

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

    2012-06-01

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

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

    Science.gov (United States)

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

    2010-04-01

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

  2. Organic Thin Film Transistors with Polyvinylpyrrolidone / Nickel Oxide Sol-Gel Derived Nanocomposite Insulator

    Directory of Open Access Journals (Sweden)

    A. Bahari

    2012-09-01

    Full Text Available Polyvinylpyrrolidone  /  Nickel  oxide  (PVP/NiO  dielectrics  were fabricated  with  sol-gel  method  using  0.2  g  of  PVP  at  different working  temperatures  of  80,  150  and  200  ºC.  Structural  properties and surface morphology of the hybrid films were investigated by X- Ray  diffraction  (XRD  and  Scanning  Electron Microscope  (SEM respectively. Energy dispersive X-ray spectroscopy (EDX was used to make  a  quantitative  chemical  analysis  of  an  unknown material. The  obtained  results  demonstrate  the  feasibility  of  using  high dielectric  constant  nanocomposite  PVP/NiO  as  gate  dielectric insulator in the organic thin film transistors (OTFTs.

  3. Sol-gel derived ZnO as an electron transport layer (ETL) for inverted organic solar cells

    Science.gov (United States)

    Tiwari, D. C.; Dwivedi, Shailendra Kumar; Dipak, Phukhrambam; Chandel, Tarun; Sharma, Rishi

    2017-05-01

    In this work, we present the study of the fabrication process of the sol-gel derived zinc oxide (ZnO) as an electron transport layer (ETL.). The solution processed inverted bulk heterojunction organic solar cells based on a thin film blend of poly (3-hexylthiophene 2, 5-diyl) and [6,6]-phenyl-C61-butyric acid methyl ester is prepared. ZnO thin films are annealed at different temperature to optimize the solar cell performance and their characterization for their structural and optical properties are carried out. We have observed Voc=70mV, Jsc=1.33 µA/cm2 and FF=26% from the inverted heterojunction solar cell.

  4. Sol-gel-derived and base-heat-treated AR coatings for-high power laser systems

    Science.gov (United States)

    Tang, Jiamiao; Zhu, Congshan

    1997-12-01

    Sol-gel derived and base-heat treated antireflective (AR) coatings with good abrasive/scratch resistant performance have been investigated and developed. The comparison of abrasive/scratch resistant property of the AR coatings from this method to that from other methods demonstrated that the base-heat treated AR coatings have still more abrasive/scratch resistant ability. After more than 30 times of drag wipe and 1000 times flashlamp glow discharges of 300 microsecond(s) duration and 15 J/cm2 for each discharge, the AR- coatings indicated no visible crazing or peeling. In the mean time, more than 6% transmission gain related to the spectrum of Nd+3 absorption can be obtained and maintained.

  5. Sol-Gel Derived Adsorbents with Enzymatic and Complexonate Functions for Complex Water Remediation.

    Science.gov (United States)

    Pogorilyi, Roman P; Pylypchuk, Ievgen; Melnyk, Inna V; Zub, Yurii L; Seisenbaeva, Gulaim A; Kessler, Vadim G

    2017-09-28

    Sol-gel technology is a versatile tool for preparation of complex silica-based materials with targeting functions for use as adsorbents in water purification. Most efficient removal of organic pollutants is achieved by using enzymatic reagents grafted on nano-carriers. However, enzymes are easily deactivated in the presence of heavy metal cations. In this work, we avoided inactivation of immobilized urease by Cu (II) and Cd (II) ions using magnetic nanoparticles provided with additional complexonate (diethylene triamine pentaacetic acid or DTPA) functions. Obtained nanomaterials were characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). According to TGA, the obtained Fe₃O₄/SiO₂-NH₂-DTPA nanoadsorbents contained up to 0.401 mmol/g of DTPA groups. In the concentration range Ceq = 0-50 mmol/L, maximum adsorption capacities towards Cu (II) and Cd (II) ions were 1.1 mmol/g and 1.7 mmol/g, respectively. Langmuir adsorption model fits experimental data in concentration range Ceq = 0-10 mmol/L. The adsorption mechanisms have been evaluated for both of cations. Crosslinking of 5 wt % of immobilized urease with glutaraldehyde prevented the loss of the enzyme in repeated use of the adsorbent and improved the stability of the enzymatic function leading to unchanged activity in at least 18 cycles. Crosslinking of 10 wt % urease on the surface of the particles allowed a decrease in urea concentration in 20 mmol/L model solutions to 2 mmol/L in up to 10 consequent decomposition cycles. Due to the presence of DTPA groups, Cu2+ ions in concentration 1 µmol/L did not significantly affect the urease activity. Obtained magnetic Fe₃O₄/SiO₂-NH₂-DTPA-Urease nanocomposite sorbents revealed a high potential for urease decomposition, even in presence of heavy metal ions.

  6. Sol-Gel Derived Adsorbents with Enzymatic and Complexonate Functions for Complex Water Remediation

    Directory of Open Access Journals (Sweden)

    Roman P. Pogorilyi

    2017-09-01

    Full Text Available Sol-gel technology is a versatile tool for preparation of complex silica-based materials with targeting functions for use as adsorbents in water purification. Most efficient removal of organic pollutants is achieved by using enzymatic reagents grafted on nano-carriers. However, enzymes are easily deactivated in the presence of heavy metal cations. In this work, we avoided inactivation of immobilized urease by Cu (II and Cd (II ions using magnetic nanoparticles provided with additional complexonate (diethylene triamine pentaacetic acid or DTPA functions. Obtained nanomaterials were characterized by Fourier transform infrared spectroscopy (FTIR, thermogravimetric analysis (TGA, and scanning electron microscopy (SEM. According to TGA, the obtained Fe3O4/SiO2-NH2-DTPA nanoadsorbents contained up to 0.401 mmol/g of DTPA groups. In the concentration range Ceq = 0–50 mmol/L, maximum adsorption capacities towards Cu (II and Cd (II ions were 1.1 mmol/g and 1.7 mmol/g, respectively. Langmuir adsorption model fits experimental data in concentration range Ceq = 0–10 mmol/L. The adsorption mechanisms have been evaluated for both of cations. Crosslinking of 5 wt % of immobilized urease with glutaraldehyde prevented the loss of the enzyme in repeated use of the adsorbent and improved the stability of the enzymatic function leading to unchanged activity in at least 18 cycles. Crosslinking of 10 wt % urease on the surface of the particles allowed a decrease in urea concentration in 20 mmol/L model solutions to 2 mmol/L in up to 10 consequent decomposition cycles. Due to the presence of DTPA groups, Cu2+ ions in concentration 1 µmol/L did not significantly affect the urease activity. Obtained magnetic Fe3O4/SiO2-NH2-DTPA-Urease nanocomposite sorbents revealed a high potential for urease decomposition, even in presence of heavy metal ions.

  7. Fabrication of mullite-bonded porous SiC ceramics from multilayer-coated SiC particles through sol-gel and in-situ polymerization techniques

    Science.gov (United States)

    Ebrahimpour, Omid

    In this work, mullite-bonded porous silicon carbide (SiC) ceramics were prepared via a reaction bonding technique with the assistance of a sol-gel technique or in-situ polymerization as well as a combination of these techniques. In a typical procedure, SiC particles were first coated by alumina using calcined powder and alumina sol via a sol-gel technique followed by drying and passing through a screen. Subsequently, they were coated with the desired amount of polyethylene via an in-situ polymerization technique in a slurry phase reactor using a Ziegler-Natta catalyst. Afterward, the coated powders were dried again and passed through a screen before being pressed into a rectangular mold to make a green body. During the heating process, the polyethylene was burnt out to form pores at a temperature of about 500°C. Increasing the temperature above 800°C led to the partial oxidation of SiC particles to silica. At higher temperatures (above 1400°C) derived silica reacted with alumina to form mullite, which bonds SiC particles together. The porous SiC specimens were characterized with various techniques. The first part of the project was devoted to investigating the oxidation of SiC particles using a Thermogravimetric analysis (TGA) apparatus. The effects of particle size (micro and nano) and oxidation temperature (910°C--1010°C) as well as the initial mass of SiC particles in TGA on the oxidation behaviour of SiC powders were evaluated. To illustrate the oxidation rate of SiC in the packed bed state, a new kinetic model, which takes into account all of the diffusion steps (bulk, inter and intra particle diffusion) and surface oxidation rate, was proposed. Furthermore, the oxidation of SiC particles was analyzed by the X-ray Diffraction (XRD) technique. The effect of different alumina sources (calcined Al2O 3, alumina sol or a combination of the two) on the mechanical, physical, and crystalline structure of mullite-bonded porous SiC ceramics was studied in the

  8. MECHANISMS CONTROLLING Ca ION RELEASE FROM SOL-GEL DERIVED IN SITU APATITE-SILICA NANOCOMPOSITE POWDER

    National Research Council Canada - National Science Library

    Seyed Mohsen Latifi; Mohammadhossein Fathi; Varshosaz Jaleh; Ghochaghi Niloufar

    2015-01-01

    .... In order to improve hydroxyapatite (HA) dissolution rate, in situ apatite-silica nanocomposite powders with various silica contents were synthesized via sol-gel method and mechanisms controlling the Ca ion release from them were investigated...

  9. Effect of sintering temperature on mechanical behaviour and bioactivity of sol-gel synthesized bioglass-ceramics using rice husk ash as a silica source

    Energy Technology Data Exchange (ETDEWEB)

    Nayak, J.P., E-mail: jyotiprakash_nitrkl@rediffmail.com [Department of Ceramic Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India); Bera, J., E-mail: bera@rediffmail.com [Department of Ceramic Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India)

    2010-11-01

    Bioglass-ceramics with SiO{sub 2}-Na{sub 2}O-CaO composition was prepared by sol-gel method using rice husk ash as a silica source. Material was sintered at different temperatures ranging from 900 to 1050 deg. C for 2 h. Phase-formation behaviour, densification characteristics, and mechanical strength of glass-ceramics were investigated. The material sintered at 1000 deg. C showed a good mechanical strength. Mechanical properties were correlated with microstructural features. Both in vitro bioactivity and biodegradability of sintered material were investigated by incubating in simulated body fluid and Tris buffer solution, respectively. Scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction were used to investigate the surface deposition during body fluid incubation. Both bioactivity and degradability decreased with increase in sintering temperature.

  10. Effect of sintering temperature on mechanical behaviour and bioactivity of sol-gel synthesized bioglass-ceramics using rice husk ash as a silica source

    Science.gov (United States)

    Nayak, J. P.; Bera, J.

    2010-11-01

    Bioglass-ceramics with SiO2-Na2O-CaO composition was prepared by sol-gel method using rice husk ash as a silica source. Material was sintered at different temperatures ranging from 900 to 1050 °C for 2 h. Phase-formation behaviour, densification characteristics, and mechanical strength of glass-ceramics were investigated. The material sintered at 1000 °C showed a good mechanical strength. Mechanical properties were correlated with microstructural features. Both in vitro bioactivity and biodegradability of sintered material were investigated by incubating in simulated body fluid and Tris buffer solution, respectively. Scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction were used to investigate the surface deposition during body fluid incubation. Both bioactivity and degradability decreased with increase in sintering temperature.

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

    Directory of Open Access Journals (Sweden)

    Krzysztof Marycz

    2015-01-01

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

  12. Study of hafnium (IV) oxide nanoparticles synthesized by polymerized complex and polymer precursor derived sol-gel methods

    KAUST Repository

    Ramos-González, R.

    2010-03-01

    This work reports the preparation and characterization of hafnium (IV) oxide (HfO2) nanoparticles grown by derived sol-gel routes that involves the formation of an organic polymeric network. A comparison between polymerized complex (PC) and polymer precursor (PP) methods is presented. For the PC method, citric acid (CA) and ethylene glycol (EG) are used as the chelating and polymerizable reagents, respectively. In the case of PP method, poly(acrylic acid) (PAA) is used as the chelating reagent. In both cases, different precursor gels were prepared and the hafnium (IV) chloride (HfCl4) molar ratio was varied from 0.1 to 1.0 for the PC method and from 0.05 to 0.5 for the PP method. In order to obtain the nanoparticles, the precursors were heat treated at 500 and 800 °C. The thermal characterization of the precursor gels was carried out by thermogravimetric analysis (TGA) and the structural and morphological characterization by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the samples obtained by both methods shows the formation of HfO2 at 500 °C with monoclinic crystalline phase. The PC method exhibited also the cubic phase. Finally, the HfO2 nanoparticles size (4 to 11 nm) was determined by TEM and XRD patterns. © (2010) Trans Tech Publications.

  13. Inverted polymer solar cells with sol-gel derived cesium-doped zinc oxide thin film as a buffer layer

    Science.gov (United States)

    Ahmadi, Mehdi; Mirabbaszadeh, Kavoos; Salari, Saeid; Fatehy, Hamed

    2014-09-01

    An inverted structure of polymer solar cells based on Poly(3-hexylthiophene)(P3HT):[6-6] Phenyl-(6) butyric acid methyl ester (PCBM) with thin films of sol-gel derived Cesium doped ZnO (Cs:ZnO) was developed as an efficient cathode buffer layer. Doped and undoped thin films were deposited using a less studied method, doctor blade, which was compatible with Roll-2-Roll printing method. By comparing the effect of Cs:ZnO thin films with various dopant ratio on the performance of inverted polymer solar cells, 0.5% Cs doped ZnO was found as the most effective doping level among the selected doping ratios. Using 30 nm thickness of 0.5% Csn:ZnO thin film as an electron transport layer led to the average efficiency which was significantly higher than (9%) that of similar devices employing the same thickness of undoped ZnO film. Results showed that the devices fabricated with 1% and 2% cesium doped ZnO yielded lower power conversion efficiency, which could be due to the lower FF. Also, the influence of dopant incorporation on the optical transmittance and electrical conductivity of ZnO films was investigated.

  14. Sol-gel processing and physic-chemical characterization of La and Ce doped lead titanate ceramics

    Directory of Open Access Journals (Sweden)

    Guaaybess Y.

    2013-09-01

    Full Text Available PbTiO3 (PT sol gel processed powders doped with lanthanum (PLT14 and cerium (PLCexT14, x = 1; 3; 6; 10 were characterized by XRD and Raman spectroscopy. The samples crystallize in a pure perovskite phase at temperatures smaller than those reported for the same compounds prepared by other conventional methods. The effect of cerium or/and lanthanum on the crystal structure, microstructural and dielectric properties of PbTiO3 were investigated using FTIR, XRD, SEM, Raman spectroscopy and impedance spectroscopy. Incorporation of Ce reduces the temperature of crystallization of the samples, the temperature of the maximum of the permittivity and the diffuseness character of the ferroelectric to paraelectric transition, and enhances the permittivity.

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

    NARCIS (Netherlands)

    Kappert, Emiel; Pavlenko, Denys; Malzbender, J.; Nijmeijer, Arian; Benes, Nieck Edwin; Tsai, Peichun Amy

    2015-01-01

    Sol–gel-derived thin films play an important role as the functional coatings for various applications that require crack-free films to fully function. However, the fast drying process of a standard sol–gel coating often induces mechanical stresses, which may fracture the thin films. An experimental

  16. Tin dioxide sol-gel derived thin films deposited on porous silicon

    NARCIS (Netherlands)

    Cobianu, C.; Savaniu, Cristian; Buiu, Octavian; Dascalu, Dan; Zaharescu, Maria; Parlog, Constanta; van den Berg, Albert; Pecz, Bela

    1997-01-01

    Undoped and Sb-doped SnO2 sol¿gel derived thin films have been prepared for the first time from tin (IV) ethoxide precursor and SbCl3 in order to be utilised for gas sensing applications where porous silicon is used as a substrate. Transparent, crack-free and adherent layers were obtained on

  17. Tin dioxide sol-gel derived thin films deposited on porous silicon

    NARCIS (Netherlands)

    Cobianu, C.; Savaniu, Cristian; Buiu, Octavian; Zaharescu, Maria; Parlog, Constanta; van den Berg, Albert; Pecz, Bela; Dascula, Dan

    1996-01-01

    Undoped and Sb-doped SnO2 sol–gel derived thin films have been prepared for the first time from tin (IV) ethoxide precursor and SbCl3 in order to be utilised for gas sensing applications where porous silicon is used as a substrate. Transparent, crack-free and adherent layers were obtained on

  18. CuCr2O4 Spinel Ceramic Pigments Synthesized by Sol-Gel Self-Combustion Method for Solar Absorber Coatings

    Science.gov (United States)

    Ma, Pengjun; Geng, Qingfen; Gao, Xianghu; Yang, Shengrong; Liu, Gang

    2016-07-01

    A series of CuCr2O4 spinel ceramic pigments have been successfully synthesized via a facile and cost-effective sol-gel self-combustion method. The reaction mechanism was systematically studied using the corresponding characterization technologies. The results suggested that CuCr2O4 spinel ceramic pigments could be obtained at annealing temperature of 600 °C for 1 h, and the size, morphology, and crystallinity of CuCr2O4 spinel were greatly influenced by the annealing temperature. The as-burnt powder and CuCr2O4 spinel ceramic pigment were then employed to fabricate thickness sensitive spectrally selective (TSSS) paint coatings by a convenient spray-coating technique. The results revealed that spectral selectivity of TSSS paint coatings based on CuCr2O4 spinel ceramic pigments was much better than that of paint coatings based on the as-burnt powders. Furthermore, the effect of surface features of TSSS paint coatings on its optical property and hydrophobicity was investigated in detailed.

  19. Quartz Crystal Microbalance Coated with Sol-gel-derived Thin Films as Gas Sensor for NO Detection

    Directory of Open Access Journals (Sweden)

    S. J. O’Shea

    2003-10-01

    Full Text Available This paper presents the possibilities and properties of Indium tin oxide (ITO-covered quartz crystal as a NOx toxic gas-sensor. The starting sol-gel solution was prepared by mixing indium chloride dissolved in acetylacetone and tin chloride dissolved in ethanol (0-20% by weight. The ITO thin films were deposited on the gold electrodes of quartz crystal by spin-coating technique and subsequently followed a standard photolithography to pattern the derived films to ensure all sensors with the same sensing areas. All heat treatment processes were controlled below 500°C in order to avoid the piezoelectric characteristics degradation of quartz crystal (Quartz will lose its piezoelectricity at ~573°C due to the phase change from α to β. The electrical and structural properties of ITO thin films were characterized with Hall analysis system, TG/DTA, XRD, XPS, SEM and etc. The gas sensor had featured with ITO thin films of ~100nm as the receptor to sense the toxic gas NO and quartz crystal with frequency of 10MHz as the transducer to transfer the surface reactions (mass loading, etc into the frequency shift. A homemade setup had been employed to measure the sensor response under the static mode. The experimental results had indicated that the ITO-coated QCM had a good sensitivity for NO gas, ~12Hz/100ppm within 5mins. These results prove that the ITO-covered quartz crystals are usable as a gas sensor and as an analytical device.

  20. Palladium Surface Modification of Nanocrystalline Sol-Gel Derived Zinc Oxide Thin Films and its Effect on Methane Sensing

    Directory of Open Access Journals (Sweden)

    P. BHATTACHARYYA

    2009-11-01

    Full Text Available Nanocrystalline n-ZnO thin films were deposited on SiO2-coated p-Si substrates by a sol-gel method to fabricate ZnO-based resistive sensors. Two types of sol-gel ZnO based sensor structure, one as deposited and other with surface modified by palladium were investigated for methane sensing. The response magnitude, response time and recovery time were studied in the temperature range of 100-350 °C and at methane concentrations of 0.01 %, 0.05 %, 0.1 %, 0.5 %, 1 % and 1.5 % for both the sensor structure. The Pd modified sol-gel ZnO based sensor was found to provide lower operating temperature (150 °C, lower response (recovery time, higher response magnitude and higher sensing range for methane compared to its earlier reported unmodified counterpart (250 °C. With Pd modification ZnO was found to sense methane concentration as low as 0.01 % and as high as 1.5 % whereas for unmodified one this range was restricted between 0.1 % to 1.0 %.

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

    Science.gov (United States)

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

    1990-01-01

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

  2. Sol gel-derived hydroxyapatite films over porous calcium polyphosphate substrates for improved tissue engineering of osteochondral-like constructs.

    Science.gov (United States)

    Lee, Whitaik David; Gawri, Rahul; Pilliar, Robert M; Stanford, William L; Kandel, Rita A

    2017-10-15

    Integration of in vitro-formed cartilage on a suitable substrate to form tissue-engineered implants for osteochondral defect repair is a considerable challenge. In healthy cartilage, a zone of calcified cartilage (ZCC) acts as an intermediary for mechanical force transfer from soft to hard tissue, as well as an effective interlocking structure to better resist interfacial shear forces. We have developed biphasic constructs that consist of scaffold-free cartilage tissue grown in vitro on, and interdigitated with, porous calcium polyphosphate (CPP) substrates. However, as CPP degrades, it releases inorganic polyphosphates (polyP) that can inhibit local mineralization, thereby preventing the formation of a ZCC at the interface. Thus, we hypothesize that coating CPP substrate with a layer of hydroxyapatite (HA) might prevent or limit this polyP release. To investigate this we tested both inorganic or organic sol-gel processing methods, asa barrier coating on CPP substrate to inhibit polyP release. Both types of coating supported the formation of ZCC in direct contact with the substrate, however the ZCC appeared more continuous in the tissue formed on the organic HA sol gel coated CPP. Tissues formed on coated substrates accumulated comparable quantities of extracellular matrix and mineral, but tissues formed on organic sol-gel (OSG)-coated substrates accumulated less polyP than tissues formed on inorganic sol-gel (ISG)-coated substrates. Constructs formed with OSG-coated CPP substrates had greater interfacial shear strength than those formed with ISG-coated and non-coated substrates. These results suggest that the OSG coating method can modify the location and distribution of ZCC and can be used to improve the mechanical integrity of tissue-engineered constructs formed on porous CPP substrates. Articular cartilage interfaces with bone through a zone of calcified cartilage. This study describes a method to generate an "osteochondral-like" implant that mimics this

  3. Sol-gel derived manganese-releasing bioactive glass as a therapeutical approach for bone tissue engineering

    Energy Technology Data Exchange (ETDEWEB)

    Barrioni, B.R.; Oliveira, A.C.; Leite, M.F.; Pereira, M.M. [Universidade Federal de Minas Gerais (UFMG), MG (Brazil)

    2016-07-01

    Full text: Bioactive glasses (BG) have been highlighted in tissue engineering, due to their high bioactivity and biocompatibility, being potential materials for bone tissue repair. Its composition is variable and quite flexible, allowing the incorporation of therapeutic metallic ions, which has been regarded as a promising approach in the development of BG with superior properties for tissue engineering. These ions can be released in a controlled manner during the dissolution process of the glass, having the advantage of being released at the exactly implant site where they are needed, thus optimizing the therapeutic efficacy and reducing undesired side effects in the patient. Among several ions that have been studied, Manganese (Mn) has been shown to favor osteogenic differentiation. Besides, this ion is also a cofactor for several enzymes involved in remodeling of extracellular matrix, presenting an important role in cell adhesion. Therefore, it is very important to study the Mn role in the BG network and its influence on the glass bioactivity. In this context, new bioactive glass compositions derived from the 58S (60%SiO2-36%CaO-4%P2O5, mol%) were synthesized in this work, using the sol-gel method, by the incorporation of Mn into their structure. FTIR and Raman spectra showed the presence of typical BG chemical groups, whereas the amorphous structure typical of these materials was confirmed by XRD analysis, which also indicated that the Mn incorporation in the glass network was well succeeded, as its precursor did not recrystallize. The role of Mn in the glass network was also evaluated by XPS. The influence of Mn on carbonated hydroxyapatite layer formation after different periods of immersion of the BG powder in Simulated Body Fluid was evaluated using zeta potential, SEM, EDS and FTIR, whereas the controlled ion release was measured through ICP-OES. MTT assay revealed that Mn-containing BG showed no cytotoxic effect on cell culture. All these results indicate

  4. Scratch resistance of SiO{sub 2} and SiO{sub 2} - ZrO{sub 2} sol-gel coatings on glass-ceramic obtained by sintering; Resistencia al desgaste de recubrimientos sol-gel de SiO{sub 2} y SiO{sub 2} - ZrO{sub 2} sobre materiales vitroceramicos obtenidos por sinterizacion

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-10-01

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

  5. Nanocrystal/sol-gel nanocomposites

    Science.gov (United States)

    Petruska, Melissa A [Los Alamos, NM; Klimov, Victor L [Los Alamos, NM

    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

  6. Structure and optical properties of rare earth doped Y{sub 2}O{sub 3} waveguide films derived by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Guo, H.; Zhang, W.; Lou, L.; Brioude, A.; Mugnier, J

    2004-06-30

    Pure and rare earth ions doped yttrium oxide (Y{sub 2}O{sub 3}) waveguide films were prepared by a simple sol-gel process and dip-coating technique. Y{sub 2}O{sub 3} were successfully synthesized by hydrolysis of yttrium acetate. The structural evolution of Y{sub 2}O{sub 3} films with annealing temperature was investigated by X-ray diffraction, Fourier transform infrared spectroscopy, waveguide Raman spectroscopy and High-resolution transmission electron microscopy. The propagation loss of Y{sub 2}O{sub 3} thin films at 632.8 nm measured by scattering-detection method is approximately 1.5 dB/cm. The fluorescence of Er{sup 3+} and Eu{sup 3+} doped Y{sub 2}O{sub 3} waveguide thin films were studied under the waveguide configuration. The fluorescence intensities evolution with annealing temperature of Y{sub 2}O{sub 3}:Er{sup 3+} films has been studied and was explained by the multi-phonon non-radiative processes. Our results show that Y{sub 2}O{sub 3} is a good host material for optically active waveguide thin films and sol-gel process is a useful method to derive pure and doped Y{sub 2}O{sub 3} waveguide films.

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

    Directory of Open Access Journals (Sweden)

    Manish Kumar

    2011-06-01

    Full Text Available Mesoporous ZrO2 thin films have been deposited by a modified sol-gel dip coating technique using HCl as catalyst. Effects of sol-age on the surface and on the optical properties are studied. Transmission electron micrographs of the films reveal the pore dimensions in mesoporous regime. A strong correlation in surface topography with sol-age has been observed where increase in sol-age induces a systematic enhancement in the value of root mean square roughness of the films. Optical study shows that deposited films have high transmittance and an enhancement of 5.6 times in porosity in films prepared with sol-age of 10 days with respect to that of 1 day. Band gap estimation by Tauc's plots of films is observed to 5.74 eV, which shows invariance with the sol-age.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-10-01

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

  9. Sol-gel dip coating of yttria-stabilized tetragonal zirconia dental ceramic by aluminosilicate nanocomposite as a novel technique to improve the bonding of veneering porcelain.

    Science.gov (United States)

    Madani, Azamsadat; Nakhaei, Mohammadreza; Karami, Parisa; Rajabzadeh, Ghadir; Salehi, Sahar; Bagheri, Hossein

    2016-01-01

    The aim of this in vitro study was to evaluate the effect of silica and aluminosilicate nanocomposite coating of zirconia-based dental ceramic by a sol-gel dip-coating technique on the bond strength of veneering porcelain to the yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) in vitro. Thirty Y-TZP blocks (10 mm ×10 mm ×3 mm) were prepared and were assigned to four experimental groups (n=10/group): C, without any further surface treatment as the control group; S, sandblasted using 110 μm alumina powder; Si, silica sol dip coating + calcination; and Si/Al, aluminosilicate sol dip coating + calcination. After preparing Y-TZP samples, a 3 mm thick layer of the recommended porcelain was fired on the coated Y-TZP surface. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray analysis were used to characterize the coating and the nature of the bonding between the coating and zirconia. To examine the zirconia-porcelain bond strength, a microtensile bond strength (μTBS) approach was chosen. FT-IR study showed the formation of silica and aluminosilicate materials. XRD pattern showed the formation of new phases consisting of Si, Al, and Zr in coated samples. SEM showed the formation of a uniform coating on Y-TZP samples. Maximum μTBS values were obtained in aluminosilicate samples, which were significantly increased compared to control and sandblasted groups (P=0.013 and Pveneering porcelain.

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

    Directory of Open Access Journals (Sweden)

    Amir A. El Hadad

    2017-01-01

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

  11. Dependence Properties of Sol-Gel Derived CuO@SiO2 Nanostructure to Diverse Concentrations of Copper Oxide

    Directory of Open Access Journals (Sweden)

    V. Homaunmir

    2013-01-01

    Full Text Available Various concentrations of copper oxide were embedded into silica matrix of xerogel forms using copper source Cu(NO32·3H2O. The xerogel samples were prepared by hydrolysis and condensation of tetraethyl orthosilicate (TEOS with determination of new molar ratios of the components by the sol-gel method. In this paper, three samples of copper oxide were doped into silica matrices using different concentrations. We obtained 10, 20, and 30 wt.% of copper oxide in silica matrices labeled as A, B, and C, respectively. The absorption and transmittance spectra of the gel matrices were treated at different concentrations by Uv-vis spectrophotometer. Quantities of water and transparency in the silica network change the spectral characteristics of Cu2+ ions in the host silica. Absorption spectra of the samples heated to higher concentration complete the conversion of Cu2+ ions to Cu+ ions. The effects of concentration of copper oxide were characterized by X-ray diffraction (XRD patterns, and the transmission electron microscope (TEM micrographs. Also, textural properties of samples were studied by surface area analysis (BET method at different concentrations.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Chun-Cheng [Department of Electrical Engineering, National Cheng Kung University, Tainan 701, Taiwan (China); Department of Mathematic and Physical Sciences, R.O.C. Air Force Academy, Kaohsiung 820, Taiwan (China); Chen, Chan-Ching; Weng, Chung-Ming [Department of Electrical Engineering, National Cheng Kung University, Tainan 701, Taiwan (China); Chu, Sheng-Yuan, E-mail: chusy@mail.ncku.edu.tw [Department of Electrical Engineering, National Cheng Kung University, Tainan 701, Taiwan (China); Center for Micro/Nano Science and Technology, National Cheng Kung University, Tainan 701, Taiwan (China); Hong, Cheng-Shong [Department of Electronic Engineering, National Kaohsiung Normal University, Kaohsiung 802, Taiwan (China); Tsai, Cheng-Che [Department of Digital Game and Animation Design, Tung-Fang Design University, Kaohsiung 829, Taiwan (China)

    2015-02-28

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

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

    Science.gov (United States)

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

    2017-01-24

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

  14. MECHANISMS CONTROLLING Ca ION RELEASE FROM SOL-GEL DERIVED IN SITU APATITE-SILICA NANOCOMPOSITE POWDER

    Directory of Open Access Journals (Sweden)

    Seyed Mohsen Latifi

    2015-03-01

    Full Text Available Ca ion release from bioactive biomaterials could play an important role in their bioactivity and osteoconductivity properties. In order to improve hydroxyapatite (HA dissolution rate, in situ apatite-silica nanocomposite powders with various silica contents were synthesized via sol-gel method and mechanisms controlling the Ca ion release from them were investigated. Obtained powders were characterized by X-ray diffraction (XRD and transmission electron spectroscopy (TEM techniques, acid dissolution test, and spectroscopy by atomic absorption spectrometer (AAS. Results indicated the possible incorporation of (SiO44- into the HA structure and tendency of amorphous silica to cover the surface of HA particles. However, 20 wt. % silica was the lowest amount that fully covered HA particles. All of the nanocomposite powders showed more Ca ion release compared with pure HA, and HA - 10 wt. % silica had the highest Ca ion release. The crystallinity, the crystallite size, and the content of HA, along with the integrity, thickness, and ion diffusion possibility through the amorphous silica layer on the surface of HA, were factors that varied due to changes in the silica content and were affected the Ca ion release from nanocomposite powders.

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

    Energy Technology Data Exchange (ETDEWEB)

    Serrao, Felcy Jyothi, E-mail: jyothiserrao@gmail.com [Department of studies in Physics, Mangalore University, Mangalagangothri 574199 (India); Department of Physics, Karnataka Government Research centre SCEM, Mangalore, 575007 (India); Sandeep, K. M.; Bhat, Shreesha; Dharmaprakash, S. M. [Department of studies in Physics, Mangalore University, Mangalagangothri 574199 (India)

    2016-05-23

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

  16. Influence of synthesis and processing conditions on the release behavior and stability of sol-gel derived silica xerogels embedded with bioactive compounds.

    Science.gov (United States)

    Morpurgo, M; Teoli, D; Palazzo, B; Bergamin, E; Realdon, N; Guglielmi, M

    2005-08-01

    The influence of processing parameters and synthetic strategies in the properties of sol-gel derived silica matrices intended for the release of bioactive compounds was investigated. The time-evolution of the matrix properties during its aging at room temperature in the dry and wet forms was investigated by measuring some of its physical and drug retaining properties. The results indicate that long term gel aging in the wet form is fundamental for the obtainment of dry matrices that are stable upon storage, a fundamental requirement for any practical application. In the case of hybrid matrices obtained by replacing part of the tetraethoxysilane precursor with mono-methyl trimethoxysilane, the order of addition of the reaction component is also important in determining the properties of the final dry gel, probably by influencing the polymer structural properties. This parameter acts synergistically with the matrix composition in determining the release properties of xerogels embedded with bioactive compounds.

  17. Bioorganically doped sol-gel materials containing amyloglucosidase activity

    Directory of Open Access Journals (Sweden)

    Vlad-Oros Beatrice

    2006-01-01

    Full Text Available Amyloglucosidase (AMG from Aspergillus niger was encapsulated in various matrices derived from tetraethoxysilane, methyltriethoxysilane, phenyltriethoxysilane and vinyltriacetoxysilane by different methods of immobilization. The immobilized enzyme was prepared by entrapment in two steps, in one-step and entrapment/deposition, respectively. The activities of the immobilized AMG were assayed and compared with that of the native enzyme. The effects of the organosilaneprecursors and their molar ratios, the immobilization method, the inorganic support (white ceramic, red ceramic, purolite, alumina, TiO2, celite, zeolite and enzyme loading upon the immobilized enzyme activity were tested. The efficiency of the sol-gel biocomposites can be improved through combination of the fundamental immobilization techniques and selection of the precursors.

  18. Luminescence of aqueous reactions derived NiWO{sub 4} powders and sol-gel deposited films

    Energy Technology Data Exchange (ETDEWEB)

    He, Haiyan [Shaanxi University of Science and Technology (China). College of Materials Science and Engineering

    2010-03-15

    NiWO{sub 4} powders have been synthesized by reaction between NiCl{sub 2} and Na{sub 2}WO{sub 4} aqueous solutions and following calcinations at different temperatures. X-ray diffraction and scanning electron microscopy analysis were used to characterize the powders. Single phase NiWO{sub 4} powders were formed above a calcining temperature of 600 C. X-ray diffraction analysis indicated that the NiWO{sub 4} powders had a monoclinic structure and particle size of 26.8 nm and 30.3 nm for calcining temperatures of 600 C and 700 C, respectively. A little increase in intensity of the X-ray diffraction peaks was observed when increasing the calcining temperature from 600 C to 700 C. Scanning electron microscopy indicated that powders had uniform and very small particle size. The powders showed a broad blue-green emission band. The broad band of NiWO{sub 4} powders calcined at 600 C consisted of 423.2 nm (2.93 eV), 487.3 nm (2.54 eV) and two weak bands at 447.0 nm (2.77 eV), and 532.0 nm (2.33 eV). Small shifts in the peaks of excitation and luminescence and small increases in intensities were observed when increasing calcining temperature to 700 C. The films were deposited using the sol-gel method and using the precipitate as starting materials. The deposited films showed a similar blue-green emission to that of the powders. (orig.)

  19. A utilização de materiais obtidos pelo processo de sol-gel na construção de biossensores The utilization of materials obtained by the sol-gel process in biosensors construction

    Directory of Open Access Journals (Sweden)

    Antonio A. S. Alfaya

    2002-09-01

    Full Text Available The use of sol-gel materials to develop new biosensors has received great attention due to its characteristics and versatility of sol-gel process. An overview is presented of the state-of-the-art of electrochemical biosensors employing sol-gel materials. Low-temperature, porous sol-gel ceramics represent a new class for the immobilization of biomolecules. The rational design of sol-gel sensing materials, based on the judicious choice of the starting alkoxide, encapsulated reagents, and preparation conditions, allows tailoring of material properties in a wide range, and offers great potential for the development of electrochemical biosensors.

  20. Dielectric and magnetic properties of BaZn{sub Z}Co{sub 2-Z}Fe{sub 16}O{sub 27}/SiO{sub 2} microcrystalline glass ceramics prepared by citrate sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Haijun [High Temperature Ceramics Institute, Zhengzhou University, Henan 450052 (China); Yao Xi [Functional Materials Research Laboratory, Tongji University, Shanghai 200092 (China); Zhang Liangying [Functional Materials Research Laboratory, Tongji University, Shanghai 200092 (China)

    2003-03-21

    BaZn{sub Z}Co{sub 2-Z}Fe{sub 16}O{sub 27} (W-type hexaferrite)/SiO{sub 2} microcrystalline glass ceramics (Z = 0.0, 0.5, 0.8 and 1.1) were prepared by citrate sol-gel process, they were characterized by x-ray powder diffraction, scanning electron microscopy and thermogravimetry-differential scanning carlorimetry. The results show that the crystallizing temperature of W-type hexaferrite in the system BaO-Fe{sub 2}O{sub 3}-CoO-ZnO-SiO{sub 2} by sol-gel process is about 1200 deg. C, the average grain size of BaZn{sub Z}Co{sub 2-Z}Fe{sub 16}O{sub 27}/SiO{sub 2} microcrystalline glass ceramics is about 0.3 {mu}m. The complex dielectric constant and complex permeability of BaZn{sub Z}Co{sub 2-Z}Fe{sub 16}O{sub 27}/SiO{sub 2} has been studied as a function of the composition, frequency and annealing temperature. The real part of permeability decreases with increase of frequency, increases with increase of annealing temperature for all samples; the natural resonance phenomena are observed in imaginary component of permeability - frequency curves for all the samples annealed at 1200 deg. C, the natural resonance frequency shifts to lower frequency with increase of zinc content.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2017-03-15

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

  3. Absorbability of bulk sol-gel bioactive glasses

    Energy Technology Data Exchange (ETDEWEB)

    Hamadouche, M.; Meunier, A.; Blanchat, C.; Sedel, L. [Paris-7 Univ. (France). Lab. de Recherches Orthopediques; Greenspan, D.C.; Zhong, J.P.; Torre, G.P. la [US Biomaterials Corp., Alachua, FL (United States)

    2001-07-01

    Melt-derived bioactive glasses have been used with success in various clinical applications for over 10 years. Recently, particles of sol-gel derived bioactive glasses with an initial high specific area have exhibited high osteoconductive properties, but also a significant degradability. In this work, we explored the in-vivo bioactivity and degradability of bulk sol-gel derived glasses. Two sol-gel compositions (58S and 77S Bioglass) were used. Bulk 45S5 were used as a control. Both sol-gel derived demonstrated similar osteoconductive properties to 45S% Bioglass. In addition, absorbability was observed for sol-gel derived glasses after 12 weeks of implantation. Total absorption reached 40% after 52 weeks. No degradation could be measured in the case of 45S5 melt derived Bioglass. The degradation process was highly time dependent as demonstrated by regression analysis. New bone formation was found to fill in areas that had been resorbed similar to bone remodeling. New bone was found to fill in areas that had been absorbed, similar to natural bone remodeling. This absorbability can be assumed to be at least partially related to an osteoclastic resorption, as viable osteoclasts-like cells were found directly in contact with the glass surfaces. (orig.)

  4. Development and Characterization of 316 L Stainless Steel Coated by Melt-derived and Sol-gel derived 45S5 Bioglass for orthopedic applications

    Directory of Open Access Journals (Sweden)

    Seyed Morteza Naghib

    2012-03-01

    Full Text Available The 316L austenitic stainless steel (SS was coated by 45S5 bioactive glass produced by melting and sol-gel techniques to increase the bioactivity and to provide a high mechanical strength for orthopedic and dental applications. The morphologies of coated specimens were investigated by scanning electron microscopy (SEM. Then, the coated specimens were immersed in simulated body fluid (SBF at 37°C for 14 days, and their microstructures after withdrawal were also investigated by SEM. All the specimens were analyzed by FTIR and XRD in order to survey the formation of hydroxyapatite layer.

  5. Identification of TiO2 clusters present during synthesis of sol-gel derived TiO2 nano-particles

    DEFF Research Database (Denmark)

    Simonsen, Morten Enggrob; Søgaard, Erik Gydesen

    Synthesis of titanium dioxide nanoparticles with controlled size distribution and morphology are of great interest for many applications i.e. photocatalysis and dye sensitized solar cells (DSSC). The sol-gel method has some advantages over other preparation techniques in the many parameters, which...

  6. Synthesis, characterization and in vitro bioactivity of sol-gel-derived SiO{sub 2}-CaO-P{sub 2}O{sub 5}-MgO bioglass

    Energy Technology Data Exchange (ETDEWEB)

    Saboori, A.; Rabiee, M.; Moztarzadeh, F. [Amirkabir University of Technology, Faculty of Biomedical Engineering, Biomaterial Group, P. O. Box: 15875-4413, Tehran (Iran, Islamic Republic of); Sheikhi, M. [Tarbiat Modarres University, Faculty of Engineering, Ceramic Engineering Group, Tehran (Iran, Islamic Republic of); Tahriri, M. [Amirkabir University of Technology, Faculty of Biomedical Engineering, Biomaterial Group, P. O. Box: 15875-4413, Tehran (Iran, Islamic Republic of)], E-mail: m-tahriri@aut.ac.ir; Karimi, M. [Amirkabir University of Technology, Faculty of Biomedical Engineering, Biomaterial Group, P. O. Box: 15875-4413, Tehran (Iran, Islamic Republic of)

    2009-01-01

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

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

    Science.gov (United States)

    Berfield, Thomas A.

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

  8. In Vitro and In Vivo Evaluation of Sol-Gel Derived TiO2 Coatings Based on a Variety of Precursors and Synthesis Conditions

    Directory of Open Access Journals (Sweden)

    Krzysztof Marycz

    2014-01-01

    Full Text Available The effect of synthesis way of TiO2 coatings on biocompatibility of transplanted materials using an in vitro and in vivo rat model was investigated. TiO2 layers were synthesized by a nonaqueous sol-gel dip-coating method on stainless steel 316L substrates applying two different precursors and their combination. Morphology and topography of newly formed biomaterials were determined as well as chemical composition and elemental distribution of a surface samples. In vitro tests were conducted by adipose-derived mesenchymal stem cells cultured on TiO2 coatings and stainless steel without coatings to assess the bioreactivity of obtained materials. A positive biological effect of TiO2/316L/1 coatings—based on titanium(IV ethoxide—was found in both in vitro and in vivo models. The TiO2/316L/1 exhibited the highest roughness and the lowest titanium concentration in TiO2 than TiO2/316L/2—based on titanium(IV propoxide and TiO2/316L/3—based on both above-mentioned precursors. The proper fibroblast-like morphology and higher proliferation rate of cells cultured on TiO2/316L/1 were observed when compared to the other biomaterials. No inflammatory response in the bone surrounding implant covered by each of the obtained TiO2 was present. Our results showed that improvement of routinely used stainless steel 316L with TiO2/316L/1 layer can stimulate beneficial biological response.

  9. Enhancement of dielectric constant at percolation threshold in CaCu3 Ti4 O12 ceramic fabricated by both solid state and sol-gel process

    Science.gov (United States)

    Mukherjee, Rupam; Garcia, Lucia; Lawes, Gavin; Nadgorny, Boris

    2014-03-01

    We have investigated the large dielectric enhancement at the percolation threshold by introducing metallic RuO2 grains into a matrix of CaCu3Ti4O12 (CCTO). The intrinsic response of the pure CCTO samples prepared by solid state and sol-gel processes results in a dielectric constant on the order of 104 and 103 respectively with low loss. Scanning electron microscopy and energy dispersive x-ray spectroscopy indicate that a difference in the thickness of the copper oxide enriched grain boundary is the main reason for the different dielectric properties between these two samples. Introducing RuO2 metallic fillers in these CCTO samples yields a sharp increase of the dielectric constant at percolation threshold fc, by a factor of 6 and 3 respectively. The temperature dependence of the dielectric constant shows that the dipolar relaxation plays an important role in enhancing dielectric constant in composite systems.

