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Sample records for silica sba-15 fabricated

  1. Adsorptive removal of selected pharmaceuticals by mesoporous silica SBA-15

    International Nuclear Information System (INIS)

    Bui, Tung Xuan; Choi, Heechul

    2009-01-01

    The removal of five selected pharmaceuticals, viz., carbamazepine, clofibric acid, diclofenac, ibuprofen, and ketoprofen was examined by batch sorption experiments onto a synthesized mesoporous silica SBA-15. SBA-15 was synthesized and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N 2 adsorption-desorption measurement, and point of zero charge (PZC) measurement. Pharmaceutical adsorption kinetics was rapid and occurred on a scale of minutes, following a pseudo-second-order rate expression. Adsorption isotherms were best fitted by the Freundlich isotherm model. High removal rates of individual pharmaceuticals were achieved in acidic media (pH 3-5) and reached 85.2% for carbamazepine, 88.3% for diclofenac, 93.0% for ibuprofen, 94.3% for ketoprofen, and 49.0% for clofibric acid at pH 3 but decreased with increase in pH. SBA-15 also showed high efficiency for removal of a mixture of 5 pharmaceuticals. Except for clofibric acid (35.6%), the removal of pharmaceuticals in the mixture ranged from 75.2 to 89.3%. Based on adsorption and desorption results, the mechanism of the selected pharmaceuticals was found to be a hydrophilic interaction, providing valuable information for further studies to design materials for the purpose. The results of this study suggest that mesoporous-silica-based materials are promising adsorbents for removing pharmaceuticals from not only surface water but also wastewater of pharmaceutical industrial manufactures.

  2. Adsorptive removal of selected pharmaceuticals by mesoporous silica SBA-15

    Energy Technology Data Exchange (ETDEWEB)

    Bui, Tung Xuan, E-mail: bxtung@gist.ac.kr [Department of Environmental Science and Engineering, Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of); Choi, Heechul, E-mail: hcchoi@gist.ac.kr [Department of Environmental Science and Engineering, Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of)

    2009-09-15

    The removal of five selected pharmaceuticals, viz., carbamazepine, clofibric acid, diclofenac, ibuprofen, and ketoprofen was examined by batch sorption experiments onto a synthesized mesoporous silica SBA-15. SBA-15 was synthesized and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N{sub 2} adsorption-desorption measurement, and point of zero charge (PZC) measurement. Pharmaceutical adsorption kinetics was rapid and occurred on a scale of minutes, following a pseudo-second-order rate expression. Adsorption isotherms were best fitted by the Freundlich isotherm model. High removal rates of individual pharmaceuticals were achieved in acidic media (pH 3-5) and reached 85.2% for carbamazepine, 88.3% for diclofenac, 93.0% for ibuprofen, 94.3% for ketoprofen, and 49.0% for clofibric acid at pH 3 but decreased with increase in pH. SBA-15 also showed high efficiency for removal of a mixture of 5 pharmaceuticals. Except for clofibric acid (35.6%), the removal of pharmaceuticals in the mixture ranged from 75.2 to 89.3%. Based on adsorption and desorption results, the mechanism of the selected pharmaceuticals was found to be a hydrophilic interaction, providing valuable information for further studies to design materials for the purpose. The results of this study suggest that mesoporous-silica-based materials are promising adsorbents for removing pharmaceuticals from not only surface water but also wastewater of pharmaceutical industrial manufactures.

  3. Preparation of mesoporous silica films SBA-15 over different substrates

    International Nuclear Information System (INIS)

    Campos, V.O.; Sousa, E.M.B. de; Macedo, W.A.A.

    2010-01-01

    Mesoporous materials have been target of frequent interest due to its wide application possibilities, for example development of gas sensors, catalysis, molecules transportation, pharmaceuticals release, synthesis of auto-organized nanostructures, among others. The possibilities of application are enhanced when such materials are disposed in the form of thin and ultrathin films. In this work the preparation of mesoporous SBA-15 silica films is explored by means of the dipcoating technique of a sol-gel on different substrates (glass slides, stainless steel, copper), using the surfactant poly(ethylene glycol)-block-poly(propylene glycol)- block-poly(ethylene glycol), known as P123, a block copolymer. Synthesis parameters surfactant concentration, aging time and temperature were investigated. In this work we present the morphological and structural characterization of the prepared films, which were obtained using atomic force microscopy and x-ray fluorescence and diffraction. (author)

  4. Facile fabrication of mesoporous Fe-Ti-SBA15 silica with enhanced visible-light-driven simultaneous photocatalytic degradation and reduction reactions

    Science.gov (United States)

    Chang, Fei; Jiao, Mingzhi; Xu, Quan; Deng, Baoqing; Hu, Xuefeng

    2018-03-01

    A series of mesoporous iron-titanium-containing silica Fe-TiO2-SBA15 (FTS) were constructed via a facile one-pot hydrothermal route and subsequently characterized by X-ray diffraction patterns, UV-vis diffuse reflection spectroscopy, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption-desorption, X-ray photoelectron spectroscopy, and X-ray energy dispersion spectroscopy. By analyses, these samples possessed ordered two-dimensional hexagonal mesoporous structures, mainly involving mixed dual-phases of anatase and rutile TiO2, like commercial titania P25. The UV-vis diffuse reflection spectra demonstrated the presence of Fe species that was further confirmed by the X-ray photoelectron spectra and X-ray energy dispersion spectrum. The existence of Fe species in form of Fe3+ cations played an important role on the phase composition and electronic structure of these samples. With structural and morphological merits, these samples exhibited relatively high photocatalytic efficiency toward the degradation of dye methylene blue (MB) and reduction of Cr(VI) under visible-light irradiation, comparing with P25. In addition, among all candidates, the sample with a Fe/Si molar ratio of 0.03 showed the highest catalytic performance under optimal conditions, especially in the coexistence of both MB and Cr(VI), revealing an obviously synergistic effect when the consumption of both contaminants occurred. Finally, a primary catalytic mechanism was speculated on basis of active species capture experiments.

  5. Mapping the location of grafted PNIPAAM in mesoporous SBA-15 silica using gas adsorption analysis

    DEFF Research Database (Denmark)

    Reichhardt, Nina Viola; Guillet-Nicolas, Rémy; Thommes, Matthias

    2012-01-01

    The thermoresponsive polymer poly-N-isopropylacrylamide (PNIPAAM) was grafted in mesoporous SBA-15 silica. The grafting process consists of three steps: (i) increasing the amount of surface silanol groups of SBA-15 by hydroxylation, (ii) attachment of an anchor (1-(trichlorosilyl)-2-(m/p- (chloro......The thermoresponsive polymer poly-N-isopropylacrylamide (PNIPAAM) was grafted in mesoporous SBA-15 silica. The grafting process consists of three steps: (i) increasing the amount of surface silanol groups of SBA-15 by hydroxylation, (ii) attachment of an anchor (1-(trichlorosilyl)-2-(m...

  6. In Situ Loading of Drugs into Mesoporous Silica SBA-15.

    Science.gov (United States)

    Wan, Mi Mi; Li, Yan Yan; Yang, Tian; Zhang, Tao; Sun, Xiao Dan; Zhu, Jian Hua

    2016-04-25

    In a new strategy for loading drugs into mesoporous silica, a hydrophilic (heparin) or hydrophobic drug (ibuprofen) is encapsulated directly in a one-pot synthesis by evaporation-induced self-assembly. In situ drug loading significantly cuts down the preparation time and dramatically increases the loaded amount and released fraction of the drug, and appropriate drug additives favor a mesoporous structure of the vessels. Drug loading was verified by FTIR spectroscopy and release tests, which revealed much longer release with a larger amount of heparin or ibuprofen compared to postloaded SBA-15. Besides, the in vitro anticoagulation properties of the released heparin and the biocompatibility of the vessels were carefully assessed, including activated partial thromboplastin time, thrombin time, hemolysis, platelet adhesion experiments, and the morphologies of red blood cells. A concept of new drug-release agents with soft core and hard shell is proposed and offers guidance for the design of novel drug-delivery systems. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. TiO2 supported on rod-like mesoporous silica SBA-15: Preparation, characterization and photocatalytic behaviour

    International Nuclear Information System (INIS)

    Li, Yanjuan; Li, Nan; Tu, Jinchun; Li, Xiaotian; Wang, Beibei; Chi, Yue; Liu, Darui; Yang, Dianfan

    2011-01-01

    Highlights: ► Rod-like SBA-15 and normal SBA-15 were used to prepare TiO 2 /SBA-15 composites. ► TiO 2 /SBA-15 composites were studied as catalysts for methyl orange photodegradation. ► TiO 2 /Rod-SBA-15 exhibited higher photocatalytic activity than TiO 2 /Nor-SBA-15. ► The higher catalytic activity was a result of the controlled morphology of SBA-15. -- Abstract: TiO 2 nanoparticles have been successfully incorporated in the pores of mesoporous silica SBA-15 with different morphologies by a wet impregnation method. The composites were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), inductively coupled plasma (ICP) emission spectroscopy, transmission electron microscopy (TEM), N 2 -sorption and UV–Vis diffuse reflectance spectroscopy. The photodegradation of methyl orange (MO) was used to study their photocatalytic property. It is indicated that the morphology of SBA-15 had a great influence on the photocatalytic activity of the composites. When TiO 2 /SBA-15 composite was prepared by loading TiO 2 nanoparticles on uniform rod-like SBA-15 of 1 μm length, it showed higher photocatalytic degradation rate than that on less regular but much larger SBA-15 support. This difference was rationalized in terms of the homogeneously distributed and shorter channels of rod-like SBA-15, which favored mass transport and improved the efficient utilization of the pore surface.

  8. Development of efficient amine-modified mesoporous silica SBA-15 for CO2 capture

    International Nuclear Information System (INIS)

    Zhang, Xiaoyun; Qin, Hongyan; Zheng, Xiuxin; Wu, Wei

    2013-01-01

    Graphical abstract: - Highlights: • A secondary amine AN-TEPA is used to modify the SBA-15. • CO 2 adsorption capacity (180.1 mg g −1 -adsorbent for 70% amine loading) is high. • The sorbent exhibits a high stability after 12 cycling runs. • The modified SBA-15 achieves complete desorption at low temperature (100 °C). - Abstract: A novel CO 2 sorbent was prepared by impregnating mesoporous silica, SBA-15, with acrylonitrile (AN)-modified tetraethylenepentamine (TEPA) in order to increase CO 2 adsorption capacity and improve cycling stability. The mesoporous silica with pre- and post-surface modification was investigated by X-ray diffraction characterization (XRD), N 2 adsorption–desorption test (N 2 -BET), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA). The adsorption/desorption performance of S-TN (TN: AN modified TEPA) and S-TEPA was studied by dynamic adsorption. Test results showed that the solid base-impregnated SBA-15 demonstrated high CO 2 adsorption capacity (180.1 mg g −1 -adsorbent for 70% amine loading level). Compared to S-TEPA (24.1% decrease of initial capacity), S-TN with 50% amine loading exhibited improved cycling stability, 99.9% activity reserved (from initial 153.0 mg g −1 to 151.3 mg g −1 ) after 12 cycles of adsorption/desorption at 100 °C. A mechanism of molecular structure of the loaded amine was attributed to the improved performance

  9. Synthesis of lithium superionic conductor by growth of a nanoglass within mesoporous silica SBA-15 template

    Science.gov (United States)

    Chatterjee, Soumi; Miah, Milon; Saha, Shyamal Kumar; Chakravorty, Dipankar

    2018-04-01

    Nanodimensional silica based glasses containing alkali ions have recently been grown using suitable templates. These have shown electrical properties drastically different from those of their bulk counterpart. We have synthesized silicophosphate glasses having lithium ions with concentrations of 15-35 mole% Li2O within mesoporous silica SBA-15 (Santa Barbara amorphous-15) comprising of pores of diameter ~5 nm. The nanoglasses are characterized by electrical conductivities 5-6 orders of magnitude higher than those of the corresponding bulk glasses. These properties are attributed to the presence of a larger free volume in the nanoglasses as compared to their bulk states. The nanocomposites with 35 mole% Li2O exhibit an electrical conductivity of ~3 × 10-4 S · cm-1 at around room temperature. The activation energy for Li+ ion migration has been estimated from the conductivity-temperature variation to be 0.078 eV. These nanocomposites are believed to be ideally suited for the fabrication of solid state lithium ion batteries. We have also explored the efficiency of silicophosphate glass powders as possible electrode materials. Glass of composition 70SiO2/30P2O5 was prepared by using Pluronic P-123 tri-block copolymer along with suitable precursor sols. Cyclic voltammetric and galvanostatic charge/discharge measurements were carried out on the samples prepared in combination with suitable conductive fillers using a two-electrode system. These exhibited a high specific capacitance of 356 F g-1 making them ideally suitable as electrode materials for making a lithium ion solid state battery system.

  10. Thermoresponsive copolymer-grafted SBA-15 porous silica particles for temperature-triggered topical delivery systems

    Directory of Open Access Journals (Sweden)

    S. A. Jadhav

    2017-02-01

    Full Text Available A series of poly(N-isopropylacrylamide-co-acrylamide thermoresponsive random copolymers with different molecular weights and composition were synthesized and characterized by attenuated total reflectance Fourier-transform infrared (ATR-FTIR, differential scanning calorimetry (DSC, size exclusion chromatography (SEC and proton nuclear magnetic resonance (NMR spectroscopy. The lower critical solution temperatures (LCST of the copolymers were tuned by changing the mole ratios of monomers. Copolymer with highest molecular weight and LCST (41.2 °C was grafted on SBA-15 type mesoporous silica particles by a two-step polymer grafting procedure. Bare SBA-15 and the thermoresponsive copolymergrafted (hybrid SBA-15 particles were fully characterized by scanning electron microscope (SEM, ATR-FTIR, thermogravimetric analysis (TGA and Brunauer-Emmett-Teller (BET analyses. The hybrid particles were tested for their efficiency as temperature-sensitive systems for dermal delivery of the antioxidant rutin (quercetin-3-O-rutinoside. Improved control over rutin release by hybrid particles was obtained which makes them attractive hybrid materials for drug delivery.

  11. Synthesis of novel magnetic iron metal-silica (Fe-SBA-15) and magnetite-silica (Fe{sub 3}O{sub 4}-SBA-15) nanocomposites with a high iron content using temperature-programed reduction

    Energy Technology Data Exchange (ETDEWEB)

    Yiu, H H P [Department of Chemistry, University of Liverpool, Liverpool, Merseyside L69 7ZD (United Kingdom); Keane, M A [Chemical Engineering, School of Engineering and Physical Sciences, Heriot-Watt University, Edinburgh EH14 4AS (United Kingdom); Lethbridge, Z A D [Department of Chemistry, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL (United Kingdom); Lees, M R [Department of Physics, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL (United Kingdom); Haj, A J El; Dobson, J [Institute of Science and Technology in Medicine, Keele University, Thornburrow Drive, Hartshill, Stoke-on-Trent ST4 7QB (United Kingdom)], E-mail: j.p.dobson@keele.ac.uk

    2008-06-25

    Magnetic iron metal-silica and magnetite-silica nanocomposites have been prepared via temperature-programed reduction (TPR) of an iron oxide-SBA-15 (SBA: Santa Barbara Amorphous) composite. TPR of the starting SBA-15 supported Fe{sub 2}O{sub 3} generated Fe{sub 3}O{sub 4} and FeO as stepwise intermediates in the ultimate formation of Fe-SBA-15. The composite materials have been characterized by means of x-ray diffraction, high resolution transmission electron microscopy and SQUID (superconducting quantum interference device) magnetometry. The Fe oxide and metal components form a core, as nanoscale particles, that is entrapped in the SBA-15 pore network. Fe{sub 3}O{sub 4}-SBA-15 and Fe-SBA-15 exhibited superparamagnetic properties with a total magnetization value of 17 emu g{sup -1}. The magnetite-silica composite (at an Fe{sub 3}O{sub 4} loading of 30% w/w) delivered a magnetization that exceeded values reported in the literature or obtained with commercial samples. Due to the high pore volume of the mesoporous template, the magnetite content can be increased to 83% w/w with a further enhancement of magnetization.

  12. Modification of mesoporous silica SBA-15 with different organic molecules to gain chemical sensors: a review

    Directory of Open Access Journals (Sweden)

    Negar Lashgari

    2016-01-01

    Full Text Available The recognition of the biologically and environmentally important ions is of great interest in the field of chemical sensors in recent years. The fluorescent sensors as a powerful optical analytical technique for the detection of low level of various analytes such as anions and metal cations have been progressively developed due to the simplicity, cost effective, and selectivity for monitoring specific analytes in various systems. Organic-inorganic hybrid nanomaterials have important advantages as solid chemosensors and various innovative hybrid materials modified by fluorescence molecules were recently prepared. On the other hand, the homogeneous porosity and large surface area of mesoporous silica make it a promising inorganic support. SBA-15 as a two-dimensional hexagonal mesoporous silica material with stable structure, thick walls, tunable pore size, and high specific surface area is a valuable substrate for modification with different organic chelating groups. This review highlights the fluorescent chemosensors for ionic species based on modification of the mesoporous silica SBA-15 with different organic molecules, which have been recently developed from our laboratory.

  13. Determination of Thallium(I by Hybrid Mesoporous Silica (SBA-15 Modified Electrode

    Directory of Open Access Journals (Sweden)

    Geeta Rani

    2016-01-01

    Full Text Available Chemically modified mesoporous silica material (SBA-15 was used for the construction of Tl(I selective carbon paste electrode. The best response was found with the electrode containing 10% modifier as electrode material. The electrode has a lower detection limit of 6.0 × 10−9 M in a working concentration range of 1.0 × 10−8–1.0 × 10−1 M. The selectivity coefficient calculated by match potential method (MPM shows the high selectivity of electrode towards Tl(I over other tested ions. The electrode was successfully applied as an indicator electrode for the titration of 0.01 M TlNO3 solution with standards EDTA solution and for sequential titration of mixture of different anions.

  14. Direct hydrothermal synthesis of iron-containing mesoporous silica SBA-15 : potential as a support for gold nanoparticles

    NARCIS (Netherlands)

    Li, Y.; Guan, Y.; Santen, van R.A.; Kooyman, P.J.; Dugulan, A.I.; Li, C.; Hensen, E.J.M.

    2009-01-01

    The preparation of mesoporous silica SBA-15 with high iron loadings (14-90 wt % Fe2O3) as a suitable support for gold nanoparticles to be used in CO oxidation catalysis has been investigated. The support materials were prepared by a direct hydrothermal two-step pH adjusting method which consisted of

  15. Physical properties of ordered mesoporous SBA-15 silica as immunological adjuvant

    Science.gov (United States)

    Mariano-Neto, F.; Matos, J. R.; Cides da Silva, L. C.; Carvalho, L. V.; Scaramuzzi, K.; Sant'Anna, O. A.; Oliveira, C. P.; Fantini, M. C. A.

    2014-10-01

    This work reports a detailed analysis of the ordered mesoporous SBA-15 silica synthesis procedure that provides a matrix with mean pore diameter around 10 nm. The encapsulation of bovine serum albumin (BSA) by four different methods allowed the determination of the best imbibition condition, which is keeping the mixture under rest and solvent evaporation. Simulation of the in situ SAXS scattered intensity of the BSA release in potassium buffer solution, gastrointestinal fluids revealed a slow evolution of BSA content, independent of the media. Proton induced x-ray emission results obtained in calcined mouse organs revealed that silica is only present in the spleen after 35 days and is completely eliminated from all mouse organs after 10 weeks. Biological studies showed that Santa Barbara Amorphous-15 is an effective adjuvant when compared to the traditional Al(OH)3, and is non-toxic to mice, rats, dogs and even cells, such as macrophages and dendritic cells. Recent studies showed that the immunological response is improved by enhancing the inflammatory response and the recruitment of immune competent cells to the site of injection as by the oral route and, most importantly, by increasing the number of phagocytes of a particulate antigen by antigen presenting cells. This research is under the scope of the International Patent WO 07030901, IN248654,ZA2008/02277, KR 1089400, MX297263, JP5091863, CN101287491B.

  16. Enhanced photocatalytic performance of mesoporous TiO{sub 2} coated SBA-15 nanocomposites fabricated through a novel approach: supercritical deposition aided by liquid-crystal template

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Chen; Lin, Xiao; Li, Youji, E-mail: bcclyj@163.com; Xu, Peng; Li, Ming; Chen, Feitai

    2016-03-15

    Highlights: • Highly uniform mesoporous TiO{sub 2} nanopartices were coated SBA-15. • MT showed smaller crystallite size, higher hydroxyl content and surface area. • MT/SBA-15 show enhanced photocatalytic activity and high reused activity. • The optimum MT loading rate and calcination temperature were obtained to be 15% and 400 °C, respectively. • Photocatalytic behaviors are discussed in terms of the Langmuir–Hinshelwood model. - Abstract: Mesoporous TiO2 coated SBA-15 (MT@S) nanocomposites were fabricated through supercritical CO{sub 2} deposition aided by liquid-crystal template. The as-prepared samples were characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, diffuse reflectance spectroscopy and so on. The results reveal that MT uniformly deposited onto silica with titania incorporated in SBA-15 channels, showed smaller crystallite size, higher hydroxyl content and surface area than nonporous TiO{sub 2} coated SBA-15 (NT@S) obtained by a similar route without template. With TiO{sub 2} loading ratio of 15 wt% and calcination temperature of 400 °C, 15%MT@S-400 showed the enhanced degradation efficiency for azo dyes (methylene blue, methyl orange, and rhodamine B) and phenol in comparsion with 15%NT@S-400, due to those improved textural and physicochemical properties. Meanwhile, the reused MT@S also showed high photoactivity. Additionally, the effects of MT content and calcination temperature have been examined as operational parameters. Photocatalytic reactions followed pseudo-first-order kinetics and are discussed in terms of the Langmuir–Hinshelwood model.

  17. Photo-Catalytic Properties of TiO2 Supported on MWCNTs, SBA-15 and Silica-Coated MWCNTs Nanocomposites.

    Science.gov (United States)

    Ramoraswi, Nteseng O; Ndungu, Patrick G

    2015-12-01

    Mesoporous silica, specifically SBA-15, acid-treated multi-walled carbon nanotubes and a hybrid nanocomposite of SBA-15 coated onto the sidewalls acid-treated multi-walled carbon nanotubes (CNTs) were prepared and used as supports for anatase TiO2. Sol-gel methods were adapted for the synthesis of selected supports and for coating the materials with selected wt% loading of titania. Physical and chemical properties of the supports and catalyst composite materials were investigated by powder X-ray diffraction (XRD), Raman spectroscopy, thermogravimetric analysis, scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), UV-vis diffuse reflectance spectroscopy and fluorescence spectroscopy. The photo-activity of the catalyst composites were evaluated on the decolorisation of methylene blue as a model pollutant. Coating CNTs with SBA-15 improved the thermal stability and textural properties of the nanotubes. All supported titania composites had high surface areas (207-301 m(2)/g), altered band gap energies and reduced TiO2 crystallite sizes. The TiO2/SBA-CNT composite showed enhanced photo-catalytic properties and activity than the TiO2/SBA-15 and TiO2/CNT composites. In addition, an interesting observation was noted with the TiO2/SBA-15 nanocomposites, which had a significantly greater photo-catalytic activity than the TiO2/CNT nanocomposites in spite of the high electron-hole recombination phenomena observed with the photoluminescence results. Discussions in terms of morphological, textural and physical-chemical aspects to account for the result are presented.

  18. Pore-expanded SBA-15 sulfonic acid silicas for biodiesel synthesis.

    Science.gov (United States)

    Dacquin, J P; Lee, A F; Pirez, C; Wilson, K

    2012-01-07

    Here we present the first application of pore-expanded SBA-15 in heterogeneous catalysis. Pore expansion over the range 6-14 nm confers a striking activity enhancement towards fatty acid methyl ester (FAME) synthesis from triglycerides (TAG), and free fatty acid (FFA), attributed to improved mass transport and acid site accessibility. This journal is © The Royal Society of Chemistry 2012

  19. The structure heterogeneity of silica mesopores of Sba-15 in respect to the pluronic 123 template concentration

    Science.gov (United States)

    Dhaneswara, D.; Fatriansyah, J. F.; Putranto, D. A.; Utami, S. A. A.; Delayori, F.

    2018-01-01

    The analysis of structure heterogeneity factor of silica mesoporous SBA-15 has been conducted. The structure factor has been found to be different for low and high concentration of Pluronic-123 template. The structure heterogeneity of high concentration of Pluronic-123 has been found less than 1 while for low concentration, the structure heterogeneity was found to be larger than 1. This indicates the dissimilarity of the structure and can be used as a probe to detect the formation of large mesopores. It also was found that the system exhibits type IV and H1 adsorption type which indicates the capillary condensation and interconnected pores.

  20. SBA-15 mesoporous silica free-standing thin films containing copper ions bounded via propyl phosphonate units - preparation and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Laskowski, Lukasz, E-mail: lukasz.laskowski@kik.pcz.pl [Czestochowa University of Technology, Institute of Computational Intelligence, Unit of Microelectronics and Nanotechnology, Al. Armii Krajowej 36, 42–201 Czestochowa (Poland); Laskowska, Magdalena, E-mail: magdalena.laskowska@onet.pl [H. Niewodniczanski Institute of Nuclear Physics, Polish Academy of Sciences, 31-342 Krakow, ul. Radzikowskiego 152 (Poland); Jelonkiewicz, Jerzy, E-mail: jerzy.jelonkiewicz@kik.pcz.pl [Czestochowa University of Technology, Institute of Computational Intelligence, Unit of Microelectronics and Nanotechnology, Al. Armii Krajowej 36, 42–201 Czestochowa (Poland); Dulski, Mateusz, E-mail: mateusz.dulski@us.edu.pl [University of Silesia, Faculty of Computer Science and Materials Science, Institute of Materials Science, Silesian Center for Education and Interdisciplinary Research, ul. 75 Pułku Piechoty 1A, 41–500 Chorzów (Poland); Wojtyniak, Marcin, E-mail: marcin.wojtyniak@us.edu.pl [University of Silesia, Institute of Physics, Silesian Center for Education and Interdisciplinary Research, ul. 75 Pułku Piechoty 1A, 41–500 Chorzów (Poland); Fitta, Magdalena, E-mail: magdalena.fitta@ifj.edu.pl [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, 31–342 Krakow, ul. Radzikowskiego 152 (Poland); Balanda, Maria, E-mail: Maria.Balanda@ifj.edu.pl [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, 31–342 Krakow, ul. Radzikowskiego 152 (Poland)

    2016-09-15

    The SBA-15 silica thin films containing copper ions anchored inside channels via propyl phosphonate groups are investigated. Such materials were prepared in the form of thin films, with hexagonally arranged pores, laying rectilinear to the substrate surface. However, in the case of our thin films, their free standing form allowed for additional research possibilities, that are not obtainable for typical thin films on a substrate. The structural properties of the samples were investigated by X-ray reflectometry, atomic force microscopy (AFM) and transmission electron microscopy (TEM). The molecular structure was examined by Raman spectroscopy supported by numerical simulations. Magnetic measurements (SQUID magnetometry and EPR spectroscopy) showed weak antiferromagnetic interactions between active units inside silica channels. Consequently, the pores arrangement was determined and the process of copper ions anchoring by propyl phosphonate groups was verified in unambiguous way. Moreover, the type of interactions between magnetic atoms was determined. - Highlights: • Functionalized free-standing SBA-15 thin films were synthesized for a first time. • Thin films synthesis procedure was described in details. • Structural properties of the films were thoroughly investigated and presented. • Magnetic properties of the novel material was investigated and presented.

  1. Efficient solid-phase microextraction of triazole pesticides from natural water samples using a Nafion-loaded trimethylsilane-modified mesoporous silica coating of type SBA-15

    International Nuclear Information System (INIS)

    Abolghasemi, Mir Mahdi; Hassani, Sona; Bamorowat, Mehdi

    2016-01-01

    A mesoporous silica surface of type SBA-15 was made more hydrophobic by modification with ethoxytrimethylsilane to obtain a hybrid organic–inorganic mesoporous nanocomposite, which then was impregnated with Nafion. The resulting nanocomposite was used as a fiber coating for solid-phase microextraction (SPME). The trimethylsilyl-modified Nafion/SBA-15 nanocomposite with high surface area was characterized by SEM and FTIR. It was immobilized on a stainless steel wire in order to fabricate a fiber for SPME. This fiber was evaluated for its suitability for extracting triazolic agrochemicals from water samples before their quantification through a combination of gas chromatography and mass spectrometry. Experimental conditions for fiber coating, extraction time, stirring rate, ionic strength, pH value, desorption temperature and desorption time were optimized. Under optimum conditions, the repeatability for one fiber (for n = 3) ranges from 4.3 to 5.6 % (relative standard deviation). The detection limits are between 50 and 90 pg⋅mL −1 . The method is simple, fast, low-cost (in terms of equipment), and the fiber used for SPME has high thermal stability and good recovery. (author)

  2. Insights into the Hydrothermal Stability of Triamine-Functionalized SBA-15 Silica for CO2 Adsorption.

    Science.gov (United States)

    Jahandar Lashaki, Masoud; Ziaei-Azad, Hessam; Sayari, Abdelhamid

    2017-10-23

    The hydrothermal stability of triamine-grafted, large-pore SBA-15 CO 2 adsorbents was studied by using steam stripping. Following two 3 h cycles of steam regeneration, lower CO 2 uptakes, lower CO 2 /N ratios, and slower adsorption kinetics were observed relative to fresh samples, particularly at the lowest adsorption temperature (25 °C). CO 2 adsorption measurements for a selected sample exposed to 48 h of steam stripping depicted that after the initial loss during the first exposure to steam (3-6 h), the adsorptive properties stabilized. For higher adsorption temperatures (i.e., 50 and 75 °C), however, all adsorptive properties remained almost unchanged after steaming, indicating the significance of diffusional limitations. Thermogravimetric analysis and FTIR spectroscopy on grafted samples before and after steam stripping showed no amine leaching and no change in the chemical nature of the amine groups, respectively. Also, a six-cycle CO 2 adsorption/desorption experiment under dry conditions showed no thermal degradation. However, N 2 adsorption measurement at 77 K showed significant reductions in the BET surface area of the grafted samples following steaming. Based on the pore size distribution of calcined, grafted samples before and after steaming, it is proposed that exposure to steam restructured the grafted materials, causing mass transfer resistance. It is inferred that triamine-grafted, large-pore SBA-15 adsorbents are potential candidates for CO 2 capture at relatively high temperatures (50-75 °C; for example, flue gas) combined with steam regeneration. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Mesostructured Au/C materials obtained by replication of functionalized SBA-15 silica containing highly dispersed gold nanoparticles

    KAUST Repository

    Kerdi, Fatmé

    2011-04-01

    The preparation and characterization of highly dispersed gold nanoparticles in ordered mesoporous carbons CMK-3 are reported. These carbons were obtained using gold-containing functionalized SBA-15 silicas as hard templates. Two series of Au/SiO2 templates were prepared, depending on the nature of the functionalization molecule. While ammonium-functionalized silicas gave gold particles with a size determined by the pores of the silica support, the use of mercaptopropyltrimethoxysilane as grafting molecule afforded the possibility to control the particle size inside the mesopores. Both series gave highly ordered mesoporous carbons with gold particles incorporated in the carbon nanorods. However, the gold particle size in mesoporous carbons was the same for both series and apparently did not depend on the nature of the silica template. Both Au/SiO2 templates and their corresponding Au/CMK-3 materials have been characterized by X-ray diffraction, nitrogen adsorption/desorption, chemical analysis, solid-state nuclear magnetic resonance and transmission electron microscopy. They were also used as catalysts in the aerobic oxidation of cyclohexene and trans-stilbene in the liquid phase. © 2010 Elsevier Inc. All rights reserved.

  4. Fluorescence properties of riboflavin-functionalized mesoporous silica SBA-15 and riboflavin solutions in presence of different metal and organic cations

    Science.gov (United States)

    Lewandowski, Dawid; Schroeder, Grzegorz; Sawczak, Mirosław; Ossowski, Tadeusz

    2015-10-01

    Riboflavin was covalently linked to mesoporous SBA-15 silica surface via grafting technique. Then fluorescence properties of the system obtained were analyzed in the presence of several metal and organic cations. Both quenching and strengthening of fluorescence as well as significant changes in the maximum fluorescence wavelength were observed. The results were compared with absorption and fluorescence data obtained for riboflavin water solutions.

  5. Physical state of poorly water soluble therapeutic molecules loaded into SBA-15 ordered mesoporous silica carriers: a case study with itraconazole and ibuprofen.

    Science.gov (United States)

    Mellaerts, Randy; Jammaer, Jasper A G; Van Speybroeck, Michiel; Chen, Hong; Van Humbeeck, Jan; Augustijns, Patrick; Van den Mooter, Guy; Martens, Johan A

    2008-08-19

    The ordered mesoporous silica material SBA-15 was loaded with the model drugs itraconazole and ibuprofen using three different procedures: (i) adsorption from solution, (ii) incipient wetness impregnation, and (iii) heating of a mixture of drug and SBA-15 powder. The location of the drug molecules in the SBA-15 particles and molecular interactions were investigated using nitrogen adsorption, TGA, DSC, DRS UV-vis, and XPS. The in vitro release of hydrophobic model drugs was evaluated in an aqueous environment simulating gastric fluid. The effectiveness of the loading method was found to be strongly compound dependent. Incipient wetness impregnation using a concentrated itraconazole solution in dichloromethane followed by solvent evaporation was most efficient for dispersing itraconazole in SBA-15. The itraconazole molecules were located on the mesopore walls and inside micropores of the mesopore walls. When SBA-15 was loaded by slurrying it in a diluted itraconazole solution from which the solvent was evaporated, the itraconazole molecules ended up in the mesopores that they plugged locally. At a loading of 30 wt %, itraconazole exhibited intermolecular interactions inside the mesopores revealed by UV spectroscopy and endothermic events traced with DSC. The physical mixing of itraconazole and SBA-15 powder followed by heating above the itraconazole melting temperature resulted in formulations in which glassy itraconazole particles were deposited externally on the SBA-15 particles. Loading with ibuprofen was successful with each of the three loading procedures. Ibuprofen preferably is positioned inside the micropores. In vitro release experiments showed fast release kinetics provided the drug molecules were evenly deposited over the mesoporous surface.

  6. Applying Mesoporous Silica SBA-15 in Electrochemical Detection of DNA Hybridization

    Czech Academy of Sciences Publication Activity Database

    Josypčuk, Oksana; Fojta, Miroslav; Daňhel, Aleš; Josypčuk, Bohdan

    2016-01-01

    Roč. 28, č. 8 (2016), s. 1860-1864 ISSN 1040-0397 R&D Projects: GA ČR GAP206/11/1638 Institutional support: RVO:68081707 ; RVO:61388955 Keywords : voltammetry * sensor DNA hybridization * mesoporous silica Subject RIV: CG - Electrochemistry Impact factor: 2.851, year: 2016

  7. Dissolution enhancement of a model poorly water-soluble drug, atorvastatin, with ordered mesoporous silica: comparison of MSF with SBA-15 as drug carriers.

    Science.gov (United States)

    Maleki, Aziz; Hamidi, Mehrdad

    2016-01-01

    The purpose of this study was to develop mesoporous silica materials incorporated with poorly water-soluble drug atorvastatin calcium (AC) in order to improve drug dissolution, and intended to be orally administrated. A comparison between 2D-hexagonal silica nanostructured SBA-15 and mesocellular siliceous foam (MSF) with continuous 3D pore system on drug release rate was investigated. AC-loaded mesoporous silicas were characterized thorough N2 adsorption-desorption analysis, Fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC) and dynamic light scattering (DLS). Results demonstrated a successful incorporation of AC into the silica-based hosts. The results taken from the drug release tests were also analyzed using different parameters, namely similarity factor (f2), difference factor (f1), dissolution efficiency (DE%), mean dissolution rate (MDR) and dissolution time (tm%). It confirmed a significant enhancement in the release profile of atorvastatin calcium with SBA-15, and MSF as drug carrier. Moreover, in comparison with SBA-15, MSF showed faster release rate of AC in enzyme-free simulated gastric fluid (pH 1.2). We believed that our findings can help the use of mesoporous silica materials in improving bioavailability of poorly water-soluble drugs.

  8. Effects of carbon coating and pore corrugation on capillary condensation of nitrogen in SBA-15 mesoporous silica.

    Science.gov (United States)

    Morishige, Kunimitsu

    2013-09-24

    To examine the origin of an ink-bottle-like structure in SBA-15 formed by carbon coating and the effects of pore corrugation on capillary condensation and evaporation of a vapor in the cylindrical pores, we measured the adsorption isotherms of nitrogen at 77 K on 10 kinds of SBA-15 samples before and after a carbon coating process by the exposure to acetylene at 1073 K, as well as desorption scanning curves and subloops on the untreated samples. These SBA-15 samples were synthesized under the different conditions of initial SiO2/P123 ratio and hydrothermal treatment. SBA-15 with relatively large microporosity tends to form easily constrictions inside the main channels by the carbon coating. This strongly suggests that the rough pore walls of SBA-15 may induce the incomplete wetting of carbon layers on the pore walls to form the constrictions inside the cylindrical pores. A comparison of two subloops implies that the pores of SBA-15 synthesized with a SiO2/P123 ratio of 75 consist of an assembly of connecting domains of different diameters; that is, the pores are highly corrugated. For SBA-15 synthesized with a SiO2/P123 ratio of 60, the amplitude of the pore corrugation is significantly decreased by the prolonged hydrothermal treatment at 373 K. On the other hand, for SBA-15 synthesized with a SiO2/P123 ratio of 45, the amplitude of the corrugation is negligibly small, although the cylindrical pores are interconnected through narrow necks with each other. It is found that the smaller the amplitude of the pore corrugation, the smaller the width of the hysteresis loop.

  9. Effect of silica/titania ratio on enhanced photooxidation of industrial hazardous materials by microwave treated mesoporous SBA-15/TiO{sub 2} nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Mehta, Akansha; Mishra, Amit; Sharma, Manisha; Singh, Satnam; Basu, Soumen, E-mail: soumen.basu@thapar.edu [Thapar University, School of Chemistry and Biochemistry (India)

    2016-07-15

    In this study microwave assisted technique has been adopted for the synthesis of different weight ratios of TiO{sub 2} dispersed on Santa barbara amorphous-15 (SBA-15) support. Morphological study revealed TiO{sub 2} particles (4–10 nm) uniformly distributed on SBA-15 while increases in SBA-15 content results in higher specific surface area (524–237 m{sup 2}/g). The diffraction intensity of 101 plane of anatase polymorph was seen increasing with increase in TiO{sub 2} ratio. All the photocatalysts were having a mesoporous nature and follow the Langmuir IV isotherm, SBA-15 posses the highest pore volume (0.93 cm{sup 3} g{sup −1}) which consistently decreased with TiO{sub 2} content and was lowest (0.50 cm{sup 3} g{sup −1}) in case of 5 wt% of TiO{sub 2} followed by P25 (0.45 cm{sup 3} g{sup −1}) while pore diameter increased after TiO{sub 2} incorporation due to pore strain. The photocatalytic activity of the nanocomposites were analysed for the photodegradation of alizarin dye and pentachlorophenol under UV light irradiation. The reaction kinetics suggested the highest efficiency (98 % for alizarin and 94 % for PCP) of 5 wt% TiO{sub 2} compared to other photocatalysts, these nanocomposites were reused for several cycles, which is most important for heterogeneous photocatalytic degradation reaction.Graphical abstractThis study demonstrates the synthesis of silica embedded TiO{sub 2} nanocomposites by microwave assisted technique and their catalytic influence on degradation of organic dyes and pollutants. Higher loading of titania (SBA-15/TiO{sub 2}, 1:5) results better catalytic performance than commercial nano TiO{sub 2} (P25).

  10. Preparation and characterization of glycidyl methacrylate organo bridges grafted mesoporous silica SBA-15 as ibuprofen and mesalamine carrier for controlled release

    International Nuclear Information System (INIS)

    Rehman, Fozia; Rahim, Abdur; Airoldi, Claudio; Volpe, Pedro L.O.

    2016-01-01

    Mesoporous silica SBA-15 was synthesized and functionalized with bridged polysilsesquioxane monomers obtained by the reaction of 3-aminopropyltriethoxy silane with glycidyl methacrylate in 2:1 ratio. The synthesized mesoporous silica materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-ray diffraction, thermogravimetry and scanning electron microscopy. The nuclear magnetic resonance in the solid state is in agreement with the sequence of carbon distributed in the attached organic chains, as expected for organically functionalized mesoporous silica. After functionalization with organic bridges the BET surface area was reduced from 1311.80 to 494.2 m 2 g −1 and pore volume was reduced from 1.98 to 0.89 cm 3 g −1 , when compared to original precursor silica. Modification of the silica surface with organic bridges resulted in high loading capacity and controlled release of ibuprofen and mesalamine in biological fluids. The Korsmeyer–Peppas model better fits the release data indicating Fickian diffusion and zero order kinetics for synthesized mesoporous silica. The drug release rate from the modified silica was slow in simulated gastric fluid, (pH 1.2) where less than 10% of mesalamine and ibuprofen were released in initial 8 h, while comparatively high release rates were observed in simulated intestinal (pH 6.8) and simulated body fluids (pH 7.2). The preferential release of mesalamine at intestinal pH suggests that the modified silica could be a simple, efficient, inexpensive and convenient carrier for colon targeted drugs, such a mesalamine and also as a controlled drug release system. - Highlights: • Modified SBA-15 silica with long hydrophobic chains was evaluated as drug carrier. • This silica showed improved loading capacity and controlled release of ibuprofen. • Compared to gastric pH high release rate of mesalamine was observed at colonic pH. • Modified silica

  11. IR spectroscopy study of SBA-15 silicas functionalized with the ethylthiocarbamidepropyl groups and their interactions with Ag(I) and Hg(II) ions

    Science.gov (United States)

    Melnyk, Inna V.; Nazarchuk, Galyna I.; Václavíková, Miroslava; Zub, Yuriy L.

    2018-04-01

    Mesoporous structure of silica is determined by the type of template, but the introduction of functional groups during the synthesis has additional influence. The structure of SBA-15 may be violated by the introduction of long functions, such as ≡Si(CH2)3NHC(=S)NHC2H5. These ethylthiocarbamidepropyl groups can form complexes with metal ions in thiol or thione tautomeric forms. We determined that the 2D hexagonal p6 mm structure is preserved for SBA-15 with thiourea groups at maximal TEOS:trifunctional silane ratio (mol) = 10:2, which was confirmed by TEM and by the presence of an intense reflex in the small-angle region of diffractograms of the final product. It was shown that the obtained sorbents possess high kinetic characteristics. The experimental data fit pseudo-second-order kinetic equation, but the rate constants depend on the content of functional groups in the surface layer. Template Pluronic P-123 defines the porosity of functional mesoporous silica materials even at increasing content of trifunctional silane in the initial solution. Infrared spectroscopy analysis showed that thione form of thiourea ligand is prevalent on the surface of pores of mesoporous samples. However, during the sorption of silver(I) ions, there are both thione and thiol forms on the surface. Thione form is transformed into thiol with increasing concentration of mercury(II) ions in the sorption solution. Adsorption experiments showed that the SBA-15 silicas functionalized with ethylthiocarbamidepropyl groups had high selectivity for silver(I) ions and could concentrate Ag(I) ions from metal ions mixture at pH 2.

  12. Iron-functionalized nanoporous silica type SBA-15: Synthesis, characterization and application in alkene epoxidation in presence of hydrogen peroxide

    Directory of Open Access Journals (Sweden)

    Mahdieh Ghazizadeh

    2017-05-01

    Full Text Available Fe(IIIsalophen complex on a SBA-15 support functionalized with (3-aminopropyltriethoxysilane as a linker. It has been synthesized and characterized by XRD, adsorption–desorption of nitrogen, SEM, FT-IR and UV–Vis. The formation of metal-salophen complex with the amino groups as connectors to the SBA-15 surface was confirmed. This material was successfully used as a heterogeneous catalyst for the epoxidation of alkenes and the effects of reaction time, different solvents and amount of catalyst on catalytic activity were investigated. This catalyst gave suitable and comparable yield and percentage conversion values. It is also stable and can be recycled and reused in the epoxidation of alkenes.

  13. A well-defined mesoporous amine silica surface via a selective treatment of SBA-15 with ammonia

    KAUST Repository

    Bendjeriou-Sedjerari, Anissa; Pelletier, Jeremie; Abou-Hamad, Edy; Emsley, Lyndon; Basset, Jean-Marie

    2012-01-01

    2D double-quantum 1H- 1H NMR unambiguously shows that the "isolated" Si-OH surface silanols of dehydroxylated SBA-15 are converted upon treatment with ammonia into single silylamine surface site Si-NH 2. The "gem" di-silanols (Si(OH) 2) remain intact. Treatment using HMDS produces (Si(OSiMe 3) 2) but leaves Si-NH 2 untouched. The resulting surface is hydrophobic and stable. © The Royal Society of Chemistry 2012.

  14. Exploiting the interactions between the ruthenium Hoveyda–Grubbs catalyst and Al-modified mesoporous silica: the case of SBA15 vs. KCC-1

    KAUST Repository

    Werghi, Baraa; Pump, Eva; Tretiakov, Mykyta; Abou-Hamad, Edy; Gurinov, Andrei; Doggali, Pradeep; Anjum, Dalaver H.; Cavallo, Luigi; Bendjeriou-Sedjerari, Anissa; Basset, Jean-Marie

    2018-01-01

    Immobilization of the 2 generation Hoveyda-Grubbs catalyst HG-II onto well-ordered 2D hexagonal (SBA15) and 3D fibrous (KCC-1) mesostructured silica, which contained tetra-coordinated Al, has been investigated through the Surface Organometallic Chemistry (SOMC) methodology. The main interest of this study lies in the peculiarity of the silica supports, which display a well-defined tetrahedral aluminum hydride site displaying a strong Lewis acid character, [(Si-O-Si)(Si-O-)Al-H]. The resulting supported Hoveyda-Grubbs catalysts have been fully characterized by advanced solid state characterization techniques (FT-IR, H and C solid state NMR, DNP-SENS, EF-TEM...). Together with DFT calculations, the immobilization of HG-II does not occur through the formation of a covalent bond between the complex and the Al-modified mesoporous silica as expected, but through an Al⋯Cl-[Ru]-coordination. It is not surprising that in functionalized olefin metathesis of diethyldiallyl malonate, DEDAM (liquid phase), leaching of the catalyst is observed which is not the case in non-functionalized olefin metathesis of propene (gas phase). Besides, the results obtained in propene metathesis with HG-II immobilized either on SBA15 (d = 6 nm) or KCC-1 (d = 4 or 8 nm) highlight the importance of the accessibility of the catalytic site. Therefore, we demonstrate that KCC-1 is a promising and suitable 3D mesoporous support to overcome the diffusion of reactants into the porous network of heterogeneous catalysts.

  15. Exploiting the interactions between the ruthenium Hoveyda–Grubbs catalyst and Al-modified mesoporous silica: the case of SBA15 vs. KCC-1

    KAUST Repository

    Werghi, Baraa

    2018-03-05

    Immobilization of the 2 generation Hoveyda-Grubbs catalyst HG-II onto well-ordered 2D hexagonal (SBA15) and 3D fibrous (KCC-1) mesostructured silica, which contained tetra-coordinated Al, has been investigated through the Surface Organometallic Chemistry (SOMC) methodology. The main interest of this study lies in the peculiarity of the silica supports, which display a well-defined tetrahedral aluminum hydride site displaying a strong Lewis acid character, [(Si-O-Si)(Si-O-)Al-H]. The resulting supported Hoveyda-Grubbs catalysts have been fully characterized by advanced solid state characterization techniques (FT-IR, H and C solid state NMR, DNP-SENS, EF-TEM...). Together with DFT calculations, the immobilization of HG-II does not occur through the formation of a covalent bond between the complex and the Al-modified mesoporous silica as expected, but through an Al⋯Cl-[Ru]-coordination. It is not surprising that in functionalized olefin metathesis of diethyldiallyl malonate, DEDAM (liquid phase), leaching of the catalyst is observed which is not the case in non-functionalized olefin metathesis of propene (gas phase). Besides, the results obtained in propene metathesis with HG-II immobilized either on SBA15 (d = 6 nm) or KCC-1 (d = 4 or 8 nm) highlight the importance of the accessibility of the catalytic site. Therefore, we demonstrate that KCC-1 is a promising and suitable 3D mesoporous support to overcome the diffusion of reactants into the porous network of heterogeneous catalysts.

  16. Au and AuCu Nanoparticles Supported on SBA-15 Ordered Mesoporous Titania-Silica as Catalysts for Methylene Blue Photodegradation

    Directory of Open Access Journals (Sweden)

    Isabel Barroso-Martín

    2018-05-01

    Full Text Available The photocatalytic degradation of methylene blue (MB dye has been performed under UV irradiation in aqueous suspension, employing photocatalysts based on Au (1.5 wt % and AuCu (Au/Cu = 1, 2.0 wt %, and supported on SBA-15-ordered mesoporous silica, with and without titania (Si/Ti = 3, in order to evaluate the versatility of this mesoporous support in this type of reaction of great impact from the environmental point of view. Samples were characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, N2 adsorption-desorption at −196 °C, and X-ray photoelectron spectroscopy (XPS, so as to study their structural, optical, and chemical properties. All the prepared catalysts were found to be active in the test reaction. The bimetallic AuCu-based catalysts attained very high MB degradation values, in particular AuCu/SBA-15 titania-silica sample reached 100% of dye oxidation after the monitored reaction period (120 min.

  17. Preparation and characterization of glycidyl methacrylate organo bridges grafted mesoporous silica SBA-15 as ibuprofen and mesalamine carrier for controlled release

    Energy Technology Data Exchange (ETDEWEB)

    Rehman, Fozia, E-mail: fozia@iqm.unicamp.br [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil); Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Rahim, Abdur [Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Airoldi, Claudio; Volpe, Pedro L.O. [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil)

    2016-02-01

    Mesoporous silica SBA-15 was synthesized and functionalized with bridged polysilsesquioxane monomers obtained by the reaction of 3-aminopropyltriethoxy silane with glycidyl methacrylate in 2:1 ratio. The synthesized mesoporous silica materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-ray diffraction, thermogravimetry and scanning electron microscopy. The nuclear magnetic resonance in the solid state is in agreement with the sequence of carbon distributed in the attached organic chains, as expected for organically functionalized mesoporous silica. After functionalization with organic bridges the BET surface area was reduced from 1311.80 to 494.2 m{sup 2} g{sup −1} and pore volume was reduced from 1.98 to 0.89 cm{sup 3} g{sup −1}, when compared to original precursor silica. Modification of the silica surface with organic bridges resulted in high loading capacity and controlled release of ibuprofen and mesalamine in biological fluids. The Korsmeyer–Peppas model better fits the release data indicating Fickian diffusion and zero order kinetics for synthesized mesoporous silica. The drug release rate from the modified silica was slow in simulated gastric fluid, (pH 1.2) where less than 10% of mesalamine and ibuprofen were released in initial 8 h, while comparatively high release rates were observed in simulated intestinal (pH 6.8) and simulated body fluids (pH 7.2). The preferential release of mesalamine at intestinal pH suggests that the modified silica could be a simple, efficient, inexpensive and convenient carrier for colon targeted drugs, such a mesalamine and also as a controlled drug release system. - Highlights: • Modified SBA-15 silica with long hydrophobic chains was evaluated as drug carrier. • This silica showed improved loading capacity and controlled release of ibuprofen. • Compared to gastric pH high release rate of mesalamine was observed at colonic pH.

  18. Enthalpy and interfacial free energy changes of water capillary condensed in mesoporous silica, MCM-41 and SBA-15.

    Science.gov (United States)

    Kittaka, Shigeharu; Ishimaru, Shinji; Kuranishi, Miki; Matsuda, Tomoko; Yamaguchi, Toshio

    2006-07-21

    The effect of confinement on the solid-liquid phase transitions of water was studied by using DSC and FT-IR measurements. Enthalpy changes upon melting of frozen water in MCM-41 and SBA-15 were determined as a function of pore size and found to decrease with decreasing pore size. The melting point also decreased almost monotonically with a decrease in pore size. Analysis of the Gibbs-Thomson relation on the basis of the thermodynamic data showed that there were two stages of interfacial free energy change after the constant region, i.e., below a pore size of 6.0 nm: a gradual decrease down to 3.4 nm and another decrease after a small jump upward. This fact demonstrates that the simple Gibbs-Thomson relation, i.e., a linear relation between the melting point change and the inverse pore size, is limited to the range not far from the melting point of bulk water. FT-IR measurements suggest that the decrease in enthalpy change and interfacial free energy change with decreasing pore size reflect the similarity of the structures of both liquid and solid phases of water in smaller pores at lower temperatures.

  19. Iron-functionalized Al-SBA-15 for benzene hydroxylation

    NARCIS (Netherlands)

    Li, Y.; Xia, H.; Fan, F.; Feng, Z.; Santen, van R.A.; Hensen, E.J.M.; Li, Can

    2008-01-01

    For the first time an ordered mesoporous silica (Fe–Al-SBA-15) with catalytically active isolated Fe surface species for the hydroxylation of benzene with nitrous oxide is prepared by introduction of Fe3+ in the synthesis gel of Al-SBA-15. Graphical abstract image for this article (ID: b717079c)

  20. Mesostructured Au/C materials obtained by replication of functionalized SBA-15 silica containing highly dispersed gold nanoparticles

    KAUST Repository

    Kerdi, Fatmé ; Caps, Valerie; Tuel, Alain

    2011-01-01

    was the same for both series and apparently did not depend on the nature of the silica template. Both Au/SiO2 templates and their corresponding Au/CMK-3 materials have been characterized by X-ray diffraction, nitrogen adsorption/desorption, chemical analysis

  1. Aminopropyl-modified mesoporous silica SBA-15 as recovery agents of Cu(II)-sulfate solutions: Adsorption efficiency, functional stability and reusability aspects

    International Nuclear Information System (INIS)

    Lombardo, M.V.; Videla, M.; Calvo, A.; Requejo, F.G.; Soler-Illia, G.J.A.A.

    2012-01-01

    Highlights: ► We produce mesoporous amino-silica as Cu(II) adsorbent (1.15–1.75 mmol Cu(II) g −1 ). ► Elemental analysis and XPS demonstrate that amino groups concentrate at the material surface. ► The integrity of the adsorbent through the adsorption, desorption and recycling processes is assessed. ► These materials can be regenerated by exposure to acidic media. ► A careful thermal processing of the material is central to better durability during reprocessing. - Abstract: Hybrid mesoporous materials are potentially useful for metal ion scavenging and retrieval because of their high surface areas, controlled accessibility and tailored functionalization. Some aspects that are linked to the performance of HMM include pore accessibility, stability of the organic functions and reusability. Knowledge of these aspects is critical in the design of adsorption–desorption protocols. In this work we produce and characterize propylamino-substituted large pore silica (SBA-15-N), which is submitted to Cu(II) adsorption from copper sulfate solutions, followed by desorption in acid media and material regeneration. We find that the hybrid material is an efficient adsorbent (1.15–1.75 mmol Cu(II) g −1 ), although a fraction of the organic groups is lost during the adsorption process. An X-ray photoelectron spectroscopy (XPS) study demonstrates that the contents of amino groups are higher in the material surface, leading to different behaviors in Cu(II) complexation along the material. These materials can be regenerated by exposure to acidic media. Thermal processing of the hybrid materials leads to better durability in aqueous solutions during reprocessing, due to enhanced polycondensation of the inorganic framework. Thermally treated samples, once regenerated, are efficient adsorbents in a second step of Cu(II) adsorption. We discuss the materials processing factors involved in the improved adsorption of Cu(II), its quantitative release and reusability of the

  2. Production of Renewable Hydrogen from Glycerol Steam Reforming over Bimetallic Ni-(Cu,Co,Cr Catalysts Supported on SBA-15 Silica

    Directory of Open Access Journals (Sweden)

    Alicia Carrero

    2017-02-01

    Full Text Available Glycerol steam reforming (GSR is a promising alternative to obtain renewable hydrogen and help the economics of the biodiesel industry. Nickel-based catalysts are typically used in reforming reactions. However, the choice of the catalyst greatly influences the process, so the development of bimetallic catalysts is a research topic of relevant interest. In this work, the effect of adding Cu, Co, and Cr to the formulation of Ni/SBA-15 catalysts for hydrogen production by GSR has been studied, looking for an enhancement of its catalytic performance. Bimetallic Ni-M/SBA-15 (M: Co, Cu, Cr samples were prepared by incipient wetness co-impregnation to reach 15 wt % of Ni and 4 wt % of the second metal. Catalysts were characterized by inductively coupled plasma atomic emission spectroscopy (ICP-AES, N2-physisorption, X-ray powder diffraction (XRD, hydrogen temperature programmed reduction (H2-TPR, transmission electron microscopy (TEM, scanning electron microscopy (SEM, and thermogravimetric analyses (TGA, and tested in GSR at 600 °C and atmospheric pressure. The addition of Cu, Co, and Cr to the Ni/SBA-15 catalyst helped to form smaller crystallites of the Ni phase, this effect being more pronounced in the case of the Ni-Cr/SBA-15 sample. This catalyst also showed a reduction profile shifted towards higher temperatures, indicating stronger metal-support interaction. As a consequence, the Ni-Cr/SBA-15 catalyst exhibited the best performance in GSR in terms of glycerol conversion and hydrogen production. Additionally, Ni-Cr/SBA-15 achieved a drastic reduction in coke formation compared to the Ni/SBA-15 material.

  3. Aminopropyl-modified mesoporous silica SBA-15 as recovery agents of Cu(II)-sulfate solutions: Adsorption efficiency, functional stability and reusability aspects

    Energy Technology Data Exchange (ETDEWEB)

    Lombardo, M.V. [Gerencia Quimica, Centro Atomico Constituyentes, CNEA, Av. General Paz 1499 (B1650KNA), San Martin, Buenos Aires (Argentina); Videla, M. [Rhein Chemie Argentina, Luis Maria Drago 1555 - (B1852LGS) Burzaco, Buenos Aires (Argentina); Calvo, A.; Requejo, F.G. [INIFTA-CONICET, Universidad Nacional de La Plata, CC 16 Sucursal 4 (1900), La Plata (Argentina); Soler-Illia, G.J.A.A., E-mail: gsoler@cnea.gov.ar [Gerencia Quimica, Centro Atomico Constituyentes, CNEA, Av. General Paz 1499 (B1650KNA), San Martin, Buenos Aires (Argentina); DQIAyQF, FCEN, Universidad de Buenos Aires, Ciudad Universitaria, Pab. II (C1428EHA), Buenos Aires (Argentina)

    2012-07-15

    Highlights: Black-Right-Pointing-Pointer We produce mesoporous amino-silica as Cu(II) adsorbent (1.15-1.75 mmol Cu(II) g{sup -1}). Black-Right-Pointing-Pointer Elemental analysis and XPS demonstrate that amino groups concentrate at the material surface. Black-Right-Pointing-Pointer The integrity of the adsorbent through the adsorption, desorption and recycling processes is assessed. Black-Right-Pointing-Pointer These materials can be regenerated by exposure to acidic media. Black-Right-Pointing-Pointer A careful thermal processing of the material is central to better durability during reprocessing. - Abstract: Hybrid mesoporous materials are potentially useful for metal ion scavenging and retrieval because of their high surface areas, controlled accessibility and tailored functionalization. Some aspects that are linked to the performance of HMM include pore accessibility, stability of the organic functions and reusability. Knowledge of these aspects is critical in the design of adsorption-desorption protocols. In this work we produce and characterize propylamino-substituted large pore silica (SBA-15-N), which is submitted to Cu(II) adsorption from copper sulfate solutions, followed by desorption in acid media and material regeneration. We find that the hybrid material is an efficient adsorbent (1.15-1.75 mmol Cu(II) g{sup -1}), although a fraction of the organic groups is lost during the adsorption process. An X-ray photoelectron spectroscopy (XPS) study demonstrates that the contents of amino groups are higher in the material surface, leading to different behaviors in Cu(II) complexation along the material. These materials can be regenerated by exposure to acidic media. Thermal processing of the hybrid materials leads to better durability in aqueous solutions during reprocessing, due to enhanced polycondensation of the inorganic framework. Thermally treated samples, once regenerated, are efficient adsorbents in a second step of Cu(II) adsorption. We discuss the

  4. Controlled and localized delivery of c-myc AS-ODN to cells by 3-aminopropyl-trimethoxylsilane modified SBA-15 mesoporous silica

    Science.gov (United States)

    Zhang, Juan; Chen, Minmin; Zhao, Xiqiu; Zhang, Min; Mao, Jinxiang; Cao, Xichuan; Zhang, Zhuoqi

    2018-01-01

    SBA-15 mesoporous silicate was synthesized and functionalized with 3-aminopropyl organic groups through a post-synthesis method. The materials were characterized consecutively by powder X-ray diffraction (XRD), N2 adsorption/desorption analysis and solid-state magic-angle spinning 29Si nuclear magnetic resonance (MAS NMR). Human c-myc anti-sense oligodeoxyneucleotide (AS-ODN) was selected as a model molecule to be loaded onto the surface of bare and functionalized SBA-15 via different loading conditions. It has been found that the amount of AS-ODN incorporated into the porous matrix is strongly dependent on the surface properties, pH of the loading solvent and AS-ODN concentration. The release behaviour of AS-ODN from modified SBA-15 materials was also investigated and depended on conditions chosen. Cellular uptake of the eluted AS-ODN into Hela cells was observed by fluorescent microscopy. The materials showed excellent cytocompatibility. The AS-ODN keeps full transfection and expression activities indicating its structural integrity. The functionalized SBA-15 is an excellent prospect as a biomedical material candidate for the future.

  5. Organically functionalized mesoporous SBA-15 as sorbents for removal of selected pharmaceuticals from water

    Energy Technology Data Exchange (ETDEWEB)

    Bui, Tung Xuan [School of Environmental Science and Engineering, Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of); Kang, Seo-Young [International Environmental Research Center (IERC), Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of); Lee, Sang-Hyup [Water Environment Center, Korea Institute of Science and Technology, Cheongryang, Seoul 130-650 (Korea, Republic of); Choi, Heechul, E-mail: hcchoi@gist.ac.kr [School of Environmental Science and Engineering, Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of)

    2011-10-15

    Highlights: {yields} SBA-15 grafted with aminopropyl, hydroxymethyl, and trimethylsilyl groups as sorbents. {yields} Sorbents for removal of a mixture of 12 pharmaceuticals from water. {yields} Hydroxymethyl-SBA-15 shows similar adsorption efficiency like SBA-15. {yields} Aminopropyl-SBA-15 makes increase for clofibric acid, diclofenac, decrease for atenolol, estrone, trimethoprim. {yields} Trimethylsilyl-SBA-15 makes increase for 9 compounds; 7 compounds from 70.6% to 98.9%. - Abstract: Mesoporous silica SBA-15 and its postfunctionalized counterparts with hydroxymethyl (HM-SBA-15), aminopropyl (AP-SBA-15), and trimethylsilyl (TMS-SBA-15) were prepared and characterized by powder X-ray diffraction, N{sub 2} adsorption-desorption measurement, Fourier-transform infrared spectroscopy, and elemental analysis. The removal of a mixture of 12 selected pharmaceuticals was investigated by batch adsorption experiments onto SBA-15 and the grafted materials. SBA-15 showed to have moderate adsorption affinity with amino-containing (atenolol, trimethoprim) and hydrophobic pharmaceuticals, but it displayed minimal adsorption affinity toward hydrophilic compounds. HM-SBA-15 was analogous with SBA-15 in terms of the adsorption efficiency toward all pharmaceuticals. AP-SBA-15 exhibited an increase in the adsorption of two acidic compounds (clofibric acid, diclofenac) but a decrease in the adsorption of estrone and the two amino-containing compounds. Among the grafted materials, TMS-SBA-15 had the highest adsorption affinity toward most pharmaceuticals. Moreover, the adsorption of nine pharmaceuticals to TMS-SBA-15 was significantly higher than that to SBA-15; seven of which showed the removal percentages from 70.6% to 98.9% onto TMS-SBA-15. The number of pharmaceuticals showing high adsorption efficiency onto TMS-SBA-15 did not alter significantly as the pH changed in the range of 5.5-7.6. The results suggest that TMS-SBA-15 is a promising material for the removal of pharmaceuticals

  6. Organically functionalized mesoporous SBA-15 as sorbents for removal of selected pharmaceuticals from water

    International Nuclear Information System (INIS)

    Bui, Tung Xuan; Kang, Seo-Young; Lee, Sang-Hyup; Choi, Heechul

    2011-01-01

    Highlights: → SBA-15 grafted with aminopropyl, hydroxymethyl, and trimethylsilyl groups as sorbents. → Sorbents for removal of a mixture of 12 pharmaceuticals from water. → Hydroxymethyl-SBA-15 shows similar adsorption efficiency like SBA-15. → Aminopropyl-SBA-15 makes increase for clofibric acid, diclofenac, decrease for atenolol, estrone, trimethoprim. → Trimethylsilyl-SBA-15 makes increase for 9 compounds; 7 compounds from 70.6% to 98.9%. - Abstract: Mesoporous silica SBA-15 and its postfunctionalized counterparts with hydroxymethyl (HM-SBA-15), aminopropyl (AP-SBA-15), and trimethylsilyl (TMS-SBA-15) were prepared and characterized by powder X-ray diffraction, N 2 adsorption-desorption measurement, Fourier-transform infrared spectroscopy, and elemental analysis. The removal of a mixture of 12 selected pharmaceuticals was investigated by batch adsorption experiments onto SBA-15 and the grafted materials. SBA-15 showed to have moderate adsorption affinity with amino-containing (atenolol, trimethoprim) and hydrophobic pharmaceuticals, but it displayed minimal adsorption affinity toward hydrophilic compounds. HM-SBA-15 was analogous with SBA-15 in terms of the adsorption efficiency toward all pharmaceuticals. AP-SBA-15 exhibited an increase in the adsorption of two acidic compounds (clofibric acid, diclofenac) but a decrease in the adsorption of estrone and the two amino-containing compounds. Among the grafted materials, TMS-SBA-15 had the highest adsorption affinity toward most pharmaceuticals. Moreover, the adsorption of nine pharmaceuticals to TMS-SBA-15 was significantly higher than that to SBA-15; seven of which showed the removal percentages from 70.6% to 98.9% onto TMS-SBA-15. The number of pharmaceuticals showing high adsorption efficiency onto TMS-SBA-15 did not alter significantly as the pH changed in the range of 5.5-7.6. The results suggest that TMS-SBA-15 is a promising material for the removal of pharmaceuticals from aqueous phase

  7. Characterization and comprehension of zeolite NaY/mesoporous SBA-15 composite as adsorbent for paraquat

    Energy Technology Data Exchange (ETDEWEB)

    Osakoo, Nattawut, E-mail: natawut.work@gmail.com [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Pansakdanon, Chaianun [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Department of Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani, 34190 (Thailand); Sosa, Narongrit; Deekamwong, Krittanun; Keawkumay, Chalermpan; Rongchapo, Wina [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Chanlek, Narong [Synchrotron Light Research Institute, Nakhon Ratchasima, 30000 (Thailand); Jitcharoen, Juthamas [Department of Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani, 34190 (Thailand); Prayoonpokarach, Sanchai [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Wittayakun, Jatuporn, E-mail: jatuporn@g.sut.ac.th [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand)

    2017-06-01

    NaY was synthesized from fumed silica and further modified to form a composite with SBA-15. Textural properties and basicity of the composite NaY-SBA-15 were between those of the parent materials. Paraquat adsorption on NaY was 204.1 mg/g, higher than that on NaY synthesized with rice husk silica from the previous work. SBA-15 was a poor adsorbent for paraquat. Based on the weight of NaY, the adsorption capacity of analytical-grade paraquat on the NaY-SBA-15 composite was 241.5 mg/g-NaY. Moreover, the composite adsorbed blue dye from a commercial grade paraquat. Interaction between the NaY-SBA-15 and paraquat could be from C and N atoms in paraquat with oxygen atom on NaY-SBA-15. - Highlights: • Zeolite NaY/mesoporous SBA-15 composite was synthesized with a simple method. • NaY and SBA-15 coexisted in the composite confirmed by FTIR, CO{sub 2}-TPD and XPS. • Adsorption capacity of paraquat (mg/g-NaY) was improved by NaY and SBA-15 composite. • C and N atoms in paraquat could interact with oxygen atom on NaY-SBA-15 composite.

  8. Preparation of Pd-Diimine@SBA-15 and Its Catalytic Performance for the Suzuki Coupling Reaction

    Directory of Open Access Journals (Sweden)

    Jiahuan Yu

    2016-11-01

    Full Text Available A highly efficient and stable Pd-diimine@SBA-15 catalyst was successfully prepared by immobilizing Pd onto diimine-functionalized mesoporous silica SBA-15. With the help of diimine functional groups grafted onto the SBA-15, Pd could be anchored on a support with high dispersion. Pd-diimine@SBA-15 catalyst exhibited excellent catalytic performance for the Suzuki coupling reaction of electronically diverse aryl halides and phenylboronic acid under mild conditions with an ultralow amount of Pd (0.05 mol % Pd. When the catalyst amount was increased, it could catalyze the coupling reaction of chlorinated aromatics with phenylboronic acid. Compared with the catalytic performances of Pd/SBA-15 and Pd-diimine@SiO2 catalysts, the Pd-diimine@SBA-15 catalyst exhibited higher hydrothermal stability and could be repeatedly used four times without a significant decrease of its catalytic activity.

  9. Highly Sensitive Fluorescence Probe Based on Functional SBA-15 for Selective Detection of Hg2+

    Directory of Open Access Journals (Sweden)

    Wang Xiaoyu

    2010-01-01

    Full Text Available Abstract An inorganic–organic hybrid fluorescence chemosensor (DA/SBA-15 was prepared by covalent immobilization of a dansylamide derivative into the channels of mesoporous silica material SBA-15 via (3-aminopropyltriethoxysilane (APTES groups. The primary hexagonally ordered mesoporous structure of SBA-15 was preserved after the grafting procedure. Fluorescence characterization shows that the obtained inorganic–organic hybrid composite is highly selective and sensitive to Hg2+ detection, suggesting the possibility for real-time qualitative or quantitative detection of Hg2+ and the convenience for potential application in toxicology and environmental science.

  10. Study on the adsorption of heavy metal ions from aqueous solution on modified SBA-15

    Directory of Open Access Journals (Sweden)

    Liliana Giraldo

    2013-01-01

    Full Text Available Amino-functionalized SBA-15 mesoporous silica was prepared, characterized, and used as an adsorbent for heavy metal ions. The organic - inorganic hybrid material was obtained by a grafting procedure using SBA-15 silica with 3-aminopropyl-triethoxysilane and bis(2,4,4-trimethylpentyl phosphinic acid (Cyanex 272, respectively. The structure and physicochemical properties of the materials were characterized by means of elemental analysis, X-ray diffraction (XRD, nitrogen adsorption - desorption, thermogravimetric analysis, FTIR spectroscopy and immersion calorimetry. The organic functional groups were successfully grafted onto the SBA-15 surface and the ordering of the support was not affected by the chemical modification. The behavior of the grafted solids was investigated for the adsorption of heavy metal ions from aqueous solutions. The hybrid materials showed high adsorption capacity and high selectivity for zinc ions. Other ions, such as cooper and cobalt were absorbed by the modified SBA-15 material.

  11. Fe3O4@mesoporous SBA-15: A magnetically recoverable catalyst for photodegradation of malachite green

    International Nuclear Information System (INIS)

    Aliyan, Hamid; Fazaeli, Razieh; Jalilian, Rahil

    2013-01-01

    Surface of mesostructured silica (SBA-15) was modified by immobilizing Fe 3 O 4 . This modified-nanosized mesoporous silica Fe 3 O 4 @SBA-15 was characterized by FTIR, XRD, BET and SEM. A comparison of the photoefficiency of Fe 3 O 4 @SBA-15 toward photodegradation of malachite green (MG) was investigated in a photocatalytic reactor using UV lamp as a light source. The effect of various experimental parameters on the degradation performance of the process was evaluated by examining catalyst dosage, initial dye concentration and pH of the dye solution in the presence of Fe 3 O 4 @SBA-15 as photocatalyst. It was found that the photocatalyst exhibited significantly high catalytic stability, and the activity loss is negligible after five MG degradation cycles.