  10. New infrared-assisted method for sol-gel derived ZnO:Ag thin films: Structural and bacterial inhibition properties.

    Science.gov (United States)

    González-Penguelly, Brenely; Morales-Ramírez, Ángel de Jesús; Rodríguez-Rosales, Miriam Guadalupe; Rodríguez-Nava, Celestino Odín; Carrera-Jota, María Luz

    2017-09-01

    A new sol-gel method, based on crystallization with Infrared heating, was developed to obtain ZnO:Ag thin films. The common sol, with zinc acetate as precursor and silver nitrate as doping source (1, 3 and 5 % molar), isopropanol and distilled water as solvents and monoethanolamine as stabilizer agent; was modified with Pluronic F127 and diethylene glycol as rheological agents, and with urea as fuel to produce enough energy to the combustion and to promote the crystallization process. Later, Corning glass-substrates were dipped into the sol at a constant speed of 3mms-1. To provide the necessary energy for obtaining the hexagonal ZnO structure of the coatings during the drying and consolidation process, instead of using the common furnace heat-treatment, the films were heated by means of an infrared (IR) ceramic lamp (800W) for 15, 30, 45, 60 and 180 minutes, and the effect of this annealing method was analyzed. The structural properties were examined by means of X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR), whereas morphology was studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The examination revealed a homogeneous distribution of particles with the characteristic pores of pluronic F127, and the coating roughness had an average value of 100nm by AFM. To evaluate the effect on the number of dipping cycles and the IR-treatment on the thickness, ellipsometry results for 1, 3 and 5 deposits were analyzed and showed increments of 780, 945 and 1082nm, respectively. Finally, to test of the antibacterial activity, instead of the common one-microorganism approach, environmental microorganisms that grow with expose of the broth to the ambient conditions were employed (microbial consortium), which is a real environmental condition. The biological test was carried out by kinetic growth inhibition (optical density) of heterotrophic bacteria in culture liquid media under conditions of light, light-dark and darkness

  11. Metal-silica sol-gel materials

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Srinet, Gunjan; Kumar, Ravindra; Sajal, Vivek

    2013-07-01

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

  13. Sol-gel precursors and products thereof

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-14

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

  14. Characterization of sol-gel synthesised lead-free (1 - x)Na{sub 0.5}Bi{sub 0.5}TiO{sub 3}-xBaTiO{sub 3}-based ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Chaouchi, A., E-mail: ahchaouchi@yahoo.fr [Laboratoire de Chimie Appliquee et Genie Chimique de l' Universite Mouloud Mammeri de Tizi-Ouzou (Algeria); Kennour, S. [Laboratoire de Chimie Appliquee et Genie Chimique de l' Universite Mouloud Mammeri de Tizi-Ouzou (Algeria); D' Astorg, S.; Rguiti, M.; Courtois, C. [Laboratoire des Materiaux Ceramiques et Procedes Associes - Universite de Valenciennes et du Hainaut-Cambresis, Z.I. du Champ de l' Abbesse, 59600 Maubeuge (France); Univ. Lille Nord de France, F-59000 Lille (France); Marinel, S. [Laboratoire CRISMAT, UMR 6508 CNRS/ENSICAEN 6 Bd Marechal Juin, 14050 Caen cedex (France); Aliouat, M. [Laboratoire de Chimie Appliquee et Genie Chimique de l' Universite Mouloud Mammeri de Tizi-Ouzou (Algeria)

    2011-09-15

    Highlights: > BaTiO{sub 3}-doped Bi{sub 0.5}Na{sub 0.5}TiO{sub 3} powders were synthesized by a sol-gel method. > Our results reveal that the 0.93Na{sub 0.5}Bi{sub 0.5}TiO{sub 3}-0.07BaTiO{sub 3} ceramic exhibits good polarization behaviour, interesting piezoelectric, dielectric and ferroelectric properties at room temperature (d{sub 33} = 120 pC/N, {epsilon}{sub r} = 1600, tan {delta} < 0.05, T{sub c} = 240 deg. C. - Abstract: The crystal structure, microstructure, dielectric and ferroelectric properties of (1 - x)Na{sub 0.5}Bi{sub 0.5}TiO{sub 3}-xBaTiO{sub 3} ceramics with x = 0, 0.03, 0.05, 0.07 and 0.1 are investigated. A structural variation according to the system composition was investigated by X-ray diffraction (XRD) analyses. The results revealed that the synthesis temperature for pure perovskite phase powder prepared by the present sol-gel process is much lower (800 deg. C), and a rhombohedral-tetragonal morphotropic phase boundary (MPB) is found for x = 0.07 composition which showing the highest remanent polarization value and the smallest coercive field. The optimum dielectric and piezoelectric properties were found with the 0.93Na{sub 0.5}Bi{sub 0.5}TiO{sub 3}-0.07BaTiO{sub 3} composition. The piezoelectric constant d{sub 33} is 120 pC/N and good polarization behaviour was observed with remanent polarization (P{sub r}) of 12.18 pC/cm{sup 2}, coercive field (E{sub c}) of 2.11 kV/mm, and enhanced dielectric properties {epsilon}{sub r} > 1500 at room temperature. The 0.93Na{sub 0.5}Bi{sub 0.5}TiO{sub 3}-0.07BaTiO{sub 3}-based ceramic is a promising lead-free piezoelectric candidate for applications in different devices.

  15. Inverted polymer solar cells with a low-temperature ramp annealed sol-gel derived aluminum-doped ZnO nano-ridge film as a cathode buffer layer

    Science.gov (United States)

    Li, Fan; Zhao, Jie; Hu, Ting; Chen, Yiwang

    2014-01-01

    The aluminum-doped zinc oxide (AZO) thin films with nano-ridge structures were fabricated via the low-temperature ramp annealed sol-gel derived process. The power conversion efficiency, especially the short circuit current density, was dramatically improved upon using the AZO nano-ridge structured thin films as the cathode buffer layers in inverted polymer solar cells (PSCs) with comparison to the intrinsic zinc oxide (i-ZnO) planar thin films. Furthermore, the thickness of AZO nano-ridge buffer layer can be enhanced significantly to about 120 nm without sacrificing the solar cell performance, which brings convenience to PSCs manufacturing by an industrial scale production.

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

    Energy Technology Data Exchange (ETDEWEB)

    King, C.M.; Thompson, M.C.; Buchanan, B.R. (Westinghouse Savannah River Co., Aiken, SC (USA)); King, R.B. (Georgia Univ., Athens, GA (USA). Dept. of Chemistry); Garber, A.R. (South Carolina Univ., Columbia, SC (USA). Dept. of Chemistry)

    1990-01-01

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

  17. Sol-gel synthesis and in vitro bioactivity of copper and zinc-doped silicate bioactive glasses and glass-ceramics.

    Science.gov (United States)

    Bejarano, Julian; Caviedes, Pablo; Palza, Humberto

    2015-03-11

    Metal doping of bioactive glasses based on ternary 60SiO2-36CaO-4P2O5 (58S) and quaternary 60SiO2-25CaO-11Na2O-4P2O5 (NaBG) mol% compositions synthesized using a sol-gel process was analyzed. In particular, the effect of incorporating 1, 5 and 10 mol% of CuO and ZnO (replacing equivalent quantities of CaO) on the texture, in vitro bioactivity, and cytocompatibility of these materials was evaluated. Our results showed that the addition of metal ions can modulate the textural property of the matrix and its crystal structure. Regarding the bioactivity, after soaking in simulated body fluid (SBF) undoped 58S and NaBG glasses developed an apatite surface layer that was reduced in the doped glasses depending on the type of metal and its concentration with Zn displaying the largest inhibitions. Both the ion release from samples and the ion adsorption from the medium depended on the type of matrix with 58S glasses showing the highest values. Pure NaBG glass was more cytocompatible to osteoblast-like cells (SaOS-2) than pure 58S glass as tested by 3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide (MTT) assay. The incorporation of metal ions decreased the cytocompatibility of the glasses depending on their concentration and on the glass matrix doped. Our results show that by changing the glass composition and by adding Cu or Zn, bioactive materials with different textures, bioactivity and cytocompatibility can be synthesized.

  18. One-pot synthesis of CdS nanoparticles exhibiting quantum size effect prepared within a sol-gel derived ureasilicate matrix

    Science.gov (United States)

    Gonçalves, Luis F. F. F.; Kanodarwala, Fehmida K.; Stride, John A.; Silva, Carlos J. R.; Gomes, Maria J. M.

    2013-12-01

    This paper describes a novel single-pot synthesis process based on sol-gel for the production of a highly transparent hybrid matrix containing CdS nanoparticles (NPs). The reaction between cadmium and sulphide ions in the presence of 3-mercaptopropyltrimethoxysilane (MPTMS) that originates the formation of quantum confined CdS NPs occurs simultaneously with the condensation and polymerization of the gel precursors that evolves to a macromolecular hybrid organic-inorganic network. The obtained xerogel matrix is based on the reaction of organically modified alkoxysilane (3-isocyanatepropyltriethoxysilane) and a di-amine functionalized oligopolyoxyethylene (Jeffamine ED-600). The final material is characterized as highly transparent, homogeneous and flexible xerogel incorporating stabilized and high crystalline CdS NPs that exhibit size-dependent optical properties due to quantum confinement of photogenerated e-h pairs as observed from UV-visible and photoluminescence spectroscopy and HRTEM microscopy measurements. The developed approach has obvious advantages comparatively to the alternative and more complex routes of production of composite materials with embedded semiconductor NPs because of the simplified one-pot preparative procedure used. The developed sol-gel process allows the control of the optical characteristics of the obtained CdS NPs embedded within the network by adjusting the molar ratio between cadmium ion and MPTMS and between cadmium and sulphide ions.

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

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Mingming, E-mail: liumm@mail.hzau.edu.cn [Key Laboratory of Arable Land Conservation (Middle and Lower Reaches of Yangtse River), Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Pi, Jiangyan; Wang, Xiaojie; Huang, Rong; Du, Yamei; Yu, Xiaoyang; Tan, Wenfeng; Liu, Fan [Key Laboratory of Arable Land Conservation (Middle and Lower Reaches of Yangtse River), Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Shea, Kenneth J., E-mail: kjshea@uci.edu [Department of Chemistry, University of California-Irvine, Irvine, CA 92697 (United States)

    2016-08-17

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

  20. Yb{sup 3+}-Er{sup 3+} co-doped sol-gel transparent nano-glass-ceramics containing NaYF{sub 4} nanocrystals for tuneable up-conversion phosphors

    Energy Technology Data Exchange (ETDEWEB)

    Yanes, A.C. [Dpto. Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain)], E-mail: ayanesh@ull.es; Santana-Alonso, A. [Dpto. Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Mendez-Ramos, J. [Dpto. Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Castillo, J. del [Dpto. Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Rodriguez, V.D. [Dpto. Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain)

    2009-07-08

    Transparent nano-glass-ceramics containing Yb{sup 3+}-Er{sup 3+} co-doped NaYF{sub 4} nanocrystals have been successfully developed for the first time by thermal treatment of precursor bulk glasses obtained by sol-gel technique. Precipitation of NaYF{sub 4} nanocrystals has been confirmed by X-ray diffraction measurements and their sizes have been determined by Scherrer's equation. Luminescence measurements confirm the partition of rare-earth ions in NaYF{sub 4} nanocrystals. Visible up-conversion luminescence has been obtained under infrared excitation at 980 nm. Up-conversion mechanisms have been discussed and the ratio between red and green up-conversion emission bands can be varied as a function of temperature of heat treatment and pump power resulting in colour tuneable up-conversion phosphors with applications in optical integrated devices. Colour tuneability has been also analyzed and quantified in terms of CIE standard chromaticity diagram.

  1. Luminescent properties of Eu{sup 3+}-Tb{sup 3+}-doped SiO{sub 2}-SnO{sub 2}-based nano-glass-ceramics prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Castillo, J. del [Departamento de Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain)], E-mail: fjvargas@ull.es; Yanes, A.C. [Departamento de Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Velazquez, J.J.; Mendez-Ramos, J.; Rodriguez, V.D. [Departamento de Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain)

    2009-04-03

    Transparent nano-glass-ceramics of composition 95SiO{sub 2}-5SnO{sub 2} mol%, single doped with 0.4 mol% of Tb{sup 3+} and co-doped with 0.4 mol% of Eu{sup 3+} and Tb{sup 3+} have been obtained by thermal treatment of precursor sol-gel glasses. The segregated SnO{sub 2} nanocrystals, precipitated in the insulator SiO{sub 2} glass matrix during heat treatment, constitute a wide band gap quantum-dot system with mean radius of nanocrystals around 2.2-2.8 nm, comparable to the bulk exciton Bohr radius. A fraction of the rare earth ions is incorporated to the SnO{sub 2} nanocrystals and can be excited by energy transfer from the semiconductor host. The efficiency of this energy transfer process is strongly dependent on the nanocrystal radius in the case of the Tb{sup 3+} ions, whereas the dependence is not appreciable in the case of Eu{sup 3+} ions. These results can be explained taking into account the variations of the overlap of the SnO{sub 2} broad visible emission due to oxygen vacancies with the rare earth excitation spectra.

  2. Effects of ion irradiation on the mechanical properties of SiNa wO xC yH z sol-gel derived thin films

    Science.gov (United States)

    Lucca, D. A.; Qi, Y.; Harriman, T. A.; Prenzel, T.; Wang, Y. Q.; Nastasi, M.; Dong, J.; Mehner, A.

    2010-10-01

    A study of the effects of ion irradiation of hybrid organic/inorganic modified silicate thin films on their mechanical properties is presented. NaOH catalyzed SiNa wO xC yH z thin films were synthesized by sol-gel processing from tetraethylorthosilicate (TEOS) and methyltriethoxysilane (MTES) precursors and spin-coated onto Si substrates. After drying at 300 °C, the films were irradiated with 125 keV H + or 250 keV N 2+ at fluences ranging from 1 × 10 14 to 2.5 × 10 16 ions/cm 2. Nanoindentation was used to characterize the films. Changes in hardness and reduced elastic modulus were examined as a function of ion fluence and irradiating species. The resulting increases in hardness and reduced elastic modulus are compared to similarly processed acid catalyzed silicate thin films.

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

    Directory of Open Access Journals (Sweden)

    B. L. Guo

    2014-09-01

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

  4. Hybrid electrode obtained by sol-gel derived Ni0.3Co2.7O4 nanoparticles incorporated into polypyrrole: Electrocatalysis of O2 reduction

    Directory of Open Access Journals (Sweden)

    Mourad Mechouet

    2016-06-01

    Full Text Available A hybrid electrode was formed on glassy carbon (GC electrode with polypyrrole (PPy and mixed valence Ni0.3Co2.7O4 nanoparticles to study their behaviour towards the oxygen reduction reaction (ORR. The oxide nanoparticles were prepared by sol-gel route using various parameters and characterized by XRD, SEM, EDX and BET methods. The result showed that desired oxide was obtained and nanocrystallites exhibit a specific surface area ranging from 39 to 73 m2/g with diameter varying from 13 to 25 nm. The hybrid electrode was then fabricated by electropolymerization of pyrrole (Py in the presence of the smallest Ni0.3Co2.7O4 nanoparticles in KCl (0.15 mol/L at room temperature and characterized by EDX, SEM and LSV methods. Investigation of the hybrid electrode confirmed that O2 reduction mechanism changes by applying potential. Thus, at low overpotential the O2 reduction involves two electrons and provides H2O2, with cathodic transfer coefficients (β of 0.33 and exchange current density ( j0 of about 8×10-3 mA/cm2, while, at high overpotential H2O2 is further reduced into H2O. The results also show that sol-gel method led to the preparation of Ni0.3Co2.7O4 nanoparticles having a spinel structure with a desired stoichiometry which exhibits a high electrocatalytic activity for reducing oxygen mostly to H2O2.

  5. Sol-gel deposited electrochromic coatings

    Energy Technology Data Exchange (ETDEWEB)

    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].

  6. Luminescence characterization of sol-gel derived Pr{sup 3+} doped NaGd(WO{sub 4}){sub 2} phosphors for solid state lighting applications

    Energy Technology Data Exchange (ETDEWEB)

    Durairajan, A., E-mail: durairajan.a@gmail.com [Crystal Growth Centre, Anna University, Chennai, 600025 (India); I3N-Aveiro, Department of Physics, University of Aveiro, Aveiro, 3810 193 (Portugal); Thangaraju, D. [Research Institute of Electronics, Shizuoka University, 3-5-1 Johoku, Hamamatsu, Shizuoka, 432-8011 (Japan); Moorthy Babu, S. [Crystal Growth Centre, Anna University, Chennai, 600025 (India); Valente, M.A. [I3N-Aveiro, Department of Physics, University of Aveiro, Aveiro, 3810 193 (Portugal)

    2016-08-15

    In the present work, xPr{sup 3+}:NaGd(WO{sub 4}){sub 2} (0.5 ≤ x ≤ 5.0 mol%) sub-micron phosphors were synthesised by sol-gel method. Low cost precursors of metal nitrates and low temperature thermal treatment was used compared to conventional solid state reaction. The formation of highly crystalline phosphors with tetragonal structure was confirmed by XRD and increase of Pr{sup 3+} ions content in host matrix leads to expansion of the unit cell volume. The surface morphology, size and particle distribution of the phosphors were observed by field emission scanning electron microscopy (FE-SEM). A rectangular shape particle with a size distribution ranging from 400 to 600 nm and tightly packed surface was seen in FE-SEM micrographs. The various internal and external phonon modes vibration corresponding to double tungstate structure was observed in Raman spectra. The optical properties of the synthesised phosphors were explored by ultraviolet visible (UV–Vis) absorption in diffuse reflectance and photoluminescence (PL) measurements. UV–Vis measurements distinguished the host and Pr{sup 3+} absorption and also reveal an increase in optical band gap values with an increase of Pr{sup 3+}. The PL measurements show various emissions from green and red regions under 450 nm. The maximum intensity emission at 489 nm is due to {sup 3}P{sub 0} → {sup 3}H{sub 4} transition of Pr{sup 3+}. From the maximum emission the critical doping concentration was calculated to be at 3.5 mol% and critical distance between two adjacent Pr{sup 3+} ions as 20.43 Å. - Highlights: • A sol-gel method was used to prepare Pr{sup 3+} doped NaGd(WO{sub 4}){sub 2} at low temperature. • Structural, spectroscopic, morphological, and optical and luminescence properties were studied. • The praseodymium ions are in trivalent state, the site symmetry is distorted and S{sub 4} local symmetry with Na{sup +} ions. • Strong green emission was observed under UV and visible excitation.

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

    Science.gov (United States)

    Liu, Mingming; Zeng, Zhaorui; Fang, Huaifang

    2005-05-27

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

  8. Effect of Annealing Temperature on Structural, Optical, and Electrical Properties of Sol-Gel Spin-Coating-Derived Cu2ZnSnS4 Thin Films

    Science.gov (United States)

    Hosseinpour, Rabie; Izadifard, Morteza; Ghazi, Mohammad Ebrahim; Bahramian, Bahram

    2018-02-01

    The effect of annealing temperature on structural, optical, and electrical properties of Cu2ZnSnS4 (CZTS) thin films grown on a glass substrate by spin coating sol-gel technique has been studied. Structural study showed that all samples had kesterite crystalline structure. Scanning electron microscopy images showed that the crystalline quality of the samples was improved by heat treatment. Optical study showed that the energy gap values for the samples ranged from 1.55 eV to 1.78 eV. Moreover, good optical conductivity values (1012 S-1 to 1014 S-1) were obtained for the samples. Investigation of the electrical properties of the CZTS thin films showed that the carrier concentration increased significantly with the annealing temperature. The photoelectrical behavior of the samples revealed that the photocurrent under light illumination increased significantly. Overall, the results show that the CZTS thin films annealed at 500°C had better structural, optical, and electrical properties and that such CZTS thin films are desirable for use as absorber layers in solar cells. The photovoltaic properties of the CZTS layer annealed at 500°C were also investigated and the associated figure of merit calculated. The results showed that the fabricated ZnS-CZTS heterojunction exhibited good rectifying behavior but rather low fill factor.

  9. In vitro characterisation of a sol-gel derived in situ silica-coated silicate and carbonate co-doped hydroxyapatite nanopowder for bone grafting.

    Science.gov (United States)

    Latifi, Seyed Mohsen; Fathi, Mohammadhossein; Sharifnabi, Ali; Varshosaz, Jaleh

    2017-06-01

    Design and synthesis of materials with better properties and performance are essential requirements in the field of biomaterials science that would directly improve patient quality of life. For this purpose, in situ silica-coated silicate and carbonate co-doped hydroxyapatite (Sc/S.C.HA) nanopowder was synthesized via the sol-gel method. Characterisation of the prepared nanopowder was carried out by XRD, FTIR, TEM, SEM, EDX, ICP, zeta potential, acid dissolution test, and cell culture test. The substitution of the silicate and carbonate ions into hydroxyapatite structure was confirmed by FTIR analysis. XRD analysis showed that silica is an amorphous phase, which played a role in covering the surface of the S.C.HA nanoparticles as confirmed by acid dissolution test. Low thickness and low integrity of the amorphous silica surface layer facilitated ions release from S.C.HA nanoparticles into physiological saline solution. Zeta potential of the prepared nanopowder suspended in physiological saline solution was -27.3±0.2mV at pH7.4. This negatively charged surface, due to the presence of amorphous silica layer upon the S.C.HA nanoparticles, not only had an accelerating effect on in vitro biomineralization of apatite, but also had a positive effect on cell attachment. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Effect of Annealing Temperature on Structural, Optical, and Electrical Properties of Sol-Gel Spin-Coating-Derived Cu2ZnSnS4 Thin Films

    Science.gov (United States)

    Hosseinpour, Rabie; Izadifard, Morteza; Ghazi, Mohammad Ebrahim; Bahramian, Bahram

    2017-10-01

    The effect of annealing temperature on structural, optical, and electrical properties of Cu2ZnSnS4 (CZTS) thin films grown on a glass substrate by spin coating sol-gel technique has been studied. Structural study showed that all samples had kesterite crystalline structure. Scanning electron microscopy images showed that the crystalline quality of the samples was improved by heat treatment. Optical study showed that the energy gap values for the samples ranged from 1.55 eV to 1.78 eV. Moreover, good optical conductivity values (1012 S-1 to 1014 S-1) were obtained for the samples. Investigation of the electrical properties of the CZTS thin films showed that the carrier concentration increased significantly with the annealing temperature. The photoelectrical behavior of the samples revealed that the photocurrent under light illumination increased significantly. Overall, the results show that the CZTS thin films annealed at 500°C had better structural, optical, and electrical properties and that such CZTS thin films are desirable for use as absorber layers in solar cells. The photovoltaic properties of the CZTS layer annealed at 500°C were also investigated and the associated figure of merit calculated. The results showed that the fabricated ZnS-CZTS heterojunction exhibited good rectifying behavior but rather low fill factor.

  11. A solid-phase microextraction coating of sol-gel-derived perhydroxy cucurbit[6]uril and its application on to the determination of polycyclic aromatic hydrocarbon.

    Science.gov (United States)

    Dong, Nan; Li, Tao; Luo, Yujie; Shao, Lin; Tao, Zhu; Zhu, Chun

    2016-10-28

    A novel solid-phase microextraction coating that contains perhydroxy cucurbit[6]uril((OH)12Q[6]) was prepared by a sol-gel method. (OH)12Q[6] was used as a starting coating material with hydroxy-terminated poly(dimethylsiloxane) (OH-PDMS) to bond chemically to a fused-silica substrate using 3-(2-cyclooxypropoxyl)propyltrimethoxysilane as cross-linking agent; hydrolysis and polycondensation reactions then led to the formation of a (OH)12Q[6]/PDMS-coating. The coating has a high thermal stability (360°C), long lifetime and can withstand organic and inorganic solvent rinsing because of the chemical binding between the coating and silica substrate. Its performance was tested by headspace (HS) solid-phase microextraction fiber coupled with gas chromatography to determine polycyclic aromatic hydrocarbon (PAHs) compounds in water samples. The (OH)12Q[6]/PDMS-coated fiber exhibited higher enrichment factors from fourfold for naphthalene to tenfold for pyrene compared with commercial PDMS fiber, and the enrichment factors increased with the number of condensed PAH rings. The strong adsorption affinity is believed to be attributed to hydrogen bonding and CH⋯π interactions between PAHs and (OH)12Q[6], according to the results of quantum chemical calculations. In the PAH analysis, the (OH)12Q[6]-coated fiber showed a good repeatability (river water samples and 90.23%-109.5% for local wastewater samples, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Effects of two-stage post-annealing process on microstructure and electrical properties of sol-gel derived non-stoichiometric NKN thin films

    Science.gov (United States)

    Lin, Chun-Cheng; Su, Chih-Wen; Weng, Chung-Ming; Chien, Yu-Chun; Chu, Sheng-Yuan; Huang, Chih-Yu; Hong, Cheng-Shong; Tsai, Cheng-Che

    2018-01-01

    Highly (100)-oriented lead-free Na0.5K0.5NbO3 (NKN) + 40 mol% Na(I) and K(I) thin films are fabricated on Pt/Ti/SiO2/Si substrates via a sol-gel processing method. A two-stage post-annealing process consisting of rapid thermal annealing (RTA) at various temperatures in the range of 650 ∼ 850 °C followed by tube furnace (TF) treatment at a temperature of 700 °C is then employed to modify the microstructure and chemical bonds of the NKN films in an attempt to improve their dielectric and ferroelectric properties. It is shown that the optimal values of the dielectric constant (ε = 658 at 100 kHz), dielectric loss (tanδ = 0.113 at 100 kHz), remnant polarization (2Pr = 17.1 μC/cm2 at 1 kHz), and coercive field (2Ec = 372 kV/cm at 1 kHz) are obtained when using an RTA temperature of 750 °C. The superior electrical properties of the NKN film are the results mainly of an improved crystallization, a higher film density and a denser grain structure. It is shown that the ferroelectric properties of the NKN film are maintained for more than 25000 cycles in thermal environments of less than 150 °C. Hence, it is inferred that NKN has good thermal stability and endurance for ferroelectric devices.

  13. Sensitized luminescence through nanoscopic effects of ZnO encapsulated in SiO{sub 2}:Tb{sup 3+} sol gel derived phosphor

    Energy Technology Data Exchange (ETDEWEB)

    Dhlamini, M.S., E-mail: mdhlamini@csir.co.z [National Center for Nanostructured Materials (NCNSM), CSIR (South Africa); Physics Department, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa); Ntwaeaborwa, O.M., E-mail: ntwaeab.sci@ufs.ac.z [Physics Department, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa); Swart, H.C. [Physics Department, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa); Ngaruiya, J.M. [Physics Department, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa); Department of Physics, Jomo Kenyatta Uniiversity of Agriculture and Technology, PO Box 62000, 00200 Nairobi (Kenya); Hillie, K.T. [National Center for Nanostructured Materials (NCNSM), CSIR (South Africa); Physics Department, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa)

    2009-12-01

    Terbium (1 mol%) doped ZnO-SiO{sub 2} binary system was prepared by a sol-gel process. Nanoscopic effects of ZnO on the photoluminescence (PL) and the cathodoluminescence (CL) properties were studied. Defects emission from ZnO nanoparticles was measured at 560 nm and the line emission from Tb{sup 3+} ions in SiO{sub 2}:Tb{sup 3+} and ZnO-SiO{sub 2}:Tb{sup 3+} with a major peak at 542 nm was measured. The PL excitation wavelength for 542 nm Tb{sup 3+} emission was measured at approx320 nm in both SiO{sub 2}:Tb{sup 3+} and ZnO-SiO{sub 2}:Tb{sup 3+}. The CL data showed quenched luminescence of the ZnO nanoparticles at 560 nm from a composite of ZnO-SiO{sub 2}:Tb{sup 3+} and a subsequent increase in 542 nm emission from the Tb{sup 3+} ions. This suggests that energy was transferred from the ZnO nanoparticles to enhance the green emission of the Tb{sup 3+} ions. The PL and CL properties of ZnO-SiO{sub 2}:Tb{sup 3+} binary system and possible mechanism for energy transfer from the ZnO nanoparticles to Tb{sup 3+} ions are discussed.

  14. Influence of Mg doping on the early steps of physico-chemical reactivity of sol-gel derived bioactive glasses in biological medium.

    Science.gov (United States)

    Soulié, J; Nedelec, J M; Jallot, E

    2009-11-28

    The aim of this study is to highlight the influence of magnesium doping on the surface reactivity of binary (SiO(2)-CaO) and ternary (SiO(2)-CaO-P(2)O(5)) bioactive glasses, prepared by sol-gel chemistry, in biological conditions. These materials were produced in powder form, and their compositional and textural properties characterized. They were then soaked in biological fluids for different delays from 0 to 4 days. The surface changes were characterized using Particles Induced X-ray Emission (PIXE) associated with Rutherford Backscattering Spectroscopy (RBS), which are efficient methods for multi-elemental analysis. Elemental maps of major and trace elements were obtained at a micrometer scale and revealed the formation of a calcium phosphate-rich layer after a few days of interaction. We demonstrate that the presence of magnesium in the material has an impact on the development and the formation rate of the bone-like apatite layer.

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

    Science.gov (United States)

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

    2014-09-01

    Highly pure SiO2 and SiO2 :RE nanoparticles were synthesized by the sol-gel method. The morphological, structural and optical properties of the nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). XRD results indicate that all the samples studied were free from impurities. SEM/TEM results indicate that the samples were well dispersed. Surface characterization of the nanocrystals by Fourier transform infrared spectroscopy has been carried out and the structure of surface-bound SiO2 based on spectral analysis is proposed. Thermoluminescence (TL) characteristics were investigated to study the influence of rare earth dopants (Tb, Ce, Eu, Dy) on SiO2 matrix subjected to 0.5 kG (1 h) γ-irradiation. Among these rare earth elements, Eu(3+) was found to be the most efficient dopant for SiO2 showing maximum thermoluminescence intensity. SiO2 :Eu0.5 seems to be a promising candidate for use as a TL dosimeter. Copyright © 2013 John Wiley & Sons, Ltd.

  16. Fabrication and characterization of novel iodine doped hollow and mesoporous hematite (Fe2O3) particles derived from sol-gel method and their photocatalytic performances.

    Science.gov (United States)

    Demirci, Selim; Yurddaskal, Metin; Dikici, Tuncay; Sarıoğlu, Cevat

    2018-03-05

    In this work, iodine (I) doped hollow and mesoporous Fe 2 O 3 photocatalyst particles were fabricated for the first time through sol-gel method. Phase structure, surface morphology, particle size, specific surface area and optical band gap of the synthesized Fe 2 O 3 photocatalysts were analyzed by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), X-ray photoelectron spectroscopy (XPS), BET surface analysis, particle size analyzer and UV-vis diffuse reflectance spectrum (UV-vis DRS), respectively. Also, electrochemical properties and photoluminescence spectra of Fe 2 O 3 particles were measured. The results illustrated that high crystalline, hollow and mesoporous Fe 2 O 3 particles were formed. The optical band gap values of the Fe 2 O 3 photocatalysts changed between 2.104 and 1.93eV. Photocatalytic efficiency of Fe 2 O 3 photocatalysts were assessed via MB solution. The photocatalytic activity results exhibited that I doping enhanced the photocatalytic efficiency. 1% mole iodine doped (I-2) Fe 2 O 3 photocatalyst had 97.723% photodegradation rate and 8.638×10 -2 min -1 kinetic constant which showed the highest photocatalytic activity within 45min. Moreover, stability and reusability experiments of Fe 2 O 3 photocatalysts were carried out. The Fe 2 O 3 photocatalysts showed outstanding stability after four sequence tests. As a result, I doped Fe 2 O 3 is a good candidate for photocatalysts. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. The effect of AgNO3 concentration on formation of Ag nanoparticles in Sol-Gel derived Ag-SiO2 thin films

    Directory of Open Access Journals (Sweden)

    A Babapour

    2007-12-01

    Full Text Available   In this investigation, Ag-SiO2 thin films with different concentrations of Ag (0.2, 0.4, 1.6 and 8% has been fabricated on soda-lime glass substrate using sol-gel method. After an annealing process, physical and chemical properties of the deposited silica films containing Ag nanoparticles have been studied including optical, topographical structural, morphological and size of the nanoparticle as well as their distribution using UV-visble spectrophotometery, atomic force microscopy (AFM, scanning electron microscopy (SEM, and transmission electron microscopy (TEM techniques, respectively. Based on our data analysis, the Ag nanoparticles did not form in the samples with low (0.2% and high Ag concentrations (8%, without any suitable annealing process. Instead, the nanoparticles were formed easily for the intermediate Ag concentrations. In fact, for the the low and high Ag concentration, the Ag nanoparticles formed at the annealing temperature of 200 º C. In addition, according to TEM observations, the minimum average size of the synthesized particles were determined about 4 hm for the thin films containing 0.2% Ag concentration.

  18. Suitability evaluation of sol-gel derived Si-substituted hydroxyapatite for dental and maxillofacial applications through in vitro osteoblasts response.

    Science.gov (United States)

    Balamurugan, A; Rebelo, A H S; Lemos, A F; Rocha, J H G; Ventura, J M G; Ferreira, J M F

    2008-10-01

    Si-hydroxyapatite (Si-HAP) has been used in orthopedic, dental, and maxillofacial surgery as a bone substitute. The aim of this investigation was to study the effect of Si substitution into the hydroxyapatite matrices and evaluate the biocompatibility effects of Si-HAP material in vitro with human osteoblasts. Silicon-substituted hydroxyapatite (Si-HAP) bioceramic materials were prepared by incorporating small amounts of silicon into the structure of hydroxyapatite [Ca10(PO4)6(OH)2, HAP] through a sol-gel method. A series of silicon substitutions ranging from 0, 1, 3 and 5 mol%, which are comparable to the measured silicon contents in natural bone, were performed. Single-phase Si-HAP was obtained upon calcining the as-prepared powders up to 800 degrees C since no secondary phases, such as tricalcium phosphate (TCP), tetracalcium phosphate (TeCP) or calcium oxide (CaO), were identified by X-ray diffraction analysis. The effects of silicon-substituted hydroxyapatite (Si-HAP) materials towards the responses of human osteoblast-like (HOB) cells were investigated and compared with pure hydroxyapatite. The Si-HAP indicated a significant increase in cell growth density with culture time irrespective of the amount of Si substituted in HAP. A high Si content (5 mol%) appears to promote rapid bone mineralization, since large amount of calcium phosphate minerals started to develop across the ECM by day 31 for a sample containing 5 mol% Si. On the other hand, a high Si content may result in fast dissolution of the material, owing to a decrease of HAP crystallite size, which might not be ideal for cell attachment for prolonged time periods. An optimum level of Si appears to exist at 3 mol%, which balances these effects.

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

    Energy Technology Data Exchange (ETDEWEB)

    Teh, Geok Bee, E-mail: sharonteh2009@gmail.com [Division of Bioscience and Chemistry, School of Arts and Science, Tunku Abdul Rahman College, Jalan Genting Kelang, 53300 Kuala Lumpur (Malaysia); Wong, Yat Choy [Faculty of Engineering and Industrial Sciences, Swinburne University of Technology, PO Box 218, Hawthorn, Victoria 3122 (Australia); Tilley, Richard D. [School of Chemical and Physical Sciences, MacDiarmid Institute of Advanced Materials and Nanotechnology, Victoria University of Wellington, PO Box 600, Wellington (New Zealand)

    2011-09-15

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

  20. The Sol-Gel-Xerogel Transition

    Science.gov (United States)

    1993-11-01

    relative mobili- ty are supported by the ESR (Electron Spin Resonance) studies of * * * Ikoma et al. [301 demonstrating that polyamine copper(II) chelates...deactivation of the triplet state of the molecule in the case of RTP. Recent studies on the photoisomerization of azobenzene in sol-gel glass films by

  1. Ceramic fibers from Sol-Gel precursors

    Energy Technology Data Exchange (ETDEWEB)

    Glaubitt, W.; Sporn, D.; Jahn, R. [Fraunhofer Institut fuer Silicatforschung, Wuerzburg (Germany)

    1995-09-01

    Powderless methods for the preparation of continuously spirmable alumina, mullite, spinel, yttrium alumina garnet (YAG) and lead zirconium titanate (PZT) precursors are presented. The Al containing solutions are based on alcoholysis, carboxylation and hydrolysis reactions, which are described in detail. In addition, a synthesis route for the preparation of piezoelectric PZT long fibers has also been developed. This novel PZT precursor contains lead subcarboxylate and zirconium titanium oxohydroxocarboxylate. In all cases, continuously spinnable precursors which have been extruded with velocities up to 200 m/min, have been obtained. Gel fibers of several kilometer length could be drawn directly from sols. After drying, pyrolysis and sintering, each of the {alpha}-Al{sub 2}O{sub 3}, mullite. spinel, YAG and PZT, fibers have been obtained.

  2. Efficient dual-wavelength excitation of Tb3+ emission in rare-earth doped KYF4 cubic nanocrystals dispersed in silica sol-gel matrix

    Science.gov (United States)

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

    2014-11-01

    Energy transfer from Ce3+ to Tb3+ ions under UV excitation, giving rise to visible emissions, is investigated in sol-gel derived transparent nano-glass-ceramics containing cubic KYF4 nanocrystals, for different doping concentrations of rare-earth ions. Moreover, visible emissions of Tb3+ are also obtained under near-infrared excitation through energy transfer from Yb3+ ions by means of cooperative up-conversion processes. Thus, Ce3+-Tb3+-Yb3+ doped nano-glass-ceramics can be activated in a dual-wavelength mode yielding efficient blue-green emissions of particular interest in photovoltaic silicon solar cells and white-light emitting diodes.

  3. Sol-gel modification of wood substrates to retard weathering

    Science.gov (United States)

    Mandla A Tshabalala; Sam Williams

    2008-01-01

    Wood specimens were treated with sol-gel systems based on metalorganic precursors of silicon (Si), iron (Fe), zirconium (Zr), and titanium (Ti). The effect of these sol-gel systems on weathering properties of wood was investigated. These sol-gel systems were found to have a positive effect on surface color stability and water vapor resistance of the specimens. Under...

  4. Epoxy Sol-Gel Hybrid Thermosets

    Directory of Open Access Journals (Sweden)

    Angels Serra

    2016-02-01

    Full Text Available Sol-gel methodologies are advantageous in the preparation of hybrid materials in front of the conventional addition of nanoparticles, because of the fine dispersion of the inorganic phase that can be reached in epoxy matrices. In addition, the use of organoalkoxysilanes as coupling agents allows covalent linkage between organic and inorganic phases, which is the key point in the improvement of mechanical properties. The sol-gel process involves hydrolysis and condensation reactions under mild conditions, starting from hydrolysable metal alkoxides, generally alkoxy silanes. Using the sol-gel procedure, the viscosity of the formulation is maintained, which is an important issue in coating applications, whereas the transparency of the polymer matrix is also maintained. However, only the proper combination of the chemistries and functionalities of both organic and inorganic structures leads to thermosets with the desired characteristics. The adequate preparation of hybrid epoxy thermosets enables their improvement in characteristics such as mechanical properties (modulus, hardness, scratch resistance, thermal and flame resistance, corrosion and antimicrobial protection, and even optical performance among others.

  5. Manufacturing of barium titanate thin films with designed microstructure by a sol-gel process: in-situ SAXS investigation of the precursor system

    Energy Technology Data Exchange (ETDEWEB)

    Stawski, Tomasz; Veldhuis, Sjoerd; Elshof, Johan ten; Goebel, Ole; Castricum, Hessel; Blank, Dave [University of Twente, Enschede (Netherlands). Inorganic Materials Science Group

    2010-07-01

    Barium titanate (BTO) is used as a high-k dielectric material in multi-layer ceramic capacitors. The minimum BTO layer thickness that can be achieved commercially with the state of the art tape casting methods is about 1 {mu}m, which implies the use of starting powders with a particle size of ca. 200 nm. Further downsizing requires finer powders. Wet-chemical methods based on sol-gel reactions are among most thoroughly investigated, and can also be applied to make BTO. Knowledge of the size, shape and kinetics of primary sol-gel derived oligomeric nanostructures in solution is crucial to optimize the processing of functional oxide thin films from these solutions. The barium titanate sol-gel precursor system was analyzed by small angle X-ray scattering analysis at the DUBBLE beamline at the ESRF in Grenoble. BTO sols were formed in the reaction of barium acetate, titanium isopropoxide and water in glacial acetic acid and 2-methoxyethanol. The relationship between size and dimensionality of the oligomers, and the influence of synthesis conditions (temperature, concentrations of reactants) were investigated. Evolutionary, systematic changes in the radii of gyration (R{sub g}) and internal structure of colloidal sols (characterized by the fractal dimension, D{sub f}) were monitored as a function of time.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P., E-mail: michelledunin@yahoo.com.b [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil)

    2010-07-01

    Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

  7. Effects of phosphorus-doping on energy band-gap, structural, surface, and photocatalytic characteristics of emulsion-based sol-gel derived TiO2 nano-powder

    Science.gov (United States)

    Ganesh, Ibram

    2017-08-01

    Different amounts of phosphorus (P)-doped TiO2 (PDT) nano-powders (P = 0-10 wt.%) were synthesized by following a new emulsion-based sol-gel (EBSG) route and calcined at 400 °C-800 °C for 6 h. These calcined PDT powders were then thoroughly characterized by means of XRD, XPS, SEM, FT-IR, FT-Raman, DRS, BET surface area, zeta-potential, cyclic-voltammetry and photocatalytic evaluation using methylene blue (MB) as a model-pollutant and established the effects of phosphorous doping on structural, surface, band-gap energy, and photocatalytic characteristics of TiO2 nano-powder formed in EBSG route. The characterization results suggest that the EBSG derived TiO2 nano-powder after calcination at 400 °C for 6 h is in the form of anatase phase when it was doped with 8 wt.% P. Furthermore, these EBSG derived PDT powders own high negative zeta-potentials, high specific surface areas (up to >250 m2/g), and suitable band-gap energies (PDT powders exhibit very high MB adsorption (up to 50%) from its aqueous 0.01 mM, 0.02 mM and 0.03 mM solutions during 30 min stirring in the dark, whereas, the commercial Degussa P-25 TiO2 nano-powder shows no adsorption. Among various photocatalysts investigated in this study, the 1 wt.% P-doped TiO2 nano-powder formed in EBSG route exhibited the highest photocatalytic activity for MB degradation reaction.

  8. Connectivity in sol-gel silica glasses

    Directory of Open Access Journals (Sweden)

    Wander L. Vasconcelos

    1998-07-01

    Full Text Available In this work it is carried out a review on structural parameters related to the evaluation of pore connectivity of nanostructures. The work describes parameters and methods of evaluation of geometric parameters. The concepts of connectivity are applied to silica gels and glasses obtained from sol-gel process. The study of pores connectivity was carried out using a combination of geometric modeling and experimental evaluation of specific surface area and pore volume. The permeability of the pore structure is evaluated and a permeability geometric factor, Pg, is proposed.

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

    Science.gov (United States)

    Uchiyama, Hiroaki; Matsui, Tadayuki; Kozuka, Hiromitsu

    2015-11-17

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

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

    Science.gov (United States)

    Tredwin, Christopher J; Young, Anne M; Georgiou, George; Shin, Song-Hee; Kim, Hae-Won; Knowles, Jonathan C

    2013-02-01

    Currently, most titanium implant coatings are made using hydroxyapatite and a plasma spraying technique. There are however limitations associated with plasma spraying processes including poor adherence, high porosity and cost. An alternative method utilising the sol-gel technique offers many potential advantages but is currently lacking research data for this application. It was the objective of this study to characterise and optimise the production of Hydroxyapatite (HA), fluorhydroxyapatite (FHA) and fluorapatite (FA) using a sol-gel technique and assess the rheological properties of these materials. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethylphosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the sol-gel derived FHA and FA. Optimisation of the chemistry and subsequent characterisation of the sol-gel derived materials was carried out using X-ray Diffraction (XRD) and Differential Thermal Analysis (DTA). Rheology of the sol-gels was investigated using a viscometer and contact angle measurement. A protocol was established that allowed synthesis of HA, FHA and FA that were at least 99% phase pure. The more fluoride incorporated into the apatite structure; the lower the crystallisation temperature, the smaller the unit cell size (changes in the a-axis), the higher the viscosity and contact angle of the sol-gel derived apatite. A technique has been developed for the production of HA, FHA and FA by the sol-gel technique. Increasing fluoride substitution in the apatite structure alters the potential coating properties. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

  11. Electrical and impedance spectroscopy analysis of sol-gel derived spin coated Cu2ZnSnS4 solar cell

    Science.gov (United States)

    Gupta, Goutam Kumar; Garg, Ashish; Dixit, Ambesh

    2018-01-01

    We carried out electrical and impedance studies on solution derived Al:ZnO/ZnO/CdS/Cu2ZnSnS4/Mo/Glass multilayered solar cell structures to understand their impact on photovoltaic performance. The Cu2ZnSnS4 layer is synthesized on a molybdenum (Mo) coated soda lime glass substrate as an absorber and characterized intensively to optimize the absorber physical properties. The optimized Cu2ZnSnS4 is p-type with 5.8 × 1017 cm-3 hole carrier concentration. The depletion width of the junction is around 20.5 nm and the diffusion capacitance is ˜35.5 nF for these devices. We observed relatively large minority carrier life time ˜23 μs for these structures using open voltage decay analysis. The measured Cu2ZnSnS4/MoS2 and Cu2ZnSnS4/CdS interface resistances are 7.6 kΩ and 12.5 kΩ, respectively. The spatial inhomogeneities are considered and the corresponding resistance is ˜11.4 kΩ. The impedance measurements suggest that in conjunction with series resistance ˜350 Ω, the interface and spatial inhomogeneity resistances also give a significant contribution to the photovoltaic performance.

  12. Dye Sensitized Solar Cell with Conventionally Annealed and Post-Hydrothermally Treated Nanocrystalline Semiconductor Oxide TiO2 Derived from Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Akhmad Yuwono

    2011-05-01

    Full Text Available Dye-sensitized solar cell (DSSC is one of the very promising alternative renewable energy sources to anticipate the declination in the fossil fuel reserves in the next few decades and to make use of the abundance of intensive sunlight energy in tropical countries like Indonesia. In the present study, TiO2 nanoparticles of different nanocrystallinity was synthesized via sol−gel process with various water to inorganic precursor ratio (Rw of 0.85, 2.00 and 3.50 upon sol preparation, followed with subsequent drying, conventional annealing and post-hydrothermal treatments. The resulting nanoparticles were integrated into the DSSC prototype and sensitized with an organic dye made of the extract of red onion. The basic performance of the fabricated DSSC has been examined and correlated to the crystallite size and band gap energy of TiO2 nanoparticles. It was found that post-hydrothermally treated TiO2 nanoparticles derived from sol of 2.00 Rw, with the most enhanced nanocrystalline size of 12.46 nm and the lowest band gap energy of 3.48 eV, showed the highest open circuit voltage (Voc of 69.33 mV.

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

    Energy Technology Data Exchange (ETDEWEB)

    Hesaraki, S., E-mail: S-hesaraki@merc.ac.ir

    2016-06-01

    This paper reports on strong and bioactive bone cement based on ternary bioactive SiO{sub 2}-CaO-P{sub 2}O{sub 5} glass particles and a photocurable resin comprising hydroxyethyl methacrylate (HEMA) and poly(acrylic/maleic) acid. The as-cured composite represented a compressive strength of about 95 MPa but it weakened during soaking in simulated body fluid, SBF, qua its compressive strength reached to about 20 MPa after immersing for 30 days. Biodegradability of the composite was confirmed by reducing its initial weight (~ 32%) as well as decreasing the molecular weight of early cured resin during the soaking procedure. The composite exhibited in vitro calcium phosphate precipitation in the form of nanosized carbonated hydroxyapatite, which indicates its bone bonding ability. Proliferation of calvarium-derived newborn rat osteoblasts seeded on top of the composite was observed during incubation at 37 °C, meanwhile, an adequate cell supporting ability was found. Consequently, it seems that the produced composite is an appropriate alternative for bone defect injuries, because of its good cell responses, high compressive strength and ongoing biodegradability, though more in vivo experiments are essential to confirm this assumption. - Highlights: • Light cure cement based on SiO{sub 2}-CaO-P{sub 2}O{sub 5} glass and polymer-like matrix was formed. • The matrix includes poly(acrylic/maleic acid) and poly(hydroxyethyl methacrylate). • The cement is as strong as polymethylmethacrylate bone cement. • The cement exhibits apatite formation ability in simulated body fluid. • The cement is biodegradable and supports proliferation of osteoblastic cells.

  14. Outdoor weathering of sol-gel-treated wood

    Science.gov (United States)

    Mandla A Tshabalala; Ryan Libert; Nancy Ross Sutherland

    2009-01-01

    Outdoor weathering of wood specimens treated with sol-gel formulations based on methyltrimethoxysilane (MTMOS), hexadecyltrimethoxysilane (HDTMOS), and ferric-zirconia-titania (Fe-Zr-Ti) sol was evaluated. The sol-gel process allowed deposition of a thin film of hybrid inorganic-organic networks (gel) in the wood cell wall that resulted in improved outdoor weathering...

  15. Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

    Science.gov (United States)

    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…

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

    Science.gov (United States)

    Malik, Abdul; Shearrow, Anne M.

    2017-01-31

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

  17. Self-Healing Corrosion Protective Sol-Gel Coatings

    NARCIS (Netherlands)

    Abdolah Zadeh, M.

    2016-01-01

    Inspired by the state of the art and the recent advances in the field of self-healing corrosion protective coatings, the thesis entitled “Self-healing corrosion protective sol-gel coatings” addresses novel routes to self-healing corrosion protective sol-gel coatings via extrinsic and intrinsic

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

    Energy Technology Data Exchange (ETDEWEB)

    King, C.M.; Thompson, M.C.; Buchanan, B.R. (Westinghouse Savannah River Co., Aiken, SC (United States)); King, R.B. (Georgia Univ., Athens, GA (United States). Dept. of Chemistry); Garber, A.R. (South Carolina Univ., Columbia, SC (United States). Dept. of Chemistry)

    1989-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    King, C.M.; Thompson, M.C.; Buchanan, B.R. [Westinghouse Savannah River Co., Aiken, SC (United States); King, R.B. [Georgia Univ., Athens, GA (United States). Dept. of Chemistry; Garber, A.R. [South Carolina Univ., Columbia, SC (United States). Dept. of Chemistry

    1989-12-31

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

  20. Effects of phosphorus-doping on energy band-gap, structural, surface, and photocatalytic characteristics of emulsion-based sol-gel derived TiO{sub 2} nano-powder

    Energy Technology Data Exchange (ETDEWEB)

    Ganesh, Ibram, E-mail: ibramganesh@arci.res.in

    2017-08-31

    Highlights: • Reported a novel route to synthesize high specific surface area P-doped TiO{sub 2} nano-powder photocatalysts. • Established methylene blue dye-sensitization mechanism of TiO{sub 2} photocatalyst. • Established the effects of methylene blue adsorption on the surface, structural and photocatalytic activity of P-doped TiO{sub 2}. • Established true quantum efficiency determination method for TiO{sub 2} photocatalysis. - Abstract: Different amounts of phosphorus (P)-doped TiO{sub 2} (PDT) nano-powders (P = 0–10 wt.%) were synthesized by following a new emulsion-based sol-gel (EBSG) route and calcined at 400 °C–800 °C for 6 h. These calcined PDT powders were then thoroughly characterized by means of XRD, XPS, SEM, FT-IR, FT-Raman, DRS, BET surface area, zeta-potential, cyclic-voltammetry and photocatalytic evaluation using methylene blue (MB) as a model-pollutant and established the effects of phosphorous doping on structural, surface, band-gap energy, and photocatalytic characteristics of TiO{sub 2} nano-powder formed in EBSG route. The characterization results suggest that the EBSG derived TiO{sub 2} nano-powder after calcination at 400 °C for 6 h is in the form of anatase phase when it was doped with <8 wt.% P, and it is in the amorphous state when doped with >8 wt.% P. Furthermore, these EBSG derived PDT powders own high negative zeta-potentials, high specific surface areas (up to >250 m{sup 2}/g), and suitable band-gap energies (<3.34 eV). Surprisingly, these PDT powders exhibit very high MB adsorption (up to 50%) from its aqueous 0.01 mM, 0.02 mM and 0.03 mM solutions during 30 min stirring in the dark, whereas, the commercial Degussa P-25 TiO{sub 2} nano-powder shows no adsorption. Among various photocatalysts investigated in this study, the 1 wt.% P-doped TiO{sub 2} nano-powder formed in EBSG route exhibited the highest photocatalytic activity for MB degradation reaction.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Dae-Sung; Ryu, Bong-ki [Pusan National University, Busan (Korea, Republic of)

    2017-04-15

    In this study, quaternary phosphate-based sol-gel derived glasses were synthesized from a P{sub 2}O{sub 5}-CaO-Na{sub 2}O-TiO{sub 2} system with a high TiO{sub 2} content of up to 50 mol%. The sol-gel method was chosen because incorporating a high percentage of titanium into a phosphate network via traditional melt-quench methods is non-trivial. The structure and thermal properties of the obtained stabilized sol-gel glasses were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and differential scanning calorimetry (DSC). The XRD results confirmed the amorphous nature of all of the stabilized sol–gel derived glasses. The FTIR results revealed that added TiO{sub 2} enters the network as (TiO{sub 6}), which likely acts as a modifier oxide. Consequently, the number of terminal oxygen atoms increases, leading to an increase in the number of P-OH bonds. In addition, DSC results confirmed a decrease in glass transition and crystallization temperatures with increasing TiO{sub 2} content. This is the first report of a sol-gel synthesis strategy combined with enameling to prepare glass at low processing temperatures and the first use of such a system for both hydrophilic and chemical resistance purposes.

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

    Science.gov (United States)

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

    2014-02-18

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

  4. Investigation of Sol-Gel coatings exposed in the condenser at Fynsvaerket. Part 2

    Energy Technology Data Exchange (ETDEWEB)

    Montgomery, M. [DTU Management Engineering, Kgs. Lyngby (Denmark); Vilhelmsen, T. [Vattenfall Heat Nordic, Copenhagen (Denmark); Bennedsen, J. [Teknologisk Institut, Aarhus (Denmark)

    2008-12-15

    The Danish Technological Institute (DTI) has developed a technique using Hybrid Sol-gel nanotechnology to produce coatings which can change the surface characteristics of various components. It is the purpose of this project to investigate where such coatings can be utilised in the power generating industry with respect to fouling and corrosion resistance. Sol-gel coatings have glass-ceramic properties and their fundamental chemical structure is based on silanes (methane where carbon is replaced with silicon) with an amorphous (not crystalline) structure. The basic structure can be modified with various metallic nanoparticles to change the properties of the coatings. In the sol-gel process, the liquid reagents are mixed together to form a sol-gel which is then applied on the surface of a component either by dipping or painting. After that the component is cured at a temperature of 160 deg. C to result in a glass ceramic surface. A report has been written with the initial results with sol-gel coatings on the condenser tubes at Fysnvaerket. Due to the presence of corrosion products on the unexposed tubes which influences the adherence and protectiveness of coatings applied, the effect of sol-gel coatings were difficult to assess. Two different sol-gel coatings have been applied to brass condenser tubes about 10 cm in length. Based on the experience from previous exposures, the surface of the condenser tubes was mechanically cleaned before coating with the sol-gel components. One set was sandblasted and the other set was grinded to a polished finish using sandpaper. The specimens grinded and polished were exposed tubes that had been removed from the condenser. Sections of unexposed cleaned condenser tubes with and without sol-gel are also investigated as control specimens. Before application of the coatings, the tubes were mechanically cleaned either by sandblasting or by grinding to a polished finish. The exact composition of these different coatings was not known

  5. Influence of Li2CO3 and V2O5 combined additions on the sintering and dielectric properties of Ca0.5Sr0.5TiO3 ceramics prepared from powders synthesized by sol-gel method

    Directory of Open Access Journals (Sweden)

    Nouara Lamrani

    2014-06-01

    Full Text Available In this work, we have studied the influence of lithium carbonate (Li2CO3 associated with the vanadium oxide (V2O5 on sintering and dielectrics properties of Ca0.5Sr0.5TiO3 ceramic materials obtained from nanopowder synthesized by sol-gel method. The nanopowder was obtained by controlled mixing of titanium butoxide dissolved in butanol-2 and acetic acid with a saturated aqueous solution of calcium acetate and strontium carbonate and subsequent drying of the formed gel at 80 °C and calcination at 1100 °C. The synthesized nanopowder was mixed with different amount of additives, and then uniaxally pressed and sintered in air atmosphere at temperature determined by dilatomertic measurements. The pure Ca0.5Sr0.5TiO3 sample obtained by this process required a sintering temperature around 1500 °C. The addition of Li2CO3 combined with V2O5 improved sinterability and caused a shift of dilatimeric shrinkage curve to much lower temperatures. Thus, dense ceramics (98% of theoretical density were obtained at sintering temperature ≤ 1300 °C. The effect of adding Li2CO3-V2O5 on the structure of ceramics and the dielectric properties is discussed and show that type I dielectric properties (linear variation of the permittivity are conserved, but with an increase of dielectric loss.

  6. Structural, dielectric and optical properties of sol-gel synthesized 0.55Ba(Zr{sub 0.2}Ti{sub 0.8})O{sub 3}-0.45(Ba{sub 0.7}Ca{sub 0.3})TiO{sub 3} ceramic

    Energy Technology Data Exchange (ETDEWEB)

    Rani, Jyoti; Yadav, K.L. [Indian Institute of Technology Roorkee, Smart Materials Research Laboratory, Department of Physics, Roorkee (India); Prakash, Satya [Indian Institute of Technology Roorkee, Metallurgical and Materials Engineering Department, Roorkee (India)

    2014-11-15

    Lead-free polycrystalline ceramic 0.55Ba(Zr{sub 0.2}Ti{sub 0.8})O{sub 3}-0.45(Ba{sub 0.7}Ca{sub 0.3})TiO{sub 3} (0.55BZT-0.45BCT) was synthesized by sol-gel method and the dielectric, impedance and optical properties of this ceramic were studied. X-ray diffraction analysis revealed the formation of pure perovskite phase with the coexistence of tetragonal and rhombohedral structures. The high value of dielectric constant (∝6,985) with low dielectric loss (∝0.013) was obtained at room temperature. Bulk and grain boundary resistances were measured by impedance analysis, which revealed negative temperature coefficient of resistance behaviour in this ceramic. The estimated value of optical band gap was found to be ∝3.16 eV, which is related to the presence of intermediate energy levels. Two emission bands one at ∝365 nm (UV region) and another at ∝465 nm (blue region) were observed in photoluminescence spectrum at room temperature. (orig.)

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

    Directory of Open Access Journals (Sweden)

    Ting Ke Tseng

    2010-05-01

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

  8. Industrial solvents analyzed on SolGel-WAX(TM)

    National Research Council Canada - National Science Library

    Angus Hibberd; Gerard Sharp; Dan DiFeo

    2002-01-01

    ... phase-bonding process in which the polyethylene glycol phase is encapsulated into a sol-gel matrix. The SolGel-WAX column, by the nature of the sol-gel bonding, is an extremely inert, low-bleed, high-temperature column. This inertness gives excellent peak shape of difficult-to-- analyze polar solvents. The high thermal stability gives a low-bleed column and therefore higher signal-to-noise ratio allowing lower detection limits, which is essential in many industrial processes. Also note the excellent separa...

  9. Electrophoretic Porosimetry of Sol-Gels

    Science.gov (United States)

    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.

  10. Micro-ion beam analysis of physico-chemical reactions in vitro induced by nano-structured sol-gel derived bioactive glasses; Caracterisation par micro-faisceau d'ions des reactions physico-chimiques induites in vitro par des verres bioactifs nanostructures elabores par la methode sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Lao, J

    2007-07-15

    The study of bioactive glasses is a multi-field area of research aiming at a major goal: the development of new generation biomaterials that would be able to bond with host tissues through the formation of a strong interfacial bond, together with helping the body heal itself through the stimulation of specific cellular responses. Thus clinical applications of bioactive glasses mainly concern dental surgery and orthopedics, for filling osseous defects. For this purpose, we have elaborated bioactive glasses in the binary SiO{sub 2}-CaO system, ternary SiO{sub 2}-CaO-P{sub 2}O{sub 5} system, and for the first time, to our knowledge, strontium-doped SiO{sub 2}-CaO-SrO and SiO{sub 2}-CaO-P{sub 2}O{sub 5}-SrO glasses. The materials were elaborated using the sol-gel process, which allowed the synthesis of nano-porous materials with great purity and homogeneity. The bio-activity of the glasses was clearly demonstrated in vitro: in contact with biological fluids, the whole lot of mate-rials were able to induce the formation of a Ca-P-Mg layer a few microns thick at their surface. Our work is characterized by the use of PIXE-RBS nuclear microprobes to study the bioactive glass/biological fluids interface. Thanks to these methods we obtained chemical maps that made possible the analysis of major and trace elements concentrations at the interface. Moreover, quantitative information regarding the local reactivity of glasses were acquired. These data are important to evaluate the kinetics and amplitude of the physico-chemical reactions involved in the bio-activity process. Thus, we highlighted that the binary glass is the highest reactive regarding the dissolution of the glassy matrix as well as the first appearance of the Ca-P rich layer. However the Ca/P atomic ratio calculated at the glass/biological fluids interface decreases slowly, indicating that the Ca-P-Mg layer encounters difficulties to be changed into a more stable apatitic phase. For the P-containing glasses, the de

  11. Sintering behavior of nano-ceramic coatings

    NARCIS (Netherlands)

    De Hosson, JTM; Popma, R; Hooijmans, J; Komarneni, S; Parker, JC; Hahn, H

    2000-01-01

    This paper concentrates on the densification of sol gel derived thin nano-ceramic coatings by laser radiation and by furnace treatment. Deposition of the film is done by means of spin coating of Zirconia. The sintering of the layer is observed using a number of different measuring techniques.

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

    Science.gov (United States)

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

    2011-10-01

    Lead-free NaBi(0.5)TiO(3) (NBT) ferroelectric thick films were prepared by a poly(vinylpyrrolidone) (PVP) modified sol-gel method. The NBT thick films annealed from 500°C to 750°C exhibit a perovskite structure. The relationship between annealing temperature, thickness, and electrical properties of the thick films has been investigated. The dielectric constants and remnant polarizations of the thick films increase with annealing temperature. The electrical properties of the NBT films show strong thickness dependence. As thickness increases from 1.0 to 4.8 μm, the dielectric constant of the NBT films increases from 620 to 848, whereas the dielectric loss is nearly independent of the thickness. The remnant polarization of the NBT thick films also increases with increasing thickness. The leakage current density first decreases and then increases with film thickness.

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

    Science.gov (United States)

    Fang, Jonathan

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-01

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

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

    DEFF Research Database (Denmark)

    Mikkelsen, Morten Bo Lindholm

    2011-01-01

    of the material. At early stages of gelation, thin gel coatings can be structured by nanoimprint lithography, and purely inorganic silica materials can be obtained by subsequent thermal annealing. The sol-gel process thus constitutes a unique method for nanofabrication of silica materials of special properties....... In this work, sol-gel silica is introduced as a new material class for the fabrication of lab-on-a-chip devices for DNA analysis. An imprint process with a rigid, non-permeable stamp was developed, which enabled fabrication of micro- and nanofluidic silica channels in a single process step without use of any......, continuous tumbling across the grooves called the ’tumbleweed’. Dynamical transitions between the two states cause DNA molecules to exhibit both size- and topology-dependent velocities that may be utilized for separation. By templating the porosity of sol-gel silica with sub-wavelength latex particles...

  16. Transparent conductive CuFeO2 thin films prepared by sol-gel processing

    Science.gov (United States)

    Chen, Hong-Ying; Wu, Jia-Hao

    2012-03-01

    In this study, transparent conductive CuFeO2 thin films were deposited onto a quartz substrate using a low-cost sol-gel process and sequential annealing in N2. The sol-gel derived films were annealed at 500 °C for 1 h in air and then annealed at 700 °C in N2 for 2 h. The CuO and CuFe2O4 phases appeared as the film annealed in air, and a single CuFeO2 phase (delafossite, R3m) appeared as the film annealed in N2. X-ray photoelectron spectroscopy showed that the chemical composition of the CuFeO2 thin films was similar to the stoichiometry. The optical bandgap of the CuFeO2 thin films was 3.1 eV. The p-type characteristics of the films were verified by Hall-effect measurements. The electrical conductivity and carrier concentration of the CuFeO2 thin films were 0.358 S cm-1 and 5.34 × 1018 cm-3, respectively. These results show that the proposed low-cost sol-gel process provides a feasible method of depositing transparent CuFeO2 thin films.

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

    Energy Technology Data Exchange (ETDEWEB)

    Danchova, Nina; Gutzov, Stoyan [Sofia Univ. ' St Kliment Ohridski' (Bulgaria). Dept. of Physical Chemistry

    2014-02-15

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

  18. Effect of pH on electrical and optical properties of sol-gel derived microcrystalline Ba 0.5Sr 0.5TiO 3 thin films

    Science.gov (United States)

    Roy, Somnath C.; Sharma, G. L.; Bhatnagar, M. C.; Manchanda, R.; Balakrishnan, V. R.; Samanta, S. B.

    2004-09-01

    Ba 0.5Sr 0.5TiO 3 thin films have been deposited by sol-gel spin coating technique and effect of pH of the precursor sol on the electrical and optical properties has been investigated. Thin films of about 480 nm thickness were deposited on platinised silicon (Pt/TiN/SiO 2/Si) and fused quartz substrates using precursor sols of pH 2.8 and 4.8. The pH of the precursor sol is found to have a pronounced effect on the surface morphology, electrical and optical properties of the deposited BST thin films. X-ray diffractograms and atomic force micrographs show increase in the grain size with the increase in pH of the precursor sol. The grain size was found to increase from about 80 nm to about 120 nm. The dielectric constant was also found to increase from 325 to 340 with increase in the pH of the precursor sol. The dielectric loss, however, changes slightly from 0.036 to 0.052. As a consequence the leakage current and interfacial charge densities also increase. The optical studies reveal that the band-gap decreases from 3.75 to 3.66 eV with increase in the pH.

  19. Investigations of sol-gel-derived highly (100)-oriented Ba{sub 0.5}Sr{sub 0.5}TiO{sub 3}: MgO composite thin films for phase-shifter applications

    Energy Technology Data Exchange (ETDEWEB)

    Jain, M.; Majumder, S.B.; Katiyar, R.S. [University of Puerto Rico, Department of Physics, P.O. Box 23 343, San Juan (Puerto Rico); Bhalla, A.S. [The Pennsylvania State University, Materials Research Institute, University Park, PA (United States); Miranda, F.A.; Van Keuls, F.W. [NASA, Glenn Research Center, Cleveland, OH (United States)

    2005-02-01

    Sol-gel deposition of highly oriented Ba{sub 0.5}Sr{sub 0.5}TiO{sub 3}:MgO composite thin films has shown desirable dielectric constant reduction and higher figure of merit for phase-shifter applications. In this multilayer configuration, MgO distributed homogeneously through the Ba{sub 0.5}Sr{sub 0.5}TiO{sub 3} (BST50) matrix, and it helped in tailoring the dielectric constant and reducing the loss tangent significantly. In the present study, the high-frequency dielectric behavior of the films has been evaluated by fabricating an eight-element coupled microstrip phase shifter and measuring the degree of phase shift and insertion loss as a function of applied voltage at room temperature. An increase in phase-shifter figure of merit (degree of phase shift per dB insertion loss) from 28 /dB for pure BST50 to 71 /dB for a BST50:MgO film (at 14 GHz and 333 kV/cm) has been observed. (orig.)

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

    Science.gov (United States)

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

    2011-04-01

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

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

    Science.gov (United States)

    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...

  2. Neutron detector based on lithiated sol-gel glass

    CERN Document Server

    Wallace, S; Miller, L F; Dai, S

    2002-01-01

    A neutron detector technology is demonstrated based on sup 6 Li/ sup 1 sup 0 B doped sol-gel glass. The detector is a sol-gel glass film coated silicon surface barrier detector (SBD). The ionized charged particles from (n, alpha) reactions in the sol-gel film enter the SBD and are counted. Data showing that gamma-ray pulse amplitudes interfere with identifying charged particles that exit the film layer with energies below the gamma-ray energy is presented. Experiments were performed showing the effect of sup 1 sup 3 sup 7 Cs and sup 6 sup 0 Co gamma rays on the SBD detector. The reaction product energies of the triton and alpha particles from sup 6 Li are significantly greater than the energies of the Compton electrons from high-energy gamma rays, allowing the measurement of neutrons in a high gamma background. The sol-gel radiation detection technology may be applicable to the characterization of transuranic waste, spent nuclear fuel and to the monitoring of stored plutonium.

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

    NARCIS (Netherlands)

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

    1998-01-01

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

  4. Sol-gel derived nanocrystalline multiferroic BiFeO{sub 3} and R{sup 3+} (R=Er and Tm) doped therein: Magnetic phase transitions and enhancement of magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Acharya, S.; Sutradhar, S.; Mandal, J.; Mukhopadhyay, K. [Solid State Research Lab., Department of Physics, Burdwan University, Burdwan 713104, WB (India); Deb, A.K. [Department of Physics, Raiganj College (University College), Uttar Dinajpur 733134, WB (India); Chakrabarti, P.K., E-mail: pabitra_c@hotmail.com [Solid State Research Lab., Department of Physics, Burdwan University, Burdwan 713104, WB (India)

    2012-12-15

    Nanocrystalline BiFeO{sub 3} and rare earth ion doped BiFeO{sub 3} (Bi{sub 0.9}R{sub 0.1}FeO{sub 3}, R=Er and Tm) were prepared by sol-gel method. Rietveld analysis of the X-ray diffractograms of the samples revealed that small amount of impurity phase of Bi{sub 2}Fe{sub 4}O{sub 9} was formed together with the desired phase. In the thermal variation of magnetic mass susceptibility ({chi}{sub m}) of the samples, one sharp transition below T{sub M} (T{sub M}{approx}100 K, 50 K and 30 K for BiFeO{sub 3}, Bi{sub 0.9}Er{sub 0.1}FeO{sub 3} and Bi{sub 0.9}Tm{sub 0.1}FeO{sub 3}, respectively) was observed, which clearly hint the change of the domination of the ferromagnetic exchange interaction over the usual antiferromagnetic exchange interaction. Also, static magnetization (M) and susceptibility of each doped sample have been drastically enhanced compared to that of BiFeO{sub 3}. The values of {chi}{sub m} and M measured at different temperatures confirmed that the magnetic behavior of the doped systems has been dominated by the paramagnetic/ferromagnetic clusters below {approx}T{sub M}. Another phase transition were observed in the {chi}{sub m} vs. T curve of the samples at relatively higher temperature T{sub B} ({approx}260 K for BiFeO{sub 3}, {approx}220 K for Bi{sub 0.9}Er{sub 0.1}FeO{sub 3} and {approx}180 K for Bi{sub 0.9}Tm{sub 0.1}FeO{sub 3}), which may be attributed to the charge ordering transition. Ferroelectric hysteresis loops of the samples observed at 100 Hz confirmed the presence of ferroelectric ordering of the samples. Measured values of dielectric constants at 1 kHz of each sample in presence and absence of magnetic field confirmed a substantial magnetoelectric coupling of all the samples. - Highlights: Black-Right-Pointing-Pointer Nanocrystalline BiFeO{sub 3} and Er{sup 3+} and Tm{sup 3+} ions doped BiFeO{sub 3} were prepared by sol-gel method. Black-Right-Pointing-Pointer Magnetizations of the doped samples were enhanced. Black

  5. Sol-gel derived nanocrystalline multiferroic BiFeO3 and R3+ (R=Er and Tm) doped therein: Magnetic phase transitions and enhancement of magnetic properties

    Science.gov (United States)

    Acharya, S.; Sutradhar, S.; Mandal, J.; Mukhopadhyay, K.; Deb, A. K.; Chakrabarti, P. K.

    2012-12-01

    Nanocrystalline BiFeO3 and rare earth ion doped BiFeO3 (Bi0.9R0.1FeO3, R=Er and Tm) were prepared by sol-gel method. Rietveld analysis of the X-ray diffractograms of the samples revealed that small amount of impurity phase of Bi2Fe4O9 was formed together with the desired phase. In the thermal variation of magnetic mass susceptibility (χm) of the samples, one sharp transition below TM (TM˜100 K, 50 K and 30 K for BiFeO3, Bi0.9Er0.1FeO3 and Bi0.9Tm0.1FeO3, respectively) was observed, which clearly hint the change of the domination of the ferromagnetic exchange interaction over the usual antiferromagnetic exchange interaction. Also, static magnetization (M) and susceptibility of each doped sample have been drastically enhanced compared to that of BiFeO3. The values of χm and M measured at different temperatures confirmed that the magnetic behavior of the doped systems has been dominated by the paramagnetic/ferromagnetic clusters below ˜TM. Another phase transition were observed in the χm vs. T curve of the samples at relatively higher temperature TB (˜260 K for BiFeO3, ˜220 K for Bi0.9Er0.1FeO3 and ˜180 K for Bi0.9Tm0.1FeO3), which may be attributed to the charge ordering transition. Ferroelectric hysteresis loops of the samples observed at 100 Hz confirmed the presence of ferroelectric ordering of the samples. Measured values of dielectric constants at 1 kHz of each sample in presence and absence of magnetic field confirmed a substantial magnetoelectric coupling of all the samples.

  6. Sol-gel zirconia nanopowders with {alpha}-cyclodextrin as organic additive

    Energy Technology Data Exchange (ETDEWEB)

    Raileanu, M., E-mail: malina_raileanu@yahoo.com [' Ilie Murgulescu' Institute of Physical Chemistry, Roumanian Academy, Splaiul Independentei 202, 060021 Bucharest (Romania); Todan, L., E-mail: ltodan@icf.ro [' Ilie Murgulescu' Institute of Physical Chemistry, Roumanian Academy, Splaiul Independentei 202, 060021 Bucharest (Romania); Crisan, D.; Dragan, N.; Crisan, M.; Stan, C.; Andronescu, C.; Voicescu, M. [' Ilie Murgulescu' Institute of Physical Chemistry, Roumanian Academy, Splaiul Independentei 202, 060021 Bucharest (Romania); Vasile, B.S.; Ianculescu, A. [Department of Oxide Materials Science and Engineering, ' Politehnica' University of Bucharest, 1-7 Gh. Polizu, P.O. Box 12-134, 011061 Bucharest (Romania)

    2012-03-15

    Highlights: Black-Right-Pointing-Pointer The sol-gel synthesis of a zirconia powder has been performed, in the presence of {alpha}-cyclodextrin as organic additive. Black-Right-Pointing-Pointer A crystalline powder consisting from a mixture of monoclinic and tetragonal zirconia phases has resulted after the thermal treatment. Black-Right-Pointing-Pointer The organic additive acted the role of metal oxides used as doppants for zirconia powders, avoiding phase transformations. Black-Right-Pointing-Pointer The {alpha}-cyclodextrin made particles to assume spherical shape and reach fairly uniform size and prevented their agglomeration. Black-Right-Pointing-Pointer The organic additive led to a certain porous morphology of the zirconia particles that is pores embedded within grains. - Abstract: Nanomaterials present unique structural and physicochemical properties due to their ultra fine size of particles that make them very useful in many domains. The most spectacular applications of nanosized zirconia include ceramics, piezoelectrics, refractories, pigments, solid electrolytes, oxygen sensors, catalysts, ultrafiltration membranes, and chromatography packing materials. Nanostructured zirconia powders can be prepared using various methods, such as sol-gel process, coprecipitation, hydrothermal synthesis, and reverse micelle method. The aim of the present work was to prepare zirconia nanopowders through the sol-gel method, using {alpha}-cyclodextrin as organic additive and to establish its influence on the structural and textural properties of the obtained product. A white, amorphous ZrO{sub 2} powder containing {alpha}-cyclodextrin was prepared, which became a crystalline, stable one, after removing the organic matter by thermal treatment. The resulted nanocrystalline powder contains both monoclinic and tetragonal zirconia phases and is very stable. It presents a relatively reduced tendency of agglomeration of particles and contains closed pores which are embedded in

  7. Sol-gel derived nanoparticles of Zn substituted lithium ferrite (Li 0.32Zn 0.36Fe 2.32O 4): magnetic and Mössbauer effect measurements and their theoretical analysis

    Science.gov (United States)

    Sutradhar, S.; Pati, S.; Acharya, S.; Das, S.; Das, D.; Chakrabarti, P. K.

    2012-04-01

    Nanoparticles of Zn substituted lithium ferrite (Li0.32Zn0.36Fe2.32O4) have been prepared by a sol-gel method where the ultra-sonication technique has been adopted to reduce the agglomeration effect among the nanoparticles. The samples were heat-treated at three different temperatures and the formation of the nanocrystalline phase was confirmed by X-ray diffractograms (XRD). The average particle size of each sample has been estimated from the (311) peak of the XRD pattern using the Debye-Scherrer formula and the average sizes are in the range of 10-21 nm. The average particle size, crystallographic phase, etc. of some selected samples obtained from the high-resolution transmission electron microscopy are in agreement with those estimated from the XRD patterns. Static magnetic measurements viz., hysteresis loops, field cooled and zero field cooled magnetization versus temperature curves of some samples carried out by SQUID in the temperature range of 300 to 5 K clearly indicate the presence of superparamagnetic (SPM) relaxation of the nanoparticles in the samples. The maximum magnetization of the SPM sample annealed at 500 °C is quite high (68 Am2/Kg) and the hysteresis loops are almost square shaped with very low value of coercive field at room temperature (827.8 A/m). The particle size, magneto-crystalline anisotropy, etc. have been estimated from the detailed theoretical analysis of the static magnetic data. The dynamic magnetic behavior of the samples was also investigated by observing the ac hysteresis loops and magnetization versus field curves with different time windows at room temperatures. The different soft magnetic quantities viz., coercive field, magnetization, remanance, hysteresis losses, etc. were extracted from dynamic measurements. Dynamic measurements confirmed that the samples are in their mixed state of SPM and ordered ferrimagnetic particles, which is in good agreement with the results of static magnetic measurements. Mössbauer spectra of the

  8. New Hybrid Materials Synthesized with Different Dyes by Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Ramona Gheonea

    2017-01-01

    Full Text Available One well-known method for hybrids synthesis with incorporated organic dyes is sol-gel method, which is based on the concept of molecular manipulation to design ceramics, glasses, and composites. The low-temperature process allows for the incorporation of guest organic molecules within the inorganic matrix, as well as for the synthesis of hybrid networks in which the organic and inorganic phases are interpenetrating. The aim of the work presented in this paper was the preparation of the gels with three different dyes, at different molar ratios by using the hydrolytic sol-gel process. The interaction of the dye and the oxide was examined by UV-vis spectroscopy and FT-IR. The thermal stability of the hybrid organic-inorganic xerogel formed here was studied by thermal analysis. The micrographs obtained by scanning electron microscopy (SEM revealed the high density of the films. Such characteristics indicate the possible application of these films in solar cells.

  9. Sol-Gel Synthesis of Ceria-Based Electrolytes and Perovskite-Type Cathodes

    Energy Technology Data Exchange (ETDEWEB)

    Pinol, S.; Calleja, A.; Capdevila, X. G.; Najib, M.; Espiell, F.

    2002-06-01

    We have successfully prepared electrolytes of Ce{sub 0.8}Sm{sub 0.2}O{sub 1.9} (SDC) and Ce{sub 0.8}Sm{sub 0.2}O{sub 1.9} (GDC) and cathodes of La{sub 1-x}Sr{sub x}CoO{sub 3} (LSCO) and La{sub 1-x}Sr{sub x}MnO{sub 3} (LSMO), useful for SOFCs, by the acrylamide sol-gel method. This method consists in the preparation of a solution from the elemental oxides and carbonates followed by a gellification with acrylamide monomer. Then, the combustion of the organic molecules is initiated, obtaining ultra fine calcined powders of the above-mentioned compounds. In this way, we have obtained high purity powders of SDC, GDC, LSCO and LSMO as confirmed by X-ray diffraction powder analysis. On the other hand, we have also studied the preparation of the same products by the solid-state reaction technique for comparison purposes. However, it was not possible to obtain pure LSCO by this ceramic method. We have observed that the optimal synthesis temperature is lower for the sol-gel samples and the final purity of the products is higher. (author)

  10. Refractive and diffractive micro-optical elements and arrays prepared by the fast sol-gel processes

    Science.gov (United States)

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

    1997-09-01

    The optical quality of films and bulk elements obtained by the fast sol-gel method and the ease of preparation make this method technologically and economically attractive for micro- optical elements and arrays. Multiple replication of high-cost metal templates necessitates a two step process: initial replication onto disposable plastic, to produce negative- templates, and casting of the glass elements onto these plastic templates. Following introduction of the fast sol-gel micro-replication processes, the fabrication of refractive and diffractive micro-optical arrays is described in detail. The study focuses of the accuracy achievable by the replication of sharp curvatures by a viscous sol-gel resins. A further question addressed is how to obtain a thick crack-free self- supporting micro-optical array by such a process. Examples of replication results of Fresnel lenses and various types of lenslet arrays by this method are shown, and the various aspects of replication accuracy are discussed. The characterization of the thus produced micro-optical arrays is described, relating to the influence of mold and resin parameters on residual stresses and thence, the surface and bulk properties of the replicas. Various approaches to stress- minimization that can facilitate accurate replication in sol- gel derived matrices are discussed. Further, the preparative approach to highly patterned crack-free self-supporting thick elements is displayed, and the wide scope of new applications stemming from such elements is discussed. Finally, the new chemical approach to crack-free stress-free silica glasses by the sol-gel method is displayed.

  11. Luminescent hybrid porphyrinosilica obtained by sol gel chemistry

    Directory of Open Access Journals (Sweden)

    Neri Cláudio Roberto

    2003-01-01

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

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

    Science.gov (United States)

    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.

  13. Covalent immobilization of carbohydrates on sol-gel-coated microplates.

    Science.gov (United States)

    Zou, Lan; Pang, Hei-Leung; Chan, Pak-Ho; Huang, Zhi-Shu; Gu, Lian-Quan; Wong, Kwok-Yin

    2008-09-01

    Carbohydrate microarrays have attracted increasing attention in recent years because of their ability to monitor biologically important protein-carbohydrate interactions in a high-throughput manner. Here we have developed an effective approach to immobilizing intact carbohydrates directly on polystyrene microtiter plates coated with amine-functionalized sol-gel monolayers. Lectin binding was monitored by fluorescence spectroscopy using these covalent arrays of carbohydrates that contained six mono- and di-saccharides on the microplates. In addition, binding affinities of lectin to carbohydrates were also quantitatively analyzed by determining IC(50) values of lectin-specific antibody with these arrays. Our results indicate that microplate-based carbohydrate arrays can be efficiently fabricated by covalent immobilization of intact carbohydrates on sol-gel-coated microplates. The microplate-based carbohydrate arrays can be applied for screening of protein-carbohydrate interactions in a high-throughput manner.

  14. Sol-Gel Thin Films for Plasmonic Gas Sensors

    Directory of Open Access Journals (Sweden)

    Enrico Della Gaspera

    2015-07-01

    Full Text Available 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.

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

    Science.gov (United States)

    Zheng, Kai; Boccaccini, Aldo R

    2017-03-21

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

  16. Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

    Directory of Open Access Journals (Sweden)

    Jolanta Gąsiorek

    2018-01-01

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

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

    Science.gov (United States)

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

    2018-01-26

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

  18. Cracks in nano-ceramic thin layers produced by laser treatments

    NARCIS (Netherlands)

    De Hosson, JTM; Teeuw, DHJ; Beltz, GE; Selinger, RLB; Kim, KS; Marder, MP

    1999-01-01

    Sol-gel derived thin nano-ceramic layers of TiO2 and Al2O3 are studied using scanning electron microscopy to reveal the microstructure and morphologies of the layers. The low-voltage scanning electron microscope with a field emission gun is equipped with an especially designed lens, where the

  19. Kinetics of the electrochemically-assisted deposition of sol-gel films.

    Science.gov (United States)

    Liu, Liang; Walcarius, Alain

    2017-06-14

    Electrochemically-assisted deposition is now becoming a widespread method for preparing sol-gel films. It is based on the electrochemical generation of OH - ions, which can then catalyze the sol-gel condensation reactions. It has a key advantage of selectively facilitating the film deposition on electrochemically active surfaces while not affecting the stability of the bulk precursor solution. Experimental studies have clearly shown that the thickness of the electrochemically-assisted deposited films is influenced by the deposition parameters such as the potential and time. However, there is still a lack of quantitative description of the kinetics of film growth due to the complexity of the process. In this preliminary study, we derived quantitative analytical expressions for describing the kinetics associated with the growth of sol-gel films generated by electrochemically assisted deposition. Both heterogeneous and homogeneous condensation reactions were considered. The key strategy was to simplify the process by separating the electrochemical step of generating OH - ions with the condensation steps of film formation under approximation. Furthermore, numerical simulation was carried out to examine the validity and any errors in the analytical expressions in the cases when the required approximations were not fulfilled. The analytical expressions could well explain the trends observed in the experimental studies and could also be used for fitting the experimental results from the literature. This study provides a deeper understanding of the mechanism and quantitative guidance for manipulating electrochemically-assisted deposition processes at a large scale in industry. It may also be referred to in regard to other indirect electrodeposition systems in which the deposition is not an electrochemical step but is instead driven by electrochemically-generated catalysts.

  20. Sol-Gel Synthesis and Characterization of Selected Transition Metal Nano-Ferrites

    Directory of Open Access Journals (Sweden)

    Aurelija GATELYTĖ

    2011-09-01

    Full Text Available In the present work, the sinterability and formation of nanosized yttrium iron garnet (Y3Fe5O12, yttrium perovskite ferrite (YFeO3, cobalt, nickel and zinc iron spinel (CoFe2O4, NiFe2O4 and ZnFe2O4, respectively powders by an aqueous sol-gel processes are investigated. The metal ions, generated by dissolving starting materials of transition metals in the diluted acetic acid were complexed by 1,2-ethanediol to obtain the precursors for the transition metal ferrite ceramics. The phase purity of synthesized nano-compounds was characterized by infrared spectroscopy (IR and powder X-ray diffraction analysis (XRD. The microstructural evolution and morphological features of obtained transition metal ferrites were studied by scanning electron microscopy (SEM.http://dx.doi.org/10.5755/j01.ms.17.3.598

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

    Directory of Open Access Journals (Sweden)

    E. P. Avés

    2008-12-01

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

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

    Science.gov (United States)

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

    2014-07-01

    More than four decades after the discovery of 45S5 Bioglass® as the first bioactive material, this composition is still one of the most promising materials in the tissue engineering field. Sol-gel-derived bioactive glasses generally possess improved properties over other bioactive glasses, because of their highly porous microstructure and unique surface chemistry which accelerate hydroxyapatite formation. In the current study, a new combination of precursors with lactic acid as the hydrolysis catalyst have been employed to design an organic, nitrate-free sol-gel procedure for synthesizing of 45S5 Bioglass®. This straightforward route is able to produce fully amorphous submicron particles of this glass with an appropriately high specific surface area on the order of ten times higher than that of the melt-derived glasses. These characteristics are expected to lead to rapid hydroxyapatite formation and consequently more efficient bone bonding. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    McLean, Michael M.

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

  4. Investigation of high temperature sol-gel coatings

    Energy Technology Data Exchange (ETDEWEB)

    Montgomery, M. [DTU Mekanik, Kgs. Lyngby (Denmark); Vilhelmsen, T. [Vattenfall Heat Nordic, Copenhagen (Denmark); Bennedsen, J. [Teknologisk Institut, Aarhus (Denmark)

    2008-03-15

    The Danish Technological Institute (DTI) has developed a technique using Hybrid Sol-gel nanotechnology to produce coatings which can change the surface characteristics of various components. It is the purpose of this project to investigate where such coatings can be utilised in the power generating industry with respect to fouling and corrosion resistance. Sol-gel coatings were fabricated at DTI with the aim of being high temperature corrosion resistance. These coatings were investigated at DTU Mechanical Engineering. The coatings contained large amounts of aluminium, oxygen, silicon and titanium with also addition of mica. Tubes of various alloys (15Mo3, X20CrMoV121, TP347H and P91,) were received from DONG Energy/Vattenfall. They were mechanically cleaned and then 15Mo3, X20CrMoV121 and TP347H were cleaned in a 10% melamine solution for 30 minutes. All tubes were then polished and coated. Two different sol-gel coatings have been applied to each end of the tube. The one coating is white ({Psi}114) and the other black ({Psi}115). The specimens were heated for 3 thermal cycle periods of 8 hours. From the analysis of the various coatings, it is clear that the coatings exposed to thermal cycles of 500 deg. C have all oxides present below the sol-gel layer. In many cases especially for the grey coating, the coating has spalled. Thus these coatings do not prevent permeation of oxidising species either due to a permable coating or cracking of the coating due to thermal cycling. For the coating on the 15Mo3 tube, there was almost no oxide, however microscopy of the surface of the specimens revealed cracking. It is suggested that lack of oxide or very thin oxide on the 15Mo3 is due to the fact that oxidation is not so fast at 400 deg. C compared to 500 deg. C, and that a longer exposure time would have given a thicker oxide. It would be difficult to understand why 15Mo3 behaves differently to the under ferritic steels when it has a lower corrosion resistance and similar

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

    Directory of Open Access Journals (Sweden)

    Peón, E.

    2005-12-01

    Full Text Available Hydroxyapatite coatings (HAp have been obtained starting from precursors of sol-gel type. The coatings previously oxidized were deposited on metal surfaces of a based on iron alloy so-called MA956. The alloys were at high temperatures, in order to improve the adhesion with the hydroxyapatite coatings. The sol-gel coating was obtained applying an aqueous route, using triethyl phosphite and aqueous calcium nitrate, as precursors of phosphorous and calcium, respectively. Different sintering thermal treatments were applied on the resulting gels in order to obtain a homogeneous, adherent and crystalline hydroxyapatite coating. The characterization techniques used for this study were optical microscopy, SEM/EDX, XDR and FTIR. Moreover, the adhesion between the hydroxylapatite coating and the substrate was assessed according to the ASTM D 3359-02 standard test method. The results of this study showed that the best thermal treatment is obtained for a sintering temperature of 550 °C during a time of 72 h.