  12. Functionalized SBA-15 materials for bilirubin adsorption

    Science.gov (United States)

    Tang, Tao; Zhao, Yanling; Xu, Yao; Wu, Dong; Xu, Jun; Deng, Feng

    2011-05-01

    To investigate the driving force for bilirubin adsorption on mesoporous materials, a comparative study was carried out between pure siliceous SBA-15 and three functionalized SBA-15 mesoporous materials: CH 3-SBA-15 (MS), NH 2-SBA-15 (AS), and CH 3/NH 2-SBA-15 (AMS) that were synthesized by one-pot method. The obtained materials exhibited large surface areas (553-810 m 2/g) and pore size (6.6-7.1 nm) demonstrated by XRD and N 2-ad/desorption analysis. The SEM images showed that the materials had similar fiberlike morphology. The functionalization extent was calculated according to 29Si MAS NMR spectra and it was close to the designed value (10%). The synthesized mesoporous materials were used as bilirubin adsorbents and showed higher bilirubin adsorption capacities than the commercial active carbon. The adsorption capacities of amine functionalized samples AMS and AS were larger than those of pure siliceous SBA-15 and MS, indicating that electrostatic interaction was the dominant driving force for bilirubin adsorption on mesoporous materials. Increasing the ionic strength of bilirubin solution by adding NaCl would decrease the bilirubin adsorption capacity of mesoporous material, which further demonstrated that the electrostatic interaction was the dominant driving force for bilirubin adsorption. In addition, the hydrophobic interaction provided by methyl groups could promote the bilirubin adsorption.

  13. Hydroxyapatite/MCM-41 and SBA-15 Nano-Composites: Preparation, Characterization and Applications

    Science.gov (United States)

    Anunziata, Oscar A.; Martínez, Maria L.; Beltramone, Andrea R.

    2009-01-01

    Composites of hydroxyapatite (HaP) and highly ordered large pore mesoporous silica molecular sieves such as, Al-SBA-15 and Al-MCM-41 (denoted as SBA-15 and MCM-41, respectively) were developed, characterized by XRD, BET, FTIR, HRTEM and NMR-MAS, and applied to fluoride retention from contaminated water. The proposed procedure by a new route to prepare the HaP/SBA-15 and HaP/MCM-41, composites generates materials with aluminum only in tetrahedral coordination, according to the 27Al NMR-MAS results. Free OH- groups of HaP nanocrystals, within the hosts, allowed high capacity fluoride retention. The activity of fluoride retention using HaP/MCM-41 or HaP/SBA-15 was 1-2 orders of magnitude greater, respectively, than with pure HaP.

  14. Development of TREN dendrimers over mesoporous SBA-15 for CO2 adsorption

    International Nuclear Information System (INIS)

    Bhagiyalakshmi, Margandan; Park, Sang Do; Cha, Wang Seog; Jang, Hyun Tae

    2010-01-01

    Mesoporous SBA-15 was synthesized using rice husk ash (RHA) as the silica source and their defective Si-OH groups were grafted with tris(2-aminoethyl) amine (TREN) dendrimers generation through step-wise growth technique. The X-ray diffraction (XRD) and nitrogen adsorption/desorption results of parent SBA-15 obtained from RHA, suggests its resemblance with SBA-15 synthesized using conventional silica sources. Furthermore, the nitrogen adsorption/desorption results of SBA-15/TREN dendrimer generations (G1-G3) illustrates the growth of dendrimer inside the mesopores of SBA-15 and their CO 2 adsorption capacity was determined at 25 deg. C. The maximum CO 2 adsorption capacity of 5-6 and 7-8 wt% over second and third dendrimer generation was observed which is discernibly higher than the reported melamine and PAMAM dendrimers. The experimental CO 2 adsorption capacity was found to be less than theoretically calculated CO 2 adsorption capacity due to inter and intra molecular amidation as result of steric hindrance during the dendrimer growth. These SBA-15/TREN dendrimer generations also exhibit thermal stability up to 350 deg. C and CO 2 adsorption capacity remains unaltered upon seven consecutive runs.

  15. A dansyl group modified SBA-15 INHIBIT logic gate with [Hg2+ and Cl-] or [Hg2+ and Br-] as inputs

    Science.gov (United States)

    Wang, Xiaoyu; Yang, Honglei

    2013-07-01

    We developed a SBA-15-based INHIBIT logic gate (DA-SBA-15) which was prepared by covalent immobilization of a dansylamide derivative into the channels of the mesoporous silica material (SBA-15) via (3-aminopropyl)triethoxysilane (APTES) groups. A series of characteristic results proved that the fluorescent ligand was successfully grafted into the mesopores of SBA-15. The fluorescent characterization revealed excellent selectivity of DA-SBA-15 to the Hg2+ ion. Moreover, DA-SBA-15 can be considered as a selective fluorescent probe for Cl- and Br-. The fluorescent changes of DA-SBA-15 upon the addition of ions (Hg2+, Cl- and Br-) were utilized as an INH logic gate at the molecular level, using [Hg2+ and Cl-] or [Hg2+ and Br-] as chemical inputs and the fluorescence intensity signal as output.

  16. Highly stable and regenerable Mn-based/SBA-15 sorbents for desulfurization of hot coal gas

    International Nuclear Information System (INIS)

    Zhang, F.M.; Liu, B.S.; Zhang, Y.; Guo, Y.H.; Wan, Z.Y.; Subhan, Fazle

    2012-01-01

    Highlights: ► A series of mesoporous Cu x Mn y O z /SBA-15 sorbents were fabricated for hot coal gas desulfurization. ► 1Cu9Mn/SBA-15 sorbent with high breakthrough sulfur capacity is high stable and regenerable. ► Utilization of SBA-15 constrained the sintering and pulverization of sorbents. - Abstract: A series of mesoporous xCuyMn/SBA-15 sorbents with different Cu/Mn atomic ratios were prepared by wet impregnation method and their desulfurization performance in hot coal gas was investigated in a fixed-bed quartz reactor in the range of 700–850 °C. The successive nine desulfurization–regeneration cycles at 800 °C revealed that 1Cu9Mn/SBA-15 presented high performance with durable regeneration ability due to the high dispersion of Mn 2 O 3 particles incorporated with a certain amount of copper oxides. The breakthrough sulfur capacity of 1Cu9Mn/SBA-15 observed 800 °C is 13.8 g S/100 g sorbents, which is remarkably higher than these of 40 wt%LaFeO 3 /SBA-15 (4.8 g S/100 g sorbents) and 50 wt%LaFe 2 O x /MCM-41 (5.58 g S/100 g sorbents) used only at 500–550 °C. This suggested that the loading of Mn 2 O 3 active species with high thermal stability to SBA-15 support significantly increased sulfur capacity at relatively higher sulfidation temperature. The fresh and used xCuyMn/SBA-15 sorbents were characterized by means of BET, XRD, XPS, XAES, TG/DSC and HRTEM techniques, confirmed that the structure of the sorbents remained intact before and after hot coal gas desulfurization.

  17. Growth and physico-chemical properties of interconnected carbon nanotubes in FeSBA-15 mesoporous molecular sieves

    Directory of Open Access Journals (Sweden)

    Ulka Suryavanshi

    2016-03-01

    Full Text Available Carbon nanotubes (CNTs with well-defined hollow interiors, and different morphologies have been grown inside the nanochannels of iron substituted SBA-15 (Santa Barbara Amorphous with different iron contents and well-ordered large mesopores by chemical vapour deposition method. This novel method requires only 3 min for the formation of high quality multiwalled CNTs inside the SBA-15. The physico-chemical characteristics of the prepared CNT/Fe-SBA-15 nanocomposite have been analysed with powder X-ray diffraction (XRD, scanning electron microscopy (SEM, Raman spectroscopy and thermogravimetric analysis (TGA. XRD, Raman spectroscopy and TGA results confirm that the formed CNTs in SBA-15 nanochannels are highly pure and graphitic in nature, which can be altered by tuning the Fe content in the support matrix. SEM images show the interconnected network of SBA-15/CNT where CNT bridges the neighbouring SBA-15 nanoparticles. Interestingly, spring like CNTs and multi-terminal junctions such as Y and H junctions were also observed. The morphology of the CNTs inside the nanochannels of the SBA-15 support can also be controlled by the simple adjustment of the iron content in the SBA-15 framework. It has also been found that the content of Fe in the silica framework of SBA-15 plays a significant role in the formation of the CNTs and the amount of deposited CNTs in the nanochannels of SBA-15 increased with increasing the concentration of iron in framework. Among the materials studied, the FeSBA-15 with the nSi/nFe ratio of 2 showed the highest catalytic activity towards the formation of high quality CNTs.

  18. Immobilization of lipase and keratinase on functionalized SBA-15 nanostructured materials

    Science.gov (United States)

    Le, Hy G.; Vu, Tuan A.; Tran, Hoa T. K.; Dang, Phuong T.

    2013-12-01

    SBA-15 nanostructured materials were synthesized via hydrothermal treatment and were functionalized with 3- aminopropyltriethoxysilane (APTES). The obtained samples were characterized by different techniques such as XRD, BET, TEM, IR and DTA. After functionalization, it showed that these nanostrucrured materials still maintained the hexagonal pore structure of the parent SBA-15. The model enzyms chosen in this study were lipase and keratinase. Lipase was a biocatalyst for hydrolyzation of long chain triglycerides or methyl esters of long chain alcohols and fatty acids; keratinase is a proteolytic enzyme that catalyzes the cleavage of keratin. The functionalized SBA-15 materials were used to immobilize lipase and keratinase, exhibiting higher activity than that of the unfunctionalized pure silica SBA-15 ones. This might be due to the enhancing of surface hydrophobicity upon functionalization. The surface functionalization of the nanostructured silicas with organic groups can favor the interaction between enzyme and the supports and consequently increasing the operational stability of the immobilized enzymes. The loading of lipase on functionalized SBA-15 materials was higher than that of keratinase. This might be rationalized by the difference in size of enzyms.

  19. Removal of patulin from aqueous solutions by propylthiol functionalized SBA-15

    International Nuclear Information System (INIS)

    Appell, Michael; Jackson, Michael A.; Dombrink-Kurtzman, Mary Ann

    2011-01-01

    Propylthiol functionalized SBA-15 silica was investigated to detoxify aqueous solutions contaminated with the regulated mycotoxin patulin. Micelle templated silicas with a specific pore size were synthetically modified to possess propylthiol groups, a functional group known to form Michael reaction products with the conjugated double bond system of patulin. BET surface area analysis indicated the propylthiol functionalized SBA-15 possesses channels with the pore size of 5.4 nm and a surface area of 345 m 2 g -1 . Elemental analysis indicates the silicon/sulfur ratio to be 10:1, inferring one propylthiol substituent for every ten silica residues. The propylthiol modified SBA-15 was effective at significantly reducing high levels of patulin from aqueous solutions (pH 7.0) in batch sorption assays at room temperature. The material was less effective at lower pH; however heating low pH solutions and apple juice to 60 deg, C in the presence of propylthiol functionalized SBA-15 significantly reduced the levels of patulin in contaminated samples. Composite molecular models developed by semi-empirical PM3 and empirical force field methods support patulin permeation through the mesoporous channels of propylthiol functionalized SBA-15. Density functional study at the B3LYP/6-31G(d,p) level predicts the proposed patulin adducts formed by reaction with the thiol residues exhibit less electrophilic properties than patulin. It is demonstrated the use of propylthiol functionalized SBA-15 is a viable approach to reduce patulin levels in aqueous solutions, including contaminated apple juice.

  20. Removal of patulin from aqueous solutions by propylthiol functionalized SBA-15

    Energy Technology Data Exchange (ETDEWEB)

    Appell, Michael, E-mail: michael.appell@ars.usda.gov [Bacterial Foodborne Pathogens and Mycology Research Unit, United States Department of Agriculture, Agricultural Research Service, National Center for Agricultural Utilization Research, 1815 N. University St., Peoria, IL 61604 (United States); Jackson, Michael A.; Dombrink-Kurtzman, Mary Ann [Renewable Product Technology Research Unit, United States Department of Agriculture, Agricultural Research Service, National Center for Agricultural Utilization Research, 1815 N. University St., Peoria, IL 61604 (United States)

    2011-03-15

    Propylthiol functionalized SBA-15 silica was investigated to detoxify aqueous solutions contaminated with the regulated mycotoxin patulin. Micelle templated silicas with a specific pore size were synthetically modified to possess propylthiol groups, a functional group known to form Michael reaction products with the conjugated double bond system of patulin. BET surface area analysis indicated the propylthiol functionalized SBA-15 possesses channels with the pore size of 5.4 nm and a surface area of 345 m{sup 2} g{sup -1}. Elemental analysis indicates the silicon/sulfur ratio to be 10:1, inferring one propylthiol substituent for every ten silica residues. The propylthiol modified SBA-15 was effective at significantly reducing high levels of patulin from aqueous solutions (pH 7.0) in batch sorption assays at room temperature. The material was less effective at lower pH; however heating low pH solutions and apple juice to 60 deg, C in the presence of propylthiol functionalized SBA-15 significantly reduced the levels of patulin in contaminated samples. Composite molecular models developed by semi-empirical PM3 and empirical force field methods support patulin permeation through the mesoporous channels of propylthiol functionalized SBA-15. Density functional study at the B3LYP/6-31G(d,p) level predicts the proposed patulin adducts formed by reaction with the thiol residues exhibit less electrophilic properties than patulin. It is demonstrated the use of propylthiol functionalized SBA-15 is a viable approach to reduce patulin levels in aqueous solutions, including contaminated apple juice.

  1. Controlling reaction pathways for alcohol dehydration and dehydrogenation over FeSBA-15 catalysts

    NARCIS (Netherlands)

    Guan, Y.; Li, Y.; Santen, van R.A.; Hensen, E.J.M.; Li, Can

    2007-01-01

    The iron location in FeSBA-15 strongly influences the selectivity to dehydrogenation and dehydration in ethanol conversion. At low iron loading, Fe is present as isolated species in the amorphous silica phase. At higher loading additional aggregated forms of iron oxide exist. Isolated species in the

  2. Carboxylic acid-functionalized SBA-15 nanorods for gemcitabine delivery

    International Nuclear Information System (INIS)

    Bahrami, Zohreh; Badiei, Alireza; Ziarani, Ghodsi Mohammadi

    2015-01-01

    The present study deals with the functionalization of mesoporous silica nanoparticles as drug delivery systems. Mono, di, and tri amino-functionalized SBA-15 nanorods were synthesized by post-grafting method using (3-aminopropyl) triethoxysilane, N-(2-aminoethyl-)3- aminopropyltrimethoxysilane, and 3-[2-(2-aminoethylamino) ethylamino] propyl trimethoxysilane, respectively. The carboxylic acid derivatives of the amino-functionalized samples were obtained using succinic anhydride. Tminopropyltrimethoxysilanehe obtained modified materials were investigated as matrixes for the anticancer drug (gemcitabine) delivery. The prepared samples were characterized by SAXS, N 2 adsorption/desorption, SEM, transmission electron microscopy, thermogravimetric analysis, and FTIR and UV spectroscopies. The adsorption and release properties of all samples were studied. It was revealed that the adsorption capacity and release behavior of gemcitabine were highly dependent on the type of the introduced functional groups. The carboxylic acid-modified samples have higher loading content, due to the strong interaction with gemcitabine. The maximum content of deposited drug in the modified SBA-15 nanorods is close to 40 wt%. It was found that the surface functionalization leads toward significant decrease of the drug release rate. The carboxylic acid-functionalized samples have slower release rate in contrast with the amino-functionalized samples

  3. Selective synthesis of vitamin K3 over mesoporous NbSBA-15 catalysts synthesized by an efficient hydrothermal method.

    Science.gov (United States)

    Selvaraj, M; Park, D-W; Kim, I; Kawi, S; Ha, C S

    2012-08-28

    Well hexagonally ordered NbSBA-15 catalysts synthesized by an efficient hydrothermal method were used, for the first time, for the selective synthesis of vitamin K(3) by liquid-phase oxidation of 2-methyl-1-naphthol (2MN1-OH) under various reaction conditions. The recyclable NbSBA-15 catalysts were also reused to find their catalytic activities. To investigate the leaching of non-framework niobium species on the surface of silica networks, the results of original and recyclable NbSBA-15 catalysts were correlated and compared. To find an optimum condition for the selective synthesis of vitamin K(3), the washed NbSBA-15(2.2pH) was extensively used in this reaction with various reaction parameters such as temperature, time and ratios of reactant (2M1N-OH to H(2)O(2)), and the obtained results were also demonstrated. Additionally, the liquid-phase oxidation of 2M1N-OH was carried out with different solvents to find the best solvent with a good catalytic activity. Based on the all catalytic studies, the vitamin K(3) selectivity (97.3%) is higher in NbSBA-15(2.2pH) than that of other NbSBA-15 catalysts, and the NbSBA-15(2.2pH) is found to be a highly active and eco-friendly heterogeneous catalyst for the selective synthesis of vitamin K(3).

  4. Inclusion of cefalexin in SBA-15 mesoporus material and release property

    International Nuclear Information System (INIS)

    Zhai, Qing-Zhou

    2012-01-01

    SBA-15 (Santa Barbara Amorphous-15) is a high ordered mesoporous material. It has the advantages of a non-toxic property, good hydrothermal stability and thermal stability, etc. Inside inner surface a lot of silanols exist. Pore diameter size is uniform and pore size distribution is narrow. This structural feature makes SBA-15 have a higher loading drug amount and be able to effectively extend the drug release cycle. In this paper, polyethylene glycol-block-polypropylene glycol-block-polyethylene glycol was used as template and tetraethyl orthosilicate was used as silica source to prepare SBA-15 by hydrothermal synthesis method. Cefalexin was included in SBA-15 and the included cefalexin drug content was 158.72 mg/g. The composite materials were characterized by using chemical analysis, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), infrared (IR) spectroscopy, and low temperature nitrogen adsorption–desorption. The results showed that cefalexin had been successfully included in host SBA-15 pore channels. Rational analyses of the release processes of cefalexin drug from the pores of SBA-15 to the simulated body fluid, simulated gastric juice and simulated intestinal fluid were made and sustained-release effects of the drug in complex system were studied. The results showed that in simulated body fluid within 1–5 h cefalexin was fast released and the cumulative release reached 50.00% at 5 h. In 15–20 h, the sustained release speed of cefalexin drug in the composite material decreased and the sustained-release cumulative amount reached 99.87% at 20 h. The release of cefalexin was basically complete. In simulated gastric fluid, composite material sustained-release ended at 4 h, the cumulative sustained release ratio reaching 26.10%. In simulated gastric fluid, the sustained-release was complete at 7 h, the cumulative sustained release ratio reaching 32.46%. The composite material of SBA-15 and cefalexin

  5. A Pd/SBA-15 composite: synthesis, characterization and protein biosensing

    Energy Technology Data Exchange (ETDEWEB)

    Liu Yuge; Zhang Jingjing; Hou Wenhua; Zhu Junjie [Key Laboratory of Mesoscopic Chemistry and Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China)], E-mail: whou@nju.edu.cn, E-mail: jjzhu@nju.edu.cn

    2008-04-02

    In this paper, palladium (Pd) nanoparticles have been successfully encapsulated into the channels of modified SBA-15 in situ via a facile, ethylene glycol (EG)-assisted sonochemical method. The products were confirmed by x-ray diffraction, transmission electron microscopy (TEM) and nitrogen adsorption analysis. The Pd/SBA-15 composite was used for the realization of direct electron transfer of hemoglobin (Hb). Electrochemical results showed that the Pd nanoparticles in the channels of SBA-15 could enhance the direct electron transfer between Hb and the electrode surface. The composite modified electrode displayed excellent electrochemical behavior. The sensor fabricated by the composite showed an excellent response to the reduction of hydrogen peroxide (H{sub 2}O{sub 2}), and the linear range for the determination of H{sub 2}O{sub 2} was from 1.8 to 119.3 {mu}M with a detection limit of 0.8 {mu}M.

  6. Thermogravimetric Analysis (TGA) Profile of Modified Sba-15 at Different Amount of Alkoxy silane Group

    International Nuclear Information System (INIS)

    Norhasyimi Rahmat; Nur Fathilah Mohd Yusof; Ezani Hafiza

    2014-01-01

    This study focused on meso porous silica SBA-15 modified with alkoxy silane functional group; phenyltriethoxysilane (PTES) and vinyltriethoxysilane (VTES) using direct synthesis and post-grafting methods. By direct synthesis method, SBA-15 template by triblock copolymer (P123) and functionalized with alkoxy silane groups at different amount of loadings were co-condensed with tetraethyl orthosilicate (TEOS) under acidic conditions. As for post-grafting method, different loadings of alkoxy silane groups were added after co-condensation of TEOS with P123 template. Both synthesis methods used calcination process to remove surfactant template at 550 degree Celsius for 5 hours. The derivatized SBA-15 was characterized by thermogravimetric analysis to evaluate the profile at different loadings of alkoxy silane groups with different synthesis method. At temperature range of 300-800 degree Celsius, post-grafting method displayed the highest weight loss of phenyl and vinyl groups. However, there was no significant difference of weight loss for different amount of organo silane groups. In this study, TGA has shown to be significant characterization means to determine the effects of different method used in synthesizing modified SBA-15. It was shown that different loading of phenyl and vinyl groups did not affect the efficiency of surfactant removal. (author)

  7. Effect of amine functionalization of spherical MCM-41 and SBA-15 on controlled drug release

    International Nuclear Information System (INIS)

    Szegedi, A.; Popova, M.; Goshev, I.; Mihaly, J.

    2011-01-01

    MCM-41 and SBA-15 silica materials with spherical morphology and different particle sizes were synthesized and modified by post-synthesis method with 3-aminopropyltriethoxysilane (APTES). A comparative study of the adsorption and release of a model drug, ibuprofen, were carried out. The modified and drug loaded mesoporous materials were characterized by XRD, TEM, N 2 physisorption, thermal analysis, elemental analysis and FT-IR spectroscopy. Surface modification with amino groups resulted in high degree of ibuprofen loading and slow rate of release for MCM-41, whereas it was the opposite for SBA-15. The adsorbed drug content and the delivery rate can be predetermined by the choice of mesoporous material with the appropriate structural characteristics and surface functionality. -- Graphical Abstract: Ibuprofen delivery from the parent and amino-modified spherical MCM-41 materials with 100 nm (small) and 500 nm (large) particle sizes. Display Omitted Highlights: → Spherical type MCM-41 and SBA-15 with different particle sizes were modified by APTES. → Adsorption and release rate of ibuprofen were compared. → High degree of ibuprofen loading, slow release rate for MCM-41, the opposite for SBA-15. → MCM-41 with 100 nm particles was more stable and showed slower release rate

  8. Propene epoxidation over Au/Ti-SBA-15 catalysts

    NARCIS (Netherlands)

    Sacaliuc, E.; Beale, A.M.; Weckhuysen, B.M.; Nijhuis, T.A.

    2007-01-01

    Highly dispersed gold nanoparticles were synthesized within the channels of a mesoporous Ti-SBA-15 support, followed by thorough catalyst characterization and testing in the selective epoxidation of propene to propene oxide. For this purpose, two series of Ti-SBA-15 materials differing in their Ti

  9. Hydrodeoxygenation of Guaiacol Over Pt/Al-SBA-15 Catalysts.

    Science.gov (United States)

    Yu, Mi Jin; Park, Sung Hoon; Jeon, Jong-Ki; Ryu, Changkook; Sohn, Jung Min; Kim, Sang Chai; Park, Young-Kwon

    2015-01-01

    Upgrading of bio-oil through catalytic hydrodeoxygenation (HDO) reaction was investigated for guaiacol as a model compound. A batch reactor was used for the reaction condition of 40 bar and 250 degrees C. The target product was cyclohexane. Pt/Al-SBA-15 with the Si/Al ratios of 20, 40, and 80 and Pt/HZSM-5 were used as the catalyst. The SBA-15 catalysts were characterized by N2 adsorption-desorption, X-ray diffraction analysis, and temperature programmed desorption of ammonia. The order of cyclohexane yield was Pt/Al-SBA-15 (Si/Al = 20) > Pt/Al-SBA-15(40) > Pt/Al-SBA-15 (80), indicating that the quantity of acid sites plays an important role in the HDO reaction. On the other hand, Pt/HZSM-5 led to a very low cyclohexane yield, in spite of its abundant strong acid sites, due to its small pore size.

  10. Stability and Catalytic Kinetics of Horseradish Peroxidase Confined in Nanoporous SBA-15

    DEFF Research Database (Denmark)

    Ikemoto, Hediki; Chi, Qijin; Ulstrup, Jens

    2010-01-01

    We have synthesized nanoporous silica, SBA-15 in the 1 m size range with the pore diameter of 7.6 nm. The redox enzyme horseradish peroxidase (HRP) was entrapped in the pores to form nanostructured hybrid materials. The catalytic activity of free and immobilized enzyme was first compared at room...... likely due to different hydrogen bonding of water and increased hydration strength of the protein inside the nanopores....

  11. Carbon material formation on SBA-15 and Ni-SBA-15 and residue constituents during acetylene decomposition

    Energy Technology Data Exchange (ETDEWEB)

    Chiang, Hung-Lung, E-mail: hlchiang@mail.cmu.edu.tw [Department of Risk Management, China Medical University, Taichung 40402, Taiwan (China); Wu, Trong-Neng [Department of Public Health, China Medical University, Taichung 40402, Taiwan (China); Ho, Yung-Shou [Department of Applied Chemistry and Materials Science, Fooyin University, Kaohsiung 831, Taiwan (China); Zeng, Li-Xuan [Department of Risk Management, China Medical University, Taichung 40402, Taiwan (China)

    2014-07-15

    Highlights: • Acetylene was decomposed on SBA-15 and Ni-SBA-15 at 650–850 °C. • Carbon spheres and filaments were formed after acetylene decomposition. • PAHs were determined in tar and residues. • Exhaust constituents include CO{sub 2}, H{sub 2}, NO{sub x} and hydrocarbon species. - Abstract: Carbon materials including carbon spheres and nanotubes were formed from acetylene decomposition on hydrogen-reduced SBA-15 and Ni-SBA-15 at 650–850 °C. The physicochemical characteristics of SBA-15, Ni-SBA-15 and carbon materials were analyzed by field emission scanning electronic microscopy (FE-SEM), Raman spectrometry, and energy dispersive spectrometry (EDS). In addition, the contents of polyaromatic hydrocarbons (PAHs) in the tar and residue and volatile organic compounds (VOCs) in the exhaust were determined during acetylene decomposition on SBA-15 and Ni-SBA-15. Spherical carbon materials were observed on SBA-15 during acetylene decomposition at 750 and 850 °C. Carbon filaments and ball spheres were formed on Ni-SBA-15 at 650–850 °C. Raman spectroscopy revealed peaks at 1290 (D-band, disorder mode, amorphous carbon) and 1590 (G-band, graphite sp{sup 2} structure) cm{sup −1}. Naphthalene (2 rings), pyrene (4 rings), phenanthrene (3 rings), and fluoranthene (4 rings) were major PAHs in tar and residues. Exhaust constituents of hydrocarbon (as propane), H{sub 2}, and C{sub 2}H{sub 2} were 3.9–2.6/2.7–1.5, 1.4–2.8/2.6–4.3, 4.2–2.4/3.2–1.7% when acetylene was decomposed on SBA-15/Ni-SBA-15, respectively, corresponding to temperatures ranging from 650 to 850 °C. The concentrations of 52 VOCs ranged from 9359 to 5658 and 2488 to 1104 ppm for SBA-15 and Ni-SBA-15 respectively, at acetylene decomposition temperatures from 650 to 850 °C, and the aromatics contributed more than 87% fraction of VOC concentrations.

  12. Synthesis of Pt-Sn core-shell nanoparticles deposited on SBA-15 modified

    Energy Technology Data Exchange (ETDEWEB)

    Alvarez-Contreras, L.; Alonso-Lemus, I. [Centro de Investigacion en Materiales Avanzados S.C., Laboratorio Nacional de Nanotecnologia (Mexico); Botte, G. G. [Ohio University, Center for Electrochemical Engineering Research, Department of Chemical and Biomolecular Engineering (United States); Verde-Gomez, Y., E-mail: ysmaelverde@yahoo.com [Instituto Tecnologico de Cancun (Mexico)

    2013-07-15

    A novel one-step synthesis method to prepare Pt-Sn bimetallic nanoparticles supported on mesoporous silica with high surface area (SBA-15, 700 m{sup 2}/g) and narrow pore size distribution (around 9.5 nm) was developed. Tin incorporation plays an important dual role, to create active sites into the silica walls that serve as particles anchors center, and to grow Pt-Sn core-shell nanoparticles. High-resolution transmission and scanning electron microscopy, and X-ray diffraction pattern confirm the formation of the Pt-Sn core-shell type nanoparticles ( Almost-Equal-To 1-10 nm). The metal loading was 2.2 and 2.3 wt% for Pt and Sn, respectively. Electron microscopy results show that the metal nanoparticles were deposited not only on the matrix, but also inside of it. Structural, textural, and morphological features of the SBA-15 were slightly affected after the nanoparticles deposition, maintaining its high surface area. The results obtained suggest that Pt-Sn on SBA-15 could be attractive material for several catalytic applications, due to the narrow particle size distribution achieved (from 1 to 10 nm) the high dispersion on the support, as well as the Pt-Sn alloy developed.Graphical Abstract.

  13. Selective Preparation of trans-Carveol over Ceria Supported Mesoporous Materials MCM-41 and SBA-15

    Directory of Open Access Journals (Sweden)

    Nariman F. Salakhutdinov

    2013-05-01

    Full Text Available Ce-modified mesoporous silica materials MCM-41 and SBA-15, namely 32 wt % Ce–Si–MCM-41, 16 wt % Ce–H–MCM-41 and 20 wt % Ce–Si–SBA-15, were prepared, characterized and studied in the selective preparation of trans-carveol by α-pinene oxide isomerization. The characterizations of these catalysts were performed using scanning electron microscopy, X-ray photoelectron spectroscopy, nitrogen adsorption and FTIR pyridine adsorption. Selective preparation of trans-carveol was carried out in the liquid phase in a batch reactor. The activity and the selectivity of catalyst were observed to be influenced by their acidity, basicity and morphology of the mesoporous materials. The formation of trans-carveol is moreover strongly influenced by the basicity of the used solvent and in order to achieve high yields of this desired alcohol it is necessary to use polar basic solvent.

  14. Preparation and characterization of catalyst 20% Co/SBA-15

    International Nuclear Information System (INIS)

    Lima, L.A.; Nogueira, A.C.; Rodrigues, J.J.; Rodrigues, M.G.F.

    2012-01-01

    The utilization of molecular sieves as supports for cobalt catalysts are promising. SBA-15 is a class of mesoporous silicate with a high thermal stability and high degree of structural order, which confers an important feature for the catalytic process. It was prepared SBA-15 molecular sieve with molar composition: 1.0 TEOS: 0017P123: 5.7 HCl: 193 H2O. The deposition of cobalt on the substrate SBA-15 was performed by wet impregnation, using a solution of 0.1M cobalt nitrate. The materials were characterized by the techniques of X-Ray Diffraction (XRD), chemical analysis by X-Ray Spectrometry by Energy Dispersive (EDX), and nitrogen adsorption (BET). By XRD and BET verified the formation of SBA-15, and after the impregnation there was no change in the structure, with EDX showed that the impregnation method is efficient, the sample showed cobalt content close to the nominal value. (author)

  15. Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Jae Hwan [Nuclear Fuel Cycle Process Development Division, Korea Atomic Energy Research Institute, 989-111 Daeduk-daero, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of); Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of); Park, Hwan Seo; Ahn, Do-Hee [Nuclear Fuel Cycle Process Development Division, Korea Atomic Energy Research Institute, 989-111 Daeduk-daero, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of); Yim, Man-Sung, E-mail: msyim@kaist.ac.kr [Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of)

    2016-11-15

    The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi{sub 2}O{sub 3} (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi{sub 2}O{sub 3} and the glass composition. It was confirmed that BiI{sub 3}, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi{sub 5}O{sub 7}I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10{sup −3}–10{sup −2} g/m{sup 2} day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of {sup 129}I. - Highlights: • Glass composite waste forms were developed to stabilize iodine confined in Bi-embedded SBA-15. • BiI{sub 3} within Bi-embedded SBA-15 was transformed to BiOI and Bi{sub 5}O{sub 7}I during sintering process. • Iodine volatility was significantly affected by glass composition and Bi{sub 2}O{sub 3} additive. • Iodine leaching rates were 10{sup −3}–10{sup −2} g/m{sup 2} day due to the stable iodine phases encapsulated by glassy networks. • Glass composite waste form of Bi-embedded SBA-15 is expected to be a candidate material for stable storage of {sup 129}I.

  16. Visible Light-Induced Metal Free Surface Initiated Atom Transfer Radical Polymerization of Methyl Methacrylate on SBA-15

    Directory of Open Access Journals (Sweden)

    Liang Ma

    2017-02-01

    Full Text Available Surface-initiated atom transfer radical polymerization (SI-ATRP is one of the most versatile techniques to modify the surface properties of materials. Recent developed metal-free SI-ATRP makes such techniques more widely applicable. Herein photo-induced metal-free SI-ATRP of methacrylates, such as methyl methacrylate, N-isopropanyl acrylamide, and N,N-dimethylaminoethyl methacrylate, on the surface of SBA-15 was reported to fabricate organic-inorganic hybrid materials. A SBA-15-based polymeric composite with an adjustable graft ratio was obtained. The structure evolution during the SI-ATRP modification of SBA-15 was monitored and verified by FT-IR, XPS, TGA, BET, and TEM. The obtained polymeric composite showed enhanced adsorption ability for the model compound toluene in aqueous conditions. This procedure provides a low-cost, readily available, and easy modification method to synthesize polymeric composites without the contamination of metal.

  17. Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

    Science.gov (United States)

    Yang, Jae Hwan; Park, Hwan Seo; Ahn, Do-Hee; Yim, Man-Sung

    2016-11-01

    The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi2O3 (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi2O3 and the glass composition. It was confirmed that BiI3, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi5O7I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10-3-10-2 g/m2 day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of 129I.

  18. Grafting of alumina on SBA-15: Effect of surface roughness

    Czech Academy of Sciences Publication Activity Database

    Zukal, Arnošt; Šiklová, Helena; Čejka, Jiří

    2008-01-01

    Roč. 24, č. 17 (2008), s. 9837-9842 ISSN 0743-7463 R&D Projects: GA AV ČR KAN100400701 Institutional research plan: CEZ:AV0Z40400503 Keywords : alumina-grafted materials * SBA-15 * Nitrogen adsorption Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.097, year: 2008

  19. Sulfated zirconia modified SBA-15 catalysts for cellobiose hydrolysis

    NARCIS (Netherlands)

    Degirmenci, V.; Uner, D.; Cinlar, B.; Shanks, B.H.; Yilmaz, A.; Santen, van R.A.; Hensen, E.J.M.

    2011-01-01

    Zirconia modified SBA-15 becomes a very active catalyst for the selective hydrolysis of cellobiose to glucose after sulfation. Spectroscopic investigations indicate the presence of Brønsted acid sites with similar properties to those present in conventional sulfated zirconia. Indications are found

  20. Immobilization of HRP in Mesoporous Silica and Its Application for the Construction of Polyaniline Modified Hydrogen Peroxide Biosensor

    Directory of Open Access Journals (Sweden)

    Chien-Chung Chen

    2009-06-01

    Full Text Available Polyaniline (PANI, an attractive conductive polymer, has been successfully applied in fabricating various types of enzyme-based biosensors. In this study, we have employed mesoporous silica SBA-15 to stably entrap horseradish peroxidase (HRP, and then deposited the loaded SBA-15 on the PANI modified platinum electrode to construct a GA/SBA-15(HRP/PANI/Pt biosensor. The mesoporous structures and morphologies of SBA-15 with or without HRP were characterized. Enzymatic protein assays were employed to evaluate HRP immobilization efficiency. Our results demonstrated that the constructed biosensor displayed a fine linear correlation between cathodic response and H2O2 concentration in the range of 0.02 to 18.5 mM, with enhanced sensitivity. In particular, the current approach provided the PANI modified biosensor with improved stability for multiple measurements.

  1. Surface PEGylation of mesoporous silica materials via surface-initiated chain transfer free radical polymerization: Characterization and controlled drug release.

    Science.gov (United States)

    Huang, Long; Liu, Meiying; Mao, Liucheng; Huang, Qiang; Huang, Hongye; Wan, Qing; Tian, Jianwen; Wen, Yuanqing; Zhang, Xiaoyong; Wei, Yen

    2017-12-01

    As a new type of mesoporous silica materials with large pore diameter (pore size between 2 and 50nm) and high specific surface areas, SBA-15 has been widely explored for different applications especially in the biomedical fields. The surface modification of SBA-15 with functional polymers has demonstrated to be an effective way for improving its properties and performance. In this work, we reported the preparation of PEGylated SBA-15 polymer composites through surface-initiated chain transfer free radical polymerization for the first time. The thiol group was first introduced on SBA-15 via co-condensation with γ-mercaptopropyltrimethoxysilane (MPTS), that were utilized to initiate the chain transfer free radical polymerization using poly(ethylene glycol) methyl ether methacrylate (PEGMA) and itaconic acid (IA) as the monomers. The successful modification of SBA-15 with poly(PEGMA-co-IA) copolymers was evidenced by a series of characterization techniques, including 1 H NMR, FT-IR, TGA and XPS. The final SBA-15-SH- poly(PEGMA-co-IA) composites display well water dispersity and high loading capability towards cisplatin (CDDP) owing to the introduction of hydrophilic PEGMA and carboxyl groups. Furthermore, the CDDP could be released from SBA-15-SH-poly(PEGMA-co-IA)-CDDP complexes in a pH dependent behavior, suggesting the potential controlled drug delivery of SBA-15-SH-poly(PEGMA-co-IA). More importantly, the strategy should be also useful for fabrication of many other functional materials for biomedical applications owing to the advantages of SBA-15 and well monomer adoptability of chain transfer free radical polymerization. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Desidratação de etanol sobre material nanoestruturado do tipo LaSBA-15 Ethanol dehydration over LaSBA-15 nanostrutured material

    Directory of Open Access Journals (Sweden)

    Geraldo E. Luz Jr

    2010-01-01

    Full Text Available La-incorporated SBA-15 mesopourous molecular sieves (LaSBA-15 were directly synthesized with aim to convert ethanol to ethylene. The samples were characterized by XRD, XRF, nitrogen sorption and acidity, by thermodesorption of n-buthylamine. The results have indicated that all the samples have showed high ordered mesostructure with a large average pore size, and that the lanthanum incorporation has caused an increase in the acidity of the SBA-15. The LaSBA-15 samples have improved, with low deactivation rate, the conversion of the ethanol to water, ether, acetaldehyde and ethylene. In addition, they have increased the ethylene selectivity.

  3. Effect of ceria and zirconia promotors on Ni/SBA-15 catalysts for coking and sintering resistant steam reforming of propylene glycol in microreactors

    NARCIS (Netherlands)

    Shanmugam, V.; Zapf, R.; Neuberg, S.; Hessel, V.; Kolb, G.

    2017-01-01

    Highly dispersed and size controlled Ni nanoparticles in CeO2, ZrO2 and CeO2-ZrO2 promoted mesoporous SBA-15 silica were achieved with the aid of treatment by ultrasound. The catalysts were characterized systematically to investigate their morphological structure and surface properties. It was found

  4. Size and spatial distribution of micropores in SBA-15 using CM-SANS

    International Nuclear Information System (INIS)

    Pollock, Rachel A.; Walsh, Brenna R.; Fry, Jason A.; Ghampson, Tyrone; Centikol, Ozgul; Melnichenko, Yuri B.; Kaiser, Helmut; Pynn, Roger; Frederick, Brian G.

    2011-01-01

    Diffraction intensity analysis of small-angle neutron scattering measurements of dry SBA-15 have been combined with nonlocal density functional theory (NLDFT) analysis of nitrogen desorption isotherms to characterize the micropore, secondary mesopore, and primary mesopore structure. The radial dependence of the scattering length density, which is sensitive to isolated surface hydroxyls, can only be modeled if the NLDFT pore size distribution is distributed relatively uniformly throughout the silica framework, not localized in a 'corona' around the primary mesopores. Contrast matching-small angle neutron scattering (CM-SANS) measurements, using water, decane, tributylamine, cyclohexane, and isooctane as direct probes of the size of micropores indicate that the smallest pores in SBA-15 have diameter between 5.7 and 6.2 (angstrom). Correlation of the minimum pore size with the onset of the micropore size distribution provides direct evidence that the shape of the smallest micropores is cylinderlike, which is consistent with their being due to unraveling of the polymer template.

  5. Template occluded SBA-15: An effective dissolution enhancer for poorly water-soluble drug

    Energy Technology Data Exchange (ETDEWEB)

    Fu Tingming, E-mail: futingming@gmail.com [College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210029 (China); Guo Liwei; Le Kang; Wang Tianyao; Lu Jin [College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210029 (China)

    2010-09-15

    The aim of the present work was to improve the dissolution rate of piroxicam by inclusion into template occluded SBA-15. Our strategy involves directly introducing piroxicam into as-prepared SBA-15 occluded with P123 (EO{sub 20}PO{sub 70}EO{sub 20}) by self assembling method in acetonitrile/methylene chloride mixture solution. Ultraviolet spectrometry experiment and thermogravimetric analysis-differential scanning calorimetry (TG-DSC) profiles show that the piroxicam and P123 contents in the inclusion compound are 12 wt% and 28 wt%, respectively. X-ray powder diffraction and DSC analysis reveal that the included piroxicam is arranged in amorphous form. N{sub 2} adsorption-desorption experiment indicates that the piroxicam has been introduced to the mesopores instead of precipitating at the outside of the silica material. The inclusion compound was submitted to in vitro dissolution tests, the results show that the piroxicam dissolve from template occluded inclusion compound more rapidly, than these from the piroxicam crystalline and template removed samples in all tested conditions. Thus a facile method to improve the dissolution rate of poorly water-soluble drug was established, and this discovery opens a new avenue for the utilization of templates used for the synthesis of mesoporous materials.

  6. Template occluded SBA-15: An effective dissolution enhancer for poorly water-soluble drug

    International Nuclear Information System (INIS)

    Fu Tingming; Guo Liwei; Le Kang; Wang Tianyao; Lu Jin

    2010-01-01

    The aim of the present work was to improve the dissolution rate of piroxicam by inclusion into template occluded SBA-15. Our strategy involves directly introducing piroxicam into as-prepared SBA-15 occluded with P123 (EO 20 PO 70 EO 20 ) by self assembling method in acetonitrile/methylene chloride mixture solution. Ultraviolet spectrometry experiment and thermogravimetric analysis-differential scanning calorimetry (TG-DSC) profiles show that the piroxicam and P123 contents in the inclusion compound are 12 wt% and 28 wt%, respectively. X-ray powder diffraction and DSC analysis reveal that the included piroxicam is arranged in amorphous form. N 2 adsorption-desorption experiment indicates that the piroxicam has been introduced to the mesopores instead of precipitating at the outside of the silica material. The inclusion compound was submitted to in vitro dissolution tests, the results show that the piroxicam dissolve from template occluded inclusion compound more rapidly, than these from the piroxicam crystalline and template removed samples in all tested conditions. Thus a facile method to improve the dissolution rate of poorly water-soluble drug was established, and this discovery opens a new avenue for the utilization of templates used for the synthesis of mesoporous materials.

  7. Preparation of SBA-15-PAMAM as a Nano Adsorbent for Removal of Acid Red 266 from Aqueous Media: Batch Adsorption and Equilibrium Studies

    Directory of Open Access Journals (Sweden)

    Maryam Mirzaie

    2017-12-01

    Full Text Available The purpose of the present study was to increase the adsorption capacity of SBA-15 for acidic dyes. Ordered mesoporous silica SBA-15 was successfully synthesized and functionalized by polyamidoamine (PAMAM dendrimer to develop an efficient anionic dye adsorbent. The prepared materials were characterized by field emission scanning electron microscope (FE-SEM, Fourier transforms infrared spectroscope (FT-IR and N2 adsorption–desorption analysis. The study was concocted in the Science and Research Branch of Islamic Azad University of Tehran, Iran in 2016. The produced adsorbent (SBA-15-Den was applied for the removal of Acid Red 266 (AR266 from aqueous media. The effects of various operational parameters including solution pH, adsorbent dosage, contact time, and temperature on removal of AR266 using SBA-15-Den were investigated in batch adsorption mode. Within the optimum conditions, SBA-15-Den exhibited an excellent adsorptive capability of 1111.11 mg/g. Equilibrium data were best described by Langmuir model (R2 > 0.98 completely.

  8. Ascorbyl Tetraisopalmitate Inclusion into Υ-Cyclodextrin and Mesoporous SBA-15: Preparation, Characterization and In Vitro Release Study

    Directory of Open Access Journals (Sweden)

    Maria Bastianini

    2017-07-01

    Full Text Available Ascorbic acid or vitamin C is a strong antioxidant widely used in cosmetic and food fields. This vitamin is very unstable and rapidly undergoes degradation. In order to solve this problem and to obtain a stable ascorbic acid, Nikkol Group has developed ascorbyltetraisopalmitate (VC-IP. This raw material is an oil phase, already well-known and employed in the cosmetic market. The objective of this study is to obtain VC-IP in micro-powder form, in order to produce a new raw material that is easily dispersible in oil and water phases and useful for make-up and color cosmetic applications. Various types of drug carriers were studied and considered in order to support VC-IP and obtain the conversion in powder. Υ-cyclodextrin and mesoporous silica SBA-15 were chosen as the best candidates. A white powder of supported VC-IP was obtained with each carrier (VC-IP@cyclodextrin, VC-IP@SBA-15. The systems underwent physicochemical characterization and in vitro release tests were carried out. Based on the conducted study, it can be concluded that by supporting VC-IP on Υ-cyclodextrin and SBA-15, it is feasible to obtain a new raw material in powder form. The two carriers possess different release profiles, adding the possibility to finely tune the release of the active component in smart formulations.

  9. In-situ infrared study of CO{sub 2} adsorption on SBA-15 grafted with {gamma}-(aminopropyl)triethoxysilane

    Energy Technology Data Exchange (ETDEWEB)

    Alex C.C. Chang; Steven S.C. Chuang; McMahan Gray; Yee Soong [University of Akron, Akron, OH (United States). Chemical Engineering Department

    2003-04-01

    CO{sub 2} adsorption/desorption on SBA-15 grafted with {gamma}-(aminopropyl)triethoxysilane (APTS) has been studied by infrared spectroscopy coupled with temperature-programmed desorption. SBA-15, a mesoporous silica material with a uniform pore size of 21 nm and a surface area of 200-230 m{sup 2}/g, provides an OH functional group for grafting of {gamma}-(aminopropyl)triethoxysilane. The amine-grafted SBA-15 adsorbed CO{sub 2} as carbonates and bicarbonates with a total capacity of 200-400 {mu}mol/g. The heat of CO{sub 2} desorption was determined to be 3.2-4.5 kJ/mol in the presence of H{sub 2}O and 6.6-11.0 kJ/mol in the absence of H{sub 2}O during temperature-programmed desorption. Repeated CO{sub 2} adsorption/desorption CO{sub 2} cycles shifted the desorption peak temperature downward and decreased the heat of CO{sub 2} adsorption. 22 refs., 9 figs., 3 tabs.

  10. Modifying the Hierarchical Porosity of SBA-15 via Mild-Detemplation Followed by Secondary Treatments

    NARCIS (Netherlands)

    Zhang, Zheng; Melian-Cabrera, Ignacio

    2014-01-01

    Fenton-chemistry-based detemplation combined with secondary treatments offers options to tune the hierarchical porosity of SBA-15. This approach has been studied on a series of SBA-15 mesophases and has been compared to the conventional calcination. The as-synthesized and detemplated materials were

  11. Selective Preparation of Furfural from Xylose over Sulfonic Acid Functionalized Mesoporous Sba-15 Materials

    Directory of Open Access Journals (Sweden)

    Panpan Li

    2011-04-01

    Full Text Available Sulfonic acid functionalized mesoporous SBA-15 materials were prepared using the co-condensation and grafting methods, respectively, and their catalytic performance in the dehydration of xylose to furfural was examined. SBA-15-SO3H(C prepared by the co-condensation method showed 92–95% xylose conversion and 74% furfural selectivity, and 68–70% furfural yield under the given reaction conditions. The deactivation and regeneration of the SBA-15-SO3H(C catalyst for the dehydration of xylose was also investigated. The results indicate that the used and regeneration catalysts retained the SBA-15 mesoporous structure, and the S content of SBA-15-SO3H(C almost did not change. The deactivation of the catalysts is proposed to be associated with the accumulation of byproducts, which is caused by the loss reaction of furfural. After regeneration by H2O2, the catalytic activity of the catalyst almost recovered.

  12. Fabrication of superhydrophobic cotton fabrics by silica hydrosol and hydrophobization

    Science.gov (United States)

    Xu, Lihui; Zhuang, Wei; Xu, Bi; Cai, Zaisheng

    2011-04-01

    Superhydrophobic cotton fabrics were prepared by the incorporation of silica nanoparticles and subsequent hydrophobization with hexadecyltrimethoxysilane (HDTMS). The silica nanoparticles were synthesized via sol-gel reaction with methyl trimethoxy silane (MTMS) as the precursor in the presence of the base catalyst and surfactant in aqueous solution. As for the resulting products, characterization by particle size analyzer, scanning electron microscopy (SEM), scanning probe microscopy (SPM), X-ray photoelectron spectroscopy (XPS), and thermal gravimetric analysis (TGA) were performed respectively. The size of SiO2 nanoparticles can be controlled by adjusting the catalyst and surfactant concentrations. The wettability of cotton textiles was evaluated by the water contact angle (WCA) and water shedding angle (WSA) measurements. The results showed that the treated cotton sample displayed remarkable water repellency with a WCA of 151.9° for a 5 μL water droplet and a WSA of 13° for a 15 μL water droplet.

  13. Fabrication of keratin-silica hydrogel for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Kakkar, Prachi; Madhan, Balaraman, E-mail: bmadhan76@yahoo.co.in

    2016-09-01

    In the recent past, keratin has been fabricated into different forms of biomaterials like scaffold, gel, sponge, film etc. In lieu of the myriad advantages of the hydrogels for biomedical applications, a keratin-silica hydrogel was fabricated using tetraethyl orthosilicate (TEOS). Textural analysis shed light on the physical properties of the fabricated hydrogel, inturn enabling the optimization of the hydrogel. The optimized keratin-silica hydrogel was found to exhibit instant springiness, optimum hardness, with ease of spreadability. Moreover, the hydrogel showed excellent swelling with highly porous microarchitecture. MTT assay and DAPI staining revealed that keratin-silica hydrogel was biocompatible with fibroblast cells. Collectively, these properties make the fabricated keratin-silica hydrogel, a suitable dressing material for biomedical applications. - Highlights: • Keratin-silica hydrogel has been fabricated using sol–gel technique. • The hydrogel shows appropriate textural properties. • The hydrogel promotes fibroblast cells proliferation. • The hydrogel has potential soft tissue engineering applications like wound healing.

  14. Preparation and thermal properties of mesoporous silica/phenolic resin nanocomposites via in situ polymerization

    Directory of Open Access Journals (Sweden)

    J. Lv

    2012-10-01

    Full Text Available In order to enhance the adhesion between inorganic particles and polymer matrix, in this paper, the mesoporous silica SBA-15 material was synthesized by the sol-gel method. The surface of SBA-15 was modified using γ-glycidyloxypropyltrimethoxysilane (GOTMS as a coupling agent, and then mesoporous silica/phenolic resin (SBA-15/PF nanocomposites were prepared via in situ polymerization. The structural parameters and physical properties of SBA-15, SBA-15-GOTMS (SBA-15 surface treated using GOTMS as coupling agents and E-SBA-15/PF (SBA-15/PF nanocomposites extracted using ethanol as solvent were characterized by X-ray diffraction (XRD, N2 adsorption-desorption, Fourier transform infrared spectroscopy (FTIR, scanning electron microscopy (SEM, transmission electron microscopy (TEM and thermogravimetric analysis (TGA. The thermal properties of the nanocomposites were studied by differential scanning calorimetry (DSC and thermogravimetric analysis (TGA. The results demonstrated that the GOTMS were successfully grafted onto the surface of SBA-15, and chemical bonds between PF and SBA-15-GOTMS were formed after in situ polymerization. In addition, it is found that the in situ polymerization method has great effects on the textural parameters of SBA-15. The results also showed that the glass transition temperatures and thermal stability of the PF nanocomposites were obviously enhanced as compared with the pure PF at silica contents between 1–3 wt%, due to the uniform dispersion of the modified SBA-15 in the matrix.

  15. Efficient epoxidation over cyanocobalamine containing SBA-15 organic-inorganic nanohybrids

    Energy Technology Data Exchange (ETDEWEB)

    Karimi, Z. [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Mahjoub, A.R., E-mail: mahjouba@modares.ac.ir [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

    2010-05-01

    SBA-15 mesoporous silica is synthesized using triblock copolymer P123 surfactant and chemically modified by aminopropyl, thiol, ammonium and sulfonic acid functional groups. Functionalization is performed via post synthesize method using 3-aminopropyltriethoxysilane (APTES) or 3-mercatopropyl trimethoxysilane (MPTMS) precursor. The as synthesized mesoporous systems are applied for immobilization of cyanocobalamine. Functionalization effectively improves sorption properties of the supports, while different functional groups exert different effects. The organic-inorganic mesoporous materials are characterized via X-ray diffraction (XRD), nitrogen adsorption and desorption, transmission electron microscopy (TEM), FT-IR and inductively coupled plasma-optical emission (ICP). The newly synthesized systems exhibit high catalytic activity for heterogeneous epoxidation of cyclooctene in presence of hydrogen peroxide. Reaction conditions are optimized, effect of functional groups on performance of the catalysts is taken into consideration and reusability of the designed heterogeneous systems is studied. Systems with chemically modified supports are shown to be more efficient and stable catalysts however; chemical nature of functional groups plays a crucial role.

  16. An efficient hybrid, nanostructured, epoxidation catalyst: titanium silsesquioxane-polystyrene copolymer supported on SBA-15.

    Science.gov (United States)

    Zhang, Lei; Abbenhuis, Hendrikus C L; Gerritsen, Gijsbert; Bhriain, Nollaig Ní; Magusin, Pieter C M M; Mezari, Brahim; Han, Wei; van Santen, Rutger A; Yang, Qihua; Li, Can

    2007-01-01

    A novel interfacial hybrid epoxidation catalyst was designed with a new immobilization method for homogeneous catalysts by coating an inorganic support with an organic polymer film containing active sites. The titanium silsesquioxane (TiPOSS) complex, which contains a single-site titanium active center, was immobilized successfully by in-situ copolymerization on a mesoporous SBA-15-supported polystyrene polymer. The resulting hybrid materials exhibit attractive textural properties (highly ordered mesostructure, large specific surface area (>380 m2 g-1) and pore volume (>or==0.46 cm3 g-1)), and high activity in the epoxidation of alkenes. In the epoxidation of cyclooctene with tert-butyl hydrogen peroxide (TBHP), the hybrid catalysts have rate constants comparable with that of their homogeneous counterpart, and can be recycled at least seven times. They can also catalyze the epoxidation of cyclooctene with aqueous H2O2 as the oxidant. In two-phase reaction media, the catalysts show much higher activity than their homogeneous counterpart due to the hydrophobic environment around the active centers. They behave as interfacial catalysts due to their multifunctionality, that is, the hydrophobicity of polystyrene and the polyhedral oligomeric silsesquioxanes (POSS), and the hydrophilicity of the silica and the mesoporous structure. Combination of the immobilization of homogeneous catalysts on two conventional supports, inorganic solid and organic polymer, is demonstrated to achieve novel heterogeneous catalytic ensembles with the merits of attractive textural properties, tunable surface properties, and optimized environments around the active sites.

  17. Interactions of NO{sub 2} at ambient temperature with cerium-zirconium mixed oxides supported on SBA-15

    Energy Technology Data Exchange (ETDEWEB)

    Levasseur, Benoit; Ebrahim, Amani M. [The City College of New York and The Graduate School of CUNY 160 Convent Ave, New York, NY 10031 (United States); Burress, Jacob [NIST Center for Neutron Research, National Institute of Standards and Technology 100 Bureau Drive, Gaithersburg, MD 20899 (United States); Bandosz, Teresa J., E-mail: tbandosz@ccny.cuny.edu [The City College of New York and The Graduate School of CUNY 160 Convent Ave, New York, NY 10031 (United States)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer Ce{sub 1-y}Zr{sub y}O{sub 2-x} mixed oxides were highly dispersed in mesoporous silica SBA-15. Black-Right-Pointing-Pointer A strong increase in the NO{sub 2} adsorption capacity was observed on composites. Black-Right-Pointing-Pointer The insertion of Zr{sup 4+} in ceria fluorite structure promotes the reduction of Ce{sup 4+} into Ce{sup 3+}. Black-Right-Pointing-Pointer Ce{sup 3+} and -OH groups were found to be the main active centers for NO{sub x} retention. Black-Right-Pointing-Pointer The structure remains quite stable after exposure to NO{sub 2} in ambient conditions. - Abstract: New silica-based composites were obtained using a slow precipitation of mixed oxide Ce{sub 1-x}Zr{sub x}O{sub 2} on the surface of mesoporous silica, SBA-15. The samples were tested as NO{sub 2} adsorbents in dynamic conditions at room temperature. The surface of the initial and exhausted materials was characterized using N{sub 2} sorption, XRD, TEM, potentiometric titration, and thermal analysis before and after exposure to NO{sub 2}. In comparison with unsupported Ce{sub 1-x}Zr{sub x}O{sub 2} mixed oxides, a significant increase in the NO{sub 2} adsorption capacity was observed. This is due to the high dispersion of active oxide phase on the surface of SBA-15. A linear trend was found between the NO{sub 2} adsorption capacity and the amount of Zr(OH){sub 4} added to the structure. Introduction of Zr{sup 4+} cations to ceria contributes to an increase in the amount of Ce{sup 3+}, which is the active center for the NO{sub 2} adsorption, and to an increase in the density of -OH groups. These groups are found to be involved in the retention of both NO{sub 2} and NO on the surface. After exposure to NO{sub 2}, an acidification of the surface caused by the oxidation of the cerium as well as the formation of nitrite and nitrates took place. The structure of the composites appears not to be affected by reactive adsorption of NO{sub 2}.

  18. Grafted chromium 13-membered dioxo-macrocyclic complex into aminopropyl-based nanoporous SBA-15

    Energy Technology Data Exchange (ETDEWEB)

    Tarlani, Aliakbar, E-mail: Tarlani@ccerci.ac.ir [Inorganic Nanostructures and Catalysts Research Laboratory, Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Boulevard, km 17, Karaj Highway, Tehran 14968-13151 (Iran, Islamic Republic of); Joharian, Monika; Narimani, Khashayar [Inorganic Nanostructures and Catalysts Research Laboratory, Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Boulevard, km 17, Karaj Highway, Tehran 14968-13151 (Iran, Islamic Republic of); Muzart, Jacques [Institut de Chimie Moléculaire de Reims, CNRS-Université de Reims Champagne-Ardenne, BP 1039, 51687 Reims Cedex 2 (France); Fallah, Mahtab [Inorganic Nanostructures and Catalysts Research Laboratory, Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Boulevard, km 17, Karaj Highway, Tehran 14968-13151 (Iran, Islamic Republic of)

    2013-07-15

    In a new approach, chromium (III) tetraaza dioxo ligand was grafted onto functionalized SBA-15 after four step reactions by using coordinating ability of anchored amino functionalized SBA-15. After the termination of each step, the obtained product was characterized by FT-IR, low-angle X-ray diffraction (LA-XRD), N{sub 2} adsorption–desorption isotherms (Brunauer–Emmett–Teller (BET)–Barret–Joyner–Halenda (BJH)) and thermogravimetric analysis (TGA), and used as catalyst for the efficient and regioselective alcoholysis of styrene oxide to 2-alkoxy-1-phenylethanol product at ambient temperature. - Graphical abstract: Chromium (III) tetraaza dioxo ligand was grafted onto functionalized SBA-15 using coordinating ability of anchored amino functionalized SBA-15. Preparation of the catalyst is depicted in Scheme 1. - Highlights: • Dioxo tetraazachromium macrocyclic complex grafted into the SBA-15-NH{sub 2} channels. • The bond is created by coordinating ability of anchored amino functionalized SBA-15. • The prepared nanocatalyst has superior activity in the alcoholysis of styrene oxide. • The catalyst is reusable at ambient temperature for the mentioned reaction.

  19. Fischer-Tropsch synthesis in slurry-phase reactors using Co/SBA-15 catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Rodrigues, J.J.; Lima, L.A.; Lima, W.S.; Rodrigues, M.G.F. [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Engenharia Quimica], e-mail: meiry@deq.ufcg.edu.br; Fernandes, F.A.N. [Universidade Federal do Ceara (UFCE), CE (Brazil). Dept. de Engenharia Quimica

    2011-07-15

    The objective of this work is to describe the production of bifunctional catalysts using the incipient humidity method, producing catalysts with 15 wt.% cobalt supported in SBA-15 molecular sieve, to be applied in the Fischer-Tropsch (FT) reaction. The originality of this work is its focus on the use of a 15 wt.% Co/SBA-15 catalyst in FT synthesis in slurry reactors. The deposition of cobalt over SBA-15 support was accomplished by impregnation with a 0.1-M aqueous solution of cobalt nitrate. The Fischer-Tropsch synthesis was carried out with the catalyst at 240 deg C and 20 atm, under a COH{sub 2} atmosphere (molar ratio= 1), in a slurry reactor for 8 hours. X-ray diffraction measurements showed that the calcined cobalt catalyst did not modify the structure of SBA-15, proving that Co was present under the form of Co{sub 3}O{sub 4} in the catalyst. The addition of cobalt in the SBA-15 decreased the specific superficial area of the molecular sieve. The 15 wt.% Co/SBA-15 catalyst had a 40% CO conversion rate and a high selectivity towards the production of C{sub 5}{sup +} (53.9% after 8 hours). (author)

  20. VOx species supported on Al2O3-SBA-15 prepared by the grafting of alumina onto SBA-15: structure and activity in the oxidative dehydrogenation of ethane

    Czech Academy of Sciences Publication Activity Database

    Botková, Š.; Čapek, L.; Setnička, M.; Bulánek, R.; Čičmanec, P.; Kalužová, A.; Pastva, Jakub; Zukal, Arnošt

    2016-01-01

    Roč. 119, č. 1 (2016), s. 319-333 ISSN 1878-5190 R&D Projects: GA ČR GAP106/10/0196 Institutional support: RVO:61388955 Keywords : Ethane * UV-Vis * VOx species * Al2O3-SBA-15 Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.264, year: 2016

  1. Preparation and evaluation of aminopropyl-functionalized manganese-loaded SBA-15 for copper removal from aqueous solution.

    Science.gov (United States)

    Lei, Di; Zheng, Qianwen; Wang, Yili; Wang, Hongjie

    2015-02-01

    A novel material, aminopropyl-functionalized manganese-loaded SBA-15 (NH2-Mn-SBA-15), was synthesized by bonding 3-aminopropyl trimethoxysilane (APTMS) onto manganese-loaded SBA-15 (Mn-SBA-15) and used as a Cu2+ adsorbent in aqueous solution. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction spectra (XRD), N2 adsorption/desorption isotherms, high resolution field emission scanning electron microscopy (FESEM) and X-ray photoelectron spectroscopy (XPS) were used to characterize the NH2-Mn-SBA-15. The ordered mesoporous structure of SBA-15 was remained after modification. The manganese oxides were mainly loaded on the internal surface of the pore channels while the aminopropyl groups were mainly anchored on the external surface of SBA-15. The adsorption of Cu2+ on NH2-Mn-SBA-15 was fitted well by the Langmuir equation and the maximum adsorption capacity of NH2-Mn-SBA-15 for Cu2+ was over two times higher than that of Mn-SBA-15 under the same conditions. The Elovich equation gave a good fit for the adsorption process of Cu2+ by NH2-Mn-SBA-15 and Mn-SBA-15. Both the loaded manganese oxides and the anchored aminopropyl groups were found to contribute to the uptake of Cu2+. The NH2-Mn-SBA-15 showed high selectivity for copper ions. Consecutive adsorption-desorption experiments showed that the NH2-Mn-SBA-15 could be regenerated by acid treatment without altering its properties. Copyright © 2014. Published by Elsevier B.V.

  2. Intermediate-range order in mesoporous silicas investigated by a high-energy X-ray diffraction technique

    International Nuclear Information System (INIS)

    Wakihara, Toru; Fan, Wei; Ogura, Masaru; Okubo, Tatsuya; Kohara, Shinji; Sankar, Gopinathan

    2008-01-01

    We perform a high-energy X-ray diffraction study comparing bulk amorphous silica with MCM-41 and SBA-15 that are representative mesoporous silicas prepared in basic and acidic conditions, respectively. It is revealed that mesoporous silicas, especially SBA-15, have less ordered structures and contain larger fractions of three- and four-membered rings than does bulk amorphous silica. (author)

  3. Iron oxide inside SBA-15 modified with amino groups as reusable adsorbent for highly efficient removal of glyphosate from water

    Science.gov (United States)

    Fiorilli, Sonia; Rivoira, Luca; Calì, Giada; Appendini, Marta; Bruzzoniti, Maria Concetta; Coïsson, Marco; Onida, Barbara

    2017-07-01

    Iron oxide clusters were incorporated into amino-functionalized SBA-15 in order to obtain a magnetically recoverable adsorbent. The physical-chemical properties of the material were characterized by FE-SEM, STEM, XRD, TGA, XPS, FT-IR and acid-base titration analysis. Iron oxide nanoparticles were uniformly dispersed into the pore of mesoporous silica and that the adsorbent is characterized high specific surface area (177 m2/g) and accessible porosity. The sorbent was successfully tested for the removal of glyphosate in real water matrices. Despite the significant content of inorganic ions, a quantitative removal of the contaminant was found. The complete regeneration of the sorbent after the adsorption process through diluted NaOH solution was also proved.

  4. Silicon oxynitrides of KCC-1, SBA-15 and MCM-41 for CO 2 capture with excellent stability and regenerability

    KAUST Repository

    Patil, Umesh

    2012-01-01

    We report the use of silicon oxynitrides as novel adsorbents for CO 2 capture. Three series of functionalized materials based on KCC-1, SBA-15 and MCM-41 with Si-NH 2 groups were prepared using a simple one-step process via thermal ammonolysis using ammonia gas, and they demonstrated excellent CO 2 capture capabilities. These materials overcome several limitations of conventional amine-grafted mesoporous silica. They offer good CO 2 capture capacity, faster adsorption-desorption kinetics, efficient regeneration and reuse, more crucially excellent thermal and mechanical stability even in oxidative environments, and a clean and green synthesis route, which allows the overall CO 2 capture process to be practical and sustainable. This journal is © The Royal Society of Chemistry 2012.

  5. Comparison of the Acidity of Heteropolyacids Encapsulated in or Impregnated on SBA-15

    Directory of Open Access Journals (Sweden)

    Pinto Teresa

    2016-03-01

    Full Text Available Heteropolyacids (HPA immobilized onto SBA-15 silica were prepared by two different ways using either impregnation or encapsulation methodologies. Two Keggin-type HPA, H3PW12O40 and H4SiW12O40 were considered in this study. The resulting hybrid materials were fully characterized by N2 adsorption-desorption isotherms, XRD, FT-IR, Raman, diffuse reflectance UV-Vis spectroscopies and 31P MAS NMR. All characterization methods showed that at room temperature the catalysts contained well-dispersed and intact Keggin units throughout the solid. The catalytic activity of these solids was investigated in the isomerization of n-hexane. The impregnated and encapsulated phosphotungstic catalysts performed similarly in catalysis showing that the amount of active sites was nearly the same in both catalysts. On the contrary, the tungstosilicic encapsulated material was completely inactive while its impregnated counterpart was even more active than the phosphotungstic derived catalysts. The acidity of the solids was measured by various methods: microcalorimetry of ammonia adsorption, ammonia desorption followed by Temperature Programmed Desorption (TPD and DRIFT/GC-MS and pyridine adsorption followed by infrared spectroscopy. Only pyridine adsorption and ammonia desorption followed by DRIFT/GC-MS agreed with the catalytic data. Ammonia adsorption followed by microcalorimetry was not able to differentiate between the four catalysts while the TPD experiments led to unreliable results, as not only the evolved ammonia but also other molecules such as water were taken into account in the measurements. The behavior difference between the encapsulated silico- and phosphotungstic acids was explained by a more pronounced encapsulation in the case of silicon.

  6. Silylated Co/SBA-15 catalysts for Fischer-Tropsch synthesis

    International Nuclear Information System (INIS)

    Jia Lihong; Jia Litao; Li Debao; Hou Bo; Wang Jungang; Sun Yuhan

    2011-01-01

    A series of silylated Co/SBA-15 catalysts were prepared via the reaction of surface Si-OH of SBA-15 with hexamethyldisilazane (HMDS) under anhydrous, vapor-phase conditions, and then characterized by FT-IR, N 2 physisorption, TG, XRD, and TPR-MS. The results showed that organic modification led to a silylated SBA-15 surface composed of stable hydrophobic Si-(CH 3 ) 3 species even after calcinations and H 2 reduction at 673 K. Furthermore, the hydrophobic surface strongly influenced both metal dispersion and reducibility. Compared with non-silylated Co/SBA, Co/S-SBA (impregnation after silylation) showed a high activity, due to the better cobalt reducibility on the hydrophobic support. However, S-Co/SBA (silylation after impregnation) had the lowest FT activity among all the catalysts, due to the lower cobalt reducibility along with the steric hindrance of grafted -Si(CH 3 ) 3 for the re-adsorption of α-olefins. -- Graphical abstract: The silylation of an SBA-15 before cobalt impregnation enhanced the reducibility of cobalt oxides on an SBA-15-supported cobalt catalyst and consequently increased the catalytic activity for Fischer-Tropsch synthesis. Display Omitted

  7. The synthesis of novel hybrid thiol-functionalized nano-structured SBA-15

    International Nuclear Information System (INIS)

    Hoang, Van Duc; Dang, Tuyet Phuong; Dinh, Quang Khieu; Vu, Anh Tuan; Nguyen, Huu Phu

    2010-01-01

    Mesoporous thiol-functionalized SBA-15 has been directly synthesized by co-condensation of tetraethyl orthosilicate (TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) with triblock copolymer P123 as-structure-directing agent under hydrothermal conditions. Surfactant removal was performed by Soxhlet ethanol extraction. These materials have been characterized by powder x-ray diffraction (XRD), nitrogen adsorption/desorption (BET model), transmission electron microscopy (TEM), thermal analysis, infrared spectroscopy (IR) and energy-dispersive x-ray spectroscopy (EDX). The main parameters, such as the initial molar ratio of MPTMS to TEOS, the time of adding MPTMS to synthesized gel and the Soxhlet ethanol extraction on the thiol functionalized SBA-15 with high thiol content and highly ordered hexagonal mesostructure, were investigated and evaluated. The adsorption capacity of the thiol-functionalized and non-functionalized SBA-15 materials for Pb 2+ ion from aqueous solution was tested. It was found that the Pb 2+ adsorption capacity of the thiol functionalized SBA-15 is three times higher than that of non-functionalized SBA-15

  8. The Effect of Nitrogen Surface Ligands on Propane Metathesis: Design and Characterizations of N-modified SBA15-Supported Schrock-type Tungsten Alkylidyne

    KAUST Repository

    Eid, Ahmed A.

    2014-04-01

    Catalysis, which is primarily a molecular phenomenon, is an important field of chemistry because it requires the chemical conversion of molecules into other molecules. It also has an effect on many fields, including, but not limited to, industry, environment and life Science[1]. Surface Organometallic Chemistry is an effective methodology for Catalysis as it imports the concept and mechanism of organometallic chemistry, to surface science and heterogeneous catalysis. So, it bridges the gap between homogenous and heterogeneous catalysis[1]. The aim of the present research work is to study the effect of Nitrogen surface ligands on the activity of Alkane, Propane in particular, metathesis. Our approach is based on the preparation of selectively well-defined group (VI) transition metal complexes supported onto mesoporous materials, SBA15 and bearing amido and/or imido ligands. We choose nitrogen ligands because, according to the literature, they showed in some cases better catalytic properties in homogenous catalysis in comparison with their oxygen counterparts[2]. The first section covers the modification of a highly dehydroxylated SBA15 surface using a controlled ammonia treatment. These will result in the preparation of two kind of Nitrogen surface ligands: -\\tOne with vicinal silylamine/silanol, (≡SiNH2)(≡SiOH), noted [N,O]SBA15 and, -\\tAnother\\tone\\twith\\tvicinal\\tbis-silylamine moieties (≡SiNH2)2, noted [N,N]SBA15[3]. The second section covers the reaction of Schrock type Tungsten Carbyne [W(≡C- tBu)(CH2-tBu)3] with those N-surface ligands and their characterizations by FT-IR, multiple quantum solid state NMR (1H, 13C), elemental analysis and gas phase analysis. The third section covers the generation of the active site, tungsten hydride species. Their performance toward propane metathesis reaction using the dynamic reactor technique PID compared toward previous well-known catalysts supported on silica oxide or mesoporous materials[4]. A fairly good

  9. High surface area TiO2/SBA-15 nanocomposites: Synthesis, microstructure and adsorption-enhanced photocatalysis

    Science.gov (United States)

    Wei, J. Q.; Chen, X. J.; Wang, P. F.; Han, Y. B.; Xu, J. C.; Hong, B.; Jin, H. X.; Jin, D. F.; Peng, X. L.; Li, J.; Yang, Y. T.; Ge, H. L.; Wang, X. Q.