    Se han preparado nuevos recubrimientos de hidroxiapatita (HAp obtenidos a partir de precursores de tipo sol-gel, depositados sobre sustratos metálicos de una aleación de base hierro denominada MA956, previamente oxidados a elevadas temperaturas, para mejorar la adherencia con los recubrimientos de hidroxiapatita. El recubrimiento sol-gel se obtuvo aplicando una ruta acuosa, utilizando como precursores del fósforo y del calcio trietilfosfito y nitrato cálcico tetrahidratado, respectivamente. Sobre los geles resultantes se aplicaron distintos tratamientos térmicos de sinterización, hasta la obtención de recubrimientos de hidroxiapatita homogéneos, adherentes y cristalinos. Las técnicas de caracterización utilizadas para realizar este estudio han sido microscopía óptica, MBE/EDX, DRX y FTIR. Así mismo, se ha determinado la adherencia entre el substrato y el recubrimiento de hidroxiapatita según la norma ASTM D 3359-02. Los resultados

  6. The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

    Directory of Open Access Journals (Sweden)

    Ales Styskalik

    2017-05-01

    Full Text Available This review is devoted to non-hydrolytic sol-gel chemistry. During the last 25 years, non-hydrolytic sol-gel (NHSG techniques were found to be attractive and versatile methods for the preparation of oxide materials. Compared to conventional hydrolytic approaches, the NHSG route allows reaction control at the atomic scale resulting in homogeneous and well defined products. Due to these features and the ability to design specific materials, the products of NHSG reactions have been used in many fields of application. The aim of this review is to present an overview of NHSG research in recent years with an emphasis on the syntheses of mixed oxides, silicates and phosphates. The first part of the review highlights well known condensation reactions with some deeper insights into their mechanism and also presents novel condensation reactions established in NHSG chemistry in recent years. In the second section we discuss porosity control and novel compositions of selected materials. In the last part, the applications of NHSG derived materials as heterogeneous catalysts and supports, luminescent materials and electrode materials in Li-ion batteries are described.

  7. Giant phase transition properties at terahertz range in VO₂ films deposited by sol-gel method.

    Science.gov (United States)

    Shi, Qiwu; Huang, Wanxia; Zhang, Yaxin; Yan, Jiazhen; Zhang, Yubo; Mao, Mao; Zhang, Yang; Tu, Mingjing

    2011-09-01

    VO(2) films were fabricated on high-purity single-crystalline silicon substrate by the sol-gel method, followed by rapid annealing. The composition and microstructure of the films were investigated by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and atomic force microscopy (AFM). The results indicated a polycrystalline nature with high crystallinity and compact nanostructure for the films, and the concentration of +4 valence vanadium is 79.85%. Correlated with these, a giant transmission modulation ratio about 81% of the film was observed by terahertz time domain spectroscopy. The experimentally observed transmission characteristics were reproduced approximately, by a simulation at different conductivities across the phase transition. According to the effective-medium theory, we assumed that it is important to increase the concentration of +4 valence vanadium oxide phases and improve the compactness of the VO(2) films for giant phase transition properties. The sol-gel-derived VO(2) films with giant phase transition properties at terahertz range, and the study on their composition and microstructure, provide considerable insight into the fabrication of VO(2) films for the application in THz modulation devices.

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

    Directory of Open Access Journals (Sweden)

    Czekaj D.

    2017-06-01

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

  9. Characterization and Modification of Mesoporous Silica Nanoparticles Prepared by Sol-Gel

    Directory of Open Access Journals (Sweden)

    Meysam Keshavarz

    2013-01-01

    Full Text Available Mesoporous silica nanoparticles (MSNs were synthesized by sol-gel reaction at normal pressure by using TEOS as a silica source and CTAB as a directing agent in ammonia solution at 323 K subsequently calcined at 823 K. Then inorganic pores were modified with metal-supported MSN with attention to the acidity, surface area, pore size, and ability of ion exchange. Crystalline size was shown to decrease up to 20 molar ratios of Si/Al followed by increasing while further adding nanoparticles-aluminium. Moreover, the XRD patterns revealed the mesostructured material for all with 2D hexagonal structure. The obtained results from the XRD patterns were confirmed by using BET and EDX. The BET surface areas revealed the spherical shape for all samples with a decrease in the pore volume and surface area for various AlMSNs which emphasized that the loading of Al and was compatible with XRD results. MSN was prepared by sol-gel methods followed by loading of Al in order to prepare AlMSN which possess strong Lewis acidic sites. This modification occurred by using various molar ratios of 0, 5, 10, 20, 50, and 100 Si/Al, respectively. The XRD patterns of various ratios of Si/Al were interpreted in terms of strain, nanocrystalline size, and distribution of the particle size by deriving Wiliamson Hall equation.

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

    Directory of Open Access Journals (Sweden)

    Dawit G. Ayana

    2016-11-01

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

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-27

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

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

    Science.gov (United States)

    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

  14. Surface chemistry and moisture sorption properties of wood coated with multifunctional alkoxysilanes by sol-gel process

    DEFF Research Database (Denmark)

    Tshabalala, M.A.; Kingshott, P.; VanLandingham, M.R.

    2003-01-01

    Sol-gel surface deposition of a hydrophobic polysiloxane coating on wood was accomplished by using a mixture of a low molecular weight multifunctional alkoxysilane, methyltrimethoxysilane (MTMOS), and a high molecular weight multifunctional alkoxysilane, hexadecyltrimethoxysilane (HDTMOS). Invest......Sol-gel surface deposition of a hydrophobic polysiloxane coating on wood was accomplished by using a mixture of a low molecular weight multifunctional alkoxysilane, methyltrimethoxysilane (MTMOS), and a high molecular weight multifunctional alkoxysilane, hexadecyltrimethoxysilane (HDTMOS......). Investigation of the surface chemistry and morphology of the wood specimens by means of ATR-FTIR, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, SEM, and atomic force microscopy indicated that the sol-gel process results in deposition of polysiloxane networks that are bonded to the wood...... penetrated the outer surface layers of the wood and condensed with hydroxyls that may not be readily accessible to the high molecular weight HDTMOS. Once attached to such sites, it is reasonable to assume that some of these surface derivatives of MTMOS condensed with other molecules of MTMOS and HDTMOS...

  15. Third-order nonlinear optical properties of metal dithiolene- and phthalocyanine-doped sol-gel materials

    Science.gov (United States)

    Gall, Gavin J.; King, Terence A.; Oliver, Stephen N.; Capozzi, Carol A.; Seddon, Angela B.; Hill, Callum A. S.; Underhill, Allan E.

    1994-10-01

    Recent studies on metal dithiolene complexes in solution and PMMA have shown this range of materials to exhibit high third-order nonlinear optical coefficients, (Chi) 3, and excellent figures of merit. Phthalocyanine dyes have been shown to exhibit optical limiting due to the nonlinear effect of reverse saturable absorption. We report here on the third-order nonlinear optical characterization of several metal dithiolene and phthalocyanine compounds doped in sol-gel derived materials. These hosts provide a physically and chemically stable environment for the nonlinear compounds, and offer the potential of high levels of doping. The dithiolene and phthalocyanine compounds were incorporated into partially densified sol-gel silica glass (xerogels) by the post-doping technique, and into the hybrid organic-inorganic materials at the sol-stage. To obtain optical quality surfaces on the porous xerogel, a unique polishing technique has been developed. Picosecond and nanosecond pulsed laser studies of nonlinear refraction and absorption are presented, together with laser damage and micro-hardness measurements. For the dithiolenes, concentrations of the order of 1018 molecules/cm3 for both the hybrid material and the xerogel were studied using the degenerate four wave mixing (DFWM) technique. (Chi) 3 values up to 1.4 X 10-19 m2/V2 (equivalent to 1.0 X 10-11 esu) were observed in the sol-gel host.

  16. Analysis of the thermoluminescent signal in the hydroxyapatite synthesized by the sol-gel method; Analisis de la senal termoluminiscente en la hidroxiapatita sintetizada por el metodo sol gel

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza A, D.; Gonzalez, P.R. [ININ, A.P. 18-1027, 11801 Mexico D.F. (Mexico); Lobato, M.; Rubio, E.; Rodriguez L, V. [Fac. de Ingenieria Quimica, BUAP, Av. San Claudio y 18 Sur, Col. San Manuel, 72570 Puebla (Mexico); Custodio, E. [Universidad Juarez Autonoma de Tabasco, DACB, Carr. Cunduacan-Jalpa Km. 1.5, 86680 Tabasco (Mexico)

    2004-07-01

    The physical properties of the ceramics are related with the chemical bonds and the crystalline structure, because the elements that constitute it can be united by ionic bonds or partially ionic giving a covalent character, this last causes that the outer layer is full of electrons. This property makes that the ceramic ones become interesting materials for thermoluminescent applications, as it demonstrates through the recent works presented on the hydroxyapatite that is a ceramic biomaterials that has shown an interesting thermoluminescent signal when being exposed to gamma radiation. In this sense, this work presents the thermoluminescent signal analysis induced by the UV and gamma radiation in a particular type of hydroxyapatite synthesized by sol gel method in which the temperature synthesis is varied. The final thermoluminescent sensitivity of materials is correlated with the crystalline degree, which is analysed through X-ray diffraction. (Author)

  17. Evaluation of Hydroxyapatite-Forsterite Glass Composite Nanopowder Prepared via Sol-Gel Method

    Science.gov (United States)

    Mazrooei Sebdani, Maryam; Fathi, Mohammadhossein

    In spite of attractive bioactivity of bioactive ceramics i.e. hydroxyapatite and bioactive glasses, their poor mechanical properties have restricted their clinical applications. To overcome these limitations, an alternative approach suggested is preparation a composite including these bioactive ceramics with others. It is expected that a ceramic reinforcement with reduced grain size below 100 nm promotes theirs. The aim of this work was fabrication and characterization of hydroxyapatite-forsterite-bioglass composite nanopowder. Novel hydroxyapatite-forsterite-bioglass composite nanopowder was synthesized by incorporation of the forsterite and bioactive glass in hydroxyapatite matrix via a sol-gel process. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fourier transform infrared (FTIR) spectroscopy techniques were utilized in order to evaluate the phase composition, agglomerates size distribution, morphology and particle size and functional groups of synthesized. The effects of sintering temperature and time were also investigated. Results showed that the appropriate temperature for calcination was 600°C and the particle size of composite nanopowder was about 60-70nm. The decomposition of hydroxyapatite was increased with the increase of the sintering temperature and sintering time. Obtained results indicate that prepared composite nanopowder could be a good candidate for medical applications.

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

    Indian Academy of Sciences (India)

    A combined sol-gel-cum-hydrothermal method has been employed to synthesize novel monometal- lic (Mn, Fe, Co) and bimetallic (Co-Fe, .... Mesoporous Al2O3 was synthesized by sol-gel method. Cetyltrimethylammonium bromide ... TEOS silica source was added to the mixture and stirred for. 2 h (solution A) to obtain ...

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

    Science.gov (United States)

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

    2014-08-01

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

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

    Science.gov (United States)

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

    2010-01-01

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

  1. Routes to extrinsic and intrinsic self-healing corrosion protective sol-gel coatings: a review

    Science.gov (United States)

    Abdolah Zadeh, M.; van der Zwaag, S.; Garcia, S. J.

    2013-06-01

    Sol-gel pre-treatments and coatings are an important class of passive protective coatings, which can effectively prevent corrosion of various metallic substrates through adhesion improvement and barrier protection. Recently, sol-gel chemistry has been proposed as an appropriate method for implementation of self-healing functionality in coatings via extrinsic concepts. In this review we will analyze the most relevant existing works on self-healing sol-gel coatings, including new work done in the direction of implementing intrinsic healing capabilities to sol-gels. The development of active sol-gel coatings is due to the broad chemical versatility of precursors and low processing temperature of this type of chemistry.

  2. Sol-gel transition of organogels observed by terahertz spectroscopy

    Science.gov (United States)

    Hoshina, Hiromichi; Ozaki, Atsumi; Itagaki, Yusuke; Yajima, Setsuko; Suzuki, Hal; Ishii, Shinya; Ishida, Misaki; Uchiyama, Tetsuji; Kimura, Keiichi; Otani, Chiko

    2014-07-01

    Terahertz (THz) absorption spectra of organogels consisting of (1R,2R)-1,2-bis(dodecanoylamino)cyclohexane/2-nitrophenyl octyl ether (RR-BDC/NPOE) and RR-BDC/n-dodecane were measured by Fourier-transform far-infrared (FT-FIR) spectroscopy. The vibrational peaks of the gels were observed at the same frequencies as those of the pure gelator, suggesting that the intermolecular structure around the Nsbnd H⋯Odbnd C hydrogen bond is maintained in the gel phase. Temperature-dependent spectroscopy showed a drastic spectral change at the sol-gel transition temperature, in which the vibrational peak at 3.5 THz disappears and a new peak appears at 2.9 THz. The change in THz vibrational frequency is indicative of the structural collapse of the hydrogen-bonded fibrous architecture in the sol phase.

  3. Mayenite Synthesized Using the Citrate Sol-Gel Method

    Energy Technology Data Exchange (ETDEWEB)

    Ude, Sabina N [ORNL; Rawn, Claudia J [ORNL; Meisner, Roberta A [University of Tennessee (UTK) and Oak Ridge National Laboratory (ORNL); Kirkham, Melanie J [ORNL; Jones, Gregory L. [University of Tennessee, Knoxville (UTK); Payzant, E Andrew [ORNL

    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.

  4. Synthesis, functionalisation and characterisation of mesoporous materials and sol-gel glasses for applications in catalysis, adsorption and photonics.

    Science.gov (United States)

    Øye, Gisle; Glomm, Wilhelm R; Vrålstad, Torbjørn; Volden, Sondre; Magnusson, Heléne; Stöcker, Michael; Sjöblom, Johan

    2006-11-16

    In this review, synthesis and functionalisation approaches for ordered mesoporous materials and sol-gel glasses are described. Catalytic and adsorption applications are emphasised for the ordered mesoporous materials, while optical applications are the focus for sol-gel glasses.

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

    Science.gov (United States)

    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. Copyright © 2013 Elsevier Inc. All rights reserved.

  6. Low temperature synthesis of magnesium oxide and spinel powders by a sol-gel process

    Directory of Open Access Journals (Sweden)

    Li-Zhai Pei

    2010-09-01

    Full Text Available Magnesium oxide and magnesium aluminate (MgAl2O4 spinel (MAS powders have been synthesized by a simple aqueous sol-gel process using citrate polymeric precursors derived from magnesium chloride, aluminium nitrate and citrate. The thermal decomposition of the precursors and subsequent formation of cubic MgO and MAS were investigated by X-ray diffraction (XRD, scanning electron microscopy (SEM, thermogravimetry-differential scanning calorimetry (TG-DSC and Fourier transform infrared spectra (FTIR. The single phase cubic MgO powder and MAS powder form after heat treatment at 800 and 1200 °C, respectively. The particle size of the MgO and MAS powders is about 100 nm and several micrometers, respectively. Ball milling eliminates the size of MgO and MgAl2O4 spinel powders by decreasing the conglomeration of the powders.

  7. Synthesis of Helical Phenolic Resin Bundles through a Sol-Gel Transcription Method

    Directory of Open Access Journals (Sweden)

    Changzhen Shao

    2017-02-01

    Full Text Available Chiral and helical polymers possess special helical structures and optical property, and may find applications in chiral catalysis and optical devices. This work presents the preparation and formation process of helical phenolic resins through a sol-gel transcription method. A pair of bola-type chiral low-molecular-weight gelators (LMWGs derived from valine are used as templates, while 2,4-dihydroxybenzoic acid and formaldehyde are used as precursors. The electron microscopy images show that the phenolic resins are single-handed helical bundles comprised of helical ultrafine nanofibers. The diffused reflection circular dichroism spectra indicate that the helical phenolic resins exhibit optical activity. A possible formation mechanism is proposed, which shows the co-assembly of the LMWGs and the precursors.

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

    Science.gov (United States)

    Barhoum, Moussa

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

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

    Science.gov (United States)

    1989-09-10

    Far. Soc. 61, 962, 975, (1965); 65, 1741 (1969). 11. L. Gengembre, A Chaperton, B. Vandorpe, C. R. Acad. Sc. Paris, Serie C, 284, 541 (1977); J. Chimie ...temperatures as low as 500°C 1]. However, when the Na20 content was more than 20 molZ the gel-derived glass had very poor durability and little usefulness...the preparation, properties and durability of largeI monolithic Na20-SiO2 gels. This is especially so for chemically durable gels in which the Na2O

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

    Science.gov (United States)

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

    2017-03-01

    Synthesis of tetragonal ZrO2 by both conventional sol-gel and ultrasound-assisted sol-gel methods and using a non-ionic surfactant Tween-20, was performed. A porous microstructure composed of nanometric particles was observed. Tetragonal ZrO2 was obtained using a low heat treatment temperature of powders, 500°C by both methods. A higher crystallinity and a shorter reaction time were observed when ultrasound was used in the sol-gel method due to the cavitation phenomenon. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Monitoring of the Viability of Cells Immobilized by Sol-Gel Process

    Czech Academy of Sciences Publication Activity Database

    Kuncová, Gabriela; Podrazký, Ondřej; Ripp, S.; Trögl, Josef; Sayler, G. S.; Demnerová, K.; Vaňková, Radomíra

    2004-01-01

    Roč. 31, 1-3 (2004), s. 335-342 ISSN 0928-0707. [International Workshop on Sol-Gel and Technology-Part I (Sol-Gel'03) /12./. Sydney, 25.08.2003-29.08.2003] R&D Projects: GA ČR GA104/01/0461; GA MŠk OC 840.20; GA MŠk OC 840.10 Institutional research plan: CEZ:AV0Z4072921 Keywords : sol-gel process * cell entrapment * viability Subject RIV: CE - Biochemistry Impact factor: 1.150, year: 2004

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

    Directory of Open Access Journals (Sweden)

    R.F.S. Lenza

    2001-07-01

    Full Text Available In this work we obtained microporous and mesoporous silica gels by sol-gel processing. Tetraethylortosilicate (TEOS was used as precursor. Nitric acid and hydrofluoric acid were used as catalysts. In order to study the affect of formamide as drying additive, we used a molar ratio alkoxide/formamide of 1/1. The performance of formamide in obtaining crack-free gels was evaluated through monolithicity measurements. The structural evolution occurring in the interconnected network of the gels during thermal treatment was monitored by Fourier transform infrared spectroscopy (FTIR, shrinkage and density measurements and nitrogen gas sorption. We noted that in the presence of formamide, the Si-O-Si bonds are stronger and belong to a more cross-linked structure. The samples obtained in the presence of formamide have larger pore volume and its pore structure is in the range of mesoporosity. The samples obtained without additive are microporous. Formamide allowed the preparation of crack-free silica gels stabilized at high temperatures.

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

    Directory of Open Access Journals (Sweden)

    Rubia F. S. Lenza

    2002-10-01

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

  14. Sol-Gel Synthesis and Characterization of Nanoparticles

    Directory of Open Access Journals (Sweden)

    S. Ramesh

    2013-01-01

    Full Text Available The nanoparticles have been synthesized by sol-gel technique. X-ray diffraction, scanning electron microscopy, optical absorption spectroscopy, and electron paramagnetic resonance spectroscopy were used to characterize the sample. The X-ray diffraction results indicate the formation of nanocrystalline materials in tetragonal lattice with P42/nnm space group. The identical distribution of elements were confirmed by scanning electron microscopy with energy dispersive X-ray spectrometry and X-ray mapping. Electron paramagnetic resonance lineshapes of the samples are obtained at various (13 K, 77 K, and 300 K temperatures. The isotropic lineshapes of the sample B1 are attributed to dipole-dipole interaction of Ti3+ ions. The incorporation of Al3+ ions into the sample B2–B5 the isotropic nature of the lineshapes are collapsed due to the distraction in crystal field. Optical absorption spectra results reveal the presence of Ag-TiO2 nanoparticles.

  15. Synthesis of Carbon Nanotubes Using Sol Gel Route

    Science.gov (United States)

    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.

  16. /dopamine films prepared by sol-gel method

    Science.gov (United States)

    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.

  17. Infrared Spectroscopy Studies on sol-gel prepared alumina Powders

    Directory of Open Access Journals (Sweden)

    Majid JAFAR TAFRESHI

    2015-03-01

    Full Text Available Gamma-alumina fine particles were synthesized by sol-gel process. Aluminum tri-sec-butoxide (ATB, anhydrous ethyl alcohol (EtOH, water (H2O and hydrochloric acid (HCl were used as starting materials. Different samples were synthesized with EtOH/ATB=60/1, HCl/ATB=0.08/1 and H2O/ATB=1/1 ratios and calcined at different temperatures. Molar ratios of H2O/ATB (from 1 to 25 and HCl/ATB (from 0.08 to 0.4 were changed for some other samples, during synthesizing process. The products were characterized by both XRD and FTIR measurements. Studies were carried out on the effect of calcination temperature and change of H2O/ATB and HCl/ATB ratios on structure and processes involved in phase transformations.DOI: http://dx.doi.org/10.5755/j01.ms.21.1.4872

  18. Characterization of carbon cryogels synthesized by sol-gel polycondensation

    Directory of Open Access Journals (Sweden)

    BILJANA BABIC

    2005-02-01

    Full Text Available Resorcinol-formaldehyde (RF cryogels were synthesized by the sol-gel polycondensation of resorcinol (R with formaldehyde (F and freeze-drying was carried out with t-butanol. Carbon cryogels were obtained by pyrolyzing RF cryogels in an inert atmosphere. Characterization by nitrogen adsorption showed that the carbon cryogels were micro and mesoporous materials with high specific surface areas (SBET ~ 550 m2/g. Cyclic voltammetry experiments at various scan rates (2 to 200 mV s-1 were performed to study the electrical double-layer charging of carbon cryogel electrodes in 0.5 mol dm-3 HClO4 solution. It has been demonstrated that it is possible to sub-divide the total specific capacitance into the mesoporous and the microporous specific capacitance by analyzing the linear dependence of the charge (q on the reciprocal of the square root of the potential scan rate (v-1/2, and the linear dependence of the reciprocal charge (1/q on the square root of the potential scan rate (v-1/2. The specific capacitance was found to be constant over a wide range of sample weight (12.5 to 50.0 mg and a very promising specific capacitance value of 150 F/g, was found for this material operating in an acidic 0.5 mol dm-3 HClO4 solution at room temperature.

  19. Sol gel growth of titania from electrospun polyacrylonitrile nanofibres

    Science.gov (United States)

    Hong, Youliang; Li, Domgmei; Zheng, Jian; Zou, Guangtian

    2006-04-01

    In this paper we report on the development of TiO2 surface-residing electrospun nanofibres with controllable density of TiO2 on the support fibre surface by means of an electrospinning technique and a sol-gel process. The TiO2 precursor/PAN composite nanofibres were synthesized by electrospinning a polyacrylonitrile (PAN) solution containing TiO2 precursors. Subsequently, an immersion of the electrospun composite nanofibres in deionized water led to the hydrolysis of the TiO2 precursors. SEM, TEM and XRD pattern analyses demonstrated that TiO2 was formed and resided on the nanofibre surface. On further calcining the hydrolysed nanofibres in air at 300 °C, TiO2 could be conveniently converted into anatase without essentially changing the morphology of the hydrolysed nanofibres. Furthermore, surface photovoltage spectroscopy (SPS) confirmed that the TiO2 surface-residing nanofibre nonwovens had a strong SPS response. It can be attributed that the surface residence of TiO2 permits the transfer of the photogenerated electron originating from TiO2 to ITO electrodes. Potential applications of the TiO2 surface-residing nanofibres include filters, catalysis films and environmental pollution remediation films.

  20. Sol-Gel Titanium Dioxide Nanoparticles: Preparation and Structural Characterization

    Directory of Open Access Journals (Sweden)

    Oon Lee Kang

    2016-01-01

    Full Text Available Titanium dioxide (TiO2 nanoparticle was achieved in an alternative sol-gel route, as involved in 1 M acidic solution: HCl-tetrahydrofuran (HCl-THF, HNO3-tetrahydrofuran (HNO3-THF, and ClHNO2-tetrahydrofuran (ClHNO2-THF solution. Resultant TiO2 nanoparticle was further investigated in a systematic analytical approach. Nanoscale TiO2 structure was observed at a moderate hydrolysis ratio (8≤RH≤16. Particle size range was much narrower in an aprotic HNO3-THF medium, as compared to a differential HCl-THF medium. Biphasic TiO2 structure was detected at a certain hydrolysis ratio (RH≥16. Even so, relative anatase content was rather insignificant in an aprotic HCl-THF medium, as compared to a differential HNO3-THF medium. Tetragonal TiO2 structure was observed in the entire hydrolysis ratio (4≤RH≤32. Interstitial lattice defect was evident in an aprotic HNO3-THF medium but absent in a differential ClHNO2-THF medium.

  1. Silsesquioxane-derived ceramic fibres

    Science.gov (United States)

    Hurwitz, F. I.; Farmer, S. C.; Terepka, F. M.; Leonhardt, T. A.

    1991-01-01

    Fibers formed from blends of silsesquioxane polymers were characterized to study the pyrolytic conversion of these precursors to ceramics. The morphology of fibers pyrolyzed to 1400 C revealed primarily amorphous glasses whose conversion to beta-SiC is a function of both blend composition and pyrolysis conditions. Formation of beta-SiC crystallites within the glassy phase is favored by higher than stoichiometric C/Si ratios, while carbothermal reduction of Si-O bonds to form SiC with loss of SiO and CO occurs at higher methyl/phenylpropyl silsesquioxane (lower C/Si) ratios. As the carbothermal reduction is assumed to be diffusion controlled, the fibers can serve as model systems to gain understanding of the silsesquioxane pyrolysis behavior, and therefore are useful in the development of polysilsesquioxane-derived ceramic matrices and coatings as well.

  2. Phosphorus-Silica Sol-Gel Hybrid Coatings for Flame Retardant Cotton Fabrics

    Directory of Open Access Journals (Sweden)

    Rosace Giuseppe

    2017-02-01

    Full Text Available This work investigates the use of organic-inorganic sol-gel coatings based on silica and phosphorous compounds for providing cotton fabrics with fl ame retardant features. To this aim, diethylphosphatoethyltriethoxysilane precursor was employed for the synthesis of several sols in combination with diff erent chemical additives. Sols were reacted with azo-based compounds and repeatedly applied onto the cellulosic substrate in a multilayer assembly, aiming at assessing the eff ect of the concurrent presence of Si, P and N on the overall fi re behaviour of the fabric. In order to evaluate the fl ame retardancy of treated cellulosic fabrics, fl ammability tests were carried out. The obtained results showed that the phosphorus-silica coating is able to promote the formation of a stable char that acts as insulator barrier. Finally, an additive P-N eff ect of the ceramic oxide coating in terms of increased residue and decreased heat release rate and total burning time was observed in cone calorimetry tests.

  3. High dose thermoluminescence dosimetry performance of Sol-gel synthesized TiO{sub 2} phosphors

    Energy Technology Data Exchange (ETDEWEB)

    Salas J, Ch. J.; Cruz V, C. [Universidad de Sonora, Departamento de Investigacion en Polimeros y Materiales, Apdo. Postal 130, 83000 Hermosillo, Sonora (Mexico); Castillo U, D. M.; Flores M, K. [Universidad de Sonora, Departamento de Ciencias Quimico Biologicas, Apdo. Postal 130, 83000 Hermosillo, Sonora (Mexico); Bernal, R. [Universidad de Sonora, Departamento de Investigacion en Fisica, Apdo. Postal 5-088, 83190 Hermosillo, Sonora (Mexico); Castano, V. M., E-mail: castillouzeta@gmail.com [UNAM, Instituto de Fisica, Centro de Fisica Aplicada y Tecnologia Avanzada, Apdo. Postal 1-1010, Queretaro, Qro. (Mexico)

    2015-10-15

    Full text: TiO{sub 2} is a ceramic material with many applications due to their different crystalline phases (rutile, anatase and brookite). It has attracted attention in several fields because their high mechanical strength, chemical stability and ion-conducting properties. Moreover, in recent years, some research groups gained interest in the thermoluminescence features of TiO{sub 2} concerning their potential use as thermoluminescence dosimeter. In this work, we present experimental results obtained in the first stage of a long-term research project focused in the synthesis of TiO{sub 2} phosphors for dosimetric applications. The thermoluminescent characterization of samples was carried out after being exposed to beta particle irradiation. TiO{sub 2} was prepared by alkoxide sol-gel route using titanium tetrabutoxide as precursor, ethanol, water and ammonia as catalyst. Pellet-shaped samples were annealed at 700 degrees C for 6 h in air atmosphere followed by slow cooling, and then were exposed to radiation doses from 25 to 400 Gy. The glow curves display maxima located at 103 and 238 degrees C when a 5 C/s heating rate is used. From the experimental results here presented, we conclude that TiO{sub 2} is a promising material to develop high dose Tl dosimeters. (Author)

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

    Science.gov (United States)

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

    2017-07-13

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

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

    Science.gov (United States)

    Li, Fa-Liang; Zhang, Hai-Jun

    2017-08-25

    The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined.

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

    Science.gov (United States)

    Li, Fa-Liang; Zhang, Hai-Jun

    2017-01-01

    The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined. PMID:28841188

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

    National Research Council Canada - National Science Library

    Xiaodong Wang; Guangming Wu; Bin Zhou; Jun Shen

    2013-01-01

      Titanium oxide coatings have been deposited by the sol-gel dip-coating method. Crystallization of titanium oxide coatings was then achieved through thermal annealing at temperatures above 400 °C...

  8. Infrared wire-grid polarizer with sol-gel antireflection films on both sides

    Science.gov (United States)

    Yamada, Itsunari; Ishihara, Yoshiro

    2017-12-01

    We fabricated an infrared wire-grid polarizer with the high transverse magnetic (TM) polarization transmittance and high extinction ratio by soft imprint lithography, sol-gel method, and Al shadow coating processes. A zilconia film was coated on Si substrate by using sol-gel method and spin coating method. Then, sol-gel zirconia grating was formed on the back side using imprinting using a silicone mold. The polarizer was produced by depositing Al obliquely on the grating. The TM transmittance of the fabricated element was greater than 80% at a wavelength of 4.8 μm. The sol-gel zilconia films acted as antireflection films. The extinction ratio exceeded 26 dB at its wavelength.

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

    Science.gov (United States)

    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.

  10. Preparation of YBCO superconductor nanoparticles by sol-gel combustion method

    National Research Council Canada - National Science Library

    M Farbod; M Tayeb Taher; I Kazeminezhad

    2010-01-01

    This paper describes the details of synthesizing nano crystalline YBCO superconductor using a sol-gel combustion method and the effect of sol pH and sintering temperature on particle size was investigated...

  11. [Effects of Sol-Gel coating on the corrosion resistance of nickel-chronium alloys].

    Science.gov (United States)

    Li, Lei; Zhu, Zhi-Min; Liao, Yun-Mao

    2009-02-01

    To investigate the effects of Sol-Gel coating on the corrosion resistance of nickel-chronium alloys in vitro. The bond strength of coating-substrate interface sintered at different temperatures (300, 400, 500, 600 degrees C) was tested by scratching method. The Sol-Gel coating was analyzed by scanning electron microscope (SEM), and its corrosion resistance was assessed by a static immersion method. The bond strength of coating-substrate interface reaches the peak at 400 degrees C. The Sol -Gel coating can apparently inhibit the release of metal ions and improve the corrosion resistance of nickel-chromium alloy. Sol-Gel coating can evidently improve corrosion resistance of the nickel-chromium alloy, which has great potential in prospective clinical practice.

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

    Science.gov (United States)

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

    2017-07-01

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Bansal, Narottam P.

    1989-01-01

    Silicon dioxide glasses containing 15 mole percent magnesium oxide prepared by sol-gel process. Not made by conventional melting because ingredients immiscible liquids. Synthesis of MgO/SiO2 glass starts with mixing of magnesium nitrate hexahydrate with silicon tetraethoxide, both in alcohol. Water added, and transparent gel forms. Subsequent processing converts gel into glass. Besides producing glasses of new composition at lower processing temperatures, sol-gel method leads to improved homogeneity and higher purity.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  17. Optical Behavior by Congo Red Doped in Polymer and Sol-Gel Film

    Directory of Open Access Journals (Sweden)

    A. Kazemzadeh

    2010-02-01

    Full Text Available A pH Chemical sensor with high sensitivity is achieved by direct attachment of Cong Red indicator over a Sol-Gel and polymeric film. This sensor is prepared by attaching Congo red over polymeric film or by adding indicator in tetra metoxysilan (TMOS in order to determining hydrogen ion in solution with high concentration of hydrogen and producing strong signals and rapid response time. Congo red is used over a Sol-Gel or polymeric film as a chemical-optical sensor. Sol-Gel layer and polymeric membrane have long lifetime as (>15 months and (>12 months and short response time as (>6 sec and (>9 sec respectively. It is a simple method and applied dye has low price and highly used. In this paper, the purpose is investigation and optimizing condition for Sol-Gel layer and polymeric film. Finally morphology of polymeric film and Sol-Gel layer surfaces were investigated by AFM apparatus and subsequently Sol-Gel layer have been found to be a favorite base for chemical sensor a fabrication.

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

    Directory of Open Access Journals (Sweden)

    DIANA HORKAVCOVÁ

    2012-12-01

    Full Text Available The objective of the submitted work was to prepare and to characterize two types of silicate coatings prepared by the sol-gel method using the dip-coating technique on a titanium substrate. Efforts have been made to use mechanical properties of bio-inert titanium and bioactive properties of a silicate layer enriched with an admixture of compounds identified below. The first group consisted of silicate coatings containing silver, brushite and monetite. The other group of silicate coatings contained calcium nitrate and triethyl phosphate. Mechanically and chemically treated titanium substrates were dipped into sols and dried and fired. Silicate coatings from the first group were also chemically treated in 10 mol.l-1 solution of sodium hydroxide. All coatings were measured to determine their adhesive and bioactive properties and furthermore the antibacterial properties were tested in the case of first group. Surfaces of the coated substrates were investigated after the firing and after the individual tests with optical and electron microscopy and X-ray microdiffraction. A tape test demonstrated excellent adhesive property of all coatings to the substrate, classified with degree 5. A static in vitro test demonstrated bioactivity of nearly all the coatings. The basic silicate coating from the first group and one type of coating from the second group were identified as inert. Antibacterial properties of silicate coatings containing silver showed to be different when tested against Escherichia coli bacteria. A complete inhibition of the growth of bacteria under our experimental conditions was observed for the coating containing silver and monetite and a partial inhibition of the growth of bacteria for coatings containing silver and silver in combination with brushite.

  19. Structural and physicochemical properties of nickel manganite NiMn{sub 2}O{sub 4-δ}synthesized by sol-gel and ultra sound assisted methods

    Energy Technology Data Exchange (ETDEWEB)

    Alburquenque, D. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Metallurgy Department, USACH, Ave Ecuador 3469, Santiago 9170124 (Chile); Troncoso, L.; Denardin, J.C. [Physics Department, USACH, Ave. Ecuador 3493, Santiago 9170124 (Chile); Butera, A. [Atomic Center, CNEA, Ito. Balseiro, Bariloche Rio Negro 84000 (Argentina); Padmasree, K.D. [Cinvestav, U.Saltillo, Monterrey Km 13.5, Saltillo CP 25900 (Mexico); Ortiz, J.; Herrera, F. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Marco, J.F. [Institute of Physical Chemistry “Rocasolano”, CSIC, Serrano 119, Madrid 28006 (Spain); Gautier, J.L., E-mail: juan.gautier@usach.cl [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile)

    2016-07-05

    In this work we present the structural, magnetic and surface characterization of the ceramic nickel manganite oxide NiMn{sub 2}O{sub 4-δ} synthesized by two methods: sol-gel and ultrasound-assisted sol-gel using nitrate salts as precursors. We have characterized the non-stoichiometric samples NiMn{sub 2}O{sub 4-δ} using different physicochemical analyses. X-ray diffraction and Rietveld refinement of the X-ray data indicated that the samples crystallize in the Fd3m space group characteristic of cubic spinel-related oxides. The specific surface area of the oxides was 1.3 m{sup 2}/g (SG) and 16.3 m{sup 2}/g (UASG). SEM results showed particle agglomerates of 1.05 μm (SG) and 0.85 μm (UASG). Temperature dependence magnetization measurements were performed and a ferrimagnetic transition was identified at 103 K and 105 K depending on the preparation method (SG and UASG, respectively). The observed Curie constant was found to vary from 7.4 to 7.7 cm{sup 3} K mol{sup −1} and hysteretic magnetization vs. applied field curves at different temperatures were obtained. XPS studies of these oxides reveal the presence of Ni{sup 2+}, Mn{sup 2+}, Mn{sup 3+} and Mn{sup 4+} ions at the surface. A probable ionic distribution as a function of the synthesis method is proposed. - Highlights: • Nickel manganite was synthesized by sol gel synthesis and a novel ultrasound-assisted sol gel method. . • Bulk and surface cation distributions are proposed. • Physicochemical properties, including magnetic and surface area measurements, were studied for both types of samples.

  20. The crystallization behavior and thermal expansion properties of {beta}-eucryptite prepared by sol-gel route

    Energy Technology Data Exchange (ETDEWEB)

    Xia Long [School of Material Science and Engineering, Harbin Institute of Technology at Weihai, 2 Wenhua West Road, Weihai 264209 (China); Wen Guangwu, E-mail: wgw@hitwh.edu.cn [School of Material Science and Engineering, Harbin Institute of Technology at Weihai, 2 Wenhua West Road, Weihai 264209 (China); Song Liang; Wang Xinyu [School of Material Science and Engineering, Harbin Institute of Technology at Weihai, 2 Wenhua West Road, Weihai 264209 (China)

    2010-02-15

    Lithium-aluminosilicate glass-ceramics in the form of eucryptite were synthesized through sol-gel technique by mixing boehmite sol, silica sol and lithium salt and sintering at different temperatures for further analysis. Thermogravimetry (TG), differential thermal analysis (DTA), X-ray diffraction (XRD), IR analysis and dilatometry were done to study sintering characteristics, phase transformation and thermal expansion behavior on the sintered specimens. XRD and FTIR results confirmed that crystallization of {beta}-eucryptite took place at about 600 deg. C, substantial increase of {beta}-eucryptite was observed in the specimens sintered at temperatures from 800 to 1300 deg. C. Trace amount of cristobalite also emerged at 600 deg. C and disappeared at 1300 deg. C. The thermal expansion behavior characteristics were found to be strongly influenced by crystalline phases in the specimens which depended on the sintering temperatures.

  1. Synthesis of nanocrystalline NiCuZn ferrite powders by sol-gel auto-combustion method

    Energy Technology Data Exchange (ETDEWEB)

    Yue, Zhenxing; Zhou, Ji; Li, Longtu; Zhang, Hongguo; Gui, Zhilun

    2000-01-01

    A nitrate-citrate gel was prepared from metal nitrates and citric acid by sol-gel process, in order to synthesize Ni{sub 0.25}Cu{sub 0.25}Zn{sub 0.50}Fe{sub 2}O{sub 4} ferrite. The thermal decomposition process was investigated by DTA-TG, IR and XRD techniques. The results revealed that the nitrate-citrate gel exhibits self-propagating combustion behavior. After combustion, the gel directly transformed into single-phase, nano-sized NiCuZn ferrite particles with spinel crystal structure. The synthesized powder can be densified at a temperature lower than 900 deg. C. The sintered body possesses fine-grained microstructure, good frequency stability and high-quality factor compared to the sample prepared by conventional ceramic route.

  2. Synthesis of ceramic powders of La{sub 9,56} (SiO{sub 4}){sub 6}O{sub 2,34} and La{sub 9,8}Si{sub 5,7}Mg{sub O,3}O{sub 26,}4 by modified sol-gel process; Sintese de pos ceramicos de La{sub 9,56} (SiO{sub 4}){sub 6}O{sub 2,34} e La{sub 9,8}Si{sub 5,7}Mg{sub O,3}O{sub 26,}4 por processo sol-gel modificado

    Energy Technology Data Exchange (ETDEWEB)

    Lira, Sabrina Lopes; Paiva, Mayara Rafaela Soares; Misso, Agatha Matos; Elias, Daniel Ricco; Yamagata, Chieko, E-mail: yamagata@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (CCTM/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencia e Tecnologia de Materiais

    2012-07-01

    Lanthanum silicate oxyapatite materials are promising for application as electrolyte in solid oxide fuel cells because of high ionic conductivity at temperatures between 600 deg C and 800 deg C. In this work, oxyapatites with the composition La{sub 9,56}(SiO{sub 4}){sub 6}O{sub 2,34}, and La{sub 9,8}Si{sub 5,7}Mg{sub 0,3}O{sub 26,4} were synthesized by using the sol-gel method, followed by precipitation. Initially, the gel of silica was synthesized from sodium silicate solution, by acid catalysis using lanthanum and magnesium chloride solution. Then, the La and Mg hydroxides were precipitated with NaOH in the gel. The powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and measurements of specific surface area. The crystalline oxyapatite phase of La{sub 9,56}(SiO{sub 4}){sub 6}O{sub 2,34}, and was La{sub 9,8}Si{sub 5,7}Mg{sub 0,3}O{sub 26,4} obtained by calcination at 900 deg C for 2 and 1h respectively (author)

  3. Sol-gel-based molecularly imprinted xerogel for capillary microextraction.

    Science.gov (United States)

    Bagheri, Habib; Piri-Moghadam, Hamed

    2012-09-01

    A novel molecularly imprinted xerogel (MIX) based on organically modified silica (ORMOSIL) was successfully prepared for on-line capillary microextraction (CME) coupled with high-performance liquid chromatography (HPLC). The sol-gel-based xerogel was prepared using only one precursor and exhibited extensive selectivity towards triazines along with significant thermal and chemical stability. Atrazine was selected as a model template molecule and 3-(trimethoxysilyl)propylmethacrylate (TMSPMA) as a precursor in which the propylmethacrylate moiety was responsible for van der Waals, dipole-dipole, and hydrogen-bond interactions with the template. This moiety plays a key role in creation of selective sites while methoxysilyl groups in TMSPMA acted as crosslinkers between the template and the propylmethacrylate moiety. Moreover, a non-imprinted xerogel (NIX) was also prepared in the absence of the template for evaluating the extraction efficiency of the prepared MIX. Then, the prepared imprinted and non-imprinted xerogels were used for extraction of three selected analytes of triazines class including atrazine, ametryn, and terbutryn, which have rather similar structures. The extraction efficiency of the prepared xerogel for atrazine, the template molecule, was found to be ten times greater than the efficiency achieved by the non-imprinted one. In the meantime, the extraction efficiency ratio of MIX to NIX for ametryn and terbutryn was also rather significant (eight times). Moreover, other compounds from different classes including dicamba, mecoprop, and estriol were also analyzed to evaluate the selectivity of the prepared MIX towards triazines. The ratio of enrichment factors (EF) of MIX to NIX for atrazine, ametryn, terbutryn, dicamba, mecoprop, and estriol were about 10, 8, 8, 2, 2, and 3, respectively. The linearity for the analytes was in the range of 5-700 μg L(-1). Limit of detection was in the range of 1-5 μg L(-1) and the RSD% values (n = 5) were all below 6

  4. Sol-Gel Deposited Double Layer TiO₂ and Al₂O₃ Anti-Reflection Coating for Silicon Solar Cell.

    Science.gov (United States)

    Jung, Jinsu; Jannat, Azmira; Akhtar, M Shaheer; Yang, O-Bong

    2018-02-01

    In this work, the deposition of double layer ARC on p-type Si solar cells was carried out by simple spin coating using sol-gel derived Al2O3 and TiO2 precursors for the fabrication of crystalline Si solar cells. The first ARC layer was created by freshly prepared sol-gel derived Al2O3 precursor using spin coating technique and then second ARC layer of TiO2 was deposited with sol-gel derived TiO2 precursor, which was finally annealed at 400 °C. The double layer Al2O3/TiO2 ARC on Si wafer exhibited the low average reflectance of 4.74% in the wavelength range of 400 and 1000 nm. The fabricated solar cells based on double TiO2/Al2O3 ARC attained the conversion efficiency of ~13.95% with short circuit current (JSC) of 35.27 mA/cm2, open circuit voltage (VOC) of 593.35 mV and fill factor (FF) of 66.67%. Moreover, the fabricated solar cells presented relatively low series resistance (Rs) as compared to single layer ARCs, resulting in the high VOC and FF.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lakshmi, R.V. [Surface Engineering Division, Council of Scientific and Industrial Research – National Aerospace Laboratories, HAL Airport Road, Kodihalli, Bengaluru 560017 (India); Aruna, S.T., E-mail: staruna194@gmail.com [Surface Engineering Division, Council of Scientific and Industrial Research – National Aerospace Laboratories, HAL Airport Road, Kodihalli, Bengaluru 560017 (India); Sampath, S. [Department of Inorganic and Physical Chemistry, Indian Institute of Science, Bengaluru 560012 (India)

    2017-01-30

    Highlights: • Corrosion protection efficiency comparison of ceria nanoparticles and cerium nitrate. • Silica-alumina hybrid coating exhibited good barrier protection. • Detailed XPS study confirm the hybrid structure and presence of Ce species in coating. • Loss of cerium ions not prevalent in ceria doped coating unlike that of cerium nitrate. • Ceria increased the coating integrity, corrosion inhibition and barrier protection. - Abstract: The present work provides a comparative study on the corrosion protection efficiency of defect free sol-gel hybrid coating containing ceria nanoparticles and cerium nitrate ions as corrosion inhibitors. Less explored organically modified alumina-silica hybrid sol-gel coatings are synthesized from 3-glycidoxypropyltrimethoxysilane and aluminium-tri-sec-butoxide. The microemulsion derived nanoparticles and the hybrid coatings are characterized and compared with coatings containing cerium nitrate. Corrosion inhibiting capability is assessed using electrochemical impedance spectroscopy. Scanning Kelvin probe measurements are also conducted on the coatings for identifying the apparent corrosion prone regions. Detailed X-ray photoelectron spectroscopy (XPS) analysis is carried out to comprehend the bonding and corrosion protection rendered by the hybrid coatings.

  6. Review and the state of the art: Sol-gel and melt quenched bioactive glasses for tissue engineering.

    Science.gov (United States)

    Kaur, Gurbinder; Pickrell, Gary; Sriranganathan, Nammalwar; Kumar, Vishal; Homa, Daniel

    2016-08-01

    Biomaterial development is currently the most active research area in the field of biomedical engineering. The bioglasses possess immense potential for being the ideal biomaterials due to their high adaptiveness to the biological environment as well as tunable properties. Bioglasses like 45S5 has shown great clinical success over the past 10 years. The bioglasses like 45S5 were prepared using melt-quenching techniques but recently porous bioactive glasses have been derived through sol-gel process. The synthesis route exhibits marked effect on the specific surface area, as well as degradability of the material. This article is an attempt to provide state of the art of the sol-gel and melt quenched bioactive bioglasses for tissue regeneration. Fabrication routes for bioglasses suitable for bone tissue engineering are highlighted and the effect of these fabrication techniques on the porosity, pore-volume, mechanical properties, cytocompatibilty and especially apatite layer formation on the surface of bioglasses is analyzed in detail. Drug delivery capability of bioglasses is addressed shortly along with the bioactivity of mesoporous glasses. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 1248-1275, 2016. © 2015 Wiley Periodicals, Inc.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-04-08

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

  8. Carbon nanotube-coated solid-phase microextraction metal fiber based on sol-gel technique.

    Science.gov (United States)

    Jiang, Ruifen; Zhu, Fang; Luan, Tiangang; Tong, Yexiang; Liu, Hong; Ouyang, Gangfeng; Pawliszyn, Janusz

    2009-05-29

    A novel carbon nanotube (CNT)-coated solid-phase microextraction fiber was prepared based on sol-gel technique. Commonly used fragile fused silica fiber was replaced with stainless steel wire, which made the fiber unbreakable. An approach was also proposed for batch producing, and good reproducibilities for fiber to fiber and between fibers were achieved. Experiments showed that the sol-gel-CNT fiber exhibited high thermal stability to resist 350 degrees C and excellent solvent durability in methanol and acetonitrile. Compared to commercial polydimethylsiloxane (PDMS) fiber, the sol-gel-CNT fiber represented significantly improved extraction efficiencies for both polar (phenols) and non-polar (benzene, toluene, ethylbenzene, and o-xylene) compounds. Meanwhile, no replacement effect, low carry-over and wide linear range demonstrated that the newly prepared sol-gel-CNT coating has liquid properties, which allow a relatively easy quantification procedure. Moreover, the characterization of the sol-gel-CNT coating was also evaluated with McReynold probe solutes. The results showed that the coating has better affinity for all the five types of solutes compared to commercial 7microm PDMS fiber, which suggested that the coating has the potential to be developed as GC stationary phase.

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

    DEFF Research Database (Denmark)

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

    2015-01-01

    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...

  10. Infrared wire-grid polarizer with sol-gel zirconia grating

    Science.gov (United States)

    Yamada, Itsunari; Ishihara, Yoshiro

    2017-05-01

    The infrared wire-grid polarizer consisting of an Al grating, Si, and sol-gel derived zirconia grating film was fabricated by soft imprint process and Al shadow coating processes. A silicone mold was used because of its low surface energy, flexibility, and capability of transferring submicrosized patterns. As a result, the Al grating with a pitch of 400 nm and a depth of 100 nm was obtained on the zirconia grating film. The fabricated polarizer exhibited a polarization function with the TM transmittance greater than that of the Si substrate in the specific wavelength range of 3.6-8.5 μm, because the zirconia film acted as an antireflection film. The maximum value was 63% at a wavelength of 5.2 μm. This increment of the TM transmission spectrum results in interference within the zirconia film. Also, the extinction ratio exceeded almost 20 dB in the 3-8.8 μm wavelength range.

  11. Bioactive sol-gel glass added ionomer cement for the regeneration of tooth structure.

    Science.gov (United States)

    Choi, Jung-Young; Lee, Hae-Hyoung; Kim, Hae-Won

    2008-10-01

    Dental cements including the glass ionomer cement (GIC) have found widespread use in restoring tooth structures. In this study, a sol-gel derived glass (SG) with a bioactive composition (70SiO(2).25CaO.5P(2)O(5)) was added to the commercial GIC (GC, Fuji I) to improve the bioactivity and tooth regeneration capability. The SG powders prepared with sizes in the range of a few micrometers were mixed with GIC at SG/GC ratios of 10 and 30 wt%. The setting time, diametral tensile strength, and in vitro bioactivity of the GC-SG cements were examined. The setting time of the GC-SG cements increased with increasing amount of SG. However, the addition of SG did not significantly alter the diametral tensile strength of the GC. GC-SG induced the precipitation of an apatite bone-mineral phase on the surface after immersion in a simulated body fluid (SBF), showing in vitro bone bioactivity. However, no mineral induction in SBF was observed in the commercial GIC after the immersion. The in vitro cell assay confirmed that the GC-SG samples produced higher cell viability than the GC sample with cell culturing for up to 7 days.

  12. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    Science.gov (United States)

    Seyyal, Emre; Malik, Abdul

    2017-04-29

    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C12) and phenethyl (PhE) ligands. Here, the ability of the PF-C12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L-1 limit of detections (LOD) (4

  13. Biodegradable and adjustable sol-gel glass based hybrid scaffolds from multi-armed oligomeric building blocks.

    Science.gov (United States)

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

    2017-11-01

    Biodegradability is a crucial characteristic to improve the clinical potential of sol-gel-derived glass materials. To this end, a set of degradable organic/inorganic class II hybrids from a tetraethoxysilane(TEOS)-derived silica sol and oligovalent cross-linker oligomers containing oligo(d,l-lactide) domains was developed and characterized. A series of 18 oligomers (Mn: 1100-3200Da) with different degrees of ethoxylation and varying length of oligoester units was established and chemical composition was determined. Applicability of an established indirect rapid prototyping method enabled fabrication of a total of 85 different hybrid scaffold formulations from 3-isocyanatopropyltriethoxysilane-functionalized macromers. In vitro degradation was analyzed over 12months and a continuous linear weight loss (0.2-0.5wt%/d) combined with only moderate material swelling was detected which was controlled by oligo(lactide) content and matrix hydrophilicity. Compressive strength (2-30MPa) and compressive modulus (44-716MPa) were determined and total content, oligo(ethylene oxide) content, oligo(lactide) content and molecular weight of the oligomeric cross-linkers as well as material porosity were identified as the main factors determining hybrid mechanics. Cytocompatibility was assessed by cell culture experiments with human adipose tissue-derived stem cells (hASC). Cell migration into the entire scaffold pore network was indicated and continuous proliferation over 14days was found. ALP activity linearly increased over 2weeks indicating osteogenic differentiation. The presented glass-based hybrid concept with precisely adjustable material properties holds promise for regenerative purposes. Adaption of degradation kinetics toward physiological relevance is still an unmet challenge of (bio-)glass engineering. We therefore present a glass-derived hybrid material with adjustable degradation. A flexible design concept based on degradable multi-armed oligomers was combined with an

  14. Microwave sintering of sol-gel composite films using a domestic microwave oven

    Science.gov (United States)

    Kobayashi, Makiko; Matsumoto, Makoto

    2016-07-01

    Feasibility study of sol-gel composite microwave sintering using a domestic microwave oven was carried out. Two kinds of lead zirconate titanate (PZT) powders were mixed with PZT sol-gel solution and the mixture was sprayed onto 3-mm-thick titanium substrate. The films were sintered by 700 W domestic oven for 10 min. Ultrasonic measurement was carried out in pulse-echo mode and clear multiple echoes were confirmed. It would be suitable method to fabricate high frequency broadband focused ultrasonic transducers. Further research is required to improve sintering degree.

  15. Experiences with sol-gel bonded high porosity alumina fiber materials for filter applications

    OpenAIRE

    Handrick, Karin E.; Mohlratzer, August; Ostertag, Rolf; Sporn, Dieter; Schmidt, Helmut K.

    1988-01-01

    High porous alumina fiber structures appear promising for hot gas filtration in particular for diesel particulate traps. For this purpose, however, a method is required for manufacturing of stable shapes resisant to the blow-out by the gas flow. The sol-gel process was expected to be the best suited method for fiber bonding to provide the required stability. The main tasks of the development-work were a uniform isotropic fiber-distribution, the adaptation of the sol-gel-process to the applica...

  16. Investigation of Sol-Gel coatings exposed in the condenser at Fynsvaerket. Part 1

    Energy Technology Data Exchange (ETDEWEB)

    Montgomery, M. [DTU Management Engineering, Kgs. Lyngby (Denmark); Vilhelmsen, T. [Vattenfall Heat Nordic, Copenhagen (Denmark)

    2007-10-15

    The Danish Technological Institute (DTI) has developed a coatings technique using Hybrid Sol-gel nanotechnology to produce coatings which can change the surface characteristics of various components. It is the purpose of this project to investigate where such coatings can be utilised in the power generating industry with respect to fouling and corrosion resistance. Four different sol-gel coatings have been applied to brass condenser tubes about 10 cm in length. The coatings are termed 23, 35, 38, 46. The exact composition of these different coatings was not given. These sections were mounted in the water chamber inlet before the tubes into the condenser and another set were placed on the condenser plate at the outlet. The condenser tube has a composition 76 wt.% Cu, 22 wt.% Zn and 2 wt.% Al corresponding to an aluminium brass. Based on the visual appearance of the four coatings it is clear that Sol-gel 38 does not reduced biological fouling and rust spots can be clearly seen on Sol-gel 46. Thus based on visual appearance, sol-gel 23 and sol-gel 35 are most promising. Due to the presence of corrosion products on the inner side of the unexposed tubes which influences the adherence and protectiveness of coatings applied, the inner side cannot be used to assess the coatings performance. In the next exposure test, better initial cleaning of the tubes is required. Based on visual assessment, Sol-gel 38 has not solved the problems with biological fouling compared to the other coatings. With respect to corrosion, it is observed that in all cases there are corrosion products, either chlorides or oxides/hydroxides/carbonates, present in the interface between the tube and the coating. Coating 38 also experienced lack of adhesion. This could be triggered by a build up of corrosion products under the coating which would eventually lead to delaminating of the coating. Whether the corrosion rate has been decreased compared to the uncoated tubes is not known, however in the next

  17. Nanoporous titania-coated alumina membranes: sol-gel synthesis and characterisation.

    Science.gov (United States)

    Kermanpur, A; Dastjerdi, V H; Ghassemali, E; Abbasi, M H

    2010-09-01

    In this work, nanoporous titania top layers were deposited by dip-coating process on microporous alpha-alumina substrates using the sol-gel process. The alumina substrates were synthesized by slip casting method using Taguchi optimising approach. The microporous substrate was then used to coat nanoporous titania layers by the sol-gel method. The thickness, pore size, structure and permeability of the membranes were characterised using SEM, XRD, STA and Hg-Porosimetry. The process conditions to achieve defect-free nanoporous titania layers with the average pore size of about 4 nm coated on the microporous alumina substrates with the average pore size of about 270 nm were determined.

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

    National Research Council Canada - National Science Library

    Schmidt, Helmut

    1998-01-01

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

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

    Science.gov (United States)

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

    2016-04-15

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

  20. Weathering characteristics and moisture uptake properties of wood coated with water-borne sol-gel thin films

    Science.gov (United States)

    M. A. Tshabalala; C. Starr; N. R. Sutherland

    2010-01-01

    In this study, wood specimens were coated with water-borne silsesquioxane oligomers by an in situ sol-gel deposition process. The effect of these water-borne sol-gel thin films on weathering characteristics and moisture-uptake properties of the wood specimens were investigated. The weathering characteristics were investigated by exposure of the specimens to artificial...

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

    NARCIS (Netherlands)

    Langanke, J.; Arfsten, N.; Buskens, P.; Habets, R.; Klankermayer, J.; Leitner, W.

    2013-01-01

    Scratch resistant sol-gel metal oxide coatings typically require a thermal post-treatment step (curing process) at temperatures between 400 and 700 C. In this report, we demonstrate that the in situ generation of amines within sol-gel films facilitates the preparation of scratch resistant metal

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

    Science.gov (United States)

    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.

  3. Effect of matrix treatment on spectroscopic properties of HCl catalysed sol-gel glasses containing coumarin laser dyes.

    Science.gov (United States)

    Deshpande, Aparna V; Jathar, Laxman V; Rane, Jayraj R

    2009-07-01

    Coumarin 1, Coumarin 2 and Coumarin 120 are embedded in transparent sol-gel glass samples prepared by sol-gel process using dip method. The sol-gel matrix is given dip treatment with Methanol /Distilled Water (50/50 vol) for 1 to 16 h before dipping into dye solution. The effect of dipping time of matrix in Methanol/ Distilled Water on spectroscopic properties of coumarin dye doped glass samples has been studied. The Optical Density (OD) at absorption maximum wavelength and Fluorescence Intensity (FI) at fluorescence maximum wavelength of all coumarin dyes increase with the time of dipping of the sol-gel sample. These absorption/fluorescence properties of coumarin dyes in sol-gel glass matrices are compared with its respective properties in methanolic solution in acidic environment. The cause of these changes in OD/FI with dipping time is discussed by taking into account the absorption / fluorescence of dye in acidified methanol.

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

    Science.gov (United States)

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

    2015-01-01

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

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

    Science.gov (United States)

    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.

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

    NARCIS (Netherlands)

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

    1994-01-01

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

  7. Thermal stability of porous sol-gel phosphosilicates and their surface area stabilisation by lanthanum addition

    NARCIS (Netherlands)

    Falco, Lorena; De Mendonca, Mariana Van Den Tempel; Mercadal, Juan J.; Zarubina, Valeriya; Melián-Cabrera, Ignacio

    2016-01-01

    The thermal stability of porous sol-gel phosphosilicates was studied by comparing the textural features upon calcination between 400 and 550 °C. A significant loss of surface area and pore volume were observed; the first is due to thermal coarsening of the nanoparticles, and the pore volume

  8. Estado del arte del proceso sol-gel en México

    Directory of Open Access Journals (Sweden)

    María Teresa Ramírez Palma

    2010-01-01

    Full Text Available A partir de una revisión bibliográfica, realizada por alumnos de la Maestría en Ciencia e Ingeniería de Materiales de la unam, se muestra el estado del arte del proceso sol-gel en México.

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

    African Journals Online (AJOL)

    Mixed metal oxides of titanium and zinc nanocomposites were prepared through sol-gel method under hydrothermal condition using titanium oxy-(1, 2 - pentadione) and zinc acetate without hazardous additives. The resulting composites were characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscope ...

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

    Directory of Open Access Journals (Sweden)

    Vinod Upadhyay

    2017-06-01

    Full Text Available In this work, the performances of several natural organic inhibitors were investigated in a sol-gel system (applied on the magnesium alloy Mg AZ31B substrate. The inhibitors were quinaldic acid (QDA, betaine (BET, dopamine hydrochloride (DOP, and diazolidinyl urea (DZU. Thin, uniform, and defect-free sol-gel coatings were prepared with and without organic inhibitors, and applied on the Mg AZ31B substrate. SEM and EDX were performed to analyze the coating surface properties, the adhesion to the substrate, and the thickness. Electrochemical measurements, including electrochemical impedance spectroscopy (EIS and anodic potentiodynamic polarization scan (PDS, were performed on the coated samples to characterize the coatings’ protective properties. Also, hydrogen evolution measurement—an easy method to measure magnesium corrosion—was performed in order to characterize the efficiency of coating protection on the magnesium substrate. Moreover, scanning vibrating electrode technique (SVET measurements were performed to examine the efficiency of the coatings loaded with inhibitors in preventing and containing corrosion events in defect areas. From the testing results it was observed that the formulated sol-gel coatings provided a good barrier to the substrate, affording some protection even without the presence of inhibitors. Finally, when the inhibitors’ performances were compared, the QDA-doped sol-gel was able to contain the corrosion event at the defect.

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

    NARCIS (Netherlands)

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

    2006-01-01

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

  12. Sol-gel-cum-hydrothermal synthesis of mesoporous Co-Fe ...

    Indian Academy of Sciences (India)

    A combined sol-gel-cum-hydrothermalmethod has been employed to synthesize novelmonometallic (Mn, Fe, Co) and bimetallic (Co-Fe, Mn-Co, Fe-Mn) nanoparticles loaded onto Al₂O₃−MCM-41. Powder XRD, N2 sorption, field emission scanning electron microscopy (FESEM) and high resolution transmission electron ...

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

    Energy Technology Data Exchange (ETDEWEB)

    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

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

    Science.gov (United States)

    Yasakau, Kiryl

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

  15. Influence of Ce{sup 3+} doping on molecular organization of Si-based organic/inorganic sol-gel layers for corrosion protection

    Energy Technology Data Exchange (ETDEWEB)

    Fedel, Michele, E-mail: michele.fedel@unitn.it [Department of Industrial Engineering, University of Trento, via Sommarive 9, Povo (Italy); Callone, Emanuela [Department of Industrial Engineering, University of Trento, via Sommarive 9, Povo (Italy); “K. Müller” Magnetic Resonance Lab, University of Trento, via Sommarive 9, Povo (Italy); Fabbian, Matias; Deflorian, Flavio [Department of Industrial Engineering, University of Trento, via Sommarive 9, Povo (Italy); Dirè, Sandra [Department of Industrial Engineering, University of Trento, via Sommarive 9, Povo (Italy); “K. Müller” Magnetic Resonance Lab, University of Trento, via Sommarive 9, Povo (Italy)

    2017-08-31

    Highlights: • Ce{sup 3+} ions promote a decrease of the degree of condensation of the silsesquioxane network. • Ce{sup 3+} ions affect ladder and cages like structures formation in the silsesquioxane network. • Ce{sup 3+} ions do not significantly affect the barrier properties of the coatings. • [Ce{sup 3+}] ≈ 5·10{sup −4} M provides the sol-gel film with an effective passivating potential. - Abstract: In this work, organosilane-derived sol-gel films containing different amounts of cerium ions applied on AA 1050 were investigated. The sol-gel coatings were prepared from 3-glycidoxypropyltrimethoxysilane (GPTMS) and methyltriethoxysilane (MTES) mixtures with the addition of cerium nitrate in order to achieve different concentrations of Ce ions (from 10{sup −5} M to 10{sup −2} M). The effect of the cerium load on the structure of the cured sol-gel films was investigated by means of solid state NMR and FT-IR spectroscopy. The corrosion protection properties of the different sol-gel layers were investigated mainly by means potentiodynamic curves and electrochemical impedance spectroscopy (EIS). FT-IR and solid state NMR suggested a significant influence of the Ce cations on the network structure: not only the degree of condensation decreases with Ce addition but also the structural modification of the silsesquioxane network is observed with preferential formation of ladder-like species for low Ce{sup 3+} content and cages predominance for Ce/Si molar ratio greater than 0.039, i.e. [Ce{sup 3+}] = 1·10{sup −4} M. Electrochemical tests revealed that the effect of Ce ions on the structure of the coatings does not lead to remarkable changes in the barrier properties. Moreover, it was found that the Ce ions seems to be present in the cured films and are able to migrate towards the metal/coating interface thus providing a stabilization of the metal interface.

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

    Directory of Open Access Journals (Sweden)

    Kisaalita William S

    2011-05-01

    Full Text Available Abstract 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.

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

    Science.gov (United States)

    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.

  18. Molecularly Imprinted Sol-Gel-Based QCM Sensor Arrays for the Detection and Recognition of Volatile Aldehydes

    Directory of Open Access Journals (Sweden)

    Chuanjun Liu

    2017-02-01

    Full Text Available The detection and recognition of metabolically derived aldehydes, which have been identified as important products of oxidative stress and biomarkers of cancers; are considered as an effective approach for early cancer detection as well as health status monitoring. Quartz crystal microbalance (QCM sensor arrays based on molecularly imprinted sol-gel (MISG materials were developed in this work for highly sensitive detection and highly selective recognition of typical aldehyde vapors including hexanal (HAL; nonanal (NAL and bezaldehyde (BAL. The MISGs were prepared by a sol-gel procedure using two matrix precursors: tetraethyl orthosilicate (TEOS and tetrabutoxytitanium (TBOT. Aminopropyltriethoxysilane (APT; diethylaminopropyltrimethoxysilane (EAP and trimethoxy-phenylsilane (TMP were added as functional monomers to adjust the imprinting effect of the matrix. Hexanoic acid (HA; nonanoic acid (NA and benzoic acid (BA were used as psuedotemplates in view of their analogous structure to the target molecules as well as the strong hydrogen-bonding interaction with the matrix. Totally 13 types of MISGs with different components were prepared and coated on QCM electrodes by spin coating. Their sensing characters towards the three aldehyde vapors with different concentrations were investigated qualitatively. The results demonstrated that the response of individual sensors to each target strongly depended on the matrix precursors; functional monomers and template molecules. An optimization of the 13 MISG materials was carried out based on statistical analysis such as principle component analysis (PCA; multivariate analysis of covariance (MANCOVA and hierarchical cluster analysis (HCA. The optimized sensor array consisting of five channels showed a high discrimination ability on the aldehyde vapors; which was confirmed by quantitative comparison with a randomly selected array. It was suggested that both the molecularly imprinting (MIP effect and the matrix

  19. Molecularly Imprinted Sol-Gel-Based QCM Sensor Arrays for the Detection and Recognition of Volatile Aldehydes.

    Science.gov (United States)

    Liu, Chuanjun; Wyszynski, Bartosz; Yatabe, Rui; Hayashi, Kenshi; Toko, Kiyoshi

    2017-02-16

    The detection and recognition of metabolically derived aldehydes, which have been identified as important products of oxidative stress and biomarkers of cancers; are considered as an effective approach for early cancer detection as well as health status monitoring. Quartz crystal microbalance (QCM) sensor arrays based on molecularly imprinted sol-gel (MISG) materials were developed in this work for highly sensitive detection and highly selective recognition of typical aldehyde vapors including hexanal (HAL); nonanal (NAL) and bezaldehyde (BAL). The MISGs were prepared by a sol-gel procedure using two matrix precursors: tetraethyl orthosilicate (TEOS) and tetrabutoxytitanium (TBOT). Aminopropyltriethoxysilane (APT); diethylaminopropyltrimethoxysilane (EAP) and trimethoxy-phenylsilane (TMP) were added as functional monomers to adjust the imprinting effect of the matrix. Hexanoic acid (HA); nonanoic acid (NA) and benzoic acid (BA) were used as psuedotemplates in view of their analogous structure to the target molecules as well as the strong hydrogen-bonding interaction with the matrix. Totally 13 types of MISGs with different components were prepared and coated on QCM electrodes by spin coating. Their sensing characters towards the three aldehyde vapors with different concentrations were investigated qualitatively. The results demonstrated that the response of individual sensors to each target strongly depended on the matrix precursors; functional monomers and template molecules. An optimization of the 13 MISG materials was carried out based on statistical analysis such as principle component analysis (PCA); multivariate analysis of covariance (MANCOVA) and hierarchical cluster analysis (HCA). The optimized sensor array consisting of five channels showed a high discrimination ability on the aldehyde vapors; which was confirmed by quantitative comparison with a randomly selected array. It was suggested that both the molecularly imprinting (MIP) effect and the matrix

  20. Synthesis and characterization of {alpha}-alumina col-gel nanometric: elaboration of biomaterials nanostructured for biomedical applications; Sintese e caracterizacao de alumina-{alpha} sol-gel nanometrica: para elaboracao de biomateriais nanoestruturados para aplicacoes biomedicas

    Energy Technology Data Exchange (ETDEWEB)

    Passoni, L.S.; Feit, G.; Camargo, N.H.A., E-mail: laispassoni@gmail.co [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Centro de Ciencias Tecnologicas

    2010-07-01

    The production of nanostructured biomaterials are research themes for these present new characteristics of biocompatibility and bioactivity. The sol-gel process allows obtaining {alpha}-alumina nanometric with purity 99.99%. The use of nanoparticles of Al{sub 2}O{sub 3}-{alpha}, SiO{sub 2} and TiO{sub 2} are being employed as a second stage in the development of nanocomposites biomaterials. The presence of the second phase within a ceramic matrix leads to obtaining nanomaterials with micropores in micro and nanostructures interconnected, what contributes within the processes of osseous integration, osseous induction. The goal of this work focused on synthesis and characterization of an {alpha}- alumina by sol-gel process. Characterization studies were conducted using the various techniques: X-ray diffraction, scanning electron microscopy, exploratory differential scanning calorimetry and infrared spectrometry by Fourier transforms. The preliminary results showed the attainment the nanometric {alpha}-alumina powder. (author)

  1. In situ analysis of phase transformation in sol-gel cogelified nanopowder mixture of Al 2O 3 and TiO 2 using synchrotron X-ray radiation diffraction experiments

    Science.gov (United States)

    Jianu, A.; Stanciu, L.; Groza, J. R.; Lathe, Ch.; Burkel, E.

    2003-01-01

    Aluminium titanate (Al 2TiO 5) has been selected for study due to its high melting point and thermal shock resistance. In situ analysis of phase transformation and of transformation kinetics of sol-gel powder mixture of alumina and titania cogelified samples was performed using high-temperature synchrotron radiation X-ray diffraction experiments. The high reactivity and molecular mixing of sol-gel cogelified precursor powders contributed to the evolution of the reaction. The stability of the TiO 2-tetragonal structure (anatase) increases due to Al 2O 3 presence. The temperature of the aluminium titanate endothermic reaction decreases when heating rate increases. The results obtained by in situ analysis have been used to establish the sintering parameters in order to obtain fully transformed, dense aluminium titanate bulk ceramics.

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

    DEFF Research Database (Denmark)

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

    2011-01-01

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

  3. Effect of ZrN coating by magnetron sputtering and sol-gel processed silica coating on titanium/porcelain interface bond strength.

    Science.gov (United States)

    Xia, Yang; Zhou, Shu; Zhang, Feimin; Gu, Ning

    2011-02-01

    In this study, a coating technique was applied to improve the bond strength of titanium (Ti) porcelain. ZrN coating was prepared by magnetron sputtering, and silica coating was processed by a sol-gel method. The treated surfaces of the specimens were analyzed by X-ray diffraction, and the Ti/porcelain interface was investigated by scanning electron microscopy (SEM) and energy dispersive spectroscopy. The coated specimens appeared fully coherent to the Ti substrate. The fractured bonding surface was also investigated by SEM. The residual porcelain on the metal surface could be observed in the ZrN group and silica group, but there was no obvious porcelain remaining in the control group. A three-point-bending test showed that the bonding strength of the ZrN group (45.99 ± 0.65 MPa) was higher than the silica group (37.77 ± 0.78 MPa) (P silica group was significantly higher than the control group (P ceramic surface with ZrN and silica coatings resulted in a stronger Ti/porcelain bond. ZrN coating by magnetron sputtering was a more effective way to improve the bond strength between Ti and porcelain compared with sol-gel processed silica coating in this study.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-01-15

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

  5. Pore characterisation and interconnectivity studies on bioactive 58 S sol-gel glass

    Energy Technology Data Exchange (ETDEWEB)

    Cook, R.; Watson, T.; Robinson, P. [Thomas Dental Inst., London (United Kingdom). Microscopy and Imaging Dept.; Fielder, E.; Hench, L.L. [Imperial Coll. of Science, Technology and Medicine, London (United Kingdom). Dept. of Materials

    2001-07-01

    The interconnecting pore network of bioactive 58S sol-gel glass is a vital structural characteristic requiring investigation, as in vivo this will provide the route of tissue fluid ingress and ultimately, the sites for early cell proliferation and osteogenesis. To characterise and visualise micropore (<20A) to macropore (>500A) dimension ranges, five complementary analytical methods were applied to 58S sol-gel monoliths, each resolving different characteristics of the pore network. Nitrogen porosimetry best resolved micro and smaller mesopores (20-500A), supplemented by helium ultra-pycnometry data. Mercury intrusion porosimetry was employed to characterise the meso and small macropores. SEM and confocal microscope imaging of the residual mercury within the matrix provided the first visual evidence of pores within the gel-glass interstices. The network's patency was clearly demonstrated by imaging fluorochrome-labelled command-set dental dentine bonding monomers, traversing the matrix. (orig.)

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

    Directory of Open Access Journals (Sweden)

    YASSUKO IAMAMOTO

    2000-03-01

    Full Text Available New materials porphyrinosilica and metalloporphyrinosilica template have been obtained by a sol-gel processing where functionalyzed porphyrins and metalloporphyrins "building blocks" were assembled into a three-dimensional silicate network. The optimized conditions for preparation of these materials are revised. The monomer precursors porphyrinopropylsilyl and metalloporphyrinopropylsilyl preparation reactions and subsequent one pot sol-gel processing with tetraethoxysilane are discussed. In the case of metalloporphyrins the nitrogen base coordinates to the central metal and acts as a template in the molecular imprinting technique. UV-visible absorption spectroscopy, thermogravimetric analysis, electron paramagnetic resonance, nuclear magnetic spectra, infrared spectra, luminescence spectra, surface area and electron spectroscopy imaging of the materials are used to characterize the prepared materials. The catalytic activities of these metalloporphyrinosilica- template are compared.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  9. Tunable erbium-doped microbubble laser fabricated by sol-gel coating

    CERN Document Server

    Yang, Yong; Kasumie, Sho; Xu, Linhua; Ward, Jonathan; Yang, Lan; Chormaic, Síle Nic

    2016-01-01

    In this work, we show that the application of a sol-gel coating renders a microbubble whispering gallery resonator into an active device. During the fabrication of the resonator, a thin layer of erbium-doped sol-gel is applied to a tapered microcapillary, then a microbubble with a wall thickness of 1.3 $\\mu$m is formed with the rare earth diffused into its walls. The doped microbubble is pumped at 980 nm and lasing in the emission band of the Er$^{3+}$ ions with a wavelength of 1535 nm is observed. The laser wavelength can be tuned by aerostatic pressure tuning of the whispering gallery modes of the microbubble. Up to 240 pm tuning is observed with 2 bar of applied pressure. It is shown that the doped microbubble could be used as a compact, tunable laser source. The lasing microbubble can also be used to improve sensing capabilities in optofluidic sensing applications.

  10. Whole Cell Imprinting in Sol-Gel Thin Films for Bacterial Recognition in Liquids: Macromolecular Fingerprinting

    Directory of Open Access Journals (Sweden)

    Robert Armon

    2010-03-01

    Full Text Available Thin films of organically modified silica (ORMOSILS produced by a sol-gel method were imprinted with whole cells of a variety of microorganisms in order to develop an easy and specific probe to concentrate and specifically identify these microorganisms in liquids (e.g., water. Microorganisms with various morphology and outer surface components were imprinted into thin sol-gel films. Adsorption of target microorganism onto imprinted films was facilitated by these macromolecular fingerprints as revealed by various microscopical examinations (SEM, AFM, HSEM and CLSM. The imprinted films showed high selectivity toward each of test microorganisms with high adsorption affinity making them excellent candidates for rapid detection of microorganisms from liquids.

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

    Directory of Open Access Journals (Sweden)

    F Esmaieli Ghodsi

    2012-03-01

    Full Text Available   Retraction Notice    The paper "Comparative study of ZnO thin films prepared by different sol-gel route" by H. Absalan and F. E. Ghodsi, which appeared in Iranian Journal of Physics Research, Vol. 11, No. 4, 423-428 (in Farsi is translation of the paper "Comparative Study of ZnO Thin Films Prepared by Different Sol-Gel Route" by F. E. Ghodsi and H. Absalan, which appeared in ACTA PHYSICA POLONICA A, Vol 118 (2010 (in English and for this reason is retracted from this journal.The corresponding author  (and also the first author is the only responsible person for this action.   

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

    Directory of Open Access Journals (Sweden)

    Faley Jean de Sousa

    2010-03-01

    Full Text Available The sol-gel process is very effective for the preparation of new materials with potential applications in optics, sensors, catalyst supports, coatings, and specialty inorganic polymers that can be used as hosts for the accommodation of organic molecules. The low temperature employed in the process is the main advantage of this methodology. In this work, the europium (III complex with 1,10-phenantroline was prepared, and this luminescent complex was incorporated into silica nanoparticles and films by the sol-gel process. The nanoparticles were obtained by the modified Stöber methodology. The films were obtained by the dip-coating technique, at different deposition rates and numbers of layers. The nanoparticles and films were characterized by photoluminescence, thermal analysis, and Raman and infrared spectroscopies. Characterization revealed that the europium (III complex was not affected upon incorporation into the nanoparticles and films, opening a new field for the application of these materials.

  13. Photonic crystal patterning of luminescent sol-gel films for light extraction

    Energy Technology Data Exchange (ETDEWEB)

    Revaux, Amelie; Dantelle, Geraldine; Guillemot, Francois; Weisbuch, Claude; Boilot, Jean-Pierre; Gacoin, Thierry [Laboratoire de Physique de la Matiere Condensee, Ecole Polytechnique/CNRS UMR7643, F-91128 Palaiseau (France); Decanini, Dominique; Haghiri-Gosnet, Anne-Marie [Laboratoire de Photonique et Nanostructures, CNRS UPR20, F-91460 Marcoussis (France); Benisty, Henri, E-mail: amelie.revaux@polytechnique.edu [Laboratoire Charles Fabry de l' Institut d' Optique, CNRS, Universite Paris-Sud, Campus Polytechnique, RD 128, F-91127 Palaiseau Cedex (France)

    2011-09-07

    Structured luminescent thin films are investigated in the context of improved light extraction of phosphors for solid-state-lighting applications. Thin films composed of a sol-gel titania matrix doped with europium chelates are studied as a model system. These films, patterned with a square photonic lattice by soft nanoimprint lithography, are characterized by angle-resolved fluorescence. Modeling of this simple technique is shown to fit well the experimental data, revealing in great detail the guided modes of the film and their extraction parameters. An eightfold extraction enhancement factor of the film emission is measured. To further improve the extraction efficiency, we investigate the role of an additional low-index mesoporous silica underlayer through its influence on the guided modes of different polarizations and their interactions with the photonic crystal. Results obtained on model systems open the way towards the optimization of light-emitting devices, using a strategy of dielectric microstructure engineering using the sol-gel process.

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

    Science.gov (United States)

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

    2004-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Raghu, P., E-mail: dpr3270@gmail.com; Naveen, C. S.; Shailaja, J.; Mahesh, H. M., E-mail: hm-mahesh@rediffmail.com [Thin Film and Solar Cell Laboratory, Department of Electronic Science, Bangalore University, Jnanabharathi, Bangalore -560056 (India)

    2016-05-06

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Hou Aiqin, E-mail: aiqinhou@dhu.edu.c [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China); Chen Huawei [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China)

    2010-03-15

    The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Ridhi, R.; Gawri, Isha; Abbas, Saeed J.; Saini, G. S. S.; Tripathi, S. K. [Department of Physics, Center of Advanced Study in Physics, Panjab University, Chandigarh-160 014 (INDIA) Fax: +91-172-2783336; Tel.:+91-172-2544362 (India)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, M., E-mail: michelina.catauro@unina2.it [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Papale, F. [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Sapio, L.; Naviglio, S. [Department of Biochemistry, Biophysics and General Pathology, Second University of Naples, Via L. De Crecchio 7, 80138 Naples (Italy)

    2016-08-01

    The objective of this work has been to develop low temperature sol-gel glass coatings to modify the substrate surface and to evaluate their bioactivity and biocompatibility. Glasses, based on SiO{sub 2}·CaO·P{sub 2}O{sub 5}, were synthesized by the sol-gel technique using tetraethyl orthosilicate, calcium nitrate tetrahydrate and triethyl phosphate as precursors of SiO{sub 2}, CaO and P{sub 2}O{sub 5}, respectively. Those materials, still in the sol phase, have been used to coat substrates by means of the dip-coating technique. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) has been used for characterize coatings and a microstructural analysis has been obtained using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated substrate was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. In order to study the cell behavior and response to our silica based materials, prepared via the sol-gel method, with various Ca/P ratio and coating substrate, we have used the human osteoblast-like U2OS cell line. - Highlights: • Coatings consisting of SiO{sub 2}·CaO·P{sub 2}O{sub 5} glasses were prepared via sol-gel dip coating. • Ca/P molar ratio affects the film morphology and biocompatibility. • Higher cell proliferation was found in response to higher Ca/P ratios coatings. • A growth cell proliferation inhibition was observed in response to lower Ca/P ratio.

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

    Science.gov (United States)

    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.

  20. Fractal dimension determination of sol-gel powders using transmission electron microscopy images

    Energy Technology Data Exchange (ETDEWEB)

    Dobrescu, Gianina; Crisan, Maria; Zaharescu, Maria; Ionescu, N.I

    2004-09-15

    SiO{sub 2}, TiO{sub 2} and AlO(OH) powders obtained by the sol-gel method were investigated by transmission electron microscopy. The mass-radius relation was used to determine the fractal dimensions from the images. These fractal dimensions were corrected in order to obtain the powder fractal dimensions. The results indicate a good fractal behavior and high fractal dimensions.

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

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

  2. Direct measurement of piezoelectric properties of Sol-Gel PZT films

    NARCIS (Netherlands)

    Gardeniers, Johannes G.E.; Verholen, A.G.B.J.; Verholen, A.G.B.J.; Tas, Niels Roelof; Elwenspoek, Michael Curt

    1998-01-01

    PbZr0.53Ti0.47O3 films were deposited on Si-SiO2-Ta-Pt substrates via a conventional sol-gel procedure. Electrical properties of the films were: resistivity ca. 5 × 1011 Ωcm, relative dielectric permittivity 900-1100, remnant polarization ca. 20 μC/cm2, breakdown electric field larger than 50 MV/m.

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

    Directory of Open Access Journals (Sweden)

    Faure Joel

    2013-11-01

    Full Text Available In this work, the 45S5 bioactive glass has been prepared by the sol-gel process using an organic acid catalyst instead of nitric acid usually used. The physico-chemical and structural characterizations confirmed and validated the elemental composition of the resulting glass. In addition, the 45S5 bioactive glass powder thus obtained was successfully used to elaborate by electrophoretic deposition a prosthetic coating on titanium alloy Ti6Al4V.

  4. Optical chemical sensors based on hybrid organic-inorganic sol-gel nanoreactors.

    Science.gov (United States)

    Tran-Thi, Thu-Hoa; Dagnelie, Romain; Crunaire, Sabine; Nicole, Lionel

    2011-02-01

    Sol-gel porous materials with tailored or nanostructured cavities have been increasingly used as nanoreactors for the enhancement of reactions between entrapped chemical reactants. The domains of applications issued from these designs and engineering are extremely wide. This tutorial review will focus on one of these domains, in particular on optical chemical sensors, which are the subject of extensive research and development in environment, industry and health.

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

    OpenAIRE

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

    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 an...

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

    Science.gov (United States)

    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.

  7. Phase structure and thermal evolution in coating films and powders obtained by sol-gel process: Part II. ZrO{sub 2}{minus}2.5mole {percent} Y{sub 2}O{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Caruso, R.; Benavidez, E.; de Sanctis, O. [Laboratorio de Materiales Ceramicos, FCEIyA, IFIR, Av. Pellegrini 250, 2000 Rosario (Argentina); Caracoche, M.C.; Rivas, P.C. [Programa TENAES, Departamento de Fisica, FCE, Universidad Nacional de La Plata, c.c. 67, 1900 La Plata (Argentina); Cervera, M. [Departamento de Ciencia y Tecnologia, Universidad Nacional de Quilmes, R.S. 184, 1864 Bernal (Argentina); Caneiro, A.; Serquis, A. [Centro Atomico Bariloche, CNEA, 8400 Bariloche (Argentina)

    1997-10-01

    Powders and coatings of zirconia doped with 2.5 mole {percent} yttria have been produced via the sol-gel route. The phase structure and subsequent thermal evolution in heating and cooling cycles have been investigated using mainly perturbed angular correlations spectroscopy. Thermal analyses and XRD as a function of temperature have also been performed to obtain complementary information. Upon heating, the amorphous gels crystallized into the tetragonal structure and showed the same hyperfine pattern and thermal behavior as observed in tetragonal zorconia obtained by the ceramic route: the two configurations vacancies around zirconium ions denoted as t{sub 1} and t{sub 2} forms and their mutual t{sub 1}{r_arrow}t{sub 2} transformation. While the powder sample exhibited an incipient thermal instability above 1000{degree}C and underwent completely the t{sub 2} form to m{endash}ZrO{sub 2} transition during subsequent, gradual cooling below 500{degree}C, the coating retained the tetragonal phase within the whole temperature range investigated. Hyperfine results suggest that the tetragonal phase stabilization is favored by the highly defective nature of the t{sub 1} form and consequently hardened by the availability of oxygen. The PAC derived activation energy for the fast diffusion of the oxygen vacancies inherent to the t{sub 2} form was determined as 0.54{plus_minus}0.14eV. {copyright} {ital 1997 Materials Research Society.}

  8. Sol-gel derived nanoparticles of Zn substituted lithium ferrite (Li{sub 0.32}Zn{sub 0.36}Fe{sub 2.32}O{sub 4}): magnetic and Moessbauer effect measurements and their theoretical analysis

    Energy Technology Data Exchange (ETDEWEB)

    Sutradhar, S. [Department of Physics, Jadavpur University, Jadavpur, Kolkata 700032 (India); Solid State Research Laboratory, Department of Physics, Burdwan University, Burdwan,West Bengal 713104 (India); Pati, S. [UGC-DAE Consortium for Scientific Research, III/LB-8, Kolkata 700092 (India); Acharya, S. [Solid State Research Laboratory, Department of Physics, Burdwan University, Burdwan,West Bengal 713104 (India); Das, S. [Department of Physics, Jadavpur University, Jadavpur, Kolkata 700032 (India); Das, D. [UGC-DAE Consortium for Scientific Research, III/LB-8, Kolkata 700092 (India); Chakrabarti, P.K., E-mail: pabitra_c@hotmail.com [Solid State Research Laboratory, Department of Physics, Burdwan University, Burdwan,West Bengal 713104 (India)

    2012-04-15

    Nanoparticles of Zn substituted lithium ferrite (Li{sub 0.32}Zn{sub 0.36}Fe{sub 2.32}O{sub 4}) have been prepared by a sol-gel method where the ultra-sonication technique has been adopted to reduce the agglomeration effect among the nanoparticles. The samples were heat-treated at three different temperatures and the formation of the nanocrystalline phase was confirmed by X-ray diffractograms (XRD). The average particle size of each sample has been estimated from the (311) peak of the XRD pattern using the Debye-Scherrer formula and the average sizes are in the range of 10-21 nm. The average particle size, crystallographic phase, etc. of some selected samples obtained from the high-resolution transmission electron microscopy are in agreement with those estimated from the XRD patterns. Static magnetic measurements viz., hysteresis loops, field cooled and zero field cooled magnetization versus temperature curves of some samples carried out by SQUID in the temperature range of 300 to 5 K clearly indicate the presence of superparamagnetic (SPM) relaxation of the nanoparticles in the samples. The maximum magnetization of the SPM sample annealed at 500 Degree-Sign C is quite high (68 Am{sup 2}/Kg) and the hysteresis loops are almost square shaped with very low value of coercive field at room temperature (827.8 A/m). The particle size, magneto-crystalline anisotropy, etc. have been estimated from the detailed theoretical analysis of the static magnetic data. The dynamic magnetic behavior of the samples was also investigated by observing the ac hysteresis loops and magnetization versus field curves with different time windows at room temperatures. The different soft magnetic quantities viz., coercive field, magnetization, remanance, hysteresis losses, etc. were extracted from dynamic measurements. Dynamic measurements confirmed that the samples are in their mixed state of SPM and ordered ferrimagnetic particles, which is in good agreement with the results of static magnetic

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

    Science.gov (United States)

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

    2017-11-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Gutierrez, J; Tercjak, A; Garcia, I; Peponi, L; Mondragon, I [' Materials-Technologies' Group, Departamento Ingenieria Quimica y Medio Ambiente, Escuela Politecnica, Universidad PaIs Vasco/Euskal Herriko Unibertsitatea, Plaza Europa 1, E-20018 Donostia-San Sebastian (Spain)], E-mail: inaki.mondragon@ehu.es

    2008-04-16

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

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

    Science.gov (United States)

    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.