    2018-06-01

    Mesoporous SBA-15 was used to anchor TiO2 nanoparticles into the mesopores to form high surface area TiO2/SBA-15 nanocomposites, and then the influence of mesoporous-structure on the photocatalytic performance was investigated. TiO2/SBA-15 nanocomposites possessed the high specific surface area and appropriate pore size, indicating the excellent adsorption performance. TiO2/SBA-15 nanocomposites exhibited the higher photocatalytic activity to degrade dyes (methylene blue: MB) than TiO2 (removing SBA-15), which should attributed to the excellent adsorption performance of the nanocomposites. MB was absorbed to form the higher concentration near TiO2/SBA-15 photocatalysts, and the photocatalytic degradation for MB was improved.

  10. Evidence for metalsupport interactions in Au modified TiO_{x}/SBA-15 materials prepared by photodeposition

    OpenAIRE

    Mei, Bastian; Wiktor, Christian; Turner, Stuart; Pougin, Anna; Tendeloo, Van, Gustaaf; Fischer, Roland A.; Muhler, Martin; Strunk, Jennifer

    2013-01-01

    Abstract: Gold nanoparticles have been efficiently photodeposited onto titanate-loaded SBA-15 (Ti(x)/SBA-15) with different titania coordination. Transmission electron microscopy shows that relatively large Au nanoparticles are photodeposited on the outer surface of the Ti(x)/SBA-15 materials and that TiOx tends to form agglomerates in close proximity to the Au nanoparticles, often forming coreshell Au/TiOx structures. This behavior resembles typical processes observed due to strong-metal sup...

  11. Dehydrogenation of Isobutane with Carbon Dioxide over SBA-15-Supported Vanadium Oxide Catalysts

    Directory of Open Access Journals (Sweden)

    Chunling Wei

    2016-10-01

    Full Text Available A series of vanadia catalysts supported on SBA-15 (V/SBA with a vanadia (V content ranging from 1% to 11% were prepared by an incipient wetness method. Their catalytic behavior in the dehydrogenation of isobutane to isobutene with CO2 was examined. The catalysts were characterized by N2 adsorption, X-ray diffraction (XRD, scanning electron microscopy (SEM, Raman spectroscopy, and temperature-programmed reduction (TPR. It was found that these catalysts were effective for the dehydrogenation reaction, and the catalytic activity is correlated with the amount of dispersed vanadium species on the SBA-15 support. The 7% V/SBA catalyst shows the highest activity, which gives 40.8% isobutane conversion and 84.8% isobutene selectivity. The SBA-15-supported vanadia exhibits higher isobutane conversion and isobutene selectivity than the MCM-41-supported one.

  12. Single-site SBA-15 supported zirconium catalysts. Synthesis, characterization and toward cyanosilylation reaction

    International Nuclear Information System (INIS)

    Xu, Wei; Yu, Bo; Zhang, Ying; Chen, Xi; Zhang, Guofang; Gao, Ziwei

    2015-01-01

    Graphical abstract: Ligand-modified signal-site SBA-15 supported zirconium catalysts were synthesized by SOMC method and characterized by a variety of techniques. The zirconium surface complexes show high catalytic efficiency for cyanosilylation of benzaldehyde. - Highlights: • Some Zr active species have been anchored on the surface of SBA-15 by SOMC technique. • The structures of the Zr species have been characterized by a variety of techniques. • The anchored Zr species are single-sited surface complexes. • The Zr surface complexes are catalytic active for cyanosilylation of benzaldehyde. - Abstract: A successive anchoring of Zr(NMe 2 ) 4 , cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on dehydroxylated SBA-15 pretreated at 500 °C for 16 h (SBA-15 -500 ) was conducted by SOMC strategy in moderate conditions. The dehydoxylation of SBA-15 was monitored by in situ Fourier transform infrared spectroscopy (in situ FT-IR). The ligand-modified SBA-15 -500 supported zirconium complexes were characterized by in situ FT-IR, 13 C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP-MAS) and elemental analysis in detail, verifying that the surface zirconium species are single-sited. The catalytic activity of these complexes was evaluated by cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the structure of surface species and the configuration of the ligands

  13. Single-site SBA-15 supported zirconium catalysts. Synthesis, characterization and toward cyanosilylation reaction

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Wei; Yu, Bo; Zhang, Ying; Chen, Xi; Zhang, Guofang, E-mail: gfzhang@snnu.edu.cn; Gao, Ziwei, E-mail: zwgao@snnu.edu.cn

    2015-01-15

    Graphical abstract: Ligand-modified signal-site SBA-15 supported zirconium catalysts were synthesized by SOMC method and characterized by a variety of techniques. The zirconium surface complexes show high catalytic efficiency for cyanosilylation of benzaldehyde. - Highlights: • Some Zr active species have been anchored on the surface of SBA-15 by SOMC technique. • The structures of the Zr species have been characterized by a variety of techniques. • The anchored Zr species are single-sited surface complexes. • The Zr surface complexes are catalytic active for cyanosilylation of benzaldehyde. - Abstract: A successive anchoring of Zr(NMe{sub 2}){sub 4}, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on dehydroxylated SBA-15 pretreated at 500 °C for 16 h (SBA-15{sub -500}) was conducted by SOMC strategy in moderate conditions. The dehydoxylation of SBA-15 was monitored by in situ Fourier transform infrared spectroscopy (in situ FT-IR). The ligand-modified SBA-15{sub -500} supported zirconium complexes were characterized by in situ FT-IR, {sup 13}C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP-MAS) and elemental analysis in detail, verifying that the surface zirconium species are single-sited. The catalytic activity of these complexes was evaluated by cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the structure of surface species and the configuration of the ligands.

  14. Surface functionalization of SBA-15 by the solvent-free method

    International Nuclear Information System (INIS)

    Wang Yimeng; Zheng Yingwu; Zhu Jianhua

    2004-01-01

    A solvent-free technique was employed for fast modification of mesoporous materials. Copper, chromium and iron oxide species could be highly dispersed in SBA-15 by manually grinding the corresponding precursor salts and the host, followed by calcinations for the first time. This method is more effective to spontaneously disperse oxide species onto SBA-15 than impregnation, probably forming monolayer or submonolayer dispersion of salts or oxides. Besides, Cr(VI) species dominate in the mixing sample while Cr(III) species dominate in the impregnation one. In the temperature programmed surface reaction of nitrosamines, the sample prepared by solvent-free method showed a higher catalytic activity than the impregnation one

  15. Fabrication and optical characterization of gold-infiltrated silica opals

    International Nuclear Information System (INIS)

    Li Wenjiang; Sun Gang; Tang Fangqiong; Tam, W.Y.; Li Jensen; Chan, C T; Sheng Ping

    2005-01-01

    We report the fabrication of metal-infiltrated silica opals for optical studies. Highly mono-dispersed silica microspheres are fabricated and assembled by a force packing method to form opals with large domain sizes. The opals are then infiltrated with gold by an electroplating technique. The optical properties of the infiltrated opals in the visible range are studied and model calculations based on a multiple-scattering formalism are used to interpret the experimental results. The calculated position of the directional gap of the silica opal agrees very well with experimental observation. We found that the optical properties of the infiltrated sample can be explained using a model system in which the voids in the silica opal are partially filled with Au and the surface of the slab is covered with a thin layer of Au

  16. Mechanism for enhanced degradation of clofibric acid in aqueous by catalytic ozonation over MnOx/SBA-15

    International Nuclear Information System (INIS)

    Sun, Qiangqiang; Wang, Yu; Li, Laisheng; Bing, Jishuai; Wang, Yingxin; Yan, Huihua

    2015-01-01

    Highlights: • Clofibric acid (CA) is efficiently mineralized by O 3 /MnO x /SBA-15. • Adsorption of CA and its intermediates on MnO x /SBA-15 is proved unimportant. • Initiation of hydroxyl radicals (·OH) is enhanced in O 3 /MnO x /SBA-15. • Uniformly distributed MnO x accounts for the high activity of MnO x /SBA-15. • Degradation routes of CA in ozonation alone and catalytic ozonation are proposed. - Abstract: Comparative experiments were conducted to investigate the catalytic ability of MnO x /SBA-15 for the ozonation of clofibric acid (CA) and its reaction mechanism. Compared with ozonation alone, the degradation of CA was barely enhanced, while the removal of TOC was significantly improved by catalytic ozonation (O 3 /MnO x /SBA-15). Adsorption of CA and its intermediates by MnO x /SBA-15 was proved unimportant in O 3 /MnO x /SBA-15 due to the insignificant adsorption of CA and little TOC variation after ceasing ozone in stopped-flow experiment. The more remarkably inhibition effect of sodium bisulfite (NaHSO 3 ) on the removal of TOC in catalytic ozonation than in ozonation alone elucidated that MnO x /SBA-15 facilitated the generation of hydroxyl radicals (·OH), which was further verified by electron spin-resonance spectroscopy (ESR). Highly dispersed MnO x on SBA-15 were believed to be the main active component in MnO x /SBA-15. Some intermediates were indentified and different degradation routes of CA were proposed in both ozonation alone and catalytic ozonation. The amounts of small molecular carboxylic acids (i.e., formic acid (FA), acetic acid (AA) and oxalic acid (OA)) generated in catalytic ozonation were lower than in ozonation alone, resulting from the generation of more ·OH

  17. Controlled drug release from bifunctionalized mesoporous silica

    Science.gov (United States)

    Xu, Wujun; Gao, Qiang; Xu, Yao; Wu, Dong; Sun, Yuhan; Shen, Wanling; Deng, Feng

    2008-10-01

    Serial of trimethylsilyl-carboxyl bifunctionalized SBA-15 (TMS/COOH/SBA-15) have been studied as carriers for controlled release of drug famotidine (Famo). To load Famo with large capacity, SBA-15 with high content of carboxyl groups was successfully synthesized by one-pot synthesis under the assistance of KCl. The mesostructure of carboxyl functionalized SBA-15 (COOH/SBA-15) could still be kept even though the content of carboxyl groups was up to 57.2%. Increasing carboxyl content could effectively enhance the loading capacity of Famo. Compared with pure SBA-15, into which Famo could be hardly adsorbed, the largest drug loading capacity of COOH/SBA-15 could achieve 396.9 mg/g. The release of Famo from mesoporous silica was studied in simulated intestine fluid (SIF, pH=7.4). For COOH/SBA-15, the release rate of Famo decreased with narrowing pore size. After grafting TMS groups on the surface of COOH/SBA-15 with hexamethyldisilazane, the release of Famo was greatly delayed with the increasing content of TMS groups.

  18. Substantially Stabilized Superacid Incorporated SBA-15 with Calcium Bridging for Selective Esterification of Glycerol

    Science.gov (United States)

    Hoo, P. Y.; Abdullah, A. Z.; Shuit, S. H.; Teoh, Y. P.; Ng, Q. H.; Kunasundari, B.

    2018-03-01

    The exploitation of the super acidity of heteropolyacids incorporated heterogeneous catalysts was only feasible if the heterogeneity of these catalysts was assured. To maintain the catalyst heterogeneity in polar medium, a novel two-step modification method was proposed to synthesize the highly active, yet stable heterogeneous catalyst, catered for selective esterification of monoglyceride. The surficial, structural and acidity properties of the modified catalysts were investigated via crucial characterization methods (N2 BET, HRTEM, and FTIR). The collective evidences verified the predicted formation of calcium oxides (CaO) on the mesopores surfaces of the SBA-15 support after the first modification, and the successful subsequent 12-tungstophosphoric acid (HPW) functionalization. The superior stability of the synthesized catalysts (10wt%-HPW/CaSBA-15) was demonstrated (negligible change in both conversion – 75% and yield – 70%), without the need for catalyst regeneration. Such result was attributed to the strong interaction between HPW and SBA-15 via calcium bridging. Being alkaline in nature, calcium oxides in the inner pores readily reacted with highly acidic HPW introduced in the subsequent wetness incipient step, forming insoluble HPW acid sites on inner pore walls of SBA-15 via the calcium bridging. This modification deemed promising and other alkaline metals should be explored in the future.

  19. Photocatalytic activity of Ce-modified SBA-15 for the degradation of ...

    Indian Academy of Sciences (India)

    transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and N2 adsorption/desorption analysis. ... water.7,8,18 Existence of different sites of cerium ions and ... hydrocarbons.21 In this study, Ce-SBA-15 and Ce-Al-SBA-.

  20. Single-site SBA-15 supported zirconium catalysts. Synthesis, characterization and toward cyanosilylation reaction

    Science.gov (United States)

    Xu, Wei; Yu, Bo; Zhang, Ying; Chen, Xi; Zhang, Guofang; Gao, Ziwei

    2015-01-01

    A successive anchoring of Zr(NMe2)4, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1‧-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on dehydroxylated SBA-15 pretreated at 500 °C for 16 h (SBA-15-500) was conducted by SOMC strategy in moderate conditions. The dehydoxylation of SBA-15 was monitored by in situ Fourier transform infrared spectroscopy (in situ FT-IR). The ligand-modified SBA-15-500 supported zirconium complexes were characterized by in situ FT-IR, 13C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP-MAS) and elemental analysis in detail, verifying that the surface zirconium species are single-sited. The catalytic activity of these complexes was evaluated by cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the structure of surface species and the configuration of the ligands.

  1. Repeated sorption of water in SBA-15 investigated by means of in situ small-angle x-ray scattering

    International Nuclear Information System (INIS)

    Erko, M; Paris, O; Wallacher, D; Findenegg, G H

    2012-01-01

    The effect of repeated cycles of water adsorption/desorption on the structural stability of ordered mesoporous silica SBA-15 is studied by small-angle x-ray scattering (SAXS). In situ sorption measurements are conducted using a custom-built sorption apparatus in connection with a laboratory SAXS setup. Two striking irreversible changes are observed in the sorption isotherms as derived from the integrated SAXS intensity. First, the capillary condensation pressure shifts progressively to lower relative pressure values with increasing number of sorption cycles. This effect is attributed to chemisorption of water at the silica walls, resulting in a change of the fluid-wall interaction. Second, the sorption cycles do not close completely at vanishing vapour pressure, suggesting that progressively more water remains trapped within the porous material after each cycle. This effect is interpreted to be the result of an irreversible collapse of parts of mesopores, originating from pore wall deformation due to the large Laplace pressure of water acting on the pore walls at capillary condensation and capillary evaporation. (paper)

  2. Facile functionalized of SBA-15 via a biomimetic coating and its application in efficient removal of uranium ions from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Jun-Kai [School of Environmental Science and Engineering, Tianjin University, Tianjin 300072 (China); School of Energy and Environmental Engineering, Hebei University of Technology, Tianjin 300401 (China); Hou, Li-An; Zhang, Guang-Hui [School of Environmental Science and Engineering, Tianjin University, Tianjin 300072 (China); Gu, Ping, E-mail: guping@tju.edu.cn [School of Environmental Science and Engineering, Tianjin University, Tianjin 300072 (China)

    2015-04-09

    Highlights: • Dopamine-functionalized SBA-15 (DMS) was developed via a biomimetic coating. • The modification approach was simple, facile and cost-effective. • The DMS was firstly used to remove U(VI) from aqueous solution. • Large adsorption capacity and rapid separation were obtained. - Abstract: A novel dopamine-functionalized mesoporous silica (DMS), synthesized by grafting dopamine onto a mesoporous molecular sieve (SBA-15), was developed as a sorbent to extract U(VI) from aqueous solution. The method used to modify SBA-15 was simple, facile and cost-effective. The DMS was characterized by SEM, TEM, XRD and BET, showing that the material had an ordered mesoporous structure and a large surface area. The effect of contact time, pH, ionic strength, temperature, and solid–liquid ratio on the sorption process was investigated. It was demonstrated that the adsorption of U(VI) by DMS was fast and that it can be described by the pseudo-second order-equation where the equilibrium time was 20 min. Additionally, the adsorption isotherm data were fitted well by the Langmuir model with the maximum adsorption capacity of DMS of 196 mg/g at pH 6.0. Furthermore, the influence of the K{sup +} and Na{sup +} concentrations and solid-to-liquid ratio on the sorption was very weak, and the values of the thermodynamic parameters revealed that the sorption process was exothermic and spontaneous. All the results suggested that the DMS could be used as an excellent adsorbent to remove U(VI) from aqueous solution.

  3. Mechanism for enhanced degradation of clofibric acid in aqueous by catalytic ozonation over MnOx/SBA-15.

    Science.gov (United States)

    Sun, Qiangqiang; Wang, Yu; Li, Laisheng; Bing, Jishuai; Wang, Yingxin; Yan, Huihua

    2015-04-09

    Comparative experiments were conducted to investigate the catalytic ability of MnO(x)/SBA-15 for the ozonation of clofibric acid (CA) and its reaction mechanism. Compared with ozonation alone, the degradation of CA was barely enhanced, while the removal of TOC was significantly improved by catalytic ozonation (O3/MnO(x)/SBA-15). Adsorption of CA and its intermediates by MnO(x)/SBA-15 was proved unimportant in O3/MnO(x)/SBA-15 due to the insignificant adsorption of CA and little TOC variation after ceasing ozone in stopped-flow experiment. The more remarkably inhibition effect of sodium bisulfite (NaHSO3) on the removal of TOC in catalytic ozonation than in ozonation alone elucidated that MnO(x)/SBA-15 facilitated the generation of hydroxyl radicals (OH), which was further verified by electron spin-resonance spectroscopy (ESR). Highly dispersed MnO(x) on SBA-15 were believed to be the main active component in MnO(x)/SBA-15. Some intermediates were indentified and different degradation routes of CA were proposed in both ozonation alone and catalytic ozonation. The amounts of small molecular carboxylic acids (i.e., formic acid (FA), acetic acid (AA) and oxalic acid (OA)) generated in catalytic ozonation were lower than in ozonation alone, resulting from the generation of more OH. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Anchoring Tri(8-QuinolinolatoIron Onto Sba-15 for Partial Oxidation of Benzyl Alcohol Using Water as the Solvent

    Directory of Open Access Journals (Sweden)

    Yang Xiaoyuan

    2014-09-01

    Full Text Available Tri(8-quinolinolatoiron complex immobilized onto SBA-15 catalyst has been synthesized through a stepwise procedure. The characterization results indicated that the BET surface area, total pore volume and average pore width decrease after stepwise modification of SBA-15, while the structure keeps intact. Catalytic tests showed that FeQ3-SBA-15 catalyzes the oxidation reaction well with 34.8% conversion of benzyl alcohol and 74.7% selectivity to benzaldehyde when water is used as the solvent after 1 h reaction. In addition, homogeneous catalyst tri(8-quinolinolatoiron exhibits very bad catalytic behavior using water as the solvent.

  5. Efficient low-temperature soot combustion by bimetallic Ag-Cu/SBA-15 catalysts.

    Science.gov (United States)

    Wen, Zhaojun; Duan, Xinping; Hu, Menglin; Cao, Yanning; Ye, Linmin; Jiang, Lilong; Yuan, Youzhu

    2018-02-01

    In this study, the effects of copper (Cu) additive on the catalytic performance of Ag/SBA-15 in complete soot combustion were investigated. The soot combustion performance of bimetallic Ag-Cu/SBA-15 catalysts was higher than that of monometallic Ag and Cu catalysts. The optimum catalytic performance was acquired with the 5Ag 1 -Cu 0.1 /SBA-15 catalyst, on which the soot combustion starts at T ig =225°C with a T 50 =285°C. The temperature for 50% of soot combustion was lower than that of conventional Ag-based catalysts to more than 50°C (Aneggi et al., 2009). Physicochemical characterizations of the catalysts indicated that addition of Cu into Ag could form smaller bimetallic Ag-Cu nanolloy particles, downsizing the mean particle size from 3.7nm in monometallic catalyst to 2.6nm in bimetallic Ag-Cu catalyst. Further experiments revealed that Ag and Cu species elicited synergistic effects, subsequently increasing the content of surface active oxygen species. As a result, the structure modifications of Ag by the addition of Cu strongly intensified the catalytic performance. Copyright © 2017. Published by Elsevier B.V.

  6. SBA-15-functionalized 3-oxo-ABNO as recyclable catalyst for aerobic oxidation of alcohols under metal-free conditions.

    Science.gov (United States)

    Karimi, Babak; Farhangi, Elham; Vali, Hojatollah; Vahdati, Saleh

    2014-09-01

    The nitroxyl radical 3-oxo-9-azabicyclo [3.3.1]nonane-N-oxyl (3-oxo-ABNO) has been prepared using a simple protocol. This organocatalyst is found to be an efficient catalyst for the aerobic oxidation of a wide variety of alcohols under metal-free conditions. In addition, the preparation and characterization of a supported version of 3-oxo-ABNO on ordered mesoporous silica SBA-15 (SABNO) is described for the first time. The catalyst has been characterized using several techniques including simultaneous thermal analysis (STA), transmission electron microscopy (TEM), and nitrogen sorption analysis. This catalyst exhibits catalytic performance comparable to its homogeneous analogue and much superior catalytic activity in comparison with (2,2,6,6-tetramethylpiperidin-1-yl)oxy (TEMPO) for the aerobic oxidation of almost the same range of alcohols under identical reaction conditions. It is also found that SABNO can be conveniently recovered and reused at least 12 times without significant effect on its catalytic efficiency. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Tungsten(VI) Carbyne/Bis(carbene) Tautomerization Enabled by N-Donor SBA15 Surface Ligands: A Solid-State NMR and DFT Study

    KAUST Repository

    Bendjeriou-Sedjerari, Anissa

    2016-08-11

    Designing supported well-defined bis(carbene) complexes remains a key challenge in heterogeneous catalysis. The reaction of W(CtBu)(CH(2)tBu)(3) with amine-modified mesoporous SBA15 silica, which has vicinal silanol/silylamine pairs [(SiOH)(SiNH2)], leads to [(SiNH2-)(SiO-)W(CHtBu)(CH(2)tBu)(2)] and [(SiNH2-)(SiO-)W(=CHtBu)(2)(CH(2)tBu). Variable temperature, H-1-H-1 2D double-quantum, H-1-C-13 HETCOR, and HETCOR with spin diffusion solid-state NMR spectroscopy demonstrate tautomerization between the alkyl alkylidyne and the bis(alkylidene) on the SBA15 surface. Such equilibrium is possible through the coordination of W to the surface [(Si-OH)(Si-NH2)] groups, which act as a [N,O] pincer ligand. DFT calculations provide a rationalization for the surface-complex tautomerization and support the experimental results. This direct observation of such a process shows the strong similarity between molecular mechanisms in homogeneous and heterogeneous catalysis. In propane metathesis (at 150 degrees C), the tungsten bis(carbene) tautomer is favorable, with a turnover number (TON) of 262. It is the highest TON among all the tungsten alkyl-supported catalysts.

  8. Facile functionalized of SBA-15 via a biomimetic coating and its application in efficient removal of uranium ions from aqueous solution.

    Science.gov (United States)

    Gao, Jun-Kai; Hou, Li-An; Zhang, Guang-Hui; Gu, Ping

    2015-04-09

    A novel dopamine-functionalized mesoporous silica (DMS), synthesized by grafting dopamine onto a mesoporous molecular sieve (SBA-15), was developed as a sorbent to extract U(VI) from aqueous solution. The method used to modify SBA-15 was simple, facile and cost-effective. The DMS was characterized by SEM, TEM, XRD and BET, showing that the material had an ordered mesoporous structure and a large surface area. The effect of contact time, pH, ionic strength, temperature, and solid-liquid ratio on the sorption process was investigated. It was demonstrated that the adsorption of U(VI) by DMS was fast and that it can be described by the pseudo-second order-equation where the equilibrium time was 20 min. Additionally, the adsorption isotherm data were fitted well by the Langmuir model with the maximum adsorption capacity of DMS of 196 mg/g at pH 6.0. Furthermore, the influence of the K(+) and Na(+) concentrations and solid-to-liquid ratio on the sorption was very weak, and the values of the thermodynamic parameters revealed that the sorption process was exothermic and spontaneous. All the results suggested that the DMS could be used as an excellent adsorbent to remove U(VI) from aqueous solution. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Tungsten(VI) Carbyne/Bis(carbene) Tautomerization Enabled by N-Donor SBA15 Surface Ligands: A Solid-State NMR and DFT Study

    KAUST Repository

    Bendjeriou-Sedjerari, Anissa; Sofack-Kreutzer, Julien; Minenkov, Yury; Abou-Hamad, Edy; Hamzaoui, Bilel; Werghi, Baraa; Anjum, Dalaver H.; Cavallo, Luigi; Huang, Kuo-Wei; Basset, Jean-Marie

    2016-01-01

    Designing supported well-defined bis(carbene) complexes remains a key challenge in heterogeneous catalysis. The reaction of W(CtBu)(CH(2)tBu)(3) with amine-modified mesoporous SBA15 silica, which has vicinal silanol/silylamine pairs [(SiOH)(SiNH2)], leads to [(SiNH2-)(SiO-)W(CHtBu)(CH(2)tBu)(2)] and [(SiNH2-)(SiO-)W(=CHtBu)(2)(CH(2)tBu). Variable temperature, H-1-H-1 2D double-quantum, H-1-C-13 HETCOR, and HETCOR with spin diffusion solid-state NMR spectroscopy demonstrate tautomerization between the alkyl alkylidyne and the bis(alkylidene) on the SBA15 surface. Such equilibrium is possible through the coordination of W to the surface [(Si-OH)(Si-NH2)] groups, which act as a [N,O] pincer ligand. DFT calculations provide a rationalization for the surface-complex tautomerization and support the experimental results. This direct observation of such a process shows the strong similarity between molecular mechanisms in homogeneous and heterogeneous catalysis. In propane metathesis (at 150 degrees C), the tungsten bis(carbene) tautomer is favorable, with a turnover number (TON) of 262. It is the highest TON among all the tungsten alkyl-supported catalysts.

  10. Fabrication of superhydrophobic fluorinated silica nanoparticles for multifunctional liquid marbles

    Science.gov (United States)

    Shang, Qianqian; Hu, Lihong; Hu, Yun; Liu, Chengguo; Zhou, Yonghong

    2018-01-01

    A facile one-pot method for the fabrication of superhydrophobic fluorinated silica nanoparticles is reported. Fluorinated aggregated silica (A-SiO2/FAS) nanoparticles were synthesized by controlling the nanoparticles assembly, in situ fixation and overgrowth of particle seeds with the assist of tetraethoxysilane (TEOS) in ethanol/water solution and then modification with fluoroalkylsilane (FAS) molecules. Such kind of A-SiO2/FAS nanoparticles showed superhydrophobicity and was not wetted by water, thus it could be served as the encapsulating shells to manipulate liquid droplets. Liquid marbles fabricated from A-SiO2/FAS nanoparticles were used for ammonia gas sensing or emitting by taking advantage of the porosity and superhydrophobicity of the liquid marble shells. In addition, the posibility of A-SiO2/FAS-based liquid marbles as microreactor for dopamine polymerization also was explored.

  11. H2 formation by electron irradiation of SBA-15 materials and the effect of Cu(II) grafting

    International Nuclear Information System (INIS)

    Brodie-Linder, N.; Le Caer, S.; Shahdo Alam, M.; Renault, J.P.; Alba-Simionesco, Ch.

    2010-01-01

    Measurement of H 2 production from electron irradiation (10 MeV) on SBA-15 materials has shown that adsorbed water is attacked preferentially. Silanol groups are only attacked when they are in the majority with respect to adsorbed water, however they are much less efficient at producing H 2 . The comparison between water content before and after electron irradiation and the corresponding H 2 production indicates that water desorption is the main route to adsorbed water loss for SBA-15 materials. On the other hand, surface silanol groups are more susceptible to attack,leading to H 2 production when SBA-15 samples have undergone extensive thermal treatment. Electron irradiation of SBA-15-Cu materials has shown that the presence of Cu(II) on the surface reduces and inhibits the production of H 2 . This inhibiting power affects adsorbed water bonded to grafted copper but not surface silanol groups. (authors)

  12. An ultrasensitive sandwich-type electrochemical immunosensor based on the signal amplification system of double-deck gold film and thionine unite with platinum nanowire inlaid globular SBA-15 microsphere.

    Science.gov (United States)

    Wang, Ping; Li, Mingdang; Pei, Fubin; Li, Yueyun; Liu, Qing; Dong, Yunhui; Chu, Qingyan; Zhu, Hongjun

    2017-05-15

    A novel thionine unites with platinum nanowire inlaid globular SBA-15 (Pt NWs@g-SBA-15/Thi) not only utilizes as an efficient electrical signal probe but also constitutes an amplifying system with double-deck gold film (D-Au film) have been applied to the fabrication of sandwich-type immunosensor for detecting hepatitis B surface antigen (HBs Ag). The D-Au film can accelerate the electron transfer on the electrode interface due to the tunneling effect between the two Au films and can improve the load capacity of primary antibodies (Ab 1 ) because of the good biocompatibility. The Pt NWs@g-SBA-15/Thi with uniform globular morphology not only can effectively reduce the spatial limitation for loading the secondary antibodies (Ab 2 ) but also can provide outstanding pore accessibility of guest species from outside and offer catalytically active sites in a large scale. Besides, the presence of Thi can well enhance the electrical conductivity of Pt NWs@g-SBA-15/Thi. With the good cooperation between D-Au film and Pt NWs@g-SBA-15/Thi, a linear relationship between current signals and the concentrations of HBs Ag was obtained in the wide range from 10 fg/mL to 100ng/mL and the detection limit of HBs Ag was 3.3 fg/mL (signal-to-noise ratio of 3). Furthermore, the designed immunosensor with excellent selectivity, reproducibility and stability shows excellent performance in detection of human serum samples and provides a promising capacity for detecting a wide range of other tumor markers in clinical application. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Microstructure and Magnetic Properties of Highly Ordered SBA-15 Nanocomposites Modified with Fe2O3 and Co3O4 Nanoparticles

    Directory of Open Access Journals (Sweden)

    P. F. Wang

    2012-01-01

    Full Text Available Owing to the unique order mesopores, mesoporous SBA-15 could be used as the carrier of the magnetic nanoparticles. The magnetic nanoparticles in the frame and the mesopores lead to the exchange-coupling interaction or other interactions, which could improve the magnetic properties of SBA-15 nanocomposites. Mesoporous Fe/SBA-15 had been prepared via in situ anchoring Fe2O3 into the frame and the micropores of SBA-15 using the sol-gel and hydrothermal processes. Co3O4 nanoparticles had been impregnated into the mesopores of Fe/SBA-15 to form mesoporous Fe/SBA-15-Co3O4 nanocomposites. XRD, HRTEM, VSM, and N2 physisorption isotherms were used to characterize the mesostructure and magnetic properties of the SBA-15 nanocomposites, and all results indicated that the Fe2O3 nanoparticles presented into the frame and micropores, while the Co3O4 nanoparticles existed inside the mesopores of Fe/SBA-15. Furthermore, the magnetic properties of SBA-15 could be conveniently adjusted by the Fe2O3 and Co3O4 magnetic nanoparticles. Fe/SBA-15 exhibited ferromagnetic properties, while the impregnation of Co3O4 nanoparticles greatly improved the coercivity with a value of 1424.6 Oe, which was much higher than that of Fe/SBA-15.

  14. Phosphoryl functionalized mesoporous silica for uranium adsorption

    International Nuclear Information System (INIS)

    Xue, Guo; Yurun, Feng; Li, Ma; Dezhi, Gao; Jie, Jing; Jincheng, Yu; Haibin, Sun; Hongyu, Gong; Yujun, Zhang

    2017-01-01

    Highlights: • Phosphoryl functionalized mesoporous silica (TBP-SBA-15) is synthesized. • The amino and phosphoryl groups are successfully grafted on SBA-15. • TBP-SBA-15 has high and rapid uranium adsorption capacity in broad pH range. • The U(VI) adsorption of TBP-SBA-15 is spontaneous and belongs to chemical adsorption. - Abstract: Phosphoryl functionalized mesoporous silica (TBP-SBA-15) was synthesized by modified mesoporous silica with γ-amino propyl triethoxy silane and tributyl phosphate. The obtained samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), small angle X-ray diffraction (SAXRD), thermo-gravimetric/differential thermalanalyzer (TG/DTA), N_2 adsorption–desorption (BET) and Fourier transform infrared spectroscopy (FT-IR) techniques. Results showed that TBP-SBA-15 had large surface areas with ordered channel structure. Moreover, the effects of adsorption time, sorbent dose, solution pH, initial uranium concentration and temperature on the uranium adsorption behaviors were investigated. TBP-SBA-15 showed a high uranium adsorption capacity in a broad range of pH values. The U(VI) adsorption rate of TBP-SBA-15 was fast and nearly achieved completion in 10 min with the sorbent dose of 1 g/L. The U(VI) adsorption of TBP-SBA-15 followed the pseudo-second-order kinetic model and Freundlich isotherm model, indicating that the process was belonged to chemical adsorption. Furthermore, the thermodynamic parameters (ΔG"0, ΔH"0 and ΔS"0) confirmed that the adsorption process was endothermic and spontaneous.

  15. Phosphoryl functionalized mesoporous silica for uranium adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Xue, Guo; Yurun, Feng; Li, Ma; Dezhi, Gao; Jie, Jing; Jincheng, Yu; Haibin, Sun [Key Laboratory for Liquid-Solid Structural Evolution & Processing of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Hongyu, Gong, E-mail: gong_hongyu@163.com [Key Laboratory for Liquid-Solid Structural Evolution & Processing of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Yujun, Zhang, E-mail: yujunzhangcn@163.com [Key Laboratory for Liquid-Solid Structural Evolution & Processing of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, Shandong University, Jinan 250061 (China)

    2017-04-30

    Highlights: • Phosphoryl functionalized mesoporous silica (TBP-SBA-15) is synthesized. • The amino and phosphoryl groups are successfully grafted on SBA-15. • TBP-SBA-15 has high and rapid uranium adsorption capacity in broad pH range. • The U(VI) adsorption of TBP-SBA-15 is spontaneous and belongs to chemical adsorption. - Abstract: Phosphoryl functionalized mesoporous silica (TBP-SBA-15) was synthesized by modified mesoporous silica with γ-amino propyl triethoxy silane and tributyl phosphate. The obtained samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), small angle X-ray diffraction (SAXRD), thermo-gravimetric/differential thermalanalyzer (TG/DTA), N{sub 2} adsorption–desorption (BET) and Fourier transform infrared spectroscopy (FT-IR) techniques. Results showed that TBP-SBA-15 had large surface areas with ordered channel structure. Moreover, the effects of adsorption time, sorbent dose, solution pH, initial uranium concentration and temperature on the uranium adsorption behaviors were investigated. TBP-SBA-15 showed a high uranium adsorption capacity in a broad range of pH values. The U(VI) adsorption rate of TBP-SBA-15 was fast and nearly achieved completion in 10 min with the sorbent dose of 1 g/L. The U(VI) adsorption of TBP-SBA-15 followed the pseudo-second-order kinetic model and Freundlich isotherm model, indicating that the process was belonged to chemical adsorption. Furthermore, the thermodynamic parameters (ΔG{sup 0}, ΔH{sup 0} and ΔS{sup 0}) confirmed that the adsorption process was endothermic and spontaneous.

  16. Highly active and durable Ca-doped Ce-SBA-15 catalyst for biodiesel production

    International Nuclear Information System (INIS)

    Thitsartarn, Warintorn; Maneerung, Thawatchai; Kawi, Sibudjing

    2015-01-01

    In this work, Ca-doped Ce-incorporated SBA-15 (Ca/CeS) catalyst was successfully synthesized by using direct synthesis of Ce-incorporated SBA-15 followed by impregnation of CaO (calcium oxide). The maximum Si/Ce molar ratio that Ce atoms can be incorporated successfully into the mesoporous framework was found to be 5 (CeS-5). After the impregnation of 30 wt. % Ca, the obtained 30Ca/CeS-5 catalysts showed the superior catalytic performance for transesterification reaction of palm oil with methanol and also the higher catalytic activity as compared to other supported catalysts, i.e. CaO/CeO 2 and CaO–CeO 2 /SBA-15. This can be attributed to the well-dispersion of CaO on the CeS-5 support surface. Furthermore, it was found that the leaching of Si, Ce and Ca from the catalyst into biodiesel produced was negligible (i.e. <1 ppm after 7 cycles), indicating the strong interaction between CaO and CeS-5 support. As a result, the 30Ca/CeS-5 catalyst can be reused at least 15 cycles with insignificant decrease in catalytic activity, offering the efficient CaO-based catalyst for biodiesel production. - Highlights: • Mesoporous Ca-based catalyst was successfully developed for biodiesel production. • Catalyst exhibited high activity towards transesterification (FAME yield > 98%). • Catalyst can be effectively re-used at least 15 cycles. • Extremely low catalyst contaminant (<1 ppm) was presented

  17. MIL-53(Fe), MIL-101, and SBA-15 porous materials: potential platforms for drug delivery.

    Science.gov (United States)

    Gordon, Jeff; Kazemian, Hossein; Rohani, Sohrab

    2015-02-01

    Conventional drug administration suffers from several drawbacks, including a lack of specificity for diseased tissue, the necessity of large and frequent doses, and adverse side effects. Great effort is currently being devoted to developing nanoparticle-based therapeutics capable of prolonging drug administration and providing better control. Here we demonstrate the use of flexible microporous MIL-53(Fe) and mesoporous MIL-101 and SBA-15 as matrices for the adsorption and in vitro drug delivery of acetaminophen, progesterone, and stavudine. A drug loading of 20 wt.% was achieved for each of the nanomaterials using an incipient wetness impregnation procedure. BET, DSC, and XRPD analyses indicated that the entire loaded amount of each of the model drugs had successfully been incorporated within the mesoporous channels of both MIL-101 and SBA-15. DSC analysis evidenced that a portion of each of the model drugs had deposited onto the outer surface of MIL-53(Fe) particles; however, the portion of each drug that had incorporated within the microporous channels was slowly delivered in a diffusion-controlled process, which occurred over a period of up to six days for acetaminophen. These results demonstrate the unique ability of MIL-53(Fe) to adapt its porosity and optimize drug-matrix interactions. Owing to its larger pore diameters and weaker host-guest interactions, MIL-101 release times were shorter, yet still prolonged, as evidenced by the complete release of stavudine after five days. Complete release of each of the drugs from SBA-15 occurred very quickly as a result of rapid drug dissolution and diffusion out of the mesopores. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Silica needle template fabrication of metal hollow microneedle arrays

    International Nuclear Information System (INIS)

    Zhu, M W; Li, H W; Chen, X L; Tang, Y F; Lu, M H; Chen, Y F

    2009-01-01

    Drug delivery through hollow microneedle (HMN) arrays has now been recognized as one of the most promising techniques because it minimizes the shortcomings of the traditional drug delivery methods and has many exciting advantages—pain free and tunable release rates, for example. However, this drug delivery method has been hindered greatly from mass clinical application because of the high fabrication cost of HMN arrays. Hence, we developed a simple and cost-effective procedure using silica needles as templates to massively fabricate HMN arrays by using popular materials and industrially applicable processes of micro- imprint, hot embossing, electroplating and polishing. Metal HMN arrays with high quality are prepared with great flexibility with tunable parameters of area, length of needle, size of hollow and array dimension. This efficient and cost-effective fabrication method can also be applied to other applications after minor alterations, such as preparation of optic, acoustic and solar harvesting materials and devices

  19. Silica needle template fabrication of metal hollow microneedle arrays

    Science.gov (United States)

    Zhu, M. W.; Li, H. W.; Chen, X. L.; Tang, Y. F.; Lu, M. H.; Chen, Y. F.

    2009-11-01

    Drug delivery through hollow microneedle (HMN) arrays has now been recognized as one of the most promising techniques because it minimizes the shortcomings of the traditional drug delivery methods and has many exciting advantages—pain free and tunable release rates, for example. However, this drug delivery method has been hindered greatly from mass clinical application because of the high fabrication cost of HMN arrays. Hence, we developed a simple and cost-effective procedure using silica needles as templates to massively fabricate HMN arrays by using popular materials and industrially applicable processes of micro- imprint, hot embossing, electroplating and polishing. Metal HMN arrays with high quality are prepared with great flexibility with tunable parameters of area, length of needle, size of hollow and array dimension. This efficient and cost-effective fabrication method can also be applied to other applications after minor alterations, such as preparation of optic, acoustic and solar harvesting materials and devices.

  20. Ordered nanoporous silica as carriers for improved delivery of water insoluble drugs: a comparative study between three dimensional and two dimensional macroporous silica

    Directory of Open Access Journals (Sweden)

    Wang Y

    2013-10-01

    Full Text Available Ying Wang, Qinfu Zhao, Yanchen Hu, Lizhang Sun, Ling Bai, Tongying Jiang, Siling WangDepartment of Pharmaceutics, Shenyang Pharmaceutical University, Liaoning Province, People’s Republic of ChinaAbstract: The goal of the present study was to compare the drug release properties and stability of the nanoporous silica with different pore architectures as a matrix for improved delivery of poorly soluble drugs. For this purpose, three dimensional ordered macroporous (3DOM silica with 3D continuous and interconnected macropores of different sizes (200 nm and 500 nm and classic mesoporous silica (ie, Mobil Composition of Matter [MCM]-41 and Santa Barbara Amorphous [SBA]-15 with well-ordered two dimensional (2D cylindrical mesopores were successfully fabricated and then loaded with the model drug indomethacin (IMC via the solvent deposition method. Scanning electron microscopy (SEM, N2 adsorption, differential scanning calorimetry (DSC, and X-ray diffraction (XRD were applied to systematically characterize all IMC-loaded nanoporous silica formulations, evidencing the successful inclusion of IMC into nanopores, the reduced crystallinity, and finally accelerated dissolution of IMC. It was worth mentioning that, in comparison to 2D mesoporous silica, 3DOM silica displayed a more rapid release profile, which may be ascribed to the 3D interconnected pore networks and the highly accessible surface areas. The results obtained from the stability test indicated that the amorphous state of IMC entrapped in the 2D mesoporous silica (SBA-15 and MCM-41 has a better physical stability than in that of 3DOM silica. Moreover, the dissolution rate and stability of IMC loaded in 3DOM silica was closely related to the pore size of macroporous silica. The colorimetric 3-(4,5-Dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide (MTT and Cell Counting Kit (CCK-8 assays in combination with direct morphology observations demonstrated the good biocompatibility of nanoporous

  1. 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 imprin......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...

  2. Microwave radiation hydrothermal synthesis and characterization of micro- and mesoporous composite molecular sieve Y/SBA-15

    Directory of Open Access Journals (Sweden)

    Wenyuan Wu

    2017-05-01

    Full Text Available A microwave radiation hydrothermal method to control synthesis of micro- and mesoporous Y/SBA-15 composite molecular sieves was reported. The synthesized SBA-15 and Y/SBA-15 were characterized by scanning electron microscopy (SEM and N2 adsorption–desorption. The three kinds of different concentrations of hydrochloric acid (0.75 M, 2 M and 3.25 M were used to investigate the effect on Y/SBA-15. The analysis results of the composite products indicated that the optimization synthesis condition employed zeolite type Y and TEOS as silicon sources under 0.75 M hydrochloric acid by the microwave radiation hydrothermal synthesis method. The N2 adsorption–desorption test results of micro–mesoporous composite molecular sieve type Y/SBA-15 in mesoporous extent indicated that SBET is 355.529 m2/g, D‾BET is 4.050 nm, and mesoporous aperture focuses on the distribution region of 5.3 nm. It was found that the received composite product has an appropriate proportion of smaller size, larger size pore structure and the thicker pore wall. In addition, its internal channels have a high degree of order and smooth flow in long-range channels.

  3. Silica/Perfluoropolymer nanocomposites fabricated by direct melt-compounding: a novel method without surface modification on nano-silica.

    Science.gov (United States)

    Tanahashi, Mitsuru; Hirose, Masaki; Watanabe, Yusuke; Lee, Jeong-Chang; Takeda, Kunihiko

    2007-07-01

    A novel method for the fabrication of silica/perfluoropolymer nanocomposites was investigated, whereby nano-sized silica particles without surface modification were dispersed uniformly through mechanical breakdown of loosely packed agglomerates of silica nanoparticles with low fracture strength in a polymer melt during direct melt-compounding. The method consists of two stages. The first stage involves preparation of the loose silica agglomerate, and the second stage involves melt-compounding of a completely hydrophobic perfluoropolymer, poly(tetrafluoroethyleneco-perfluoropropylvinylether), with the loose silica agglomerates prepared in the first stage. In the first stage, the packing structure and the fracture strength of the silica agglomerate were controlled by destabilizing an aqueous colloidal silica solution with a mean primary diameter of 190 nm via pH control and salt addition. In the next stage, the silica/perfluoropolymer nanocomposite was fabricated by breaking down the prepared loose silica agglomerates with low fracture strength by means of a shear force inside the polymer melt during melt-compounding.

  4. Fabrication of amorphous silica nanowires via oxygen plasma treatment of polymers on silicon

    Science.gov (United States)

    Chen, Zhuojie; She, Didi; Chen, Qinghua; Li, Yanmei; Wu, Wengang

    2018-02-01

    We demonstrate a facile non-catalytic method of fabricating silica nanowires at room temperature. Different polymers including photoresists, parylene C and polystyrene are patterned into pedestals on the silicon substrates. The silica nanowires are obtained via the oxygen plasma treatment on those pedestals. Compared to traditional strategies of silica nanowire fabrication, this method is much simpler and low-cost. Through designing the proper initial patterns and plasma process parameters, the method can be used to fabricate various regiment nano-scale silica structure arrays in any laboratory with a regular oxygen-plasma-based cleaner or reactive-ion-etching equipment.

  5. Giant dielectric permittivity in interrupted silver nanowires grown within mesoporous silica

    Science.gov (United States)

    Maity, Anupam; Samanta, Subha; Chatterjee, Soumi; Maiti, Ramaprasad; Biswas, Debasish; Saha, Shyamal K.; Chakravorty, Dipankar

    2018-06-01

    Nanoglasses in the system Ag2O–SiO2 were formed within the pores of mesoporous silica SBA-15 (Santa Barbara Amorphous). Silver nanowires of diameter 5 nm were grown within SBA-15 by the process of electrodeposition. The nanowires were disrupted by applying a suitable voltage pulse. Detailed transmission and scanning electron microscopy studies were carried out. The disrupted silver strands were found to have an average length of 90 nm. The density of interrupted strands was estimated from the electron micrographs and found to have values in the range (10–20)  ×  1010 cm‑2. Dielectric constant and dielectric loss factors of the nanocomposites of disrupted silver strand—containing Ag2O–SiO2 glass and SBA-15 were found to have values in the range 200–300 and 0.014–0.008 respectively at frequencies in the range 10 kHz–2 MHz. These values were found to be in satisfactory agreement with the theoretical model of Rice and Bernasconi emanating from the theory of Gorkhov and Eliashberg. These nanocomposites are expected to be useful in the fabrication of supercapacitors, after developing suitable electrode system for the material.

  6. Metathesis of 2-pentene over Mo and W supported mesoporous molecular sieves MCM-41 and SBA-15

    Czech Academy of Sciences Publication Activity Database

    Ibrahim, M. A.; Akhtar, M. N.; Čejka, Jiří; Montanari, E.; Balcar, Hynek; Kubů, Martin; Al-Khattaf, S. S.

    2017-01-01

    Roč. 53, SEP 2017 (2017), s. 119-126 ISSN 1226-086X R&D Projects: GA ČR(CZ) GAP106/12/0189 Institutional support: RVO:61388955 Keywords : metathesis * MCM-41 * SBA-15 Subject RIV: CF - Physical ; Theoretical Chemistry OBOR OECD: Physical chemistry Impact factor: 4.421, year: 2016

  7. Catalytic Synthesis of n-Butyl Oleate by Cerium Complex Doped Y/SBA-15 Composite Molecular Sieve

    Science.gov (United States)

    Shi, Chunwei; Bian, Xue; Wu, Yongfu; Cong, Yufeng; Pei, Mingyuan

    2018-01-01

    Cerium ion was successfully incorporated into Y/SBA-15 micro-mesoporous molecular sieves via the hydrothermal synthesis method to give a series of composite materials. The prepared materials were thoroughly characterized using Fourier transform infrared spectroscopy (FT-IR), X-ray fluorescence spectroscopy (XRF), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and differential thermo gravimetric analysis (TG-DTG). The results showed that the prepared composite materials retained the highly ordered mesoporous two-dimensional hexagonal structure of SBA-15 and the octagonal structure of Y. The catalyst Ce-Y/SBA-15 was prepared and characterized, then the esterification of n-butanol and oleic acid was studied with bismuth phosphotungstate as a catalyst. Using this model reaction, the effects of Ce-HY/SBA-15, molar ratio of alcohol to oleic acid, amount of catalysts, reaction time and reaction temperature were investigated. The experimental results show that the optimal reaction conditions were: 1.8:1 molar ratio of alcohol to acid, 5 % catalyst amount (based on weight of oleic acid), 4 h reaction time and reflux conditions. Under these conditions, the yield of esterification was 90.6 %. The results suggest that the addition of Ce can effectively improve the catalytic properties of composite molecular sieves.

  8. CO2 activation through silylimido and silylamido zirconium hydrides supported on N-donor chelating SBA15 surface ligand

    KAUST Repository

    Pasha, Fahran Ahmad; Bendjeriou-Sedjerari, Anissa; Abou-Hamad, Edy; Huang, Kuo-Wei; Basset, Jean-Marie

    2016-01-01

    Density functional theory calculations and 2D 1H-13C HETCOR solid state NMR spectroscopy prove that CO2 can probe, by its own reactivity, different types of N-donor surface ligands on SBA15-supported ZrIV hydrides: [(≡Si-O-)(≡Si-N=)[Zr]H] and [(≡Si

  9. Understanding the effect of post-synthesis ammonium treatment on the catalytic activity of Au/Ti-SBA-15 catalysts for the oxidation of propene

    NARCIS (Netherlands)

    Sacaliuc-Parvulescu, E.; Friedrich, H.; Palkovits, R.; Weckhuysen, B.M.; Nijhuis, T.A.

    2008-01-01

    Postsynthesis ammonium treatment induces a substantial increase in the catalytic activity of Au/Ti- SBA-15 catalysts for the direct vapor-phase epoxidation of propylene using hydrogen and oxygen. The PO formation rate of a calcined Au/Ti-SBA-15 catalyst prepared by this method increased from 4.3

  10. Understanding the effect of postsynthesis ammonium treatment on the catalytic activity of Au/TI-SBA-15 catalysts for the oxidation of propene

    NARCIS (Netherlands)

    Sacaliuc, E.; Friedrich, H.; Palkovits, R.; Weckhuysen, B.M.; Nijhuis, T.A.

    2008-01-01

    Postsynthesis ammonium treatment induces a substantial increase in the catalytic activity of Au/Ti-SBA-15 catalysts for the direct vapor-phase epoxidation of propylene using hydrogen and oxygen. The PO formation rate of a calcined Au/Ti-SBA-15 catalyst prepared by this method increased from 4.3 mgPO

  11. A Dual-Functional [SBA-15/Fe3O4/P(N-iPAAm] Hybrid System as a Potential Nanoplatform for Biomedical Application

    Directory of Open Access Journals (Sweden)

    Andreza de Sousa

    2014-01-01

    Full Text Available The synthesis strategy of a multifunctional system of [SBA-15/Fe3O4/P(N-iPAAm] hybrids of interest for bioapplications was explored. Magnetite nanoparticles coated by mesoporous silica were prepared by an alternative chemical route using neutral surfactant and without the application of any functionalization method. Monomer adsorption followed by in situ polymerization initiated by a radical was the adopted procedure to incorporate the hydrogel into the pore channels of silica nanocomposite. Characterization of the materials was carried out by using X-ray diffraction (XRD, Fourier-transform infrared spectroscopy (FTIR, N2 adsorption, transmission electron microscopy (TEM, and Temperature programmed reduction studies (TPR. Their application as drug delivery system using atenolol as a model drug to assess the influence of the application of low frequency alternating magnetic fields on drug release was evaluated. The structural characteristics of the magnetic hybrid nanocomposite, including the effect of the swelling behavior on heating by the application of an alternating magnetic field, are presented and discussed.

  12. Innovative preparation of Au/C by replication of gold-containing mesoporous silica catalysts

    KAUST Repository

    Kerdi, Fatmé ; Caps, Valerie; Tuel, Alain

    2010-01-01

    A new strategy, based on the nanocasting concept, has been used to prepare gold nanoparticles (NPs) highly dispersed in meso-structured carbons. Gold is first introduced in various functionalized mesostructured silicas (MCM-48 and SBA-15

  13. Covalent Anchoring of Chloroperoxidase and Glucose Oxidase on the Mesoporous Molecular Sieve SBA-15

    Directory of Open Access Journals (Sweden)

    Martin Hartmann

    2010-02-01

    Full Text Available Functionalization of porous solids plays an important role in many areas, including heterogeneous catalysis and enzyme immobilization. In this study, large-pore ordered mesoporous SBA-15 molecular sieves were synthesized with tetraethyl orthosilicate (TEOS in the presence of the non-ionic triblock co-polymer Pluronic P123 under acidic conditions. These materials were grafted with 3 aminopropyltrimethoxysilane (ATS, 3-glycidoxypropyltrimethoxysilane (GTS and with 3 aminopropyltrimethoxysilane and glutaraldehyde (GA-ATS in order to provide covalent anchoring points for enzymes. The samples were characterized by nitrogen adsorption, powder X-ray diffraction, solid-state NMR spectroscopy, elemental analysis, diffuse reflectance fourier transform infrared spectroscopy and diffuse reflectance UV/Vis spectroscopy. The obtained grafted materials were then used for the immobilization of chloroperoxidase (CPO and glucose oxidase (GOx and the resulting biocatalysts were tested in the oxidation of indole. It is found that enzymes anchored to the mesoporous host by the organic moieties can be stored for weeks without losing their activity. Furthermore, the covalently linked enzymes are shown to be less prone to leaching than the physically adsorbed enzymes, as tested in a fixed-bed reactor under continuous operation conditions.

  14. Summary different routes for procurement of molecular sieves type AL-SBA-15

    International Nuclear Information System (INIS)

    Figueiroa, D.S.; Santos, J.O.P.N.; Medeiros, C.D.; Sousa, B.V.

    2012-01-01

    The search for new materials to assist industrial development, especially in the chemical industry has been growing more and more. Molecular sieves are great examples of these materials that aim the improvement of various chemical processes. The present work aimed to synthesize the molecular sieve Al-SBA-15 by two different synthesis procedures. In procedure A was used a temperature of 40°C for 24 hours during stirring process. For B process the stirring procedure was done at room temperature. The molar composition of reactants was: 1.0 SiO 2 : 0.04 Al 2 O 3 :0.0168 EO 20 PO 70 EO 20 : 5.85 HCl: 160 H 2 O. The pH of the reaction gel was adjusted to 7 and after the gel was putted under 100 deg C for 48 hours for the heat treatment. Then the sample was calcined under flowing air at 500° C for 6 hours. By techniques such as XRD and SEM, it was confirmed the formation of the hexagonal mesoporous structure, with an orderly distribution of its pores, also indicating the successful incorporation of aluminum into the hexagonal structure of the catalyst support. (author)

  15. The Epoxidation of Limonene over the TS-1 and Ti-SBA-15 Catalysts

    Directory of Open Access Journals (Sweden)

    Agnieszka Wróblewska

    2014-11-01

    Full Text Available Limonene belongs to a group of very important intermediates used in the production of fine chemicals. This monoterpene compound can be obtained from peels of oranges or lemon which are a (biomass waste from the orange juice industry. Thus, limonene is a renewable, easy available and a relatively cheap compound. This work presents preliminary studies on the process of limonene epoxidation over zeolite type catalysts such as: TS-1 and Ti-SBA-15. In these studies methanol was used as a solvent and as an oxidizing agent a 60 wt % hydrogen peroxide solution was applied. The activity of each catalyst was investigated for four chosen temperatures (0 °C, 40 °C, 80 °C and 120 °C. The reaction time was changed from 0.5 to 24 h. For each catalyst the most beneficial conditions (the appropriate temperature and the reaction time have been established. The obtained results were compared and the most active catalyst was chosen. These studies have also shown different possible ways of limonene transformation, not only in the direction of 1,2-epoxylimonene and its corresponding diol, but also in direction of carveol, carvone and perillyl alcohol—compounds with a lot of applications. The possible mechanisms of formation of the allylic oxidation products were proposed.

  16. Preparation of ionic liquid-modified SBA-15 doped with molybdovanadophosphoric acid for oxidative desulfurization

    International Nuclear Information System (INIS)

    Zhuang, Jiang Zhou; Jin, Xiao Yin; Shen, Xian Lin; Tan, Jun Jun; Nie, Long Hui; Xiang, Jian; Hu, Bing

    2015-01-01

    A series of catalysts, ionic liquid-modified SBA-15 (denoted ILSBA) doped with H 5 PMo 10 V 2 O 40 (HPMoV 2 ) have been synthesized and characterized by XRD, FT-IR, 1 H NMR, TG-DTA, and TEM. The catalyst was used for the removal of dibenzothiophene (DBT) in model oil combined with hydrogen peroxide (the oxidant) and acetonitrile (the phase-transfer agent). It was observed that the sulfur content of DBT can be reduced from 500 to 2 ppm by adjusting the amount of catalyst, the reaction temperatures and the reaction time. Besides, the catalyst activity for different sulfur compounds showed a huge difference which may be mainly affected by the electron densities of sulfur atom. Moreover, the catalyst can be recycled seven times without a significant loss in activity, which could be ascribed to the strong electrostatic interaction between ILSBA and HPMoV 2 . In addition, a postulated mechanism was proposed to reveal the oxidative desulfurization process

  17. Preparation of ionic liquid-modified SBA-15 doped with molybdovanadophosphoric acid for oxidative desulfurization

    Energy Technology Data Exchange (ETDEWEB)

    Zhuang, Jiang Zhou; Jin, Xiao Yin; Shen, Xian Lin; Tan, Jun Jun; Nie, Long Hui; Xiang, Jian; Hu, Bing [Dept. of chool of Chemistry and Chemical Engineering, Hubei University of Technology, Wuhan (China)

    2015-07-15

    A series of catalysts, ionic liquid-modified SBA-15 (denoted ILSBA) doped with H{sub 5}PMo{sub 10}V{sub 2}O{sub 40} (HPMoV{sub 2}) have been synthesized and characterized by XRD, FT-IR, {sup 1}H NMR, TG-DTA, and TEM. The catalyst was used for the removal of dibenzothiophene (DBT) in model oil combined with hydrogen peroxide (the oxidant) and acetonitrile (the phase-transfer agent). It was observed that the sulfur content of DBT can be reduced from 500 to 2 ppm by adjusting the amount of catalyst, the reaction temperatures and the reaction time. Besides, the catalyst activity for different sulfur compounds showed a huge difference which may be mainly affected by the electron densities of sulfur atom. Moreover, the catalyst can be recycled seven times without a significant loss in activity, which could be ascribed to the strong electrostatic interaction between ILSBA and HPMoV{sub 2}. In addition, a postulated mechanism was proposed to reveal the oxidative desulfurization process.

  18. Fabrication of superhydrophobic and antibacterial surface on cotton fabric by doped silica -based sols with nanoparticles of copper

    Science.gov (United States)

    Berendjchi, Amirhosein; Khajavi, Ramin; Yazdanshenas, Mohammad Esmaeil

    2011-11-01

    The study discussed the synthesis of silica sol using the sol-gel method, doped with two different amounts of Cu nanoparticles. Cotton fabric samples were impregnated by the prepared sols and then dried and cured. To block hydroxyl groups, some samples were also treated with hexadecyltrimethoxysilane. The average particle size of colloidal silica nanoparticles were measured by the particle size analyzer. The morphology, roughness, and hydrophobic properties of the surface fabricated on cotton samples were analyzed and compared via the scanning electron microscopy, the transmission electron microscopy, the scanning probe microscopy, with static water contact angle (SWC), and water shedding angle measurements. Furthermore, the antibacterial efficiency of samples was quantitatively evaluated using AATCC 100 method. The addition of 0.5% (wt/wt) Cu into silica sol caused the silica nanoparticles to agglomerate in more grape-like clusters on cotton fabrics. Such fabricated surface revealed the highest value of SWC (155° for a 10-μl droplet) due to air trapping capability of its inclined structure. However, the presence of higher amounts of Cu nanoparticles (2% wt/wt) in silica sol resulted in the most slippery smooth surface on cotton fabrics. All fabricated surfaces containing Cu nanoparticles showed the perfect antibacterial activity against both of gram-negative and gram-positive bacteria.

  19. 新型靛红衍生化β-环糊精键合SBA-15液相色谱固定相的制备与表征%Preparation and Characterization of a Novel Isatin Derivative of β-Cyclodextrin-bonded SBA-15 Stationary Phase for HPLC

    Institute of Scientific and Technical Information of China (English)

    张杨; 李来生; 程彪平; 周仁丹; 聂桂珍

    2014-01-01

    利用靛红的羰基与β-环糊精单取代乙二胺的缩合反应,合成得到一种靛红衍生化β-环糊精Schiff碱类化合物。以3-异氰酸丙基三乙氧基硅烷为偶联剂,将其键合到自制的有序介孔二氧化硅材料SBA-15表面,制得一种新型的靛红衍生化β-环糊精键合SBA-15液相色谱固定相( ISCDP)。分别对β-环糊精衍生物、SBA-15及固定相进行必要的结构表征。在反相色谱条件下,以卤代尿嘧啶类极性化合物和二取代苯位置异构体为探针,评价新固定相的基本色谱性能。在极性有机溶剂和反相模式下,将新固定相分别用于β-受体阻滞剂药物和丹磺酰化氨基酸对映体的拆分,探讨了相关色谱分离机理。实验表明,靛红吲哚环的引入,增强了环糊精类固定相对卤代尿嘧啶的反相色谱分离能力,分析时间小于7 min。固定相分离硝基苯胺、氨基苯酚和苯二酚的位置异构体时也表现出较高的立体选择性,其中对位异构体均最后被洗脱,这与包结作用相关;靛红衍生化β-环糊精配体也提高了固定相的手性分离能力,除疏水作用外,靛红衍生化β-环糊精配体还能提供偶极、氢键、π-π和包结等作用,多种协同作用力有利于提高新固定相的手性和非手性分离的选择性。 SBA-15作为键合基质,其有序的孔结构有利于保持色谱柱的良好渗透性和小的传质阻力,在快速高效分离分析中具有应用潜能。%An isatin derivative ofβ-cyclodextrin Schiff base was first synthesized by the condensation reaction between the carbonyl group of isatin and ethylenediamino group of the mono-substituted β-cyclodextrin. The Schiff base ligand was chemically linked to homemade ordered mesoporous SBA-15 silica gel via 3-( triethoxysilyl) propyl isocyanate coupling agent. In this way, a novel isatin derivative of β-cyclodextrin-bonded SBA-15 stationary phase ( ISCDP) was prepared

  20. Self-immobilization of acidogenic mixed consortia on mesoporous material (SBA-15) and activated carbon to enhance fermentative hydrogen production

    Energy Technology Data Exchange (ETDEWEB)

    Mohan, S. Venkata; Mohanakrishna, G.; Sarma, P.N. [Bioengineering and Environmental Centre, Indian Institute of Chemical Technology, Hyderabad 500607 (India); Reddy, S. Sreevardhan; Raju, B. David; Rao, K.S. Rama [Catalysis and Physical Chemistry Division, Indian Institute of Chemical Technology, Hyderabad 500607 (India)

    2008-11-15

    The influence of self-immobilization of enriched acidogenic mixed consortia on fermentative hydrogen (H{sub 2}) production was studied on different supporting materials [SBA-15 (mesoporous) and activated carbon (granular; GAC and powder; PAC)] using chemical wastewater as substrate. Batch fermentation experiments were performed with same substrate at different organic loading rates (OLRs) under acidophilic microenvironment (pH 5.5) and room temperature (28 {+-} 2 C). Experimental data evidenced the effectiveness of attached growth on both the H{sub 2} yields and substrate degradation efficiency, particularly at higher loading rates. Among the three materials evaluated, immobilization on SBA-15 material showed comparatively effective performance in enhancing both H{sub 2} yield and substrate degradation. Suspended growth (SG-control) culture showed inhibition in terms of both H{sub 2} production and substrate degradation especially at applied higher loading rates. Immobilization on SBA-15 resulted in nine times higher H{sub 2} production (7.29 mol/kg COD{sub R}-day at OLR of 0.83 kg COD/m{sup 3}-day) than the lowest yield observed (suspended growth at OLR of 2.55 kg COD/m{sup 3}-day). Maximum substrate degradation rate (SDR) of 0.96 kg COD/m{sup 3}-day (OLR 2.55 kg COD/m{sup 3}-day) was also observed with SBA-15 immobilization, which is 1.62 times higher than the lowest substrate degradation observed with SG-control experiments with the same OLR. Attached growth on GAC and PAC also showed remarkable improvement in the process performance at higher OLRs compared to SG-control. (author)

  1. Study of DDT and its derivatives DDD, DDE adsorption and degradation over Fe-SBA-15 at low temperature

    Institute of Scientific and Technical Information of China (English)

    Hailin Wang; Hua Tian; Zhengping Hao

    2012-01-01

    Mesoporous SBA-15 with different Fe2O3 loading were synthesized by an in-situ coating progress for removals of dichlorodiphenyltrichloroethane(DDT)and its derivatives,i.e.,1,1-dichloro-2,2-bis-(p-chlorophenyl)ethane(DDD)and 1,l-dichloro-2,2-bis-(4-chloro -phenyl)ethane(DDE).The results from XRD(X-ray diffractometer),TEM(transmission electron microscopy)indicated that the iron could be well dispersed on SBA-15 within 6 wt.% Fe2O3 loading.Nitrogen adsorption-desorption tests indicated that the synthesized materials were characterized by ordered meso-structure,high surface area and large pore volume.DDTs were removed from aqueous media in 12-hr treatment and high removal efficiency of DDTs was achieved at over 94%.DDTs could be completely degraded at 350℃ under the existence of SBA-15 with 4 wt.% Fe2O3 loading.The final degradation products of DDT were dichlorobenzophenone (DCB)and bis-(4-chloro-phenyl)methane(DDM),suggesting a complete dechlorination from trichloromethyl.

  2. Highly selective epoxidation of styrene over mesoporous Au-Ti-SBA-15 via photocatalysis process: Synthesis, characterization, and catalytic application

    Energy Technology Data Exchange (ETDEWEB)

    Guo Yajie; Liu Zhengwang [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000, Anhui (China); Wang Guangjian, E-mail: wgj2260@chnu.edu.cn [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000, Anhui (China); Huang Yanhog; Kang Fangfang [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000, Anhui (China)

    2011-11-15

    Highly ordered Au-Ti-SBA-15 mesoporous molecular sieves were successfully synthesized by one-pot hydrothermal synthesis in acid medium, and were characterized by XRD, UV-vis, SEM, element-mapping, HRTEM, N{sub 2} adsorption, XPS, {sup 29}Si MAS NMR, NH{sub 3}-TPD and FT-IR. The as-prepared Au-Ti-SBA-15 samples were possessed of highly ordered mesostructures with larger pore diameter, pore volume and uniform mesopore size distribution. In the oxidation of styrene with H{sub 2}O{sub 2} as the oxidant over Au-Ti-SBA-15 catalyst under photo-irradiation, reaction parameters, such as molar ratio of H{sub 2}O{sub 2} to styrene, reaction time, solvent, the amount of catalyst, catalyst species, and the amount of 3% NaOH, were conditioned at length. As a result, highly selective epoxidation of styrene over catalyst was carried out perfectly for 10 min with high TOF of 4.75 Multiplication-Sign 10{sup 3} min{sup -1}.

  3. Synthesis of α-MoC1-x Nanoparticles with a Surface-Modified SBA-15 Hard Template: Determination of Structure-Function Relationships in Acetic Acid Deoxygenation.

    Science.gov (United States)

    Baddour, Frederick G; Nash, Connor P; Schaidle, Joshua A; Ruddy, Daniel A

    2016-07-25

    Surface modification of mesoporous SBA-15 silica generated a hydrophobic environment for a molybdenum diamine (Mo-diamine) precursor solution, enabling direct growth of isolated 1.9±0.4 nm α-MoC1-x nanoparticles (NPs) inside the pores of the support. The resulting NP catalysts are bifunctional, and compared to bulk α-MoC1-x and β-Mo2 C, the NPs exhibit a greater acid-site:H-site ratio and a fraction of stronger acid sites. The greater acid-site:H-site ratio results in higher decarbonylation (DCO) selectivity during acetic acid hydrodeoxygenation (HDO) reactions, and the stronger acid sites lead to higher activity and ketonization (KET) selectivity at high temperatures. The hard-templating synthetic method could be a versatile route toward carbide NPs of varying size, composition, and phase, on a range of mesoporous oxide supports. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Biodiesel from Hydrolyzed Waste Cooking Oil Using a S-ZrO2/SBA-15 Super Acid Catalyst under Sub-Critical Conditions

    Directory of Open Access Journals (Sweden)

    Muhammad Nobi Hossain

    2018-01-01

    Full Text Available Due to rapid changes in food habits, a substantial amount of waste fat and used oils are generated each year. Due to strong policies, the disposal of this material into nearby sewers causes ecological and environmental problems in many parts of the world. For efficient management, waste cooking oil, a less expensive, alternative and promising feedstock, can be used as a raw material for producing biofuel. In the present study, we produced a biodiesel from hydrolyzed waste cooking oil with a subcritical methanol process using a synthesized solid super acid catalyst, a sulfated zirconium oxide supported on Santa Barbara Amorphous silica (S-ZrO2/SBA-15. The characterization of the synthesized catalyst was carried out using scanning electron microscopy (SEM, X-ray diffraction (XRD, and the Brunauer-Emmett-Teller (BET method. The catalytic effect on biodiesel production was examined by varying the parameters: temperatures of 120 to 200 °C, 5–20 min times, oil-to-methanol mole ratios between 1:5 to 1:20, and catalyst loadings of 1–2.5%. The maximum biodiesel yield was 96.383%, obtained under optimum reaction conditions of 140 °C, 10 min, and a 1:10 oil-to-methanol molar ratio with a 2.0% catalyst loading. We successfully reused the catalyst five times without regeneration with a 90% efficiency. The fuel properties were found to be within the limits set by the biodiesel standard.

  5. Transition Metal Phosphide Nanoparticles Supported on SBA-15 as Highly Selective Hydrodeoxygenation Catalysts for the Production of Advanced Biofuels.

    Science.gov (United States)

    Yang, Yongxing; Ochoa-Hernández, Cristina; de la Peña O'Shea, Víctor A; Pizarro, Patricia; Coronado, Juan M; Serrano, David P

    2015-09-01

    A series of catalysts constituted by nanoparticles of transition metal (M = Fe, Co, Ni and Mo) phosphides (TMP) dispersed on SBA-15 were synthesized by reduction of the corresponding metal phosphate precursors previously impregnated on the mesostructured support. All the samples contained a metal-loading of 20 wt% and with an initial M/P mole ratio of 1, and they were characterized by X-ray diffraction (XRD), N2 sorption, H2-TPR and transmission electron microscopy (TEM). Metal phosphide nanocatalysts were tested in a high pressure continuous flow reactor for the hydrodeoxygenation (HDO) of a methyl ester blend containing methyl oleate (C17H33-COO-CH3) as main component (70%). This mixture constitutes a convenient surrogate of triglycerides present in vegetable oils, and following catalytic hydrotreating yields mainly n-alkanes. The results of the catalytic assays indicate that Ni2P/SBA-15 catalyst presents the highest ester conversion, whereas the transformation rate is about 20% lower for MoP/SBA-15. In contrast, catalysts based on Fe and Co phosphides show a rather limited activity. Hydrocarbon distribution in the liquid product suggests that both hydrodeoxygenation and decarboxylation/decarbonylation reactions occur simultaneously over the different catalysts, although MoP/SBA-15 possess a selectivity towards hydrodeoxygenation exceeding 90%. Accordingly, the catalyst based on MoP affords the highest yield of n-octadecane, which is the preferred product in terms of carbon atom economy. Subsequently, in order to conjugate the advantages of both Ni and Mo phosphides, a series of catalysts containing variable proportions of both metals were prepared. The obtained results reveal that the mixed phosphides catalysts present a catalytic behavior intermediate between those of the monometallic phosphides. Accordingly, only marginal enhancement of the yield of n-octadecane is obtained for the catalysts with a Mo/Ni ratio of 3. Nevertheless, owing to this high selectivity

  6. Melt flow and mechanical properties of silica/perfluoropolymer nanocomposites Fabricated by direct melt-compounding without surface modification on nano-silica.

    Science.gov (United States)

    Tanahashi, Mitsuru; Watanabe, Yusuke; Lee, Jeong-Chang; Takeda, Kunihiko; Fujisawa, Toshiharu

    2009-01-01

    The authors have previously developed a novel method for the fabrication of silica/perfluoropolymer nanocomposites, wherein nano-sized silica particles without surface modification were dispersed uniformly through breakdown of loosely packed agglomerates of silica nanoparticles with low fracture strength in a polymer melt during direct melt-compounding. The method consists of two stages; the first stage involves preparation of the loose silica agglomerate, and the second stage involves melt-compounding of a completely hydrophobic perfluoropolymer, PFA (poly(tetrafluoroethylene-co-perfluoropropylvinylether)), with the loose silica agglomerates. By using this simple method without any lipophilic treatment of the silica surfaces, silica nanoparticles with a primary diameter of 190 nm could be dispersed uniformly into the PFA matrix. The main purpose of the present study is to evaluate the melt flow and tensile properties of silica/PFA nanocomposites fabricated by the above method. In order to elucidate the effects of the size of the dispersed silica in the PFA matrix on the properties of the composites, silica/PFA composite samples exhibiting the dispersion of larger-sized silica particle-clusters were fabricated as negative controls of the silica dispersion state. The results obtained under the present experimental conditions showed that the size of the dispersed silica in the PFA matrix exerts a strong influence on the ultimate tensile properties, such as tensile strength and elongation at break, and the melt flow rate (MFR) of the composite materials. The MFR of the silica/PFA nanocomposite became higher than that of the pure PFA without silica addition, although the MFR of the PFA composites containing larger silica particle-clusters became much lower than that of the pure PFA. Furthermore, uniform dispersion of isolated silica nanoparticles was found to improve not only the Young's modulus but also the ultimate tensile properties of the composite.

  7. Mechanism for enhanced degradation of clofibric acid in aqueous by catalytic ozonation over MnO{sub x}/SBA-15

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Qiangqiang; Wang, Yu [School of Chemistry & Environment, South China Normal University, Guangzhou 510006 (China); Li, Laisheng, E-mail: llsh@scnu.edu.cn [School of Chemistry & Environment, South China Normal University, Guangzhou 510006 (China); Bing, Jishuai [Key Laboratory of Aquatic Science and Technology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China); Wang, Yingxin; Yan, Huihua [School of Chemistry & Environment, South China Normal University, Guangzhou 510006 (China)

    2015-04-09

    Highlights: • Clofibric acid (CA) is efficiently mineralized by O{sub 3}/MnO{sub x}/SBA-15. • Adsorption of CA and its intermediates on MnO{sub x}/SBA-15 is proved unimportant. • Initiation of hydroxyl radicals (·OH) is enhanced in O{sub 3}/MnO{sub x}/SBA-15. • Uniformly distributed MnO{sub x} accounts for the high activity of MnO{sub x}/SBA-15. • Degradation routes of CA in ozonation alone and catalytic ozonation are proposed. - Abstract: Comparative experiments were conducted to investigate the catalytic ability of MnO{sub x}/SBA-15 for the ozonation of clofibric acid (CA) and its reaction mechanism. Compared with ozonation alone, the degradation of CA was barely enhanced, while the removal of TOC was significantly improved by catalytic ozonation (O{sub 3}/MnO{sub x}/SBA-15). Adsorption of CA and its intermediates by MnO{sub x}/SBA-15 was proved unimportant in O{sub 3}/MnO{sub x}/SBA-15 due to the insignificant adsorption of CA and little TOC variation after ceasing ozone in stopped-flow experiment. The more remarkably inhibition effect of sodium bisulfite (NaHSO{sub 3}) on the removal of TOC in catalytic ozonation than in ozonation alone elucidated that MnO{sub x}/SBA-15 facilitated the generation of hydroxyl radicals (·OH), which was further verified by electron spin-resonance spectroscopy (ESR). Highly dispersed MnO{sub x} on SBA-15 were believed to be the main active component in MnO{sub x}/SBA-15. Some intermediates were indentified and different degradation routes of CA were proposed in both ozonation alone and catalytic ozonation. The amounts of small molecular carboxylic acids (i.e., formic acid (FA), acetic acid (AA) and oxalic acid (OA)) generated in catalytic ozonation were lower than in ozonation alone, resulting from the generation of more ·OH.

  8. Comparative Study of Molecular Basket Sorbents Consisting of Polyallylamine and Polyethylenimine Functionalized SBA-15 for CO2 Capture from Flue Gas.

    Science.gov (United States)

    Wang, Dongxiang; Wang, Xiaoxing; Song, Chunshan

    2017-11-17

    Polyallylamine (PAA)-based molecular basket sorbents (MBS) have been studied for CO 2 capture in comparison with polyethylenimine (PEI)-based MBS. The characterizations including N 2 physisorption, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and thermogravimetric analysis (TGA) showed that PAA (M n =15 000) is more rigid and has more steric hindrance inside SBA-15 pores than PEI owing mainly to its different polymer structure. The effects of temperature and PAA loading on the CO 2 sorption capacity of PAA-based MBS have been examined by TGA by using 100 % CO 2 gas stream and compared with PEI/SBA-15. It was found that the capacity of the PAA/SBA-15 sorbent increased with increasing temperature. The optimum capacity of 88 mg CO2  g sorb -1 was obtained at 140 °C for PAA(50)/SBA-15 whereas the optimum sorption temperature was 75 and 90 °C for PEI-I(50)/SBA-15 (PEI-I, M n =423) and PEI-II(50)/SBA-15 (PEI-II, M n =25 000), respectively. The capacity initially increased with the increase of PAA loading and then dropped at high amine contents, owing to the increased diffusion barrier. The highest CO 2 capacity of 109 mg CO2  g sorb -1 was obtained at a PAA loading of 65 wt %, whereas the PAA(50)/SBA-15 sorbent gave the best amine efficiency of 0.23 mol CO2  mol N -1 . The effect of moisture was examined in a fixed-bed flow system with simulated flue gas containing 15 % CO 2 and 4.5 % O 2 in N 2 . It was found that the presence of moisture significantly enhanced CO 2 sorption over PAA(50)/SBA-15 and greatly improved its cyclic stability and regenerability. Compared with PEI/SBA-15, PAA/SBA-15 possesses a better thermal stability and higher resistance to oxidative degradation. However, the CO 2 sorption rate over the PAA(50)/SBA-15 sorbent was much slower. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Production of Ethylene through Ethanol Dehydration on SBA-15 Catalysts Synthesized by Sol-gel and One-step Hydrothermal Methods.

    Science.gov (United States)

    Autthanit, Chaowat; Jongsomjit, Bunjerd

    2018-02-01

    The present work deals with the catalytic performance of SBA-15 supported catalysts in the gas phase catalytic dehydration of ethanol in the temperature range of 200 to 400°C. The SBA-15 support was incorporated on a zirconium (Zr) and bimetal of zirconium and lanthanum (Zr-La) prepared by sol-gel (SG) and hydrothermal (HT) methods. The catalysts were characterized by means of N 2 physisorption, SEM/EDX, and NH 3 -TPD. The experimental results demonstrated that the Zr-La/SBA-15-HT exhibited the highest catalytic activity. Ethanol conversion and ethylene selectivity were found to increase with increased reaction temperature. The best catalytic results were achieved for Zr-La/SBA-15-HT indicating values of ethanol conversion and ethylene yield of ca. 84% and 80%, respectively at 400°C. The most important parameter influencing their catalytic properties appears to be the interaction between metal and support depending on different methods. The metal dispersion inside the siliceous matrix of SBA-15 has a direct influence on their surface acidity. Meanwhile, the performance of these SBA-15 supported catalysts in ethanol dehydration is also related with the alteration of surface acidity caused by the introduction of Zr and Zr-La.

  10. Pore fabrication in various silica-based nanoparticles by controlled etching

    KAUST Repository

    Zhao, Lan

    2010-07-20

    A novel method based on controlled etching was developed to fabricate nanopores on preformed silica nanoparticles (<100 nm in diameter). The obtained monodisperse nanoporous particles could form highly stable homogeneous colloidal solution. Fluorescent silica nanoparticles and magnetic silica-coated γ-Fe 2O 3 nanoparticles were investigated as examples to illustrate that this strategy could be generally applied to various silica-based functional nanoparticles. The results indicated that this method was effective for generating pores on these nanoparticles without altering their original functionalities. The obtained multifunctional nanoparticles would be useful for many biological and biomedical applications. These porous nanoparticles could also serve as building blocks to fabricate three-dimensionally periodic structures that have the potential to be used as photonic crystals. © 2010 American Chemical Society.

  11. Syngas Production from CO2 Reforming and CO2-steam Reforming of Methane over Ni/Ce-SBA-15 Catalyst

    Science.gov (United States)

    Tan, J. S.; Danh, H. T.; Singh, S.; Truong, Q. D.; Setiabudi, H. D.; Vo, D.-V. N.

    2017-06-01

    This study compares the catalytic performance of mesoporous 10 Ni/Ce-SBA-15 catalyst for CO2 reforming and CO2-steam reforming of methane reactions in syngas production. The catalytic performance of 10 Ni/Ce-SBA-15 catalyst for CO2 reforming and CO2-steam reforming of methane was evaluated in a temperature-controlled tubular fixed-bed reactor at stoichiometric feed composition, 1023 K and atmospheric pressure for 12 h on-stream with gas hourly space velocity (GHSV) of 36 L gcat -1 h-1. The 10 Ni/Ce-SBA-15 catalyst possessed a high specific BET surface area and average pore volume of 595.04 m2 g-1. The XRD measurement revealed the presence of NiO phase with crystallite dimension of about 13.60 nm whilst H2-TPR result indicates that NiO phase was completely reduced to metallic Ni0 phase at temperature beyond 800 K and the reduction temperature relied on different degrees of metal-support interaction associated with the location and size of NiO particles. The catalytic reactivity was significantly enhanced with increasing H2O/CO2 feed ratio. Interestingly, the H2/CO ratio for CO2-steam reforming of methane varied between 1 and 3 indicated the occurrence of parallel reactions, i.e., CH4 steam reforming giving a H2/CO of 3 whilst reverse water-gas shift (RWGS) reaction consuming H2 to produce CO gaseous product.

  12. Fabrication of Magnetite/Silica/Titania Core-Shell Nanoparticles

    Directory of Open Access Journals (Sweden)

    Suh Cem Pang

    2012-01-01

    Full Text Available Fe3O4/SiO2/TiO2 core-shell nanoparticles were synthesized via a sol-gel method with the aid of sonication. Fe3O4 nanoparticles were being encapsulated within discrete silica nanospheres, and a layer of TiO2 shell was then coated directly onto each silica nanosphere. As-synthesized Fe3O4/SiO2/TiO2 core-shell nanoparticles showed enhanced photocatalytic properties as evidenced by the enhanced photodegradation of methylene blue under UV light irradiation.

  13. Heat storage properties of organic phase-change materials confined in the nanospace of mesoporous SBA-15 and CMK-3.

    Science.gov (United States)

    Kadoono, Tomosuke; Ogura, Masaru

    2014-03-28

    A novel type of material encapsulating phase-change materials (PCMs) is reported concerning their implication for use as thermal energy storage devices. The composites of siliceous SBA-15 or carbonaceous CMK-3 mesoporous assemblies and organic PCMs could be used to make leak-free devices that retain their capabilities over many thermal cycles for heat storage/release. A confinement effect was observed that alters the thermal properties of the encapsulated PCM, especially in CMK-3 without any similar effects in other carbon materials.

  14. CO2 activation through silylimido and silylamido zirconium hydrides supported on N-donor chelating SBA15 surface ligand

    KAUST Repository

    Pasha, Fahran Ahmad

    2016-01-04

    Density functional theory calculations and 2D 1H-13C HETCOR solid state NMR spectroscopy prove that CO2 can probe, by its own reactivity, different types of N-donor surface ligands on SBA15-supported ZrIV hydrides: [(≡Si-O-)(≡Si-N=)[Zr]H] and [(≡Si-NH-)(≡Si-X-)[Zr]H2] (X = O or NH). Moreover, [(≡Si-O-)(≡Si-N=)[Zr]H] activates CO2 more efficiently than the other complexes and leads to a carbimato Zr formate.

  15. Novel fabrication of silica nanotubes using multi-walled carbon ...

    Indian Academy of Sciences (India)

    Administrator

    Abstract. Silica nanotubes were synthesized using multi-walled carbon nanotubes (MWCNTs) as template. The as-obtained samples were characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscope (FE–SEM) and photo-.

  16. Fabrication of transparent superhydrophobic glass with fibered-silica network

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Feng [College of Physics, Optoelectronics and Energy & Collaborative Innovation Center of Suzhou Nano Science and Technology, Soochow University, Suzhou 215006 (China); Key Lab of Advanced Optical Manufacturing Technologies of Jiangsu Province & Key Lab of Modern Optical Technologies of Education Ministry of China, Soochow University, Suzhou 215006 (China); Shi, Zhenwu, E-mail: zwshi@suda.edu.cn [College of Physics, Optoelectronics and Energy & Collaborative Innovation Center of Suzhou Nano Science and Technology, Soochow University, Suzhou 215006 (China); Key Lab of Advanced Optical Manufacturing Technologies of Jiangsu Province & Key Lab of Modern Optical Technologies of Education Ministry of China, Soochow University, Suzhou 215006 (China); Jiang, Yingjie; Xu, Chengyun; Wu, Zhuhui; Wang, Yanyan [College of Physics, Optoelectronics and Energy & Collaborative Innovation Center of Suzhou Nano Science and Technology, Soochow University, Suzhou 215006 (China); Key Lab of Advanced Optical Manufacturing Technologies of Jiangsu Province & Key Lab of Modern Optical Technologies of Education Ministry of China, Soochow University, Suzhou 215006 (China); Peng, Changsi, E-mail: changsipeng@suda.edu.cn [College of Physics, Optoelectronics and Energy & Collaborative Innovation Center of Suzhou Nano Science and Technology, Soochow University, Suzhou 215006 (China); Key Lab of Advanced Optical Manufacturing Technologies of Jiangsu Province & Key Lab of Modern Optical Technologies of Education Ministry of China, Soochow University, Suzhou 215006 (China)

    2017-06-15

    Highlights: • Superhydrophobic fibred-silica film with water contact angle of 166° and sliding angle of 1° was efficiently prepared using soot as template by CVD. • The film showed transmittance of 88% in visible range. • The superhydrophobic film possesses excellent mechanical robustness, chemical corrosion resistance, and thermal stability. • The superhydrophobic film showed outstanding self-cleaning behavior. - Abstract: In this paper, silica was deposited on the soot film pre-coated glass via chemical vapor deposition. Through calcination at 500 °C with the assistance of O{sub 2} airflow, the soot film was removed and a novel robust fibered-silica network film was then decorated onto the glass substrate. After modification with fluorosilane, the surface water contact angle (WCA) was 166° and sliding angle (SA) was 1° which behaves a good self-cleaning for the as-prepared glass. And its average transmittance was still over 88% in visible wavelength. Moreover, this fibered-silica coating showed a strong tolerance for heavy water droplets, acid/alkali corrosion, salt solution immersion and thermal treatment.

  17. Fabrication and evaluation of hybrid silica/polymer optical fiber sensors for large strain measurement

    Science.gov (United States)

    Huang, Haiying

    2007-04-01

    Silica-based optical fiber sensors are widely used in structural health monitoring systems for strain and deflection measurement. One drawback of silica-based optical fiber sensors is their low strain toughness. In general, silica-based optical fiber sensors can only reliably measure strains up to 2%. Recently, polymer optical fiber sensors have been employed to measure large strain and deflection. Due to their high optical losses, the length of the polymer optical fibers is limited to 100 meters. In this paper, we present a novel economical technique to fabricate hybrid silica/polymer optical fiber strain sensors for large strain measurement. First, stress analysis of a surface-mounted optical fiber sensor is performed to understand the load distribution between the host structure and the optical fiber in relation to their mechanical properties. Next, the procedure of fabricating a polymer sensing element between two optical fibers is explained. The experimental set-up and the components used in the fabrication process are described in details. Mechanical testing results of the fabricated silica/polymer optical fiber strain sensor are presented.

  18. One-Pot Synthesis of Mesoporous SBA-15 Containing Protonated 3- Aminopropyl Groups

    Czech Academy of Sciences Publication Activity Database

    Sliesarenko, V.V.; Dudarko, O.A.; Zub, Y.L.; Seisenbaeva, G.A.; Kessler, V.G.; Topka, Pavel; Šolcová, Olga

    2013-01-01

    Roč. 20, č. 5 (2013), s. 1315-1321 ISSN 1380-2224 R&D Projects: GA TA ČR TA01020804 Grant - others:NATO SPSP(US) SfP-984398 Institutional support: RVO:67985858 Keywords : mesoporous silica * molybdophosphoric acid immobilization * alkyl ammonium group Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.316, year: 2013

  19. One-Pot Synthesis of Mesoporous SBA-15 Containing Protonated 3- Aminopropyl Groups

    Czech Academy of Sciences Publication Activity Database

    Sliesarenko, V.V.; Dudarko, O.A.; Zub, Y.L.; Seisenbaeva, G.A.; Kessler, V.G.; Topka, Pavel; Šolcová, Olga

    2013-01-01

    Roč. 20, č. 5 (2013), s. 1315-1321 ISSN 1380-2224 R&D Projects: GA TA ČR TA01020804 Grant - others: NATO SPSP(US) SfP-984398 Institutional support: RVO:67985858 Keywords : mesoporous silica * molybdophosphoric acid immobilization * alkyl ammonium group Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.316, year: 2013

  20. Jet-Fuel Range Hydrocarbons from Biomass-Derived Sorbitol over Ni-HZSM-5/SBA-15 Catalyst

    Directory of Open Access Journals (Sweden)

    Yujing Weng

    2015-12-01

    Full Text Available Aromatics and cyclic-hydrocarbons are the significant components of jet fuel with high energy-density. However, conventional technologies for bio-fuel production cannot produce these products without further aromatization and isomerization. In this work, renewable liquid fuel with high content of aromatics and cyclic-hydrocarbons was obtained through aqueous catalytic conversion of biomass sorbitol over Ni-HZSM-5/SBA-15 catalyst. Texture characteristics of the catalyst were determined by physisorption of N2, which indicated its bimodal pore structures were microporous (HZSM-5, pore width: 0.56 nm and mesoporous (SBA-15, pore width: 8 nm. The surface acidity included weak and strong acid sites, predominantly Lewis type, and was further confirmed by the NH3-TPD and Py-IR analysis. The catalytic performances were tested in a fixed-bed reactor under the conditions of 593 K, WHSV of 0.75 h−1, GHSV of 2500 h−1 and 4.0 MPa of hydrogen pressure, whereby oil yield of 40.4 wt. % with aromatics and cyclic-hydrocarbons content of 80.0% was obtained.

  1. A novel visible light-driven Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite: Preparation and application in the photo-degradation of pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Chai, Yuanyuan; Wang, Li; Ren, Jia; Dai, Wei-Lin, E-mail: wldai@fudan.edu.cn

    2015-01-01

    Graphical abstract: - Highlights: • Highly efficient visible-light-driven Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite. • Application in the photo-degradation of RhB. • Synthesis from a facile and simple colloidal method. • 20%-Ag{sub 3}PO{sub 4}/SBA-15 shows 8 times faster degradation rate than Ag{sub 3}PO{sub 4}. • Super stability and recycling ability. - Abstract: A novel visible light-driven environmental-benign Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite photo-catalyst was synthesized for the photo-degradation of pollutants. The exploration on adsorption and photo-catalysis of dye or organic pollution for the nanocomposite was carried out. The adsorption capability for Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite increases by 3 times compared with that of the Ag{sub 3}PO{sub 4} particles. The photo-catalytic activity of nanocomposite is higher than pristine Ag{sub 3}PO{sub 4} nanoparticle for the degradation of RhB or MO under visible light irradiation (λ > 420 nm). The effect of Ag{sub 3}PO{sub 4} loading on the catalytic performance was also studied. The results show that the optimum degradation is achieved over 20% Ag{sub 3}PO{sub 4}/SBA-15. Compared to pure Ag{sub 3}PO{sub 4} nanoparticle, the most efficient catalyst showed 8 times higher photo-catalytic activity for the degradation of RhB. The Ag{sub 3}PO{sub 4}/SBA-15 catalysts were systematically characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–Vis diffuse reflectance spectroscopy (DRS), and N{sub 2}-adsorption–desorption isotherms (BET). A possible mechanism scheme regarding photo-degradation enhancement induced by dye enrichments has been proposed on the Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite. Additionally, the SBA-15 support can enhance the efficiency of separation of catalyst from the reaction mixture, implying that the Ag{sub 3}PO{sub 4} loading on the SBA-15 catalyst will not result in the extra environment and health

  2. A novel visible light-driven Ag3PO4/SBA-15 nanocomposite: Preparation and application in the photo-degradation of pollutants

    International Nuclear Information System (INIS)

    Chai, Yuanyuan; Wang, Li; Ren, Jia; Dai, Wei-Lin

    2015-01-01

    Graphical abstract: - Highlights: • Highly efficient visible-light-driven Ag 3 PO 4 /SBA-15 nanocomposite. • Application in the photo-degradation of RhB. • Synthesis from a facile and simple colloidal method. • 20%-Ag 3 PO 4 /SBA-15 shows 8 times faster degradation rate than Ag 3 PO 4 . • Super stability and recycling ability. - Abstract: A novel visible light-driven environmental-benign Ag 3 PO 4 /SBA-15 nanocomposite photo-catalyst was synthesized for the photo-degradation of pollutants. The exploration on adsorption and photo-catalysis of dye or organic pollution for the nanocomposite was carried out. The adsorption capability for Ag 3 PO 4 /SBA-15 nanocomposite increases by 3 times compared with that of the Ag 3 PO 4 particles. The photo-catalytic activity of nanocomposite is higher than pristine Ag 3 PO 4 nanoparticle for the degradation of RhB or MO under visible light irradiation (λ > 420 nm). The effect of Ag 3 PO 4 loading on the catalytic performance was also studied. The results show that the optimum degradation is achieved over 20% Ag 3 PO 4 /SBA-15. Compared to pure Ag 3 PO 4 nanoparticle, the most efficient catalyst showed 8 times higher photo-catalytic activity for the degradation of RhB. The Ag 3 PO 4 /SBA-15 catalysts were systematically characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–Vis diffuse reflectance spectroscopy (DRS), and N 2 -adsorption–desorption isotherms (BET). A possible mechanism scheme regarding photo-degradation enhancement induced by dye enrichments has been proposed on the Ag 3 PO 4 /SBA-15 nanocomposite. Additionally, the SBA-15 support can enhance the efficiency of separation of catalyst from the reaction mixture, implying that the Ag 3 PO 4 loading on the SBA-15 catalyst will not result in the extra environment and health problems and reduce the cost of wastewater treatment

  3. A highly sensitive electrochemical sensor for the determination of methanol based on PdNPs@SBA-15-PrEn modified electrode.

    Science.gov (United States)

    Karimi, Ziba; Shamsipur, Mojtaba; Tabrizi, Mahmoud Amouzadeh; Rostamnia, Sadegh

    2018-05-01

    In this study, a novel electrochemical sensor for the determination of methanol based on palladium nanoparticles supported on Santa barbara amorphous-15- PrNHEtNH 2 (PdNPs@SBA-15-PrEn) as nanocatalysis platform is presented. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electrochemical methods are employed to characterize the PdNPs@SBA-15-PrEn nanocomposite. The Nafion-Pd@SBA-15-PrEn modified glassy carbon electrode (Nafion-PdNPs@SBA-15-PrEn/GCE) displayed the high electrochemical activity and excellent catalytic characteristic for electro-oxidation of methanol in an alkaline solution. The electro-oxidation performance of the proposed sensor was investigated using cyclic voltammetry (CV) and amperometry. The sensor exhibits a good sensitivity of 0.0905 Amol -1 Lcm -2 , linear range of 20-1000 μM and the corresponding detection limit of 12 μM (3σ). The results demonstrate that the Nafion-PdNPs@SBA-15-PrEn/GCE has potential as an efficient and integrated sensor for methanol detection. Copyright © 2018 Elsevier Inc. All rights reserved.

  4. Catalytic Steam Reforming of Toluene as a Model Compound of Biomass Gasification Tar Using Ni-CeO2/SBA-15 Catalysts

    Directory of Open Access Journals (Sweden)

    Erik Dahlquist

    2013-07-01

    Full Text Available Nickel supported on SBA-15 doped with CeO2 catalysts (Ni-CeO2/SBA-15 was prepared, and used for steam reforming of toluene which was selected as a model compound of biomass gasification tar. A fixed-bed lab-scale set was designed and employed to evaluate the catalytic performances of the Ni-CeO2/SBA-15 catalysts. Experiments were performed to reveal the effects of several factors on the toluene conversion and product gas composition, including the reaction temperature, steam/carbon (S/C ratio, and CeO2 loading content. Moreover, the catalysts were subjected to analysis of their carbon contents after the steam reforming experiments, as well as to test the catalytic stability over a long experimental period. The results indicated that the Ni-CeO2/SBA-15 catalysts exhibited promising capabilities on the toluene conversion, anti-coke deposition and catalytic stability. The toluene conversion reached as high as 98.9% at steam reforming temperature of 850 °C and S/C ratio of 3 using the Ni-CeO2(3wt%/SBA-15 catalyst. Negligible coke formation was detected on the used catalyst. The gaseous products mainly consisted of H2 and CO, together with a little CO2 and CH4.

  5. Optimization of the Adsorption of Malachite Green on the NH2-SBA-15 Nano-adsorbent Using the Taguchi Method by Qualitek-4 Software An Isotherm, Kinetic, and Thermodynamic Study

    Directory of Open Access Journals (Sweden)

    Arghavan Mirahsani

    2015-01-01

    Full Text Available SBA-15 nanoporous silica was prepared and functionalized with propylamine groups via post-synthesis grafting to develop efficient adsorbents of dyes in wastewater. The materials thus prepared were then characterized by XRD, N2 adsorption-desorption, and FTIR. Adsorption of a cationic dye, malachite green, on functionalized SBA-15 was investigated under various conditions of pH (5, 6, and 7, temperature (10, 20, and 30 °C, adsorbent dosage (0.1, 0.3, and 0.5 g/L, and dye concentration (50, 100, 150, 200, 250, 300 mg/L. Maximum equilibrium adsorption capacity to achieve maximum removal percentage (R%=100% in optimum conditions (dye concentration=100 mg/L, pH=7, adsorbent dosage= 0.3 g/L was estimated at 333 mg/g. The Taguchi method was used to optimize the adsorption performances of the materials , and then the isotherm, kinetic, and thermodynamic properties were analyzed under the optimum conditions. The results showed that the overall process was fast and its kinetics was well-fitted by pseudo-second-order kinetic model. The experimental data agreed well with Freundlich model. Therefore, the maximum amount of multilayer dye adsorbed was estimated as 500 mg/g. Based on the results obtained, this process may be regarded as an endothermic one with a negative ∆G, which shows the process is also spontaneous. Finally, the results indicate that the silica‐based nanoporous organic–inorganic hybrid material can be a promising sorbent for the removal of malachite green from aquatic solutions

  6. Research on the Ordered Mesoporous Silica for Tobacco Harm Reduction

    Science.gov (United States)

    Wang, Y.; Y Li, Z.; Ding, J. X.; Hu, Z. J.; Liu, Z.; Zhou, G.; Huang, T. H.

    2017-12-01

    For reducting tobacco harm, this paper prepared an ordered mesoporous silica by using triblock copolymer Pluronic P123 as template. The property of this material was characterized by the X-ray scattering spectrum(XRD), Transmission electron microscopy(TEM), Scanning electron microscopy (SEM) and Nitrogen adsorption/desorption. Then this ordered mesoporous silica was added into the cigarette filter in order to researching its effect of cigarette harm index. The result shows that the feature of SBA-15 was grain morphology, ordered arrangement, tubular porous 2-D hexagonal structure. The application of SBA-15 in cigarette filter can selectively reduce harmful components in cigarette smoke such as crotonaldehyde, hydrogen cyanide, benzo pyrene and tar. The synthesized SBA-15 could properly reduce cigarette harm index.

  7. Superhydrophobic transparent films from silica powder: Comparison of fabrication methods

    KAUST Repository

    Liu, Li-Der; Lin, Chao-Sung; Tikekar, Mukul; Chen, Ping-Hei

    2011-01-01

    The lotus leaf is known for its self-clean, superhydrophobic surface, which displays a hierarchical structure covered with a thin wax-like material. In this study, three fabrication techniques, using silicon dioxide particles to create surface roughness followed by a surface modification with a film of polydimethylsiloxane, were applied on a transparent glass substrate. The fabrication techniques differed mainly on the deposition of silicon dioxide particles, which included organic, inorganic, and physical methods. Each technique was used to coat three samples of varying particle load. The surface of each sample was evaluated with contact angle goniometer and optical spectrometer. Results confirmed the inverse relationships between contact angle and optical transmissivity independent of fabrication techniques. Microstructural morphologies also suggested the advantage of physical deposition over chemical methods. In summary, the direct sintering method proved outstanding for its contact angle vs transmissivity efficiency, and capable of generating a contact angle as high as 174°. © 2011 Elsevier B.V. All rights reserved.

  8. Superhydrophobic transparent films from silica powder: Comparison of fabrication methods

    KAUST Repository

    Liu, Li-Der

    2011-07-01

    The lotus leaf is known for its self-clean, superhydrophobic surface, which displays a hierarchical structure covered with a thin wax-like material. In this study, three fabrication techniques, using silicon dioxide particles to create surface roughness followed by a surface modification with a film of polydimethylsiloxane, were applied on a transparent glass substrate. The fabrication techniques differed mainly on the deposition of silicon dioxide particles, which included organic, inorganic, and physical methods. Each technique was used to coat three samples of varying particle load. The surface of each sample was evaluated with contact angle goniometer and optical spectrometer. Results confirmed the inverse relationships between contact angle and optical transmissivity independent of fabrication techniques. Microstructural morphologies also suggested the advantage of physical deposition over chemical methods. In summary, the direct sintering method proved outstanding for its contact angle vs transmissivity efficiency, and capable of generating a contact angle as high as 174°. © 2011 Elsevier B.V. All rights reserved.

  9. Preparation and physical characterization of calcium sulfate cement/silica-based mesoporous material composites for controlled release of BMP-2

    Directory of Open Access Journals (Sweden)

    Tan H

    2015-07-01

    Full Text Available Honglue Tan,1 Shengbing Yang,2 Pengyi Dai,1 Wuyin Li,1 Bing Yue2 1Luoyang Orthopedics and Traumatology Institution, Luoyang Orthopedic-Traumatological Hospital, Luoyang, 2Shanghai Key Laboratory of Orthopedic Implants, Department of Orthopedic Surgery, Shanghai Ninth People’s Hospital, Shanghai Jiao Tong University School of Medicine, Shanghai, People’s Republic of China Abstract: As a commonly used implant material, calcium sulfate cement (CSC, has some shortcomings, including low compressive strength, weak osteoinduction capability, and rapid degradation. In this study, silica-based mesoporous materials such as SBA-15 were synthesized and combined with CSC to prepare CSC/SBA-15 composites. The properties of SBA-15 were characterized by X-ray diffraction, transmission electron microscopy, and nitrogen adsorption–desorption isotherms. SBA-15 was blended into CSC at 0, 5, 10, and 20 wt%, referred to as CSC, CSC-5S (5% mass ratio, CSC-10S (10% mass ratio, and CSC-20S (20% mass ratio, respectively. Fourier-transform infrared spectroscopy and compression tests were used to determine the structure and mechanical properties of the composites, respectively. The formation of hydroxyapatite on composite surfaces was analyzed using scanning electron microscopy and X-ray diffraction after soaking in simulated body fluid. BMP-2 was loaded into the composites by vacuum freeze-drying, and its release characteristics were detected by Bradford protein assay. The in vitro degradation of the CSC/SBA-15 composite was investigated by measuring weight loss. The results showed that the orderly, nanostructured, mesoporous SBA-15 possessed regular pore size and structure. The compressive strength of CSC/SBA-15 increased with the increase in SBA-15 mass ratio, and CSC-20S demonstrated the maximum strength. Compared to CSC, hydroxyapatite that formed on the surfaces of CSC/SBA-15 was uniform and compact. The degradation rate of CSC/SBA-15 decreased with increasing

  10. Generation of Well-Defined Pairs of Silylamine on Highly Dehydroxylated SBA-15: Application to the Surface Organometallic Chemistry of Zirconium

    KAUST Repository

    Azzi, Joachim

    2012-01-01

    achieved by an ammonia treatment of a highly dehydroxylated SBA-15 at 1000°C (SBA-151000). This support is known to contain mainly strained reactive siloxane bridges (≡Si-O-Si≡)[1] along with a small amount of isolated plus germinal silanols =Si(OH)2

  11. Facile synthesis of gold nanoparticles on propylamine functionalized SBA-15 and effect of surface functionality of its enhanced bactericidal activity against gram positive bacteria

    International Nuclear Information System (INIS)

    Bhuyan, Diganta; Saikia, Mrinal; Saikia, Lakshi; Gogoi, Animesh; Saikia, Ratul

    2015-01-01

    The facile synthesis of an SBA-15-pr- + NH 3 .Au 0 nano-hybrid material by spontaneous autoreduction of aqueous chloroaurate anions on propylamine functionalized SBA-15 was successfully demonstrated. The as-synthesized SBA-15-pr- + NH 3 .Au 0 nano-hybrid material was well characterized using low and wide angle x-ray diffraction (XRD), N 2 adsorption–desorption isotherms, Fourier transform infrared (FTIR), transmission electron microscopy (TEM), scanning electron microscopy-energy dispersive x-ray spectroscopy (SEM-EDX), x-ray photoelectron spectroscopy (XPS), UV-Visible spectroscopy and atomic absorption spectroscopy (AAS). The activity of the nano-hybrid material as a potent bactericidal agent was successfully tested against Gram positive/negative bacteria viz. Bacillus subtilis, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa. The colony killing percentage of Gram positive bacteria was found to be higher than Gram negative bacteria due to the stronger electrostatic interaction between the positively-charged amine functionality of SBA-15 and the negatively charged functionality of the bacterial cell wall. (paper)

  12. NiMo Catalysts Supported on the Nb Modified Mesoporous SBA-15 and HMS: Effect of Thioglycolic Acid Addition on HDS.

    Czech Academy of Sciences Publication Activity Database

    Palcheva, R.; Kaluža, Luděk; Dimitrov, L.; Tyuliev, G.; Avdeev, G.; Jirátová, Květa; Spojakina, A.

    2016-01-01

    Roč. 50, JUN 25 (2016), s. 24-34 ISSN 0926-860X R&D Projects: GA ČR GAP106/11/0902 Institutional support: RVO:67985858 Keywords : HDS * mesoporous SBA-15 and HMS * thioglycolic acid Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 4.339, year: 2016

  13. Encapsulated heterogeneous base catalysts onto SBA-15 nanoporous material as highly active catalysts in the transesterification of sunflower oil to biodiesel

    Science.gov (United States)

    Albayati, Talib M.; Doyle, Aidan M.

    2015-02-01

    Alkali metals and their hydroxides, Na, NaOH, Li, and LiOH, were encapsulated onto SBA-15 nanoporous material as highly active catalysts for the production of biodiesel fuel from sunflower oil. The incipient wetness impregnation method was adopted for the prepared catalysts. The characterization properties of the catalysts and unmodified SBA-15 were determined using X-ray diffraction, scanning electron microscopy, EDAX, nitrogen adsorption-desorption porosimetry (Brunauer-Emmett-Teller), Fourier-transform infrared spectroscopy, and transmission electron microscopy. Transesterification was conducted in a batch reactor at atmospheric pressure and 65 °C. The catalysts were highly active with yields of fatty acid methyl ester (FAME) in the range 96-99 %. Na/SBA-15 catalyst was reused for seven consecutive cycles under the same reaction conditions; the yield to FAME on the final cycle was 96 %. This study shows that the alkali metals and their hydroxides supported on SBA-15-based catalyst are excellent catalysts for the biodiesel reaction.

  14. Encapsulated heterogeneous base catalysts onto SBA-15 nanoporous material as highly active catalysts in the transesterification of sunflower oil to biodiesel

    Energy Technology Data Exchange (ETDEWEB)

    Albayati, Talib M., E-mail: talib-albyati@yahoo.com [University of Technology, Department of Chemical Engineering (Iraq); Doyle, Aidan M., E-mail: a.m.doyle@mmu.ac.uk [Manchester Metropolitan University, Division of Chemistry and Environmental Science (United Kingdom)

    2015-02-15

    Alkali metals and their hydroxides, Na, NaOH, Li, and LiOH, were encapsulated onto SBA-15 nanoporous material as highly active catalysts for the production of biodiesel fuel from sunflower oil. The incipient wetness impregnation method was adopted for the prepared catalysts. The characterization properties of the catalysts and unmodified SBA-15 were determined using X-ray diffraction, scanning electron microscopy, EDAX, nitrogen adsorption–desorption porosimetry (Brunauer–Emmett–Teller), Fourier-transform infrared spectroscopy, and transmission electron microscopy. Transesterification was conducted in a batch reactor at atmospheric pressure and 65 °C. The catalysts were highly active with yields of fatty acid methyl ester (FAME) in the range 96–99 %. Na/SBA-15 catalyst was reused for seven consecutive cycles under the same reaction conditions; the yield to FAME on the final cycle was 96 %. This study shows that the alkali metals and their hydroxides supported on SBA-15-based catalyst are excellent catalysts for the biodiesel reaction.

  15. Encapsulated heterogeneous base catalysts onto SBA-15 nanoporous material as highly active catalysts in the transesterification of sunflower oil to biodiesel

    International Nuclear Information System (INIS)

    Albayati, Talib M.; Doyle, Aidan M.

    2015-01-01

    Alkali metals and their hydroxides, Na, NaOH, Li, and LiOH, were encapsulated onto SBA-15 nanoporous material as highly active catalysts for the production of biodiesel fuel from sunflower oil. The incipient wetness impregnation method was adopted for the prepared catalysts. The characterization properties of the catalysts and unmodified SBA-15 were determined using X-ray diffraction, scanning electron microscopy, EDAX, nitrogen adsorption–desorption porosimetry (Brunauer–Emmett–Teller), Fourier-transform infrared spectroscopy, and transmission electron microscopy. Transesterification was conducted in a batch reactor at atmospheric pressure and 65 °C. The catalysts were highly active with yields of fatty acid methyl ester (FAME) in the range 96–99 %. Na/SBA-15 catalyst was reused for seven consecutive cycles under the same reaction conditions; the yield to FAME on the final cycle was 96 %. This study shows that the alkali metals and their hydroxides supported on SBA-15-based catalyst are excellent catalysts for the biodiesel reaction

  16. Effect of the preform fabrication process on the properties of all-silica optical fibres

    Science.gov (United States)

    Grishchenko, A. B.

    2017-12-01

    In this paper, we present a detailed comparison of technical capabilities of processes for the fabrication of all-silica optical fibre preforms with the use of an atmospheric pressure radio frequency plasma (POVD process) and low-pressure microwave plasma (PCVD process) and analyse the origin of the difference in optical properties between fibres produced by these methods. It is shown that the higher temperature of the core material and the higher oxygen partial pressure in preform fabrication by the POVD process lead to an increase in optical losses in the visible and UV spectral regions in the silica fibres with low hydroxyl (OH) content and a decrease in the solarisation resistance of the fibres with high OH content, i.e. to a more rapid increase in background losses in response to UV irradiation. No such drawbacks are detected in the case of the growth of reflective layers by the PCVD process.

  17. 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.

  18. Catalytic Activity and Photophysical Properties of Biomolecules Immobilized on Mesoporous Silica

    DEFF Research Database (Denmark)

    Ikemoto, Hideki

    Mesoporous silicas, based on Santa Barbara Amorphous-15 (SBA-15), with different morphology, structure, pore size and functional groups have been synthesized. Two metalloenzymes and a photosynthetic membrane protein were immobilized on or confined in the pores of the mesoporous silicas to prepare...

  19. Microspectroscopic analysis of green fluorescent proteins infiltrated into mesoporous silica nanochannels

    NARCIS (Netherlands)

    Ma, Yujie; Rajendran, Prayanka; Blum, Christian; Cesa, Yanina; Gartmann, Nando; Brühwiler, Dominik; Subramaniam, Vinod

    2011-01-01

    The infiltration of enhanced green fluorescent protein (EGFP) into nanochannels of different diameters in mesoporous silica particles was studied in detail by fluorescence microspectroscopy at room temperature. Silica particles from the MCM-41, ASNCs and SBA-15 families possessing nanometer-sized

  20. Silica Treatments: A Fire Retardant Strategy for Hemp Fabric/Epoxy Composites

    OpenAIRE

    Branda, Francesco; Malucelli, Giulio; Durante, Massimo; Piccolo, Alessandro; Mazzei, Pierluigi; Costantini, Aniello; Silvestri, Brigida; Pennetta, Miriam; Bifulco, Aurelio

    2016-01-01

    In this paper, for the first time, inexpensive waterglass solutions are exploited as a new, simple and ecofriendly chemical approach for promoting the formation of a silica-based coating on hemp fabrics, able to act as a thermal shield and to protect the latter from heat sources. Fourier Transform Infrared (FTIR) and solid-state Nuclear Magnetic Resonance (NMR) analysis confirm the formation of –C–O–Si– covalent bonds between the coating and the cellulosic substrate. The proposed waterglass t...

  1. Fabrication of Ge nanocrystals doped silica-on-silicon waveguides and observation of their strong quantum confinement effect

    DEFF Research Database (Denmark)

    Ou, Haiyan; Rottwitt, Karsten

    2009-01-01

    Germanium (Ge) nanocrystals embedded in silica matrix is an interesting material for new optoelectronic devices. In this paper, standard silica-on-silicon waveguides with a core doped by Ge nanocrystals were fabricated using plasma enhanced chemical vapour deposition and reactive ion etching...

  2. The Multi-Template Molecularly Imprinted Polymer Based on SBA-15 for Selective Separation and Determination of Panax notoginseng Saponins Simultaneously in Biological Samples

    Directory of Open Access Journals (Sweden)

    Chenghong Sun

    2017-11-01

    Full Text Available The feasible, reliable and selective multi-template molecularly imprinted polymers (MT-MIPs based on SBA-15 (SBA-15@MT-MIPs for the selective separation and determination of the trace level of ginsenoside Rb1 (Rb1, ginsenoside Rg1 (Rg1 and notoginsenoside R1 (R1 simultaneously from biological samples were developed. The polymers were constructed by SBA-15 as support, Rb1, Rg1, R1 as multi-template, acrylamide (AM as functional monomer and ethylene glycol dimethacrylate (EGDMA as cross-linker. The new synthetic SBA-15@MT-MIPs were satisfactorily applied to solid-phase extraction (SPE coupled with high performance liquid chromatography (HPLC for the separation and determination of trace Rb1, Rg1 and R1 in plasma samples. Under the optimized conditions, the limits of detection (LODs and quantitation (LOQs of the proposed method for Rb1, Rg1 and R1 were in the range of 0.63–0.75 ng·mL−1 and 2.1–2.5 ng·mL−1, respectively. The recoveries of R1, Rb1 and Rg1 were obtained between 93.4% and 104.3% with relative standard deviations (RSDs in the range of 3.3–4.2%. All results show that the obtained SBA-15@MT-MIPs could be a promising prospect for the practical application in the selective separation and enrichment of trace Panax notoginseng saponins (PNS in the biological samples.

  3. Polypyrrole/hexagonally ordered silica nanocomposite as a novel fiber coating for solid-phase microextraction

    International Nuclear Information System (INIS)

    Gholivand, Mohammad Bagher; Abolghasemi, Mir Mahdi; Fattahpour, Peyman

    2011-01-01

    Highlights: → The polypyrrole/SBA15) nanocomposite was used as a novel coating for SPME fiber. → The proposed fiber was used for the extraction of polycyclic aromatic hydrocarbons. → The proposed SPME fiber is thermal stable, and it has a low limit of detection. → The SPME fiber was applied in polluted river water and wastewater samples. - Abstract: A highly porous fiber coated polypyrrole/hexagonally ordered silica (PPy/SBA15) materials were prepared for solid-phase microextraction (SPME). The PPy/SBA15 nanocomposite was synthesized by an in situ polymerization technique. The resulting material was characterized by the scanning electron microscopy, thermogravimetric analysis and differential thermal analysis. The prepared nanomaterial was immobilized onto a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). A one at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, desorption time and desorption temperature. In optimum conditions (extraction temperature 70 deg. C, extraction time 20 min, ionic strength 20% (W V -1 ), stirring rate 500 rpm, desorption temperature 270 deg. C, desorption time 5 min) the repeatability for one fiber (n = 3), expressed as relative standard deviation (R.S.D. %), was between 5.0% and 9.3% for the tested compounds. The quantitation limit for the studied compounds were between 13.3 and 66.6 pg mL -1 . The life span and stability of the PPy/SBA15 fiber are good, and it can be used more than 50 times at 260 deg. C without any significant change in sorption properties. The developed method offers the advantage of being simple to use, with shorter analysis times, lower cost of equipment, thermal stability of fiber and high

  4. Durable flame retardant finish for silk fabric using boron hybrid silica sol

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Qiang-hua; Gu, Jiali; Chen, Guo-qiang [National Engineering Laboratory for Modern Silk, Soochow University (China); Xing, Tie-ling, E-mail: xingtieling@suda.edu.cn [National Engineering Laboratory for Modern Silk, Soochow University (China); Jiangsu HuaJia Group (China)

    2016-11-30

    Highlights: • Highly homogeneous boron hybrid silica sol flame retardant system was prepared through sol-gel method. • The silk samples treated and cross-linked by this hybrid sol and BTCA solution showed a higher limiting oxygen index (LOI) more than 31.0% and a better washing durability for more than 30 times washing. • The smoke suppression, combustion performance and thermal stability properties of the treated samples have a significant improvement. - Abstract: A hybrid silica sol was prepared via sol gel method using tetraethoxysilane (TEOS) as a precursor and boric acid (H{sub 3}BO{sub 3}) as flame retardant additive and then applied to silk fabric. In order to endow silk fabric with durable flame retardancy, 1,2,3,4-butanetetracarboxylic acid (BTCA) was used as cross-linking agent for the sake of strong linkage formation between the hybrid silica sol and silk fabric. The FT-IR and XPS analysis demonstrated the Si-O-B formation in the sol system, as well as the linkage between the sol and silk after the treatment. The limiting oxygen index (LOI) and smoke density test indicated good flame retardancy and smoke suppression of the treated silk fabrics. The micro calorimeter combustion (MCC) test and thermo gravimetric (TG) analysis showed that the treated samples had less weight loss in the high temperature and lower heat release rate when burning. The washing durability evaluation results indicated that there was a distinct improvement for the silk samples treated with BTCA even after 30 times washing. In addition, the influence of the processing order of BTCA and silica sol treatment on the limiting oxygen index (LOI) of the finished silk fabric was also investigated. And the results demonstrated that the sample treated with BTCA first and then with the silica sol exhibited better LOI value (32.3%) than that of the sample by the conversed treatment order. Moreover the tensile property of treated samples was nearly unchanged, but the handle of sol treated

  5. Selective Hydrogenation of Furfural to Furfuryl Alcohol in the Presence of a Recyclable Cobalt/SBA-15 Catalyst.

    Science.gov (United States)

    Audemar, Maïté; Ciotonea, Carmen; De Oliveira Vigier, Karine; Royer, Sébastien; Ungureanu, Adrian; Dragoi, Brindusa; Dumitriu, Emil; Jérôme, François

    2015-06-08

    The hydrogenation of furfural to furfuryl alcohol was performed in the presence of a Co/SBA-15 catalyst. High selectivity (96 %) at a conversion higher than 95 % is reported over this catalytic system. As the conversion of furfural to furfuryl alcohol occurs over metallic Co sites, the effect of reduction temperature, H2 pressure, and reaction temperature were studied. Optimum reaction conditions were: 150 °C, 1.5 h, 2.0 MPa of H2 . The catalyst was recyclable, and furfuryl alcohol was recovered with a purity higher than 90 %. The effect of the solvent concentration was also studied. With a minimum of 50 wt % of solvent, the selectivity to furfuryl alcohol and the conversion of furfural remained high (both over 80 %). Likewise, the activity of the catalyst is maintained even in pure furfural, which confirms the real potential of the proposed catalytic system. This catalyst was also used in the hydrogenation of levulinic acid to produce γ-valerolactone selectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Catalytic Cracking of Triglyceride-Rich Biomass toward Lower Olefins over a Nano-ZSM-5/SBA-15 Analog Composite

    Directory of Open Access Journals (Sweden)

    Xuan Hoan Vu

    2015-10-01

    Full Text Available The catalytic cracking of triglyceride-rich biomass toward C2–C4 olefins was evaluated over a hierarchically textured nano-ZSM-5/SBA-15 analog composite (ZSC-24 under fluid catalytic cracking (FCC conditions. The experiments were performed on a fully automated Single-Receiver Short-Contact-Time Microactivity Test unit (SR-SCT-MAT, Grace Davison at 550 °C and different catalyst-to-oil mass ratios (0–1.2 g∙g−1. The ZSC-24 catalyst is very effective for transformation of triglycerides to valuable hydrocarbons, particularly lower olefins. The selectivity to C2–C4 olefins is remarkably high (>90% throughout the investigated catalyst-to-oil ratio range. The superior catalytic performance of the ZSC-24 catalyst can be attributed to the combination of its medium acid site amount and improved molecular transport provided by the bimodal pore system, which effectively suppresses the secondary reactions of primarily formed lower olefins.

  7. Straightforward fabrication of black nano silica dusting powder for latent fingerprint imaging

    Science.gov (United States)

    Komalasari, Isna; Krismastuti, Fransiska Sri Herwahyu; Elishian, Christine; Handayani, Eka Mardika; Nugraha, Willy Cahya; Ketrin, Rosi

    2017-11-01

    Imaging of latent fingerprint pattern (aka fingermark) is one of the most important and accurate detection methods in forensic investigation because of the characteristic of individual fingerprint. This detection technique relies on the mechanical adherence of fingerprint powder to the moisture and oily component of the skin left on the surface. The particle size of fingerprint powder is one of the critical parameter to obtain excellent fingerprint image. This study develops a simple, cheap and straightforward method to fabricate Nano size black dusting fingerprint powder based on Nano silica and applies the powder to visualize latent fingerprint. The nanostructured silica was prepared from tetraethoxysilane (TEOS) and then modified with Nano carbon, methylene blue and sodium acetate to color the powder. Finally, as a proof-of-principle, the ability of this black Nano silica dusting powder to image latent fingerprint is successfully demonstrated and the results show that this fingerprint powder provides clearer fingerprint pattern compared to the commercial one highlighting the potential application of the nanostructured silica in forensic science.

  8. Fabrication of high specificity hollow mesoporous silica nanoparticles assisted by Eudragit for targeted drug delivery.

    Science.gov (United States)

    She, Xiaodong; Chen, Lijue; Velleman, Leonora; Li, Chengpeng; Zhu, Haijin; He, Canzhong; Wang, Tao; Shigdar, Sarah; Duan, Wei; Kong, Lingxue

    2015-05-01

    Hollow mesoporous silica nanoparticles (HMSNs) are one of the most promising carriers for effective drug delivery due to their large surface area, high volume for drug loading and excellent biocompatibility. However, the non-ionic surfactant templated HMSNs often have a broad size distribution and a defective mesoporous structure because of the difficulties involved in controlling the formation and organization of micelles for the growth of silica framework. In this paper, a novel "Eudragit assisted" strategy has been developed to fabricate HMSNs by utilising the Eudragit nanoparticles as cores and to assist in the self-assembly of micelle organisation. Highly dispersed mesoporous silica spheres with intact hollow interiors and through pores on the shell were fabricated. The HMSNs have a high surface area (670 m(2)/g), small diameter (120 nm) and uniform pore size (2.5 nm) that facilitated the effective encapsulation of 5-fluorouracil within HMSNs, achieving a high loading capacity of 194.5 mg(5-FU)/g(HMSNs). The HMSNs were non-cytotoxic to colorectal cancer cells SW480 and can be bioconjugated with Epidermal Growth Factor (EGF) for efficient and specific cell internalization. The high specificity and excellent targeting performance of EGF grafted HMSNs have demonstrated that they can become potential intracellular drug delivery vehicles for colorectal cancers via EGF-EGFR interaction. Copyright © 2014 Elsevier Inc. All rights reserved.

  9. Complete Procedure for Fabrication of a Fused Silica Ultrarapid Microfluidic Mixer Used in Biophysical Measurements

    Directory of Open Access Journals (Sweden)

    Dena Izadi

    2017-01-01

    Full Text Available In this paper we present a method to fabricate a fused silica microfluidic device by employing low viscosity KMPR photoresists. The resulting device is a continuous-flow microfluidic mixer based on hydrodynamic focusing. The advantages of this new fabrication method compared to the traditional approach using a poly-silicon mask are simplification, and time and cost reduction, while still preserving the quality and the performance of the mixers. This process results in devices in which the focusing channel has an aspect ratio of 10:1. The newly-fabricated mixer is successfully used to observe the folding of the Pin1 WW domain at the microsecond time scale.

  10. Fabrication of 3D solenoid microcoils in silica glass by femtosecond laser wet etch and microsolidics

    Science.gov (United States)

    Meng, Xiangwei; Yang, Qing; Chen, Feng; Shan, Chao; Liu, Keyin; Li, Yanyang; Bian, Hao; Du, Guangqing; Hou, Xun

    2015-02-01

    This paper reports a flexible fabrication method for 3D solenoid microcoils in silica glass. The method consists of femtosecond laser wet etching (FLWE) and microsolidics process. The 3D microchannel with high aspect ratio is fabricated by an improved FLWE method. In the microsolidics process, an alloy was chosen as the conductive metal. The microwires are achieved by injecting liquid alloy into the microchannel, and allowing the alloy to cool and solidify. The alloy microwires with high melting point can overcome the limitation of working temperature and improve the electrical property. The geometry, the height and diameter of microcoils were flexibly fabricated by the pre-designed laser writing path, the laser power and etching time. The 3D microcoils can provide uniform magnetic field and be widely integrated in many magnetic microsystems.

  11. Fabrication of isolated platinum nanowire gratings and nanoparticles on silica substrate by femtosecond laser irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Nakajima, Yasutaka [School of Integrated Design Engineering, Keio University, 3-14-1, Hiyoshi, Kohoku-ku, Yokohama 223- 8522 (Japan); Nedyalkov, Nikolay [Institute of Electronics, Bulgarian Academy of Sciences, Tzarigradsko shouse 72, Sofia 1784 (Bulgaria); Department of Electronics and Electrical Engineering, Keio University, 3-14-1, Hiyoshi, Kohoku-ku, Yokohama, 223-8522 (Japan); Takami, Akihiro [School of Integrated Design Engineering, Keio University, 3-14-1, Hiyoshi, Kohoku-ku, Yokohama 223- 8522 (Japan); Terakawa, Mitsuhiro, E-mail: terakawa@elec.keio.ac.jp [School of Integrated Design Engineering, Keio University, 3-14-1, Hiyoshi, Kohoku-ku, Yokohama 223- 8522 (Japan); Department of Electronics and Electrical Engineering, Keio University, 3-14-1, Hiyoshi, Kohoku-ku, Yokohama, 223-8522 (Japan)

    2017-02-01

    Highlights: • Formation of HSFL with periodicities shorter than 100 nm. • Structural evolution from platinum nanowire gratings to platinum nanoparticles only by increasing the number of pulses. • Melting and fragmentation of the nanowire gratings would play a key role in structural evolution. - Abstract: We demonstrate the fabrication of isolated platinum nanostructures on a silica substrate by using femtosecond laser. Nanowire gratings which have short periodicities of approximately 50 nm were formed by irradiating a platinum thin film deposited on a fused silica substrate with 800-nm wavelength femtosecond laser pulses. The structural evolution from the nanowire gratings to nanoparticles was observed only by increasing the number of pulses. The periodicities or diameters of the structures showed good uniformity. Scanning electron microscopy of the surfaces and theoretical calculation of temperature profile using a two-temperature model revealed that the structural evolution can be attributed to the fragmentation of the formed nanowires. The presented method provides a simple and high-throughput technique for fabricating both metal nanowire gratings and nanoparticles, which have the potential to be used for the fabrication of optical, electrical and biomedical devices.

  12. Fabrication and optical characterization of silica optical fibers containing gold nanoparticles.

    Science.gov (United States)

    de Oliveira, Rafael E P; Sjödin, Niclas; Fokine, Michael; Margulis, Walter; de Matos, Christiano J S; Norin, Lars

    2015-01-14

    Gold nanoparticles have been used since antiquity for the production of red-colored glasses. More recently, it was determined that this color is caused by plasmon resonance, which additionally increases the material's nonlinear optical response, allowing for the improvement of numerous optical devices. Interest in silica fibers containing gold nanoparticles has increased recently, aiming at the integration of nonlinear devices with conventional optical fibers. However, fabrication is challenging due to the high temperatures required for silica processing and fibers with gold nanoparticles were solely demonstrated using sol-gel techniques. We show a new fabrication technique based on standard preform/fiber fabrication methods, where nanoparticles are nucleated by heat in a furnace or by laser exposure with unprecedented control over particle size, concentration, and distribution. Plasmon absorption peaks exceeding 800 dB m(-1) at 514-536 nm wavelengths were observed, indicating higher achievable nanoparticle concentrations than previously reported. The measured resonant nonlinear refractive index, (6.75 ± 0.55) × 10(-15) m(2) W(-1), represents an improvement of >50×.

  13. Fabrication, Light Emission, and Magnetism of Silica Nanoparticles Hybridized with AIE Luminogens and Inorganic Nanostructures

    Science.gov (United States)

    Faisal, Mahtab

    Much research efforts have been devoted in developing new synthetic approaches for fluorescent silica nanoparticles (FSNPs) due to their potential high-technological applications. However, light emissions from most of the FSNPs prepared so far have been rather weak. This is due to the emission quenching caused by the aggregation of fluorophores in the solid state. We have observed a novel phenomenon of aggregation-induced emission (AIE): a series of propeller-shaped molecules such as tetraphenylethene (TPE) and silole are induced to emit efficiently by aggregate formation. Thus, they are ideal fluorophors for the construction of FSNPs and my thesis work focuses on the synthesis of silica nanoparticles containing these luminogens and magnetic nanostructures. Highly emissive FSNPs with core-shell structures are fabricated by surfactant-free sol-gel reactions of tetraphenylethene- (TPE) and silole-functionalized siloxanes followed by the reactions with tetraethoxysilane. The FSNPs are uniformly sized, surface-charged and colloidally stable. The diameters of the FSNPs are tunable in the range of 45--295 nm by changing the reaction conditions. Whereas their TPE and silole precursors are non-emissive, the FSNPs emit strong visible lights, thanks to the novel aggregation-induced emission characteristics of the TPE and silole aggregates in the hybrid nanoparticles. The FSNPs pose no toxicity to living cells and can be utilized to selectively image cytoplasm of HeLa cells. Applying the same tool in the presence of citrate-coated magnetite nanoparticles, uniform magnetic fluorescent silica nanoparticles (MFSNPs) with smooth surfaces are fabricated. These particles exhibit appreciable surface charges and hence good colloidal stability. They are superparamagnetic, exhibiting no hysteresis at room temperature. UV irradiation of a suspension of MFSNPs in ethanol gives strong blue and green emissions. The MFSNPs can selectively stain the cytoplasmic regions of the living cells

  14. Preparation of Al-SBA-15 Pellets with Low Amount of Additives: Effect of Binder Content on Texture and Mechanical Properties. Application to Friedel-Crafts Alkylation

    Czech Academy of Sciences Publication Activity Database

    Topka, Pavel; Karban, Jindřich; Soukup, Karel; Jirátová, Květa; Šolcová, Olga

    2011-01-01

    Roč. 168, č. 1 (2011), s. 433-440 ISSN 1385-8947 R&D Projects: GA ČR GA104/09/0694; GA AV ČR KAN400720701 Institutional research plan: CEZ:AV0Z40720504 Keywords : mesoporous aluminosilicates * pellets * Al-SBA-15 Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 3.461, year: 2011

  15. Fabrication of fluorescent silica nanoparticles with aggregation-induced emission luminogens for cell imaging.

    Science.gov (United States)

    Chen, Sijie; Lam, Jacky W Y; Tang, Ben Zhong

    2013-01-01

    Fluorescence-based techniques have found wide applications in life science. Among various luminogenic materials, fluorescent nanoparticles have attracted much attention due to their fabulous emission properties and potential applications as sensors. Here, we describe the fabrication of fluorescent silica nanoparticles (FSNPs) containing aggregation-induced emission (AIE) luminogens. By employing surfactant-free sol-gel reaction, FSNPs with uniform size and high surface charge and colloidal stability are generated. The FSNPs emit strong light upon photoexcitation, due to the AIE characteristic of the silole -aggregates in the hybrid nanoparticles. The FSNPs are cytocompatible and can be utilized as fluorescent visualizer for intracellular imaging for HeLa cells.

  16. Mass fabrication of homogeneously Yb-doped silica nanoparticles and their spectroscopic properties

    International Nuclear Information System (INIS)

    Xiong Liangming; Sekiya, Edson H; Saito, Kazuya

    2009-01-01

    A large number of homogeneously Yb-doped silica nanoparticles were continually fabricated in a vapor synthesis route, in which the Yb doping level can be well controlled by varying either the heating temperature or the carrier gas flow rate of the Yb precursor. The sizes, shapes, and morphologies of the nanoparticles were examined, and no crystallites and no Yb 2 O 3 clusters were observed in the nanoparticles. These nanoparticles exhibit a clear Yb 3+ -derived absorption at around 973-975 nm and a dependence of the emission intensity and decay time on the doping level, much different from that of sintered pellets.

  17. Atomic-Level Organization of Vicinal Acid-Base Pairs through the Chemisorption of Aniline and Derivatives onto Mesoporous SBA15

    KAUST Repository

    Basset, Jean-Marie

    2016-06-09

    The design of novel heterogeneous catalysts with multiple adjacent functionalities is of high interest for heterogeneous catalysis. Herein, we report a method to obtain a majority bifunctional acid-base pairs on SBA15. Aniline reacts with SBA15 by opening siloxane bridges leading to N-phenylsilanamine-silanol pairs. In contrast with ammonia treated surfaces, the material is stable under air/moisture. Advanced solid state MAS NMR: 2D ¹H-¹H double-quantum, ¹H-¹³C HETCOR experiments and dynamic nuclear polarization enhanced ²⁹Si and ¹⁵N spectra demonstrate both the close proximity between the two moieties and the formation of a covalent Si-N surface bond and confirm the design of vicinal acid-base pairs. This approach was successfully applied to the design of a series of aniline derivatives bifunctional SBA15. A correlation of the substituents effects on the aromatic ring (Hammet parameters) on the kinetics of the model reaction of Knoevenagel is observed.

  18. Preparation, characterization and catalytic activity of mesoporous Ag2HPW12O40/SBA-15 and Ag2HPW12O40/TiO2 composites

    International Nuclear Information System (INIS)

    Holclajtner-Antunović, Ivanka; Bajuk-Bogdanović, Danica; Popa, Alexandru; Sasca, Viorel; Nedić Vasiljević, Bojana; Rakić, Aleksandra; Uskoković-Marković, Snežana

    2015-01-01

    The current study reports the synthesis and characterization of tungstophosphoric acid and its acid silver salt supported on mesoporous molecular sieve SBA-15 and TiO 2 . Because silver salts are partially insoluble, the SBA-15 and TiO 2 supported silver acid salts were prepared by two step sequential impregnations. The synthesized catalysts were characterized by various physicochemical methods such as Fourier transform infrared and Raman spectroscopy, differential thermal analysis, thermogravimetric analysis, X-ray diffraction, scanning electron microscopy and nitrogen physisorption at −196 °C. It is observed that both active phases keep their Keggin-type structure after being supported on the supports while their specific surface area is considerably increased by deposition on mesoporous substrates. The results also indicated that the synthesized catalysts retained the morphology specific for each of the supports, while their thermal stability is increased in comparison with their active phases. The catalytic activity of the prepared catalysts was probed for the vapor phase dehydration of ethanol at 300 °C. Results revealed that all the catalysts show considerably improved catalytic activity in comparison to the bulk active phases. - Highlights: • SBA-15 and TiO 2 supported Ag 2 HPW 12 O 40 and H 3 PW 12 O 40 were prepared. • Active phases are uniformly dispersed without changing morphology of the substrates. • Composites are more thermally stable than active phases. • Composites exhibit high catalytic activity for gas phase ethanol dehydration

  19. Silica-Silver Nanocomposites as Regenerable Sorbents for Hg0 Removal from Flue Gases.

    Science.gov (United States)

    Cao, Tiantian; Li, Zhen; Xiong, Yong; Yang, Yue; Xu, Shengming; Bisson, Teresa; Gupta, Rajender; Xu, Zhenghe

    2017-10-17

    Silica-silver nanocomposites (Ag-SBA-15) are a novel class of multifunctional materials with potential applications as sorbents, catalysts, sensors, and disinfectants. In this work, an innovative yet simple and robust method of depositing silver nanoparticles on a mesoporous silica (SBA-15) was developed. The synthesized Ag-SBA-15 was found to achieve a complete capture of Hg 0 at temperatures up to 200 °C. Silver nanoparticles on the SBA-15 were shown to be the critical active sites for the capture of Hg 0 by the Ag-Hg 0 amalgamation mechanism. An Hg 0 capture capacity as high as 13.2 mg·g -1 was achieved by Ag(10)-SBA-15, which is much higher than that achievable by existing Ag-based sorbents and comparable with that achieved by commercial activated carbon. Even after exposure to more complex simulated flue gas flow for 1 h, the Ag(10)-SBA-15 could still achieve an Hg 0 removal efficiency as high as 91.6% with a Hg 0 capture capacity of 457.3 μg·g -1 . More importantly, the spent sorbent could be effectively regenerated and reused without noticeable performance degradation over five cycles. The excellent Hg 0 removal efficiency combined with a simple synthesis procedure, strong tolerance to complex flue gas environment, great thermal stability, and outstanding regeneration capability make the Ag-SBA-15 a promising sorbent for practical applications to Hg 0 capture from coal-fired flue gases.

  20. The fabrication and testing of electrospun silica nanofiber membranes for the detection of proteins

    International Nuclear Information System (INIS)

    Tsou, P-H; Kameoka, J; Chou, C-K; Saldana, S M; Hung, M-C

    2008-01-01

    In this study, we fabricated electrospun silica nanofiber membranes and investigated their use in biomolecular sensing. The diameter, porosity and surface-to-volume ratio of nanofiber membranes were investigated under different fabrication conditions. Using this type of nanofiber membrane, enzyme-linked immunosorbent assay (ELISA) was performed, and the results were compared with those obtained with conventional ELISA using polystyrene well plates. The minimum detectable concentration was determined as 0.19 ng ml -1 (1.6 pM), which is 32 times lower than that of conventional ELISA. In addition, the detection time for all processes for the nanofiber membrane was reduced to 1 h, compared with 1 day for conventional ELISA. The increased sensitivity, faster reaction time, and affordability of the nanofiber membrane make it well suited for bio-chip use.

  1. Fabrication of mesoporous silica/polymer composites through solvent evaporation process and investigation of their excellent low thermal expansion property.

    Science.gov (United States)

    Suzuki, Norihiro; Kiba, Shosuke; Yamauchi, Yusuke

    2011-03-21

    We fabricate mesoporous silica/epoxy polymer composites through a solvent evaporation process. The easy penetration of the epoxy polymers into mesopores is achieved by using a diluted polymer solution including a volatile organic solvent. After the complete solvent evaporation, around 90% of the mesopores are estimated to be filled with the epoxy polymer chains. Here we carefully investigate the thermal expansion behavior of the obtained mesoporous silica/polymer composites. Thermal mechanical analysis (TMA) charts revealed that coefficient of linear thermal expansion (CTE) gradually decreases, as the amount of the doped mesoporous silica increases. Compared with spherical silica particle without mesopores, mesoporous silica particles show a greater effect on lowering the CTE values. Interestingly, it is found that the CTE values are proportionally decreased with the decrease of the total amount of the polymers outside the mesopores. These data demonstrate that polymers embedded inside the mesopores become thermally stable, and do not greatly contribute to the thermal expansion behavior of the composites.

  2. Fabrication of epoxy composites with large-pore sized mesoporous silica and investigation of their thermal expansion.

    Science.gov (United States)

    Suzuki, Norihiro; Kiba, Shosuke; Yamauchi, Yusuke

    2012-02-01

    We fabricate epoxy composites with low thermal expansion by using mesoporous silica particles with a large pore diameter (around 10 nm) as inorganic fillers. From a simple calculation, almost all the mesopores are estimated to be completely filled with the epoxy polymer. The coefficient of linear thermal expansion (CTE) values of the obtained epoxy composites proportionally decrease with the increase of the mesoporous silica content.

  3. A mesoporous silica composite scaffold: Cell behaviors, biomineralization and mechanical properties

    Science.gov (United States)

    Xu, Yong; Gao, Dan; Feng, Pei; Gao, Chengde; Peng, Shuping; Ma, HaoTian; Yang, Sheng; Shuai, Cijun

    2017-11-01

    Mesoporous structure is beneficial to cellular response due to the large specific surface area and high pore volume. In this study, mesoporous silica (SBA15) was incorporated into poly-L-lactic acid (PLLA) to construct composite scaffold by selective laser sintering. The results showed that SBA15 facilitated cells proliferation, which was mainly attributed to its unique intrinsic mesoporous structure and the released bioactive silicon. Moreover, the hydrolyzate of soluble mesoporous silica can adsorb ions to form nucleation sites that promote biomineralization, leading to improve biological activity of the composite scaffold. In addition, the compressive strength, compressive modulus and Vickers hardness of the scaffold were increased by 47.6%, 35.5% and 29.53% respectively with 1.5 wt.% SBA15. It was found that the particle enhancement of uniform distributed SBA15 accounted for the mechanic reinforcement of the composite scaffold. It indicated that the PLLA-SBA15 composite scaffold had potential applications in bone tissue engineering.

  4. Silicon oxynitrides of KCC-1, SBA-15 and MCM-41 for CO 2 capture with excellent stability and regenerability

    KAUST Repository

    Patil, Umesh; Fihri, Aziz; Emwas, Abdul-Hamid M.; Polshettiwar, Vivek

    2012-01-01

    ammonia gas, and they demonstrated excellent CO 2 capture capabilities. These materials overcome several limitations of conventional amine-grafted mesoporous silica. They offer good CO 2 capture capacity, faster adsorption-desorption kinetics, efficient

  5. Silica Treatments: A Fire Retardant Strategy for Hemp Fabric/Epoxy Composites

    Directory of Open Access Journals (Sweden)

    Francesco Branda

    2016-08-01

    Full Text Available In this paper, for the first time, inexpensive waterglass solutions are exploited as a new, simple and ecofriendly chemical approach for promoting the formation of a silica-based coating on hemp fabrics, able to act as a thermal shield and to protect the latter from heat sources. Fourier Transform Infrared (FTIR and solid-state Nuclear Magnetic Resonance (NMR analysis confirm the formation of –C–O–Si– covalent bonds between the coating and the cellulosic substrate. The proposed waterglass treatment, which is resistant to washing, seems to be very effective for improving the fire behavior of hemp fabric/epoxy composites, also in combination with ammonium polyphosphate. In particular, the exploitation of hemp surface treatment and Ammonium Polyphosphate (APP addition to epoxy favors a remarkable decrease of the Heat Release Rate (HRR, Total Heat Release (THR, Total Smoke Release (TSR and Specific Extinction Area (SEA (respectively by 83%, 35%, 45% and 44% as compared to untreated hemp/epoxy composites, favoring the formation of a very stable char, as also assessed by Thermogravimetric Analysis (TGA. Because of the low interfacial adhesion between the fabrics and the epoxy matrix, the obtained composites show low strength and stiffness; however, the energy absorbed by the material is higher when using treated hemp. The presence of APP in the epoxy matrix does not affect the mechanical behavior of the composites.