  12. Methane combustion of Pd/SiO{sub 2} sol gel catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Pecchi, G.; Reyes, P.; Concha, I. [Univ. de Concepcion (Chile). Facultad de Ciencias Quimicas; Fierro, J.L.G. [CSIC, Madrid (Spain). Inst. de Catalisis y Petroleoquimica

    1998-10-01

    Surface properties and catalytic activity changes of Pd/SiO{sub 2} catalysts prepared by sol-gel processing have been investigated by evaluating the specific surface area, porosity, metal dispersion, surface acidity, and surface composition. As a comparison, Pd/SiO{sub 2} catalysts prepared by impregnation of SiO{sub 2} obtained by the sol-gel method were also studied. Both series of catalysts were tested in cycles of methane combustion. It has been found that the pH of gelation modifies strongly the porosity and surface area of the catalysts. However, no significant changes were observed in the metal dispersion. XPS results showed that for the catalysts obtained by the sol-gel procedure the Pd/Si surface atomic ratio does not change before or after the combustion cycle. However, in those catalysts prepared by the impregnation method, a significant decrease in the Pd/Si ratio was observed. The catalytic activity in the methane combustion under stoichiometric mixture of diluted CH{sub 4}/O{sub 2} was studied at different temperatures from 473 K up to the temperature required for a total conversion of all the catalysts. It was found that the activity is higher after their use in the catalytic reaction. This behavior is attributed to the presence of Pd{sub {delta}+} species which improve the catalytic activity.

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

    Science.gov (United States)

    Yadav, Reeta

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

  14. Improvement in Tensile Strength of Bamboo Knitted Fabric by Sol-Gel Coating

    Directory of Open Access Journals (Sweden)

    Awais Khatri

    2013-07-01

    Full Text Available Textiles made of bamboo regenerated fibre are reported to have lower tensile strength than the other cellulosic fibres, due to high porosity of the fibre. This paper was aimed to modify the bamboo knitted fabric by the sol-gel coating to improve the tensile strength with minimum effect on its inherent morphology and ultimate relevant properties such as good absorbency and air permeability. The paddry- bake process was employed for the coating where tetraethyl-orthosilicate and nano-titanium-dioxide were used as the active ingredients. The treated fabrics were tested for the tensile behaviour in terms of breaking strength and elongation and the sol-gel process recipe and parameters were optimised. The absorbency, air-permeability and washing durability of the coating were also tested for the optimised process. Results showed the increase in tensile strength of the fabric by sol-gel coating, whereas absorbency and air-permeability were almost unaffected. The coating results were unaffected even after a washing treatment (equivalent to 5 industrial washings. Additionally, the wrinkle recovery angle of the coated fabric was also tested and found improved.

  15. Advancement in corrosion resistance of AA 2024-T3 through sol-gel coatings including nanocontainers

    Directory of Open Access Journals (Sweden)

    Kartsonakis Ioannis A.

    2017-01-01

    Full Text Available The current study investigates the effect of nanocontainers incorporation into sol-gel coatings for the protection improvement of aluminium alloys 2024-T3 against corrosion. The nanocontainers were synthesized via a combination of radical polymerization process and sol-gel technique. They consist of cerium and molybdenum oxides and loaded with the anodic corrosion inhibitor 2-mercaptobenzothiazole (MBT. The preparation of the coating matrix was accomplished using (3-glycidoxypropyltrimethoxysilane as precursor. These organic modified silicate based sol-gel films were evaluated for their corrosion behaviour as well as nanomechanical properties using electrochemical and nanoindentation techniques, respectively. The results reveal that the presence of loaded nanocontainers improved the corrosion protection of the coatings; outcome that can be attributed to either the increase coherence of the coating or the simultaneously inhibition action of cerium and molybdate ions together with the corrosion inhibitor MBT. Moreover, the addition of nanocontainers empty or loaded with inhibitor amount strengthens (increase of wear resistance the coating and decreases the coefficient of friction.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Directory of Open Access Journals (Sweden)

    Roland Himmelhuber

    2015-07-01

    Full Text Available 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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Wang, Yazi; Wang, Renlin; Habib, Eric; Wang, Ruili; Zhang, Qinghong; Sun, Bin; Zhu, Meifang

    2017-05-01

    In this study, quartz fibres (QFs) surface modification using a sol-gel method was proposed and dental posts reinforced with modified QFs were produced. A silica sol (SS) was prepared using tetraethoxysilane (TEOS) and 3-methacryloxypropyltrimethoxysilane (γ-MPS) as precursors. The amount of γ-MPS in the sol-gel system was varied from 0 to 24wt.% with a constant molar ratio of TEOS, ethanol, deionized water, and HCl. Thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), and contact angle (CA) measurements were used to characterize the modified QFs, which confirmed that SS had successfully coated the surface of QFs. SEM images showed good interfacial bonding between the modified QFs and the resin matrix. The results of three-point bending tests of the fibre reinforced composite (FRC) posts showed that the QFs modified by SS with 12wt.% γ-MPS presented the best mechanical properties, demonstrating improvements of 108.3% and 89.6% for the flexural strength and flexural modulus, respectively, compared with untreated QFs. Furthermore, the sorption and solubility of the prepared dental posts were also studied by immersing the posts in artificial saliva (AS) for 4weeks, and yielded favourable results. This sol-gel surface modification method promises to resolve interfacial bonding issues of fibres with the resin matrix, and produce FRC posts with excellent properties. Copyright © 2017. Published by Elsevier B.V.

  20. Recuperación de sílice residual de columnas de cromatografía en la síntesis sol-gel de pigmentos

    Directory of Open Access Journals (Sweden)

    Grañana, M. C.

    2000-04-01

    Full Text Available The use of a silica waste of support chromatography process as raw material in the synthesis of ceramic pigments based in zircon network (yellow of praseodymium, turkish blue of vanadium and pink koral of iron, is analized in this study. The synthesis has been carried out by ceramic method and also by colloidal sol-gel and coprecipitation routes. Silica waste becomes an effective precursor in the zircon ceramic stains. Likewise, the high temperature and long soaking time used in the synthesis ensure the whole combustion of adsorbed organics on the waste.

    En este trabajo se caracteriza una sílice residual de procesos de cromatografía de columna y se analiza su utilización como precursor en la síntesis de los tres pigmentos triaxiales del circón (amarillo de praseodimio, turquesa de vanadio y coral de hierro utilizando tanto la vía sol-gel coloidal, la coprecipitación y el método cerámico. La sílice residual se muestra como un precursor muy efectivo en la obtención de los colores del circón tanto vía cerámica como a partir de geles. La alta temperatura así como los relativamente largos periodos de retención utilizados en la síntesis de los pigmentos cerámicos, permite una total combustión de los orgánicos adsorbidos sobre la sílice.

  1. A sol-gel-integrated protein array system for affinity analysis of aptamer-target protein interaction.

    Science.gov (United States)

    Ahn, Ji-Young; Kim, Eunkyung; Kang, Jeehye; Kim, Soyoun

    2011-06-01

    A sol-gel microarray system was developed for a protein interaction assay with high activity. Comparing to 2-dimensional microarray surfaces, sol-gel can offer a more dynamic and broad range for proteins. In the present study, this sol-gel-integrated protein array was used in binding affinity analysis for aptamers. Six RNA aptamers and their target protein, yeast TBP (TATA-binding protein), were used to evaluate this method. A TBP-containing sol-gel mixture was spotted using a dispensing workstation under high-humidity conditions and each Cy-3-labeled aptamer was incubated. The dissociation constants (K(d)) were calculated by plotting the fluorescent intensity of the bound aptamers as a function of the TBP concentrations. The K(d) value of the control aptamer was found to be 8 nM, which agrees well with the values obtained using the conventional method, electric mobility shift assay. The sol-gel-based binding affinity measurements fit well with conventional binding affinity measurements, suggesting their possible use as an alternative to the conventional method. In addition, aptamer affinity measurements by the sol-gel-integrated protein chip make it possible to develop a simple high-throughput affinity method for screening high-affinity aptamers.

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

    Directory of Open Access Journals (Sweden)

    Moran Shalev

    2011-02-01

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

  3. Investigation of Sol-Gel coatings exposed in the condenser at Fynsvaerket. Part 3

    Energy Technology Data Exchange (ETDEWEB)

    Montgomery, M. [DTU Mekanik, Kgs. Lyngby (Denmark); Vilhelmsen, T. [Vattenfall Heat Nordic, Copenhagen (Denmark)

    2009-05-15

    The Danish Technological Institute (DTI) has developed a technique using Hybrid Solgel nanotechnology to produce coatings which can change the surface characteristics of various components. It is the purpose of this project to investigate where such coatings can be utilised in the power generating industry with respect to fouling and corrosion resistance. The initial results with sol-gel coatings on the condenser tubes at Fysnvaerket showed that due to the presence of corrosion products on the unexposed tubes which influences the adherence and protectiveness of coatings applied, the effect of sol-gel coatings was difficult to assess. Further specimens were tested where the outer surface had been mechanically cleaned by sand blasting or by grinding and polishing. The results of 3 months exposure in the condenser plate at the outlet (hottest part of condenser) has been reported. Many coatings showed the anti-fouling effect, however closer inspection with scanning electron microscopy revealed cracks in the coating and oxide below the coating indicating the coating was permeable to corrosive species. The specimens described in this report are from the cold side of the condenser after 1 year's exposure. Due to lack of time, the assessment is based on visual assessment and light optical microscopy. Two different sol-gel coatings have been applied to brass and titanium condenser tubes about 10 cm in length. Based on the experience from previous exposures, the surface of the condenser tubes was mechanically cleaned before coating with the sol-gel components. One set was sandblasted and the other set was grinded to a polished finish using sandpaper. The specimens grinded and polished were exposed tubes that had been removed from the condenser. Investigations of unexposed cleaned condenser tubes with and without sol-gel have been reported previously. Before application of the coatings, the tubes were mechanically cleaned either by sandblasting or by grinding to a

  4. Sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) electrogenerated chemiluminescence sensor for high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Han Nim [Department of Chemistry and Center for Bioactive Molecular Hybrids, Yonsei University, Seoul 120-749 (Korea, Republic of); Cho, Sung-Hee [Department of Chemistry and Center for Bioactive Molecular Hybrids, Yonsei University, Seoul 120-749 (Korea, Republic of); Park, Yu-Jin [Department of Chemistry and Center for Bioactive Molecular Hybrids, Yonsei University, Seoul 120-749 (Korea, Republic of); Lee, Dai Woon [Department of Chemistry and Center for Bioactive Molecular Hybrids, Yonsei University, Seoul 120-749 (Korea, Republic of); Lee, Won-Yong [Department of Chemistry and Center for Bioactive Molecular Hybrids, Yonsei University, Seoul 120-749 (Korea, Republic of)]. E-mail: wylee@yonsei.ac.kr

    2005-06-13

    The sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy){sub 3} {sup 2+}] electrogenerated chemiluminescence (ECL) sensor was applied to the reversed-phase high-performance liquid chromatography (HPLC) determination of phenothiazine derivatives (promazine, chlorpromazine, triflupromazine, thioridazine, and trifluoperazine) and erythromycin in human urine samples. In this method, Ru(bpy){sub 3} {sup 2+} was immobilized in sol-gel-derived titania (TiO{sub 2})-Nafion nanocomposite films coated on a dual platinum electrode. This method eliminates an extra pump needed for the delivery of Ru(bpy){sub 3} {sup 2+} reagent into a reaction/observation zone in front of photomultiplier tube because the immobilized-Ru(bpy){sub 3} {sup 2+} is recycled on the electrode surface by an applied potential at +1.3 V versus Ag/AgCl (3 M NaCl) reference electrode. The resulting analytical performances such as detection limit, working range, sensitivity, and measurement precision were slightly worse than those obtained with the conventional post-column Ru(bpy){sub 3} {sup 2+} addition approach. The lack of significant interferences and the low detection limits for phenothiazine derivatives and erythromycin indicate that the proposed HPLC-Ru(bpy){sub 3} {sup 2+} ECL detection method is suitable for the determination of those compounds in biological fluids.

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

    Energy Technology Data Exchange (ETDEWEB)

    Tirado G, S.; Olvera A, R., E-mail: tirado@esfm.ipn.mx [IPN, Escuela Superior de Fisica y Matematicas, Edificio 9, Unidad Profesional A. L. M., San Pedro Zacatenco, 07788 Mexico D. F. (Mexico)

    2014-08-15

    Zn O films and those superficially modified with chromium were deposited on substrates of soda-lime glass, using the Sol-Gel process and the repeated immersion method. Starting from dehydrated zinc acetate was prepared a solution to 0.6 M to ambient temperature in 2-methoxyethanol and monoethanolamine (Mea) stirring magnetically. The Sol was prepared with an aging to seven days and was used to grow a films group with thickness to eight immersions. These same films were superficially modified with several depositions of a chromium nitrate Sol dissolved in ethanol to low concentration. The Zn O films were structurally characterized by X-ray diffraction, its chemical composition by energy dispersive X-ray spectroscopy and its morphology by scanning electron microscopy and atomic force microscopy, as well as their optical properties by UV-vis. Of the obtained results are proposed possible applications. (author)

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

    Science.gov (United States)

    Tran, MinhPhuong; Turner, Erica B; Segro, Scott S; Fang, Li; Seyyal, Emre; Malik, Abdul

    2017-11-03

    A sol-gel organic-inorganic hybrid sorbent, consisting of chemically integrated tantalum (V) ethoxide (TaEO) and polypropylene glycol methacrylate (PPGM), was developed for capillary microextraction (CME). The sol-gel sorbent was synthesized within a fused silica capillary through hydrolytic polycondensation of TaEO and chemical incorporation of PPGM into the evolving sol-gel tantala network. A part of the organic-inorganic hybrid sol-gel network evolving in the vicinity of the capillary walls had favorable conditions to get chemically bonded to the silanol groups on the capillary surface forming a surface-bonded coating. The newly developed sol-gel sorbent was employed to isolate and enrich a variety of analytes from aqueous samples for on-line analysis by high-performance liquid chromatography (HPLC) equipped with a UV detector. CME was performed on aqueous samples containing trace concentrations of analytes representing polycyclic aromatic hydrocarbons, ketones, alcohols, amines, nucleosides, and nucleotides. This sol-gel hybrid coating provided efficient extraction with CME-HPLC detection limits ranging from 4.41pM to 28.19 pM. Due to direct chemical bonding between the sol-gel sorbent coating and the fused silica capillary inner surface, this sol-gel sorbent exhibited enhanced solvent stability. The sol-gel tantala-based sorbent also exhibited excellent pH stability over a wide pH range (pH 0-pH 14). Furthermore, it displayed great performance reproducibility in CME-HPLC providing run-to-run HPLC peak area relative standard deviation (RSD) values between 0.23% and 3.83%. The capillary-to-capillary RSD (n=3), characterizing capillary preparation method reproducibility, ranged from 0.24% to 4.11%. The results show great performance consistency and application potential for the sol-gel tantala-PPGM sorbent in various fields including biomedical, pharmaceutical, and environmental areas. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2015-02-01

    In this paper a new sol-gel approach was explored for the synthesis of the 45S5 bioactive glass. We demonstrate that citric acid can be used instead of the usual nitric acid to catalyze the sol-gel reactions. The substitution of nitric acid by citric acid allows to reduce strongly the concentration of the acid solution necessary to catalyze the hydrolysis of silicon and phosphorus alkoxides. Two sol-gel powders with chemical compositions very close to that of the 45S5 were obtained by using either a 2M nitric acid solution or either a 5mM citric acid solution. These powders were characterized and compared to the commercial Bioglass®. The surface properties of the two bioglass powders were assessed by scanning electron microscopy (SEM) and by Brunauer-Emmett-Teller method (BET). The Fourier transformed infrared spectroscopy (FTIR) and the X-ray diffraction (XRD) revealed a partial crystallization associated to the formation of crystalline phases on the two sol-gel powders. The in vitro bioactivity was then studied at the key times during the first hours of immersion into acellular Simulated Body Fluid (SBF). After 4h immersion into SBF we clearly demonstrate that the bioactivity level of the two sol-gel powders is similar and much higher than that of the commercial Bioglass®. This bioactivity improvement is associated to the increase of the porosity and the specific surface area of the powders synthesized by the sol-gel process. Moreover, the nitric acid is efficiently substituted by the citric acid to catalyze the sol-gel reactions without alteration of the bioactivity of the 45S5 bioactive glass. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Literature Review of Polymer Derived Ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Peterson, Reuben James [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-05-25

    Polymer Derived Ceramics (PDCs), also known as preceramic polymers, are valuable coating agents that are used to produce surface barriers on substrates such as stainless steel. These barriers protect against a multitude of environmental threats, and have been used since their research and development in 19772. This paper seeks to review and demonstrate the remarkable properties and versatility that PDCs have to offer, while also giving a brief overview of the processing techniques used today.

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

    Science.gov (United States)

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

    2017-10-18

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Jameel, Zainab N., E-mail: zeinb76-alrekbe@yahoo.com; Haider, Adawiya J., E-mail: adawiyahaider@yahoo.com [Nanotechnology and Advanced Materials Research Center, The University of Technology, Baghdad (Iraq); Taha, Samar Y., E-mail: samarjam2002@yahoo.com [College of Science for Women, University of Baghdad, Baghdad (Iraq); Gangopadhyay, Shubhra, E-mail: gangopadhyays@missouri.edu; Bok, Sangho, E-mail: BokSa@missouri.edu [Department of Electrical and Computer, University of Missouri, Engineering, Building West, Columbia, Missouri 65211 (United States)

    2016-07-25

    A coating with self-cleaning characteristics has been developed using a TiO{sub 2}/SiO{sub 2} hybrid sol-gel, TiO{sub 2} nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO{sub 2} nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO{sub 2} nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO{sub 2} phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO{sub 2} NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

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

    Science.gov (United States)

    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.

  12. One- and three-dimensional growth of hydroxyapatite nanowires during sol-gel-hydrothermal synthesis.

    Science.gov (United States)

    Costa, Daniel O; Dixon, S Jeffrey; Rizkalla, Amin S

    2012-03-01

    Nanoscale hydroxyapatite (HA) is an optimal candidate biomaterial for bone tissue engineering because of its bioactive and osteoconductive properties. In this study, micro- and nanoscale HA particles with rod- and wirelike morphology were synthesized by a novel sol-gel-hydrothermal process. Sol-gel chemistry was used to produce a dry gel containing amorphous calcium phosphate (ACP), which was used as a precursor material in a hydrothermal process. The sol-gel-hydrothermal products were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) to determine particle morphology, crystal structure, and the presence of chemical functional groups. A pure HA crystal was synthesized, which underwent both one- and three-dimensional growth, resulting in tunable microrod and nanorod, and wire morphologies. The effects of solution pH and reaction time on particle diameter and length were assessed. Particle diameter ranged from 25 to 800 nm and decreased with an increase in solution pH, whereas both particle length and diameter increased as the hydrothermal process was prolonged. Nanowire HA powders (10-50 wt %) were mixed with poly(ε-caprolactone) (PCL) to produce PCL/HA composites. Fracture surfaces of PCL/HA composites showed a well-dispersed and homogeneous distribution of HA nanowires within the PCL matrix. Mechanical testing revealed a significant (p < 0.05) increase in the Young's and compressive moduli of PCL/HA composites compared to PCL alone, with 50 wt % HA producing a 3-fold increase in Young's modulus from 193 to 665 MPa and 2-fold increase in compressive modulus from 230 to 487 MPa. These HA nanowires can be used to reinforce polymer composites and are excellent biomaterials for tissue engineering of bone. © 2012 American Chemical Society

  13. Thermal properties and water repellency of cotton fabric prepared through sol-gel method

    Directory of Open Access Journals (Sweden)

    Gu Jia-Li

    2016-01-01

    Full Text Available Cotton fabrics were treated by one-step sol-gel method. The pure silica hydrosol and phosphorus-doped hydrosol were prepared with the addition of a hydrophobic hexadecyltrimethoxysilane to decrease the surface energy of cotton fabric. The thermal properties and water repellency of treated cotton fabric were characterized by thermo-gravimetric analysis, micro combustion, limiting oxygen index, and contact angle measurement. The results showed that cotton fabric treated by phosphorus-doped silica hydrosol had excellent flame retardance, and the water repellence was apparently improved with the addition of hexadecyltrimethoxysilane.

  14. KINETICS OF GRAIN-GROWTH OF YTTRIUM ALUMINUM GARNET FIBERS PREPARED BY SOL-GEL METHOD

    Directory of Open Access Journals (Sweden)

    Tan H.

    2013-12-01

    Full Text Available The yttrium aluminum garnet (YAG long fibers were prepared by the sol-gel method using aluminum chloride, aluminum powder, yttrium oxide and acetic acid as raw materials. The grain growth law is given by Dn – D0n = Kt (D0 = initial grain size, D = average grain size at time t, n = grain growth exponent and K = reaction constant. The grain growth exponent and activation energy of YAG fibers are ≈ 3 and 200 kJ/mol, respectively. The grain-growth behaviors of YAG were influenced by experimental conditions such as raw materials, initial particle size, initial particle distribution, etc.

  15. Novel Materials through Non-Hydrolytic Sol-Gel Processing: Negative Thermal Expansion Oxides and Beyond

    Directory of Open Access Journals (Sweden)

    Cora Lind

    2010-04-01

    Full Text Available Low temperature methods have been applied to the synthesis of many advanced materials. Non-hydrolytic sol-gel (NHSG processes offer an elegant route to stable and metastable phases at low temperatures. Excellent atomic level homogeneity gives access to polymorphs that are difficult or impossible to obtain by other methods. The NHSG approach is most commonly applied to the preparation of metal oxides, but can be easily extended to metal sulfides. Exploration of experimental variables allows control over product stoichiometry and crystal structure. This paper reviews the application of NHSG chemistry to the synthesis of negative thermal expansion oxides and selected metal sulfides.

  16. Synthesis of CoFe 2O 4 nanowire arrays by sol-gel template method

    Science.gov (United States)

    Ji, Guangbin; Tang, Shaolong; Xu, Baolong; Gu, Benxi; Du, Youwei

    2003-10-01

    CoFe 2O 4 nanowire arrays with an average diameter of about 40 nm were prepared in porous anodic aluminum oxide (AAO) template using sol-gel process. Transmission electron microscopy (TEM) diffraction pattern and X-ray diffraction (XRD) showed that the nanowires were polycrystalline phase. Magnetic measurements showed the arrays of nanowires did not show a preferential magnetic orientation, the reason was briefly discussed. The effect of heating rate on the structure and magnetic properties of CoFe 2O 4 nanowire arrays was investigated. The result showed that the coercivity decreased with the increase of the heating rate.

  17. Preparasi Polimer Hibrid dengan Metode Sol-Gel dan Penerapannya untuk Komponen Mikro-Optik

    Directory of Open Access Journals (Sweden)

    Pina Pitriana

    2016-12-01

    Full Text Available Polimer hibrid merupakan gabungan antara polimer organik dan anorganik. Penggabungan tersebut diharapkan akan menghasilkan sifat unggul dari bahan organik dan anorganik yang dapat dimanfaatkan untuk aplikasi. Polimer hibrid dapat digunakan untuk membuat pola dalam aplikasi mikro optik seperti pandu gelombang. Dalam penelitian ini dibuat variasi film tipis polimer hibrid dengan variasi konsentrasi berat fotoinisiator dan termoinisiator, selain itu dibuat pola pandu gelombang dengan proses fotopolimerisasi. Pembuatan polimer hibrid dilakukan dengan metode sol-gel dan fotopolimerisasi. Proses sol-gel menghasilkan rantai polimer anorganik, sedangkan proses fotopolimerisasi menghasilkan rantai polimer organik. Setelah proses fotopolimerisasi, rantai organik dan anorganik akan berikatan silang (cross-linking. Spektrum reflektansi dari film tipis polimer hibrid sebelum, sesudah fotopolimerisasi dan setelah post-bake terdapat perbedaan fasa gelombang yang menunjukkan perbedaan ketebalan film. Sampel dengan variasi konsentrasi berat Irgacure 819 sebesar 0,3%wt dan 2%wt mengalami penyusutan volume film masing-masing 2,44% dan 4,93%. Sampel dengan penambahan variasi konsentrasi berat Dicumyl peroxide sebesar 1%wt dan 10%wt mengalami penyusutan volume film masing-masing 8,34% dan 5,83%. Pola pandu gelombang dihasilkan dengan proses fotopolimerisasi yang diikuti dengan proses etching, menghasilkan pandu gelombang dengan bentuk struktur kanal persegi yang baik dan tidak terputus-putus. Hal tersebut mengindikasikan proses polimerisasi rantai organik telah berjalan dengan baik dan dapat bertahan setelah dilakukan etching. Hybrid polymer is composite between organic and inorganic polymer. This composite could make good properties from organic and inorganic which can be used for applications. Hybrid polymer can be used as photo-patternable material to produce micro-optical components like waveguide. In this work, weight concentration of photoinitiator and

  18. Characterization of protective sol-gel coatings on magnesium based on phenyl-triethoxysilane precursor

    Energy Technology Data Exchange (ETDEWEB)

    Yekehtaz, M., E-mail: yekehtaz@ca.tu-darmstadt.d [Technische Universitaet Darmstadt, Department of Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany); Sittner, F.; Ugas-Carrion, R.; Flege, S.; Broetz, J.; Ensinger, W. [Technische Universitaet Darmstadt, Department of Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany)

    2010-07-01

    Sol-gel coatings were deposited from a Phenyl-triethoxysilane precursor for corrosion protection on magnesium samples. Film porosity was measured with potentiodynamic scans and the coating's structure was characterized with secondary ion mass spectrometry and X-ray diffraction analysis. At the interface between substrate and coating a magnesium silicate layer was found which was formed by interdiffusion during the deposition process. The coated samples showed a good corrosion resistance and low porosity after heating at comparatively low temperature.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-03-01

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

  20. Rheological model for sol-gel phase transition of thermo-aged heavy oil fractions

    Directory of Open Access Journals (Sweden)

    Xiomara Andrea Vargas Arenas

    2010-01-01

    Full Text Available A power-law rheological model is proposed in this paper: G’’ (ω ∼ ωn and G’ (ω ~ ωn. It represents the increased connectivity between thermo-aged asphalt molecules in a rheo-reactor as one of the applications of systematic rheology. The results confirmed a sol-gel phase transition tendency for aged asphalt in the experimental frequency window at temperatures below 40°C. Such pattern could have been related to the structuring effect arising from the thermo-oxidative asphalt aging process during continuous agitation which has been suitably described by the micellar model of asphalt.

  1. Obtention of nanostructured silica glass by sol-gel process with incorporation of lead compounds

    Directory of Open Access Journals (Sweden)

    Ana Maria M. Santos

    1999-07-01

    Full Text Available The methodology of obtention of nanostructured glass, incorporated with lead compounds, obtained by sol-gel processing and the structural characterizations are presented. Specific surface area, porosity, pore morphology and pore size distributions of the gels were characterized with nitrogen sorption (BET and mercury pycnometry. The pore size distributions of gels obtained using lead nitrate were more narrow than the ones observed for gels made with lead acetate. It was also observed the presence of a bimodal pore size distribution for gels produced using lead nitrate.

  2. Sol-Gel Synthesis, X-Ray Diffraction Studies, and Electric Conductivity of Sodium Europium Silicate

    Directory of Open Access Journals (Sweden)

    Ekaterina V. Borisova

    2013-01-01

    Full Text Available Sodium europium silicate, NaEu9(SiO46O2, with apatite structure has been obtained and studied using X-ray diffraction and SEM. It has been shown that sodium sublimation does not take place upon synthesis by the sol-gel method. Rietveld refinement has revealed that sodium atoms are ordered and occupy the 4f position. O(4 atoms not related to silicate ions are placed at the centers of Eu(2 triangles. DC and AC electric conductivity and activation energy have been determined for the compound studied.

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

    Science.gov (United States)

    2015-10-19

    Report 3. DATES COVERED (From - To) 1 Jan 2009-31 Jul 2015 4. TITLE AND SUBTITLE Minimally Adhesive , Advanced Non-toxic Coatings of Dendrimeric...Technical Report for ONR N00014-09-1-0217 Minimally Adhesive , Advanced Non-toxic Coatings of Dendrimeric Catalysts in Sol-Gel Matrices Michael R. Detty, PI...PD Summary of Research Highlights Supported by ONR N00014-09-1-0217 1) Hydrophobie xerogel coatings are "robust" - good adhesion to glass, aluminum

  4. Effect of preparation conditions in sol-gel method on yellow phosphor with wide spectrum

    Directory of Open Access Journals (Sweden)

    Yenchen Lin

    2017-01-01

    Full Text Available Among several methods to obtain white light in light emitting diodes (LEDs, mixing blue light with yellow light excited by blue light is the most effective and economical method. However, the quality of white light achieved by this method is poor, making it essential to develop high-quality yellow phosphors. In this study, we synthesized yellow phosphors with broad spectral width by the sol-gel method and studied the effect of various synthetic conditions on their photoluminescence spectra. Consequently, we optimized synthesis conditions for a series of yellow phosphors and found that excess europium doping caused quenching and reduced the quantum yield.

  5. Magnetic Characterizations of Sol-Gel-Produced Mn-Doped ZnO

    Directory of Open Access Journals (Sweden)

    R. Asmatulu

    2010-01-01

    Full Text Available Nanoparticles of ZnO doped with 6 at.% Mn were produced by a sol-gel method. X-ray diffraction confirms the hexagonal structure as that of the parent compound ZnO, and high-resolution electron transmission microscopy reveals a single-crystallite lattice. Magnetic measurements using a superconducting quantum interference device indicate that about one half of the Mn2+ ions follow Curie's law for paramagnetism. The remaining Mn2+ ions exhibit a weak ferromagnetic character, which might be induced through canted antiferromagnetic interactions.

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

    Science.gov (United States)

    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.

  7. Construction of flame retardant coating on polyamide 6.6 via UV grafting of phosphorylated chitosan and sol-gel process of organo-silane.

    Science.gov (United States)

    Kundu, Chanchal Kumar; Wang, Xin; Hou, Yanbei; Hu, Yuan

    2018-02-01

    Phosphorylated chitosan (PCS) was synthesized and grafted onto the surface of polyamide 6.6 (PA 6.6) fabrics via UV-induced grafting polymerization in order to improve the flame retardant properties. Subsequently, PCS grafted PA 6.6 fabrics were modified by (3-aminopropyl) triethoxysilane (APTES) through sol-gel process in order to form a cross-linking coating. The results obtained from the vertical burning test indicated that only the PCS grafted and simultaneously sol-gel treated fabrics could stop the melt dripping. A maximum reduction (30%) in the peak heat release rate was achieved for the PA6.6-PCS-4W-SG fabric sample. The optimal flame retardant effect was achieved for the PA6.6 fabrics treated by PCS and APTES simultaneously, which was attributed to the joint effect of thermal shielding exerted by the silica and char-forming effect derived from PCS. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Preparation by Poly(Acrylic Acid) Sol-Gel Method and Thermoelectric Properties of γ-Na x CoO2 Bulk Materials

    Science.gov (United States)

    Li, Xiaoyu; Zhang, Li; Tang, Xinfeng

    2017-11-01

    γ-Na x CoO2 single-phase powders have been synthesized by a poly(acrylic acid) (PAA) sol-gel (SG) method, and γ-Na x CoO2 bulk ceramic fabricated using spark plasma sintering. The effects of the PAA concentration on the sample phase composition and morphology were investigated. The thermoelectric properties of the γ-Na x CoO2 bulk ceramic were also studied. The results show that the PAA concentration did not significantly affect the crystalline phase of the product. However, agglomeration of γ-Na x CoO2 crystals was suppressed by the steric effect of PAA. The Na x CoO2 bulk ceramic obtained using the PAA SG method had higher crystallographic anisotropy, better chemical homogeneity, and higher density than the sample obtained by solid-state reaction (SSR), leading to improved thermoelectric performance. The PAA SG sample had power factor (in-plane PF = σS 2) of 0.61 mW m-1 K-2 and dimensionless figure of merit ( ZT) along the in-plane direction of 0.19 at 900 K, higher than for the SSR sample (in-plane PF = 0.51 mW m-1 K-2, in-plane ZT = 0.17). These results demonstrate that a simple and feasible PAA SG method can be used for synthesis of Na x CoO2 ceramics with improved thermoelectric properties.

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

    Science.gov (United States)

    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.

  10. Microporous alumina ceramic membranes

    Science.gov (United States)

    Anderson, Marc A.; Sheng, Guangyao

    1993-01-01

    Several methods are disclosed for the preparation microporous alumina ceramic membranes. For the first time, porous alumina membranes are made which have mean pore sizes less than 100 Angstroms and substantially no pores larger than that size. The methods are based on improved sol-gel techniques.

  11. Sol-gel synthesis of quaternary (P2O5)55-(CaO)25-(Na2O)(20-x)-(TiO2) x bioresorbable glasses for bone tissue engineering applications (x = 0, 5, 10, or 15).

    Science.gov (United States)

    Foroutan, Farzad; Walters, Nick J; Owens, Gareth J; Mordan, Nicola J; Kim, Hae-Won; de Leeuw, Nora H; Knowles, Jonathan C

    2015-08-26

    In the present study, we report a new and facile sol-gel synthesis of phosphate-based glasses with the general formula of (P2O5)55-(CaO)25-(Na2O)(20-x)-(TiO2) x , where x = 0, 5, 10 or 15, for bone tissue engineering applications. The sol-gel synthesis method allows greater control over glass morphology at relatively low processing temperature (200 °C) in comparison with phosphate-based melt-derived glasses (~1000 °C). The glasses were analyzed using several characterization techniques, including x-ray diffraction (XRD), (31)P magic angle spinning nuclear magnetic resonance ((31)P MAS-NMR), Fourier transform infrared (FTIR) spectroscopy and energy-dispersive x-ray (EDX) spectroscopy, which confirmed the amorphous and glassy nature of the prepared samples. Degradation was assessed by measuring the ion release and pH change of the storage medium. Cytocompatibility was also confirmed by culturing osteoblast-like osteosarcoma cell line MG-63 on the glass microparticles over a seven-day period. Cell attachment to the particles was imaged using scanning electron microscopy (SEM) and confocal laser scanning microscopy (CLSM). The results revealed the potential of phosphate-based sol-gel derived glasses containing 5 or 10 mol% TiO2, with high surface area, ideal dissolution rate for cell attachment and easily metabolized dissolution products, for bone tissue engineering applications.

  12. Heat-treatment controlled structural and optical properties of sol-gel fabricated Eu:ZnO thin films

    Science.gov (United States)

    Ghosh, Subhabrata; Uma Mahendra Kumar, K.; Bhaktha, B. N. Shivakiran

    2017-02-01

    We report on the fabrication of sol-gel derived Eu-doped ZnO films and the effects of heat-treatment on their structural and optical properties. X-ray diffraction data analysis confirms the decrease in strain in the thin films with increasing heat-treatment temperatures, and the compressive stress of the samples is found to become tensile for heat-treatments between 650 °C and 800 °C. X-ray-absorption fine-structure spectra performed at the Eu L3-edge confirm the absence of clustering of Eu-ions. The photoluminescence (PL) spectra of undoped and doped films consist of near-band edge emissions along with the defect state emissions of ZnO. Intense red emission (612 nm) is observed under UV excitation attributed to the 5D0 →7F2 energy level transition of Eu3+ ions in the doped films. The elemental composition and the existence of Eu2+ as well as Eu3+ has been discussed with the help of X-ray photoelectron spectroscopy. ZnO → Eu3+ energy transfer has also been confirmed with the help of PL excitation spectra in these transparent ZnO thin films for applications in integrated optic devices operating in the UV-visible region.

  13. PPHASE AND MORPHOLOGY FORMATION OF Na DOPED PMN THIN FILMS PREPARED BY MODIFIED SOL-GEL METHOD

    Directory of Open Access Journals (Sweden)

    HELENA BRUNCKOVÁ

    2013-03-01

    Full Text Available Na doped lead magnesium niobate Pb(Mg1/3Nb2/3O3 (Na-PMN thin films of 100 nm thickness were prepared by modified sol-gel route with niobium precursor. Na-PMN films were deposited from sol derived using tartaric acid modified polymerizable complex method by mixing of Nb-tartarate (Pechini complex with Na, Pb and Mg acetates at 80°C with molar ratio of Na : Pb : Mg : Nb = 1/2 : 1 :1/3 : 2/3 on Pt/Al2O3 substrates by spin-coating method. In Na doped PMN film the perovskite Pb(Mg1/3Nb2/3O3 phase (65 vol. % and a small amount of pyrochlore Na2Nb8O21 phase were revealed after sintering at 650°C. In the microstructure of 2-layered Na-PMN/Pt/Al2O3 thin film, with ~9.5 nm of roughness, the bimodal particle distribution was observed with small spherical particles of pyrochlore phase and larger sponge-like particles of the perovskite phase. The smallest visible spherical particles (~30 nm and mutually interconected particles (~125 nm were found in TEM and AFM micrographs.

  14. ESTUDO DA IMOBILIZAÇÃO DE LIPASE EM SÍLICA OBTIDA PELA TÉCNICA SOL-GEL

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    Aline Matuella Moreira Ficanha

    2015-03-01

    Full Text Available The objective of this work was the immobilization of the enzyme Candida antarctica lipase B (CAL B using the sol-gel method of immobilization and three different initiators of the polymerization reaction: one acid (HCl, one basic (NH4OH and the other nucleophilic (HBr. Tetraethylorthosilicate was used as the silica precursor. The influence of the additive PEG 1500 on immobilization was assessed. The efficiency of the process was evaluated considering the esterification activity of the xerogels. The immobilization process provided enhanced thermal stability, storage and operational aspects relative to the free enzyme. Storage temperature proved one of the main variables to be considered in the process, with the xerogels stored under refrigeration showing better results in terms of residual activity (nearly 200 days with ≥ 90% residual activity of basic and nucleophilic xerogels when compared with storage at ambient temperature (nearly 40 days. The results demonstrated the possibility of reuse of derivatives and a greater number of cycles (nine, considering a residual activity of 50%.

  15. Evidence of organic luminescent centers in sol-gel-synthesized yttrium aluminum borate matrix leading to bright visible emission

    Energy Technology Data Exchange (ETDEWEB)

    Burner, Pauline; Salauen, Mathieu; Ibanez, Alain; Gautier-Luneau, Isabelle [Univ. Grenoble Alpes, Inst NEEL, Grenoble (France); CNRS, Inst NEEL, Grenoble (France); Sontakke, Atul D.; Viana, Bruno [PSL Research University, Chimie ParisTech - CNRS, Institut de Recherche de Chimie Paris (France); Bardet, Michel [Universite Grenoble Alpes, CEA, CNRS, INAC, MEM, Grenoble (France); Mouesca, Jean-Marie; Gambarelli, Serge; Maurel, Vincent [Universite Grenoble Alpes, CEA, CNRS, INAC, SyMMES, Grenoble (France); Barra, Anne-Laure [Laboratoire National des Champs Magnetiques Intenses, UPR CNRS 3228, Universite Grenoble Alpes, Grenoble (France); Ferrier, Alban [PSL Research University, Chimie ParisTech - CNRS, Institut de Recherche de Chimie Paris (France); Sorbonne Universites UPMC Universites Paris 06, Paris (France)

    2017-11-06

    Yttrium aluminum borate (YAB) powders prepared by sol-gel process have been investigated to understand their photoluminescence (PL) mechanism. The amorphous YAB powders exhibit bright visible PL from blue emission for powders calcined at 450 C to broad white PL for higher calcination temperature. Thanks to {sup 13}C labelling, NMR and EPR studies show that propionic acid initially used to solubilize the yttrium nitrate is decomposed into aromatic molecules confined within the inorganic matrix. DTA-TG-MS analyses show around 2 wt % of carbogenic species. The PL broadening corresponds to the apparition of a new band at 550 nm, associated with the formation of aromatic species. Furthermore, pulsed ENDOR spectroscopy combined with DFT calculations enables us to ascribe EPR spectra to free radicals derived from small (2 to 3 rings) polycyclic aromatic hydrocarbons (PAH). PAH molecules are thus at the origin of the PL as corroborated by slow afterglow decay and thermoluminescence experiments. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  16. Alkali corrosion resistant coatings and ceramic foams having superfine open cell structure and method of processing

    Science.gov (United States)

    Brown, Jr., Jesse J.; Hirschfeld, Deidre A.; Li, Tingkai

    1993-12-07

    Alkali corrosion resistant coatings and ceramic foams having superfine open cell structure are created using sol-gel processes. The processes have particular application in creating calcium magnesium zirconium phosphate, CMZP, coatings and foams.

  17. Preparation and Characterization of Titania-silica Composite Particles by Pechini Sol-gel Method

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    Wu Yuanting

    2016-01-01

    Full Text Available Two Pechini sol-gel processes were used to prepare titania-silica composite particles. The dynamic oxidation behavior of the TiO2-SiO2 powders has been characterized by thermogravimetry-differential scanning calorimetry (TG-DTG-DSC. The crystal phase and microstructure of the composite particles were investigated by X-ray diffraction (XRD and field emission scanning electron microscope (FE-SEM. The effects of Si:Ti molar ratio and sol-gel process on the TiO2-SiO2 powders were studied. The preparation of the polymeric precursors can influence the morphology of obtained TiO2-SiO2 composite particles. The spherical TiO2-SiO2 composite particles which are 20 nm~400 nm in diameter appear in gel-1 system. However, the TiO2-SiO2 powders obtained by gel-2 system are irregular in shape and 2~15 μm in diameter which show a loose porous structure consisted of very fine granules.

  18. Characterization of LiCoO Nanopowders Produced by Sol-Gel Processing

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    Sina Soltanmohammad

    2010-01-01

    Full Text Available LiCoO2 nanopowders, one of the most important cathode materials for lithium-ion batteries, were synthesized via a modified sol-gel process assisted with triethanolamine (TEA as a complexing agent. The influence of three different chelating agents including acrylic acid, citric acid, and oxalic acid on the size and morphology of particles was investigated. Structure and morphology of the synthesized powders were characterized by thermogravimetric/differential thermal analyses (TG/DTA, X-ray diffraction (XRD, and transmission electron microscopy (TEM. Results indicate that the powder processed with TEA and calcinated at 800∘C had an excellent hexagonal ordering of -NaFeO2-type (space group R3m. Also, the other three complexing agents had a decisive influence on the particle size, shape, morphology, and degree of agglomeration of the resulting oxides. Based on the data presented in this work, it is proposed that the optimized size and distribution of LiCoO2 powders may be achieved through sol-gel processing using TEA as a chelating agent.

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

    Science.gov (United States)

    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. Effect of preparation methods on the properties of titania nanoparticles: solvothermal versus sol-gel

    Science.gov (United States)

    Dastan, Davoud

    2017-11-01

    Titania (TiO2) nanoparticles (NP's) have been prepared by solvothermal and sol-gel techniques using different surfactants such as acetic acid (AA), oleylamine (OM), and AA + OM. The solution was thermally treated at growth temperature 180 °C in solvothermal method. TiO2 powder, prepared using both methods, was subjected to post heat treatment at 550 and 950 °C. The effect of surfactants on the morphology of TiO2 NP's was studied by transmission electron microscopy (TEM) and field emission scanning electron microscopy (FESEM). The structural and thermal properties of titania NP's are investigated by means of X-ray diffraction, Raman spectroscopy, thermogravimetric analysis, and differential scanning calorimetry (TGA/DSC). TEM and FESEM images illustrated various shapes of titania NP's such as irregular spherical, rounded rectangular, truncated rhombic, oval, and rod-like structure in presence of different surfactants. Moreover, TiO2 particles prepared by sol-gel method were almost 40 times greater than those prepared by solvothermal method. In addition to the improvement in the crystallinity, thermal stability has been enhanced due to consolidation of individual particles at higher annealing temperature in solvothermal technique. Furthermore, a reduction in the degradation temperature and phase transformation of TiO2 NP's were conspicuously corroborated after post-heat treatment.

  1. New optical fiber type: microporous sol-gel-clad optical fibers

    Science.gov (United States)

    Skutnik, Bolesh J.

    1999-04-01

    A new type of optical fiber has been developed. It is made with all pure silica in both the core and cladding. This is possible because the cladding is a micro porous silica produced by a modified sol-gel technology. The formation and characteristics of this new optical fiber type are described. In particular the optical and mechanical properties are illustrated and described. The strength and fatigue of these optical fibers are very good, even without additional protective jackets. Unjacketed fibers have mean Weibull strengths in bending of 6.5 to 7.6 GPa with Weibull slopes in the 40 to 60 range. Fatigue results for fibers tested in ambient air, ambient water and boiling water are presented. The dynamic and static fatigue parameters are around 20. The micro porous structure of the sol-gel cladding provides sites for attaching different moieties which could activate biochemical reactions or be useful as sensing sites. Based on preliminary experiments, some possibilities are presented. In general this new structure can provide opportunities for as yet unidentified applications where chemicals and or light must be brought in close contact with body tissue to effect beneficial reactions there.