  6. Fabrication of silica-coated gold nanorods and investigation of their property of photothermal conversion

    International Nuclear Information System (INIS)

    Inose, Tomoya; Oikawa, Takahiro; Shibuya, Kyosuke; Tokunaga, Masayuki; Hatoyama, Keiichiro; Nakashima, Kouichi; Kamei, Takashi; Gonda, Kohsuke; Kobayashi, Yoshio

    2017-01-01

    This study described the preparation of silica-coated Au nanorods (AuNR/SiO 2 ) in a colloidal solution, assessed their property of photothermal conversion, and investigated their ability to kill cancer cells using photothermal conversion. Au-seed nanoparticles were produced by reducing hydrogen tetrachloroaurate (HAuCl 4 ) with sodium borohydride (NaBH 4 ) in aqueous n-hexadecyltrimethylammonium bromide (CTAB) solution. AuNRs were then fabricated by reducing HAuCl 4 and silver nitrate (AgNO 3 ) with L-ascorbic acid in the aqueous CTAB solution in the presence of Au-seed nanoparticles. The as-prepared AuNRs were washed by a process composed mainly of centrifugation to remove the CTAB. The washed AuNRs were coated with silica by mixing the AuNR colloidal solution, an aqueous solution of (3-aminopropyl)trimethoxysilane, and tetraethylorthosilicate/ethanol solution with a water/ethanol solution. We found that the addition of AuNR/SiO 2 in water, in mice, and in a culture medium with cancer cells, followed by irradiation with a laser, cause an increase in temperature, demonstrating that AuNR/SiO 2 have the ability of photothermal conversion. In addition, the cancer cells in the culture medium were found to be killed due to the increase in temperature caused by the photothermal conversion. - Highlights: • This study described the preparation of silica-coated Au nanorods (AuNR/SiO 2 ) colloidal solution. • The AuNR/SiO 2 had the ability of photothermal conversion. • The AuNR/SiO 2 also had the ability to kill cancer cells using the photothermal conversion.

  7. Evaluation of bi-functionalized mesoporous silicas as reversed phase/cation-exchange mixed-mode sorbents for multi-residue solid phase extraction of veterinary drug residues in meat samples.

    Science.gov (United States)

    Casado, Natalia; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

    2017-04-01

    A SBA-15 type mesoporous silica was synthesized and bi-functionalized with octadecylsilane (C18) or octylsilane (C8), and sulfonic acid (SO 3 - ) groups in order to obtain materials with reversed-phase/strong cation-exchange mixed-mode retention mechanism. The resulting hybrid materials (SBA-15-C18-SO 3 - and SBA-15-C8-SO 3 - ) were comprehensively characterized. They showed high surface area, high pore volume and controlled porous size. Elemental analysis of the materials revealed differences in the amount of C18 and C8. SBA-15-C18-SO 3 - contained 0.19mmol/g of C18, while SBA-15-C8-SO 3 - presented 0.54mmol/g of C8. The SO 3 - groups anchored to the silica surface of the pore walls were 0.20 and 0.09mmol/g, respectively. The bi-functionalized materials were evaluated as SPE sorbents for the multi-residue extraction of 26 veterinary drug residues in meat samples using ultra-high-performance liquid chromatography coupled to mass spectrometry detector (UHPLC-MS/MS). Different sorbent amounts (100 and 200mg) and organic solvents were tested to optimize the extraction procedure. Both silicas showed big extraction potential and were successful in the extraction of the target analytes. The mixed-mode retention mechanism was confirmed by comparing both silicas with SBA-15 mesoporous silica mono-functionalized with C18 and C8. Best results were achieved with 200mg of SBA-15-C18-SO 3 - obtaining recoveries higher than 70% for the majority of analytes. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. In-situ fabrication of halloysite nanotubes/silica nano hybrid and its application in unsaturated polyester resin

    Science.gov (United States)

    Lin, Jing; Zhong, Bangchao; Jia, Zhixin; Hu, Dechao; Ding, Yong; Luo, Yuanfang; Jia, Demin

    2017-06-01

    Silica nanoparticles was in-situ grown on the surface of halloysite nanotubes (HNTs) by a facile one-step approach to prepare a unique nano-structured hybrid (HNTs-g-Silica). The structure, morphology and composition of HNTs-g-Silica were investigated. It was confirmed that silica nanoparticles with the diameter of 10-20 nm were chemically grafted through Sisbnd O bonds and uniformly dispersed onto the surface of HNTs, leading to the formation of nano-protrusions on the nanotube surface. Due to the significantly improved interface strength between HNTs-g-Silica and polymer matrix, HNTs-g-Silica effectively toughened unsaturated polyester resin (UPE) and endowed UPE with superior thermal stability compared to HNTs. Based on the unique hybrid architecture and the improved properties of UPE nanocomposites, it is envisioned that HNTs-g-Silica may be a promising filler for more high performance and functional polymers composites and the fabrication method may have implications in the synthesis of nano hybrid materials.

  9. Inorganic Nanocrystals Functionalized Mesoporous Silica Nanoparticles: Fabrication and Enhanced Bio-applications

    Directory of Open Access Journals (Sweden)

    Tiancong Zhao

    2017-12-01

    Full Text Available Mesoporous SiO2 nanoparticles (MSNs are one of the most promising materials for bio-related applications due to advantages such as good biocompatibility, tunable mesopores, and large pore volume. However, unlike the inorganic nanocrystals with abundant physical properties, MSNs alone lack functional features. Thus, they are not sufficiently suitable for bio-applications that require special functions. Consequently, MSNs are often functionalized by incorporating inorganic nanocrystals, which provide a wide range of intriguing properties. This review focuses on inorganic nanocrystals functionalized MSNs, both their fabrication and bio-applications. Some of the most utilized methods for coating mesoporous silica (mSiO2 on nanoparticles were summarized. Magnetic, fluorescence and photothermal inorganic nanocrystals functionalized MSNs were taken as examples to demonstrate the bio-applications. Furthermore, asymmetry of MSNs and their effects on functions were also highlighted.

  10. Fabrication of 3D electro-thermal micro actuators in silica glass by femtosecond laser wet etch and microsolidics

    Science.gov (United States)

    Li, Qichao; Shan, Chao; Yang, Qing; Chen, Feng; Bian, Hao; Hou, Xun

    2017-02-01

    This paper demonstrates a novel electro-thermal micro actuator's design, fabrication and device tests which combine microfluidic technology and microsolidics process. A three-dimensional solenoid microchannel with high aspect ratio is fabricated inside the silica glass by an improved femtosecond laser wet etch (FLWE) technology, and the diameter of the spiral coil is only 200 μm. Molten alloy (Bi/In/Sn/Pb) with high melting point is injected into the three-dimensional solenoid microchannel inside the silica glass , then it solidifys and forms an electro-thermal micro actuator. The device is capable of achieving precise temperature control and quick response, and can also be easily integrated into MEMS, sensors and `lab on a chip' (LOC) platform inside the fused silica substrate.

  11. MgO-modified mesoporous silicas impregnated by potassium carbonate for carbon dioxide adsorption

    Czech Academy of Sciences Publication Activity Database

    Zukal, Arnošt; Pastva, Jakub; Čejka, Jiří

    2013-01-01

    Roč. 167, FEB 2013 (2013), s. 44-50 ISSN 1387-1811 R&D Projects: GA ČR GA203/08/0604 Institutional support: RVO:61388955 Keywords : mesoporous adsorbents * SBA-15 silica * introducing of MgO and K2CO3 Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.209, year: 2013

  12. Assessment of the adjuvant activity of mesoporous silica nanoparticles in recombinant Mycoplasma hyopneumoniae antigen vaccines

    Directory of Open Access Journals (Sweden)

    Veridiana Gomes Virginio

    2017-01-01

    Full Text Available The adjuvant potential of two mesoporous silica nanoparticles (MSNs, SBa-15 and SBa-16, was assessed in combination with a recombinant HSP70 surface polypeptide domain from Mycoplasma hyopneumoniae, the etiological agent of porcine enzootic pneumonia (PEP. The recombinant antigen (HSP70212-600, previously shown as immunogenic in formulation with classic adjuvants, was used to immunize BALB/c mice in combination with SBa-15 or SBa-16 MSNs, and the effects obtained with these formulations were compared to those obtained with alum, the adjuvant traditionally used in anti-PEP bacterins. The HSP70212-600 + SBa-15 vaccine elicited a strong humoral immune response, with high serum total IgG levels, comparable to those obtained using HSP70212-600 + alum. The HSP70212-600 + SBa-16 vaccine elicited a moderate humoral immune response, with lower levels of total IgG. The cellular immune response was assessed by the detection of IFN-γ, IL-4 and IL-10 in splenocyte culture supernatants. The HSP70212-600 + SBa-15 vaccine increased IFN-γ, IL-4 and IL-10 levels, while no stimulation was detected with the HSP70212-600 + SBa-16 vaccine. The HSP70212-600 + SBa-15 vaccine induced a mixed Th1/Th2-type response, with an additional IL-10 mediated anti-inflammatory effect, both of relevance for an anti-PEP vaccine. Alum adjuvant controls stimulated an unspecific cellular immune response, with similar levels of cytokines detected in mice immunized either with HSP70212-600 + alum or with the adjuvant alone. The better humoral and cellular immune responses elicited in mice indicated that SBa-15 has adjuvant potential, and can be considered as an alternative to the use of alum in veterinary vaccines. The use of SBa-15 with HSP70212-600 is also promising as a potential anti-PEP subunit vaccine formulation.

  13. Fabrication of 2 × 8 power splitters in silica-on-silicon by the direct UV writing technique

    DEFF Research Database (Denmark)

    Olivero, Massimo; Svalgaard, Mikael

    2006-01-01

    In this letter, we present the first demonstration of 2 × 8 power splitters made in silica-on-silicon by direct ultraviolet (UV) writing. The fabricated components are compact and exhibit good performance in terms of loss, uniformity, and bandwidth, showing that direct UV writing can become...

  14. Fabrication of BCP/Silica Scaffolds with Dual-Pore by Combining Fused Deposition Modeling and the Particle Leaching Method

    International Nuclear Information System (INIS)

    Sa, Min-Woo; Kim, Jong Young

    2016-01-01

    In recent years, traditional scaffold fabrication techniques such as gas foaming, salt leaching, sponge replica, and freeze casting in tissue engineering have significantly limited sufficient mechanical property and cell interaction effect due to only random pores. Fused deposition modeling is the most apposite technology for fabricating the 3D scaffolds using the polymeric materials in tissue engineering application. In this study, 3D slurry mould was fabricated with a blended biphasic calcium phosphate (BCP)/Silica/Alginic acid sodium salt slurry in PCL mould and heated for two hours at 100 .deg. C to harden the blended slurry. 3D dual-pore BCP/Silica scaffold, composed of macro pores interconnected with micro pores, was successfully fabricated by sintering at furnace of 1100 .deg. C. Surface morphology and 3D shape of dual-pore BCP/Silica scaffold from scanning electron microscopy were observed. Also, the mechanical properties of 3D BCP/Silica scaffold, according to blending ratio of alginic acid sodium salt, were evaluated through compression test

  15. Fabrication of BCP/Silica Scaffolds with Dual-Pore by Combining Fused Deposition Modeling and the Particle Leaching Method

    Energy Technology Data Exchange (ETDEWEB)

    Sa, Min-Woo; Kim, Jong Young [Andong National Univ., Andong (Korea, Republic of)

    2016-10-15

    In recent years, traditional scaffold fabrication techniques such as gas foaming, salt leaching, sponge replica, and freeze casting in tissue engineering have significantly limited sufficient mechanical property and cell interaction effect due to only random pores. Fused deposition modeling is the most apposite technology for fabricating the 3D scaffolds using the polymeric materials in tissue engineering application. In this study, 3D slurry mould was fabricated with a blended biphasic calcium phosphate (BCP)/Silica/Alginic acid sodium salt slurry in PCL mould and heated for two hours at 100 .deg. C to harden the blended slurry. 3D dual-pore BCP/Silica scaffold, composed of macro pores interconnected with micro pores, was successfully fabricated by sintering at furnace of 1100 .deg. C. Surface morphology and 3D shape of dual-pore BCP/Silica scaffold from scanning electron microscopy were observed. Also, the mechanical properties of 3D BCP/Silica scaffold, according to blending ratio of alginic acid sodium salt, were evaluated through compression test.

  16. Fabrication and Characterization of Linear and Nonlinear Photonic Devices in Fused Silica by Femtosecond Laser Writing

    Science.gov (United States)

    Ng, Jason Clement

    Femtosecond laser processing is a flexible, three-dimensional (3D) fabrication technique used to make integrated low-loss photonic devices in fused silica. My work expanded the suite of available optical devices through the design and optimization of linear optical components such as low-loss (70-nm spectral window. My work further complemented femtosecond laser processing with the development of nonlinear device capabilities. While thermal poling is a well known process, significant challenges had restricted the development of nonlinear devices in fused silica. The laser writing process would erase the induced nonlinearity (erasing) while a written waveguide core acted as a barrier to the thermal poling process (blocking). Using second harmonic (SH) microscopy, the effectiveness of thermal poling on laser-written waveguides was systematically analyzed leading to the technique of "double poling", which effectively overcomes the two challenges of erasing and blocking. In this new process the substrate is poled before and after waveguide writing to restore the induced nonlinearity within the vicinity of the waveguide to enable effective poling for inducing a second-order nonlinearity (SON) in fused silica. A new flexible, femtosecond laser based erasure process was also developed to enable quasi-phase matching and to form arbitrarily chirped gratings. Following this result, second harmonic generation (SHG) in a quasiphase-matched (QPM) femtosecond laser written waveguide device was demonstrated. SHG in a chirped QPM structure was also demonstrated to illustrate the flexibility of the femtosecond laser writing technique. These are the first demonstration of frequency doubling in an all-femtosecond-laser-written structure. A maximum SHG conversion efficiency of 1.3 +/- 0.1x10 -11/W-cm-2 was achieved for the fundamental wavelength of 1552.8 nm with a phase-matching bandwidth of 4.4 nm for a 10.0-mm-long waveguide. For a shorter sample, an effective SON of chi(2) = 0

  17. Mesoporous Silica-Supported Sulfonyldiamine Ligand for Microwave-Assisted Transfer Hydrogenation

    Directory of Open Access Journals (Sweden)

    Shaheen M. Sarkar

    2015-01-01

    Full Text Available N-Sulfonyl-1,2-diamine ligands, derived from 1,2-diaminocyclohexane and 1,2-diaminopropane, were immobilized onto mesoporous SBA-15 silica. The SBA-15-supported sulfonyldiamine-Ru complex was prepared in situ under microwave heating at 60 W for 3 min. The prepared sulfonyldiamine-Ru complex was used as an efficient catalyst for the transfer hydrogenation of ketones to the corresponding secondary alcohols. The heterogeneous complex showed extremely high catalytic activity with 99% conversion rate under microwave heating condition. The complexes were regenerated by simple filtration and reused two times without significant loss of activity.

  18. Low-temperature fabrication of mesoporous solid strong bases by using multifunction of a carbon interlayer.

    Science.gov (United States)

    Liu, Xiao-Yan; Sun, Lin-Bing; Liu, Xiao-Dan; Li, Ai-Guo; Lu, Feng; Liu, Xiao-Qin

    2013-10-09

    Mesoporous solid strong bases are highly promising for applications as environmentally benign catalysts in various reactions. Their preparation attracts increasing attention for the demand of sustainable chemistry. In the present study, a new strategy was designed to fabricate strong basicity on mesoporous silica by using multifunction of a carbon interlayer. A typical mesoporous silica, SBA-15, was precoated with a layer of carbon prior to the introduction of base precursor LiNO3. The carbon interlayer performs two functions by promoting the conversion of LiNO3 at low temperatures and by improving the alkali-resistant ability of siliceous host. Only a tiny amount of LiNO3 was decomposed on pristine SBA-15 at 400 °C; for the samples containing >8 wt % of carbon, however, LiNO3 can be entirely converted to strongly basic sites Li2O under the same conditions. The guest-host redox reaction was proven to be the answer for the conversion of LiNO3, which breaks the tradition of thermally induced decomposition. More importantly, the residual carbon layer can prevent the siliceous frameworks from corroding by the newly formed strongly basic species, which is different from the complete destruction of mesostructure in the absence of carbon. Therefore, materials possessing both ordered mesostructure and strong basicity were successfully fabricated, which is extremely desirable for catalysis and impossible to realize by conventional methods. We also demonstrated that the resultant mesoporous basic materials are active in heterogeneous synthesis of dimethyl carbonate (DMC) and the yield of DMC can reach 32.4%, which is apparently higher than that over the catalysts without a carbon interlayer (<12.9%) despite the same lithium content. The strong basicity, in combination with the uniform mesopores, is believed to be responsible for such a high activity.

  19. The polarization modulation and fabrication method of two dimensional silica photonic crystals based on UV nanoimprint lithography and hot imprint.

    Science.gov (United States)

    Guo, Shuai; Niu, Chunhui; Liang, Liang; Chai, Ke; Jia, Yaqing; Zhao, Fangyin; Li, Ya; Zou, Bingsuo; Liu, Ruibin

    2016-10-04

    Based on a silica sol-gel technique, highly-structurally ordered silica photonic structures were fabricated by UV lithography and hot manual nanoimprint efforts, which makes large-scale fabrication of silica photonic crystals easy and results in low-cost. These photonic structures show perfect periodicity, smooth and flat surfaces and consistent aspect ratios, which are checked by scanning electron microscopy (SEM) and atomic force microscopy (AFM). In addition, glass substrates with imprinted photonic nanostructures show good diffraction performance in both transmission and reflection mode. Furthermore, the reflection efficiency can be enhanced by 5 nm Au nanoparticle coating, which does not affect the original imprint structure. Also the refractive index and dielectric constant of the imprinted silica is close to that of the dielectric layer in nanodevices. In addition, the polarization characteristics of the reflected light can be modulated by stripe nanostructures through changing the incident light angle. The experimental findings match with theoretical results, making silica photonic nanostructures functional integration layers in many optical or optoelectronic devices, such as LED and microlasers to enhance the optical performance and modulate polarization properties in an economical and large-scale way.

  20. Polymeric carbon nitride/mesoporous silica composites as catalyst support for Au and Pt nanoparticles.

    Science.gov (United States)

    Xiao, Ping; Zhao, Yanxi; Wang, Tao; Zhan, Yingying; Wang, Huihu; Li, Jinlin; Thomas, Arne; Zhu, Junjiang

    2014-03-03

    Small and homogeneously dispersed Au and Pt nanoparticles (NPs) were prepared on polymeric carbon nitride (CNx )/mesoporous silica (SBA-15) composites, which were synthesized by thermal polycondensation of dicyandiamide-impregnated preformed SBA-15. By changing the condensation temperature, the degree of condensation and the loading of CNx can be controlled to give adjustable particle sizes of the Pt and Au NPs subsequently formed on the composites. In contrast to the pure SBA-15 support, coating of SBA-15 with polymeric CNx resulted in much smaller and better-dispersed metal NPs. Furthermore, under catalytic conditions the CNx coating helps to stabilize the metal NPs. However, metal NPs on CNx /SBA-15 can show very different catalytic behaviors in, for example, the CO oxidation reaction. Whereas the Pt NPs already show full CO conversion at 160 °C, the catalytic activity of Au NPs seems to be inhibited by the CNx support. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Double layer approach to create durable superhydrophobicity on cotton fabric using nano silica and auxiliary non fluorinated materials

    Energy Technology Data Exchange (ETDEWEB)

    Manatunga, Danushika Charyangi [Sri Lanka Institute of Nanotechnology, Nanotechnology & Science Park, Mahenwatte, Pitipana, Homagama (Sri Lanka); Silva, Rohini M. de [Department of Chemistry, University of Colombo, Colombo 03 (Sri Lanka); Nalin de Silva, K.M., E-mail: nalinds@slintec.lk [Sri Lanka Institute of Nanotechnology, Nanotechnology & Science Park, Mahenwatte, Pitipana, Homagama (Sri Lanka); Department of Chemistry, University of Colombo, Colombo 03 (Sri Lanka)

    2016-01-01

    Graphical abstract: - Highlights: • Superhydrophobicity using nonfluorinated agents on cotton roughened with nanosilica. • Sol–gel method to hydrophobize with HDTMS, SA, OTES, and HDTMS/SA HDTMS/OTES hybrids. • WCA of 150° or greater with the treatment. • Increased hydrophobicity and soil repellency obtained when a hybrid mixture is used. • Combinational treatment is effective when compared with the fluorosilane treatment. - Abstract: Creation of differential superhydrophobicity by applying different non-fluorinated hydrophobization agents on a cotton fabric roughened with silica nanoparticles was studied. Cotton fabric surface has been functionalized with silica nanoparticles and further hydrophobized with different hydrophobic agents such as hexadecyltrimethoxy silane (HDTMS), stearic acid (SA), triethoxyoctyl silane (OTES) and hybrid mixtures of HDTMS/SA and HDTMS/OTES. The cotton fabrics before and after the treatment were characterized using scanning electron microscopy (SEM), atomic force microscopy (AFM) and thermogravimetric analysis (TGA). The wetting behavior of cotton samples was investigated by water contact angle (WCA) measurement, water uptake, water repellency and soil repellency testing. The treated fabrics exhibited excellent water repellency and high water contact angles (WCA). When the mixture of two hydrophobization agents such as HDTMS/OTES and HDTMS/SA is used, the water contact angle has increased (145°–160°) compared to systems containing HDTMS, OTES, SA alone (130°–140°). It was also noted that this fabricated double layer (silica + hydrophobization agent) was robust even after applying harsh washing conditions and there is an excellent anti-soiling effect observed over different stains. Therefore superhydrophobic cotton surfaces with high WCA and soil repellency could be obtained with silica and mixture of hydrophobization agents which are cost effective and environmentally friendly when compared with the fluorosilane

  2. The effects of composition and sintering temperature on the silica foam fabricated by slurry method

    International Nuclear Information System (INIS)

    Baharom, Syazwani; Ahmad, Sufizar; Taib, Hariati; Muda, Rizamarhaiza

    2016-01-01

    Reticulated ceramic or open pore ceramic foam is a well-known material which exhibits extremely high porosities, with a significant degree of interconnectivity that makes them desirable in a wide range of applications. There were broad types of ceramic foam fabrication method such as polymeric sponge method, direct foaming, and starch consolidation. In this study, the slurry method has been chosen to fabricate Silica (SiO_2) foam. In this process, Polyurethane (PU) foam template was dipped into ceramic slurry and followed by drying and sintering to obtain foam which contains porosity in the range of 50% to 70%. The compositions of SiO_2 were varied starting from 55 wt.%, 60 wt.%, 65 wt.% and 70 wt.%. The samples of SiO_2 that have been dipped and dried were sintered at 900°C, 1000°C, 1100°C, and 1250°C. The sintered SiO_2 ceramic foam samples were characterized to observe their morphology, and physical properties. Thus, the microstructure of the SiO_2 ceramic foams samples was examined by Scanning Electron Microscopy (SEM), and Electron Dispersive Spectroscopy (EDS). Meanwhile, the physical properties of the SiO_2 ceramic foam samples such as the total porosity (%) and bulk density were determined using Archimedes method. It was found that the density of ceramic foam produced was in the range of 0.25 g/cm"3 up to 0.75 g/cm"3, whereas the level of porosity percentage was in the range of 61.81% to 82.18% with the size of open pore or window cells were in between 141 µm up to 626 µm.

  3. The effects of composition and sintering temperature on the silica foam fabricated by slurry method

    Energy Technology Data Exchange (ETDEWEB)

    Baharom, Syazwani, E-mail: hd140001@siswa.uthm.edu.my; Ahmad, Sufizar, E-mail: sufizar@uthm.edu.my; Taib, Hariati, E-mail: hariati@uthm.edu.my; Muda, Rizamarhaiza, E-mail: hd130013@siswa.uthm.edu.my [Department of Material and Design Engineering, Faculty of Mechanical and Manufacturing Engineering, Universiti Tun Hussein Onn Malaysia (UTHM), 86400 Parit Raja, Batu Pahat, Johor (Malaysia)

    2016-07-19

    Reticulated ceramic or open pore ceramic foam is a well-known material which exhibits extremely high porosities, with a significant degree of interconnectivity that makes them desirable in a wide range of applications. There were broad types of ceramic foam fabrication method such as polymeric sponge method, direct foaming, and starch consolidation. In this study, the slurry method has been chosen to fabricate Silica (SiO{sub 2}) foam. In this process, Polyurethane (PU) foam template was dipped into ceramic slurry and followed by drying and sintering to obtain foam which contains porosity in the range of 50% to 70%. The compositions of SiO{sub 2} were varied starting from 55 wt.%, 60 wt.%, 65 wt.% and 70 wt.%. The samples of SiO{sub 2} that have been dipped and dried were sintered at 900°C, 1000°C, 1100°C, and 1250°C. The sintered SiO{sub 2} ceramic foam samples were characterized to observe their morphology, and physical properties. Thus, the microstructure of the SiO{sub 2} ceramic foams samples was examined by Scanning Electron Microscopy (SEM), and Electron Dispersive Spectroscopy (EDS). Meanwhile, the physical properties of the SiO{sub 2} ceramic foam samples such as the total porosity (%) and bulk density were determined using Archimedes method. It was found that the density of ceramic foam produced was in the range of 0.25 g/cm{sup 3} up to 0.75 g/cm{sup 3}, whereas the level of porosity percentage was in the range of 61.81% to 82.18% with the size of open pore or window cells were in between 141 µm up to 626 µm.

  4. Solution-processable precursor route for fabricating ultrathin silica film for high performance and low voltage organic transistors

    Institute of Scientific and Technical Information of China (English)

    Shujing Guo; Liqiang Li; Zhongwu Wang; Zeyang Xu; Shuguang Wang; Kunjie Wu; Shufeng Chen; Zongbo Zhang; Caihong Xu; Wenfeng Qiu

    2017-01-01

    Silica is one of the most commonly used materials for dielectric layer in organic thin-film transistors due to its excellent stability,excellent electrical properties,mature preparation process,and good compatibility with organic semiconductors.However,most of conventional preparation methods for silica film are generally performed at high temperature and/or high vacuum.In this paper,we introduce a simple solution spin-coating method to fabricate silica thin film from precursor route,which possesses a low leakage current,high capacitance,and low surface roughness.The silica thin film can be produced in the condition of low temperature and atmospheric environment.To meet various demands,the thickness of film can be adjusted by means of preparation conditions such as the speed of spin-coating and the concentration of solution.The p-type and n-type organic field effect transistors fabricated by using this film as gate electrodes exhibit excellent electrical performance including low voltage and high performance.This method shows great potential for industrialization owing to its characteristic of low consumption and energy saving,time-saving and easy to operate.

  5. Fabrication of robust and thermally stable superhydrophobic nanocomposite coatings based on thermoplastic polyurethane and silica nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Seyfi, Javad [School of Chemical Engineering, University of Tehran, P.O. Box 11155-4563, Tehran (Iran, Islamic Republic of); Jafari, Seyed Hassan, E-mail: shjafari@ut.ac.ir [School of Chemical Engineering, University of Tehran, P.O. Box 11155-4563, Tehran (Iran, Islamic Republic of); Khonakdar, Hossein Ali [Leibniz-Institut für Polymerforschung Dresden e.V., Hohe Strasse 6, D-01069 Dresden (Germany); Sadeghi, Gity Mir Mohamad [Department of Polymer Engineering & Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Zohuri, Gholamhossein [Polymer Group, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of); Hejazi, Iman [Department of Polymer Engineering & Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Simon, Frank [Leibniz-Institut für Polymerforschung Dresden e.V., Hohe Strasse 6, D-01069 Dresden (Germany)

    2015-08-30

    Highlights: • Superhydrophobic coatings were prepared from an intrinsically hydrophilic polymer. • The superhydrophobicity remained intact at elevated temperatures. • Polyurethane plays a key role in improving the mechanical robustness of the coatings. • A complete surface coverage of nanosilica is necessary for superhydrophobicity. - Abstract: In this paper, superhydrophobic nanocomposite coatings based on thermoplastic polyurethane (TPU) and modified nanosilica were fabricated using a simple solution-based method. The main challenge was to impart superhydrophobicity to an intrinsically hydrophilic polymer substrate. The prepared nanocomposite coatings were characterized by means of scanning electron microscopy, confocal microscopy and X-ray photoelectron spectroscopy. Based on the obtained results, it was proved that in order to achieve superhydrophobicity, no TPU macromolecule should be present on the coating's top layer, thus a complete coverage of coating's top layer by nanosilica particles was necessary for achieving ultra water repellent coatings. Mechanical and thermal resistance of the coatings, which are the main challenges in commercializing superhydrophobic surfaces, were also studied by drop impact and thermal annealing tests, respectively. It was proved that using TPU as a sublayer results in improving mechanical resistance of the coatings as compared with the pure silica nanocoating. Moreover, the samples showed an excellent resistance against elevated temperatures (150 °C) and remained superhydrophobic; however, further increment of the annealing temperatures to 200 °C caused the TPU macromolecules to migrate onto the top layer of the coatings significantly reducing the water repellency, which was visually proved by SEM.

  6. Fabrication of robust and thermally stable superhydrophobic nanocomposite coatings based on thermoplastic polyurethane and silica nanoparticles

    Science.gov (United States)

    Seyfi, Javad; Jafari, Seyed Hassan; Khonakdar, Hossein Ali; Sadeghi, Gity Mir Mohamad; Zohuri, Gholamhossein; Hejazi, Iman; Simon, Frank

    2015-08-01

    In this paper, superhydrophobic nanocomposite coatings based on thermoplastic polyurethane (TPU) and modified nanosilica were fabricated using a simple solution-based method. The main challenge was to impart superhydrophobicity to an intrinsically hydrophilic polymer substrate. The prepared nanocomposite coatings were characterized by means of scanning electron microscopy, confocal microscopy and X-ray photoelectron spectroscopy. Based on the obtained results, it was proved that in order to achieve superhydrophobicity, no TPU macromolecule should be present on the coating's top layer, thus a complete coverage of coating's top layer by nanosilica particles was necessary for achieving ultra water repellent coatings. Mechanical and thermal resistance of the coatings, which are the main challenges in commercializing superhydrophobic surfaces, were also studied by drop impact and thermal annealing tests, respectively. It was proved that using TPU as a sublayer results in improving mechanical resistance of the coatings as compared with the pure silica nanocoating. Moreover, the samples showed an excellent resistance against elevated temperatures (150 °C) and remained superhydrophobic; however, further increment of the annealing temperatures to 200 °C caused the TPU macromolecules to migrate onto the top layer of the coatings significantly reducing the water repellency, which was visually proved by SEM.

  7. Synthesis and structure of pyridine-functionalized mesoporous SBA-15 organosilicas and their application for sorption of diclofenac

    Science.gov (United States)

    Barczak, Mariusz

    2018-02-01

    A series of pyridine-functionalized mesoporous silicas have been prepared for the first time via direct co-condensation of tetraethoxysilane (TEOS) and 2-(2-pyridyl)ethyltrimethoxysilane (PETS) using the block copolymer Pluronic P123 as a structure-directing agent. The obtained materials were fully characterized by a wide range of instrumental techniques and employed as adsorbents for the removal of a diclofenac which is considered a priority hazardous drug. The synthesized materials exhibit a high adsorption capacities and rapid adsorption rates. The structural and adsorption properties depend largely on the relative amount of PETS/TEOS ratio: the gradual degradation of ordered structure and porosity was observed with the increasing amount of PETS. However due to the highest loading of pyridine units the most structurally degraded material had the highest adsorption uptake (631 mg g-1) indicating that the surface chemistry plays - along with porosity - an important role in governing the adsorption process. The experimental adsorption data were modelled using the Langmuir, Freundlich and Langmuir-Freundlich isotherms - among them the Langmuir-Freundlich model turned out to be the most suitable for describing adsorption behaviour of diclofenac onto the materials. The collected data show that the pyridine-functionalized mesoporous silicas can be a promising absorbent of pharmaceuticals.

  8. FABRICATION AND CHARACTERIZATION OF POLYIMIDE/POLYETHERSULFONE-FUMED SILICA MIXED MATRIX MEMBRANE FOR GAS SEPARATION

    Directory of Open Access Journals (Sweden)

    A. F. Ismail

    2012-01-01

    Full Text Available This study is performed primarily to investigate the feasibility of fumed silica as inorganic material towards gas separation performance of mixed matrix membrane. In this study, polyimide/polyethersulfone (PES-fumed silica mixed matrix membranes were casted using dry/wet technique. The results from the FESEM, DSC and FTIR analysis confirmed that the structure and physical properties of membrane is influenced by inorganic filler. FESEM’s cross-section view indicated good compatibility between polymer and fumed silica for all of range fumed silica used in this study. The gas separation performance of the mixed matrix membranes with fumed silica were relatively higher compared to that of the neat PI/PES membrane. PI/PES-fumed silica 5 wt% yielded significant selectivity enhancement of 7.21 and 40.47 for O2/N2, and CO2/CH4, respectively.

  9. Covalent immobilization of lipase onto chitosan-mesoporous silica hybrid nanomaterials by carboxyl functionalized ionic liquids as the coupling agent.

    Science.gov (United States)

    Xiang, Xinran; Suo, Hongbo; Xu, Chao; Hu, Yi

    2018-05-01

    Chitosan-mesoporous silica SBA-15 hybrid nanomaterials (CTS-SBA-15) were synthesized by means of carboxyl functionalized ionic liquids as the coupling agent. The as-prepared CTS-SBA-15 support was characterized by TEM, FTIR, TG and nitrogen adsorption-desorption techniques. Porcine pancreas lipase (PPL) was then bound to the hybrid nanomaterials by using the cross-linking reagent glutaraldehyde (GA). Further, the parameters like cross-linking concentration, time and ratio of supports to enzyme were optimized. The property of immobilized lipase were tested in detail by enzyme activity assays. The results indicated that the hybrid nanomaterials could form three-dimensional (3D) structure with homogeneous mesoporous structures and immobilized PPL revealed excellent enzymatic performance. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Thiol-Functionalized Mesoporous Silica for Effective Trap of Mercury in Rats

    Directory of Open Access Journals (Sweden)

    Wei Zhao

    2016-01-01

    Full Text Available The chance of exposure to heavy metal for human being rises severely today due to the increasing water contamination and air pollution. Here, we prepared a series of thiol-functionalized mesoporous silica as oral formulation for the prevention and treatment of heavy metal poisoning. The successful incorporation of thiol was verified by the FTIR spectra. SBA15-SH-10 was used for the study as it is of uniform mesopores and fine water dispersibility. In simulated gastrointestinal fluid, the thiol-functionalized mesoporous silica can selectively capture heavy metal, showing a very high affinity for inorganic mercury (II. The blood and urine mercury levels of rats fed with a diet containing Hg (II and material were significantly lower than those of rats fed with the metal-rich diet only. On the contrary, the mercury content in fecal excretion of the treatment group increased more than twice as much as that of the control group. This result indicated that SBA15-SH-10 could effectively remove mercury (II in vivo and the mercury loaded on SBA15-SH-10 would be excreted out. Hence, SBA15-SH-10 has potential application in preventing and treating heavy metal poisoning via digestive system.

  11. Insight into the adsorption of tetracycline onto amino and amino-Fe3+ gunctionalized mesoporous silica: Effect of functionalized groups.

    Science.gov (United States)

    Zhang, Ziyang; Li, Haiyan; Liu, Huijuan

    2018-03-01

    In order to study the influences of functionalized groups onto the adsorption of tetracycline, we prepared a series of amino and amino-Fe 3+ complex mesoporous silica adsorbents with diverse content of amino and Fe 3+ groups (named N,N-SBA15 and Fe-N,N-SBA15). The resulting mesoporous silica adsorbents were fully characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectrometer (FTIR) and N 2 adsorption/desorption isotherms. Furthermore, the effects of functionalized groups on the removal of TC were investigated. The results showed that the periodic ordered structure of SBA-15 was maintained after modification of amino/Fe 3+ groups. The functionalized amino groups decreased the adsorption capacity while the coordinated Fe 3+ increased the adsorption capacity. The adsorption kinetics of TC fitted pseudo-second-order model well and the equilibrium was achieved quickly. The adsorption isotherms fitted the Langmuir model well and with the Fe 3+ content increased from 3.93% to 8.26%, the Q max of the adsorbents increased from 102 to 188mmol/kg. The solution pH affected the adsorption of TC onto amino complex adsorbents slightly while influenced the adsorption onto Fe-amine complex adsorbents greatly. The adsorption of TC on SBA15 and N,N-SBA15 may be related to the formation of outer-sphere surface complexes, while the adsorption of TC onto Fe-N,N-SBA15 was mainly attributed to the inner-sphere surface complexes. This study could offer potential materials that have excellent adsorption behavior for environmental remediation and suggested useful information for the preparing other adsorbents in environmental applications. Copyright © 2017. Published by Elsevier B.V.

  12. Space-confined preparation of high surface area tungsten oxide and tungsten nitride inside the pores of mesoporous silica SBA-15

    DEFF Research Database (Denmark)

    Meyer, Simon; Beyer, Hans; Köhler, Klaus

    2015-01-01

    For the direct preparation of high surface area nitride materials, a lack of suitable precursors exists. Indirect preparation by gas phase nitridation (e.g. by ammonia) requires high temperatures and often results in sintering. The present work demonstrates that the space-confined preparation of ...

  13. Fabrication of semi-transparent super-hydrophobic surface based on silica hierarchical structures

    KAUST Repository

    Chen, Ping-Hei

    2011-01-01

    This study successfully develops a versatile method of producing superhydrophobic surfaces with micro/nano-silica hierarchical structures on glass surfaces. Optically transparent super hydrophobic silica thin films were prepared by spin-coating silica particles suspended in a precursor solution of silane, ethanol, and H2O with molar ratio of 1:4:4. The resulting super hydrophobic films were characterized by scanning electron microscopy (SEM), optical transmission, and contact angle measurements. The glass substrates in this study were modified with different particles: micro-silica particles, nano-silica particles, and hierarchical structures. This study includes SEM micrographs of the modified glass surfaces with hierarchical structures at different magnifications. © 2011 The Korean Society of Mechanical Engineers and Springer-Verlag Berlin Heidelberg.

  14. Alizarin red S functionalized mesoporous silica modified glassy carbon electrode for electrochemical determination of anthracene

    International Nuclear Information System (INIS)

    Liu, Shan; Wei, Maochao; Zheng, Xiangli; Xu, Shuai; Xia, Fangquan; Zhou, Changli

    2015-01-01

    Highlights: • Alizarin red S-SBA15 composite was prepared and characterized. • A novel sensing platform was constructed for anthracene determination. • The proposed sensor exhibited high sensitivity and low detection limit for detecting anthracene. • This method can be applied to the practical detection of anthracene in waste water. - Abstract: In the paper, a novel and sensitive electrochemical sensor based on modification of electroactive alizarin red S functionalized mesoporous silica material SBA15 onto glassy carbon electrode (ARS-SBA15/GCE) was developed. Alizarin red S, called electrochemical probe that can selectively recognize polycyclic aromatic hydrocarbons (PAHs), as tools for the detection of tricyclic aromatic hydrocarbon anthracene. The morphology and interface property of ARS modified SBA15 (ARS-SBA15) were examined by transmission electron microscopy (TEM) and fourier transform infrared spectroscopy (FTIR). Taking advantage of the π-π stacking force between alizarin red S and anthracene, the ARS-SBA15/GCE sensor could detect anthracene quantitatively in a wide range of 1.0 pM–10.0 nM and a low detection limit of 0.5 pM (S/N = 3). Other PAHs, such as naphthalene, phenanthrene, pyrene, and benzo[a]pyrene show little interference on the detection. Consequently, a simple and sensitive electrochemical method was proposed for the determination of anthracene, which can be used to determine anthracene in waste water samples. The electrochemical method provides a general tool that complements the commonly used spectroscopic methods and immune method for the detection of PAHs

  15. Mesoporous silica particles modified with graphitic carbon: interaction with human red blood cells and plasma proteins

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, Diego Stefani Teodoro; Franqui, Lidiane Silva; Bettini, Jefferson; Strauss, Mathias, E-mail: diego.martinez@lnnano.cnpem.br [Centro Nacional de Pesquisa em Energia e Materiais (CNPEM), Campinas, SP (Brazil); Damasceno, Joao Paulo Vita; Mazali, Italo Odone [Universidade Estadual de Campinas (UNICAMP), SP (Brazil)

    2016-07-01

    Full text: In this work the interaction of the mesoporous silica particles (SBA-15, ∼700 nm) modified with graphitic carbon (SBA-15/C) on human red blood cells (hemolysis) and plasma proteins (protein corona formation) is studied. XPS and CHN analysis showed that the carbon content on the SBA-15/C samples varied from 2 to 10% and was tuned by the functionalization step. The formed carbon structures where associated to graphitic nanodomains coating the pores surface as verified by Raman spectroscopy and {sup 13}C NMR. Advanced TEM/EELS analysis showed that the carbon structures are distributed along the SBA-15 mesopores. SAXS and textural analyses were used to confirm that the porous structure of the silica support is kept after the modification procedure and to calculate the number of graphitic carbon stacked layers coating the mesopores. After incubation of SBA-15 with human red blood cells (RBCs), it was observed a dose-dependent hemolytic effect, probably, due to binding of the material silanol-rich surface to the phosphatidylcholine molecules from the RBC membrane. The graphitic carbon modifications have mitigated this effect, indicating that the graphitic carbon coating protected the silanol groups of the particle surface hindering the hemolysis. Considering the protein corona formation, selective biomolecular interaction of proteins was observed for the different materials using gel electrophoresis (SDS-PAGE) analysis. Besides, graphitic carbon modification decreased the amount of proteins on the corona. Together, the in vitro hemolysis and protein corona assays are promising biological models to understand the influence of silica surface functionalization on their bionano-interactions. Finally, our work contributes to the development of fundamental research on such nanomaterials chemistry in the emerging field of nanobioscience and nanotoxicology. (author)

  16. Fabrication of Mesoporous Silica/Alumina Hybrid Membrane Film Nanocomposites using Template Sol-Gel Synthesis of Amphiphilic Triphenylene

    Science.gov (United States)

    Lintang, H. O.; Jalani, M. A.; Yuliati, L.; Salleh, M. M.

    2017-05-01

    Herein we reported that by introducing a one-dimensional (1D) substrate with a porous structure such as anodic aluminum oxide (AAO) membrane, mesoporous silica/alumina hybrid nanocomposites were successfully fabricated by using amphiphilic triphenylene (TPC10TEG) as a template in sol-gel synthesis (TPC10TEG/silicahex). For the optical study of the nanocomposites, TPC10TEG/silicahex showed absorption peak at 264 nm due to the ordered and long-range π-π stacking of the disc-like aromatic triphenylene core. Moreover, the hexagonal arrangement of TPC10TEG/silicahex was proven based on their diffraction peaks of d 100 and d 200 at 2θ = 2.52° and 5.04° and images of transmission electron microscopy (TEM), respectively. For fabrication of mesoporous silica/alumina hybrid membrane, TPC10TEG/silicahex was drop-casted onto AAO membrane for penetration into the porous structure via gravity. X-ray diffraction (XRD) analysis on the resulted hybrid nanocomposites showed that the diffraction peaks of d 100 and d 200 of TPC10TEG/silicahex were still preserved, indicating that the hexagonal arrangements of mesoporous silica were maintained even on AAO substrate. The morphology study on the hybrid nanocomposites using TEM, scanning electron microscope (SEM) and field emission scanning electron microscope (FE-SEM) showed the successful filling of most AAO channels with the TPC10TEG/silicahex nanocomposites.

  17. Amine-modified ordered mesoporous silica: Effect of pore size on carbon dioxide capture

    Energy Technology Data Exchange (ETDEWEB)

    V. Zelenak; M. Badanicova; D. Halamova; J. Cejka; A. Zukal; N. Murafa; G. Goerigk [P.J. Safarik University, Kosice (Slovak Republic)

    2008-10-15

    Three mesoporous silica materials with different pore sizes and pore connectivity were prepared and functionalized with aminopropyl (AP) ligands by post-synthesis treatment. The materials were characterized by small angle X-ray scattering (SAXS), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and nitrogen adsorption/desorption experiments. The carbon dioxide sorption on modified mesoporous molecular sieves was investigated by using of microbalances at 25{sup o}C, and the influence of pore size and pore architecture on CO{sub 2} sorption was discussed. The large pore silica, SBA-15, showed the largest carbon dioxide sorption capacity (1.5 mmol/g), relating to highest amine surface density in this material. On the other hand, three-dimensional accessibility of amine sites inside the pores of SBA-12 silica resulted in a faster response to CO{sub 2} uptake in comparison with MCM-41 and SBA-15 molecular sieves

  18. Direct esterification of olive-pomace oil using mesoporous silica supported sulfonic acids

    Directory of Open Access Journals (Sweden)

    F. Alrouh

    2017-02-01

    Full Text Available Mesoporous silica MCM-41 and SBA-15 containing propyl sulfonic acid groups were synthesized according to the literature and were characterized by X-ray diffraction, N2 adsorption and the H+ exchange capacities of the sulfonic acid groups were titrated. The esterification reaction of glycerol with olive-pomace oil has been carried out by using prepared functionalized mesoporous silica (MCM-41 and SBA-15 as catalysts. It has been monitored by GC two fatty acids (palmitic and oleic acids as reactants in olive-pomace oil and their related monoacylglycerols (Glycerol monopalmitate GMP and monooleate GMO as reaction product. The catalytic activities of the functionalized mesoporous silica were compared with commercial catalysts, these included homogeneous catalysts (p-toluenesulfonic acid and heterogeneous catalysts (Amberlyst-15. The total yield of monoacylglycerols (GMO + GMP was nearly 40%. Remarkably, we found that MCM-41-SO3H was recycled at least 3 times without any loss of activity.

  19. Fabrication of mesoporous silica nanoparticles by sol gel method followed various hydrothermal temperature

    Science.gov (United States)

    Purwaningsih, Hariyati; Pratiwi, Vania Mitha; Purwana, Siti Annisa Bani; Nurdiansyah, Haniffudin; Rahmawati, Yenny; Susanti, Diah

    2018-04-01

    Rice husk is an agricultural waste that is potentially used as natural silica resources. Natural silica claimed to be safe in handling, cheap and can be generate from cheap resource. In this study mesoporous silica was synthesized using sodium silicate extracted from rice husk ash. This research's aim are to study the optimization of silica extraction from rice husk, characterizing mesoporous silica from sol-gel method and surfactant templating from rice husk and the effect of hydrothermal temperature on mesoporous silica nanoparticle (MSNp) formation. In this research, rice husk was extracted with sol-gel method and was followed by hydrothermal treatment; several of hydrothermal temperatures were 85°C, 100°C, 115°C, 130°C and 145° for 24 hours. X-ray diffraction analysis was identified of α-SiO2 phase and NaCl compound impurities. Scherer's analysis method for crystallite size have resulted 6.27-40.3 nm. FTIR results of silica from extraction and MSNp indicated Si-O-Si bonds on the sample. SEM result showed the morphology of the sample that has spherical shape and smooth surface. TEM result showed particle size ranged between 69,69-84,42 nm. BET showed that the pore size classified as mesoporous with pore diameter size is 19,29 nm.

  20. A novel approach to fabrication of superparamagnetite hollow silica/magnetic composite spheres

    Energy Technology Data Exchange (ETDEWEB)

    Yuan Junjie, E-mail: yuanjunjie@tongji.edu.c [School of Materials Science and Engineering, Tongji University, Shanghai 200092 (China); Key Laboratory of Molecular Engineering of Polymers, Fudan University, Shanghai 200433 (China); Zhang Xiong; Qian He [School of Materials Science and Engineering, Tongji University, Shanghai 200092 (China)

    2010-08-15

    We described a method for synthesizing hollow silica/magnetic composite spheres using sulfonic acid functionalized hollow silica spheres (SAFHSS) as templates. The Fe{sub 3}O{sub 4} nanoparticles were deposited on or imbedded in the hollow silica shell by a precipitation reaction. The morphologies, composition and properties of the hollow composite spheres were characterized by transmission electron microscopy, Fourier transform infrared analysis, X-ray diffraction measurement and vibrating-sample magnetometry measurement. The results indicated crystal sizes and amount of the Fe{sub 3}O{sub 4} nanoparticles on the SAFHSS. The magnetic properties of the hollow composite spheres were controlled by adjusting the proportion between Fe{sup 2+} and Fe{sup 3+} and iron ion total concentration. When appropriate loading species were added into the system, superparamagnetite hollow composite spheres were obtained. The method also could be applicable to prepare other superparamagnetite hollow silica/ferrite composite spheres.

  1. Room Temperature Imprint Using Crack-Free Monolithic SiO2-PVA Nanocomposite for Fabricating Microhole Array on Silica Glass

    Directory of Open Access Journals (Sweden)

    Shigeru Fujino

    2015-01-01

    Full Text Available This paper aims to fabricate microhole arrays onto a silica glass via a room temperature imprint and subsequent sintering by using a monolithic SiO2-poly(vinyl alcohol (PVA nanocomposite as the silica glass precursor. The SiO2-PVA suspension was prepared from fumed silica particles and PVA, followed by drying to obtain tailored SiO2-PVA nanocomposites. The dependence of particle size of the fumed silica particles on pore size of the nanocomposite was examined. Nanocomposites prepared from 7 nm silica particles possessed suitable mesopores, whereas the corresponding nanocomposites prepared from 30 nm silica particles hardly possessed mesopores. The pore size of the nanocomposites increased as a function of decreasing pH of the SiO2-PVA suspension. As a consequence, the crack-free monolithic SiO2-PVA nanocomposite was obtained using 7 nm silica particles via the suspension at pH 3. Micropatterns were imprinted on the monolithic SiO2-PVA nanocomposite at room temperature. The imprinted nanocomposite was sintered to a transparent silica glass at 1200°C in air. The fabricated sintered glass possessed the microhole array on their surface with aspect ratios identical to the mold.

  2. Properties of CdSe quantum dots coated with silica fabricated in a facile way

    International Nuclear Information System (INIS)

    Liao Yufeng; Li Wenjiang; He Sailing

    2007-01-01

    High quality quantum dots (QDs) CdSe were prepared using a novel and non-TOP method. Quantum dots of different sizes ranging from 2 to 4 nm could be obtained by removing aliquots of the reaction solution at different time intervals or by adjusting some reaction conditions. The CdSe quantum dots (core) were directly coated with silica (shell) using a microemulsion method. The design and preparation of a model QD/silica was described and characterized using transmission electron microscopy (TEM), UV-vis absorption, photoluminescence and laser confocal scanning microscopy. TEM images confirmed the well-monodispersed QDs and the silica shell around the CdSe core, respectively; laser confocal microscope images, UV-vis absorption and photoluminescence spectra clearly indicated that both the original QDs and the silica-coated QDs had good fluorescence properties. The quantum dots coated with silica shells were stable, water-soluble and less toxic (due to the silica shells), and are anticipated to be used as fluorescent probes for biosensing and imaging applications

  3. Generation of Well-Defined Pairs of Silylamine on Highly Dehydroxylated SBA-15: Application to the Surface Organometallic Chemistry of Zirconium

    KAUST Repository

    Azzi, Joachim

    2012-11-01

    Design of a new well-defined surface organometallic species [O-(=Si–NH)2Zr(IV)Np2] has been obtained by reaction of tetraneopentyl zirconium (ZrNp4) on SBA-15 surface displaying mainly silylamine pairs [O-(=Si–NH2)2]. These surface species have been achieved by an ammonia treatment of a highly dehydroxylated SBA-15 at 1000°C (SBA-151000). This support is known to contain mainly strained reactive siloxane bridges (≡Si-O-Si≡)[1] along with a small amount of isolated plus germinal silanols =Si(OH)2. Chemisorption of ammonia occurs primarily by opening these siloxane bridges[2] to generate silanol/silylamine pairs [O-(=Si–NH2)(=SiOH)] followed by substitution of the remaining silanol. Further treatment using hexamethyldisilazane (HMDS) results in the protection of the isolated remaining silanol groups by formation of ≡Si-O-SiMe3 and =Si(OSiMe3)2 but leaves ≡SiNH2 untouched. After reaction of this functionalized surface with ZrNp4, this latter displays mainly a bi-podal zirconium neopentyl organometallic complex [O-(=Si–NH)2Zr(IV)Np2] which has been fully characterized by diverse methods such as infrared transmission spectroscopy, magic angle spinning solid state nuclear magnetic resonance, surface elemental analysis, small angle X-ray powder diffraction (XRD), nitrogen adsorption and energy filtered transmission electron microscopy (EFTEM). These different characterization tools unambiguously prove that the zirconium organometallic complex reacts mostly with silylamine pairs to give a bi-podal zirconium bis-neopentyl complex, uniformly distributed into the channels of SBA-151000. Therefore this new material opens a new promising research area in Surface Organometallic Chemistry which, so far, was dealing mainly with O containing surface. It is expected that vicinal amine functions may play a very different role as compared with classical inorganic supports. Given the importance in the last decades of N containing ligands in catalysis, one may expect

  4. Mesoporous silica as carrier of antioxidant for food packaging materials

    Science.gov (United States)

    Buonocore, Giovanna Giuliana; Gargiulo, Nicola; Verdolotti, Letizia; Liguori, Barbara; Lavorgna, Marino; Caputo, Domenico

    2014-05-01

    Mesoporous silicas have been long recognized as very promising materials for the preparation of drug delivery systems. In this work SBA-15 mesoporous silica has been functionalized with amino-silane to be used as carrier of antioxidant compound in the preparation of active food packaging materials exhibiting tailored release properties. Active films have been prepared by loading the antioxidant tocopherol, the purely siliceous SBA-15 and the aminofunctionalized SBA-15 loaded with tocopherol into LDPE matrix trough a two-step process (mixing+extrusion). The aim of the present work is the study of the effect of the pore size and of the chemical functionality of the internal walls of the mesophase on the migration of tocopherol from active LDPE polymer films. Moreover, it has been proved that the addition of the active compound do not worsen the properties of the film such as optical characteristic and water vapor permeability, thus leading to the development of a material which could be favorably used mainly, but not exclusively, in the sector of food packaging.

  5. Enhancement of Ag-Based Plasmonic Photocatalysis in Hydrogen Production from Ammonia Borane by the Assistance of Single-Site Ti-Oxide Moieties within a Silica Framework.

    Science.gov (United States)

    Verma, Priyanka; Kuwahara, Yasutaka; Mori, Kohsuke; Yamashita, Hiromi

    2017-03-13

    Ag nanoparticles (NPs) have gained great attention owing to their interesting plasmonic properties and efficient catalysis under visible-light irradiation. In this study, an Ag-based plasmonic catalyst supported on mesoporous silica with isolated and tetrahedrally coordinated single-site Ti-oxide moieties, namely, Ag/Ti-SBA-15, was designed with the purpose of utilizing the broad spectral range of solar energy. The Ti-SBA-15 support allows the deposition of small Ag NPs with a narrow size distribution. The chemical structure, morphology, and optical properties of the prepared catalyst were characterized by techniques such as UV/Vis, FT extended X-ray absorption fine structure, and X-ray photoelectron spectroscopy, field-emission SEM, TEM, and N 2 physisorption studies. The catalytic activity of Ag/Ti-SBA-15 in hydrogen production from ammonia borane by hydrolysis was significantly enhanced in comparison with Ag/SBA-15 without Ti-oxide moieties and Ag/TiO 2 /SBA-15 involving agglomerated TiO 2 , both in the dark and under light irradiation. Improved electron transfer under light irradiation caused by the creation of heterojunctions between Ag NPs and Ti-oxide moieties explains the results obtained in the present study. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Fabrication of poly(o-anisidine) coated silica core-shell microspheres and their electrorheological response

    Science.gov (United States)

    Lee, Chul Joo; Choi, Hyoung Jin

    2017-11-01

    In this work, silica/poly(o-anisidine) (POA) core-shell structured microspheres were synthesized by coating the silica core surface with POA with a help of a chemical grafting agent, N-[(3-trimethoxylsilyl)-propyl] aniline. The synthesized silica microspheres were then applied as a polymer/inorganic composite particle-based electrorheological (ER) fluid. The morphology of the silica/POA microspheres was examined by using both transmission electron microscopy and scanning electron microscopy, while their thermal properties and chemical structure were checked by thermogravimetric analysis and Fourier-transform infrared spectroscopy, respectively. The ER properties of the silica/POA particle-based ER fluid were examined by using a Couette-type rotational rheometer equipped with a high-voltage power supplier and analyzed by the Bingham model and modified Mason number. In order to obtain additional information about the electrical polarization properties, the dielectric spectra were measured by an LCR meter and fitted by using the Cole-Cole equation. Furthermore, suspension stability of the ER fluid was tested using Turbiscan.

  7. Fabrication of silica hollow particles using yeast cells as a template

    Science.gov (United States)

    Liao, Shenglan; Lin, Liqin; Chen, Xiaofang; Liu, Jingru; Zhang, Biao

    2018-04-01

    Inorganic hollow particles have attracted great interest in recent years. In this study, silica micro spheres were produced. Yeast cells were used as a biological template. The silica shell was synthesized by the hydrolysis of tetraethoxysilane (TEOS) in water-alcohol mixtures as solvent using ammonia as a catalyst according to the Stoeber process. Various approaches including X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the products. The results showed that the thermally treated samples were SiO2 hollow microspheres with a diameter varying between 1-5μm.

  8. Facile fabrication of nano-structured silica hybrid film with superhydrophobicity by one-step VAFS approach

    Science.gov (United States)

    Jia, Yi; Yue, Renliang; Liu, Gang; Yang, Jie; Ni, Yong; Wu, Xiaofeng; Chen, Yunfa

    2013-01-01

    Here we report a novel one-step vapor-fed aerosol flame synthesis (VAFS) method to attain silica hybrid film with superhydrophobicity on normal glass and other engineering material substrates using hexamethyldisiloxane (HMDSO) as precursor. The deposited nano-structured silica films represent excellent superhydrophobicity with contact angle larger than 150° and sliding angle below 5°, without any surface modification or other post treatments. SEM photographs proved that flame-made SiO2 nanoparticles formed dual-scale surface roughness on the substrates. It was confirmed by FTIR and XPS that the in situ formed organic fragments on the particle surface as species like (CH3)xSiO2-x/2 (x = 1, 2, 3) which progressively lowered the surface energy of fabricated films. Thus, these combined dual-scale roughness and lowered surface energy cooperatively produced superhydrophobic films. IR camera had been used to monitor the real-time flame temperature. It is found that the inert dilution gas inflow played a critical role in attaining superhydrophobicity due to its cooling and anti-oxidation effect. This method is facile and scalable for diverse substrates, without any requirement of complex equipments and multiple processing steps. It may contribute to the industrial fabrication of superhydrophobic films.

  9. Optical oxygen sensing materials based on a novel dirhenium(I) complex assembled in mesoporous silica

    International Nuclear Information System (INIS)

    Liu Yanhong; Li Bin; Cong Yan; Zhang Liming; Fan Di; Shi Linfang

    2011-01-01

    A new dirhenium(I) complex fac-[{Re(CO) 3 (4,7-dinonadecyl-1,10-phenanthro -line)} 2 (4,4'-bipyridyl)] (trifluoromethanesulfonate) 2 (denoted as D-Re(I) ) is assembled in MCM-41 and SBA-15 type mesoporous silica support. The emission peaks of D-Re(I) in D-Re(I)/MCM-41 and D-Re(I)/SBA-15 are observed at 522 and 517 nm, respectively. Their long excited lifetimes, which are of the order of microseconds, indicate the presence of phosphorescence emission arising from the metal to ligand charge-transfer (MLCT) transition. The luminescence intensities of D-Re(I)/MCM-41 and D-Re(I)/SBA-15 decrease remarkably with increase in the oxygen concentration, meaning that they can be used as optical oxygen sensing materials based on luminescence quenching. The ratios I 0 /I 100 of D-Re(I)/MCM-41 and D-Re(I)/SBA-15 are estimated to be 5.6 and 20.1, respectively. The obtained Stern-Volmer oxygen quenching plots of the mesoporous sensing materials could be fitted well to the two-site Demas model and Lehrer model. - Research highlights: → Dirhenium(I) complex assembled in mesoporous molecular sieves for oxygen sensor design. → Large α-diimine ligand L used to improve oxygen sensing properties. → High sensitivity (I 0 /I 100 ) up to 20.1.

  10. Fabrication of highly hydrophobic two-component thermosetting polyurethane surfaces with silica nanoparticles

    Science.gov (United States)

    Yang, Guang; Song, Jialu; Hou, Xianghui

    2018-05-01

    Highly hydrophobic thermosetting polyurethane (TSU) surfaces with micro-nano hierarchical structures were developed by a simple process combined with sandpaper templates and nano-silica embellishment. Sandpapers with grit sizes varying from 240 to 7000 grit were used to obtain micro-scale roughness on an intrinsic hydrophilic TSU surface. The surface wettability was investigated by contact angle measurement. It was found that the largest contact angle of the TSU surface without nanoparticles at 102 ± 3° was obtained when the template was 240-grit sandpaper and the molding progress started after 45 min curing of TSU. Silica nanoparticles modified with polydimethylsiloxane were scattered onto the surfaces of both the polymer and the template to construct the desirable nanostructures. The influences of the morphology, surface composition and the silica content on the TSU surface wettability were studied by scanning electron microscopy (SEM), attenuated total reflection (ATR) infrared (IR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and contact angle measurements. The surface of the TSU/SiO2 nanocomposites containing 4 wt% silica nanoparticles exhibited a distinctive dual-scale structure and excellent hydrophobicity with the contact angle above 150°. The mechanism of wettability was also discussed by Wenzel model and Cassie-Baxter model.

  11. Fabrication of semi-transparent super-hydrophobic surface based on silica hierarchical structures

    KAUST Repository

    Chen, Ping-Hei; Hsu, Chin-Chi; Lee, Pei-Shan; Lin, Chao-Sung

    2011-01-01

    -coating silica particles suspended in a precursor solution of silane, ethanol, and H2O with molar ratio of 1:4:4. The resulting super hydrophobic films were characterized by scanning electron microscopy (SEM), optical transmission, and contact angle measurements

  12. A study of luminescence from silicon-rich silica fabricated by plasma enhanced chemical vapour deposition

    International Nuclear Information System (INIS)

    Trwoga, P.F.

    1998-01-01

    Silicon is the most studied electronic material known to man and dominates the electronics industry in its use as a semiconductors for nearly all integrated electronics. However, optoelectronics is almost entirely based on III-V materials. This technology is used because silicon is a very inefficient light source, whereas the III-V band structure can lend itself to efficient light emission by electron injection. However, due to the overwhelming dominance of silicon based electronics it is still a highly desirable goal to generate light efficiently from silicon based materials. Recently, studies have demonstrated that efficient visible luminescence can be obtained from certain novel forms of silicon. These materials include porous silicon, hydrogenated amorphous silicon, and silicon-rich silica (SiO x x x is studied in detail; in addition, electroluminescence and rare-earth doping of silicon-rich silica is also addressed. (author)

  13. Topology of silica supported vanadium–titanium oxide catalysts for oxidative dehydrogenation of propane

    OpenAIRE

    Hamilton, N.; Wolfram, T.; Tzolova-Müller, G.; Hävecker, M.; Kröhnert, J.; Carrero, C.; Schomäcker, R.; Trunschke, A.; Schlögl, R.

    2012-01-01

    Dieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG geförderten) Allianz- bzw. Nationallizenz frei zugänglich. This publication is with permission of the rights owner freely accessible due to an Alliance licence and a national licence (funded by the DFG, German Research Foundation) respectively. Two-dimensional vanadia and titania surface clusters were hosted on the walls of the hierarchical pore system of mesoporous silica SBA-15. The topology of the catalyst surfa...

  14. Well-defined azazirconacyclopropane complexes supported on silica structurally determined by 2D NMR comparative elucidation

    KAUST Repository

    El Eter, Mohamad; Hamzaoui, Bilel; Abou-Hamad, Edy; Pelletier, Jeremie; Basset, Jean-Marie

    2013-01-01

    Grafting of Zr(NMe2)4 on mesoporous silica SBA-15 afforded selectively well-defined surface species SiOZr(NMe2) (η2NMeCH2). 2D solid-state NMR (1H- 13C HETCOR, Multiple Quantum) experiments have shown a unique structural rearrangement occurring on the immobilised zirconium bis methylamido ligand. © The Royal Society of Chemistry 2013.

  15. Enhancing the performance of Ce:YAG phosphor-in-silica-glass by controlling interface reaction

    International Nuclear Information System (INIS)

    Zhou, Beiying; Luo, Wei; Liu, Sheng; Gu, Shijia; Lu, Mengchen; Zhang, Yan; Fan, Yuchi; Jiang, Wan; Wang, Lianjun

    2017-01-01

    Dispersing the Ce"3"+ doped yttrium aluminum garnet (Ce:YAG) phosphor in the glass matrix has been widely investigated to replace conventional organic resin or silicone packaging. However, the reaction layer formed between commercial phosphors and glass matrix severely degrades the optical performance of Ce:YAG phosphor in silica glass (PiSG) materials. This paper demonstrates an ultra-fast method for preparing high performance PiSG materials. Instead of traditional melting process, the highly transparent PiSG samples can be rapidly fabricated from mixtures of commercial Ce:YAG phosphor and mesoporous SiO_2 (SBA-15) powders using spark plasma sintering (SPS) at relatively low temperature (1000 °C) within short time (10 min). Owing to the inhibition of the deleterious interface reactions between Ce:YAG phosphor and silica glass matrix, the phosphor has been perfectly preserved, and the internal relative quantum yield of the PiSG sample reaches as high as 93.5% when excited at 455 nm, which is the highest efficiency in current research. Furthermore, combining the PiSG sample, we successfully fabricate a light-emitting diode (LED) module exhibiting a superior performance with luminous efficacy of 127.9 lm/W, correlated color temperature of 5877 K and color rendering index of 69 at the operating current of 120 mA. This work on the high performance LED modules provides not only a new approach to fabricate the functional glass-based materials that is sensitive to the high temperature, but also a possibility to extend the lifetime and improve the optical performances of the glass based LEDs.

  16. A process to fabricate fused silica nanofluidic devices with embedded electrodes using an optimized room temperature bonding technique

    Science.gov (United States)

    Boden, Seth; Karam, P.; Schmidt, A.; Pennathur, S.

    2017-05-01

    Fused silica is an ideal material for nanofluidic systems due to its extreme purity, chemical inertness, optical transparency, and native hydrophilicity. However, devices requiring embedded electrodes (e.g., for bioanalytical applications) are difficult to realize given the typical high temperature fusion bonding requirements (˜1000 °C). In this work, we optimize a two-step plasma activation process which involves an oxygen plasma treatment followed by a nitrogen plasma treatment to increase the fusion bonding strength of fused silica at room temperature. We conduct a parametric study of this treatment to investigate its effect on bonding strength, surface roughness, and microstructure morphology. We find that by including a nitrogen plasma treatment to the standard oxygen plasma activation process, the room temperature bonding strength increases by 70% (0.342 J/m2 to 0.578 J/m2). Employing this optimized process, we fabricate and characterize a nanofluidic device with an integrated and dielectrically separated electrode. Our results prove that the channels do not leak with over 1 MPa of applied pressure after a 24 h storage time, and the electrode exhibits capacitive behavior with a finite parallel resistance in the upper MΩ range for up to a 6.3Vdc bias. These data thus allow us to overcome the barrier that has barred nanofluidic progress for the last decade, namely, the development of nanometer scale well-defined channels with embedded metallic materials for far-reaching applications such as the exquisite manipulation of biomolecules.

  17. Facile control of silica nanoparticles using a novel solvent varying method for the fabrication of artificial opal photonic crystals

    International Nuclear Information System (INIS)

    Gao, Weihong; Rigout, Muriel; Owens, Huw

    2016-01-01

    In this work, the Stöber process was applied to produce uniform silica nanoparticles (SNPs) in the meso-scale size range. The novel aspect of this work was to control the produced silica particle size by only varying the volume of the solvent ethanol used, whilst fixing the other reaction conditions. Using this one-step Stöber-based solvent varying (SV) method, seven batches of SNPs with target diameters ranging from 70 to 400 nm were repeatedly reproduced, and the size distribution in terms of the polydispersity index (PDI) was well maintained (within 0.1). An exponential equation was used to fit the relationship between the particle diameter and ethanol volume. This equation allows the prediction of the amount of ethanol required in order to produce particles of any target diameter within this size range. In addition, it was found that the reaction was completed in approximately 2 h for all batches regardless of the volume of ethanol. Structurally coloured artificial opal photonic crystals (PCs) were fabricated from the prepared SNPs by self-assembly under gravity sedimentation.

  18. Facile control of silica nanoparticles using a novel solvent varying method for the fabrication of artificial opal photonic crystals

    Science.gov (United States)

    Gao, Weihong; Rigout, Muriel; Owens, Huw

    2016-12-01

    In this work, the Stöber process was applied to produce uniform silica nanoparticles (SNPs) in the meso-scale size range. The novel aspect of this work was to control the produced silica particle size by only varying the volume of the solvent ethanol used, whilst fixing the other reaction conditions. Using this one-step Stöber-based solvent varying (SV) method, seven batches of SNPs with target diameters ranging from 70 to 400 nm were repeatedly reproduced, and the size distribution in terms of the polydispersity index (PDI) was well maintained (within 0.1). An exponential equation was used to fit the relationship between the particle diameter and ethanol volume. This equation allows the prediction of the amount of ethanol required in order to produce particles of any target diameter within this size range. In addition, it was found that the reaction was completed in approximately 2 h for all batches regardless of the volume of ethanol. Structurally coloured artificial opal photonic crystals (PCs) were fabricated from the prepared SNPs by self-assembly under gravity sedimentation.

  19. Facile control of silica nanoparticles using a novel solvent varying method for the fabrication of artificial opal photonic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Weihong [The University of Manchester, School of Materials (United Kingdom); Rigout, Muriel [University of Leeds, School of Design (United Kingdom); Owens, Huw, E-mail: Huw.Owens@manchester.ac.uk [The University of Manchester, School of Materials (United Kingdom)

    2016-12-15

    In this work, the Stöber process was applied to produce uniform silica nanoparticles (SNPs) in the meso-scale size range. The novel aspect of this work was to control the produced silica particle size by only varying the volume of the solvent ethanol used, whilst fixing the other reaction conditions. Using this one-step Stöber-based solvent varying (SV) method, seven batches of SNPs with target diameters ranging from 70 to 400 nm were repeatedly reproduced, and the size distribution in terms of the polydispersity index (PDI) was well maintained (within 0.1). An exponential equation was used to fit the relationship between the particle diameter and ethanol volume. This equation allows the prediction of the amount of ethanol required in order to produce particles of any target diameter within this size range. In addition, it was found that the reaction was completed in approximately 2 h for all batches regardless of the volume of ethanol. Structurally coloured artificial opal photonic crystals (PCs) were fabricated from the prepared SNPs by self-assembly under gravity sedimentation.

  20. Temperature-modified photonic bandgap in colloidal photonic crystals fabricated by vinyl functionalized silica spheres

    International Nuclear Information System (INIS)

    Deng Tiansong; Zhang Junyan; Zhu Kongtao; Zhang Qifeng; Wu Jinlei

    2011-01-01

    Graphical abstract: A thermal annealing procedure was described for fine modifying the photonic bandgap properties of colloidal photonic crystals, which were self-assembled from vinyl-functionalized silica spheres by a gravity sedimentation process. Highlights: → We described a thermal annealing procedure for fine modifying the photonic bandgap properties of colloidal photonic crystals. → The position of its stop band had more than 25% blue shift by annealing the sample from 60 to 600 deg. C. → The annealing temperature and the Bragg peak values have a linear relationship in the 120-440 deg. C range. → The effects provide a simple and controllable method for modifying the photonic bandgap properties of colloidal photonic crystals. - Abstract: A thermal annealing procedure for fine modifying the photonic bandgap properties of colloidal photonic crystals was described. The colloidal photonic crystals were assembled from monodisperse vinyl functionalized silica spheres by a gravity sedimentation process. The samples diffract light following Bragg's law combined with Snell's law. By annealing the sample at temperatures in the range of 60-600 deg. C, the position of its stop band shifted from 943 to 706 nm. It had more than 25% blue shift. In addition, the annealing temperature and the Bragg peak values have a linear relationship in the 120-440 deg. C range. Fourier transform infrared (FT-IR) spectra and thermo-gravimetric analysis (TGA) curves of vinyl functionalized silica spheres confirmed the above results. The effects provide a simple and controllable method for modifying the photonic bandgap properties of colloidal photonic crystals.

  1. Fabrication of silica glass containing yellow oxynitride phosphor by the sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Segawa, Hiroyo; Yoshimizu, Hisato; Hirosaki, Naoto; Inoue, Satoru, E-mail: SEGAWA.Hiroyo@nims.go.jp [National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan)

    2011-06-15

    We have prepared silica glass by the sol-gel method and studied its ability to disperse the Ca-{alpha}-SiAlON:Eu{sup 2+} phosphor for application in white light emitting diodes (LEDs). The emission color generated by irradiating doped glass with a blue LED at 450 nm depended on the concentration of SiAlON and the glass thickness, resulting in nearly white light. The luminescence efficiency of 1-mm-thick glass depended on the SiAlON concentration, and was highest at 4 wt% SiAlON.