  2. Development of sol-gel bioactive glass for hard tissue regeneration

    Science.gov (United States)

    Noor, Siti Noor Fazliah Mohd; Zain, Nurul Shazwani Mohd; Wei, Poh Yong; Azizan, Nur Syazana; Mohamad, Hasmaliza

    2016-12-01

    The regeneration of hard tissues requires various contributing factors such as cells, scaffolds and growth factors. Bioactive glasses are known for its properties to stimulate hard tissue regeneration. In this study, sol-gel bioactive glasses (BG) were prepared and characterized. Sol-gel BG powders having particle size less than 25 µm were incubated with cell culture medium for 4 hours at 37°C on continuous rolling, and then the medium was filtered using 0.22 µm syringe filters. Prior to use, the SGBG-conditioned media were supplemented with 10% (v/v) fetal bovine serum and 1% (v/v) antibiotic-antimycotic, and were allowed to equilibrate overnight inside a CO2 incubator. The human dental pulp stem cells (DPSC) were incubated with the BG-conditioned media and their viability and proliferation were assessed at day 1, 2, 4 and 7 using Alamar Blue and MTT assays. The results showed that BG at various powders to liquid ratio concentrations promoted DPSC growth. The BG have potential to be used for hard tissue regeneration especially in the field of regenerative dentistry.

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

    Directory of Open Access Journals (Sweden)

    Josef Trögl

    2015-02-01

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

  4. Microalgae fiber optic biosensors for herbicide monitoring using sol-gel technology.

    Science.gov (United States)

    Peña-Vázquez, Elena; Maneiro, Emilia; Pérez-Conde, Concepción; Moreno-Bondi, Maria Cruz; Costas, Eduardo

    2009-08-15

    Three microalgal species (Dictyosphaerium chlorelloides (D.c.), Scenedesmus intermedius (S.i.) and Scenedesmus sp. (S.s.)) were encapsulated in silicate sol-gel matrices and the increase in the amount of chlorophyll fluorescence signal was used to quantify simazine. Influence of several parameters on the preparation of the sensing layers has been evaluated: effect of pH on sol-gel gelation time; effect of algae density on sensor response; influence of glycerol (%) on the membrane stability. Long term stability was also tested and the fluorescence signal from biosensors remained stable for at least 3 weeks. D.c. biosensor presented the lowest detection limits for simazine (3.6 microg L(-1)) and the broadest dynamic calibration range (19-860 microg L(-1)) with IC(50) 125+/-14 microg L(-1). Biosensor was validated by HPLC with UV/DAD detection. The biosensor showed response to those herbicides that inhibit the photosynthesis at photosystem II (triazines: simazine, atrazine, propazine, terbuthylazine; urea based herbicides: linuron). However, no significant increases of fluorescence response was obtained for similar concentrations of 2,4-D (hormonal herbicide) or Cu(II). The combined use of two biosensors that use two different genotypes, sensitive and resistant to simazine, jointly allowed improving microalgae biosensor specificity.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lau, L. N., E-mail: lau7798@gmail.com; Ibrahim, N. B., E-mail: baayah@ukm.edu.my [School of Applied Physics, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor. Malaysia (Malaysia)

    2015-09-25

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

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

    Science.gov (United States)

    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. Copyright © 2014. Published by Elsevier B.V.

  7. Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

    Science.gov (United States)

    Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

    2014-01-01

    In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x Ag = 0.5 are effective against E. coli and S. aureus after 24 h. PMID:24523630

  8. A modified sol-gel technique for pore size control in porous aluminum oxide nanowire templates.

    Science.gov (United States)

    Kelly, Daniel N; Wakabayashi, Ryo H; Stacy, Angelica M

    2014-11-26

    A modified sol-gel technique was developed to continuously vary the pore diameters in porous alumina templates for the purpose of growing nanowires. To coat the pore walls, the porous alumina film is initially soaked in a methanol/water solution to fill the pores with the desired concentration of water. The porous alumina film is then exposed to a solution of 3-aminopropyltriethoxysilane (APTES) in toluene, creating a surface layer of APTES. The concentration of water in the pores correlates with the thickness of the APTES polymer coating that is obtained. This approach exerts greater control over the extent of silane polymerization than traditional sol-gel reactions by limiting the amount of water present for reaction. Factors such as the APTES concentration, exposure time, and organic cosolvent choice did not influence the coating thickness. However, the density and thickness of the APTES coating can be manipulated by varying the pH of the methanol/water solution as well as post-treatment annealing. Further modification of the pore size was achieved by subsequent reaction of the APTES coating with poly(methyl methacrylate) (PMMA). The PMMA couples to amine groups on the APTES polymer surface by an aminolysis reaction. Bismuth telluride nanowires were electrodeposited in the polymer-coated porous alumina templates using previously established methods. Nanowire diameters were smaller when the nanowires were prepared in modified templates as anticipated.

  9. Synthesis of zinc oxide thin films prepared by sol-gel for specific bioactivity

    Science.gov (United States)

    Adam, Tijjani; Basri, B.; Dhahi, Th. S.; Mohammed, Mohammed; Hashim, U.; Noriman, N. Z.; Dahham, Omar S.

    2017-09-01

    Zinc oxide (ZnO) thin films this device to used for many application like chemical sensor, biosensor, solar energy, etc but my project to use for bioactivity(biosensor). Zinc oxide (ZnO) thin films have been grown using sol-gel technique. Characterization was done using Scanning Electron Microscope (SEM), Energy Dispersive X-ray(EDX) and Electrical Measurement(I-V). ZnO thin film was successfully synthesized using low cost sol-gel spin coating method. The coupling of DNA probe to ZnO thin film supports modified with carboxylic acid (COOH) is certainly the best practical method to make DNA immobilization and it does not require any coupling agent which could be a source of variability during the spotting with an automatic device. So, selected this coupling procedure for further experiments. The sensor was tested with initial trial with low concentrated DNA and able to detect detection of the disease effectively. Silicon-on-insulator (SOI) wafer device with ZnO can detect at different concentration in order to valid the device capabilities for detecting development. The lowest concentration 1 µM HPV DNA probe can detect is 0.1 nM HPV target DNA.

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

    Directory of Open Access Journals (Sweden)

    Ahmed S. Razeen

    2017-01-01

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

  11. Sol-Gel Behavior of Hydroxypropyl Methylcellulose (HPMC) in Ionic Media Including Drug Release.

    Science.gov (United States)

    Joshi, Sunil C

    2011-10-24

    Sol-gel transformations in HPMC (hydroxypropyl methylcellulose) are being increasingly studied because of their role in bio-related applications. The thermo-reversible behavior of HPMC is particularly affected by its properties and concentration in solvent media, nature of additives, and the thermal environment it is exposed to. This article contains investigations on the effects of salt additives in Hofmeister series on the HPMC gelation. Various findings regarding gelation with salt ions as well as with the ionic and non-ionic surfactants are presented. The gel formation in physiological salt fluids such as simulated gastric and intestine fluids is also examined with the interest in oral drug delivery systems. The processes of swelling, dissolution and dispersion of HPMC tablets in simulated bio-fluids are explored and the release of a drug from the tablet affected by such processes is studied. Explanations are provided based on the chemical structure and the molecular binding/association of HPMC in a media. The test results at the body or near-body temperature conditions helped in understanding the progress of the gelation process within the human body environment. The detailed interpretation of various molecule level interactions unfolded the sol-gel mechanisms and the influence of a few other factors. The obtained test data and the established mathematical models are expected to serve as a guide in customizing applications of HPMC hydrogels.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  13. Diameter deviation calculation for UO{sub 2} kernel by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Guo Wenli; Xing Juan [Beijing Key Lab of Fine Ceramics, Institution of Nuclear and New Energy Technology, Tsinghua University, Beijing 10084 (China); Liang, T.X., E-mail: txliang@tsinghua.edu.cn [Beijing Key Lab of Fine Ceramics, Institution of Nuclear and New Energy Technology, Tsinghua University, Beijing 10084 (China); Jin Xin [CNNC China Nuclear Power Engineering Co. Ltd., Beijing 100840 (China)

    2011-08-15

    Highlights: > UO{sub 2} kernels are produced by a sol-gel method. > The formula about jet velocity, solution level and gas pressure on solution was established. > The decline of solution level leads to the decreasing of jet velocity and the solution mass flow rate, as a result, the diameter deviation increased. > After compensating the pressure on the liquid gradually during the casting process, the standard deviation of kernel diameter was less than 12 {mu}m. - Abstract: UO{sub 2} kernels for HTR (High Temperature Gas-cooled Reactor) fuel element are produced using a sol-gel method. The size of UO{sub 2} kernels was controlled strictly by minimizing the dispersion of the UO{sub 2} kernel diameter during the casting process. A relationship between the filling gas tank pressure and solution level in the tank was developed to keep a constant solution mass flow rate in the nozzles. Based on equation of flow energy conservation, a formula about jet velocity, solution level and gas tank pressure on solution was established. Using the formula, the minimum pressure and maximum pressure were calculated. During the casting process, the decline of solution level will lead to the decreasing of jet velocity and the solution mass flow rate that can cause the increasing of diameter deviation. By compensating the pressure on the liquid gradually during the casting process, the flow fluency was kept in an acceptable range stably, the standard deviation of kernel diameter was less than 12 {mu}m.

  14. Biocompatibility of sol-gel hydroxyapatite-titania composite and bilayer coatings.

    Science.gov (United States)

    Sidane, D; Rammal, H; Beljebbar, A; Gangloff, S C; Chicot, D; Velard, F; Khireddine, H; Montagne, A; Kerdjoudj, H

    2017-03-01

    Titania-Hydroxyapatite (TiO2/HAP) reinforced coatings are proposed to enhance the bioactivity and corrosion resistance of 316L stainless steel (316L SS). Herein, spin- and dip-coating sol-gel processes were investigated to construct two kinds of coatings: TiO2/HAP composite and TiO2/HAP bilayer. Physicochemical characterization highlighted the bioactivity response of the TiO2/HAP composite once incubated in physiological conditions for 7days whereas the TiO2/HAP bilayer showed instability and dissolution. Biological analysis revealed a failure in human stem cells adhesion on TiO2/HAP bilayer whereas on TiO2/HAP composite the presence of polygonal shaped cells, possessing good behaviour attested a good biocompatibility of the composite coating. Finally, TiO2/HAP composite with hardness up to 0.6GPa and elastic modulus up to 18GPa, showed an increased corrosion resistance of 316L SS. In conclusion, the user-friendly sol-gel processes led to bioactive TiO2/HAP composite buildup suitable for biomedical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Sol-gel Process in Preparation of Organic-inorganic Hybrid Materials

    Directory of Open Access Journals (Sweden)

    Macan, J

    2008-07-01

    Full Text Available Organic-inorganic hybrid materials are a sort of nanostructured material in which the organic and inorganic phases are mixed at molecular level. The inorganic phase in hybrid materials is formed by the sol-gel process, which consists of reactions of hydrolysis and condensation of metal (usually silicon alkoxides. Flexibility of sol-gel process enables creation of hybrid materials with varying organic and inorganic phases in different ratios, and consequently fine-tuning of their properties. In order to obtain true hybrid materials, contact between the phases should be at molecular level, so phase separation between thermodynamically incompatible organic and inorganic phases has to be prevented. Phase interaction can be improved by formation of hydrogen or covalent bonds between them during preparation of hybrid materials. Covalent bond can be introduced by organically modified silicon alkoxides containing a reactive organic group (substituent capable of reacting with the organic phase. In order to obtain hybrid materials with desired structures, a detailed knowledge of hydrolysis and condensation mechanism is necessary. The choice of catalyst, whether acid or base, has the most significant influence on the structure of the inorganic phase. Other important parameters are alkoxide concentration, water: alkoxide ratio, type of alkoxide groups, solvent used, temperature, purity of chemicals used, etc. Hydrolysis and condensation of organically modified silicon alkoxides are additionally influenced by nature and size of the organic supstituent.

  16. Sol-Gel Behavior of Hydroxypropyl Methylcellulose (HPMC in Ionic Media Including Drug Release

    Directory of Open Access Journals (Sweden)

    Sunil C. Joshi

    2011-10-01

    Full Text Available Sol-gel transformations in HPMC (hydroxypropyl methylcellulose are being increasingly studied because of their role in bio-related applications. The thermo-reversible behavior of HPMC is particularly affected by its properties and concentration in solvent media, nature of additives, and the thermal environment it is exposed to. This article contains investigations on the effects of salt additives in Hofmeister series on the HPMC gelation. Various findings regarding gelation with salt ions as well as with the ionic and non-ionic surfactants are presented. The gel formation in physiological salt fluids such as simulated gastric and intestine fluids is also examined with the interest in oral drug delivery systems. The processes of swelling, dissolution and dispersion of HPMC tablets in simulated bio-fluids are explored and the release of a drug from the tablet affected by such processes is studied. Explanations are provided based on the chemical structure and the molecular binding/association of HPMC in a media. The test results at the body or near-body temperature conditions helped in understanding the progress of the gelation process within the human body environment. The detailed interpretation of various molecule level interactions unfolded the sol-gel mechanisms and the influence of a few other factors. The obtained test data and the established mathematical models are expected to serve as a guide in customizing applications of HPMC hydrogels.

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

    Science.gov (United States)

    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.

  18. Hydroxyapatite Coating on TiO₂ Nanotube by Sol-Gel Method for Implant Applications.

    Science.gov (United States)

    Lim, Hyun-Pil; Park, Sang-Won; Yun, Kwi-Dug; Park, Chan; Ji, Min-Kyung; Oh, Gye-Jeong; Lee, Jong-Tak; Lee, Kwangmin

    2018-02-01

    The aim of this study was to determine the effect of hydroxyapatite (HA) coating on titanium dioxide (TiO2) nanotube by sol-gel process on viability of osteoblast like cell (MC3T3-E1) and bone formation in rat tibia. Specimens were divided into three groups including commercially pure titanium (control group), TiO2 nanotubes (group N), and HA coated TiO2 nanotubes (group HN). Surface characteristics were determined using field emission scanning electron microscope (FE-SEM; S-4700, Hitachi, Japan) and contact angles were measured. Cell viability was investigated in vitro after 1 day, 3 days, and 7 days of incubation. Implants (2.0 mm in diameter and 5.0 mm in length) were inserted into the tibia of rats. After 4 weeks, histomorphometric analysis was performed. Both N and HN groups showed enhanced hydrophilicity compared to control group. After 7 days of implantation, group HN showed higher cell viability with marginal significance (0.05 < P < 0.1). Bone to implant contact (BIC) ratio in the control group, group N, and group HN were 32.5%, 33.1%, and 43.8%, respectively. Results of this study showed that HA coated TiO2 nanotube using sol-gel process could be used to enhance hydrophilicity and improve osseointegration of dental implant surface.

  19. Synthesis of ZnO-CuO Nanocomposite Aerogels by the Sol-Gel Route

    Directory of Open Access Journals (Sweden)

    Rula M. Allaf

    2014-01-01

    Full Text Available The epoxide addition sol-gel method has been utilized to synthesize porous zinc-copper composite aerogels in the zinc-to-copper molar ratios of 50 : 50 to 90 : 10. A two-step mixing approach has been employed to produce aerogels composed of nano- to micrometer sized particles. The aerogels were characterized by ultrahigh resolution scanning electron microscopy, transmission electron microscopy, and powder X-ray diffraction. The as-synthesized aerogels had a thin flake- or petal-like microstructure comprised of clustered flakes on two size scales; they were identified as being crystalline with the crystalline species identified as copper nitrate hydroxide, zinc hydroxide chloride hydrate, and zinc hydroxide nitrate hydrate. Annealing of the aerogel materials at a relatively low temperature (400°C resulted in a complete phase transition of the material to give highly crystalline ZnO-CuO aerogels; the aerogels consisted of networked nanoparticles in the ~25–550 nm size range with an average crystallite size of ~3 nm and average crystallinity of 98%. ZnO-CuO aerogels are of particular interest due to their particular catalytic and sensing properties. This work emphasizes the versatility of this sol-gel route in synthesizing aerogels; this method offers a possible route for the fabrication of aerogels of different metal oxides and their composites.

  20. Surface Modification of Zirconia Substrate by Calcium Phosphate Particles Using Sol-Gel Method.

    Science.gov (United States)

    Jin, So Dam; Um, Sang Cheol; Lee, Jong Kook

    2015-08-01

    Surface modification with a biphasic composition of hydroxyapatite (HA) and tricalcium phosphate (TCP) was performed on a zirconia substrate using a sol-gel method. An initial calcium phosphate sol was prepared by mixing a solution of Ca(NO3)2 · 4H20 and (C2H5O)3P(O), while both porous and dense zirconia were used as substrates. The sol-gel coating was performed using a spin coater. The coated porous zirconia substrate was re-sintered at 1350 °C 2 h, while coated dense zirconia substrate was heat-treated at 750 °C 1 h. The microstructure of the resultant HA/TCP coatings was found to be dependent on the type of zirconia substrate used. With porous zirconia as a starting substrate, numerous isolated calcium phosphate particles (TCP and HA) were uniformly dispersed on the surface, and the particle size and covered area were dependent on the viscosity of the calcium phosphate sol. Conversely, when dense zirconia was used as a starting substrate, a thick film of nano-sized HA particles was obtained after heat treatment, however, substantial agglomeration and cracking was also observed.

  1. Silica doped with lanthanum sol-gel thin films for corrosion protection

    Energy Technology Data Exchange (ETDEWEB)

    Abuin, M. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Serrano, A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); Llopis, J. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Garcia, M.A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); IMDEA Nanoscience, Fco. Tomas y Valiente 7, 28049 Madrid (Spain); Carmona, N., E-mail: n.carmona@fis.ucm.es [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain)

    2012-06-01

    We present here anticorrosive silica coatings doped with lanthanum ions for the protection of metallic surfaces as an alternative to chromate (VI)-based conversion coatings. The coatings were synthesized by the sol-gel method starting from silicon alkoxides and two different lanthanum precursors: La (III) acetate hydrate and La (III) isopropoxide. Artificial corrosion tests in acid and alkaline media showed their effectiveness for the corrosion protection of AA2024 aluminum alloy sheets for coating prepared with both precursors. The X-ray absorption Near Edge Structure and X-ray Absorption Fine Structure analysis of the coatings confirmed the key role of lanthanum in the structural properties of the coating determining its anticorrosive properties. - Highlights: Black-Right-Pointing-Pointer Silica sol-gel films doped with lanthanum ions were synthesized. Black-Right-Pointing-Pointer Films from lanthanum-acetate and La-alkoxide were prepared for comparison purposes. Black-Right-Pointing-Pointer La-acetate is an affordable chemical reactive preferred for the industry. Black-Right-Pointing-Pointer Films properties were explored by scanning electron microscopy and X-Ray absorption spectroscopy. Black-Right-Pointing-Pointer An alternative to anticorrosive pre-treatments for metallic surfaces is suggested.

  2. Preparation of the SnO2 gate pH-ISFET by sol gel technology

    Science.gov (United States)

    Chou, Jung Chuan; Wang, Yii Fang

    2001-10-01

    In this paper, the sol-gel prepared SnO2 thin film is first applied for the pH sensing. We use the SnCl2(DOT)2H2O as the precursor. It is cheaper than other methods. The resulting solution is dropped on the gate of the SiO2 gate pH-ISFET (ion sensitive field effect transistor). After baking, the thin film will convert to SnO2. We also use the thermal evaporation system to prepare the SnO2 gate MOSFET. Then, we use the Keithley 236 instrument to measure the IDS-VG curves of the SnO2 gate MOSFET and pH-ISFET for the different pH buffer solutions. Since the MOSFET and pH-ISFET are fabricated on the same silicon wafer, the properties of these devices are identical. Therefore, we can use the experimental results and theoretical model of the pH-ISFET to find the pH sensitivity and pHPZC (pH at the point of zero charge) of the sol-gel prepared SnO2 gate pH-ISFET, which are about 57.36 mV/pH and 11.3, respectively.

  3. Preparation of single phase {beta}-spodumene powders by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Wen, Shawbing; Yang, Sheng [National Cheng-Kung University, Tainan (Taiwan). Dept. of Resources Engineering; Chen, Jenmin; Wu, Nangchung [National Cheng-Kung University, Tainan (Taiwan). Dept. of Material Science and Engineering; Wang, Moochin [National Kaohsiung Institute of Technology, Kaohsiung (Taiwan). Dept. of Mechanical Engineering

    1999-12-01

    The {beta}-spodumene (Li{sub 2}O{center_dot}Al{sub 2}O{sub 3}{center_dot}4SiO{sub 2}, LAS) powders were prepared by the sol-gel process using a mixture of silica sol, alumina sol and lithium nitrate solution. Si(OC{sub 2}H{sub 5}){sub 4}, Al(OC{sub 4}H{sub 9}{sup 8ec}){sub 3} and LiNO{sub 3} were used as the starting compounds. Thermogravimetric and differential thermal analyses (TG/DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), wavelength-dispersive spectroscopy (WDS), transmission electron microscopy (TEM) and electron diffraction (ED) analysis were utilized to characterize the {beta}-spodumene powders prepared by the sol-gel process. The crystallization temperature of the LAS gel powder estimated by TG/DTA was about 630 degree C. When the LAS dried gel was heated from 600 to 850 degree C, the crystallized powders of the single phase {beta}-spodumene were obtained. (author)

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

    Directory of Open Access Journals (Sweden)

    María Aymerich

    2016-08-01

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

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

    Science.gov (United States)

    Svobodová, Jana; Kofroňová, Olga; Benada, Oldřich; Král, Vladimír; Mikšík, Ivan

    2017-09-29

    The aim of this article is to study the modification of an inner capillary wall with sol-gel coating (pure silica sol-gel or silica sol-gel containing porphyrin-brucine conjugate) and determine its influence on the separation process using capillary electrophoresis/electrochromatography method. After modification of the inner capillary surface the separation of analytes was performed using two different phosphate buffers (pH 2.5 and 9.0) and finally the changes in electrophoretic mobilities of various samples were calculated. To confirm that the modification of the inner capillary surface was successful, the parts of the inner surfaces of capillaries were observed using scanning electron microscopy. The analytes used as testing samples were oligopeptides, nucleosides, nucleobases and finally nucleotides. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Soft nanoimprint lithography on SiO2 sol-gel to elaborate sensitive substrates for SERS detection

    Directory of Open Access Journals (Sweden)

    Frédéric Hamouda

    2017-12-01

    Full Text Available This paper presents a new alternative fabrication of biochemical sensor based on surface enhanced Raman scattering (SERS by soft nanoimprint lithography (S-NIL on SiO2 sol-gel. Stabilization of the sol-gel film is obtained by annealing which simplifies the manufacturing of these biosensors and is compatible with mass production at low cost. This detector relies on a specific pattern of gold nanodisks on a thin gold film to obtain a better sensitivity of molecules’ detection. Characterizations of SERS devices were performed on a confocal Raman microspectrophotometer after a chemical functionalization. We report a lateral collapse effect on poly(diméthylsiloxane (PDMS stamp for specific nanostructure dimensions. This unintentional effect is used to evaluate S-NIL resolution in SiO2 sol-gel.

  8. Fabrication of Meso-Porous Gamma-Alumina Films by Sol-Gel and Gel Casting Processes for Making Moisture Sensors

    Directory of Open Access Journals (Sweden)

    Kalyan Kumar Mistry

    2007-04-01

    Full Text Available Meso-porous g-Al2O3 film may be used as a highly sensitive trace moisture sensor. The crack-free alumina film was developed using a combination of sol-gel and tape casting processes, which produce high porosity, high surface area and small pore dimensions in the range of few nano-meter at uniform distribution. Sol-gel processes are well known in nano-technology and nano-material preparation, but it is difficult to make crack-free thick or thin films using this method. Tape cast methods are used for the fabrication of flexible crack-free thick ceramic sheets. Our objective was to develop nano-structured, crack-free, transparent Al2O3 film a few microns thick, has a highly porous and stable crystallographic nature. A metallic paste was printed by screen printing on both side of the film surface for electrodes to form a sensitive element. A silver wire (dia j=0.1mm lead was connected to a grid structure electrode using a silver paste spot for fine joining. Alumina is absorbs moisture molecules into its meso-porous layer and changes its electrical characteristics according to the moisture content, its dielectric constant increase as moisture increase. Moisture molecules can be conceived of as dipoles in random state before the application of an electric field. When the dipole orientation was changed from random to an equilibrium state under the application of external field, a large change in dielectric constant was observed. The number of water molecules absorbed determines the electrical impedance of the capacitor, which in turn is proportional to water vapor pressure.

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

    Science.gov (United States)

    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. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: bonding to titanium and scanning electron microscopy.

    Science.gov (United States)

    Tredwin, Christopher J; Georgiou, George; Kim, Hae-Won; Knowles, Jonathan C

    2013-05-01

    Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) production has been characterised and optimised by the sol-gel method and the dissolution and biological properties of these materials were investigated. It was the objective of this study to investigate the potential bond strength and interaction of these materials with titanium. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the FHA and FA sol-gels. Using a spin coating technique the sol-gels were coated onto commercially pure titanium disks and crystallised at various temperatures. Using scanning electron microscopy (SEM) and elemental analysis, the surface characteristics, coating thickness and interaction of the Ti substrate and coating were investigated. The bond strengths of the coating to the Ti were investigated using an Instron Universal Load Testing Machine. Statistical analysis was performed with a two-way analysis of variance and post hoc testing with a Bonferroni correction. (1) Coating speed inversely influenced the coating thickness. (2) Increasing fluoride ion substitution and heating temperature significantly increased bond strength and (3) increasing fluoride ion substitution increased the coating thickness. FHA and FA synthesised using the sol-gel technique may offer a superior alternative to coating titanium implants with HA and plasma spraying. HA, FHA and FA materials synthesised by the sol-gel method may also have a use as bone grafting materials. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  11. Preparation of Aligned ZnO Nanorod Arrays on Sn-Doped ZnO Thin Films by Sonicated Sol-Gel Immersion Fabricated for Dye-Sensitized Solar Cell

    Directory of Open Access Journals (Sweden)

    I. Saurdi

    2014-01-01

    Full Text Available Aligned ZnO Nanorod arrays are deposited on the Sn-doped ZnO thin film via sonicated sol-gel immersion method. The structural, optical, and electrical properties of the Sn-doped ZnO thin films were investigated. Results show that the Sn-doped ZnO thin films with small grain size (~20 nm, high average transmittance (96% in visible region, and good resistivity 7.7 × 102 Ω·cm are obtained for 2 at.% Sn doping concentration. The aligned ZnO nanorod arrays with large surface area were also obtained for 2 at.% Sn-doped ZnO thin film. They were grown on sol-gel derived Sn-doped ZnO thin film, which acts as a seed layer, via sonicated sol-gel immersion method. The grown aligned ZnO nanorod arrays show high transmittance at visible region. The fabricated dye-sensitised solar cell based on the 2.0 at.% Sn-doped ZnO thin film with aligned ZnO nanorod arrays exhibits improved current density, open-circuit voltage, fill factor, and conversion efficiency compared with the undoped ZnO and 1 at.% Sn-doped ZnO thin films.

  12. Improvement of UV Protection Properties of the Textile from Natural Fibres by the Sol-Gel Method

    OpenAIRE

    Vihodceva, S; Kukle, S

    2013-01-01

    In this research pure cotton textile has been modified by the sol-gel technology to implement zinc oxide nanolevel coating on textile surface to ensure ultraviolet (UV) radiation protection. One of the advantages of this method is the possibility to obtain thin layers on various materials, as well as the sol-gel layers can cover all fibres with enough high adhesion. Comparison of coatings of samples prepared using different concentrations of TEOS in nano-sols and thermal post-treatment of sam...

  13. X-ray diffraction measurement of residual stress in sol-gel grown lead zirconate titanate thick films on nickel-based super alloy substrate

    Energy Technology Data Exchange (ETDEWEB)

    Hoshyarmanesh, Hamidreza; Nehzat, Naser; Salehi, Mehdi [Isfahan University of Technology, Isfahan (Iran, Islamic Republic of); Ghodsi, Mojtaba [Sultan Qaboos University, Muscat (Oman)

    2015-02-15

    Residual compressive stress of Pb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} thick films was investigated using residual strains derived from X-ray diffraction patterns. Sin{sup 2}ψ method was applied for the 5, 10 and 15 μm sol-gel derived thick films annealed at 700 .deg. C for 1 hr as high frequency structural health monitoring square-shape transducers of 10 x10 mm, deposited onto the curved nickel-based super alloy substrates. A triaxial model was proposed based on piezoelectric constitutive equations, and Bragg's law at a large diffraction angle (∼89°) was utilized considering the electromechanical coupling factor as well as elastic, dielectric and piezoelectric constants. Thickness variations led to a significant change in residual stress magnitudes delineated from more-accurate triaxial model compared to small angle plane-stress results not considering the piezoelectric coupling effects.

  14. Sol-gel synthesis of magnetic sorbents based on porous iron oxides for the removal of U(VI) from aqueous solution

    Science.gov (United States)

    Papynov, E. K.; Portnyagin, A. S.; Cherednichenko, A. I.; Tkachenko, I. A.; Modin, E. B.; Dran'kov, A. N.; Kvach, A. A.; Zemchenko, I. V.; Tananaev, I. G.; Avramenko, V. A.

    2017-02-01

    An original synthetic route to nanostructured iron oxides with porous structure and to their reduced derivatives, prospective for uranium (VI) uptake from water media, is presented. The uniqueness of method includes combination of sol-gel technology, which used for generating inorganic framework, and template synthesis for porous structure formation with the help of poreforming agent (polymer latex). Method of consolidating porous iron oxides and its influence on such characteristics as porosity, magnetization, morphology, phase composition and sorption properties are described. Sorption properties of the materials based on iron oxides and their reduced derivatives with respect to uranium (VI) from water media of different acidity has been investigated. Mechanism of uranium (VI) sorption on the obtained materials has been determined. The interaction of the sorbents with uranyl-ions was shown to change depending on phase composition and structure of the solid matrix.

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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

  17. Exploitation of the Sol-Gel Route in Processing of Ceramics and Composites.

    Science.gov (United States)

    1987-07-10

    the wet gel by long the post-formation of a non-crystalline or stirring with a micro- spatula . Other mixtures 0025-5416, 861$3.50 © Elsevier Sequoia...matter of seconds in a standard kitchen -type rmcrowave oven with a frequency of 2.45 GHz. This dielectnc heating behavior is controlled in part by the

  18. Investigation of the relaxor behavior of sol gel processed lanthanum lead titanium ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Limame, K. [Centre Régional des Metiers de l' Education et de la Formation (CRMEF) de Fès, Rue deKuwait, BP 49, Fès (Morocco); Laboratoire de Physique Théorique et Appliquée, (LPTA), FSDM, B.P. 1796, Fès-Atlas, Fès (Morocco); Sayouri, S., E-mail: ssayouri@gmail.com [Laboratoire de Physique Théorique et Appliquée, (LPTA), FSDM, B.P. 1796, Fès-Atlas, Fès (Morocco); Yahyaoui, M.M. [Laboratoire de Physique Théorique et Appliquée, (LPTA), FSDM, B.P. 1796, Fès-Atlas, Fès (Morocco); Housni, A. [Laboratoire de Physique Théorique et Appliquée, (LPTA), FSDM, B.P. 1796, Fès-Atlas, Fès (Morocco); Institut Supérieur des Professions Infirmières et Techniques de Santé (ISPITS), Fès (Morocco); Jaber, B. [Centre National pour la Recherche Scientifique et Technique (CNRST), Angle Avenue Allal El Fassi avenue des FAR, Quartie Hay Ryad, BP8027 Nation Unies, Rabat (Morocco)

    2016-08-01

    A series of La doped lead titanate samples, with composition Pb{sub 1−x}La{sub x}Ti{sub 1−x/4}O{sub 3} (PLTx), where x=0.00; 0.02; 0.04; 0.06; 0.07; 0.08; 0.10; 0.12; 0.14; 0.16; 0.18; 0.21 and 0.22 was prepared using the sol–gel process. Addition of La gives rise to the two well-known phenomena: diffuseness and relaxation around the ferro-to-paraelectric transition; the two parameters related to these phenomena, and which give a satisfactory interpretation of them, have been estimated using the Uchino's quadratic law. This diffuse phase transition (DPT) has been investigated with the help of the Landau–Devonshire cluster theory and the model of Cheng et al., to show that polar regions may be generated around the DPT and far from the temperature, T{sub m}, of the maximum of the dielectric permittivity, which have as a direct consequence a non vanishing polarization even if T>T{sub m}.

  19. Analysis of milk ageing by a sol-gel sensors array

    Science.gov (United States)

    Siciliano, P.; Rella, R.; Capone, S.; Taurino, A.; Vasanelli, L.

    2000-12-01

    There is growing interest in the development of electronic odours-detection multisensor systems for objective evaluation of aroma food. Study of food storage, freshness control and ageing is one of the most important application field for this new class of device (named "electronic nose"). In this paper we report a specific application of a semiconductor thin films based electronic nose in the control of the rancidity of two different milk (UHT and pasteurised) during their storage days. The active elements of the array were undoped and Os-, Ni-, Pt-, Pd-doped SnO2 thin films prepared by the sol-gel method. Principal Component Analysis (PCA), applied to the data coming from the response of the sensors, gave satisfactory results in tracking dynamic evolution of milk, that could lead to commercial application in the food industry.

  20. Coating of LaCoO3 thin film with sol-gel dip coating method.

    Science.gov (United States)

    Okuyucu, Hasan; Dahl, Paul Inge; Einarsrud, Mari Ann

    2008-02-01

    LaCoO3 thin film was coated on Al2O3 single crystal by sol-gel route. Appropriate composition of precursors, chelating agents and the solvent put together into a flask and magnetically stirred on a magnetic stirrer. After having the red transparent solution, it was stirred for 12 hours before coating. Ultrasonically cleaned substrate is dipped into the solution and taken immediately into vertical furnace which is preheated at 550 degrees C. A dense amorphous film is coated on the substrate. Fired amorphous films are annealed at temperature between 900 degrees C and 1000 degrees C for 20 minutes in the air. Then coated film was characterized by means of XRD, AFM, and SEM. Conductivity of the film was measured to be -0.1819 for 881 degrees C for the log sigma value by assuming the thickness as

  1. Sol-gel synthesis and characterization of mesoporous iron-titanium mixed oxide for catalytic application

    Energy Technology Data Exchange (ETDEWEB)

    Parida, K.M., E-mail: paridakulamani@yahoo.com [Colloids and Materials Chemistry Department, Institute of Minerals and Materials Technology, Bhubaneswar 751013, Orissa (India); Pradhan, Gajendra Kumar [Colloids and Materials Chemistry Department, Institute of Minerals and Materials Technology, Bhubaneswar 751013, Orissa (India)

    2010-10-01

    A mixed phase of mesoporous iron-titanium mixed oxide (ITMO) has been successfully synthesized by simple sol-gel technique by taking iron (II) sulphate and Ti-isopropoxide as the precursors and sodium dodecyl sulphate (SDS) as the surfactant. The prepared catalysts were characterized by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), diffuse reflectance UV-vis spectra (UV-vis DRS), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), atomic absorption spectroscopy (AAS), N{sub 2} adsorption-desorptions isotherm, temperature programmed desorption (TPD) and gas chromatography (GC). Low-angle XRD (LAXRD) as well as surface area analysis confirms the mesoporosity nature of the catalysts. The phase and crystallinity were revealed by XRD study. The crystallinity of the catalysts increased with increase in calcinations temperature. Catalysts screening were performed for oxidation of cyclohexane to cyclohexanol and cyclohexanone.

  2. Nano crystals of Ni doped Zn O semiconductor by Sol-Gel combustion method

    Energy Technology Data Exchange (ETDEWEB)

    Carrero, A.; Sagredo, V. [Universidad de Los Andes, Departamento de Fisica, Laboratorio de Magnetismo, 5101 Merida (Venezuela, Bolivarian Republic of); Larionova, J., E-mail: aneelyc@gmail.com [Universite Montpellier II, 2 Place Eugene Bataillon, 34090 Montpellier (France)

    2016-11-01

    Nanoparticles of the system Zn{sub 0.95}O were prepared by sol-gel self - combustion method and a study of their structural, optical and magnetic properties were conducted. X-ray diffraction study shows a hexagonal wurtzite structure for the nano compound. The formation of the wurtzite structure in Ni doped Zn O was further confirmed by Fourier transform infra-red spectrometry. Transmission electron microscopy revealed an average size of 31 nm for the particles. Optical absorption spectra shows that the band energy of Zn{sub 0.95}Ni{sub 0.}9{sub 5}O powders is about 2.54 eV at room temperature. A study of the magnetic properties of the nano powders of Zn O: Ni, reveals paramagnetic behavior, with interaction ferromagnetic between particles. (Author)

  3. Synthesis and Characterization of Modified Cellulose Acetate Propionate Nanocomposites via Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Patrycja Wojciechowska

    2013-01-01

    Full Text Available In this study novel organic-inorganic hybrid nanocomposites were synthesized from modified cellulose acetate propionate (MCAP via sol-gel reaction at ambient temperature. The inorganic phase was introduced in situ by hydrolysis-condensation of tetraethoxysilane (TEOS in different concentrations, under acid catalysis, in the presence of organic polymer dissolved in acetone. The chemical modification of CAP was monitored by infrared spectroscopy (IR. The nanocomposites structure was characterized by IR analysis and solid state 29Si NMR studies. The spectral data revealed that organic and inorganic phases are linked through covalent bound. Surface morphology of the samples and the degree of dispersion of inorganic phase in the polymer matrix were investigated using atomic force microscopy (AFM and scanning electron microscopy (SEM. The actual incorporation of the inorganic component into the hybrid nanocomposites was deducted from the residual weight according to thermogravimetric analysis (TGA.

  4. Biochemical properties of Bacillus sp. ITP-001 lipase immobilized with a sol gel process

    Directory of Open Access Journals (Sweden)

    Nayara Bezerra Carvalho

    2013-01-01

    Full Text Available This work presents biochemical characterization of a lipase from a new strain of Bacillus sp. ITP-001, immobilized using a sol gel process (IB. The results from the biochemical characterization of IB showed increased activity for hydrolysis, with 526.63 U g-1 at pH 5.0 and 80 ºC, and thermal stability at 37 ºC. Enzymatic activity was stimulated by ions such as EDTA, Fe+3, Mn+2, Zn+2, and Ca+2, and in various organic solvents. Kinetic parameters obtained for the IB were Km = 14.62 mM, and Vmax = 0.102 mM min-1 g-1. The results of biochemical characterization revealed the improved catalytic properties of IB.

  5. Organofunctional Trialkoxysilane Sol-Gel Precursors for Chemical Modi! cation of Textile Fibres

    Directory of Open Access Journals (Sweden)

    Jelena Vasiljević

    2017-07-01

    Full Text Available This paper reviews the use of organofunctional trialkoxysilane sol-gel precursors as contemporary fi nishing agents for the chemical modification of textile fires. The structures of organofunctional trialkoxysilanes are presented and compared to those of other silicon-based organic-inorganic hybrid materials. We describe the steps in the application procedure and the polysilsesquioxane coating fabrication on the surface of textile fibres. The functionalities, e.g., water and oil repellency, flame retardancy, antimicrobial properties, electrical conductivity and anti-static properties, are discussed in relation to the chemical structures of the precursor organic moiety, mechanisms and principals of the coating activity and its washing fastness. The most important published scientific results on organofunctional trialkoxysilanes applications to the surface of textile fibres are discussed with an emphasis on the creation of a multicomponent coating with multifunctional protective properties.

  6. Effect of Polymers (PEG and PVP on Sol-Gel Synthesis of Microsized Zinc Oxide

    Directory of Open Access Journals (Sweden)

    Thilagavathi Thirugnanam

    2013-01-01

    Full Text Available Fibers irregular and seed-like microcrystalline ZnO were synthesized by using a cost-effective and low temperature aqueous sol-gel method. Various polymers, namely, polyethylene glycol 6000 (PEG 6000 and polyvinyl pyrrolidone (PVP, were used as structure directing agents. The samples were characterized by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, and scanning electron microscopy (SEM. The X-ray diffraction pattern revealed the formation of phase-pure ZnO micropowders. It is observed that the polymers play an important role in modifying the surface morphology and the size of the crystallites. A compact granular morphology is observed for the ZnO samples without polymer. The samples exhibit microparticles of size 100 nm for PVP and for PEG-mediated growth, whereas microporous corrugated morphology is observed for added PEG-mediated micropowder. FTIR study is used to confirm the structural modifications occurring in the polymers.

  7. Photocatalytic and antibacterial activity of ZnO powders prepared via sol-gel method

    Directory of Open Access Journals (Sweden)

    Weerachai Sangchay

    2016-02-01

    Full Text Available We report on synthesis of ZnO powders via sol-gel method. The prepared powders were calcined at the temperature of 300, 500 and 700°C for 1 h with the heating rate of 10°C/min. The microstructures of the fabricated powders were characterized by SEM and XRD techniques, and the results show that all samples were the agglomeration and spherical shape and reveal only the wurtzite phase. The photocatalytic activities of the powders were also tested via the degradation of methylene blue (MB solution under UV irradiation. Finally, antibacterial activity efficiency was evaluated by the inactivation of E. coli. It was observed that higher calcined at the temperature gives better photocatalytic and antibacterial activity. With the highest calcined at the temperature investigated in this experiment (T700 condition the powders show photocatalytic and antibacterial activities of 80.06 and 99.00%, respectively.

  8. Surfactant-less Sol-Gel Technique for the Synthesis of Mg-ZnO Nanoparticle

    Directory of Open Access Journals (Sweden)

    Kadhim Wafaa A.

    2017-01-01

    Full Text Available In this study, sol–gel technique has been used to prepare nanoparticle Mg doped ZnO with 2 wt. % at low pH without using any capping or surfactant agent. The Mg-ZnO nanostructure, surface area and porosity, surface morphology and element analysis was analyzed by X-Ray Diffraction (XRD, Fourier Transforms Infra-Red (FTIR, N2 Physisorption and Field Emission Scanning Electron Microscopy with energy dispersive X-ray spectroscopy (FESEM-EDX. The characterizations confirmed that the surfactant is not necessary for sol-gel synthesis technique, whereby highly crystalline material with smaller crystallite size (30nm and high surface area (21.7 was obtained. Besides, the synthesis approach is useful for accurately immobilized the required amount of Mg as doping element on ZnO material with the accuracy up to 99.5% confirmed through EDX analysis.

  9. Seed-assisted sol-gel synthesis and characterization of nanoparticular V2O5/anatase

    DEFF Research Database (Denmark)

    Kunov-Kruse, Andreas Jonas; Kristensen, Steffen Buus; Riisager, Anders

    2009-01-01

    Nanoparticular supported vanadia materials with crystalline anatase support with a narrow size distribution around 12 nm have been synthesized by a new facile sol-gel, co-precipitation method using decomposable ammonium chloride seed crystals. The materials have been characterized by means of X......-ray powder diffraction, transmission electron microscopy and nitrogen physisorption. The synthesized high-surface area anatase particles allowed a loading of up to 15 wt.% vanadia without exceeding monolayer coverage of V2O5 in contrast to typical analogous industrial catalysts which only can accommodate 3......-5 wt.% vanadia. These materials are promising candidates for improved catalysts for, e.g., oxidation reactions and selective catalytic reduction of NO (X) in flue gases....

  10. Synthesis and Characterization of ZnO Nanoparticles Using Sol-gel Process

    Directory of Open Access Journals (Sweden)

    Jayasree ALURI

    2016-05-01

    Full Text Available In the Present work structural, morphological and compositional properties of ZnO nanopowders synthesized using Zinc nitrate and NaOH using sol-gel process were reported. The synthesized nanopowders were further analyzed using X-Ray Diffraction (XRD, Scanning electron microscopy (SEM and Fourier Transform Infrared (FTIR spectroscopic characterizations. Crystalline size and Lattice strain determined from XRD spectra. Morphology of Nanopowders viewed from SEM images observed at different magnifications. The presence of Functional groups analyzed from FTIR spectra. From the results it was very clear that particles synthesized using Zinc nitrate and NaOH plays a vital role on crystalline size, surface morphology of Nanopowders. Synthesized nanopowders can be utilized as building materials in fabrication of various optoelectronic devices including solar cells, LED’s etc. due to its significant structural, morphological and optical properties.

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

    Science.gov (United States)

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

    2013-07-01

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

  12. Sol- Gel Synthesis of Hematite Nanoparticles and Photo Degradation of Cibacron Red FN-R Dye

    Directory of Open Access Journals (Sweden)

    Ahlam M. Farhan

    2017-09-01

    Full Text Available This paper describes the synthesis of α- Fe2O3 nanoparticles by sol-gel route using carboxylic acid(2-hydroxy benzoic acid as gelatin media and its photo activity for degradation of cibacron red dye . Hematite samples are synthesized at different temperatures: 400, 500, 600, 700, 800 and 900 ᴼC at 700 ᴼC the α-Fe2O3 nanoparticles are formed with particle size 71.93 nm. The nanoparticles are characterized by XRD , SEM, AFM and FTIR . The 0.046 g /l of the catalyst sample shows high photo activity at 3x10-5M dye concentration in acidic medium at pH 3.

  13. New Synthesis of Ferrite-Silica Nanocomposites by a Sol-Gel Auto-Combustion

    Science.gov (United States)

    Cannas, C.; Musinu, A.; Peddis, D.; Piccaluga, G.