  2. Microwave-induced synthesis of highly dispersed gold nanoparticles within the pore channels of mesoporous silica

    International Nuclear Information System (INIS)

    Gu Jinlou; Fan Wei; Shimojima, Atsushi; Okubo, Tatsuya

    2008-01-01

    Highly dispersed gold nanoparticles have been incorporated into the pore channels of SBA-15 mesoporous silica through a newly developed strategy assisted by microwave radiation (MR). The sizes of gold are effectively controlled attributed to the rapid and homogeneous nucleation, simultaneous propagation and termination of gold precursor by MR. Diol moieties with high dielectric and dielectric loss constants, and hence a high microwave activation, were firstly introduced to the pore channels of SBA-15 by a simple addition reaction between amino group and glycidiol and subsequently served as the reduction centers for gold nanoparticles. Extraction of the entrapped gold from the nanocomposite resulted in milligram quantities of gold nanoparticles with low dispersity. The successful assembly process of diol groups and formation of gold nanoparticles were monitored and tracked by solid-state NMR and UV-vis measurements. Characterization by small angle X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated that the incorporation of gold nanoparticles would not breakup the structural integrity and long-range periodicity of SBA-15. The gold nanoparticles had a narrow size distribution with diameters in the size range of 5-10 nm through TEM observation. The average particles size is 7.9 nm via calculation by the Scherrer formula and TEM measurements. Nitrogen adsorption and desorption isotherms gave further evidence that the employed method was efficient and gold nanoparticles were successfully incorporated into the pore channels of SBA-15. - Graphical abstract: A facile and novel strategy has been developed to incorporate gold nanoparticles into the pore channels of mesoporous SBA-15 assisted by microwave radiation (MR) with mild reaction condition and rapid reaction speed. Due to the rapid and homogeneous nucleation, simultaneous propagation and termination by MR, the size of gold nanoparticles are effectively controlled

  3. Fabrication of high-capacity polyelectrolyte brush-grafted porous AAO-silica composite membrane via RAFT polymerization.

    Science.gov (United States)

    Song, Cunfeng; Wang, Meijie; Liu, Xin; Wang, He; Chen, Xiaoling; Dai, Lizong

    2017-09-01

    Surface-initiated reversible addition-fragmentation chain transfer (RAFT) polymerization has been utilized to fabricate high-capacity strong anion-exchange (AEX) membrane for the separation of protein. By means of RAFT polymerization, quaternized poly(3-(methacrylamidomethyl)-pyridine) brushes formed 3-dimensional nanolayers on the surface of porous anodic aluminum oxide (AAO)-silica composite membrane. The surface properties of the membranes were analyzed by SEM, water contact angle, ATR-FTIR, XPS and TGA. To investigate the adsorption performance, the new AEX membranes were applied to recover a model protein, ovalbumin (OVA). High adsorption capacities of 95.8mg/g membranes (static) and 65.3mg/g membranes (dynamic) were obtained at ambient temperature. In the further studies, up to 90% of the adsorbed OVA was efficiently eluted by using phosphate buffer-1M NaCl as elution medium. The successful separation of OVA with high purity from a mixture protein solution was also achieved by using the AEX membranes. The present study demonstrated that under mild reaction condition, RAFT polymerization can be used to fabricate ion-exchange membrane which has many remarkable features, such as high capacity and selectivity, easy elution and so on. Copyright © 2017. Published by Elsevier B.V.

  4. Fabrication and characterization of bioactive glass-ceramic using soda-lime-silica waste glass.

    Science.gov (United States)

    Abbasi, Mojtaba; Hashemi, Babak

    2014-04-01

    Soda-lime-silica waste glass was used to synthesize a bioactive glass-ceramic through solid-state reactions. In comparison with the conventional route, that is, the melt-quenching and subsequent heat treatment, the present work is an economical technique. Structural and thermal properties of the samples were examined by X-ray diffraction (XRD) and differential thermal analysis (DTA). The in vitro test was utilized to assess the bioactivity level of the samples by Hanks' solution as simulated body fluid (SBF). Bioactivity assessment by atomic absorption spectroscopy (AAS) and scanning electron microscopy (SEM) was revealed that the samples with smaller amount of crystalline phase had a higher level of bioactivity. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Fabrication and characterization of silica aerogel as synthetic tissues for medical imaging phantoms

    Science.gov (United States)

    In, Eunji; Naguib, Hani

    2015-05-01

    Medical imaging plays an important role in the field of healthcare industry both in clinical settings and in research and development. It is used in prevention, early detection of disease, in choosing the optimal treatment, during surgical interventions and monitoring of the treatment effects. Despite much advancement in the last few decades, rapid change on its technology development and variety of imaging parameters that differ with the manufacturer restrict its further development. Imaging phantom is a calibrating medium that is scanned or imaged in the field of medical imaging to evaluate, analyze and tune the performance of various imaging devices. A phantom used to evaluate an imaging device should respond in a similar manner to how human tissue and organs would act in that specific imaging modality. There has been many research on the phantom materials; however, there has been no attempt to study on the material that mimics the structure of lung or fibrous tissue. So with the need for development of gel with such structure, we tried to mimic this structure with aerogel. Silica aerogels have unique properties that include low density (0.003g/cm) and mesoporosity (pore size 2-50nm), with a high thermal insulation value (0.005W/mK) and high surface area (500-1200m-2/g).] In this study, we cross-linked with di-isocyanate, which is a group in polyurethane to covalently bond the polymer to the surface of silica aerogel to enhance the mechanical properties. By formation of covalent bonds, the structure can be reinforced by widening the interparticle necks while minimally reducing porosity.

  6. Utilization of rice husk ash as silica source for the synthesis of mesoporous silicas and their application to CO2 adsorption through TREN/TEPA grafting

    International Nuclear Information System (INIS)

    Bhagiyalakshmi, Margandan; Yun, Lee Ji; Anuradha, Ramani; Jang, Hyun Tae

    2010-01-01

    Mesoporous MCM-41, MCM-48 and SBA-15 were synthesized using Rice husk ash (RHA) as the silica source and their defective Si-OH sites were functionalized by 3-cholropropyltrimethoxysilane (CPTMS) which was subsequently grafted with amine compounds, Tris(2-aminoethyl)amine (TREN) and Tetraethylenepentamine (TEPA). X-ray powder diffraction (XRD) and BET results of the parent mesoporous silica suggested their closeness of structural properties to those obtained from conventional silica sources. CO 2 adsorption of branched amine TREN and straight chain amine TEPA at 25, 50 and 75 deg. C was obtained by Thermogravimetric Analyser (TGA) at atmospheric pressure. TREN grafted mesoporous silica showed 7% of CO 2 adsorption while TEPA grafted mesoporous silicas showed less CO 2 adsorption, which is due to the presence of isolated amine groups in TREN. TREN grafted mesoporous silicas were also observed to be selective towards CO 2 , thermally stable and recyclable. The order of CO 2 adsorption with respect to amount of amine grafting was observed to be MCM-48/TREN > MCM-41/TREN > SBA-15/TREN.

  7. Controllable Fabrication of Ordered Mesoporous Bi2WO6 and Its High Photocatalytic Activity under Visible Light

    Directory of Open Access Journals (Sweden)

    Xueming Dang

    2014-01-01

    Full Text Available Ordered mesoporous Bi2WO6 was fabricated by nanocasting technique using SBA-15 as the template. The effect of the dosage of SBA-15 on the formation of the ordered structure and the photocatalytic ability of mesoporous Bi2WO6 was discussed. It was confirmed that the ordered mesoporous structure was obtained as the dosage of SBA-15 was 0.3 g. It was found that, compared to Bi2WO6, the RhB degradation rate with ordered mesoporous Bi2WO6 was enhanced under visible light (λ>400 nm by the photocatalytic measurements. The enhanced photocatalytic performance of ordered mesoporous Bi2WO6 was attributed to its particular ordered mesoporous structure which could increase the light-harvesting efficiency, reduce the recombination of the photogenerated charge carriers, and promote the surface reaction.

  8. Preparation, characterization and catalytic activity of mesoporous Ag{sub 2}HPW{sub 12}O{sub 40}/SBA-15 and Ag{sub 2}HPW{sub 12}O{sub 40}/TiO{sub 2} composites

    Energy Technology Data Exchange (ETDEWEB)

    Holclajtner-Antunović, Ivanka; Bajuk-Bogdanović, Danica [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11158 Belgrade (Serbia); Popa, Alexandru; Sasca, Viorel [Institute of Chemistry Timişoara, Bl. Mihail Viteazul 24, 300223 Timişoara (Romania); Nedić Vasiljević, Bojana; Rakić, Aleksandra [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11158 Belgrade (Serbia); Uskoković-Marković, Snežana, E-mail: snezaum@pharmacy.bg.ac.rs [Faculty of Pharmacy, University of Belgrade, Vojvode Stepe 450, 11221 Belgrade (Serbia)

    2015-06-15

    The current study reports the synthesis and characterization of tungstophosphoric acid and its acid silver salt supported on mesoporous molecular sieve SBA-15 and TiO{sub 2}. Because silver salts are partially insoluble, the SBA-15 and TiO{sub 2} supported silver acid salts were prepared by two step sequential impregnations. The synthesized catalysts were characterized by various physicochemical methods such as Fourier transform infrared and Raman spectroscopy, differential thermal analysis, thermogravimetric analysis, X-ray diffraction, scanning electron microscopy and nitrogen physisorption at −196 °C. It is observed that both active phases keep their Keggin-type structure after being supported on the supports while their specific surface area is considerably increased by deposition on mesoporous substrates. The results also indicated that the synthesized catalysts retained the morphology specific for each of the supports, while their thermal stability is increased in comparison with their active phases. The catalytic activity of the prepared catalysts was probed for the vapor phase dehydration of ethanol at 300 °C. Results revealed that all the catalysts show considerably improved catalytic activity in comparison to the bulk active phases. - Highlights: • SBA-15 and TiO{sub 2} supported Ag{sub 2}HPW{sub 12}O{sub 40} and H{sub 3}PW{sub 12}O{sub 40} were prepared. • Active phases are uniformly dispersed without changing morphology of the substrates. • Composites are more thermally stable than active phases. • Composites exhibit high catalytic activity for gas phase ethanol dehydration.

  9. Fabrication and characterization of stable superhydrophobic fluorinated-polyacrylate/silica hybrid coating

    International Nuclear Information System (INIS)

    Li, Kunquan; Zeng, Xingrong; Li, Hongqiang; Lai, Xuejun

    2014-01-01

    Graphical abstract: - Highlights: • The superhydrophobic PFA/SiO 2 coating was successfully fabricated by spraying. • The synthesized PFA latex showed core–shell structure and good dispersion. • The PFA/SiO 2 coating showed good resistance to acid and base, weather and heat. • The superhydrophobic coating could be fabricated on various substrates. - Abstract: The core–shell fluorinated-polyacrylate (PFA) emulsion was synthesized through emulsion polymerization method and the superhydrophobic PFA/SiO 2 hybrid coating was successfully fabricated on the slide glass by spraying the mixture of PFA emulsion and hydrophobic SiO 2 particles using ethanol as cosolvent. The PFA emulsion was characterized by Fourier transform infrared spectroscopy (FTIR), dynamic light scattering (DLS), water contact angle (WCA), transmission electron microscopy (TEM), and the effects of SiO 2 content on the wetting behavior and surface morphology of PFA/SiO 2 hybrid coating were investigated. To evaluate the stability of the hybrid coating, the acid and base resistance, weatherability and thermal stability were also studied. Results showed that the obtained PFA latex exhibited a core–shell structure with a particle size of 134.1 nm and a narrow polydispersity of 0.03. With the increase of dodecafluoroheptyl methacrylate (DFMA) content in the latex shell from 0 wt% to 31.8 wt%, the WCA of the PFA film enlarged from 85° to 104°, indicating that the introduction of fluorinated monomer was effective in reducing the surface energy. By adding different amount of SiO 2 particles, the surface morphology and wetting behavior of the PFA/SiO 2 hybrid coatings could be controlled. When the mass ratio of SiO 2 to PFA emulsion was 0.2, the surface roughness (Rq) increased to 173.6 nm and the wetting behavior of the surface became superhydrophobic with a WCA of 153°, resulted from the corporation of low surface energy and the binary nano/microstructure on the surface. The as-prepared PFA

  10. Cr(VI) adsorption on functionalized amorphous and mesoporous silica from aqueous and non-aqueous media

    International Nuclear Information System (INIS)

    Perez-Quintanilla, Damian; Hierro, Isabel del; Fajardo, Mariano; Sierra, Isabel

    2007-01-01

    A mesoporous silica (SBA-15) and amorphous silica (SG) have been chemically modified with 2-mercaptopyridine using the homogeneous route. This synthetic route involved the reaction of 2-mercaptopyridine with 3-chloropropyltriethoxysilane prior to immobilization on the support. The resulting material has been characterized by powder X-ray diffraction, nitrogen gas sorption, FT-IR and MAS NMR spectroscopy, thermogravimetry and elemental analysis. The solid was employed as a Cr(VI) adsorbent from aqueous and non-aqueous solutions at room temperature. The effect of several variables (stirring time, pH, metal concentration and solvent polarity) has been studied using the batch technique. The results indicate that under the optimum conditions, the maximum adsorption value for Cr(VI) was 1.83 ± 0.03 mmol/g for MP-SBA-15, whereas the adsorption capacity of the MP-SG was 0.86 ± 0.02 mmol/g. On the basis of these results, it can be concluded that it is possible to modify chemically SBA-15 and SG with 2-mercaptopyridine and to use the resulting modified silicas as effective adsorbents for Cr(VI)

  11. FABRICATION OF MICROPOROUS SILICA CERAMICS WITH VARIED POLYMORPHIC FORMS AND INVESTIGATION OF THEIR THERMAL SHOCK BEHAVIOUR

    Directory of Open Access Journals (Sweden)

    Osman ŞAN

    2011-06-01

    Full Text Available In this study; the SiO₂ micro-porous ceramics in the phase α-quartz, α-cristobalite and β-cristobalite were produced and thermal shock resistance of products were compared. In the production of ceramic materials; α-quartz obtained from natural quartz powder, α-cristobalite from pure silica powder which prepared by Stöber technique and β-cristobalite from sol-gel approach. The β-composition was designed as Si₁₋⨯Al⨯Ca⨯/₂O₂ where x=0.05 and obtained gel was calcined at 850 °C. Before shaping, α-quartz powder and calcined β-cristobalite powder were grind in the planetary mill and the powder produced by Stöber technique was shaped directly without any milling process. The prepared powders were shaped by uniaxally press at 50 bars. The samples produced from α-quartz and β-cristobalite powders were sintered at 1150 °C and α-cristobalite obtained by Stöber technique was sintered at 1400 °C. In the defined polymorphic structure, micro-porous materials with pore size ~0.1-5 µm were produced and thermal shock tests were applied. Irrespective of β-cristobalite material, the samples were cracked and the tests could only repeat on the samples with β-cristobalite material. In the result, the β-cristobalite sample is believed to be great potential to use as a membrane filters for harsh thermal environments.

  12. Fabrication and characterization of chromium-doped nanophase separated yttria-alumina-silica glass-based optical fibers

    Energy Technology Data Exchange (ETDEWEB)

    Dutta, Debjit; Dhar, Anirban; Das, Shyamal; Paul, Mukul C. [Fiber Optics and Photonics Division, CSIR-Central Glass and Ceramic Research Institute, Kolkata (India); Kir' yanov, Alexander V. [Centro de Investigaciones en Optica, Guanajuato (Mexico); Bysakh, Sandip [Electron Microscopic Section, Material Characterization Division, CSIR-Central Glass and Ceramic Research Institute, Kolkata (India)

    2015-08-15

    The basic material and optical properties of chromium-doped nanophase-separated yttria-alumina-silica (YAS) glass based optical preforms and fibers, fabricated through the modified chemical vapor deposition process in conjunction with solution doping technique under suitable thermal annealing conditions are reported. The size of the phase-separated particles within the core of the annealed preform is around 20-30 nm which is significantly reduced to around 5.0 nm in the drawn fiber. The absorption spectra of fibers drawn from the annealed and non-annealed preform samples revealed the presence of Cr{sup 4+}, Cr{sup 3+}, and Cr{sup 6+} specie. Numerically, extinction of absorption drops ∝3-3.5 times for the annealed sample as a result of nano-phase restructuration during annealing process. Intense broadband emission (within 500-800 nm) in case of the annealed preform sample is observed as compared to the non-annealed one and is associated with the presence of Cr{sup 3+} ions in nanostructured environment inside the YAS core glass. The final fibers show broadband emission ranging from 900 to 1400 nm under pumping at 1064 nm which is attributed mainly to the presence of Cr{sup 3+}/Cr{sup 4+} ions. The fabricated fibers seem to be a potential candidate for the development of fiber laser sources for the visible and near-infra ranges and for effective Q-switching units for ∝1-1.1 μm all-fiber ytterbium lasers. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  13. Synthesis of Hierarchically Structured Hybrid Materials by Controlled Self-Assembly of Metal-Organic Framework with Mesoporous Silica for CO2 Adsorption.

    Science.gov (United States)

    Chen, Chong; Li, Bingxue; Zhou, Lijin; Xia, Zefeng; Feng, Nengjie; Ding, Jing; Wang, Lei; Wan, Hui; Guan, Guofeng

    2017-07-12

    The HKUST-1@SBA-15 composites with hierarchical pore structure were constructed by in situ self-assembly of metal-organic framework (MOF) with mesoporous silica. The structure directing role of SBA-15 had an obvious impact on the growth of MOF crystals, which in turn affected the morphologies and structural properties of the composites. The pristine HKUST-1 and the composites with different content of SBA-15 were characterized by XRD, N 2 adsorption-desorption, SEM, TEM, FT-IR, TG, XPS, and CO 2 -TPD techniques. It was found that the composites were assembled by oriented growth of MOF nanocrystals on the surfaces of SBA-15 matrix. The interactions between surface silanol groups and metal centers induced structural changes and resulted in the increases in surface areas as well as micropore volumes of hybrid materials. Besides, the additional constraints from SBA-15 also restrained the expansion of HKUST-1, contributing to their smaller crystal sizes in the composites. The adsorption isotherms of CO 2 on the materials were measured and applied to calculate the isosteric heats of adsorption. The HS-1 composite exhibited an increase of 15.9% in CO 2 uptake capacity compared with that of HKUST-1. Moreover, its higher isosteric heats of CO 2 adsorption indicated the stronger interactions between the surfaces and CO 2 molecules. The adsorption rate of the composite was also improved due to the introduction of mesopores. Ten cycles of CO 2 adsorption-desorption experiments implied that the HS-1 had excellent reversibility of CO 2 adsorption. This study was intended to provide the possibility of assembling new composites with tailored properties based on MOF and mesoporous silica to satisfy the requirements of various applications.

  14. Electroless porous silicon formation applied to fabrication of boron-silica-glass cantilevers

    DEFF Research Database (Denmark)

    Teva, Jordi; Davis, Zachary James; Hansen, Ole

    2010-01-01

    This work describes the characterization and optimization of anisotropic formation of porous silicon in large volumes (0.5-1 mm3) of silicon by an electroless wet etching technique. The main goal is to use porous silicon as a sacrificial volume for bulk micromachining processes, especially in cases...... where etching of the full wafer thickness is needed. The porous silicon volume is formed by a metal-assisted etching in a wet chemical solution composed of hydrogen peroxide (30%), hydrofluoric acid (40%) and ethanol. This paper focuses on optimizing the etching conditions in terms of maximizing...... for bio-chemical sensors. The porous silicon volume is formed in an early step of the fabrication process, allowing easy handling of the wafer during all of the micromachining processes in the process flow. In the final process step, the porous silicon is quickly etched by immersing the wafer in a KOH...

  15. Nitridated fibrous silica (KCC-1) as a sustainable solid base nanocatalyst

    KAUST Repository

    Bouhrara, Mohamed; Ranga, Chanakya; Fihri, Aziz; Shaikh, Rafik; Sarawade, Pradip; Emwas, Abdul-Hamid M.; Hedhili, Mohamed N.; Polshettiwar, Vivek

    2013-01-01

    We observed that support morphology has dramatic effects on the performance of nitridated silica as a base. By simply replacing conventional silica supports (such as SBA-15 and MCM-41) with fibrous nanosilica (KCC-1), we observed multifold enhancement in the catalytic activity of the nitridated solid base for Knoevenagel condensations and transesterification reactions. This enhancement of the activity can be explained by amine accessibility, which is excellent in KCC-1 due to its open and flexible fibrous structure, that facilitates penetration and interaction with basic amine sites. © 2013 American Chemical Society.

  16. Monodisperse metal nanoparticle catalysts on silica mesoporous supports: synthesis, characterizations, and catalytic reactions

    Energy Technology Data Exchange (ETDEWEB)

    Somorjai, G.A.

    2009-09-14

    The design of high performance catalyst achieving near 100% product selectivity at maximum activity is one of the most important goals in the modern catalytic science research. To this end, the preparation of model catalysts whose catalytic performances can be predicted in a systematic and rational manner is of significant importance, which thereby allows understanding of the molecular ingredients affecting the catalytic performances. We have designed novel 3-dimensional (3D) high surface area model catalysts by the integration of colloidal metal nanoparticles and mesoporous silica supports. Monodisperse colloidal metal NPs with controllable size and shape were synthesized using dendrimers, polymers, or surfactants as the surface stabilizers. The size of Pt, and Rh nanoparticles can be varied from sub 1 nm to 15 nm, while the shape of Pt can be controlled to cube, cuboctahedron, and octahedron. The 3D model catalysts were generated by the incorporation of metal nanoparticles into the pores of mesoporous silica supports via two methods: capillary inclusion (CI) and nanoparticle encapsulation (NE). The former method relies on the sonication-induced inclusion of metal nanoparticles into the pores of mesoporous silica, whereas the latter is performed by the encapsulation of metal nanoparticles during the hydrothermal synthesis of mesoporous silica. The 3D model catalysts were comprehensively characterized by a variety of physical and chemical methods. These catalysts were found to show structure sensitivity in hydrocarbon conversion reactions. The Pt NPs supported on mesoporous SBA-15 silica (Pt/SBA-15) displayed significant particle size sensitivity in ethane hydrogenolysis over the size range of 1-7 nm. The Pt/SBA-15 catalysts also exhibited particle size dependent product selectivity in cyclohexene hydrogenation, crotonaldehyde hydrogenation, and pyrrole hydrogenation. The Rh loaded SBA-15 silica catalyst showed structure sensitivity in CO oxidation reaction. In

  17. Nitridated fibrous silica (KCC-1) as a sustainable solid base nanocatalyst

    KAUST Repository

    Bouhrara, Mohamed

    2013-09-03

    We observed that support morphology has dramatic effects on the performance of nitridated silica as a base. By simply replacing conventional silica supports (such as SBA-15 and MCM-41) with fibrous nanosilica (KCC-1), we observed multifold enhancement in the catalytic activity of the nitridated solid base for Knoevenagel condensations and transesterification reactions. This enhancement of the activity can be explained by amine accessibility, which is excellent in KCC-1 due to its open and flexible fibrous structure, that facilitates penetration and interaction with basic amine sites. © 2013 American Chemical Society.

  18. Fabrication and characterization of stable superhydrophobic fluorinated-polyacrylate/silica hybrid coating

    Science.gov (United States)

    Li, Kunquan; Zeng, Xingrong; Li, Hongqiang; Lai, Xuejun

    2014-04-01

    The core-shell fluorinated-polyacrylate (PFA) emulsion was synthesized through emulsion polymerization method and the superhydrophobic PFA/SiO2 hybrid coating was successfully fabricated on the slide glass by spraying the mixture of PFA emulsion and hydrophobic SiO2 particles using ethanol as cosolvent. The PFA emulsion was characterized by Fourier transform infrared spectroscopy (FTIR), dynamic light scattering (DLS), water contact angle (WCA), transmission electron microscopy (TEM), and the effects of SiO2 content on the wetting behavior and surface morphology of PFA/SiO2 hybrid coating were investigated. To evaluate the stability of the hybrid coating, the acid and base resistance, weatherability and thermal stability were also studied. Results showed that the obtained PFA latex exhibited a core-shell structure with a particle size of 134.1 nm and a narrow polydispersity of 0.03. With the increase of dodecafluoroheptyl methacrylate (DFMA) content in the latex shell from 0 wt% to 31.8 wt%, the WCA of the PFA film enlarged from 85° to 104°, indicating that the introduction of fluorinated monomer was effective in reducing the surface energy. By adding different amount of SiO2 particles, the surface morphology and wetting behavior of the PFA/SiO2 hybrid coatings could be controlled. When the mass ratio of SiO2 to PFA emulsion was 0.2, the surface roughness (Rq) increased to 173.6 nm and the wetting behavior of the surface became superhydrophobic with a WCA of 153°, resulted from the corporation of low surface energy and the binary nano/microstructure on the surface. The as-prepared PFA/SiO2 hybrid coating showed good acid and base corrosion resistance, and it could keep superhydrophobicity after being heated at 250 °C for 2 h or exposed to ambient atmosphere for more than 3 months. Additionally, the superhydrophobic PFA/SiO2 hybrid coating could be applied to various substrates through spraying. This was a green and eco-friendly method in fabricating stable

  19. Flame retardant and hydrophobic properties of novel sol-gel derived phytic acid/silica hybrid organic-inorganic coatings for silk fabric

    Science.gov (United States)

    Cheng, Xian-Wei; Liang, Cheng-Xi; Guan, Jin-Ping; Yang, Xu-Hong; Tang, Ren-Cheng

    2018-01-01

    In this work, a novel phosphorus-rich hybrid organic-inorganic silica coating for improving the flame retardancy of silk fabric was prepared using naturally occurring phytic acid as phosphorus precursor and catalyst for the hydrolysis of tetraethoxysilane. In addition, three silane coupling agents, namely 3-aminopropyldimethoxymethylsilane, 3-chloropropyltrimethoxysilane and 3-methacryloxypropyltrimethoxysilane, were added in the hybrid sol as cross-linkers with the aim of developing hydrophobic coatings and improving the washing durability of the treated silk fabric. The condensation degree of the hybrid sol was characterized by solid-state 29Si nuclear magnetic resonance spectroscopy. The flammability and thermal degradation properties of the treated silk fabrics were determined in terms of limiting oxygen index, vertical burning, pyrolysis combustion flow calorimetry and thermogravimetric analyses. The surface morphology and hydrophobicity of the treated silk fabrics were evaluated by scanning electron microscopy, atomic force microscopy and water contact angle tests. The flammability tests revealed that the silicon sol could endow silk fabric with excellent flame retardancy when doped with phytic acid, and the treated silk fabrics self-extinguished immediately when the ignition source was removed. The silk fabrics treated with the modified hybrid sols exhibited hydrophobic surface and also better durability to washing.

  20. Tunable thick porous silica coating fabricated by multilayer-by-multilayer bonding of silica nanoparticles for open-tubular capillary chromatographic separation.

    Science.gov (United States)

    Qu, Qishu; Liu, Yuanyuan; Shi, Wenjun; Yan, Chao; Tang, Xiaoqing

    2015-06-19

    A simple coating procedure employing a multilayer-by-multilayer process to modify the inner surface of bare fused-silica capillaries with silica nanoparticles was established. The silica nanoparticles were adsorbed onto the capillary wall via a strong electrostatic interaction between amino functional groups and silica particles. The thickness of the coating could be tuned from 130 to 600 nm by increasing the coating cycles from one to three. Both the retention factor and the resolution were greatly increased with increasing coating cycles. The loading capacity determined by naphthalene in the column with three coating cycles is 152.1 pmol. The effects of buffer concentration and pH value on the stability of the coating were evaluated. The retention reproducibility of the separation of toluene was 0.8, 1.2, 2.3, and 4.5%, respectively, for run-to-run, day-to-day, column-to-column, and batch-to-batch, respectively. The chromatographic performance of these columns was evaluated by both capillary liquid chromatography and open-tubular capillary electrochromatography (OT-CEC). Separation of aromatic hydrocarbons in the column with three coating cycles provided high theoretical plate numbers (up to 269,280 plates m(-1) for toluene) and short separation time (<15 min) by using OT-CEC mode. The method was also used to separate egg white proteins. Both acidic and basic proteins as well as four glycoisoforms were separated in a single run. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Adsorptive performance of chromium-containing ordered mesoporous silica on volatile organic compounds (VOCs

    Directory of Open Access Journals (Sweden)

    Jianwei Fan

    2017-09-01

    Full Text Available Volatile organic compounds (VOCs are the primary poisonous emissions into the atmosphere in natural gas exploitation and disposing process. The adsorption method has been widely applied in actual production because of its good features such as low cost, low energy consumption, flexible devices needed, etc. The commonly used adsorbents like activated carbon, silicon molecular sieves and so on are not only susceptible to plugging or spontaneous combustion but difficult to be recycled. In view of this, a new adsorbent (CrSBA15 was made by the co-assembly method to synthesize the ordered mesoporous silica materials with different amounts of chromium to eliminate VOCs. This new adsorbent was characterized by small-angle-X-ray scattering (SAXS, nitrogen adsorption/desorption, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. Its adsorption performance to eliminate VOCs (toluene, benzene, cyclohexane and ethyl acetate used as typical pollutants was also tested systematically. Research results indicate that this new adsorbent of CrSBA-15(30, with the silicon/chromium ration being 30, owns the maximum micropore volume, and shows a higher adsorption performance in eliminating toluene, benzene, cyclohexane and ethyl acetate. Besides, it is cost-effective and much easier to be recycled than the activated carbon. In conclusion, CrSBA-15(30 is a good adsorbent to eliminate VOCs with broad application prospects. Keywords: Mesoporous materials, Silicon dioxide, Synthesis, Adsorption, Volatile organic compounds (VOCs, Recyclability, Energy saving

  2. Effect of the nature of the surface on the reactivity of nanoporous silica under irradiation

    International Nuclear Information System (INIS)

    Le Caer, S.; Alam, M.S.; Chatelain, C.; Brunet, F.; Charpentier, T.; Renault, J.P.; Brodie-Linder, N.; Alba-Simionesco, C.

    2011-01-01

    Complete text of publication follows. Materials such as concrete, clays and zeolites which embed radioactive wastes adsorb in their pores significant amounts of water that can be decomposed under ionizing radiation leading to the formation of H 2 which is potentially explosive. It is well established that the H 2 production arises from chemi- or physi-sorbed OH groups at the surface of oxides. In this context, we have studied the behaviour of water confined in nanoporous silica. To distinguish the behavior of the two kinds of OH, we have performed different thermal treatments on SBA-15 materials prior to their irradiation. The IR analysis and H 2 measurements have proven that in the radiolysis of SBA-15 materials, silanol groups are only attacked when they are in the majority with respect to adsorbed water. However they are much less efficient at producing H 2 . The comparison between water content before and after electron irradiation and the corresponding H 2 production indicates that water desorption is the main route to adsorbed water loss. On the other hand, surface silanol groups are more susceptible to attack, leading to H 2 production when SBA-15 samples have undergone extensive thermal treatment. The surface of nanoporous glasses were then grafted using chloroaklyldimethylsilane. The effect of irradiation on these grafted surfaces was studied by means of mass spectrometry and NMR experiments. These different techniques reveal an original reactivity of the surface under irradiation.

  3. Functionalized mesoporous silicas with crown ether moieties for selective adsorption of lithium ions in artificial sea water.

    Science.gov (United States)

    Sung, Soo Park; Moorthy, Madhappan Santha; Song, Hyun-Jin; Ha, Chang-Sik

    2014-11-01

    Lithium ion has been increasingly recognized in a wide range of industrial applications. In this work, we studied on the adsorption of Li+ in the artificial seawater with high selectivity using methyl-crown ether (AC-SBA-15) and aza-crown ether (HMC-SBA-15) moieties-functionalized mesoporous silica materials. First, methyl-crown ether and aza-crown ether moieties-functionalized mesoporous silica materials were synthesized via two-step post-synthesis process using a grafting method. The functionalized materials were employed to the metal ion adsorption from aqueous solution (artificial seawater) containing Li+, Co2+, Cr3+ and Hg2+. The prepared hybrid material showed high selectivity for Li+ ion in the artificial seawater at pH 8.0. The absorbed amount of Li+ was 73 times higher than Cr3+ for aza-crown ether containing AC-SBA-15 as an absorbent. The absorbed amount of Co2+ (4.5 x 10(-5) mol/g), Cr3+ (1.5 x 10(-5) mol/g) and Hg2+ (2.25 x 10(-4) mol/g) were remarkably lower than the case of Li+. On the other hand, the absorbed amount of various metal ions of HMC-SBA-15 with amine groups in alky chains and crown ether moieties were 1.1 x 10(-3) mol/g for Li+, 5.0 x 10(-5) mol/g for Co2+, 2.9 x 10(-4) mol/g for Cr3+, 2.8 x 10(-4) mol/g for Hg2+ mol/g, respectively.

  4. Optimal Surface Amino-Functionalization Following Thermo-Alkaline Treatment of Nanostructured Silica Adsorbents for Enhanced CO2 Adsorption

    Directory of Open Access Journals (Sweden)

    Obdulia Medina-Juárez

    2016-11-01

    Full Text Available Special preparation of Santa Barbara Amorphous (SBA-15, mesoporous silica with highly hexagonal ordered, these materials have been carried out for creating adsorbents exhibiting an enhanced and partially selective adsorption toward CO2. This creation starts from an adequate conditioning of the silica surface, via a thermo-alkaline treatment to increase the population of silanol species on it. CO2 adsorption is only reasonably achieved when the SiO2 surface becomes aminated after put in contact with a solution of an amino alkoxide compound in the right solvent. Unfunctionalized and amine-functionalized substrates were characterized through X-ray diffraction, N2 sorption, Raman spectroscopy, electron microscopy, 29Si solid-state Nuclear Magnetic Resonance (NMR, and NH3 thermal programmed desorption. These analyses proved that the thermo-alkaline procedure desilicates the substrate and eliminates the micropores (without affecting the SBA-15 capillaries, present in the original solid. NMR analysis confirms that the hydroxylated solid anchors more amino functionalizing molecules than the unhydroxylated material. The SBA-15 sample subjected to hydroxylation and amino-functionalization displays a high enthalpy of interaction, a reason why this solid is suitable for a strong deposition of CO2 but with the possibility of observing a low-pressure hysteresis phenomenon. Contrastingly, CH4 adsorption on amino-functionalized, hydroxylated SBA-15 substrates becomes almost five times lower than the CO2 one, thus giving proof of their selectivity toward CO2. Although the amount of retained CO2 is not yet similar to or higher than those determined in other investigations, the methodology herein described is still susceptible to optimization.

  5. The Deep-Sea Natural Products, Biogenic Polyphosphate (Bio-PolyP and Biogenic Silica (Bio-Silica, as Biomimetic Scaffolds for Bone Tissue Engineering: Fabrication of a Morphogenetically-Active Polymer

    Directory of Open Access Journals (Sweden)

    Florian Draenert

    2013-03-01

    Full Text Available Bone defects in human, caused by fractures/nonunions or trauma, gain increasing impact and have become a medical challenge in the present-day aging population. Frequently, those fractures require surgical intervention which ideally relies on autografts or suboptimally on allografts. Therefore, it is pressing and likewise challenging to develop bone substitution materials to heal bone defects. During the differentiation of osteoblasts from their mesenchymal progenitor/stem cells and of osteoclasts from their hemopoietic precursor cells, a lineage-specific release of growth factors and a trans-lineage homeostatic cross-talk via signaling molecules take place. Hence, the major hurdle is to fabricate a template that is functioning in a way mimicking the morphogenetic, inductive role(s of the native extracellular matrix. In the last few years, two naturally occurring polymers that are produced by deep-sea sponges, the biogenic polyphosphate (bio-polyP and biogenic silica (bio-silica have also been identified as promoting morphogenetic on both osteoblasts and osteoclasts. These polymers elicit cytokines that affect bone mineralization (hydroxyapatite formation. In this manner, bio-silica and bio-polyP cause an increased release of BMP-2, the key mediator activating the anabolic arm of the hydroxyapatite forming cells, and of RANKL. In addition, bio-polyP inhibits the progression of the pre-osteoclasts to functionally active osteoclasts. Based on these findings, new bioinspired strategies for the fabrication of bone biomimetic templates have been developed applying 3D-printing techniques. Finally, a strategy is outlined by which these two morphogenetically active polymers might be used to develop a novel functionally active polymer.

  6. The Deep-Sea Natural Products, Biogenic Polyphosphate (Bio-PolyP) and Biogenic Silica (Bio-Silica), as Biomimetic Scaffolds for Bone Tissue Engineering: Fabrication of a Morphogenetically-Active Polymer

    Science.gov (United States)

    Wang, Xiaohong; Schröder, Heinz C.; Feng, Qingling; Draenert, Florian; Müller, Werner E. G.

    2013-01-01

    Bone defects in human, caused by fractures/nonunions or trauma, gain increasing impact and have become a medical challenge in the present-day aging population. Frequently, those fractures require surgical intervention which ideally relies on autografts or suboptimally on allografts. Therefore, it is pressing and likewise challenging to develop bone substitution materials to heal bone defects. During the differentiation of osteoblasts from their mesenchymal progenitor/stem cells and of osteoclasts from their hemopoietic precursor cells, a lineage-specific release of growth factors and a trans-lineage homeostatic cross-talk via signaling molecules take place. Hence, the major hurdle is to fabricate a template that is functioning in a way mimicking the morphogenetic, inductive role(s) of the native extracellular matrix. In the last few years, two naturally occurring polymers that are produced by deep-sea sponges, the biogenic polyphosphate (bio-polyP) and biogenic silica (bio-silica) have also been identified as promoting morphogenetic on both osteoblasts and osteoclasts. These polymers elicit cytokines that affect bone mineralization (hydroxyapatite formation). In this manner, bio-silica and bio-polyP cause an increased release of BMP-2, the key mediator activating the anabolic arm of the hydroxyapatite forming cells, and of RANKL. In addition, bio-polyP inhibits the progression of the pre-osteoclasts to functionally active osteoclasts. Based on these findings, new bioinspired strategies for the fabrication of bone biomimetic templates have been developed applying 3D-printing techniques. Finally, a strategy is outlined by which these two morphogenetically active polymers might be used to develop a novel functionally active polymer. PMID:23528950

  7. Influences of surface charge, size, and concentration of colloidal nanoparticles on fabrication of self-organized porous silica in film and particle forms.

    Science.gov (United States)

    Nandiyanto, Asep Bayu Dani; Suhendi, Asep; Arutanti, Osi; Ogi, Takashi; Okuyama, Kikuo

    2013-05-28

    Studies on preparation of porous material have attracted tremendous attention because existence of pores can provide material with excellent performances. However, current preparation reports described successful production of porous material with only partial information on charges, interactions, sizes, and compositions of the template and host materials. In this report, influences of self-assembly parameters (i.e., surface charge, size, and concentration of colloidal nanoparticles) on self-organized porous material fabrication were investigated. Silica nanoparticles (as a host material) and polystyrene (PS) spheres (as a template) were combined to produce self-assembly porous materials in film and particle forms. The experimental results showed that the porous structure and pore size were controllable and strongly depended on the self-assembly parameters. Materials containing highly ordered pores were effectively created only when process parameters fall within appropriate conditions (i.e., PS surface charge ≤ -30 mV; silica-to-PS size ratio ≤0.078; and silica-to-PS mass ratio of about 0.50). The investigation of the self-assembly parameter landscape was also completed using geometric considerations. Because optimization of these parameters provides significant information in regard to practical uses, results of this report could be relevant to other functional properties.

  8. Vapor-Liquid Sol-Gel Approach to Fabricating Highly Durable and Robust Superhydrophobic Polydimethylsiloxane@Silica Surface on Polyester Textile for Oil-Water Separation.

    Science.gov (United States)

    Su, Xiaojing; Li, Hongqiang; Lai, Xuejun; Zhang, Lin; Wang, Jing; Liao, Xiaofeng; Zeng, Xingrong

    2017-08-23

    Large-scale fabrication of superhydrophobic surfaces with excellent durability by simple techniques has been of considerable interest for its urgent practical application in oil-water separation in recent years. Herein, we proposed a facile vapor-liquid sol-gel approach to fabricating highly durable and robust superhydrophobic polydimethylsiloxane@silica surfaces on the cross-structure polyester textiles. Scanning electron microscopy and Fourier transform infrared spectroscopy demonstrated that the silica generated from the hydrolysis-condensation of tetraethyl orthosilicate (TEOS) gradually aggregated at microscale driven by the extreme nonpolar dihydroxyl-terminated polydimethylsiloxane (PDMS(OH)). This led to construction of hierarchical roughness and micronano structures of the superhydrophobic textile surface. The as-fabricated superhydrophobic textile possessed outstanding durability in deionized water, various solvents, strong acid/base solutions, and boiling/ice water. Remarkably, the polyester textile still retained great water repellency and even after ultrasonic treatment for 18 h, 96 laundering cycles, and 600 abrasion cycles, exhibiting excellent mechanical robustness. Importantly, the superhydrophobic polyester textile was further applied for oil-water separation as absorption materials and/or filter pipes, presenting high separation efficiency and great reusability. Our method to construct superhydrophobic textiles is simple but highly efficient; no special equipment, chemicals, or atmosphere is required. Additionally, no fluorinated slianes and organic solvents are involved, which is very beneficial for environment safety and protection. Our findings conceivably stand out as a new tool to fabricate organic-inorganic superhydrophobic surfaces with strong durability and robustness for practical applications in oil spill accidents and industrial sewage emission.

  9. Innovative preparation of Au/C by replication of gold-containing mesoporous silica catalysts

    KAUST Repository

    Kerdi, Fatmé

    2010-01-01

    A new strategy, based on the nanocasting concept, has been used to prepare gold nanoparticles (NPs) highly dispersed in meso-structured carbons. Gold is first introduced in various functionalized mesostructured silicas (MCM-48 and SBA-15) and particles are formed inside the porosity upon reduction of Au 3+ cations. Silica pores are then impregnated with a carbon precursor and the composite material is heated at 900°C under vacuum. Silica is then removed by acid leaching, leading to partially encapsulated gold particles in mesoporous carbon. Carbon prevents aggregation of gold particles at high temperature, both the mean size and distribution being similar to those observed in silica. However, while Au@SiO2 exhibit significant catalytic activity in the aerobic oxidation of trans-stilbene in the liquid phase, its Au@C mesostructured replica is quite inactive. © 2010 Elsevier B.V. All rights reserved.

  10. Mesoporous silica materials modified with alumina polycations as catalysts for the synthesis of dimethyl ether from methanol

    Energy Technology Data Exchange (ETDEWEB)

    Macina, Daniel; Piwowarska, Zofia; Tarach, Karolina; Góra-Marek, Kinga [Jagiellonian University, Faculty of Chemistry, Ingardena 3, 30-060 Kraków (Poland); Ryczkowski, Janusz [Maria Curie Skłodowska University, Faculty of Chemistry, Maria Curie-Skłodowska 2, 20-031 Lublin (Poland); Chmielarz, Lucjan, E-mail: chmielar@chemia.uj.edu.pl [Jagiellonian University, Faculty of Chemistry, Ingardena 3, 30-060 Kraków (Poland)

    2016-02-15

    Highlights: • Deposition of alumina ologoctaions on mesoporous silicas modified with surface −SO{sub 3}H groups. • Alumina aggregates generated acid properties in the silica supports. • Alumina modified SBA-15 and MCF were active and selective catalysts in DME synthesis. - Abstract: Mesoporous silica materials (SBA-15 and MCF) were used as catalytic supports for the deposition of aggregated alumina species using the method consisting of the following steps: (i) anchoring 3-(mercaptopropyl)trimethoxysilane (MPTMS) on the silica surface followed by (ii) oxidation of −SH to−SO{sub 3}H groups and then (iii) deposition of aluminum Keggin oligocations by ion-exchange method and (iv) calcination. The obtained samples were tested as catalysts for synthesis of dimethyl ether from methanol. The modified silicas were characterized with respect to the ordering of their porous structure (XRD), textural properties (BET), chemical composition (EDS, CHNS), structure ({sup 27}Al NMR, FTIR) and location of alumina species (EDX-TEM), surface acidity (NH{sub 3}-TPD, Py-FTIR) and thermal stability (TGA). The obtained materials were found to be active and selective catalysts for methanol dehydration to dimethyl ether (DME) in the MTD process (methanol-to-dimethyl ether).

  11. Modified mesoporous silica materials for on-line separation and preconcentration of hexavalent chromium using a microcolumn coupled with flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wang Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Fang Dongmei; Li Qing [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); East China University of Science and Technology, Shanghai 200237 (China); Zhang Lingxia; Qian Rong; Zhu Yan; Qu Haiyun [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Du Yiping [East China University of Science and Technology, Shanghai 200237 (China)

    2012-05-06

    Highlights: Black-Right-Pointing-Pointer A modified SBA-15 mesoporous silica material (NH{sub 2}-SBA-15) was synthesized as sorbent. Black-Right-Pointing-Pointer The material was used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Black-Right-Pointing-Pointer The NH{sub 2}-SBA-15 enables retain Cr (VI) with an enrichment factor of 44. Black-Right-Pointing-Pointer The micro-column of NH{sub 2}-SBA-15 underwent more than 100 adsorption/desorption cycles. - Abstract: A modified SBA-15 mesoporous silica material NH{sub 2}-SBA-15 was synthesized successfully by grafting {gamma}-aminopropyl-triethoxysilane. The material was characterized using transmission electron microscopy (TEM) and Fourier transform infrared/Raman (FT-IR/Raman) spectroscopy, and used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Effective sorption of Cr (VI) was achieved at pH 2.0 with no interference from Cr (III) and other ions and 0.5 mol L{sup -1} NH{sub 3}{center_dot}H{sub 2}O solution was found optimal for the complete elution of Cr (VI). An enrichment factor of 44 and was achieved under optimized experimental conditions at a sample loading of 2.0 mL min{sup -1} sample loading (300 s) and an elution flow rate of 2.0 mL min{sup -1} (24 s). The precision of the 11 replicate Cr (VI) measurements was 2.1% at the 100 {mu}g L{sup -1} level with a detection limit of 0.2 {mu}g L{sup -1} (3 s, n = 10) using the FAAS. The developed method was successfully applied to trace chromium determination in waste water. The accuracy was validated using a certified reference material of riverine water (GBW08607).

  12. Fabrication and characterization of an inorganic gold and silica nanoparticle mediated drug delivery system for nitric oxide

    Energy Technology Data Exchange (ETDEWEB)

    Das, Amitava; Singla, Sumit K; Shah, Vijay H [Gastroenterology Research Unit, Department of Internal Medicine, Mayo Clinic College of Medicine, 200 First Street S.W., Rochester, MN 55905 (United States); Mukherjee, Priyabrata; Mukhopadhyay, Debabrata; Patra, Chitta Ranjan [Department of Biochemistry and Molecular Biology, Mayo Clinic College of Medicine, 200 First Street S.W., Rochester, MN 55905 (United States); Guturu, Praveen [Department of Internal Medicine, UTMB, Galveston, TX 77555 (United States); Frost, Megan C, E-mail: patra.chittaranjan@mayo.edu, E-mail: patra.chitta@gmail.com [Department of Biomedical Engineering, Michigan Technological University, Houghton, MI 49931 (United States)

    2010-07-30

    Nitric oxide (NO) plays an important role in inhibiting the development of hepatic fibrosis and its ensuing complication of portal hypertension by inhibiting human hepatic stellate cell (HSC) activation. Here we have developed a gold nanoparticle and silica nanoparticle mediated drug delivery system containing NO donors, which could be used for potential therapeutic application in chronic liver disease. The gold nanoconjugates were characterized using several physico-chemical techniques such as UV-visible spectroscopy and transmission electron microscopy. Silica nanoconjugates were synthesized and characterized as reported previously. NO released from gold and silica nanoconjugates was quantified under physiological conditions (pH = 7.4 at 37 deg. C) for a substantial period of time. HSC proliferation and the vascular tube formation ability, manifestations of their activation, were significantly attenuated by the NO released from these nanoconjugates. This study indicates that gold and silica nanoparticle mediated drug delivery systems for introducing NO could be used as a strategy for the treatment of hepatic fibrosis or chronic liver diseases, by limiting HSC activation.

  13. Fabrication and characterization of an inorganic gold and silica nanoparticle mediated drug delivery system for nitric oxide

    International Nuclear Information System (INIS)

    Das, Amitava; Singla, Sumit K; Shah, Vijay H; Mukherjee, Priyabrata; Mukhopadhyay, Debabrata; Patra, Chitta Ranjan; Guturu, Praveen; Frost, Megan C

    2010-01-01

    Nitric oxide (NO) plays an important role in inhibiting the development of hepatic fibrosis and its ensuing complication of portal hypertension by inhibiting human hepatic stellate cell (HSC) activation. Here we have developed a gold nanoparticle and silica nanoparticle mediated drug delivery system containing NO donors, which could be used for potential therapeutic application in chronic liver disease. The gold nanoconjugates were characterized using several physico-chemical techniques such as UV-visible spectroscopy and transmission electron microscopy. Silica nanoconjugates were synthesized and characterized as reported previously. NO released from gold and silica nanoconjugates was quantified under physiological conditions (pH = 7.4 at 37 deg. C) for a substantial period of time. HSC proliferation and the vascular tube formation ability, manifestations of their activation, were significantly attenuated by the NO released from these nanoconjugates. This study indicates that gold and silica nanoparticle mediated drug delivery systems for introducing NO could be used as a strategy for the treatment of hepatic fibrosis or chronic liver diseases, by limiting HSC activation.

  14. Insignificant influence of the matrix on the melting of ice confined in decorated mesoporous silica

    Science.gov (United States)

    Xu, Yunbo; Zhao, Zhenyan; Wang, Lianwen

    2018-01-01

    For a critical examination of matrix effect on the melting of confined ice, mesoporous silica (SBA-15) are synthesised and decorated with n-Alkyl and aminopropyl groups to tune the surface hydrophobicity. Water contact angle to these decorated surfaces are estimated to be about 100° and 60°, respectively. By examining the melting of ice confined in these decorated samples, we find that the influence of the matrix is indeed not significant. The reported apparent matrix effect is more likely method effect in the determination of pore diameters as was demonstrated in our previous studies (Philos. Mag. 93 (2013), p. 1827).

  15. Improved antimicrobial property and controlled drug release kinetics of silver sulfadiazine loaded ordered mesoporous silica

    Directory of Open Access Journals (Sweden)

    Suman Jangra

    2016-09-01

    Full Text Available The present study deals with the loading of silver sulfadiazine into ordered mesoporous silica material by post-impregnation method and its effect on the in vitro release kinetics and antimicrobial property of the drug. The formulated SBA-15 silica material with rope-like morphology and SBA-15-silver sulfadiazine (SBA-AgSD were characterized by UV–visible spectrophotometer, small and wide-angle powder X-ray diffraction (PXRD, field emission scanning electron microscope (FESEM and high resolution transmission electron microscope (HRTEM. Thermo-gravimetric analysis of SBA-AgSD revealed a high loading amount of 52.87%. Nitrogen adsorption–desorption analysis confirmed the drug entrapment into host material by revealing a reduced surface area (214 m2/g and pore diameter (6.7 nm of the SBA-AgSD. The controlled release of silver sulfadiazine drug from the mesoporous silica to simulated gastric, intestinal and body fluids was evaluated. The Korsmeyer–Peppas model fits the drug release data with the non-Fickian diffusion model and zero order kinetics of SBA-AgSD. The antibacterial performance of the SBA-AgSD was evaluated with respect to Staphylococcus aureus, Bacillus subtilis and Pseudomonas aeruginosa. The controlled drug delivery of the SBA-AgSD revealed improved antibacterial activity, thus endorsing its applicability in effective wound dressing.

  16. Fabrication of Through via Holes in Ultra-Thin Fused Silica Wafers for Microwave and Millimeter-Wave Applications

    Directory of Open Access Journals (Sweden)

    Xiao Li

    2018-03-01

    Full Text Available Through via holes in fused silica are a key infrastructure element of microwave and millimeter-wave circuits and 3D integration. In this work, etching through via holes in ultra-thin fused silica wafers using deep reactive-ion etching (DRIE and laser ablation was developed and analyzed. The experimental setup and process parameters for both methods are presented and compared. For DRIE, three types of mask materials including KMPR 1035 (Nippon Kayaku, Tokyo, Japan photoresist, amorphous silicon and chromium—with their corresponding optimized processing recipes—were tested, aiming at etching through a 100 μm fused silica wafer. From the experiments, we concluded that using chromium as the masking material is the best choice when using DRIE. However, we found that the laser ablation method with a laser pulse fluence of 2.89 J/cm2 and a pulse overlap of 91% has advantages over DRIE. The laser ablation method has a simpler process complexity, while offering a fair etching result. In particular, the sidewall profile angle is measured to be 75° to the bottom surface of the wafer, which is ideal for the subsequent metallization process. As a demonstration, a two-inch wafer with 624 via holes was processed using both technologies, and the laser ablation method showed better efficiency compared to DRIE.

  17. Fabrication and Properties of Silica Gel/Calcium Sulfate/Strontium-doped β-tricalcium Phosphate Composite Porous Scaffolds for Bone Tissue Engineering

    Directory of Open Access Journals (Sweden)

    QIN Xiao-su

    2018-03-01

    Full Text Available The calcium sulfate/strontium-doped β-tricalcium phosphate composite spherical pellets was fabricated, using the calcium sulfate/strontium-doped β-TCP as raw material, and through the stirring spray drying method, and then composite spherical pellets were combined with silica gel, porous silica gel/calcium sulfate/strontium-doped β-tricalcium phosphate scaffold was obtained by stacking aggregation method in the mould. The XRD, SEM and FT-IR, etc are employed to examine the chemical composition, composite morphology and structure characteristics, and the degradability, porosity, mechanical properties and cytotoxicity of the scaffolds materials were studied. The results reveal that the composite porous scaffolds have irregular pore structure with pore size between 0.2-1.0mm, and they have a large number of micropores on each of the composite spherical pellets, with the aperture between 50-200μm. Moreover, the porosity of the composite scaffolds is about 62%, which can meet the requirements of scaffolds for bone tissue engineering in porosity; the cytotoxicity tests show the composite scaffolds have no cytotoxic effect and it has good degradation. Therefore, it has good application prospect in bone tissue engineering of the bone defect repair of non-bearing site.

  18. Microporous silica membranes

    DEFF Research Database (Denmark)

    Boffa, Vittorio; Yue, Yuanzheng

    2012-01-01

    Hydrothermal stability is a crucial factor for the application of microporous silica-based membranes in industrial processes. Indeed, it is well established that steam exposure may cause densification and defect formation in microporous silica membranes, which are detrimental to both membrane...... permeability and selectivity. Numerous previous studies show that microporous transition metal doped-silica membranes are hydrothermally more stable than pure silica membranes, but less permeable. Here we present a quantitative study on the impact of type and concentration of transition metal ions...... on the microporous structure, stability and permeability of amorphous silica-based membranes, providing information on how to design chemical compositions and synthetic paths for the fabrication of silica-based membranes with a well accessible and highly stabile microporous structure....

  19. Submicrometric gratings fabrication from photosensitive organo-silica-hafnia thin films elaborated by sol-gel processing

    Energy Technology Data Exchange (ETDEWEB)

    Franc, Janyce [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Barnier, Vincent, E-mail: barnier@emse.fr [Ecole Nationale Superieure des Mines, SMS-EMSE, CNRS:UMR 5146, LCG, F-42023 Saint-Etienne (France); Vocanson, Francis, E-mail: francis.vocanson@univ-st-etienne.fr [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Gamet, Emilie; Lesage, Maryline [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Jamon, Damien [Universite de Lyon, F-42023 Saint-Etienne (France); Laboratoire Claude Chappe, Telecom Saint-Etienne, 42000 Saint-Etienne Cedex 2 (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Jourlin, Yves [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France)

    2012-07-31

    The aim of this study is the elaboration of a high index sol-gel material in order to prepare submicrometric grating. The gratings were obtained after few seconds of UV exposure in one step using an organically modified silica-hafnia matrix. The chemical composition of thin films after UV and annealing treatments were studied using Fourier Transform Infrared Spectroscopy and X-Ray Photoelectron Spectroscopy. The study of optical properties revealed that the annealed films are transparent from 200 to 1000 nm and have a refractive index from 1.550 to 1.701 depending on the hafnium concentration. - Highlights: Black-Right-Pointing-Pointer Silica-hafnia matrix with high refractive index was prepared using sol-gel process. Black-Right-Pointing-Pointer Organic and inorganic networks formation of thin films was investigated. Black-Right-Pointing-Pointer Optical properties are influenced by annealing treatment and initial hafnium amount. Black-Right-Pointing-Pointer The use of high Si:Hf molar ratio can lead to a loss transmittance below 300 nm. Black-Right-Pointing-Pointer Submicrometric grating period can be prepared using a holographic method.

  20. Functionalized silica nanoparticles as a carrier for Betamethasone Sodium Phosphate: Drug release study and statistical optimization of drug loading by response surface method.

    Science.gov (United States)

    Ghasemnejad, M; Ahmadi, E; Mohamadnia, Z; Doustgani, A; Hashemikia, S

    2015-11-01

    Mesoporous silica nanoparticles with a hexagonal structure (SBA-15) were synthesized and modified with (3-aminopropyl) triethoxysilane (APTES), and their performance as a carrier for drug delivery system was studied. Chemical structure and morphology of the synthesized and modified SBA-15 were characterized by SEM, BET, TEM, FT-IR and CHN technique. Betamethasone Sodium Phosphate (BSP) as a water soluble drug was loaded on the mesoporous silica particle for the first time. The response surface method was employed to obtain the optimum conditions for the drug/silica nanoparticle preparation, by using Design-Expert software. The effect of time, pH of preparative media, and drug/silica ratio on the drug loading efficiency was investigated by the software. The maximum loading (33.69%) was achieved under optimized condition (pH: 1.8, time: 3.54 (h) and drug/silica ratio: 1.7). The in vitro release behavior of drug loaded particles under various pH values was evaluated. Finally, the release kinetic of the drug was investigated using the Higuchi and Korsmeyer-Peppas models. Cell culture and cytotoxicity assays revealed the synthesized product doesn't have any cytotoxicity against human bladder cell line 5637. Accordingly, the produced drug-loaded nanostructures can be applied via different routes, such as implantation and topical or oral administration. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Synthesis and characterization of novel mesocomposites Co3O4 and CuO@OMS (ordered mesoporous silica) as active catalysts for hydrocarbon oxidation

    Science.gov (United States)

    Comănescu, Cezar

    2014-03-01

    Novel metal nanoporous transition metal oxides M x O y (Co3O4, CuO) have been synthesized by thermal decomposition of inorganic salts precursors (acetates, nitrates) impregnated into hexagonal mesoporous silica (OMS, ordered mesoporous silica) of SBA-15 type (prepared in-house) at different precursor loadings, the mesocomposites thus obtained being monitored after each impregnation-calcination step by small and wide angle powder XRD. The pore size for the ordered silica host range from 5.08 to 7.06 nm. Retention of the hexagonal silica framework has been observed in spite of the temperatures up to 500 °C. Mesoporous Co3O4 has been obtained by leaching the silica through overnight HF dissolution, which partially preserved the small-range ordering found in the parent Co3O4@OMS composite prior to leaching. Both Co3O4 ( meso) and Co3O4@SBA-15 have been tested in methane oxidation and were found to be superior to the bulk Co3O4 performance, with mesoporous Co3O4 being able to fully oxidize methane to CO2 and H2O at 350 °C, while Co3O4@OMS exhibits a lower activity with 20 % conversion at 350 °C. CuO@OMS shows the lowest activity, with only 13 % conversion at 500 °C.

  2. Silica-supported, single-site titanium catalysts for olefin epoxidation. A molecular precursor strategy for control of catalyst structure.

    Science.gov (United States)

    Jarupatrakorn, Jonggol; Don Tilley, T

    2002-07-17

    A molecular precursor approach involving simple grafting procedures was used to produce site-isolated titanium-supported epoxidation catalysts of high activity and selectivity. The tris(tert-butoxy)siloxy titanium complexes Ti[OSi(O(t)Bu)(3)](4) (TiSi4), ((i)PrO)Ti[OSi(O(t)Bu)(3)](3) (TiSi3), and ((t)BuO)(3)TiOSi(O(t)Bu)(3) (TiSi) react with the hydroxyl groups of amorphous Aerosil, mesoporous MCM-41, and SBA-15 via loss of HO(t)Bu and/or HOSi(O(t)Bu)(3) and introduction of titanium species onto the silica surface. Powder X-ray diffraction, nitrogen adsorption/desorption, infrared, and diffuse reflectance ultraviolet spectroscopies were used to investigate the structures and chemical natures of the surface-bound titanium species. The titanium species exist mainly in isolated, tetrahedral coordination environments. Increasing the number of siloxide ligands in the molecular precursor decreases the amount of titanium that can be introduced this way, but also enhances the catalytic activity and selectivity for the epoxidation of cyclohexene with cumene hydroperoxide as oxidant. In addition, the high surface area mesoporous silicas (MCM-41 and SBA-15) are more effective than amorphous silica as supports for these catalysts. Supporting TiSi3 on the SBA-15 affords highly active cyclohexene epoxidation catalysts (0.25-1.77 wt % Ti loading) that provide turnover frequencies (TOFs) of 500-1500 h(-1) after 1 h (TOFs are reduced by about half after calcination). These results demonstrate that oxygen-rich siloxide complexes of titanium are useful as precursors to supported epoxidation catalysts.

  3. Controlled release of phenytoin for epilepsy treatment from titania and silica based materials

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, Tessy, E-mail: tessy3@prodigy.net.mx [Universidad Autonoma Metropolitana-Xochimilco. Departamento de Microbiologia. Calzada del Hueso 1100, Col. Villa Quietud, Coyoacan, C.P. 04960, Mexico D.F. Mexico (Mexico); Instituto Nacional de Neurologia y Neurocirugia ' MVS' . Laboratorio de Nanotecnologia. Av. Insurgentes Sur 3877, Col. La Fama, Tlalpan, 14269, Mexico, D.F. Mexico (Mexico); Department of Chemical and Biomolecular Engineering, Tulane University, New Orleans, LA 70118 (United States); Ortiz, Emma [Instituto Nacional de Neurologia y Neurocirugia ' MVS' . Laboratorio de Nanotecnologia. Av. Insurgentes Sur 3877, Col. La Fama, Tlalpan, 14269, Mexico, D.F. Mexico (Mexico); Meza, Doraliz [Universidad Autonoma Metropolitana-Iztapalapa, Departamento de Quimica, Av. San Rafael Atlixco 186, A.P. 55-534, Mexico D.F., C.P. 09340 (Mexico); Basaldella, Elena [CIC-CINDECA - Universidad Nacional de La Plata - Calle 47 No 257 - La Plata (Argentina); Bokhimi, Xim; Magana, Carlos [Instituto de fisica, UNAM. Circuito de la Investigacion s/n. C.U. Mexico D.F. 01000 (Mexico); Sepulveda, Antonio; Rodriguez, Francisco; Ruiz, Javier [Departamento de Quimica Inorganica, Universidad de Alicante. Apartado 99, E-03080 Alicante, Espana Spain (Spain)

    2011-04-15

    Research highlights: {yields} Template technique was used to obtain well ordered nanostructured materials: SBA-15 and titania tubes. {yields} Phenytoin (PH), a drug used in epilepsy treatment, was loaded in these materials to used como PH release. {yields} Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. {yields} The load-release PH are faster in nanostructured TiO2 tubes than in mesoporous silica matrix. {yields} There is an inverse effect of the surface area of the structured materials on the amount of released PH. - Abstract: Template technique was used to obtain well ordered nanostructured materials: mesoporous silica and nanostructured titania tubes. This technique permits the synthesis of solids with controlled mesoporosity, where a large variety of molecules that have therapeutic activity can be hosted and further released to specific sites. In this work phenytoin (PH), a drug used in epilepsy treatment, was loaded in ordered mesoporous silica (SBA 15) and nanostructured titania tubes (TiO{sub 2}). The pure materials and those containing PH were characterized by X-ray diffraction, FTIR spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and N{sub 2} adsorption-desorption at 77 K. In order to determine the loading capacity of the antiepileptic drug on these silica- and titania-based materials, the loading and release of PH was investigated using UV-vis spectroscopy. Tubular structures were found for the titania samples, for which the X-ray diffractograms showed to be formed by anatase and rutile phases. On the other hand, an amorphous phase was found in the silica sample. A highly ordered hexagonal structure of 1D cylindrical channels was also observed for this material. Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. The adsorption and desorption of PH are faster in nanostructured TiO{sub 2} tubes than in mesoporous silica

  4. Controlled release of phenytoin for epilepsy treatment from titania and silica based materials

    International Nuclear Information System (INIS)

    Lopez, Tessy; Ortiz, Emma; Meza, Doraliz; Basaldella, Elena; Bokhimi, Xim; Magana, Carlos; Sepulveda, Antonio; Rodriguez, Francisco; Ruiz, Javier

    2011-01-01

    Research highlights: → Template technique was used to obtain well ordered nanostructured materials: SBA-15 and titania tubes. → Phenytoin (PH), a drug used in epilepsy treatment, was loaded in these materials to used como PH release. → Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. → The load-release PH are faster in nanostructured TiO2 tubes than in mesoporous silica matrix. → There is an inverse effect of the surface area of the structured materials on the amount of released PH. - Abstract: Template technique was used to obtain well ordered nanostructured materials: mesoporous silica and nanostructured titania tubes. This technique permits the synthesis of solids with controlled mesoporosity, where a large variety of molecules that have therapeutic activity can be hosted and further released to specific sites. In this work phenytoin (PH), a drug used in epilepsy treatment, was loaded in ordered mesoporous silica (SBA 15) and nanostructured titania tubes (TiO 2 ). The pure materials and those containing PH were characterized by X-ray diffraction, FTIR spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and N 2 adsorption-desorption at 77 K. In order to determine the loading capacity of the antiepileptic drug on these silica- and titania-based materials, the loading and release of PH was investigated using UV-vis spectroscopy. Tubular structures were found for the titania samples, for which the X-ray diffractograms showed to be formed by anatase and rutile phases. On the other hand, an amorphous phase was found in the silica sample. A highly ordered hexagonal structure of 1D cylindrical channels was also observed for this material. Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. The adsorption and desorption of PH are faster in nanostructured TiO 2 tubes than in mesoporous silica matrix.

  5. Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

    Science.gov (United States)

    Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

    2016-08-12

    A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Functionalized nanostructured silica by tetradentate-amine chelating ligand as efficient heavy metals adsorbent : Applications to industrial effluent treatment

    Energy Technology Data Exchange (ETDEWEB)

    Shahbazi, Afsaneh [Shahid Beheshti University, Tehran (Iran, Islamic Republic of); Younesi, Habibollah [Tarbiat Modares University, Noor (Iran, Islamic Republic of); Badiei, Alireza [University of Tehran, Tehran (Iran, Islamic Republic of)

    2014-09-15

    Organofunctionalized nanostructured silica SBA-15 with tri(2-aminoethyl)amine tetradentate-amine ligand was synthesized and applied as adsorbent for the removal of Cu{sup 2+}, Pb{sup 2+}, and Cd{sup 2+} from both synthetic wastewater and real paper mill and electroplating industrial effluents. The prepared materials were characterized by XRD, N{sub 2} adsorption-desorption, TGA, and FT-IR analysis. The Tren-SBA-15 was found to be a fast adsorbent for heavy metal ions from single solution with affinity for Cu{sup 2+}, Pb{sup 2+}, than for Cd{sup 2+} due to the complicated impacts of metal ion electronegativity. The kinetic rate constant decreased with increasing metal ion concentration due to increasing of ion repulsion force. The equilibrium batch experimental data is well described by the Langmuir isotherm. The maximum adsorption capacity was 1.85 mmol g{sup -1} for Cu{sup 2+}, 1.34 mmol g{sup -1} for Pb{sup 2+}, and 1.08 mmol g{sup -1} for Cd{sup 2+} at the optimized adsorption conditions (pH=4, T=323 K, t=2 h, C0=3 mmol L{sup -1}, and adsorbent dose=1 g L{sup -1}). All Gibbs energy was negative as expected for spontaneous interactions, and the positive entropic values from 103.7 to 138.7 J mol{sup -1} K{sup -1} also reinforced this favorable adsorption process in heterogeneous system. Experiment with real wastewaters showed that approximately a half fraction of the total amount of studied metal ions was removed within the first cycle of adsorption. Hence, desorption experiments were performed by 0.3M HCl eluent, and Tren-SBA-15 successfully reused for four adsorption/desorption cycles to complete removal of metal ions from real effluents. The regenerated Tren-SBA-15 displayed almost similar adsorption capacity of Cu{sup 2+}, Pb{sup 2+}, and Cd{sup 2+} even after four recycles. The results suggest that Tren-SBA-15 is a good candidate as an adsorbent in the removal of Cu{sup 2+}, Pb{sup 2+}, and Cd{sup 2+} from aqueous solutions.

  7. One-Pot Fabrication of Antireflective/Antibacterial Dual-Function Ag NP-Containing Mesoporous Silica Thin Films.

    Science.gov (United States)

    Wang, Kaikai; He, Junhui

    2018-04-04

    Thin films that integrate antireflective and antibacterial dual functions are not only scientifically interesting but also highly desired in many practical applications. Unfortunately, very few studies have been devoted to the preparation of thin films with both antireflective and antibacterial properties. In this study, mesoporous silica (MSiO 2 ) thin films with uniformly dispersed Ag nanoparticles (Ag NPs) were prepared through a one-pot process, which simultaneously shows high transmittance, excellent antibacterial activity, and mechanical robustness. The optimal thin-film-coated glass substrate demonstrates a maximum transmittance of 98.8% and an average transmittance of 97.1%, respectively, in the spectral range of 400-800 nm. The growth and multiplication of typical bacteria, Escherichia coli ( E. coli), were effectively inhibited on the coated glass. Pencil hardness test, tape adhesion test, and sponge washing test showed favorable mechanical robustness with 5H pencil hardness, 5A grade adhesion, and functional durability of the coating, which promises great potential for applications in various touch screens, windows for hygiene environments, and optical apparatuses for medical uses such as endoscope, and so on.

  8. Fabrication Flexible and Luminescent Nanofibrillated Cellulose Films with Modified SrAl2O4: Eu, Dy Phosphors via Nanoscale Silica and Aminosilane

    Directory of Open Access Journals (Sweden)

    Longfei Zhang

    2018-05-01

    Full Text Available Flexible 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO-oxidized nanofibrillated cellulose (ONFC films with long afterglow luminescence containing modified SrAl2O4: Eu2+, Dy3+ (SAOED phosphors were fabricated by a template method. Tetraethyl orthosilicate (TEOS and (3-aminopropyl trimethoxy-silane (APTMS were employed cooperatively to improve the water resistance and compatibility of the SAOED particles in the ONFC suspension. The structure and morphology after modification evidenced the formation of a superior SiO2 layer and coarse amino-compounds on the surface of the phosphors. Homogeneous dispersions containing ONFC and the modified phosphors were prepared and the interface of composite films containing the amino-modified particles showed a more closely packed structure and had less voids at the interface between the cellulose and luminescent particles than that of silica-modified phosphors. The emission spectra for luminescent films showed a slight blue shift (3.2 nm at around 512 nm. Such flexible films with good luminescence, thermal resistance, and mechanical properties can find applications in fields like luminous flexible equipment, night indication, and portable logo or labels.