    2004-06-01

    A sol-gel autocombustion method was used to synthesize nanometric metal-oxide powders, and was extended for the first time to prepare ferrite-silica nanocomposites. The gels obtained by mixing suitable amounts of citric acid, metal nitrates, ammonia (pure phases) and tetraethylortosilicate (nanocomposites) were converted directly to ferrite (either γ-Fe2O3 or CoFe2O4) or ferrite-silica composites through a rapid autocombustion reaction. The combustion involves a thermally induced autocatalytic oxidation-reduction reaction between the nitrate and the citrate ions. The sample characterization by X-ray diffraction, transmission electron microscopy and N2 physisorption measurements revealed nanosized pure phase powders and nanocomposites in which small spherical nanoparticles (mean size 3.5 and 5.0nm, respectively for the γ-Fe2O3and CoFe2O4) are homogeneously dispersed over a mesoporous silica matrix.

  14. Optical and Mechanical Characterization of Zirconium Based Sol-Gel Coatings on Glass

    Directory of Open Access Journals (Sweden)

    Sitarz M.

    2016-12-01

    Full Text Available The basic factor limiting the use of glasses is their unsatisfactory mechanical strength. The improvement of the mechanical strength of glasses is usually obtained by applying their respective thin surface layers. The object of the research was glass coated with zirconium oxide. For the application of zirconium oxide layer, dip-coating method was used. The resulting materials were subjected to detailed examination of the microstructure (SEM, and mechanical tests (Vickers hardness and modulus of elasticity. In order to evaluate the optical characteristics, the tests were performed by UV/VIS. The thickness of the overlying layers were determined using the method of ellipsometry. The study showed that the obtained sol-gel layer of zirconium oxide (IV on glasses influence the improvement of the mechanical properties. It has been shown that the applied layers have high adhesion to the substrate.

  15. A novel green nonaqueous sol-gel process for preparation of partially stabilized zirconia nanopowder

    Directory of Open Access Journals (Sweden)

    Guo Feng

    2017-09-01

    Full Text Available A novel green nonaqueous sol-gel process was developed to prepare 3 mol% Y2O3-doped ZrO2 nanopowder from zirconium oxychloride and without need for washing of the obtained particles. It was shown that highly dispersive nanometer-scale zirconia powder with the particle size of 15–25 nm and BET surface area of 41.2 m2/g can be prepared. The sintering behaviour was also investigated. Density of the translucent body sintered at 1400 °C is 98.7 ± 0.3% of its theoretical density and the surface and cross section areas are dense without holes or other defects. The bending strength of the sintered sample is 928 ± 64 MPa.

  16. Synthesis of indium tin oxide nanoparticles by a nonhydrolytic sol-gel method

    Directory of Open Access Journals (Sweden)

    Gabriel M. Silva

    2012-01-01

    Full Text Available Indium tin oxide nanoparticles were synthesized in two different sizes by a nonhydrolytic sol-gel method. These powders were then transformed into ITO via an intermediate metastable state at between 300 and 600 ºC. The presence of characteristic O-In-O and O-Sn-O bands at 480 and 670 cm-1 confirmed the formation of ITO. The X-ray diffraction patterns indicated the preferential formation of metastable hexagonal phase ITO (corundum type as opposed to cubic phase ITO when the reflux time was less than 3 h and the heat treatment temperature was below 600 ºC. Particle morphology and crystal size were examined by scanning electron microscopy.

  17. Structural and optical properties of KNN nanoparticles synthesized by a sol-gel combustion method

    Science.gov (United States)

    Khorrami, Gh. H.; Mousavi, M.; Dowran, M.

    2017-05-01

    In this paper, potassium sodium niobate (KNN) nanopowders were successfully obtained by sol-gel combustion method. According to thermogravimetric analysis (TGA) results, the produced xerogel was calcined at 500∘C, 600∘C, and 700∘C to obtain KNN powders. The structural and optical properties of the prepared powders were studied using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, transmission electron microscopy (TEM), and UV-vis spectroscopy. The XRD patterns indicated formation of orthorhombic KNN samples. The Scherrer formula and size-strain plot (SSP) method were employed to calculate crystallite size and lattice strain of the KNN powders. The TEM image revealed that the average particle size of the prepared samples is about 30 nm and they have cubic shape. The optical band gap energy of the samples was calculated using UV-vis absorbance spectra of the samples along with Tauc relation.

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

    Science.gov (United States)

    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.

  19. SINTESIS LAPIS TIPIS BERBASIS NANOPARTIKEL TITANIA TERMODIFIKASI SILIKA SECARA SOL-GEL SEBAGAI BAHAN ANTIFOGGING

    Directory of Open Access Journals (Sweden)

    L.V. Rissa

    2012-09-01

    Full Text Available Telah dilakukan penelitian tentang sintesis lapis tipis berbasis nanopartikel titania termodifikasi silika (TiO2-SiO2 secara sol-gel sebagai bahan antifogging untuk (i mengetahui pengaruh temperatur kalsinasi terhadap energi band-gap, struktur dan ukuran kristal, serta porositas titania-silika, (ii mengetahui pengaruh komposisi sol terhadap karakteristik lapis tipis titania-silika yang meliputi hidrofilitas dan sifat transparan, serta (iii mengetahui kinerja antifogging lapis tipis titania-silika pada substrat kaca. Sintesis dilakukan melalui  metode sol-gel. Teknik pelapisan pada kaca menggunakan teknik celup, kemudian diaplikasikan sebagai bahan anti-kabut. Hasil sintesis TiO2-SiO2 dikarakterisasi dengan XRD untuk mengetahui struktur dan ukuran kristal, SEM-EDX untuk mengetahui morfologi dan komposisi padatan, serta DR-UV untuk mengetahui band-gap TiO2-SiO2. Hasil karakterisasi menunjukkan bahwa TiO2-SiO2 dengan 15% b/b silika  pada temperatur kalsinasi 500°C memiliki ukuran partikel dan band gap optimum  yaitu masing-masing sebesar 11,15 nm dan  3,20 eV. Hasil ini bersesuaian dengan hasil pengukuran sudut kontak minimum yaitu sebesar sebesar 14,49°. Hasil uji kinerja antifogging menunjukkan bahwa lapis tipis TiO2-SiO2 memiliki kemampuan untuk digunakan sebagai bahan anti-kabut. The research on synthesis of thin layer Based on TiO2 nanoparticle modified silica by sol gel as antifogging materials has been conducted to (i determine the effect of calcination temperature on the gap energy, structure and size of crystal, and porous titania-silica, (ii determine the effect of sol composition on thin layer titania-silica covering hydrophilic and transparent character, and (iii determine the performance of antifogging thin layer titania-silica on glass substrate. The synthesis is done by using sol-gel method. Dye technique was used to coat the glass, and then applied as antifogging materials. The result of synthesis of TiO2-SiO2

  20. TEM characterization of organic nanocrystals grown in sol-gel thin films

    Energy Technology Data Exchange (ETDEWEB)

    Monnier, Virginie; Bacia, Maria [CNRS and Universite Joseph Fourier, Institut Neel (France); Putaux, Jean-Luc [ICMG-CNRS, Centre de Recherches sur les Macromolecules Vegetales (France); Ibanez, Alain [CNRS and Universite Joseph Fourier, Institut Neel (France)], E-mail: alain.ibanez@grenoble.cnrs.fr

    2008-01-15

    The tetracene molecule (2,3-benzanthracene, C{sub 8}H{sub 12}) was used to synthesize nanocrystals grown in sol-gel thin films, ranging from 10 to 100 nm of diameter. This confined nucleation and growth was compared to microcrystallizations of the same molecule in free solution. Transmission electron microscopy (TEM) was used to characterize these two kinds of tetracene crystals. The observation was performed under low-dose illumination to avoid amorphization of the samples during electron irradiation. Spatial confinement and size distribution of micro- and nanocrystals were compared. Using electron microdiffraction and diffraction patterns simulations, we showed that free microcrystals and nanocrystals confined in gel glasses exhibit the same triclinic P-bar 1 structure. In addition, time-resolved spectroscopy was used to record fluorescence decays, showing a monoexponential fluorescence decay for nanocrystals while microcrystals exhibit a multiexponential decay. The simple signature of nanocrystals luminescence is promising for the future development of chemical or biological sensors.

  1. The effect of Ni and Fe doping on YBCO powder prepared by sol gel method

    Directory of Open Access Journals (Sweden)

    F Saeb

    2009-08-01

    Full Text Available  We fabricated YBa2Cu3-xMxO7- d (M=Ni, Fe bulk samples, with stochiometric amount 0≤x≤0.045 by sol-gel method. The phase analysis and microstructure of specimens were examined by XRD and SEM. The electrical resistivity was measured using standard four probe technique for 77-300K. Investigation of XRD spectrum by MAUD shows Ni and Fe ions substitute in Cu(2 and Cu(1 site, respectively. Transition temperature decreases in 93-87K for Ni-doped samples and 93-92K for Fe-doped series. It seems that the suppression of superconductivity has no direct correlation with the magnetism of ions itself .

  2. Ozonation and sol-gel method to obtain Cu/Cu O nanoparticles from cyanidation wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Soria A, M. J.; Puente S, D. M.; Carrillo P, F. R. [Universidad Autonoma de Coahuila, Facultad de Metalurgia, Carretera 57 Km 4.5, 25710 Monclova, Coahuila (Mexico); Garcia C, L. A. [Centro de Investigacion en Quimica Aplicada, Blvd. Enrique Reyna No. 140, Col. Los Pinos, 25253 Saltillo, Coahuila (Mexico); Velazquez S, J., E-mail: frrcarrillo@yahoo.com.mx [University of Texas at San Antonio, Department of Physics and Astronomy, San Antonio TX 78249 (United States)

    2015-07-01

    The extraction process of gold and silver by cyanidation generates large amounts of effluent which also contain contaminants such as cyanide and significant metal values such as copper. This paper presents the results of the removal and recovery of copper from ozonation treatment of a residual aqueous cyanide. The residual solution was treated by ozonation-precipitation to obtain a precipitate of copper. From this, copper nano composites obtained by Pechini modified sol-gel method were obtained. The compounds obtained were characterized by X-ray diffraction, showing a dependence of the type of compounds formed over time of ozonation and heat treatment of the gel. The particle size was measured by scanning electron microscopy and calculated by the Scherrer equation, being between 50 and 120 nm. (Author)

  3. Structural properties and gas sensing behavior of sol-gel grown nanostructured zinc oxide

    Energy Technology Data Exchange (ETDEWEB)

    Rajyaguru, Bhargav; Gadani, Keval; Kansara, S. B.; Pandya, D. D.; Shah, N. A.; Solanki, P. S., E-mail: piyush.physics@gmail.com [Department of Physics, Saurashtra University, Rajkot – 360 005 (India); Rathod, K. N.; Solanki, Sapana [Department of Physics, Saurashtra University, Rajkot – 360 005 (India); V.V.P. Engineering College, Gujarat Technological University, Rajkot – 360 005 (India)

    2016-05-06

    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 20.96 nm 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.

  4. Synthesis and Characterization of CZTS Thin Films by Sol-Gel Method without Sulfurization

    Directory of Open Access Journals (Sweden)

    Xiaoqi Yu

    2014-01-01

    Full Text Available One process of layer-by-layer sol-gel deposition without sulfurization was developed. The CZTS films with 1.2 μm and the sulfur ratio of ~48% were prepared and their characteristics were measured. The as-deposited and annealed films are of Kesterite structure. The as-deposited films do not present obvious electric conduction type. However, the annealed 9-LAY-ANN film is p-type conduction and has sheet resistance of 4.08 kΩ/□ and resistivity of 4.896 × 10−1 Ω·cm. The optic energy gap is 1.50 eV for as-deposited films and is 1.46 eV after being annealed. The region deposited by using Lo-Con solution is more compact than that by the Hi-Con solution from SEM morphology images.

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

    Directory of Open Access Journals (Sweden)

    Alexis Fischer

    2013-03-01

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

  6. Sol-gel fabrication and optical absorption properties of C-NiO nanocomposite coatings

    CSIR Research Space (South Africa)

    Tile

    2010-12-01

    Full Text Available stream_source_info Tile1_2010.pdf.txt stream_content_type text/plain stream_size 1961 Content-Encoding ISO-8859-1 stream_name Tile1_2010.pdf.txt Content-Type text/plain; charset=ISO-8859-1 Sol-gel fabrication and optical... absorption properties of C-NiO nanocomposite coatings Ngcali Tile1,2, Kittessa Roro1, Andrew Forbes1,2 1 CSIR National Laser Centre, Pretoria 2 School of physics, university of KwaZulu-Natal, Durban 0 200 400 600 800 1000 1200 0 0.2 0.4 0.6 0...

  7. Nanostructured porous sol-gel materials for applications in solar cells engineering

    Energy Technology Data Exchange (ETDEWEB)

    Zakharchenko, R.V.; Diaz-Flores, L.L.; Perez-Robles, J.F.; Vorobiev, Y.V. [CINVESTAV-IPN, Unidad Queretaro, Libramiento Norponiente 2000, Juriquilla, Queretaro (Mexico); Gonzalez-Hernandez, J. [CIMAV, Miguel de Cervantes 120, Chihuahua (Mexico)

    2005-06-01

    Two nanostructured Sol-Gel composite materials for application in solar cells engineering were created and studied: the TiO{sub 2}/SiO{sub 2} films for antireflecting coatings of cells, and PMMA/SiO{sub 2} insulating layers on metal substrate for efficient heat extraction from a cell. Structural and optical investigation of the first composite proved that its parameters are adequate to serve the purpose; when doped with the dye absorbing UV light and emitting in the visible, it could also increase quantum yield of a cell. The second composite is designed for use in a hybrid PV/Thermal system, where it could optimize the heat exchange between a cell and solar plane collector, which also leads to an increase of efficiency of the system. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  8. Organo-silica-titania nanocomposite elaborated by sol-gel processing with tunable optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Franc, J. [Laboratoire Traitement du Signal et Instrumentation, CNRS-UMR 5516, Universite Jean Monnet, 10 rue Barrouin, 42100 Saint-Etienne, 18 rue Benoit Lauras, F-42000 Saint-Etienne (France)]. E-mail: janyce.franc@univ-st-etienne.fr; Blanc, D. [Laboratoire Traitement du Signal et Instrumentation, CNRS-UMR 5516, Universite Jean Monnet, 10 rue Barrouin, 42100 Saint-Etienne, 18 rue Benoit Lauras, F-42000 Saint-Etienne (France); Zerroukhi, A. [Laboratoire de Rheologie des Matieres Plastiques, UMR CNRS 5156, 23 rue Paul Michelon, F-42023 Saint-Etienne Cedex 2 (France); Chalamet, Y. [Laboratoire de Rheologie des Matieres Plastiques, UMR CNRS 5156, 23 rue Paul Michelon, F-42023 Saint-Etienne Cedex 2 (France); Last, A. [Research Center Karlsruhe, Institute for Microstructure Technology, P.O. Box 3640, 76021 Karlsruhe (Germany); Destouches, N. [Laboratoire Traitement du Signal et Instrumentation, CNRS-UMR 5516, Universite Jean Monnet, 10 rue Barrouin, 42100 Saint-Etienne, 18 rue Benoit Lauras, F-42000 Saint-Etienne (France)

    2006-04-15

    Organically modified silica-titania thin films were elaborated by a sol-gel process and UV assisted photopolymerisation. Two different chelating agents, methacrylic acid (MAA) and a {beta}-diketone (2-(methacryloyloxy) ethyl acetoacetone (MAEA)) were compared in this work. It was demonstrated that the choice of the chelating agent is a key parameter to increase the molar ratio Si:Ti and therefore raise the refractive index of the material. {beta}-Diketone has proven to be a good candidate to stabilise the titanium precursor and its effects were compared to those observed with methacrylic acid. Fourier transform infrared spectroscopy was used to monitor the material formation and modification upon irradiation. M-lines spectroscopy was used to measure the refractive index of the material that varied between 1.51 and 1.59 depending on the titanium molar concentration. Optical properties were analysed in view of applications in the field of micro-optics and optical coatings.

  9. Large low-field magnetoresistance in nanocrystalline magnetite prepared by sol-gel method.

    Science.gov (United States)

    Lu, Z L; Zou, W Q; Lv, L Y; Liu, X C; Li, S D; Zhu, J M; Zhang, F M; Du, Y W

    2006-11-30

    Nanocrystalline magnetite Fe3O4 samples with a grain size of about 40 nm have been synthesized by an optimized sol-gel method. The single phase of spinel magnetite was confirmed by both X-ray diffraction and transmission electron microscopy. It has been found that the magnetoresistance of the samples at low field (LFMR) is relatively large, and with the decrease of temperature its value at a field of 0.5 T changes dramatically from -2.5% at 300 K to -17.0% at 55 K. With the further decrease of temperature a sharp drop occurs for the magnitude of the magnetoresistance (MR), regarded as a spin (cluster) glass transition in the surface region of the grains that can be confirmed by the zero-field-cooled and field-cooled magnetization and ac susceptibility measurement. The mechanism of the magnetic and transport properties was discussed.

  10. Development of flame retardant cotton fabric based on ionic liquids via sol-gel technique.

    Science.gov (United States)

    Bentis, A.; Boukhriss, A.; Boyer, D.; Gmouh, S.

    2017-10-01

    In this study, flame retardant cotton fabrics were developed by the sol-gel method, in order to enhance their flame retardant proprieties. For this aim, seven sols were prepared using tetraethylorthosilicate (TEOS) and different ionic liquids (ILs) consist on pyridinium and Methylimidazolium cations with different anions such as: PF6‑, CH3COO‑, and Br‑. Those sols were applied separately to the cotton fabrics by a pad-dry-cure process. The flame retardant properties of functionalized cotton fabrics before and after washing were determined by the vertical flame tests according to ISO6940:2004(F) standard. The effects of anions have been thoroughly investigated, aiming at the optimization of the targeted properties. Thermogravimetric and mechanical according to NF EN ISO 13934-1:2013standard, analyses have been also investigated. The results showed that flame retardancy, thermal stability and mechanical properties of treated fabrics were enhanced by using ionic liquids.

  11. Microencapsulation of probiotic bacteria using thermo-sensitive sol-gel polymers for powdered infant formula.

    Science.gov (United States)

    Penhasi, Adel

    2015-01-01

    In this study the application of thermo-sensitive sol-gel polymers in microencapsulation formulation of probiotic bacteria, Bifidobacterium animalis spp lactis, for powdered infant formula (PIF), which is reconstituted at 70 °C, has been assessed. A double-layered microcapsule containing hydroxypropyl methyl cellulose (HPMC) as an inner layer and an outer layer, as the smart coating layer, based on a combination of hydroxypropyl cellulose (HPC) and poloxamer was designed. Generally, this specific microencapsulation provided superior protection against the reconstitution temperature. A high molecular weight of HPC and a greater thickness of the smart coating layer resulted in a delayed release of the bacteria from the microcapsules especially in the PIF composition. However, this was compensated by a high stability of the bacteria at 70 °C. Both the surface texture and particle size distribution of microcapsules have been respectively characterised by scanning electron microscopy and particle size analysis.

  12. Investigation of the Peroxovanadate Sol-Gel Process and Characterization of the Gels

    Energy Technology Data Exchange (ETDEWEB)

    Fontenot, Craig Joseph [Iowa State Univ., Ames, IA (United States)

    2001-01-01

    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.

  13. Fabrication and properties of nanocrystalline zinc oxide thin film prepared by sol-gel method

    Directory of Open Access Journals (Sweden)

    Sumetha Suwanboon

    2008-01-01

    Full Text Available Zinc oxide (ZnO thin films were prepared on glass substrate by sol-gel dip-coating method. The structural properties were investigated by x-ray diffraction (XRD method and atomic force microscope (AFM. The optical properties were measured by UV-Vis spectrophotometer. The XRD patterns showed that the films formed preferred orientation along c-axis which increased as a function of polyvinyl pyrrolidone (PVP concentration. The films gave the crystallite size of 15-18 nm calculated by Scherrer’s formula and grain size of 48-70 nm measured by AFM at different PVP concentrations. The direct optical band gap of the films was in the range of 3.80-4.08 eV.

  14. Cultivation and energy efficient harvesting of microalgae using thermoreversible sol-gel transition

    Science.gov (United States)

    Estime, Bendy; Ren, Dacheng; Sureshkumar, Radhakrishna

    2017-01-01

    Microalgae represent a promising source of renewable biomass for the production of biofuels and valuable chemicals. However, energy efficient cultivation and harvesting technologies are necessary to improve economic viability. A Tris-Acetate-Phosphate-Pluronic (TAPP) medium that undergoes a thermoreversible sol-gel transition is developed to efficiently culture and harvest microalgae without affecting the productivity as compared to that in traditional culture in a well-mixed suspension. After seeding microalgae in the TAPP medium in a solution phase at 15 °C, the temperature is increased by 7 °C to induce gelation. Within the gel, microalgae are observed to grow in large clusters rather than as isolated cells. The settling velocity of the microalgal clusters is approximately ten times larger than that of individual cells cultured in typical solution media. Such clusters are easily harvested gravimetrically by decreasing the temperature to bring the medium to a solution phase.

  15. Europium incorporated in silica matrix obtained by sol-gel: luminescent materials

    Directory of Open Access Journals (Sweden)

    Nassar Eduardo José

    2003-01-01

    Full Text Available In this work we report some aspects of the chemistry involved in the preparation of modified silicon oxide by the sol-gel process. Europium III compounds were used as luminescent probe. An organic-inorganic hybrid was obtained by hydrolysis of tetraethylorthosilicate (TEOS and 3-aminopropyltriethoxysilane (APTS. The Eu III compounds were added in different ways. In the first, silica was prepared in the presence of Eu III, and in the second, Eu III was added on the silica surface. These materials were studied by luminescence, infrared spectroscopy and termogravimetric analysis. The results obtained for the hybrid material show different behavior for Eu III emission, which could be excited by the antenna effect and the influence of the surrounding in the luminescence quenching. The thermogravimetric data present different mass loss in samples to range temperature 50 - 150 °C. Thermogravimetric and infrared spectra showed that inorganic polymers incorporated the organic part.

  16. Sol-gel coatings: An alternative route for producing planar optical waveguides

    Energy Technology Data Exchange (ETDEWEB)

    Rey-Garcia, F.; Gomez-Reino, C. [Unidad Asociada de Optica and Microoptica GRIN (CSIC-ICMA), Departamento de Fisica Aplicada, Escola Universitaria de Optica e Optometria, Universidade de Santiago de Compostela, Campus Sur s/n, E-15782 Santiago de Compostela (Spain); Flores-Arias, M.T., E-mail: maite.flores@usc.es [Unidad Asociada de Optica and Microoptica GRIN (CSIC-ICMA), Departamento de Fisica Aplicada, Escola Universitaria de Optica e Optometria, Universidade de Santiago de Compostela, Campus Sur s/n, E-15782 Santiago de Compostela (Spain); De La Fuente, G.F., E-mail: xerman@unizar.es [Instituto de Ciencia de Materiales de Aragon (CSIC-Universidad de Zaragoza), Maria de Luna 3, E-50018 Zaragoza (Spain); Duran, A. [Instituto de Ceramica y Vidrio (CSIC), Kelsen 5, E-28049, Madrid (Spain); Castro, Y., E-mail: castro@icv.csic.es [Instituto de Ceramica y Vidrio (CSIC), Kelsen 5, E-28049, Madrid (Spain)

    2011-09-01

    Inorganic and hybrid planar waveguides with different compositions (silica-titania, methacrylate-silica-cerium oxide, zirconia-cerium oxide and silica-zirconia) have been obtained by sol-gel synthesis followed by dip-coating. Soda-lime glass slides and conventional commercial window glass were used as substrates. The thickness and refractive index of the coatings were determined by profilometry and Spectroscopic Ellipsometry. Waveguide efficiency was measured at ca. 70.8% with a He-Ne laser beam, coupled with an optical microscope objective into and out of the waveguiding layer via a double prism configuration. Thicknesses between 150 and 2000 nm, along with refractive index values ranging between 1.45 and {approx} 1.99 ({lambda} = 633 nm) were obtained depending on the sol composition and the dip-coating conditions. This wide range of values allows designing multilayered guides that can be used in a variety of applications.

  17. Immobilized Aspergillus niger Lipase with SiO2 Nanoparticles in Sol-Gel Materials

    Directory of Open Access Journals (Sweden)

    Li Xu

    2016-09-01

    Full Text Available Lipase from Aspergillus niger was “doubly immobilized” with SiO2 nanoparticles in sol-gel powders prepared via the base-catalyzed polymerization of tetramethoxysilane (TMOS and methyltreimethoxysilane (MTMS. The hydrolytic activity of the immobilized lipase was measured using the p-nitrophenyl palmitate hydrolysis method. The results showed that the optimum preparation conditions for the gels were made using a MTMS/TMOS molar ratio of 5, 60 mg of SiO2 nanoparticles, a water/silane molar ratio of 12, 120 mg of enzyme supply, and 120 μL of PEG400. Under the optimal conditions, the immobilized lipase retained 92% of the loading protein and 94% of the total enzyme activity. Characteristic tests indicated that the immobilized lipase exhibited much higher thermal and pH stability than its free form, which shows great potential for industrial applications.

  18. Sol-gel methods for synthesis of aluminosilicates for dental applications.

    Science.gov (United States)

    Cestari, Alexandre

    2016-12-01

    Amorphous aluminosilicates glasses containing fluorine, phosphorus and calcium are used as a component of the glass ionomer dental cement. This cement is used as a restorative, basis or filling material, but presents lower mechanical resistance than resin-modified materials. The Sol-Gel method is a possible route for preparation of glasses with lower temperature and energy consumption, with higher homogeneity and with uniform and nanometric particles, compared to the industrial methods Glass ionomer cements with uniform, homogeneous and nanometric particles can present higher mechanical resistance than commercial ionomers. The aim of this work was to adapt the Sol-Gel methods to produce new aluminosilicate glass particles by non-hydrolytic, hydrolytic acid and hydrolytic basic routes, to improve glass ionomer cements characteristics. Three materials were synthesized with the same composition, to evaluate the properties of the glasses produced from the different methods, because multicomponent oxides are difficult to prepare with homogeneity. The objective was to develop a new route to produce new glass particles for ionomer cements with possible higher resistance. The particles were characterized by thermal analysis (TG, DTA, DSC), transmission electron microscopy (TEM), X-ray diffraction (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS). The glasses were tested with polyacrylic acid to form the glass ionomer cement by the setting reaction. It was possible to produce distinct materials for dental applications and a sample presented superior characteristics (homogeneity, nanometric particles, and homogenous elemental distribution) than commercial glasses for ionomer cements. The new route for glass production can possible improve the mechanical resistance of the ionomer cements. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Low temperature self-agglomeration of metallic Ag nanoparticles on silica sol-gel thin films

    Energy Technology Data Exchange (ETDEWEB)

    Akhavan, O; Azimirad, R; Moshfegh, A Z [Department of Physics, Sharif University of Technology, PO Box 11155-9161, Tehran (Iran, Islamic Republic of)], E-mail: oakhavan@sharif.edu

    2008-10-07

    A facile sol-gel synthesis for self-agglomeration of metallic silver nanoparticles, with fcc crystalline structure, on the silica surface in a low annealing temperature has been introduced. X-ray photoelectron spectroscopy (XPS) revealed initial agglomeration ({approx}30 times greater than the nominal concentration of Ag) of the nanoparticles on the surface of the dried film (100 deg. C) and also their oxidation as well as easy diffusion (with 0.08 eV required activation energy) into the porous silica thin films, by increasing the annealing temperature (200-400 deg. C). By raising the Ag concentration from 0.2 to 1.6 mol% in the sol, the average size of the Ag nanoparticles increased from {approx}5 to 37 nm corresponding to a redshift of the optical plasmon resonance absorption peak from 404 to 467 nm. The high concentration of Ag (1.6 mol%) in the sol resulted in a rough surface containing compact nanoparticles. Using power spectral density analysis of the atomic force microscopy images, we have found that the highest contributions in the surface roughness of the dried silica films were caused by the particles ranging from {approx}62 to 159 nm. The particles smaller than {approx}39 nm did not show any detectable contributions in the surface roughness of the dried silica film. Based on the XPS analysis, a mechanism has also been proposed for the self-agglomeration of the Ag nanoparticles on the surface of the aqueous sol-gel silica thin films.

  20. Magnetic properties of sol-gel synthesized C-doped ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Dung, Nguyen Duc, E-mail: dung.nguyenduc@hust.edu.vn [Advanced Institute of Science and Technology (AIST), Hanoi University of Science and Technology, No.1 Dai Co Viet, Hanoi (Viet Nam); Son, Cao Thai; Loc, Pham Vu; Cuong, Nguyen Huu; Kien, Pham The; Huy, Pham Thanh [Advanced Institute of Science and Technology (AIST), Hanoi University of Science and Technology, No.1 Dai Co Viet, Hanoi (Viet Nam); Ha, Ngo Ngoc [International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology, No.1 Dai Co Viet, Hanoi (Viet Nam)

    2016-05-25

    ZnO doping with Carbon (C-doped ZnO) materials were prepared by sol-gel technique following with a heat treatment process. Single phase of Wurtzite crystal structure of ZnO was concluded via x-ray diffraction (XRD) with a large amount of excess C tracking by energy dispersive X-ray spectroscopy (EDX) analysis. Two types of ZnO crystals (twinning particles) with different grain sizes and shapes were identified via scanning electron microscopy (FE-SEM). The first type has a smaller grain size of about 20 nm and hexagonal shape. And the second type has a larger grain size of about 80–120 nm and round shape. C substitutions of both Zn and O sites to form C–O and C–Zn bonds were conclusively confirmed via x-ray photoelectron spectroscope (XPS). Experimental evidences for the co-existence of different ferromagnetic phases in the materials are reported and discussed. Two Curie points at high temperatures (>500 °C) are presented. A metamagnetic transition was observed at magnetic field H = 19.2 kOe which was related to the co-existence of ferromagnetic phases. These involve in the formation of twinning C-doped ZnO nanoparticles. - Highlights: • Formation of sol-gel prepared single phase wurtzite ZnO nanoparticles. • Two morphological C-doped ZnO nanoparticles of different grain sizes. • The room temperature ferromagnetism. • An abnormal metamagnetic transition at magnetic field H = 19.2 kOe. • Two different Curie points (T{sub C}) at 500–600 °C.

  1. Obtención de Cordierita por Sol-Gel a partir de fuentes nacionales cubanas

    Directory of Open Access Journals (Sweden)

    Pacheco, P.

    2003-10-01

    Full Text Available For cordierite synthesis through the Sol-Gel method, the sodium silicate obtained from the dissolution of a solid residue coming from the aluminum sulfate production based on kaolin, was used. The sources of magnesium and aluminum were obtained using the technologies previously developed by CIPIMM. The elements were mixed in a determined order and quantity to obtain a Gel with cordierite stechiometry. The gel was washed and dried and briquettes were made to treat them at different temperatures, obtaining cordierite in a major phase at 1200ºC. This was checked through the X-Ray diffraction analysis of the products coming from the thermical treatment. The method used when compared to the traditional ones, permitted to reduce crystallization temperature, obtaining more dense products and clean technology.

    Para la síntesis de la Cordierita por el método de Sol-Gel se utilizó, el silicato de sodio, obtenido de la disolución de un residuo sólido proveniente de la producción de sulfato de aluminio a partir de caolín. Los precursores de magnesio y aluminio fueron obtenidos utilizando las tecnologías previamente desarrolladas por el CIPIMM. Los materiales fueron mezclados en un orden y cantidad determinada hasta obtener el Gel con estequiometría de cordierita. El gel fue lavado, secado, briqueteado y tratado térmicamente a diferentes temperaturas, lográndose cordierita en fase mayoritaria a los 1200 ºC, lo cual fue corroborado mediante el análisis por difracción de rayos X de los productos del tratamiento térmico. El método utilizado comparado con los tradicionales permitió reducir la temperatura de cristalización, obtener productos más densificados y tecnología limpia.

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

    Science.gov (United States)

    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. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Cuong M. Nguyen

    2015-02-01

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

  4. Probing sol-gel matrices microenvironments by PGSE HR-MAS NMR.

    Science.gov (United States)

    Ferreira, Ana S D; Barreiros, Susana; Cabrita, Eurico J

    2017-05-01

    We applied Pulsed Gradient Spin Echo diffusion with high-resolution magic angle spinning NMR to study sol-gel matrices used to encapsulate enzymes for biocatalysis (TMOS/MTMS and TMOS/BTMS) to gain insight into the local chemical microenvironment. Transport properties of solvents with different polarities (1-pentanol, acetonitrile and n-hexane) were studied through their apparent self-diffusion coefficients. The spin echo attenuation of the solvents shows two distinct diffusion domains, one with fast diffusion (Dfast ) associated with interparticle diffusion and another with slow diffusion (Dslow ) corresponding to the displacement inside the pores within the sol-gel particles. The analysis of the root mean square displacements at different diffusion times showed that the Dfast domain has a free diffusion regime in both matrices (the root mean square displacement is linearly dependent of the diffusion time), while the Dslow domain shows a different regime that depends on the matrix. We investigated the exchange regime between the two diffusion sites. In both matrices, n-hexane was in intermediate exchange between diffusion domains, while the polar solvents were in slow exchange in TMOS/BTMS and in intermediate exchange in TMOS/MTMS. Data were fitted for TMOS/BTMS with the Kärger model, and the physical parameters were obtained. The results add to the evidence that the pores are a hydrophobic environment but that the presence of some free hydrophilic groups inside the pore, as observed in the TMOS/BTMS, has a key role in slowing down the exchange of polar solvents and that this is relevant to explain previously reported enzyme activity in these materials. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  5. Nano rods for coloured glasses obtained by hybrid sol-gel coating.

    Science.gov (United States)

    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.

  6. Synthetic aspects and characterization of polypropylene-silica nanocomposites prepared via solid-state modification and sol-gel reactions

    NARCIS (Netherlands)

    Jain, S; Goossens, H; Picchioni, F; Magusin, P; Mezari, B

    2005-01-01

    A new route is developed by combining solid-state modification (SSM) by grafting vinyl triethoxysilane (VTES) with a sol-gel method to prepare PP/silica nanocomposites with varying degree of adhesion between filler and matrix. VTES was grafted via SSM in porous PP particles. Bulk polymerization

  7. Athermal silicon optical add-drop multiplexers based on thermo-optic coefficient tuning of sol-gel material.

    Science.gov (United States)

    Namnabat, Soha; Kim, Kyung-Jo; Jones, Adam; Himmelhuber, Roland; DeRose, Christopher T; Trotter, Douglas C; Starbuck, Andrew L; Pomerene, Andrew; Lentine, Anthony L; Norwood, Robert A

    2017-09-04

    Silicon photonics has gained interest for its potential to provide higher efficiency, bandwidth and reduced power consumption compared to electrical interconnects in datacenters and high performance computing environments. However, it is well known that silicon photonic devices suffer from temperature fluctuations due to silicon's high thermo-optic coefficient and therefore, temperature control in many applications is required. Here we present an athermal optical add-drop multiplexer fabricated from ring resonators. We used a sol-gel inorganic-organic hybrid material as an alternative to previously used materials such as polymers and titanium dioxide. In this work we studied the thermal curing parameters of the sol-gel and their effect on thermal wavelength shift of the rings. With this method, we were able to demonstrate a thermal shift down to -6.8 pm/°C for transverse electric (TE) polarization in ring resonators with waveguide widths of 325 nm when the sol-gel was cured at 130°C for 10.5 hours. We also achieved thermal shifts below 1 pm/°C for transverse magnetic (TM) polarization in the C band under different curing conditions. Curing time compared to curing temperature shows to be the most important factor to control sol-gel's thermo-optic value in order to obtain an athermal device in a wide temperature range.

  8. The application of silicon sol-gel technology to forensic blood substitute development: Mimicking aspects of whole human blood rheology.

    Science.gov (United States)

    Stotesbury, Theresa; Illes, Mike; Wilson, Paul; Vreugdenhil, Andrew J

    2017-01-01

    Solution-gelation chemistry has promising applications in forensic synthetic blood substitute development. This research offers a silicon-based sol-gel approach to creating stable materials that share similar rheological properties to that of whole human blood samples. Room temperature, high water content, silicon sol-gels were created using the organosilane precursors 3-glycidoxypropyltrimethoxysilane and tetraethylorthosilicate along with various concentrations of filler and pigment. Shear-thinning non-Newtonian properties were observed within most formulations of the presented materials. The effects of colloidal concentration, temperature, age and filler addition on the viscosity of the sol-gels were investigated. SEM-EDS analysis was used to identify the behavior of the fillers within the film and support their inclusion for basic bloodstain pattern simulation. A final proposed candidate sol-gel was assessed using a previously reported passive drip simulation test on a hard, dry surface and passed. This works represents encouraging development in providing safe material alternatives to using whole human blood for forensic training and research. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  9. ELISA AND SOL-GEL BASED IMMUNOAFFINITY PURIFICATION OF THE PYRETHROID BIOALLETHRIN IN FOOD AND ENVIRONMENTAL SAMPLES

    Science.gov (United States)

    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...

  10. Tailoring Wettability Through the Surface Modification of Electro-spun Polymers by Plasma and Sol-gel Treatments

    Science.gov (United States)

    2014-11-01

    nanoparticles , sol-gel reactions and by producing beads-on-a-string morphologies. Low surface energy was added by using fluorinated polymers, or through... nanoparticles ................................................................... 13 3.2.3 Effect of TEOS addition to electrospinning solutions...could benefit a number of applications: anti-biofouling; corrosion resistant paints for hulls; coatings that prevent ice buildup; water, stain and

  11. Femtosecond double proton transfer dynamics in [2,2'-bipyridyl]-3,3'-diol in sol-gel glasses

    NARCIS (Netherlands)

    Prosposito, P.; Marks, D.R.A.; Zhang, H.; Glasbeek, M.

    1998-01-01

    Abstract: Intramolecular excited state double proton-transfer dynamics has been studied for [2,2'-bipyridyl]-3,3'-diol (BP(OH)2) in sol-gel glass. By means of the femtosecond fluorescence up-conversion technique, the spectral dependence of the fluorescence transients obtained for BP(OH)2 in a few

  12. Modular bioink for 3D printing of biocompatible hydrogels : sol-gel polymerization of hybrid peptides and polymers

    NARCIS (Netherlands)

    Echalier, C.; Levato, R.; Mateos-Timoneda, Miguel A; Castaño, O.; Déjean, S.; Garric, X.; Pinese, C.; Noël, D.; Engel, E.; Martinez, J.; Mehdi, A.; Subra, G.

    2017-01-01

    An unprecedented generic system allowing the 3D printing of peptide-functionalized hydrogels by soft sol-gel inorganic polymerization is presented. Hybrid silylated inorganic/bioorganic blocks are mixed in biological buffer in an appropriate ratio, to yield a multicomponent bioink that can be

  13. Sol-gel synthesis of ternary phosphate-ZrO2-SiO2 catalysts for alcohol dehydration

    National Research Council Canada - National Science Library

    Zhuang, Quan; Miller, Jack M

    2001-01-01

    ..., DRIFTS. Résumé : On a synthétisé des catalyseurs phosphate–ZrO 2 –SiO 2 par la méthode sol-gel utilisant du phosphite de triéthyle, du propylate de zirconium et de l’orthosilicate de té...

  14. Temperature annealing effect on structural and optical properties of ZnO thin films prepared by sol-gel method

    Directory of Open Access Journals (Sweden)

    Elamal Bouzit S.

    2013-09-01

    Full Text Available ZnO thin films have been synthesized by sol-gel method. The effect of the annealing temperature on the morphological, structural and optical properties of the ZnO thin films was investigated. A good crystllinity and good transmittance in the visible spectrum was obtained at the annealing temperature of 400°C.

  15. TEM study of indium and gallium nitride nanocrystals in silica gasses obtained by the sol-gel method.

    Science.gov (United States)

    Krajczyk, L; Jabłoński, J M; Nyk, M; Strek, W; Misiewicz, J

    2006-09-01

    GaN and InN nanocrystals in silica glasses prepared by the sol-gel method were studied by transmission electron microscopy techniques. Morphology, structure and phase composition of silica gel containing Ga or In as function of the calcination and nitridation temperature were investigated.

  16. Sol-Gel Application for Consolidating Stone: An Example of Project-Based Learning in a Physical Chemistry Lab

    Science.gov (United States)

    de los Santos, Desiree´ M.; Montes, Antonio; Sa´nchez-Coronilla, Antonio; Navas, Javier

    2014-01-01

    A Project Based Learning (PBL) methodology was used in the practical laboratories of the Advanced Physical Chemistry department. The project type proposed simulates "real research" focusing on sol-gel synthesis and the application of the obtained sol as a stone consolidant. Students were divided into small groups (2 to 3 students) to…

  17. Influence of silane on the structure of polystyrene prepared by sol-gel coatings via UV curing

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    Balbay, Senay; Acıkgoz, Caglayan

    2017-11-01

    Light, heat, oxygen, moisture, ozone, atmospheric pollution and biological effects are the most important effectives wreak to chemical degradation in the polymer structure. In result of chemical degradation on the polymer consist of problems such as discoloration, brittleness, surface cracks, perspiration, crumbling, smell, surface acidity. In this work, it is aimed to improve the problem of the polystyrene (PS) material against chemical degradation. For this reason, PS is coated with silica sol-gel hybrid coating. Silica sol-gel was synthesized by using vinyltrimethoxysilane (VTMS) as a cross-linker and tetraethylorthosilicate (TEOS) as a silica source. Firstly, four different pre-treatment technique (oven, vacuum oven, lyophilizer and freezing) was studied to determine the most suitable pre-treatment technique for coating on PS substrate of sol-gel prepared with initial formulation (S1). A freezing technique gave the best results for coating sample. The change of surface colour of coated PS was measured by CIE L*a*b* methods. Secondly, the most suitable curing agent (Irgacure 184, Irgacure 819, Darocur 1173 and TiO2 as crystalline anatase phase) was determined to coat the sol-gel on PS. It was determined to the lowest yellowing of PS surface hybrid coated as UV curing of TEOS sol modified by VTMS and TiO2 as photo-initiators. Finally, the chemical and morphological structure of the coated PS samples was determined by FT-IR and SEM instruments, respectively.

  18. ITO/Poly(Aniline/Sol-Gel Glass: An Optically Transparent, pH-Responsive Substrate for Supported Lipid Bilayers

    Directory of Open Access Journals (Sweden)

    Ahmed Al-Obeidi

    2013-01-01

    Full Text Available Described here is fabrication of a pH-sensitive, optically transparent transducer composed of a planar indium-tin oxide (ITO electrode overcoated with a poly(aniline (PANI thin film and a porous sol-gel layer. Adsorption of the PANI film renders the ITO electrode sensitive to pH, whereas the sol-gel spin-coated layer makes the upper surface compatible with fusion of phospholipid vesicles to form a planar supported lipid bilayer (PSLB. The response to changes in the pH of the buffer contacting the sol-gel/PANI/ITO electrode is pseudo-Nernstian with a slope of 52 mV/pH over a pH range of 4–9. Vesicle fusion forms a laterally continuous PSLB on the upper sol-gel surface that is fluid with a lateral lipid diffusion coefficient of 2.2 μm2/s measured by fluorescence recovery after photobleaching. Due to its lateral continuity and lack of defects, the PSLB blocks the pH response of the underlying electrode to changes in the pH of the overlying buffer. This architecture is simpler to fabricate than previously reported ITO electrodes derivatized for PSLB formation and should be useful for optical monitoring of proton transport across supported membranes derivatized with ionophores and ion channels.

  19. Effect of Aging Time and Film Thickness on the Photoelectrochemical Properties of TiO2 Sol-Gel Photoanodes

    Directory of Open Access Journals (Sweden)

    D. Regonini

    2014-01-01

    Full Text Available This work has focused on the investigation of a non-aqueous based sol-gel process to produce TiO2 based photoelectrodes for solar water splitting. In particular, the effect of the aging time of the sol and TiO2 film thickness on the photoelectrochemical properties of the photoanodes has been investigated. In order to achieve optimal performances (i.e., photocurrent density up to 570 µA/cm2 and IPCE of 26% at 300 nm, the sol needs to be aged for 3 to 6 h, before being dip-coated to produce the photoanodes. The importance of the aging time can also be appreciated from the optical properties of the TiO2 films; the absorbance threshold of the sol-gel aged for 3–6 h is slightly shifted towards longer wavelenghts in comparison to 0 h aging. Aging is necessary to build up a well-interconnected sol-gel network which finally leads to a photoelectrode with optimized light absorption and electron collection properties. This is also confirmed by the higher IPCE signal of aged photoelectrodes, especially below 340 nm. Among thicknesses considered, there is no apparent significant difference in the photoresponse (photocurrent density and IPCE of the TiO2 sol-gel films.

  20. Surface chemistry and moisture sorption properties of wood coated with multifunctional alkoxysilanes by sol-gel process

    Science.gov (United States)

    Mandla A. Tshabalala; Peter Kingshott; Mark R. VanLandingham; David Plackett

    2003-01-01

    Sol-gel surface deposition of a hydrophobic polysiloxane coating on wood was accomplished by using a mixture of a low molecular weight multifunctional alkoxysilane, methyltrimethoxysilane (MTMOS), and a high molecular weight multifunctional alkoxysilane, hexadecyltrimethoxysilane (HDTMOS). Investigation of the surface chemistry and morphology of the wood specimens by...