  9. Rational design and fabrication of highly transparent, flexible, and thermally stable superhydrophobic coatings from raspberry-like hollow silica nanoparticles

    Science.gov (United States)

    Zou, Xinshu; Tao, Chaoyou; Yang, Ke; Yang, Fan; Lv, Haibing; Yan, Lianghong; Yan, Hongwei; Li, Yuan; Xie, Yongyong; Yuan, Xiaodong; Zhang, Lin

    2018-05-01

    Multifunctional coatings with superhydrophobicity, high transparency, thermal stability, flexibility, and ultralow refractive index have been investigated for many years. They have promising applications in industries such as in electronic and optical devices, photonic materials, and templates for fabricating biological and chemical sensors. However, the relatively complex preparation technology of these coatings or difficult to possess these properties simultaneously are still the main factors that limit their wide application. In this paper, we report a facile atmospheric approach to create transparent multifunctional raspberry-like particulate coatings with a low refractive index, which were obtained via one-pot base-catalyzed sol-gel process using tetraethyl orthosilicate (TEOS) and 1H, 1H, 2H, 2H-perfluorooctyltrimethoxysilane (POTS) as co-precursors. The excellent superhydrophobicity, mechanical flexibility, self-cleaning property, thermal and chemical stability of the as-fabricated coatings were demonstrated. The refractive indices of coatings can be easily tuned at a range of 1.07-1.16. Particularly, the resulted samples on the K9 glasses exhibited superhydrophobicity with a water contact angle (WCA) of 162° when the scale ratio of the POTS and TEOS was 1.0. The superhydrophobicity of the as-prepared coatings could last for more than half a year under indoor condition, demonstrating the long stability of the superhydrophobicity. Furthermore, we demonstrated that this simple efficient method could be extended to different substrates, including K9 glass, Polyvinyl chloride (PVC), stainless steel, aluminum alloy, and gingko leaf, to achieve superhydrophobicity. Interestingly, the superhydrophobicty of the coatings transferred to superhydrophilicity (WCA < 5°) by calcination at 500 °C, which resulted in a good antifogging property. Moreover, the coatings were not sensitive to the strong acid (pH = 1) and kept their superhydrophobic state for a long time

  10. Fumed silica. Fumed silica

    Energy Technology Data Exchange (ETDEWEB)

    Sukawa, T.; Shirono, H. (Nippon Aerosil Co. Ltd., Tokyo (Japan))

    1991-10-18

    The fumed silica is explained in particulate superfineness, high purity, high dispersiveness and other remarkable characteristics, and wide application. The fumed silica, being presently produced, is 7 to 40nm in average primary particulate diameter and 50 to 380m{sup 2}/g in specific surface area. On the surface, there coexist hydrophilic silanol group (Si-OH) and hydrophobic siloxane group (Si-O-Si). There are many characteristics, mutually different between the fumed silica, made hydrophobic by the surface treatment, and untreated hydrophilic silica. The treated silica, if added to the liquid product, serves as agent to heighten the viscosity, prevent the sedimentation and disperse the particles. The highest effect is given to heighten the viscosity in a region of 4 to 9 in pH in water and alcohol. As filling agent to strengthen the elastomer and polymer, and powder product, it gives an effect to prevent the consolidation and improve the fluidity. As for its other applications, utilization is made of particulate superfineness, high purity, thermal insulation properties and adsorption characteristics. 2 to 3 patents are published for it as raw material of quartz glass. 38 refs., 16 figs., 4 tabs.

  11. Synthesis Mechanism and Thermal Optimization of an Economical Mesoporous Material Using Silica: Implications for the Effective Removal or Delivery of Ibuprofen.

    Directory of Open Access Journals (Sweden)

    Shanmuga Kittappa

    Full Text Available Mesoporous silica materials (MSMs were synthesized economically using silica (SiO2 as a precursor via a modified alkaline fusion method. The MSM prepared at 500°C (MSM-500 had the highest surface area, pore size, and volume, and the results of isotherms and the kinetics of ibuprofen (IBP removal indicated that MSM-500 had the highest sorption capacity and fastest removal speed vs. SBA-15 and zeolite. Compared with commercial granular activated carbon (GAC, MSM-500 had a ~100 times higher sorption rate at neutral pH. IBP uptake by MSM-500 was thermodynamically favorable at room temperature, which was interpreted as indicating relatively weak bonding because the entropy (∆adsS, -0.07 J mol(-1 K(-1 was much smaller. Five times recycling tests revealed that MSM-500 had 83-87% recovery efficiencies and slower uptake speeds due to slight deformation of the outer pore structure. In the IBP delivery test, MSM-500 drug loading was 41%, higher than the reported value of SBA-15 (31%. The in vitro release of IBP was faster, almost 100%, reaching equilibrium within a few hours, indicating its effective loading and unloading characteristics. A cost analysis study revealed that the MSM was ~10-70 times cheaper than any other mesoporous silica material for the removal or delivery of IBP.

  12. Amine bridges grafted mesoporous silica, as a prolonged/controlled drug release system for the enhanced therapeutic effect of short life drugs

    International Nuclear Information System (INIS)

    Rehman, Fozia; Ahmed, Khalid; Airoldi, Claudio; Gaisford, Simon; Buanz, Asma; Rahim, Abdur; Muhammad, Nawshad; Volpe, Pedro L.O.

    2017-01-01

    Hybrid mesoporous silica SBA-15, with surface incorporated cross-linked long hydrophobic organic bridges was synthesized using stepwise synthesis. The synthesized materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-rays diffraction, thermogravimetry and scanning and transmission electron microscopy. The functionalized material showed highly ordered mesoporous network with a surface area of 629.0 m 2 g −1 . The incorporation of long hydrophobic amine chains on silica surface resulted in high drug loading capacity (21% Mass/Mass) and prolonged release of ibuprofen up till 75.5 h. The preliminary investigations suggests that the synthesized materials could be proposed as controlled release devices to prolong the therapeutic effect of short life drugs such as ibuprofen to increase its efficacy and to reduce frequent dosage. - Highlights: • Silica SBA-15 was synthesized and modified with long hydrophobic amine linkers. • These materials were characterized using different techniques. • The modified material showed high drug loading capacity and control ibuprofen release in biological fluids.

  13. Amine bridges grafted mesoporous silica, as a prolonged/controlled drug release system for the enhanced therapeutic effect of short life drugs

    Energy Technology Data Exchange (ETDEWEB)

    Rehman, Fozia, E-mail: foziaics@yahoo.com [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084–971 Campinas, SP (Brazil); Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Ahmed, Khalid; Airoldi, Claudio [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084–971 Campinas, SP (Brazil); Gaisford, Simon; Buanz, Asma [UCL School of Pharmacy, University College London, 29-39 Brunswick Square, London WC1N 1AX (United Kingdom); Rahim, Abdur; Muhammad, Nawshad [Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Volpe, Pedro L.O. [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084–971 Campinas, SP (Brazil)

    2017-03-01

    Hybrid mesoporous silica SBA-15, with surface incorporated cross-linked long hydrophobic organic bridges was synthesized using stepwise synthesis. The synthesized materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-rays diffraction, thermogravimetry and scanning and transmission electron microscopy. The functionalized material showed highly ordered mesoporous network with a surface area of 629.0 m{sup 2} g{sup −1}. The incorporation of long hydrophobic amine chains on silica surface resulted in high drug loading capacity (21% Mass/Mass) and prolonged release of ibuprofen up till 75.5 h. The preliminary investigations suggests that the synthesized materials could be proposed as controlled release devices to prolong the therapeutic effect of short life drugs such as ibuprofen to increase its efficacy and to reduce frequent dosage. - Highlights: • Silica SBA-15 was synthesized and modified with long hydrophobic amine linkers. • These materials were characterized using different techniques. • The modified material showed high drug loading capacity and control ibuprofen release in biological fluids.

  14. Effect of sintering temperature variations on fabrication of 45S5 bioactive glass-ceramics using rice husk as a source for silica.

    Science.gov (United States)

    Leenakul, Wilaiwan; Tunkasiri, Tawee; Tongsiri, Natee; Pengpat, Kamonpan; Ruangsuriya, Jetsada

    2016-04-01

    45S5 bioactive glass is a highly bioactive substance that has the ability to promote stem cell differentiation into osteoblasts--the cells that create bone matrix. The aim of this work is to analyze physical and mechanical properties of 45S5 bioactive glass fabricated by using rice husk ash as its silica source. The 45S5 bioactive glass was prepared by melting the batch at 1300 °C for 3h. The samples were sintered at different temperatures ranging from 900 to 1050 °C with a fixed dwell-time of 2h. The phase transitions, density, porosity and microhardness values were investigated and reported. DTA analysis was used to examine the crystallization temperatures of the glasses prepared. We found that the sintering temperature had a significant effect on the mechanical and physical properties of the bioactive glass. The XRD showed that when the sintering temperature was above 650 °C, crystallization occurred and bioactive glass-ceramics with Na2Ca2Si3O9, Na2Ca4(PO4)2SiO4 and Ca3Si2O7 were formed. The optimum sintering temperature resulting in maximum mechanical values was around 1050 °C, with a high density of 2.27 g/cm(3), 16.96% porosity and the vicker microhardness value of 364HV. Additionally, in vitro assay was used to examine biological activities in stimulated body fluid (SBF). After incubation in SBF for 7 days, all of the samples showed formations of apatite layers indicating that the 45S5 bioactive glasses using rice husk as a raw material were also bioactive. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Modeling of boldine alkaloid adsorption onto pure and propyl-sulfonic acid-modified mesoporous silicas. A comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Geszke-Moritz, Małgorzata, E-mail: Malgorzata.Geszke-Moritz@amu.edu.pl [NanoBioMedical Centre, Adam Mickiewicz University, Umultowska 85, 61-614 Poznań (Poland); Moritz, Michał, E-mail: michal.moritz@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemistry and Technical Electrochemistry, Berdychowo 4, 60-965 Poznań (Poland)

    2016-12-01

    The present study deals with the adsorption of boldine onto pure and propyl-sulfonic acid-functionalized SBA-15, SBA-16 and mesocellular foam (MCF) materials. Siliceous adsorbents were characterized by nitrogen sorption analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier-transform infrared (FT-IR) spectroscopy and thermogravimetric analysis. The equilibrium adsorption data were analyzed using the Langmuir, Freundlich, Redlich-Peterson, and Temkin isotherms. Moreover, the Dubinin-Radushkevich and Dubinin-Astakhov isotherm models based on the Polanyi adsorption potential were employed. The latter was calculated using two alternative formulas including solubility-normalized (S-model) and empirical C-model. In order to find the best-fit isotherm, both linear regression and nonlinear fitting analysis were carried out. The Dubinin-Astakhov (S-model) isotherm revealed the best fit to the experimental points for adsorption of boldine onto pure mesoporous materials using both linear and nonlinear fitting analysis. Meanwhile, the process of boldine sorption onto modified silicas was described the best by the Langmuir and Temkin isotherms using linear regression and nonlinear fitting analysis, respectively. The values of adsorption energy (below 8 kJ/mol) indicate the physical nature of boldine adsorption onto unmodified silicas whereas the ionic interactions seem to be the main force of alkaloid adsorption onto functionalized sorbents (energy of adsorption above 8 kJ/mol). - Graphical abstract: Modeling of boldine adsorption onto unmodified and propyl-sulfonic acid-modified mesoporous adsorbents. - Highlights: • The process of boldine adsorption onto SBA-15, SBA-16 and MCF silicas was examined. • Siliceous adsorbents were functionalized with propyl-sulfonic acid groups. • The equilibrium adsorption data were analyzed using several isotherm models. • Both linear regression and nonlinear fitting analysis were carried out.

  16. Liquid Phase Deposition of Silica on the Hexagonally Close-Packed Monolayer of Silica Spheres

    Directory of Open Access Journals (Sweden)

    Seo Young Yoon

    2013-01-01

    Full Text Available Liquid phase deposition is a method used for the nonelectrochemical production of polycrystalline ceramic films at low temperatures, most commonly silicon dioxide films. Herein, we report that silica spheres are organized in a hexagonal close-packed array using a patterned substrate. On this monolayer of silica spheres, we could fabricate new nanostructures in which deposition and etching compete through a modified LPD reaction. In the early stage, silica spheres began to undergo etching, and then, silica bridges between the silica spheres appeared by the local deposition reaction. Finally, the silica spheres and bridges disappeared completely. We propose the mechanism for the formation of nanostructure.

  17. Chlorodiethylaluminum supported on silica: A dinuclear aluminum surface species with bridging μ2-Cl-ligand as a highly efficient co-catalyst for the Ni-catalyzed dimerization of ethene

    KAUST Repository

    Kermagoret, Anthony

    2014-05-01

    Silica-supported chloro alkyl aluminum co-catalysts (DEAC@support) were prepared via Surface Organometallic Chemistry by contacting diethylaluminum chloride (DEAC) and high specific surface silica materials, i.e. SBA-15, MCM-41, and Aerosil SiO2. Such systems efficiently activate NiCl 2(PBu3)2 for catalytic ethene dimerization, with turnover frequency (TOF) reaching up to 498,000 molC2H4/ (molNi h) for DEAC@MCM-41. A detailed analysis of the DEAC@SBA-15 co-catalyst structure by solid-state aluminum-27 NMR at high-field (17.6 T and 20.0 T) and ultrafast spinning rates allows to detect six sites, characterized by a distribution of quadrupolar interaction principal values CQ and isotropic chemical shifts δiso. Identification of the corresponding Al-grafted structures was possible by comparison of the experimental NMR signatures with these calculated by DFT on a wide range of models for the aluminum species (mono- versus di-nuclear, mono- versus bis-grafted with bridging Cl or ethyl). Most of the sites were identified as dinuclear species with retention of the structure of DEAC, namely with the presence of μ2-Cl-ligands between two aluminum, and this probably explains the high catalytic performance of this silica-supported co-catalysts. © 2014 Elsevier Inc. All rights reserved.

  18. Single-Site Tetracoordinated Aluminum Hydride Supported on Mesoporous Silica. From Dream to Reality!

    KAUST Repository

    Werghi, Baraa

    2016-09-26

    The reaction of mesoporous silica (SBA15) dehydroxylated at 700 °C with diisobutylaluminum hydride, i-Bu2AlH, gives after thermal treatment a single-site tetrahedral aluminum hydride with high selectivity. The starting aluminum isobutyl and the final aluminum hydride have been fully characterized by FT-IR, advanced SS NMR spectroscopy (1H, 13C, multiple quanta (MQ) 2D 1H-1H, and 27Al), and elemental analysis, while DFT calculations provide a rationalization of the occurring reactivity. Trimeric i-Bu2AlH reacts selectively with surface silanols without affecting the siloxane bridges. Its analogous hydride catalyzes ethylene polymerization. Indeed, catalytic tests show that this single aluminum hydride site is active in the production of a high-density polyethylene (HDPE). © 2016 American Chemical Society.

  19. A novel method for preparation of 8-hydroxyquinoline functionalized mesoporous silica: Aluminum complexes and photoluminescence studies

    Energy Technology Data Exchange (ETDEWEB)

    Badiei, Alireza, E-mail: abadiei@khayam.ut.ac.ir [School of Chemistry, College of Science, University of Tehran, P.O. Box 14155-6455, Tehran (Iran, Islamic Republic of); Goldooz, Hassan [Department of Chemistry, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Ziarani, Ghodsi Mohammadi [Department of Chemistry, Faculty of Science, Alzahra University, Tehran (Iran, Islamic Republic of)

    2011-03-15

    8-Hydroxyquinoline (8-HQ) was attached to mesoporous silica by sulfonamide bond formation between 8-hydroxyquinoline-5-sulfonyl chloride (8-HQ-SO{sub 2}Cl) and aminopropyl functionalized SBA-15 (designated as SBA-SPS-Q) and then aluminum complexes of 8-HQ was covalently bonded to SBA-SPS-Q using coordinating ability of grafted 8-HQ.The prepared materials were characterized by powder X-ray diffraction (XRD), nitrogen adsorption-desorption, Fourier transform infrared (FT-IR), thermal analysis (TGA-DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), elemental analysis and fluorescence spectra. The environmental effects on the emission spectra of grafted 8-HQ and its complexes were studied and discussed in details.

  20. Single-Site Tetracoordinated Aluminum Hydride Supported on Mesoporous Silica. From Dream to Reality!

    KAUST Repository

    Werghi, Baraa; Bendjeriou-Sedjerari, Anissa; Jedidi, Abdesslem; Abou-Hamad, Edy; Cavallo, Luigi; Basset, Jean-Marie

    2016-01-01

    The reaction of mesoporous silica (SBA15) dehydroxylated at 700 °C with diisobutylaluminum hydride, i-Bu2AlH, gives after thermal treatment a single-site tetrahedral aluminum hydride with high selectivity. The starting aluminum isobutyl and the final aluminum hydride have been fully characterized by FT-IR, advanced SS NMR spectroscopy (1H, 13C, multiple quanta (MQ) 2D 1H-1H, and 27Al), and elemental analysis, while DFT calculations provide a rationalization of the occurring reactivity. Trimeric i-Bu2AlH reacts selectively with surface silanols without affecting the siloxane bridges. Its analogous hydride catalyzes ethylene polymerization. Indeed, catalytic tests show that this single aluminum hydride site is active in the production of a high-density polyethylene (HDPE). © 2016 American Chemical Society.

  1. Spectroscopy of nanosized composites silicon-organic polymer/nanoporous silicas

    International Nuclear Information System (INIS)

    Ostapenko, N.; Kozlova, N.; Suto, S.; Watanabe, A.

    2006-01-01

    Fluorescence and excitation spectra (T=5-290 K) of nanosized silicon-organic polymers poly(di-n-hexylsilane) and poly(methyl(phenyl)silane) incorporated into porous silica materials MCM-41 and SBA-15 have been studied with varying pore diameter from 2.8 to 10 nm. The controlled variation of the pore diameter in a wide range (2.8-10 nm) permitted us, for the first time, to investigate the optical properties of the polymers on their transition from isolated macromolecules to a film. It is found that this transition depends on polymer type and occurs via the formation of new spatially independent structures of the polymers not observed in the spectra of the film, namely, via the formation of disordered and (or) ordered conformations of polymer chains and clusters

  2. Selective production of oxygenates from CO2 hydrogenation over mesoporous silica supported Cu-Ga nanocomposite catalyst

    KAUST Repository

    Huang, Kuo-Wei

    2017-11-23

    Carbon dioxide hydrogenation to oxygenates (methanol and dimethyl ether (DME)) was investigated over bifunctional supported copper catalysts promoted with gallium (Ga). Supported Cu-Ga nanocomposite catalysts were characterized by X-ray diffraction, transmission electron microscopy with energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy and H2 temperature programmed reduction. In comparison with Cu-SBA-15 based catalysts, Ga promoted catalysts prepared by the urea deposition method (CuGa/SBA-15-UDP) was found active and selective for CO2 hydrogenation to oxygenates. The use of Ga as the promoter showed increased acidic sites as confirmed by the NH3-TPD, Pyridine-IR and 2,6-lutidine-IR studies. The favorable effect of Ga on CO2 conversion and selectivity to oxygenate may come from the strong interaction of Ga with silica, which is responsible for the enhanced metal surface area, formation of nanocomposite and metal dispersion. Notably, incorporation of Ga to Cu/SiO2 showed a several-fold higher rate for methanol formation (13.12 mol/gCu·sec) with a reasonable rate for the DME formation (2.15 mol/gCu·sec) as compared to those of Cu/SiO2 catalysts.

  3. Application of nanoporous silicas as adsorbents for chlorinated aromatic compounds. A comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Moritz, Michał, E-mail: michal.moritz@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemistry and Technical Electrochemistry, Piotrowo 3, 60-965 Poznań (Poland); Adam Mickiewicz University, Faculty of Chemistry, Umultowska 89b, 61-614 Poznań (Poland); Geszke-Moritz, Małgorzata, E-mail: Malgorzata.Geszke-Moritz@amu.edu.pl [NanoBioMedical Centre, Adam Mickiewicz University, Umultowska 85, 61-614 Poznań (Poland)

    2014-08-01

    The removal of two selected environmental pollutants such as 2,4-dichlorophenoxyacetic acid (2,4-D) and Triclosan (TC) was examined by adsorption experiments on the modified SBA-15 and MCF mesoporous silicas. Mesoporous adsorbents were modified by a grafting process with (3-aminopropyl)triethoxysilane (APTES) and 1-[3-(trimethoxysilyl)propyl]urea (TMSPU). Mesoporous materials were synthesized and characterized by N{sub 2} adsorption–desorption experiment, transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), elemental analysis and adsorption studies. The results show that both APTES-functionalized SBA-15 and MCF nanoporous carriers are potentially good adsorbents for the removal of 2,4-D in a wide range of concentrations from 0.1 to 4 mg/cm{sup 3}. Maximum adsorption capacity of as-modified adsorbents for 2,4-D estimated from the Langmuir model was ∼ 280 mg/g. The ionic interaction between the adsorbent and 2,4-D seems to play a key role in the adsorption process of the pollutant on APTES-modified siliceous matrices. The efficiency of TC sorption onto all prepared mesoporous adsorbents was significantly lower as compared to the entrapment of 2,4-D. Experimental data were best fitted by the Langmuir isotherm model. The results of this study suggest that mesoporous silica-based materials are promising adsorbents for the removal of selected organic pollutants. - Graphical abstract: Adsorption of 2,4-dichlorophenoxyacetic acid and Triclosan inside 3-amino-functionalized mesoporous channel.

  4. Silica Nephropathy

    Directory of Open Access Journals (Sweden)

    N Ghahramani

    2010-06-01

    Full Text Available Occupational exposure to heavy metals, organic solvents and silica is associated with a variety of renal manifestations. Improved understanding of occupational renal disease provides insight into environmental renal disease, improving knowledge of disease pathogenesis. Silica (SiO2 is an abundant mineral found in sand, rock, and soil. Workers exposed to silica include sandblasters, miners, quarry workers, masons, ceramic workers and glass manufacturers. New cases of silicosis per year have been estimated in the US to be 3600–7300. Exposure to silica has been associated with tubulointerstitial disease, immune-mediated multisystem disease, chronic kidney disease and end-stage renal disease. A rare syndrome of painful, nodular skin lesions has been described in dialysis patients with excessive levels of silicon. Balkan endemic nephropathy is postulated to be due to chronic intoxication with drinking water polluted by silicates released during soil erosion. The mechanism of silica nephrotoxicity is thought to be through direct nephrotoxicity, as well as silica-induced autoimmune diseases such as scleroderma and systemic lupus erythematosus. The renal histopathology varies from focal to crescentic and necrotizing glomerulonephritis with aneurysm formation suggestive of polyarteritis nodosa. The treatment for silica nephrotoxicity is non-specific and depends on the mechanism and stage of the disease. It is quite clear that further research is needed, particularly to elucidate the pathogenesis of silica nephropathy. Considering the importance of diagnosing exposure-related renal disease at early stages, it is imperative to obtain a thorough occupational history in all patients with renal disease, with particular emphasis on exposure to silica, heavy metals, and solvents.

  5. The enhancement of photoresponse of an ordered inorganic-organic hybrid architecture by increasing interfacial contacts

    International Nuclear Information System (INIS)

    Zhang Bin; Chen Xudong; Ma Shaohua; Yang Jin; Zhang Mingqiu; Chen Yujie

    2010-01-01

    A modified ZnO quantum dot/polythiophene (ZnO/PTh) inorganic-organic hybrid architecture was fabricated by using ordered mesoporous silica (SBA-15) as the retaining template. First, a two-step strategy was developed to synthesize an ordered organic conducting polymer composite (PTh/SBA-15). Then, ZnO quantum dots were in situ formed on the pore walls of the ordered PTh/SBA-15 composite. Photoresponse of the inorganic-organic hybrid was studied with respect to its incident photon to collected electron conversion efficiency (IPCE) and morphology. The presence of SBA-15 proved to be critical for controlling the interfacial morphology and hence enlarging the interfacial area of the inorganic-organic heterojunction. The proposed approach may act as a key method to open up potential applications in photovoltaic devices.

  6. The enhancement of photoresponse of an ordered inorganic-organic hybrid architecture by increasing interfacial contacts.

    Science.gov (United States)

    Zhang, Bin; Chen, Xudong; Ma, Shaohua; Chen, Yujie; Yang, Jin; Zhang, Mingqiu

    2010-02-10

    A modified ZnO quantum dot/polythiophene (ZnO/PTh) inorganic-organic hybrid architecture was fabricated by using ordered mesoporous silica (SBA-15) as the retaining template. First, a two-step strategy was developed to synthesize an ordered organic conducting polymer composite (PTh/SBA-15). Then, ZnO quantum dots were in situ formed on the pore walls of the ordered PTh/SBA-15 composite. Photoresponse of the inorganic-organic hybrid was studied with respect to its incident photon to collected electron conversion efficiency (IPCE) and morphology. The presence of SBA-15 proved to be critical for controlling the interfacial morphology and hence enlarging the interfacial area of the inorganic-organic heterojunction. The proposed approach may act as a key method to open up potential applications in photovoltaic devices.

  7. Photocatalytic removal of Congo red dye using MCM-48/Ni2O3 composite synthesized based on silica gel extracted from rice husk ash; fabrication and application.

    Science.gov (United States)

    Shaban, Mohamed; Abukhadra, Mostafa R; Hamd, Ahmed; Amin, Ragab R; Abdel Khalek, Ahmed

    2017-12-15

    MCM-48 mesoporous silica was successfully synthesized from silica gel extracted from rice husk ash and loaded by nickel oxide (Ni 2 O 3 ). The resulted composite was characterized using X-ray diffraction, scanning electron microscope, and UV-vis spectrophotometer. The role of MCM-48 as catalyst support in enhancing the photocatalytic properties of nickel oxide was evaluated through the photocatalytic degradation of Congo red dye under visible light source. MCM-48 as catalyst support for Ni 2 O 3 shows considerable enhancement in the adsorption capacity by 17% and 29% higher than the adsorption capacity of MCM-48 and Ni 2 O 3 , respectively. Additionally, the photocatalytic degradation percentage increased by about 64% relative to the degradation percentage using Ni 2 O 3 as a single component. The adsorption mechanism of MCM-48/Ni 2 O 3 is chemisorption process of multilayer form. The using of MCM-48 as catalyst support for Ni 2 O 3 enhanced the adsorption capacity and the photocatalytic degradation through increasing the surface area and prevents the nickel oxide particles from agglomeration. This was done through fixing nickel oxide particles throughout the porous structure which providing more exposed active adsorption sites and active photocatalyst sites for the incident photons. Based on the obtained results, supporting of nickel oxide particles onto MCM-48 are promising active centers for the degradation of Congo red dye molecules. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. A membrane electrode assembled photoelectrochemical cell with a solar-responsive cadmium sulfide-zinc sulfide-titanium dioxide/mesoporous silica photoanode

    Science.gov (United States)

    Chen, Ming; Chen, Rong; Zhu, Xun; Liao, Qiang; An, Liang; Ye, Dingding; Zhou, Yuan; He, Xuefeng; Zhang, Wei

    2017-12-01

    In this work, a membrane electrode assembled photoelectrochemical cell (PEC) is developed for the electricity generation by degrading the organic compounds. The photocatalyst is prepared by the incorporation of mesoporous silica SBA-15 into TiO2 and the photosensitization of CdS-ZnS to enhance the photoanode performance, while the cathode employs the air-breathing mode to enhance the oxygen transport. The experimental results show that the developed PEC exhibits good photoresponse to the illumination and the appropriate SBA-15 mass ratio in the photoanode enables the enhancement of the performance. It is also shown that the developed PEC yields better performance in the alkaline environment than that in the neutral environment. Increasing the KOH concentration can improve the cell performance. There exist optimal liquid flow rate and organics concentration leading to the best performance. Besides, it is found that increasing the light intensity can generate more electron-hole pairs and thus enhance the cell performance. These results are helpful for optimizing the design.

  9. Determination of picomolar silver concentrations by differential pulse anodic stripping voltammetry at a carbon paste electrode modified with phenylthiourea-functionalized high ordered nanoporous silica gel

    International Nuclear Information System (INIS)

    Javanbakht, Mehran; Divsar, Faten; Badiei, Alireza; Fatollahi, Fatemeh; Khaniani, Yeganeh; Ganjali, Mohammad Reza; Norouzi, Parviz; Chaloosi, Marzieh; Ziarani, Ghodsi Mohammadi

    2009-01-01

    This study introduces the design of an anodic stripping voltammetric (ASV) method for the silver ion determination at a carbon paste electrode (CPE), chemically modified with phenylthiourea-nanoporous silica gel (Tu-SBA-15-CPE). The electroanalytical pro includes two steps: preconcentration of metal ions at an electrode surface, followed by quantification of the accumulated species by differential pulse anodic stripping voltammetric methods. Factors affecting the performance of the anodic stripping were investigated, including the modifier quantity in the paste, the electrolyte concentrations, the solution pH and the accumulation potential or time. The most sensitive and reliable electrode contained 10% Tu-SBA-15 and 90% carbon paste. The accumulation potential and time were set at, -200 mV and 300 s, respectively, and the scan rate at 50 mV s -1 in the scan range of -200 to 700 mV. The resulting electrode demonstrated a linear response over range of silver ion concentration of 8.0-80 pmol/L with detection limit (S/N = 3) of 5 pmol/L. The prepared electrodes were used for the silver determination in sea and tap water samples and very good recovery results were obtained. The accuracy was assessed through recovery experiments and independent analysis by graphite furnace atomic absorption spectrometry.

  10. Determination of picomolar silver concentrations by differential pulse anodic stripping voltammetry at a carbon paste electrode modified with phenylthiourea-functionalized high ordered nanoporous silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Javanbakht, Mehran [Department of Chemistry, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Nano Science and Technology Research Center, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of)], E-mail: mehranjavanbakht@gmail.com; Divsar, Faten [Department of Chemistry, University of Tarbiat Moallem, Tehran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, University College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Fatollahi, Fatemeh [Department of Chemistry, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Khaniani, Yeganeh [School of Chemistry, University College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Ganjali, Mohammad Reza; Norouzi, Parviz [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Chaloosi, Marzieh [Department of Chemistry, University of Tarbiat Moallem, Tehran (Iran, Islamic Republic of); Ziarani, Ghodsi Mohammadi [Department of Chemistry, University of Alzahra, Tehran (Iran, Islamic Republic of)

    2009-09-30

    This study introduces the design of an anodic stripping voltammetric (ASV) method for the silver ion determination at a carbon paste electrode (CPE), chemically modified with phenylthiourea-nanoporous silica gel (Tu-SBA-15-CPE). The electroanalytical pro includes two steps: preconcentration of metal ions at an electrode surface, followed by quantification of the accumulated species by differential pulse anodic stripping voltammetric methods. Factors affecting the performance of the anodic stripping were investigated, including the modifier quantity in the paste, the electrolyte concentrations, the solution pH and the accumulation potential or time. The most sensitive and reliable electrode contained 10% Tu-SBA-15 and 90% carbon paste. The accumulation potential and time were set at, -200 mV and 300 s, respectively, and the scan rate at 50 mV s{sup -1} in the scan range of -200 to 700 mV. The resulting electrode demonstrated a linear response over range of silver ion concentration of 8.0-80 pmol/L with detection limit (S/N = 3) of 5 pmol/L. The prepared electrodes were used for the silver determination in sea and tap water samples and very good recovery results were obtained. The accuracy was assessed through recovery experiments and independent analysis by graphite furnace atomic absorption spectrometry.

  11. Conductivity of liquid lithium electrolytes with dispersed mesoporous silica particles

    International Nuclear Information System (INIS)

    Sann, K.; Roggenbuck, J.; Krawczyk, N.; Buschmann, H.; Luerßen, B.; Fröba, M.; Janek, J.

    2012-01-01

    Highlights: ► The conductivity of disperse lithium electrolytes with mesoporous fillers is studied. ► In contrast to other investigations in literature, no conductivity enhancement could be observed for standard battery electrolytes and typical mesoporous fillers in various combinations. ► Disperse electrolytes can become relevant in terms of battery safety. ► Dispersions of silicas and electrolyte with LiPF 6 as conducting salt are not stable, although the silicas were dried prior to preparation and the electrolyte water content was controlled. Surface modification of the fillers improved the stability. ► The observed conductivity decrease varied considerably for various fillers. - Abstract: The electrical conductivity of disperse electrolytes was systematically measured as a function of temperature (0 °C to 60 °C) and filler content for different types of fillers with a range of pore geometry, pore structure and specific surface area. As fillers mesoporous silicas SBA-15, MCM-41 and KIT-6 with pore ranges between 3 nm and 15 nm were dispersed in commercially available liquid lithium electrolytes. As electrolytes 1 M of lithium hexafluorophosphate (LiPF 6 ) in a mixture of ethylene carbonate (EC) and diethylene carbonate (DEC) at the ratio 3:7 (wt/wt) and the same solvent mixture with 0.96 M lithium bis(trifluoromethanesulfon)imide (LiTFSI) were used. No conductivity enhancement could be observed, but with respect to safety aspects the highly viscous disperse pastes might be useful. The conductivity decrease varied considerably for the different fillers.

  12. Deep glass etched microring resonators based on silica-on-silicon technology

    DEFF Research Database (Denmark)

    Ou, Haiyan; Rottwitt, Karsten; Philipp, Hugh Taylor

    2006-01-01

    Microring resonators fabricated on silica-on-silicon technology using deep glass etching are demonstrated. The fabrication procedures are introduced and the transmission spectrum of a resonator is presented.......Microring resonators fabricated on silica-on-silicon technology using deep glass etching are demonstrated. The fabrication procedures are introduced and the transmission spectrum of a resonator is presented....

  13. Ordered mesoporous polymer-silica hybrid nanoparticles as vehicles for the intracellular controlled release of macromolecules.

    Science.gov (United States)

    Kim, Tae-Wan; Slowing, Igor I; Chung, Po-Wen; Lin, Victor Shang-Yi

    2011-01-25

    A two-dimensional hexagonal ordered mesoporous polymer-silica hybrid nanoparticle (PSN) material was synthesized by polymerization of acrylate monomers on the surface of SBA-15 mesoporous silica nanoparticles. The structure of the PSN material was analyzed using a series of different techniques, including transmission electron microscopy, powder X-ray diffraction, and N(2) sorption analysis. These structurally ordered mesoporous polymer-silica hybrid nanoparticles were used for the controlled release of membrane-impermeable macromolecules inside eukaryotic cells. The cellular uptake efficiency and biocompatibility of PSN with human cervical cancer cells (HeLa) were investigated. Our results show that the inhibitory concentration (IC(50)) of PSN is very high (>100 μg/mL per million cells), while the median effective concentration for the uptake (EC(50)) of PSN is low (EC(50) = 4.4 μg/mL), indicating that PSNs are fairly biocompatible and easily up-taken in vitro. A membrane-impermeable macromolecule, 40 kDa FITC-Dextran, was loaded into the mesopores of PSNs at low pH. We demonstrated that the PSN material could indeed serve as a transmembrane carrier for the controlled release of FITC-Dextran at the pH level inside live HeLa cells. We believe that further developments of this PSN material will lead to a new generation of nanodevices for intracellular controlled delivery applications.

  14. Investigating in vitro bioactivity and magnetic properties of the ferrimagnetic bioactive glass–ceramic fabricated using soda-lime–silica waste glass

    Energy Technology Data Exchange (ETDEWEB)

    Abbasi, M. [Department of Materials Science and Engineering, School of Engineering, Shiraz University, Zand Street, Shiraz (Iran, Islamic Republic of); Hashemi, B., E-mail: hashemib@shirazu.ac.ir [Department of Materials Science and Engineering, School of Engineering, Shiraz University, Zand Street, Shiraz (Iran, Islamic Republic of); Shokrollahi, H. [Electroceramics Group, Materials Science and Engineering Department, Shiraz University of Technology, Shiraz (Iran, Islamic Republic of)

    2014-04-01

    The main purpose of the current research is the production and characterization of a ferrimagnetic bioactive glass–ceramic prepared through the solid-state reaction method using soda-lime–silica waste glass as the main raw material. In comparison with the conventional route, that is, the melt-quenching and subsequent heat treatment, the present work is an economical technique. Structural, thermal and magnetic properties of the samples were examined by X-ray diffraction (XRD), differential thermal analysis (DTA) and vibrating sample magnetometer (VSM). The in vitro test was utilized to assess the bioactivity level of the samples by Hanks' solution as simulated body fluid (SBF). The apatite surface layer formation was examined by the scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS). The calcium ion concentration in the solutions was measured by atomic absorption spectroscopy (AAS). VSM results revealed that with the addition of 5–20 wt% strontium hexaferrite to bioactive glass–ceramics, the ferrimagnetic bioactive glass–ceramics with hysteresis losses between 7024 and 75,852 erg/g were obtained. The in vitro test showed that the onset formation time of hydroxyapatite layer on the surface of the samples was 14 days and after 30 days, this layer was completed. - Highlights: • A novel ferrimagnetic bioactive glass–ceramic was synthesized by an incorporation method. • The bioactive part was synthesized by the solid-state reaction method using soda-lime–silica waste glass. • The doping of SrFe{sub 12}O{sub 19} to Bioglass{sup ®} 45S5 glass–ceramic is likely to decrease bioactivity.

  15. C-H and C-C activation of n -butane with zirconium hydrides supported on SBA15 containing N-donor ligands: [(≡SiNH-)(≡SiX-)ZrH2], [(≡SiNH-)(≡SiX-)2ZrH], and[(≡SiN=)(≡SiX-)ZrH] (X = -NH-, -O-). A DFT study

    KAUST Repository

    Pasha, Farhan Ahmad

    2014-07-01

    Density functional theory (DFT) was used to elucidate the mechanism of n-butane hydrogenolysis (into propane, ethane, and methane) on well-defined zirconium hydrides supported on SBA15 coordinated to the surface via N-donor surface pincer ligands: [(≡SiNH-)(≡SiO-)ZrH2] (A), [(≡SiNH-)2ZrH2] (B), [(≡SiNH-)(≡SiO-) 2ZrH] (C), [(≡SiNH-)2(≡SiO-)ZrH] (D), [(≡SiN=)(≡Si-O-)ZrH] (E), and [(≡SiN=)(≡SiNH-)ZrH] (F). The roles of these hydrides have been investigated in C-H/C-C bond activation and cleavage. The dihydride A linked via a chelating [N,O] surface ligand was found to be more active than B, linked to the chelating [N,N] surface ligand. Moreover, the dihydride zirconium complexes are also more active than their corresponding monohydrides C-F. The C-C cleavage step occurs preferentially via β-alkyl transfer, which is the rate-limiting step in the alkane hydrogenolysis. The energetics of the comparative pathways over the potential energy surface diagram (PES) reveals the hydrogenolysis of n-butane into propane and ethane. © 2014 American Chemical Society.

  16. Planar and channel waveguides in fused silica fabricated by multi-energy C ion in the visible and near-infrared band

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Tao; Huang, Qing; Liu, Peng; Guo, Sha-Sha; Zhang, Lian; Zhou, Yu-Fan [School of Physics, State Key Laboratory of Crystal Materials and Key Laboratory of Particle Physics and Particle Irradiation (MOE), Shandong University, Jinan 250100 (China); Wang, Xue-Lin, E-mail: xuelinwang@sdu.edu.cn [School of Physics, State Key Laboratory of Crystal Materials and Key Laboratory of Particle Physics and Particle Irradiation (MOE), Shandong University, Jinan 250100 (China)

    2013-07-15

    Fused quartz is a key material in fabrication of integrated devices, which transmits extends from ultraviolet to infrared. We report the fabrication of planar and channel waveguides in fused quartz using multi-energy C ion at energies of (5 + 5.5 + 6) MeV and fluences of (1 + 1 + 1.5) × 10{sup 15} ions/cm{sup 2}. The guiding modes at the wavelength of 633 nm (He–Ne laser) and 1539 nm (diode laser) were detected using the prism-coupling method, and the modes were stable after annealing in air. The refractive index profiles of planar and channel waveguides at the wavelength of 633 nm and 1539 nm were typical “well + barrier” distributions, which were reconstructed using the reflectivity calculation method (RCM) software and intensity calculation method (ICM), respectively. For comparison to the experimental results, the finite difference beam propagation method (FD-BPM) was used to simulate the guiding modes of the waveguides. We measured the near-field intensity distributions for the visible (633 nm) and near-infrared (1300 nm, 1539 nm and 1620 nm) wavelength regions, suggesting that the modes can be effective transmission in the wavelength range for optical fiber communications.

  17. Fast determination of Ziziphora tenuior L. essential oil by inorganic-organic hybrid material based on ZnO nanoparticles anchored to a composite made from polythiophene and hexagonally ordered silica.

    Science.gov (United States)

    Piryaei, Marzieh; Abolghasemi, Mir Mahdi; Nazemiyeh, Hossein

    2015-01-01

    In this paper, for the first time, an inorganic-organic hybrid material based on ZnO nanoparticles was anchored to a composite made from polythiophene and hexagonally ordered silica (ZnO/PT/SBA-15) for use in solid-phase fibre microextraction (SPME) of medicinal plants. A homemade SPME apparatus was used for the extraction of volatile components of Ziziphora tenuior L. A simplex method was used for optimisation of five different parameters affecting the efficiency of the extraction. The main constituents extracted by ZnO/PT/SBA-15 and PDMS fibres and hydrodistillation (HD) methods, respectively, included pulegone (51.25%, 53.64% and 56.68%), limonene (6.73%, 6.58% and 8.3%), caryophyllene oxide (5.33%, 4.31% and 4.53%) and 1,8-cineole (4.21%, 3.31% and 3.18%). In comparison with the HD method, the proposed technique could equally monitor almost all the components of the sample, in an easier way, in a shorter time and requiring a much lower amount of the sample.

  18. Sustainable and long-time 'rejuvenation' of biomimetic water-repellent silica coating on polyester fabrics induced by rough mechanical abrasion.

    Science.gov (United States)

    Rosu, Cornelia; Lin, Haisheng; Jiang, Lu; Breedveld, Victor; Hess, Dennis W

    2018-04-15

    The economical use of water-repellent coatings on polymeric materials in commercial and industrial applications is limited by their mechanical wear robustness and long-term durability. In this study, we demonstrate that polyethylene terephthalate (PET) fabric modified with inorganic, methyltrimethoxysilane (MTMS)-based coatings shows excellent resistance against various types of wear damage, thereby mimicking superhydrophobic biological materials. These features were facilitated by the rational design of coating processing that also enabled tunable hierarchical surface structure. A series of custom and standard testing protocols revealed that coating-to-substrate adhesion was remarkably high, as was the resistance to various mechanical abradents. The most intriguing characteristic observed during aging and abrasion cycles was the enhancement in non-wettability or 'rejuvenation' reflected by water droplet roll-off behavior, a characteristic of self-cleaning materials. Water-repellent properties of coated polyester were also enhanced by prolonged thermal annealing and were maintained after custom laundry. The developed technology offers opportunities to design low cost, durable and functional textiles for both indoor and outdoor applications. Copyright © 2018 Elsevier Inc. All rights reserved.

  19. Influence of polymer matrix and adsorption onto silica materials on the migration of alpha-tocopherol into 95% ethanol from active packaging.

    Science.gov (United States)

    Heirlings, L; Siró, I; Devlieghere, F; Van Bavel, E; Cool, P; De Meulenaer, B; Vansant, E F; Debevere, J

    2004-11-01

    In this study, the effect of polymer materials with different polarity, namely low density polyethylene (LDPE) and ethylene vinyl acetate (EVA), on the migration behaviour of alpha-tocopherol from active packaging was investigated. The antioxidant was also adsorbed onto silica materials, namely SBA-15 (Santa Barbara-15) and Syloblock, in order to protect the antioxidant during extrusion and to ensure a controlled and sufficient release during the shelf-life of the food product. Migration experiments were performed at 7.0 +/- 0.5 degrees C and 95% ethanol was used as fatty food simulant. All films contained a high concentration of alpha-tocopherol, approximately 2000 mg kg(-1), to obtain an active packaging. Polymer matrix had a small influence on the migration profile. The migration of 80% of total migrated amount of antioxidant was retarded for 2.4 days by using LDPE instead of EVA. When alpha-tocopherol was adsorbed onto both silica materials, the migration of 80% of total migrated amount of antioxidant was retarded for 3.4 days in comparison to pure alpha-tocopherol. No difference was seen between the migration profiles of alpha-tocopherol adsorbed onto both silica materials. In the case of pure alpha-tocopherol, 82% of the initial amount of alpha-tocopherol in the film migrated into the food simulant at a rather fast migration rate. In the case of adsorption on silica materials, a total migration was observed. These antioxidative films can have positive food applications.

  20. Silica artificial opal incorporated with silver nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Li Wenjiang, E-mail: wjli@zju.edu.cn [Center for Optical and Electromagnetic Research, State Key Laboratory for Modern Optical Instrumentation, Zhejiang University, Joint Research Center of Photonics of the Royal Institute of Technology and Zhejiang University, Zijingang Campus, Room 210, East Building 5, Hangzhou 310058 (China); Sun Tan [Center for Optical and Electromagnetic Research, State Key Laboratory for Modern Optical Instrumentation, Zhejiang University, Joint Research Center of Photonics of the Royal Institute of Technology and Zhejiang University, Zijingang Campus, Room 210, East Building 5, Hangzhou 310058 (China)

    2009-07-15

    The silica artificial opal with a three-dimensional (3D) periodic structure was prepared using highly monodispersed silica microspheres by a force packing method in ITO glass cell. The silica artificial opal incorporated with silver nanoparticles was fabricated by the electroplating technique. The optical microscope images of the synthetic sample and the corresponding optical properties were measured after each treatment of electroplating-washing-drying circle. The transmission and reflection spectra presented a red shift, showing that the effective refractive index of the complex silver/silica opal increased after each electroplating. Combining the SEM images, it was seen that the silver nanoparticles could be directly deposited on the surface of silica spheres in the opaline structure. The silver/silica complex opal film could provide a simple way to tune the opal properties by controlling silver nanoparticles in the silica opal. The silver/silica opal crystal structures could be used for nano-photonic circuits, white-light LEDs or as photocatalysts.

  1. Silica artificial opal incorporated with silver nanoparticles

    International Nuclear Information System (INIS)

    Li Wenjiang; Sun Tan

    2009-01-01

    The silica artificial opal with a three-dimensional (3D) periodic structure was prepared using highly monodispersed silica microspheres by a force packing method in ITO glass cell. The silica artificial opal incorporated with silver nanoparticles was fabricated by the electroplating technique. The optical microscope images of the synthetic sample and the corresponding optical properties were measured after each treatment of electroplating-washing-drying circle. The transmission and reflection spectra presented a red shift, showing that the effective refractive index of the complex silver/silica opal increased after each electroplating. Combining the SEM images, it was seen that the silver nanoparticles could be directly deposited on the surface of silica spheres in the opaline structure. The silver/silica complex opal film could provide a simple way to tune the opal properties by controlling silver nanoparticles in the silica opal. The silver/silica opal crystal structures could be used for nano-photonic circuits, white-light LEDs or as photocatalysts.

  2. Nature and structure of aluminum surface sites grafted on silica from a combination of high-field aluminum-27 solid-state NMR spectroscopy and first-principles calculations

    KAUST Repository

    Kerber, Rachel Nathaniel; Kermagoret, Anthony; Callens, Emmanuel; Florian, Pierre A.; Massiot, Dominique; Lesage, Anne; Copé ret, Christophe; Delbecq, Franç oise; Rozanska, Xavier; Sautet, Philippe

    2012-01-01

    The determination of the nature and structure of surface sites after chemical modification of large surface area oxides such as silica is a key point for many applications and challenging from a spectroscopic point of view. This has been, for instance, a long-standing problem for silica reacted with alkylaluminum compounds, a system typically studied as a model for a supported methylaluminoxane and aluminum cocatalyst. While 27Al solid-state NMR spectroscopy would be a method of choice, it has been difficult to apply this technique because of large quadrupolar broadenings. Here, from a combined use of the highest stable field NMR instruments (17.6, 20.0, and 23.5 T) and ultrafast magic angle spinning (>60 kHz), high-quality spectra were obtained, allowing isotropic chemical shifts, quadrupolar couplings, and asymmetric parameters to be extracted. Combined with first-principles calculations, these NMR signatures were then assigned to actual structures of surface aluminum sites. For silica (here SBA-15) reacted with triethylaluminum, the surface sites are in fact mainly dinuclear Al species, grafted on the silica surface via either two terminal or two bridging siloxy ligands. Tetrahedral sites, resulting from the incorporation of Al inside the silica matrix, are also seen as minor species. No evidence for putative tri-coordinated Al atoms has been found. © 2012 American Chemical Society.

  3. Nature and structure of aluminum surface sites grafted on silica from a combination of high-field aluminum-27 solid-state NMR spectroscopy and first-principles calculations

    KAUST Repository

    Kerber, Rachel Nathaniel

    2012-04-18

    The determination of the nature and structure of surface sites after chemical modification of large surface area oxides such as silica is a key point for many applications and challenging from a spectroscopic point of view. This has been, for instance, a long-standing problem for silica reacted with alkylaluminum compounds, a system typically studied as a model for a supported methylaluminoxane and aluminum cocatalyst. While 27Al solid-state NMR spectroscopy would be a method of choice, it has been difficult to apply this technique because of large quadrupolar broadenings. Here, from a combined use of the highest stable field NMR instruments (17.6, 20.0, and 23.5 T) and ultrafast magic angle spinning (>60 kHz), high-quality spectra were obtained, allowing isotropic chemical shifts, quadrupolar couplings, and asymmetric parameters to be extracted. Combined with first-principles calculations, these NMR signatures were then assigned to actual structures of surface aluminum sites. For silica (here SBA-15) reacted with triethylaluminum, the surface sites are in fact mainly dinuclear Al species, grafted on the silica surface via either two terminal or two bridging siloxy ligands. Tetrahedral sites, resulting from the incorporation of Al inside the silica matrix, are also seen as minor species. No evidence for putative tri-coordinated Al atoms has been found. © 2012 American Chemical Society.

  4. Bioinspired silica as drug delivery systems and their biocompatibility

    DEFF Research Database (Denmark)

    Steven, Christopher R.; Busby, Grahame A.; Mather, Craig

    2014-01-01

    Silica nanoparticles have been shown to have great potential as drug delivery systems (DDS), however, their fabrication often involves harsh chemicals and energy intensive laborious methods. This work details the employment of a bioinspired "green" method for the controlled synthesis of silica, use...

  5. Active Iron Sites of Disordered Mesoporous Silica Catalyst FeKIL-2 in the Oxidation of Volatile Organic Compounds (VOC

    Directory of Open Access Journals (Sweden)

    Mojca Rangus

    2014-05-01

    Full Text Available Iron-functionalized disordered mesoporous silica (FeKIL-2 is a promising, environmentally friendly, cost-effective and highly efficient catalyst for the elimination of volatile organic compounds (VOCs from polluted air via catalytic oxidation. In this study, we investigated the type of catalytically active iron sites for different iron concentrations in FeKIL-2 catalysts using advanced characterization of the local environment of iron atoms by a combination of X-ray Absorption Spectroscopy Techniques (XANES, EXAFS and Atomic-Resolution Scanning Transmission Electron Microscopy (AR STEM. We found that the molar ratio Fe/Si ≤ 0.01 leads to the formation of stable, mostly isolated Fe3+ sites in the silica matrix, while higher iron content Fe/Si > 0.01 leads to the formation of oligonuclear iron clusters. STEM imaging and EELS techniques confirmed the existence of these clusters. Their size ranges from one to a few nanometers, and they are unevenly distributed throughout the material. The size of the clusters was also found to be similar, regardless of the nominal concentration of iron (Fe/Si = 0.02 and Fe/Si = 0.05. From the results obtained from sample characterization and model catalytic tests, we established that the enhanced activity of FeKIL-2 with the optimal Fe/Si = 0.01 ratio can be attributed to: (1 the optimal concentration of stable isolated Fe3+ in the silica support; and (2 accelerated diffusion of the reactants in disordered mesoporous silica (FeKIL-2 when compared to ordered mesoporous silica materials (FeSBA-15, FeMCM-41.

  6. RT Self-assembly of Silica Nanoparticles on Optical Fibres

    DEFF Research Database (Denmark)

    Canning, John; Lindoy, Lachlan; Huyang, George

    2013-01-01

    The room temperature deposition of self-assembling silica nanoparticles onto D-shaped optical fibres x201c;D-fibrex201d;), drawn from milled preforms fabricated by modified chemical vapor deposition, is studied and preliminary results reported here.......The room temperature deposition of self-assembling silica nanoparticles onto D-shaped optical fibres x201c;D-fibrex201d;), drawn from milled preforms fabricated by modified chemical vapor deposition, is studied and preliminary results reported here....

  7. Synthesis and characterization of mesoporous silica modified with chiral auxiliaries for their potential application as chiral stationary phase.

    Science.gov (United States)

    Mayani, Vishal J; Abdi, S H R; Kureshy, R I; Khan, N H; Agrawal, Santosh; Jasra, R V

    2008-05-16

    Novel chiral stationary phase (CSP) based on chiral aminoalcohol immobilized on ordered mesoporous silica SBA-15 1a and standard silica 1b and their copper complexes 1a' and 1b', respectively, was synthesized as potential material for chiral ligand exchange chromatography (CLEC). Microanalysis, inductively coupled plasma spectroscopy (ICP), thermo-gravimetric analysis (TGA), cross polarized magic angle spinning (CP-MAS) (13)C NMR, Powder X-ray diffraction (PXRD), FTIR, N(2) adsorption isotherm, scanning electron microscopy (SEM), transmitted electron microscope (TEM) and solid reflectance UV-vis spectroscopy were used to characterize these materials. All the chiral stationary phases thus synthesized were used for the separation of different racemic compounds such as mandelic acid, 2,2'-dihydroxy-1,1'-binaphthalene BINOL) and diethyl tartrate by simple medium-pressure column chromatography. Successful enantio-separation of racemic mandelic acid was achieved with all the stationary phases but 1a and 1b gave slightly better resolution than their copper complexes 1a' and 1b'. Remarkably these materials are stable under the given experimental conditions and can be used repeatedly for several cycles of enantioresolution. It was observed that the porosity and surface area of the stationary phase play an important role in the chiral separation.

  8. Magnetic solid-phase extraction based on mesoporous silica-coated magnetic nanoparticles for analysis of oral antidiabetic drugs in human plasma

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Karynne Cristina de; Andrade, Gracielle Ferreira [Centro de Desenvolvimento da Tecnologia Nuclear, CDTN/CNEN, Rua Professor Mário Werneck, s/n. Campus Universitário, Belo Horizonte, MG CEP 30.123-970 (Brazil); Vasconcelos, Ingrid; Oliveira Viana, Iara Maíra de; Fernandes, Christian [Departamento de Produtos Farmacêuticos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Belo Horizonte, MG (Brazil); Martins Barros de Sousa, Edésia, E-mail: sousaem@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear, CDTN/CNEN, Rua Professor Mário Werneck, s/n. Campus Universitário, Belo Horizonte, MG CEP 30.123-970 (Brazil)

    2014-07-01

    In the present work, magnetic nanoparticles embedded into mesoporous silica were prepared in two steps: first, magnetite was synthesized by oxidation–precipitation method, and next, the magnetic nanoparticles were coated with mesoporous silica by using nonionic block copolymer surfactants as structure-directing agents. The mesoporous SiO{sub 2}-coated Fe{sub 3}O{sub 4} samples were functionalized using octadecyltrimethoxysilane as silanizing agent. The pure and functionalized silica nanoparticles were physicochemically and morphologically characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), N{sub 2} adsorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The resultant magnetic silica nanoparticles were applied as sorbents for magnetic solid-phase extraction (MSPE) of oral antidiabetic drugs in human plasma. Our results revealed that the magnetite nanoparticles were completely coated by well-ordered mesoporous silica with free pores and stable pore walls, and that the structural and magnetic properties of the Fe{sub 3}O{sub 4} nanoparticles were preserved in the applied synthesis route. Indeed, the sorbent material was capable of extracting the antidiabetic drugs from human plasma, being useful for the sample preparation in biological matrices. - Highlights: • SBA-15/Fe{sub 3}O{sub 4} was synthesized and functionalized with octadecyltrimethoxysilane. • Magnetite nanoparticles were completely coated by well-ordered mesoporous silica. • The samples were used as sorbent for magnetic solid-phase extraction (MSPE). • The sorbent material was capable of extracting drugs from human plasma. • The extraction ability makes the material a candidate to be employed as MSPE.

  9. Grassy Silica Nanoribbons and Strong Blue Luminescence

    Science.gov (United States)

    Wang, Shengping; Xie, Shuang; Huang, Guowei; Guo, Hongxuan; Cho, Yujin; Chen, Jun; Fujita, Daisuke; Xu, Mingsheng

    2016-09-01

    Silicon dioxide (SiO2) is one of the key materials in many modern technological applications such as in metal oxide semiconductor transistors, photovoltaic solar cells, pollution removal, and biomedicine. We report the accidental discovery of free-standing grassy silica nanoribbons directly grown on SiO2/Si platform which is commonly used for field-effect transistors fabrication without other precursor. We investigate the formation mechanism of this novel silica nanostructure that has not been previously documented. The silica nanoribbons are flexible and can be manipulated by electron-beam. The silica nanoribbons exhibit strong blue emission at about 467 nm, together with UV and red emissions as investigated by cathodoluminescence technique. The origins of the luminescence are attributed to various defects in the silica nanoribbons; and the intensity change of the blue emission and green emission at about 550 nm is discussed in the frame of the defect density. Our study may lead to rational design of the new silica-based materials for a wide range of applications.

  10. Formation of Uniform Hollow Silica microcapsules

    Science.gov (United States)

    Yan, Huan; Kim, Chanjoong

    2013-03-01

    Microcapsules are small containers with diameters in the range of 0.1 - 100 μm. Mesoporous microcapsules with hollow morphologies possess unique properties such as low-density and high encapsulation capacity, while allowing controlled release by permeating substances with a specific size and chemistry. Our process is a one-step fabrication of monodisperse hollow silica capsules with a hierarchical pore structure and high size uniformity using double emulsion templates obtained by the glass-capillary microfluidic technique to encapsulate various active ingredients. These hollow silica microcapsules can be used as biomedical applications such as drug delivery and controlled release.

  11. Functionalized Mesoporous Silica Membranes for CO2 Separation Applications

    Directory of Open Access Journals (Sweden)

    Hyung-Ju Kim

    2015-01-01

    Full Text Available Mesoporous silica molecular sieves are emerging candidates for a number of potential applications involving adsorption and molecular transport due to their large surface areas, high pore volumes, and tunable pore sizes. Recently, several research groups have investigated the potential of functionalized mesoporous silica molecular sieves as advanced materials in separation devices, such as membranes. In particular, mesoporous silica with a two- or three-dimensional pore structure is one of the most promising types of molecular sieve materials for gas separation membranes. However, several important challenges must first be addressed regarding the successful fabrication of mesoporous silica membranes. First, a novel, high throughput process for the fabrication of continuous and defect-free mesoporous silica membranes is required. Second, functionalization of mesopores on membranes is desirable in order to impart selective properties. Finally, the separation characteristics and performance of functionalized mesoporous silica membranes must be further investigated. Herein, the synthesis, characterization, and applications of mesoporous silica membranes and functionalized mesoporous silica membranes are reviewed with a focus on CO2 separation.

  12. High drug load, stable, manufacturable and bioavailable fenofibrate formulations in mesoporous silica: a comparison of spray drying versus solvent impregnation methods.

    Science.gov (United States)

    Hong, Shiqi; Shen, Shoucang; Tan, David Cheng Thiam; Ng, Wai Kiong; Liu, Xueming; Chia, Leonard S O; Irwan, Anastasia W; Tan, Reginald; Nowak, Steven A; Marsh, Kennan; Gokhale, Rajeev

    2016-01-01

    Encapsulation of drugs in mesoporous silica using co-spray drying process has been recently explored as potential industrial method. However, the impact of spray drying on manufacturability, physiochemical stability and bioavailability in relation to conventional drug load processes are yet to be fully investigated. Using a 2(3) factorial design, this study aims to investigate the effect of drug-loading process (co-spray drying and solvent impregnation), mesoporous silica pore size (SBA-15, 6.5 nm and MCM-41, 2.5 nm) and percentage drug load (30% w/w and 50% w/w) on material properties, crystallinity, physicochemical stability, release profiles and bioavailability of fenofibrate (FEN) loaded into mesoporous silica. From the scanning electronic microscopy (SEM) images, powder X-ray diffraction and Differential scanning calorimetry measurements, it is indicated that the co-spray drying process was able to load up to 50% (w/w) FEN in amorphous form onto the mesoporous silica as compared to the 30% (w/w) for solvent impregnation. The in vitro dissolution rate of the co-spray dried formulations was also significantly (p = 0.044) better than solvent impregnated formulations at the same drug loading. Six-month accelerated stability test at 40 °C/75 RH in open dish indicated excellent physical and chemical stability of formulations prepared by both methods. The amorphous state of FEN and the enhanced dissolution profiles were well preserved, and very low levels of degradation were detected after storage. The dog data for the three selected co-spray-dried formulations revealed multiple fold increment in FEN bioavailability compared to the reference crystalline FEN. These results validate the viability of co-spray-dried mesoporous silica formulations with high amorphous drug load as potential drug delivery systems for poorly water soluble drugs.

  13. Fabrication of cotton fabric with superhydrophobicity and flame retardancy.

    Science.gov (United States)

    Zhang, Ming; Wang, Chengyu

    2013-07-25

    A simple and facile method for fabricating the cotton fabric with superhydrophobicity and flame retardancy is described in the present work. The cotton fabric with the maximal WCA of 160° has been prepared by the covalent deposition of amino-silica nanospheres and the further graft with (heptadecafluoro-1,1,2,2-tetradecyl) trimethoxysilane. The geometric microstructure of silica spheres was measured by transmission electron microscopy (TEM). The cotton textiles before and after treatment were characterized by using scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS). The wetting behavior of cotton samples was investigated by water contact angle measurement. Moreover, diverse performances of superhydrophobic cotton textiles have been evaluated as well. The results exhibited the outstanding superhydrophobicity, excellent waterproofing durability and flame retardancy of the cotton fabric after treatment, offering a good opportunity to accelerate the large-scale production of superhydrophobic textiles materials for new industrial applications. Copyright © 2013 Elsevier Ltd. All rights reserved.

  14. Palladium nanoparticles supported on fibrous-structured silica nanospheres (KCC-1): An efficient and selective catalyst for the transfer hydrogenation of alkenes

    KAUST Repository

    Qureshi, Ziyauddin; Sarawade, Pradip; Albert, Matthias; D'Elia, Valerio; Hedhili, Mohamed Nejib; Kö hler, Klaus; Basset, Jean-Marie

    2015-01-01

    An efficient palladium catalyst supported on fibrous silica nanospheres (KCC-1) has been developed for the hydrogenation of alkenes and α,β-unsaturated carbonyl compounds, providing excellent yields of the corresponding products with remarkable chemoselectivity. Comparison (high-resolution TEM, chemisorption) with analogous mesoporous (MCM-41, SBA-15) silica-supported Pd nanocatalysts prepared under identical conditions, demonstrates the advantage of employing the fibrous KCC-1 morphology versus traditional supports because it ensures superior accessibility of the catalytically active cores along with excellent Pd dispersion at high metal loading. This morphology ultimately leads to higher catalytic activity for the KCC-1-supported nanoparticles. The protocol developed for hydrogenation is advantageous and environmentally benign owing to the use of HCOOH as a source of hydrogen, water as a solvent, and because of efficient catalyst recyclability and durability. The recycled catalyst has been analyzed by XPS spectroscopy and TEM showing only minor changes in the oxidation state of Pd and in the morphology after the reaction, thus confirming the robustness of the catalyst.

  15. Palladium nanoparticles supported on fibrous-structured silica nanospheres (KCC-1): An efficient and selective catalyst for the transfer hydrogenation of alkenes

    KAUST Repository

    Qureshi, Ziyauddin

    2015-01-09

    An efficient palladium catalyst supported on fibrous silica nanospheres (KCC-1) has been developed for the hydrogenation of alkenes and α,β-unsaturated carbonyl compounds, providing excellent yields of the corresponding products with remarkable chemoselectivity. Comparison (high-resolution TEM, chemisorption) with analogous mesoporous (MCM-41, SBA-15) silica-supported Pd nanocatalysts prepared under identical conditions, demonstrates the advantage of employing the fibrous KCC-1 morphology versus traditional supports because it ensures superior accessibility of the catalytically active cores along with excellent Pd dispersion at high metal loading. This morphology ultimately leads to higher catalytic activity for the KCC-1-supported nanoparticles. The protocol developed for hydrogenation is advantageous and environmentally benign owing to the use of HCOOH as a source of hydrogen, water as a solvent, and because of efficient catalyst recyclability and durability. The recycled catalyst has been analyzed by XPS spectroscopy and TEM showing only minor changes in the oxidation state of Pd and in the morphology after the reaction, thus confirming the robustness of the catalyst.

  16. What Is Crystalline Silica?

    Science.gov (United States)

    ... and ceramic manufacturing and the tool and die, steel and foundry industries. Crystalline silica is used in manufacturing, household abrasives, adhesives, paints, soaps, and glass. Additionally, ...

  17. Crystalline Silica Primer

    Science.gov (United States)

    ,

    1992-01-01

    Crystalline silica is the scientific name for a group of minerals composed of silicon and oxygen. The term crystalline refers to the fact that the oxygen and silicon atoms are arranged in a threedimensional repeating pattern. This group of minerals has shaped human history since the beginning of civilization. From the sand used for making glass to the piezoelectric quartz crystals used in advanced communication systems, crystalline silica has been a part of our technological development. Crystalline silica's pervasiveness in our technology is matched only by its abundance in nature. It's found in samples from every geologic era and from every location around the globe. Scientists have known for decades that prolonged and excessive exposure to crystalline silica dust in mining environments can cause silicosis, a noncancerous lung disease. During the 1980's, studies were conducted that suggested that crystalline silica also was a carcinogen. As a result of these findings, crystalline silica has been regulated under the Occupational Safety and Health Administration's (OSHA) Hazard Communication Standard (HCS). Under HCS, OSHAregulated businesses that use materials containing 0.1% or more crystalline silica must follow Federal guidelines concerning hazard communication and worker training. Although the HCS does not require that samples be analyzed for crystalline silica, mineral suppliers or OSHAregulated

  18. A facile method to fabricate superhydrophobic cotton fabrics

    Science.gov (United States)

    Zhang, Ming; Wang, Shuliang; Wang, Chengyu; Li, Jian

    2012-11-01

    A facile and novel method for fabricating superhydrophobic cotton fabrics is described in the present work. The superhydrophobic surface has been prepared by utilizing cationic poly (dimethyldiallylammonium chloride) and silica particles together with subsequent modification of (heptadecafluoro-1,1,2,2-tetradecyl) trimethoxysilane. The size distribution of silica particles was measured by Particle Size Analyzer. The cotton textiles before and after treatment were characterized by using scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS). The wetting behavior of cotton samples was investigated by water contact angle measurement. Moreover, the superhydrophobic durability of coated cotton textiles has been evaluated by exposure, immersion and washing tests. The results show that the treated cotton fabrics exhibited excellent chemical stability and outstanding non-wettability with the WCA of 155 ± 2°, which offers an opportunity to accelerate the large-scale production of superhydrophobic textiles materials for new industrial applications.

  19. Functionalized mesoporous silica materials for molsidomine adsorption: Thermodynamic study

    Energy Technology Data Exchange (ETDEWEB)

    Alyoshina, Nonna A.; Parfenyuk, Elena V., E-mail: evp@iscras.ru

    2013-09-15

    A series of unmodified and organically modified mesoporous silica materials was prepared. The unmodified mesoporous silica was synthesized via sol–gel synthesis in the presence of D-glucose as pore-forming agent. The functionalized by phenyl, aminopropyl and mercaptopropyl groups silica materials were prepared via grafting. The fabricated adsorbent materials were characterized by Fourier transform infrared spectroscopy (FTIR) analysis, N{sub 2} adsorption/desorption and elemental analysis methods. Then their adsorption properties for mesoionic dug molsidomine were investigated at 290–313 K and physiological pH value. Thermodynamic parameters of molsidomine adsorption on the synthesized materials have been calculated. The obtained results showed that the adsorption process of molsidomine on the phenyl modified silica is the most quantitatively and energetically favorable. The unmodified and mercaptopropyl modified silica materials exhibit significantly higher adsorption capacities and energies for molsidomine than the aminopropyl modified sample. The effects are discussed from the viewpoint of nature of specific interactions responsible for the adsorption. - Graphical abstract: Comparative analysis of the thermodynamic characteristics of molsidomine adsorption showed that the adsorption process on mesoporous silica materials is controlled by chemical nature of surface functional groups. Molsidomine adsorption on the phenyl modified silica is the most quantitatively and energetically favorable. Taking into account ambiguous nature of mesoionic compounds, it was found that molsidomine is rather aromatic than dipolar. Display Omitted - Highlights: • Unmodified and organically modified mesoporous silica materials were prepared. • Molsidomine adsorption on the silica materials was studied. • Phenyl modified silica shows the highest adsorption capacity and favorable energy. • Molsidomine exhibits the lowest affinity to aminopropyl modified silica.

  20. Functionalized mesoporous silica materials for molsidomine adsorption: Thermodynamic study

    International Nuclear Information System (INIS)

    Alyoshina, Nonna A.; Parfenyuk, Elena V.

    2013-01-01

    A series of unmodified and organically modified mesoporous silica materials was prepared. The unmodified mesoporous silica was synthesized via sol–gel synthesis in the presence of D-glucose as pore-forming agent. The functionalized by phenyl, aminopropyl and mercaptopropyl groups silica materials were prepared via grafting. The fabricated adsorbent materials were characterized by Fourier transform infrared spectroscopy (FTIR) analysis, N 2 adsorption/desorption and elemental analysis methods. Then their adsorption properties for mesoionic dug molsidomine were investigated at 290–313 K and physiological pH value. Thermodynamic parameters of molsidomine adsorption on the synthesized materials have been calculated. The obtained results showed that the adsorption process of molsidomine on the phenyl modified silica is the most quantitatively and energetically favorable. The unmodified and mercaptopropyl modified silica materials exhibit significantly higher adsorption capacities and energies for molsidomine than the aminopropyl modified sample. The effects are discussed from the viewpoint of nature of specific interactions responsible for the adsorption. - Graphical abstract: Comparative analysis of the thermodynamic characteristics of molsidomine adsorption showed that the adsorption process on mesoporous silica materials is controlled by chemical nature of surface functional groups. Molsidomine adsorption on the phenyl modified silica is the most quantitatively and energetically favorable. Taking into account ambiguous nature of mesoionic compounds, it was found that molsidomine is rather aromatic than dipolar. Display Omitted - Highlights: • Unmodified and organically modified mesoporous silica materials were prepared. • Molsidomine adsorption on the silica materials was studied. • Phenyl modified silica shows the highest adsorption capacity and favorable energy. • Molsidomine exhibits the lowest affinity to aminopropyl modified silica

  1. Novel silica membranes for high temperature gas separations

    KAUST Repository

    Bighane, Neha

    2011-04-01

    This article describes fabrication of novel silica membranes derived via controlled oxidative thermolysis of polydimethylsiloxane and their gas separation performance. The optimized protocol for fabrication of the silica membranes is described and pure gas separation performance in the temperature range 35-80°C is presented. It is observed that the membranes exhibit activated transport for small gas penetrants such as He, H 2 and CO 2. The membranes can withstand temperatures up to 350°C in air and may ultimately find use in H 2/CO 2 separations to improve efficiency in the water-gas shift reactor process. © 2011 Elsevier B.V.

  2. Surface structural, morphological, and catalytic studies of homogeneously dispersed anisotropic Ag nanostructures within mesoporous silica

    Energy Technology Data Exchange (ETDEWEB)

    Sareen, Shweta [Thapar University, School of Chemistry and Biochemistry (India); Mutreja, Vishal [Maharishi Markandeshwar University, Department of Chemistry (India); Pal, Bonamali; Singh, Satnam, E-mail: ssingh@thapar.edu [Thapar University, School of Chemistry and Biochemistry (India)

    2016-11-15

    Highly dispersed anisotropic Ag nanostructures were synthesized within the channels of 3-aminopropyltrimethoxysilane (APTMS)-modified mesoporous SBA-15 for catalyzing the reduction of p-dinitrobenzene, p-nitrophenol, and p-nitroacetophenone, respectively. A green templating process without involving any reducing agent, by varying the amount (1–10 wt.%) of Ag loading followed by calcination at 350 °C under H{sub 2} led to change in the morphology of Ag nanoparticles from nanospheres (~7–8 nm) to nanorods (aspect ratio ~12–30 nm) without any deformation in mesoporous sieves. In comparison to white bare SBA-15, gray-colored samples were formed with Ag impregnation exhibiting absorption bands at 484 and 840 nm indicating the formation of anisotropic Ag nanostructures within mesoporous matrix. TEM and FE-SEM micrographs confirmed the presence of evenly dispersed Ag nanostructures within as well as on the surface of mesoporous matrix. AFM studies indicated a small decrease in the average roughness of SBA-15 from 20.59 to 19.21 nm for 4 wt.% Ag/m-SBA-15, illustrating the encapsulation of majority of Ag nanoparticles in the siliceous matrix and presence of small amount of Ag nanoparticles on the mesoporous support. Moreover, due to plugging of mesopores with Ag, a significant decrease in surface area from 680 m{sup 2}/g of SBA-15 to 385 m{sup 2}/g was observed. The Ag-impregnated SBA-15 catalyst displayed superior catalytic activity than did bare SBA-15 with 4 wt.% Ag-loaded catalyst exhibiting optimum activity for selective reduction of p-nitrophenol to p-aminophenol (100 %), p-nitroacetophenone to p-aminoacetophenone (100 %), and p-dinitrobenzene to p-nitroaniline (87 %), with a small amount of p-phenylenediamine formation.

  3. Surge-Resistant Nanocomposite Enameled Wire Using Silica Nanoparticles with Binary Chemical Compositions on the Surface

    Directory of Open Access Journals (Sweden)

    Jeseung Yoo

    2015-01-01

    Full Text Available We developed polyesterimide (PEI nanocomposite enameled wires using surface-modified silica nanoparticles with binary chemical compositions on the surface. The modification was done using silanes assisted by ultrasound, which facilitated high density modification. Two different trimethoxysilanes were chosen for the modification on the basis of resemblance of chemical compositions on the silica surface to PEI varnish. The surface-modified silica was well dispersed in PEI varnish, which was confirmed by optical observation and viscosity measurement. The glass transition temperature of the silica-PEI nanocomposite increased with the silica content. The silica-dispersed PEI varnish was then used for enameled wire fabrication. The silica-PEI nanocomposite enameled wire exhibited a much longer lifetime compared to that of neat PEI enameled wire in partial discharge conditions.

  4. Oxygen configurations in silica

    International Nuclear Information System (INIS)

    Chelikowsky, James R.; Chadi, D. J.; Binggeli, N.

    2000-01-01

    We propose a transition state for oxygen in silica. This state is produced by the insertion of an oxygen molecule into the Si-O-Si bond, i.e., it consists of producing a Si-O-O-O-Si bond. This state allows molecular oxygen diffusion in silica without breaking the molecular O 2 bond and it is energetically more stable than a peroxy configuration. This configuration may allow for exchange of molecular oxygen with the oxygen in the silica framework. (c) 2000 The American Physical Society

  5. Silica coatings on clarithromycin.

    Science.gov (United States)

    Bele, Marjan; Dmitrasinovic, Dorde; Planinsek, Odon; Salobir, Mateja; Srcic, Stane; Gaberscek, Miran; Jamnik, Janko

    2005-03-03

    Pre-crystallized clarithromycin (6-O-methylerythromycin A) particles were coated with silica from the tetraethyl orthosilicate (TEOS)-ethanol-aqueous ammonia system. The coatings had a typical thickness of 100-150 nm and presented about 15 wt.% of the silica-drug composite material. The properties of the coatings depended on reactant concentration, temperature and mixing rate and, in particular, on the presence of a cationic surfactant (cetylpyridinium chloride). In the presence of cetylpyridinium chloride the silica coatings slightly decreased the rate of pure clarithromycin dissolution.

  6. A new nanocomposite polymer electrolyte based on poly(vinyl alcohol) incorporating hypergrafted nano-silica

    KAUST Repository

    Hu, Xian-Lei; Hou, Gao-Ming; Zhang, Ming-Qiu; Rong, Min-Zhi; Ruan, Wen-Hong; Giannelis, Emmanuel P.

    2012-01-01

    perchlorate via mold casting method to fabricate nanocomposite polymer electrolytes. By introducing hypergrafted nanoparticles, ionic conductivity of solid composite is improved significantly at the testing temperature. Hypergrafted nano-silica may act

  7. Fabrication and application of a new modified electrochemical sensor using nano-silica and a newly synthesized Schiff base for simultaneous determination of Cd2+, Cu2+ and Hg2+ ions in water and some foodstuff samples

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Soltani-Felehgari, Farzaneh; Madrakian, Tayyebeh; Ghaedi, Hamed; Rezaeivala, Majid

    2013-01-01

    Highlights: ► A new modified electrochemical sensor was constructed and used. ► A new Schiff base coated nano-silica was used as modifier. ► The electrochemical properties of electrode were studied. ► This modifier enhanced the electrochemical properties of electrode. ► The electrode was used for simultaneous determination of Cd 2+ , Cu 2+ and Hg 2+ ions. -- Abstract: A new chemically modified carbon paste electrode was constructed and used for rapid, simple, accurate, selective and highly sensitive simultaneous determination of cadmium, copper and mercury using square wave anodic stripping voltammetry (SWASV). The carbon paste electrode was modified by N,N′-bis(3-(2-thenylidenimino)propyl)piperazine coated silica nanoparticles. Compared with carbon paste electrode, the stripping peak currents had a significant increase at the modified electrode. Under the optimized conditions (deposition potential, −1.100 V vs. Ag/AgCl; deposition time, 60 s; resting time, 10 s; SW frequency, 25 Hz; pulse amplitude, 0.15 V; dc voltage step height, 4.4 mV), the detection limit was 0.3, 0.1 and 0.05 ng mL −1 for the determination of Cd 2+ , Cu 2+ and Hg 2+ , respectively. The complexation reaction of the ligand with several metal cations in methanol was studied and the stability constants of the complexes were obtained. The effects of different cations and anions on the simultaneous determination of metal ions were studied and it was found that the electrode is highly selective for the simultaneous determination of Cd 2+ , Cu 2+ and Hg 2+ . Furthermore, the present method was applied to the determination of Cd 2+ , Cu 2+ and Hg 2+ in water and some foodstuff samples

  8. Silica aerogel Cerenkov counter

    International Nuclear Information System (INIS)

    Yasumi, S.; Masaike, A.; Yamamoto, A.; Yoshimura, Y.; Kawai, H.

    1984-03-01

    In order to obtain silica aerogel radiators of good quality, the prescription used by Saclay group has been developed. We have done several experiments using beams from KEK.PS to test the performance of a Cerenkov counter with aerogel modules produced in KEK. It turned out that these modules had excellent quality. The production rate of silica aerogel in KEK is 15 -- 20 litres a week. Silica aerogel modules of 20 x 10 x 3 cm 3 having the refractive index of 1.058 are successfully being used by Kyoto University group in the KEK experiment E92 (Σ). Methodes to produce silica aerogel with higher refractive index than 1.06 has been investigated both by heating an module with the refractive index of 1.06 and by hydrolyzing tetraethyl silicate. (author)

  9. The impact of framework organic functional groups on the hydrophobicity and overall stability of mesoporous silica materials

    International Nuclear Information System (INIS)

    Smeulders, Geert; Meynen, Vera; Silvestre-Albero, Ana; Houthoofd, Kristof; Mertens, Myrjam; Silvestre-Albero, Joaquin; Martens, Johan A.; Cool, Pegie

    2012-01-01

    Graphical abstract: The stability (hydrothermal, mechanical and chemical) of PMOs is studied in a systematic way and ranks them between classic and other hybrid mesoporous silica materials. Highlights: ► The stability (hydrothermal, mechanical and chemical) of PMOs is studied. ► Compared stability of PMOs with classic and other hybrid mesoporous silica materials. ► Immersion calorimetry to study the effect of hydrophobicity. ► PMOs show superior stability. - Abstract: The hydrothermal, mechanical and chemical stability of various mesoporous materials have been studied in detail, using X-ray diffraction and nitrogen sorption. Pure siliceous nanoporous powders (MCM-41 and SBA-15) are evaluated against their hybrid counterparts; namely 2 types of periodic mesoporous organosilicas (benzene and ethane bridged PMOs) and an organosilane grafted MCM-41 material. In primary tests, the stability of the hybrid materials is found to be superior compared to that of the pure siliceous ones. The stability of the materials was correlated to their hydrophobicity via immersion calorimetry, applied for the first time in this context. Based on these results, a clear correlation between the hydrophobicity of a material and its stability has been revealed. In addition, with 29 Si-MAS-NMR and vacuum experiments, the mechanism of the structural deterioration in the three different stability treatments could be unambiguously identified as the hydrolyzation of the siloxane bonds. The homogeneity of the hydrophobic groups throughout the entire network was found to be of great importance, irrespective of the hydrophobic nature at the surface as determined by calorimetric measurements. The results reveal that the most stable material can withstand (a) a pressure of 740 MPa during 5 min, (b) a 2 h stirring in a 2 M NaOH solution and (c) a 3 day steaming treatment at 393 K.

  10. The impact of framework organic functional groups on the hydrophobicity and overall stability of mesoporous silica materials

    Energy Technology Data Exchange (ETDEWEB)

    Smeulders, Geert, E-mail: geert.smeulders@ua.ac.be [University of Antwerpen (Ukraine), Laboratory of Adsorption and Catalysis, Universiteitsplein 1, 2610 Wilrijk (Belgium); Meynen, Vera [University of Antwerpen (Ukraine), Laboratory of Adsorption and Catalysis, Universiteitsplein 1, 2610 Wilrijk (Belgium); Silvestre-Albero, Ana [Universidad de Alicante, Laboratorio de Materiales Avanzados, Apartado 99, 03080 Alicante (Spain); Houthoofd, Kristof [KULeuven, Centre for Surface Chemistry and Catalysis, Kasteelpark Arenberg 23, 3001 Heverlee (Belgium); Mertens, Myrjam [Flemish Institute for Technological Research (VITO N.V.), Boeretang 200, 2400 Mol (Belgium); Silvestre-Albero, Joaquin [Universidad de Alicante, Laboratorio de Materiales Avanzados, Apartado 99, 03080 Alicante (Spain); Martens, Johan A. [KULeuven, Centre for Surface Chemistry and Catalysis, Kasteelpark Arenberg 23, 3001 Heverlee (Belgium); Cool, Pegie [University of Antwerpen (Ukraine), Laboratory of Adsorption and Catalysis, Universiteitsplein 1, 2610 Wilrijk (Belgium)

    2012-02-15

    Graphical abstract: The stability (hydrothermal, mechanical and chemical) of PMOs is studied in a systematic way and ranks them between classic and other hybrid mesoporous silica materials. Highlights: Black-Right-Pointing-Pointer The stability (hydrothermal, mechanical and chemical) of PMOs is studied. Black-Right-Pointing-Pointer Compared stability of PMOs with classic and other hybrid mesoporous silica materials. Black-Right-Pointing-Pointer Immersion calorimetry to study the effect of hydrophobicity. Black-Right-Pointing-Pointer PMOs show superior stability. - Abstract: The hydrothermal, mechanical and chemical stability of various mesoporous materials have been studied in detail, using X-ray diffraction and nitrogen sorption. Pure siliceous nanoporous powders (MCM-41 and SBA-15) are evaluated against their hybrid counterparts; namely 2 types of periodic mesoporous organosilicas (benzene and ethane bridged PMOs) and an organosilane grafted MCM-41 material. In primary tests, the stability of the hybrid materials is found to be superior compared to that of the pure siliceous ones. The stability of the materials was correlated to their hydrophobicity via immersion calorimetry, applied for the first time in this context. Based on these results, a clear correlation between the hydrophobicity of a material and its stability has been revealed. In addition, with {sup 29}Si-MAS-NMR and vacuum experiments, the mechanism of the structural deterioration in the three different stability treatments could be unambiguously identified as the hydrolyzation of the siloxane bonds. The homogeneity of the hydrophobic groups throughout the entire network was found to be of great importance, irrespective of the hydrophobic nature at the surface as determined by calorimetric measurements. The results reveal that the most stable material can withstand (a) a pressure of 740 MPa during 5 min, (b) a 2 h stirring in a 2 M NaOH solution and (c) a 3 day steaming treatment at 393 K.

  11. Mesoporous templated silicas: stability, pore size engineering and catalytic activation

    International Nuclear Information System (INIS)

    Vansant, Etienne

    2003-01-01

    The Laboratory of Adsorption and Catalysis has focused its research activities on the synthesis and activation of new porous materials. In the past few years, we have succeeded in developing easy and reproducible pathways to synthesize a huge variety of mesoporous crystalline materials. Points of interest in the synthesis of Mesoporous Templated Silicas are (i) stabilization of the structure, to withstand hydrothermal, thermal and mechanical pressure, (ii) pore size engineering to systematically control the pore size, pore volume and the ratio micro/mesopores and (iii) ease and reproducibility of the synthesis procedure, applying green principles, such as template recuperation. By carefully adapting the synthesis conditions and composition of the synthesis gel, using surfactants (long chain quaternary ammonium ions) and co-templates (long chain amines, alcohols or alkanes), the pore size of the obtained materials can be controlled from 1.5 to 7.0 nm, retaining the very narrow pore size distribution. Alternatively, materials with combined micro- and mesoporosity can be synthesized, using neutral surfactants (triblock copolymers). Hereby, the optimization of the SBA-15 and SBA-16 synthesis is being done in order to create mesoporous materials with microporous walls. The second research line is the controlled activation of MTS materials, by grafting or incorporation of catalytic active centers. We have developed for this purpose the Molecular Designed Dispersion method, which uses metal diketonate complexes as precursors. It is shown that in all cases the dispersion of the metal oxides on the surface is much better compared to the conventional grafting techniques. We have studied and published activation with V, Ti, Mo, Fe, Al and Cr species on different MTS materials. The structure and location of the active metal ion is the subject of an extensive spectroscopic investigation, using FT-IR, FT-Raman, UV-Vis DR coupled with selective chemisorption experiments and

  12. Behaviour of Epoxy Silica Nanocomposites Under Static and Creep Loading

    Science.gov (United States)

    Constantinescu, Dan Mihai; Picu, Radu Catalin; Sandu, Marin; Apostol, Dragos Alexandru; Sandu, Adriana; Baciu, Florin

    2017-12-01

    Specific manufacturing technologies were applied for the fabrication of epoxy-based nanocomposites with silica nanoparticles. For dispersing the fillers in the epoxy resin special equipment such as a shear mixer and a high energy sonicator with temperature control were used. Both functionalized and unfunctionalized silica nanoparticles were added in three epoxy resins. The considered filling fraction was in most cases 0.1, 0.3 and 0.5 wt%.. The obtained nanocomposites were subjected to monotonic uniaxial and creep loading at room temperature. The static mechanical properties were not significantly improved regardless the filler percentage and type of epoxy resin. Under creep loading, by increasing the stress level, the nanocomposite with 0.1 wt% silica creeps less than all other materials. Also the creep rate is reduced by adding silica nanofillers.

  13. Silica biomineralization via the self-assembly of helical biomolecules.

    Science.gov (United States)

    Liu, Ben; Cao, Yuanyuan; Huang, Zhehao; Duan, Yingying; Che, Shunai

    2015-01-21

    The biomimetic synthesis of relevant silica materials using biological macromolecules as templates via silica biomineralization processes attract rapidly rising attention toward natural and artificial materials. Biomimetic synthesis studies are useful for improving the understanding of the formation mechanism of the hierarchical structures found in living organisms (such as diatoms and sponges) and for promoting significant developments in the biotechnology, nanotechnology and materials chemistry fields. Chirality is a ubiquitous phenomenon in nature and is an inherent feature of biomolecular components in organisms. Helical biomolecules, one of the most important types of chiral macromolecules, can self-assemble into multiple liquid-crystal structures and be used as biotemplates for silica biomineralization, which renders them particularly useful for fabricating complex silica materials under ambient conditions. Over the past two decades, many new silica materials with hierarchical structures and complex morphologies have been created using helical biomolecules. In this review, the developments in this field are described and the recent progress in silica biomineralization templating using several classes of helical biomolecules, including DNA, polypeptides, cellulose and rod-like viruses is summarized. Particular focus is placed on the formation mechanism of biomolecule-silica materials (BSMs) with hierarchical structures. Finally, current research challenges and future developments are discussed in the conclusion. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

    López, A. J.; Rico, A.; Rodríguez, J.; Rams, J.

    2010-08-01

    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.

  15. Silica-Immobilized Enzyme Reactors

    Science.gov (United States)

    2007-08-01

    Silica-IMERs 14 implicated in neurological disorders such as Schizophrenia and Parkinson’s disease.[86] Drug discovery for targets that can alter the...primarily the activation of prodrugs and proantibiotics for cancer treatments or antibiotic therapy , respectively.[87] Nitrobenzene nitroreductase was...BuChE) Monolith disks* Packed Silica Biosilica Epoxide- Silica Silica-gel Enzyme Human AChE Human AChE Human AChE Equine BuChE Human

  16. Silica reinforced triblock copolymer gels

    DEFF Research Database (Denmark)

    Theunissen, E.; Overbergh, N.; Reynaers, H.

    2004-01-01

    The effect of silica and polymer coated silica particles as reinforcing agents on the structural and mechanical properties of polystyrene-poly(ethylene/butylene)-polystyrene (PS-PEB-PS) triblock gel has been investigated. Different types of chemically modified silica have been compared in order...

  17. Preparation of fluorescent mesoporous hollow silica-fullerene nanoparticles via selective etching for combined chemotherapy and photodynamic therapy

    Science.gov (United States)

    Yang, Yannan; Yu, Meihua; Song, Hao; Wang, Yue; Yu, Chengzhong

    2015-07-01

    Well-dispersed mesoporous hollow silica-fullerene nanoparticles with particle sizes of ~50 nm have been successfully prepared by incorporating fullerene molecules into the silica framework followed by a selective etching method. The fabricated fluorescent silica-fullerene composite with high porosity demonstrates excellent performance in combined chemo/photodynamic therapy.Well-dispersed mesoporous hollow silica-fullerene nanoparticles with particle sizes of ~50 nm have been successfully prepared by incorporating fullerene molecules into the silica framework followed by a selective etching method. The fabricated fluorescent silica-fullerene composite with high porosity demonstrates excellent performance in combined chemo/photodynamic therapy. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr02769a

  18. Silica from Ash

    Indian Academy of Sciences (India)

    management, polymer composites and chemical process design. Figure 1 Difference in color of the ash ... The selection of ash is important as the quality of ash determines the total amount as well as quality of silica recoverable Ash which has undergone maximum extent of combustion is highly desirable as it contains ...

  19. Hydrothermal stability of silica, hybrid silica and Zr-doped hybrid silica membranes

    NARCIS (Netherlands)

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

    2017-01-01

    Hybrid silica membranes have demonstrated to possess a remarkable hydrothermal stability in pervaporation and gas separation processes allowing them to be used in industrial applications. In several publications the hydrothermal stability of pure silica or that of hybrid silica membranes are

  20. Mesoporous silica nanotubes hybrid membranes for functional nanofiltration

    International Nuclear Information System (INIS)

    El-Safty, Sherif A; Shahat, Ahmed; Mekawy, Moataz; Nguyen, Hoa; Warkocki, Wojciech; Ohnuma, Masato

    2010-01-01

    The development of nanofiltration systems would greatly assist in the production of well-defined particles and biomolecules with unique properties. We report a direct, simple synthesis of hexagonal silica nanotubes (NTs), which vertically aligned inside anodic alumina membranes (AAM) by means of a direct templating method of microemulsion phases with cationic surfactants. The direct approach was used as soft templates for predicting ordered assemblies of surfactant/silica composites through strong interactions within AAM pockets. Thus, densely packed NTs were successfully formed in the entirety of the AAM channels. These silica NTs were coated with layers of organic moieties to create a powerful technique for the ultrafine filtration. The resulting modified-silica NTs were chemically robust and showed affinity toward the transport of small molecular particles. The rigid silica NTs inside AAM channels had a pore diameter of ≤ 4 nm and were used as ultrafine filtration systems for noble metal nanoparticles (NM NPs) and semiconductor nanocrystals (SC NCs) fabricated with a wide range of sizes (1.0-50 nm) and spherical/pyramidal morphologies. Moreover, the silica NTs hybrid membranes were also found to be suitable for separation of biomolecules such as cytochrome c (CytC). Importantly, this nanofilter design retains high nanofiltration efficiency of NM NPs, SC NCs and biomolecules after a number of reuse cycles. Such retention is crucial in industrial applications.

  1. Strategy and method for nanoporous cladding formation on silica optical fiber

    Czech Academy of Sciences Publication Activity Database

    Chen, H.; Tian, F.; Liu, K.; Kaňka, Jiří; Du, H.

    2016-01-01

    Roč. 41, č. 12 (2016), s. 2831-2834 ISSN 0146-9592 R&D Projects: GA ČR(CZ) GBP205/12/G118 Institutional support: RVO:67985882 Keywords : Fabrication strategies * Optical fiber fabrication * Silica Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 3.416, year: 2016

  2. Fabrication Facilities

    Data.gov (United States)

    Federal Laboratory Consortium — The Fabrication Facilities are a direct result of years of testing support. Through years of experience, the three fabrication facilities (Fort Hood, Fort Lewis, and...

  3. Silica suspended waveguide splitter-based biosensor

    Science.gov (United States)

    Harrison, M. C.; Hawk, R. M.; Armani, A. M.

    2012-03-01

    Recently, a novel integrated optical waveguide 50/50 splitter was developed. It is fabricated using standard lithographic methods, a pair of etching steps and a laser reflow step. However, unlike other integrated waveguide splitters, the waveguide is elevated off of the silicon substrate, improving its interaction with biomolecules in solution and in a flow field. Additionally, because it is fabricated from silica, it has very low optical loss, resulting in a high signal-to-noise ratio, making it ideal for biosensing. By functionalizing the device using an epoxy-silane method using small samples and confining the protein solutions to the device, we enable highly efficient detection of CREB with only 1 μL of solution. Therefore, the waveguide coupler sensor is representative of the next generation of ultra-sensitive optical biosensors, and, when combined with microfluidic capabilities, it will be an ideal candidate for a more fully-realized lab-on-a-chip device.

  4. The effect of heat treatment on the magnitude and composition of residual gas in sealed silica glass ampoules

    Science.gov (United States)

    Palosz, W.; Szofran, F. R.; Lehoczky, S. L.

    1994-01-01

    The residual gas pressure and composition in sealed silica glass ampoules as a function of different treatment procedures has been investigated. The dependence of the residual gas on the outgassing and annealing parameters has been determined. The effects of the fused silica brand, of the ampoule fabrication, and of post-outgassing procedures have been evaluated.

  5. Control of silicification by genetically engineered fusion proteins: Silk–silica binding peptides

    Science.gov (United States)

    Zhou, Shun; Huang, Wenwen; Belton, David J.; Simmons, Leo O.; Perry, Carole C.; Wang, Xiaoqin; Kaplan, David L.

    2014-01-01

    In the present study, an artificial spider silk gene, 6mer, derived from the consensus sequence of Nephila clavipes dragline silk gene, was fused with different silica-binding peptides (SiBPs), A1, A3 and R5, to study the impact of the fusion protein sequence chemistry on silica formation and the ability to generate a silk–silica composite in two different bioinspired silicification systems: solution–solution and solution– solid. Condensed silica nanoscale particles (600–800 nm) were formed in the presence of the recombinant silk and chimeras, which were smaller than those formed by 15mer-SiBP chimeras [1], revealing that the molecular weight of the silk domain correlated to the sizes of the condensed silica particles in the solution system. In addition, the chimeras (6mer-A1/A3/R5) produced smaller condensed silica particles than the control (6mer), revealing that the silica particle size formed in the solution system is controlled by the size of protein assemblies in solution. In the solution–solid interface system, silicification reactions were performed on the surface of films fabricated from the recombinant silk proteins and chimeras and then treated to induce β-sheet formation. A higher density of condensed silica formed on the films containing the lowest β-sheet content while the films with the highest β-sheet content precipitated the lowest density of silica, revealing an inverse correlation between the β-sheet secondary structure and the silica content formed on the films. Intriguingly, the 6mer-A3 showed the highest rate of silica condensation but the lowest density of silica deposition on the films, compared with 6mer-A1 and -R5, revealing antagonistic crosstalk between the silk and the SiBP domains in terms of protein assembly. These findings offer a path forward in the tailoring of biopolymer–silica composites for biomaterial related needs. PMID:25462851

  6. 无外加酸体系中AlSBA¯15为模板,有序介孔炭材料CMK¯3的合成与表征%Synthesis and characterization of ordered mesoporous carbons CMK_3 produced by tailoring the mesopores of an AlSBA_15 hard template synthesized without acid

    Institute of Scientific and Technical Information of China (English)

    石磊; 徐艳; 邢立淑; 李湘萍; 杨成; 林森

    2014-01-01

    在无外加酸体系中改变晶化温度合成AlSBA¯15介孔材料,并以此为刚性模板,蔗糖为碳源,合成出一系列具有不同孔结构的有序介孔炭材料CMK¯3,系统考察晶化温度对AlSBA¯15和其反相复制结构CMK¯3孔道结构的影响。结果显示在无外加酸合成体系中改变晶化温度可对AlSBA¯15的孔道结构进行有效调控,通过结构复制技术可制备出具有不同结构的CMK¯3。控制刚性模板AlSBA¯15的晶化温度为90益,所得介孔炭材料CMK¯3(CMK¯3(90))结构最佳,除介孔排列高度有序外,还具有高比表面积(1688 m2·g-1)和大孔容(0.95 cm3·g-1)。另外,对CMK¯3的微孔性质与刚性模板孔壁中的次级介孔结构的内在联系进行研究,发现调变刚性模板的晶化温度可以有效改善有序介孔炭材料CMK¯3的结构性质。%Highly ordered mesoporous carbons ( OMCs) designated CMK¯3 were synthesized using mesoporous Al¯SBA¯15 with different textural properties as hard templates and sucrose as a carbon source. Al¯SBA¯15 is an ordered mesoporous alumina¯silica synthesized with a soft template, P123. The effect of the aging temperature for the hard templates on the pore structure of CMK¯3 was investigated. X¯ray diffraction, N2 adsorption and transmission electron microscopy were used to characterize the pore structures of the hard templates and the resultant CMK¯3. Result indicates that CMK¯3 with different pore structures can be obtained by tailor¯ ing the pore structures of the hard templates bysimply controlling the aging temperature in an acid¯free medium. The best CMK¯3 possessed a highly¯ordered pore structure, and a very high BET surface area (1 688 m2 ·g-1 ) and pore volume (0. 95 cm3 ·g-1 ) when the hard template was aged at 90 ℃. The microporous character of the CMK¯3 was related to the thickness of the mesopore wall of the hard templates. The textural characteristics of the resultant CMK¯3 can be improved by simply

  7. Optical diffraction by ordered 2D arrays of silica microspheres

    International Nuclear Information System (INIS)

    Shcherbakov, A.A.; Shavdina, O.; Tishchenko, A.V.; Veillas, C.; Verrier, I.; Dellea, O.; Jourlin, Y.

    2017-01-01

    The article presents experimental and theoretical studies of angular dependent diffraction properties of 2D monolayer arrays of silica microspheres. High-quality large area defect-free monolayers of 1 μm diameter silica microspheres were deposited by the Langmuir-Blodgett technique under an accurate optical control. Measured angular dependencies of zeroth and one of the first order diffraction efficiencies produced by deposited samples were simulated by the rigorous Generalized Source Method taking into account particle size dispersion and lattice nonideality. - Highlights: • High quality silica microsphere monolayer was fabricated. • Accurate measurements of diffraction efficiency angular dependencies. • Rigorous diffraction simulation of both ideal hexagonal and realistic microsphere arrangements. • Qualitative rationalization of the obtained results and the observed differences between the experiment and the theory.

  8. Silica particles and method of preparation thereof

    NARCIS (Netherlands)

    2015-01-01

    The invention is in the field of silica products. More in particular, the invention is in the field of amorphous silica particles. The invention is directed to amorphous silica particles and related products including clusters of said silica particles, a suspension of said silica particles, and an

  9. Serpentinization processes: Influence of silica

    Science.gov (United States)

    Huang, R.; Sun, W.; Ding, X.; Song, M.; Zhan, W.

    2016-12-01

    Serpentinization systems are highly enriched in molecular hydrogen (H2) and hydrocarbons (e.g. methane, ethane and propane). The production of hydrocarbons results from reactions between H2 and oxidized carbon (carbon dioxide and carbon monoxide), which possibly contribute to climate changes during early history of the Earth. However, the influence of silica on the production of H2 and hydrocarbons was poorly constrained. We performed experiments at 311-500 °C and 3.0 kbar using mechanical mixtures of silica and olivine in ratios ranging from 0 to 40%. Molecular hydrogen (H2), methane, ethane and propane were formed, which were analyzed by gas chromatography. It was found that silica largely decreased H2 production. Without any silica, olivine serpentinization produced 94.5 mmol/kg H2 after 20 days of reaction time. By contrast, with the presence of 20% silica, H2 concentrations decreased largely, 8.5 mmol/kg. However, the influence of silica on the production of hydrocarbons is negligible. Moreover, with the addition of 20%-40% silica, the major hydrous minerals are talc, which was quantified according to an established standard curve calibrated by infrared spectroscopy analyses. It shows that silica greatly enhances olivine hydration, especially at 500 °C. Without any addition of silica, reaction extents were serpentinization at 500 °C and 3.0 kbar. By contrast, with the presence of 50% silica, olivine was completely transformed to talc within 9 days. This study indicates that silica impedes the oxidation of ferrous iron into ferric iron, and that rates of olivine hydration in natural geological settings are much faster with silica supply.

  10. Surface modification of silica nanoparticles by UV-induced graft polymerization of methyl methacrylate.

    Science.gov (United States)

    Kim, Sooyeon; Kim, Eunhye; Kim, Sungsoo; Kim, Woosik

    2005-12-01

    In this study we modified the surface of silica nanoparticles with methyl methacrylate by UV-induced graft polymerization. It is a surface-initiated polymerization reaction induced by ultraviolet irradiation. The resulting organic-inorganic nanocomposites were near-monodisperse and fabricated without homopolymerization of the monomer. Substantial increase in mean particle size was observed by SEM image analysis after UV-induced grafting of methyl methacrylate onto pure silica particles. FT-Raman spectroscopy and X-ray photoelectron spectroscopy studies of these materials revealed the successful grafting of methyl methacrylate onto the silica surface. The formation of a covalent bond between the grafted PMMA chains and silica surface was indicated by FT-Raman spectra. Thermogravimetric analysis of the PMMA-grafted silica particles indicated the polymer contents in good agreement with SEM photographs.

  11. Study of Physical Properties of Nano-Silica Coated Cotton Textiles

    OpenAIRE

    Sidra Saleemi; Farooq Ahmed; Samandar Malik

    2015-01-01

    This research was aimed to investigate the effect of silica sol-gel coating on air permeability, stiffness and tensile properties of dyed cotton fabric. Various concentrations of silica nanoparticles were applied on dyed cotton substrate using two different cross-linkers through sol-gel method. The homogenous sol-gel coating dispersions were prepared by using an ultrasonicator. Coated samples were tested for mechanical and comfort properties such as tensile strength, stiffness, crease recover...

  12. High density thoria-silica-metal (III) oxide fibers

    International Nuclear Information System (INIS)

    1974-01-01

    Transparent refractory fibers, at least 50% thoria and additionally containing silica and metal(III) oxides, particularly Al 2 O 3 and B 2 O 3 or Cr 2 O 3 are made by shaping and dehydratively gelling, particularly by extruding in air, viscous aqueous thoria solutions or sols containing colloidal silica with boric acid-stabilized aluminum acetate, or additionally chromium acetate or colloidal Cr 2 O 3 , and heating the resulting gelled fibers in a controlled manner to decompose and volatilize undesired constituents and convert fibers to refractory fibers which are useful to form, for example, refractory fabrics, or as reinforcement for composites. The fabrics are heat resistant. A special application is X-ray protective clothing

  13. Synthesis, characterisation and functionalisation of luminescent silica nanoparticles

    International Nuclear Information System (INIS)

    Labéguerie-Egéa, Jessica; McEvoy, Helen M.; McDonagh, Colette

    2011-01-01

    The synthesis of highly monodispersed, homogeneous and stable luminescent silica nanoparticles, synthesized using a process based on the Stöber method is reported here. These particles have been functionalised with the ruthenium and europium complexes: bis (2,2′-bipyridine)-(5-aminophenanthroline) Ru bis (hexafluorophosphate), abbreviated to (Ru(bpy) 2 (phen-5-NH 2 )(PF 6 )), and tris (dibenzoylmethane)-mono (5-aminophenanthroline) europium(III), abbreviated to (Eu:TDMAP). Both dyes have a free amino group available, facilitating the covalent conjugation of the dyes inside the silica matrix. Due to the covalent bond between the dyes and the silica, no dye leaching or nanoparticle diameter modification was observed. The generic and versatile nature of the synthesis process was demonstrated via the synthesis of both europium and ruthenium-functionalised nanoparticles. Following this, the main emphasis of the study was the characterisation of the luminescence of the ruthenium-functionalised silica nanoparticles, in particular, as a function of surface carboxyl or amino group functionalisation. It was demonstrated that the luminescence of the ruthenium dye is highly affected by the ionic environment at the surface of the nanoparticle, and that these effects can be counteracted by encapsulating the ruthenium-functionalised nanoparticles in a plain 15 nm silica layer. Moreover, the ruthenium-functionalised silica nanoparticles showed high relative brightness compared to the free dye in solution and efficient functionalisation with amino or carboxyl groups. Due to their ease of fabrication and attractive characteristics, the ruthenium-functionalised silica nanoparticles described here have the potential to be highly desirable fluorescent labels, particularly, for biological applications.

  14. Liquid phase deposition of silica: Thin films, colloids and fullerenes

    Science.gov (United States)

    Whitsitt, Elizabeth A.

    Little research has been done to explore liquid phase deposition (LPD) of silica on non-planar substrates. This thesis proves that the seeded growth of silica colloids from fullerene and surfactant micelles is possible via LPD, as is the coating of individual single walled carbon nanotubes (SWNTs) and carbon fibers. Working on the premise that a molecular growth mechanism (versus colloidal/gel deposition) is valid for LPD, nanostructured substrates and specific chemical functional groups should act as "seeds," or templates, for silica growth. Seeded growth is confirmed by reactions of the growth solution with a range of surfactants and with materials with distinctive surface moieties. LPD promises lower production costs and environmental impact as compared to present methods of coating technology, because it is an inherently simple process, using low temperatures and inexpensive air-stable reactants. Silica is ubiquitous in materials science. Its applications range from thixotropic additives for paint to gate dielectrics in the semiconductor industry. Nano-structured coatings and thin films are integral in today's electronics industry and will become more vital as the size of electronics shrinks. With the incorporation of nanoparticles in future devices, the ability to deposit quality coatings with finely tuned properties becomes paramount. The methods developed herein have applications in fabricating insulators for use in the future molecular scale electronics industry. Additionally, these silica nanoparticles have applications as templates for use in photonics and fuel cell membrane production and lend strength and durability to composites.

  15. Silica coated ionic liquid templated mesoporous silica nanoparticles ...

    African Journals Online (AJOL)

    A series of long chain pyridinium based ionic liquids 1-tetradecylpyridinium bromide, 1-hexadecylpyridinium bromide and 1-1-octadecylpyridinium bromide were used as templates to prepare silica coated mesoporous silica nanoparticles via condensation method under basic condition. The effects of alkyl chain length on ...

  16. Hydrothermal stability of microporous silica and niobia-silica membranes

    NARCIS (Netherlands)

    Boffa, V.; Blank, David H.A.; ten Elshof, Johan E.

    2008-01-01

    The hydrothermal stability of microporous niobia–silica membranes was investigated and compared with silica membranes. The membranes were exposed to hydrothermal conditions at 150 and 200 °C for 70 h. The change of pore structure before and after exposure to steam was probed by single-gas permeation

  17. Wear resistance and electrical properties of functionally graded epoxy-resin/silica composites

    International Nuclear Information System (INIS)

    Rihan, Y. A.; Abd El-Bary, B.

    2012-12-01

    In this paper graded Silica/Epoxy composite fabricated by controlled mold filling to obtain a stepwise graded structure. The generated graded structure was controlled by the w 1% content of silica particulates of size range from (45 μm-250 μm). Microstructural characterization was conducted using Scanning Electron Microscope (SEM). Electrical properties were conducted in High Voltage-Lab using Sphere-Plate Electrode System and Insulating resistance equipment s. Wear characteristics were studied using Block-on-Ring wear testing machine for the different layers of the graded silica/epoxy composites, The prepared materials are used as coating materials for the floors of chemical laboratories. (Author)

  18. Pecan drying with silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Ghate, S.R.; Chhinnan, M.S.

    1983-07-01

    High moisture in-shell pecans were dried by keeping them in direct and indirect contact with silica gel to investigate their drying characteristics. In-shell pecans were also dried with ambient air from a controlled environment chamber and with air dehumidified by silica gel. Direct contact and dehumidified air drying seemed feasible approaches.

  19. Tetragonal zirconia quantum dots in silica matrix prepared by a modified sol-gel protocol

    Science.gov (United States)

    Verma, Surbhi; Rani, Saruchi; Kumar, Sushil

    2018-05-01

    Tetragonal zirconia quantum dots (t-ZrO2 QDs) in silica matrix with different compositions ( x)ZrO2-(100 - x)SiO2 were fabricated by a modified sol-gel protocol. Acetylacetone was added as a chelating agent to zirconium propoxide to avoid precipitation. The powders as well as thin films were given thermal treatment at 650, 875 and 1100 °C for 4 h. The silica matrix remained amorphous after thermal treatment and acted as an inert support for zirconia quantum dots. The tetragonal zirconia embedded in silica matrix transformed into monoclinic form due to thermal treatment ≥ 1100 °C. The stability of tetragonal phase of zirconia is found to enhance with increase in silica content. A homogenous dispersion of t-ZrO2 QDs in silica matrix was indicated by the mapping of Zr, Si and O elements obtained from scanning electron microscope with energy dispersive X-ray analyser. The transmission electron images confirmed the formation of tetragonal zirconia quantum dots embedded in silica. The optical band gap of zirconia QDs (3.65-5.58 eV) was found to increase with increase in zirconia content in silica. The red shift of PL emission has been exhibited with increase in zirconia content in silica.

  20. Repetitive heterocoagulation of oppositely charged particles for enhancement of magnetic nanoparticle loading into monodisperse silica particles.

    Science.gov (United States)

    Matsumoto, Hideki; Nagao, Daisuke; Konno, Mikio

    2010-03-16

    Oppositely charged particles were repetitively heterocoagulated to fabricate highly monodisperse magnetic silica particles with high loading of magnetic nanoparticles. Positively charged magnetic nanoparticles prepared by surface modification with N-trimethoxysilylpropyl-N,N,N-trimethylammonium chloride (TSA) were used to heterocoagulate with silica particles under basic conditions to give rise to negative silica surface charge and prevent the oxidation of the magnetic nanoparticles. The resultant particles of silica core homogeneously coated with the magnetic nanoparticles were further coated with thin silica layer with sodium silicate in order to enhance colloidal stability and avoid desorption of the magnetic nanoparticles from the silica cores. Five repetitions of the heterocoagulation and the silica coating could increase saturation magnetization of the magnetic silica particles to 27.7 emu/g, keeping the coefficient of variation of particle sizes (C(V)) less than 6.5%. Highly homogeneous loading of the magnetic component was confirmed by measuring Fe-to-Si atomic ratios of individual particles with energy dispersive X-ray spectroscopy.

  1. Digital fabrication

    CERN Document Server

    2012-01-01

    The Winter 2012 (vol. 14 no. 3) issue of the Nexus Network Journal features seven original papers dedicated to the theme “Digital Fabrication”. Digital fabrication is changing architecture in fundamental ways in every phase, from concept to artifact. Projects growing out of research in digital fabrication are dependent on software that is entirely surface-oriented in its underlying mathematics. Decisions made during design, prototyping, fabrication and assembly rely on codes, scripts, parameters, operating systems and software, creating the need for teams with multidisciplinary expertise and different skills, from IT to architecture, design, material engineering, and mathematics, among others The papers grew out of a Lisbon symposium hosted by the ISCTE-Instituto Universitario de Lisboa entitled “Digital Fabrication – A State of the Art”. The issue is completed with four other research papers which address different mathematical instruments applied to architecture, including geometric tracing system...

  2. Silica research in Glasgow

    International Nuclear Information System (INIS)

    Barr, B W; Cagnoli, G; Casey, M M; Clubley, D; Crooks, D R M; Danzmann, K; Elliffe, E J; Gossler, S; Grant, A; Grote, H; Heptonstall, A; Hough, J; Jennrich, O; Lueck, H; McIntosh, S A; Newton, G P; Palmer, D A; Plissi, M V; Robertson, D I; Robertson, N A; Rowan, S; Skeldon, K D; Sneddon, P; Strain, K A; Torrie, C I; Ward, H; Willems, P A; Willke, B; Winkler, W

    2002-01-01

    The Glasgow group is involved in the construction of the GEO600 interferometer as well as in R and D activity on technology for advanced gravitational wave detectors. GEO600 will be the first GW detector using quasi-monolithic silica suspensions in order to decrease thermal noise significantly with respect to steel wire suspensions. The results concerning GEO600 suspension mounting and performance will be shown in the first section. Section 2 is devoted to the present results from the direct measurement of thermal noise in mirrors mounted in the 10 m interferometer in Glasgow which has a sensitivity limit of 4 x 10 -19 m Hz -1/2 above 1 kHz. Section 3 presents results on the measurements of coating losses. R and D activity has been carried out to understand better how thermal noise in the suspensions affects the detector sensitivity, and in section 4 a discussion on the non-linear thermoelastic effect is presented

  3. 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.

  4. An efficient hybrid, nanostructured, epoxidation catalyst: titanium silsesquioxane-polystyrene copolymer supported on SBA-15

    NARCIS (Netherlands)

    Santen, van R.A.; Zhang, Lei; Abbenhuis, H.C.L.; Gerritsen, G.; Ní Bhriain, N.M.; Magusin, P.C.M.M.; Mezari, B.; Han, W.; Yang, Q.; Li, Can

    2007-01-01

    A novel interfacial hybrid epoxidation catalyst was designed with a new immobilization method for homogeneous catalysts by coating an inorganic support with an organic polymer film containing active sites. The titanium silsesquioxane (TiPOSS) complex, which contains a single-site titanium active

  5. SBA-15-Pr–SO3H: An efficient, environment friendly and recyclable ...

    Indian Academy of Sciences (India)

    heterogeneous nanoreactor catalyst for the one-pot multicomponent ... synthetic methodology is of paramount importance. ..... a All products were characterised by comparison of their spectral and physical data with those of the authentic ...

  6. Metathesis of cardanol over Ru catalysts supported on mesoporousmolecular sieve SBA-15

    Czech Academy of Sciences Publication Activity Database

    Shinde, Tushar; Varga, Vojtěch; Polášek, Miroslav; Horáček, Michal; Žilková, Naděžda; Balcar, Hynek

    2014-01-01

    Roč. 478, MAY 2014 (2014), s. 138-145 ISSN 0926-860X R&D Projects: GA ČR(CZ) GAP106/12/0189 Institutional support: RVO:61388955 Keywords : cardanol * metathesis * supported catalysts Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.942, year: 2014

  7. Hoveyda-Grubbs type metathesis catalyst immobilized on mesoporous molecular sieves MCM-41 and SBA-15

    Czech Academy of Sciences Publication Activity Database

    Balcar, Hynek; Shinde, Tushar; Žilková, Naděžda; Bastl, Zdeněk

    2011-01-01

    Roč. 7, January (2011), s. 22-28 ISSN 1860-5397 R&D Projects: GA AV ČR IAA400400805; GA AV ČR KAN100400701 Institutional research plan: CEZ:AV0Z40400503 Keywords : alkene metathesis * catalyst immobilization * hybrid catalysis Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.517, year: 2011

  8. Metathesis of cardanol over ammonium tagged Hoveyda-Grubbs type catalyst supported on SBA-15

    Czech Academy of Sciences Publication Activity Database

    Balcar, Hynek; Žilková, Naděžda; Kubů, Martin; Polášek, Miroslav; Zedník, J.

    2018-01-01

    Roč. 304, APR 2018 (2018), s. 127-134 ISSN 0920-5861 R&D Projects: GA ČR GA17-01440S Institutional support: RVO:61388955 Keywords : Cardanol * Flow chemistry * Hoveyda-Grubbs type catalyst * Immobilized catalyst Subject RIV: CF - Physical ; Theoretical Chemistry OBOR OECD: Physical chemistry Impact factor: 4.636, year: 2016

  9. Superamphiphobic cotton fabrics with enhanced stability

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Bi, E-mail: xubi@dhu.edu.cn [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, Shanghai 201620 (China); Key Laboratory of Science & Technology of Eco-Textile, Ministry of Education, Donghua University, Shanghai 201620 (China); College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai 201620 (China); Ding, Yinyan; Qu, Shaobo [College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai 201620 (China); Cai, Zaisheng, E-mail: zshcai@dhu.edu [College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai 201620 (China)

    2015-11-30

    Highlights: • Superamphiphobic cotton fabrics were prepared. • Water and hexadecane contact angels reach to 164.4° and 156.3°, respectively. • Nanoporous organically modified silica alcogel particles were synthesized. • The superamphiphobic cotton fabrics exhibit enhanced stability against abrasion, laundering and acid. - Abstract: Superamphiphobic cotton fabrics were prepared by alternately depositing organically modified silica alcogel (ormosil) particles onto chitosan precoated cotton fabrics and subsequent 1H, 1H, 2H, 2H-perfluorooctyltrimethoxysilane (PFOTMS) modification. Transmission electron microscopy and scanning electron microscopy images reveal that the ormosil particles display a fluffy, sponge-like nanoporous structure, and the entire cotton fiber surface is covered with highly porous networks. PFOTMS acts as not only a modifier to lower the surface energy of the cotton fabric but also a binder to enhance the coating stability against abrasion and washing. The treated cotton fabrics show highly liquid repellency with the water, cooking oil and hexadecane contact angels reaching to 164.4°, 160.1° and 156.3°, respectively. Meanwhile, the treated cotton fabrics exhibit good abrasion resistance and high laundering durability, which can withstand 10,000 cycles of abrasion and 30 cycles of machine wash without apparently changing the superamphiphobicity. The superamphiphobic cotton fabric also shows high acid stability, and can withstand 98% H{sub 2}SO{sub 4}. Moreover, the superamphiphobic coating has almost no influence on the other physical properties of the cotton fabrics including tensile strength, whiteness and air permeability. This durable non-wetting surface may provide a wide range of new applications in the future.

  10. Photonic bandgap structure of 3-D fcc silica nanospheres

    Energy Technology Data Exchange (ETDEWEB)

    Woo, Y. K.; Ha, N. Y.; Hwang, Ji Soo; Chang, H. J.; Wu, J. W. [Dept. of Physics, Ewha Womans University, Seoul (Korea, Republic of)

    2002-07-01

    Photonic crystal is an artificial optical material with a periodic dielectric potential, hence exhibiting a bandgap for a propagating electromagnetic wave. We fabricated crystal possessing 3-D fcc opal structure from silica nanospheres. The crystals are self-assembled on a flat glass by evaporating the solvent in the nanosphere suspension at the room temperature. The suspension consists of silica nanospheres with a diameter of 200 nm. The microscopic arrangement of nanospheres is identified by a scanning electron microscope, the resulting structure being fcc.Transmission spectrum of the fabricated photonic crystal in the visible and near-infrared regions is measured at different incident angles to find the distinct Bragg peaks, analysis of which further confirmed the fcc structure of the photonic crystal. From the optical microscopic image, we find that the opal domain varies from 30 μm to 125 μm in size. In order to relate the observed Bragg peaks with the microscopic arrangement of silica nanospheres, we introduced the scalar wave approximation, where the electric field in the medium is treated as a scalar rather than a vector quantity. It is found that the theoretical prediction of the position of bandgap is in a good agreement with the experimental measurement.

  11. Photonic bandgap structure of 3-D fcc silica nanospheres

    International Nuclear Information System (INIS)

    Woo, Y. K.; Ha, N. Y.; Hwang, Ji Soo; Chang, H. J.; Wu, J. W.

    2002-01-01

    Photonic crystal is an artificial optical material with a periodic dielectric potential, hence exhibiting a bandgap for a propagating electromagnetic wave. We fabricated crystal possessing 3-D fcc opal structure from silica nanospheres. The crystals are self-assembled on a flat glass by evaporating the solvent in the nanosphere suspension at the room temperature. The suspension consists of silica nanospheres with a diameter of 200 nm. The microscopic arrangement of nanospheres is identified by a scanning electron microscope, the resulting structure being fcc.Transmission spectrum of the fabricated photonic crystal in the visible and near-infrared regions is measured at different incident angles to find the distinct Bragg peaks, analysis of which further confirmed the fcc structure of the photonic crystal. From the optical microscopic image, we find that the opal domain varies from 30 μm to 125 μm in size. In order to relate the observed Bragg peaks with the microscopic arrangement of silica nanospheres, we introduced the scalar wave approximation, where the electric field in the medium is treated as a scalar rather than a vector quantity. It is found that the theoretical prediction of the position of bandgap is in a good agreement with the experimental measurement.

  12. Macrocyclic ligand decorated ordered mesoporous silica with large-pore and short-channel characteristics for effective separation of lithium isotopes: synthesis, adsorptive behavior study and DFT modeling.

    Science.gov (United States)

    Liu, Yuekun; Liu, Fei; Ye, Gang; Pu, Ning; Wu, Fengcheng; Wang, Zhe; Huo, Xiaomei; Xu, Jian; Chen, Jing

    2016-10-18

    Effective separation of lithium isotopes is of strategic value which attracts growing attention worldwide. This study reports a new class of macrocyclic ligand decorated ordered mesoporous silica (OMS) with large-pore and short-channel characteristics, which holds the potential to effectively separate lithium isotopes in aqueous solutions. Initially, a series of benzo-15-crown-5 (B15C5) derivatives containing different electron-donating or -withdrawing substituents were synthesized. Extractive separation of lithium isotopes in a liquid-liquid system was comparatively studied, highlighting the effect of the substituent, solvent, counter anion and temperature. The optimal NH 2 -B15C5 ligands were then covalently anchored to a short-channel SBA-15 OMS precursor bearing alkyl halides via a post-modification protocol. Adsorptive separation of the lithium isotopes was fully investigated, combined with kinetics and thermodynamics analysis, and simulation by using classic adsorption isotherm models. The NH 2 -B15C5 ligand functionalized OMSs exhibited selectivity to lithium ions against other alkali metal ions including K(i). Additionally, a more efficient separation of lithium isotopes could be obtained at a lower temperature in systems with softer counter anions and solvents with a lower dielectric constant. The highest value separation factor (α = 1.049 ± 0.002) was obtained in CF 3 COOLi aqueous solution at 288.15 K. Moreover, theoretical computation based on the density functional theory (DFT) was performed to elucidate the complexation interactions between the macrocyclic ligands and lithium ions. A suggested mechanism involving an isotopic exchange equilibrium was proposed to describe the lithium isotope separation by the functionalized OMSs.

  13. Comparison of different mesoporous silicas for off-line solid phase extraction of 17β-estradiol from waters and its determination by HPLC-DAD.

    Science.gov (United States)

    Gañán, Judith; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

    2013-09-15

    Functionalized (SBA-C₁₈ and SM-C₁₈) and non-functionalized (SBA-15 and SM) mesoporous silicas were then examined as sorbents for solid-phase extraction of 17β-estradiol in aqueous media. Experiments were run in order to test critical factors affecting the procedure extraction efficiency, including the type of sorbent, the analyte concentration, the solvent and volume used for elution and the sample volume. Among the prepared materials, SBA-C₁₈ had the highest adsorption affinity towards 17β-estradiol and under optimized conditions (200mg of sorbent, 150 mL of water sample, elution with 3 × 2 mL of methanol) this sorbent proved good extraction capacity and elution efficiency for this hormone from aqueous media (recovery near 100%). To evaluate the analytical applicability of the proposed method, it was applied to the determination of 17β-estradiol in drinking water by high performance liquid chromatography with a photodiode array detector. Calibration curves were shown to be linear between 1.25 and 100 mg L(-1)with correlation coefficients ≥0.999 (n=5) for 17β-estradiol. The instrumental detection and quantitation limits calculated were 0.38 and 1.25 mg L(-1), respectively. The relative standard deviation obtained values were ≤3% and the mean recoveries obtained were of 82%. The results suggest that SBA-C18 is a promising material for the off-line solid phase extraction of 17β-estradiol from waters. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Silica research in Glasgow

    CERN Document Server

    Barr, B W; Casey, M M; Clubley, D; Crooks, D R M; Danzmann, K; Elliffe, E J; Gossler, S; Grant, A; Grote, H; Heptonstall, A; Hough, J; Jennrich, O; Lück, H B; McIntosh, S A; Newton, G P; Palmer, D A; Plissi, M V; Robertson, D I; Robertson, N A; Rowan, S; Skeldon, K D; Sneddon, P; Strain, K A; Torrie, C I; Ward, H; Willems, P A; Willke, B; Winkler, W

    2002-01-01

    The Glasgow group is involved in the construction of the GEO600 interferometer as well as in R and D activity on technology for advanced gravitational wave detectors. GEO600 will be the first GW detector using quasi-monolithic silica suspensions in order to decrease thermal noise significantly with respect to steel wire suspensions. The results concerning GEO600 suspension mounting and performance will be shown in the first section. Section 2 is devoted to the present results from the direct measurement of thermal noise in mirrors mounted in the 10 m interferometer in Glasgow which has a sensitivity limit of 4 x 10 sup - sup 1 sup 9 m Hz sup - sup 1 sup / sup 2 above 1 kHz. Section 3 presents results on the measurements of coating losses. R and D activity has been carried out to understand better how thermal noise in the suspensions affects the detector sensitivity, and in section 4 a discussion on the non-linear thermoelastic effect is presented.

  15. Silica decorated on porous activated carbon nanofiber composites for high-performance supercapacitors

    Science.gov (United States)

    Kim, So Yeun; Kim, Bo-Hye

    2016-10-01

    A hybrid of silica decorated on porous activated carbon nanofibers (ACNFs) is fabricated in the form of a web via electrospinning and an activation process as an electrode material for electrochemical capacitors in an organic electrolyte. The introduction of PhSiH3 (PS) into the polyacrylonitrile (PAN) solution induces a porous ACNF structure containing silica nanoparticles (NPs) via the spontaneous sol-gel process of PS by steam in the subsequent physical activation process. These inorganic-organic hybrid composites of porous ACNF containing silica NPs show superior specific capacitance and energy density in electrochemical tests, along with good rate capability and excellent cycle life in an organic electrolyte, which is attributed to the combination of ACNF's high surface area and silica's hydrophilicity. The electrochemical performance decreases with increasing PS concentration, and this trend is consistent with the specific surface area results, which reveal the rapid formation of a double layer.

  16. Surface-Enhanced Raman Scattering Using Silica Whispering-Gallery Mode Resonators

    Science.gov (United States)

    Anderson, Mark S.

    2013-01-01

    The motivation of this work was to have robust spectroscopic sensors for sensitive detection and chemical analysis of organic and molecular compounds. The solution is to use silica sphere optical resonators to provide surface-enhanced spectroscopic signal. Whispering-gallery mode (WGM) resonators made from silica microspheres were used for surface-enhanced Raman scattering (SERS) without coupling to a plasmonic mechanism. Large Raman signal enhancement is observed by exclusively using 5.08-micron silica spheres with 785-nm laser excitation. The advantage of this non-plasmonic approach is that the active substrate is chemically inert silica, thermally stable, and relatively simple to fabricate. The Raman signal enhancement is broadly applicable to a wide range of molecular functional groups including aliphatic hydrocarbons, siloxanes, and esters. Applications include trace organic analysis, particularly for in situ planetary instruments that require robust sensors with consistent response.

  17. Sodium alginate/gelatin with silica nanoparticles a novel hydrogel for 3D printing

    Science.gov (United States)

    Soni, Raghav; Roopavath, Uday Kiran; Mahanta, Urbashi; Deshpande, A. S.; Rath, S. N.

    2018-05-01

    Sodium alginate/gelatin hydrogels are promising materials for 3D bio-printing due to its good biocompatibility and biodegradability. Gelatin is used for thermal crosslinking and its cell adhesion properties. Hence patient specific sodium alginate/gelatin hydrogel scaffolds can be bio-fabricated in a temperature range of 4-14 oC. In this study we made an attempt to introduce silica (SiO2) nanoparticles in the polymer network of sodium alginate (2.5%)/gelatin (8%) hydrogel at different concentrations (w/v) as 0%, 1.25%, 2.5%, 5%, and 7.5%. The effect of silica nanoparticles on viscosity, swelling behavior, and degradation rate are analyzed. Hydrogels with 5% silica nanoparticles show significantly less swelling and degradation when compared to other concentrations. The viscosity of the hydrogels gradually increases up to 5% addition of silica nanoparticles enhancing the stability of 3D printed structures.

  18. Miniature all-silica optical fiber pressure sensor with an ultrathin uniform diaphragm.

    Science.gov (United States)

    Wang, Wenhui; Wu, Nan; Tian, Ye; Niezrecki, Christopher; Wang, Xingwei

    2010-04-26

    This paper presents an all-silica miniature optical fiber pressure/acoustic sensor based on the Fabry-Perot (FP) interferometric principle. The endface of the etched optical fiber tip and silica thin diaphragm on it form the FP structure. The uniform and thin silica diaphragm was fabricated by etching away the silicon substrate from a commercial silicon wafer that has a thermal oxide layer. The thin film was directly thermally bonded to the endface of the optical fiber thus creating the Fabry-Perot cavity. Thin films with a thickness from 1microm to 3microm have been bonded successfully. The sensor shows good linearity and hysteresis during measurement. A sensor with 0.75 microm-thick diaphragm thinned by post silica etching was demonstrated to have a sensitivity of 11 nm/kPa. The new sensor has great potential to be used as a non-intrusive pressure sensor in a variety of sensing applications.

  19. Double-Layer Magnetic Nanoparticle-Embedded Silica Particles for Efficient Bio-Separation.

    Directory of Open Access Journals (Sweden)

    San Kyeong

    Full Text Available Superparamagnetic Fe3O4 nanoparticles (NPs based nanomaterials have been exploited in various biotechnology fields including biomolecule separation. However, slow accumulation of Fe3O4 NPs by magnets may limit broad applications of Fe3O4 NP-based nanomaterials. In this study, we report fabrication of Fe3O4 NPs double-layered silica nanoparticles (DL MNPs with a silica core and highly packed Fe3O4 NPs layers. The DL MNPs had a superparamagnetic property and efficient accumulation kinetics under an external magnetic field. Moreover, the magnetic field-exposed DL MNPs show quantitative accumulation, whereas Fe3O4 NPs single-layered silica nanoparticles (SL MNPs and silica-coated Fe3O4 NPs produced a saturated plateau under full recovery of the NPs. DL MNPs are promising nanomaterials with great potential to separate and analyze biomolecules.

  20. Gas Separation through Bilayer Silica, the Thinnest Possible Silica Membrane.

    Science.gov (United States)

    Yao, Bowen; Mandrà, Salvatore; Curry, John O; Shaikhutdinov, Shamil; Freund, Hans-Joachim; Schrier, Joshua

    2017-12-13

    Membrane-based gas separation processes can address key challenges in energy and environment, but for many applications the permeance and selectivity of bulk membranes is insufficient for economical use. Theory and experiment indicate that permeance and selectivity can be increased by using two-dimensional materials with subnanometer pores as membranes. Motivated by experiments showing selective permeation of H 2 /CO mixtures through amorphous silica bilayers, here we perform a theoretical study of gas separation through silica bilayers. Using density functional theory calculations, we obtain geometries of crystalline free-standing silica bilayers (comprised of six-membered rings), as well as the seven-, eight-, and nine-membered rings that are observed in glassy silica bilayers, which arise due to Stone-Wales defects and vacancies. We then compute the potential energy barriers for gas passage through these various pore types for He, Ne, Ar, Kr, H 2 , N 2 , CO, and CO 2 gases, and use the data to assess their capability for selective gas separation. Our calculations indicate that crystalline bilayer silica, which is less than a nanometer thick, can be a high-selectivity and high-permeance membrane material for 3 He/ 4 He, He/natural gas, and H 2 /CO separations.

  1. Study of silica sol-gel materials for sensor development

    Science.gov (United States)

    Lei, Qiong

    Silica sol-gel is a transparent, highly porous silicon oxide glass made at room temperature by sol-gel process. The name of silica sol-gel comes from the observable physical phase transition from liquid sol to solid gel during its preparation. Silica sol-gel is chemically inert, thermally stable, and photostable, it can be fabricated into different desired shapes during or after gelation, and its porous structure allows encapsulation of guest molecules either before or after gelation while still retaining their functions and sensitivities to surrounding environments. All those distinctive features make silica sol-gel ideal for sensor development. Study of guest-host interactions in silica sol-gel is important for silica-based sensor development, because it helps to tailor local environments inside sol-gel matrix so that higher guest loading, longer shelf-life, higher sensitivity and faster response of silica gel based sensors could be achieved. We focused on pore surface modification of two different types of silica sol-gel by post-grafting method, and construction of stable silica hydrogel-like thin films for sensor development. By monitoring the mobility and photostability of rhodamine 6G (R6G) molecules in silica alcogel thin films through single molecule spectroscopy (SMS), the guest-host interactions altered by post-synthesis grafting were examined. While physical confinement remains the major factor that controls mobility in modified alcogels, both R6G mobility and photostability register discernable changes after surface charges are respectively reversed and neutralized by aminopropyltriethoxysilane (APTS) and methyltriethoxysilane (MTES) grafting. The change in R6G photostability was found to be more sensitive to surface grafting than that of mobility. In addition, silica film modification by 0.4% APTS is as efficient as that by pure MTES in lowering R6G photostability, which suggests that surface charge reversal is more effective than charge neutralization

  2. Influence of p H on optical properties of nano structure sol-gel-derived silica films

    International Nuclear Information System (INIS)

    Heshmatpuor, F.; Adelkhani, H.; Nahavandi, M.; Noorbakhsh Shourabadi, M.

    2006-01-01

    Sol-gel derived silica films were fabricated by dip-coating onto glass microscope substrates. Film properties such as transmission and surface morphology were monitored as function of dip speed and sol p H. Film transmission was increased with increasing of p H in visible range. The surface morphology of films were investigated with scanning electron microscopy.

  3. Spin-on nanostructured silicon-silica film displaying room-temperature nanosecond lifetime photoluminescence

    Energy Technology Data Exchange (ETDEWEB)

    Cohen, Y.; Hatton, B.; Miguez, H.; Coombs, N.; Fournier-Bidoz, S.; Ozin, G.A. [Materials Chemistry Research Group, Department of Chemistry, Lash Miller Chemical Laboratories, University of Toronto, 80 St. George Street, Toronto, Ontario, M5S 3H6 (Canada); Grey, J.K.; Beaulac, R.; Reber, C. [Department of Chemistry, University of Montreal, Montreal, Quebec H3C 3J7 (Canada)

    2003-04-17

    A yellow transparent mesoporous silica film has been achieved by the incorporation of silicon nanoclusters into its channels. The resulting nanocomposite - fabricated using a combination of evaporation induced self- assembly and chemical vapor deposition - emits light brightly at visible wavelengths and has nanosecond radiative lifetimes at room temperature when excited by ultraviolet light (see Figure). (Abstract Copyright [2003], Wiley Periodicals, Inc.)

  4. 5.4W cladding-pumped Nd:YAG silica fiber laser

    OpenAIRE

    Yoo, S.; Webb, A.S.; Standish, R.J.; May-Smith, T.C.; Sahu, J.K.

    2012-01-01

    We report on the spectroscopy and laser characteristics of Nd-doped fiber, fabricated by rod-in-tube from Nd:YAG as a core material with silica cladding. A cladding-pumped CW laser operation at 1058nm with 52% slope-efficiency is demonstrated.

  5. Effect of air on water capillary flow in silica nanochannels

    DEFF Research Database (Denmark)

    Zambrano, Harvey; Walther, Jens Honore; Oyarzua, Elton

    2013-01-01

    , with the fabrication of microsystems integrated by nanochannels, a thorough understanding of the transport of fluids in nanoconfinement is required for a successful operation of the functional parts of such devices. In this work, Molecular Dynamics simulations are conducted to study the spontaneous imbibition of water...... in sub 10 nm silica channels. The capillary filling speed is computed in channels subjected to different air pressures. In order to describe the interactions between the species, an effective force field is developed, which is calibrated by reproducing the water contact angle. The results show...... that the capillary filling speed qualitatively follows the classical Washburn model, however, quantitatively it is lower than expected. Furthermore, it is observed that the deviations increase as air pressure is higher. We attribute the deviations to amounts of air trapped at the silica-water interface which leads...

  6. A trifunctional mesoporous silica-based, highly active catalyst for one-pot, three-step cascade reactions.

    Science.gov (United States)

    Biradar, Ankush V; Patil, Vijayshinha S; Chandra, Prakash; Doke, Dhananjay S; Asefa, Tewodros

    2015-05-18

    We report the synthesis of a trifunctional catalyst containing amine, sulphonic acid and Pd nanoparticle catalytic groups anchored on the pore walls of SBA-15. The catalyst efficiently catalyzes one-pot three-step cascade reactions comprising deacetylation, Henry reaction and hydrogenation, giving up to ∼100% conversion and 92% selectivity to the final product.

  7. Pumping Iron and Silica Bodybuilding

    Science.gov (United States)

    Mcnair, H.; Brzezinski, M. A.; Krause, J. W.; Parker, C.; Brown, M.; Coale, T.; Bruland, K. W.

    2016-02-01

    The availability of dissolved iron influences the stoichiometry of nutrient uptake by diatoms. Under nutrient replete conditions diatoms consume silicic acid and nitrate in a 1:1 ratio, this ratio increases under iron stress. Using the tracers 32Si and PDMPO, the total community and group-specific silica production rates were measured along a gradient of dissolved iron in an upwelling plume off the California coast. At each station, a control (ambient silicic acid) and +20 µM silicic acid treatment were conducted with each tracer to determine whether silicic acid limitation controlled the rate of silica production. Dissolved iron was 1.3 nmol kg-1 nearshore and decreased to 0.15 nmol kg-1 offshore. Silicic acid decreased more rapidly than nitrate, it was nearly 9 µM higher in the nearshore and 7 µM lower than nitrate in the middle of the transect where the iron concentration had decreased. The rate of diatom silica production decreased in tandem with silicic acid concentration, and silica production limitation by low silicic acid was most pronounced when iron concentrations were >0.4 nmol kg-1. The composition of the diatom assemblage shifted from Chaetoceros spp. dominated nearshore to a more sparse pennate-dominated assemblage offshore. Changes in taxa-specific silica production rates will be reported based on examination of PDMPO labeled cells using confocal microscopy.

  8. Three-dimensional metallic opals fabricated by double templating

    International Nuclear Information System (INIS)

    Yan Qingfeng; Nukala, Pavan; Chiang, Yet-Ming; Wong, C.C.

    2009-01-01

    We report a simple and cost-effective double templating method for fabricating large-area three-dimensional metallic photonic crystals of controlled thickness. A self-assembled polystyrene opal was used as the first template to fabricate a silica inverse opal on a gold-coated glass substrate via sol-gel processing. Gold was subsequently infiltrated to the pores of the silica inverse opal using electrochemical deposition. A high-quality three-dimensional gold photonic crystal was obtained after removal of the secondary template (silica inverse opal). The effects of template sphere size and deposition current density on the gold growth rate, and the resulting morphology and growth mechanism of the gold opal, were investigated.

  9. Characteristics of silica rice husk ash from Mojogedang Karanganyar Indonesia

    Science.gov (United States)

    Suryana, R.; Iriani, Y.; Nurosyid, F.; Fasquelle, D.

    2018-05-01

    Indonesia is one of the countries in the world as the most abundant rice producer. Many researchers have demonstrated that the highest composition in the rice husk ash (RHA) is silica. Some of the advantages in utilizing silica as the raw material is the manufacture of ceramics, zeolite synthesis, fabrication of glass, electronic insulator materials, and as a catalyst. The amount of silica from rice husk ash is different for each region. Therefore, the study of silica from RHA is still promising, especially rice organic fertilizers. In this study, the rice came from Mojogedang Karanganyar Indonesia. Rice husk was dried under the solar radiation. Then the rice husk was heated in two steps: the first step at a temperature of 300°C and the second step at a temperature of 1200°C with a holding time at 2 h and 1 h, respectively. Furthermore, the temperature of the second step was varied at 1400 °C and 1600 °C. This heating process produced RHA. The content of RHA was observed on the EDAX spectrums while the morphology was observed from SEM images. The crystal structure of RHA was determined from XRD spectrums. The EDAX spectrums showed that RHA composition was dominated by elements Si and O for all the heating temperature. SEM images showed an agglomeration towards larger domains as heating temperatures increase. Analysis of XRD spectra is polycrystalline silica formed with the significant crystal orientation at 101, 102 and 200. The intensity of 101 increases significantly with increasing temperature. It is concluded that the crystal growth in the direction of 101 is preferred.

  10. Fabrication and characterization of Aerogel-Polydimethyl siloxane (PDMS) Insulation Film

    Science.gov (United States)

    Noh, Yeoung ah; Song, Sinae; Taik Kim, Hee

    2018-03-01

    The building has a large impact on the space heating demand and the indoor environment is affected by climate or daylight. Hence, silica aerogel has generally used as a film to reduce the coefficient of the window in the building. Silica aerogel is a suitable material to apply for insulation material with lower thermal conductivity than that of air to save interior energy. However expensive precursor and drying process were the main issue of the silica aerogel synthesis and practical usage. We attempt to fabricate aerogel insulation film for energy saving through the economic process under ambient pressure. Silica aerogel was synthesized from rice husk ash, which was an agricultural waste to be able to recycle. Taguchi design was used to optimize the parameters (amount of rice husk ash, pH, aging time) controlling the surface area of silica aerogel. The silica aerogel is prepared by sol-gel processing through acidic treatment and aging. The silica aerogel was obtained by modification of silica hydrogel surface and dry at ambient pressure. Finally, aerogel film was respectively fabricated by the different content of aerogel in polydimethylsiloxane (PDMS). Silica aerogel obtained 21 – 24nm average particle size was analyzed by SEM and silica aerogel with high surface area (832.26 m2/g), pore size ( 3.30nm ) was characterized by BET. Then silica Aerogel – PDMS insulation film with thermal conductivity (0.002 W/mK) was analyzed by thermal wave system. The study demonstrates an eco-friendly and low-cost route toward silica – PDMS insulation film with low thermal conductivity (0.002 W/mK).

  11. Impact behavior of f-silica and amine terminated polybutadiene co-acrylonitrile rubber modified novolac epoxy/Kevlar nanocomposites

    Science.gov (United States)

    Kavita, Pal, Vijayeta; Tiwari, R. K.

    2018-05-01

    In the present work, nano-fumed silica treated with 3-Glycidoxypropyl trimethoxy silane (f-silica) was used as a nanoreinforcement in the fabrication of amine terminated polybutadiene co-acrylonitrile rubber (ATBN) modified Kevlar/epoxy based nanocomposites. Nanocomposites with different f-silica loading (0, 0.5, 1.0 and 2.0 wt. %) and having same ATBN (10 wt. %) were made and characterized by Izod impact test for evaluating impact strength values. All the nanocomposites showed better impact strength than neat Kevlar/novolac epoxy based composite.

  12. Wash fastness improvement of malachite green-dyed cotton fabrics ...

    Indian Academy of Sciences (India)

    Administrator

    Nano-size features of both silica and titania nanosols are predicted to enhance the wash fastness of ... The cotton fabric was obtained from traditional market and was previously tested to contain fully cellulose ..... The authors acknowledge financial support of DP2M,. Directorate General of Higher Education, Indonesia,.

  13. Symmetrical waveguide devices fabricated by direct UV writing

    DEFF Research Database (Denmark)

    Færch, Kjartan Ullitz; Svalgaard, Mikael

    2002-01-01

    Power splitters and directional couplers fabricated by direct UV writing in index matched silica-on-silicon samples can suffer from an asymmetrical device performance, even though the UV writing is carried out in a symmetrical fashion. This effect originates from a reduced photosensitivity...

  14. Silica-sol-based spin-coating barrier layer against phosphorous diffusion for crystalline silicon solar cells.

    Science.gov (United States)

    Uzum, Abdullah; Fukatsu, Ken; Kanda, Hiroyuki; Kimura, Yutaka; Tanimoto, Kenji; Yoshinaga, Seiya; Jiang, Yunjian; Ishikawa, Yasuaki; Uraoka, Yukiharu; Ito, Seigo

    2014-01-01

    The phosphorus barrier layers at the doping procedure of silicon wafers were fabricated using a spin-coating method with a mixture of silica-sol and tetramethylammonium hydroxide, which can be formed at the rear surface prior to the front phosphorus spin-on-demand (SOD) diffusion and directly annealed simultaneously with the front phosphorus layer. The optimization of coating thickness was obtained by changing the applied spin-coating speed; from 2,000 to 8,000 rpm. The CZ-Si p-type silicon solar cells were fabricated with/without using the rear silica-sol layer after taking the sheet resistance measurements, SIMS analysis, and SEM measurements of the silica-sol material evaluations into consideration. For the fabrication of solar cells, a spin-coating phosphorus source was used to form the n(+) emitter and was then diffused at 930°C for 35 min. The out-gas diffusion of phosphorus could be completely prevented by spin-coated silica-sol film placed on the rear side of the wafers coated prior to the diffusion process. A roughly 2% improvement in the conversion efficiency was observed when silica-sol was utilized during the phosphorus diffusion step. These results can suggest that the silica-sol material can be an attractive candidate for low-cost and easily applicable spin-coating barrier for any masking purpose involving phosphorus diffusion.

  15. Power Generation from Concentration Gradient by Reverse Electrodialysis in Dense Silica Membranes for Microfluidic and Nanofluidic Systems

    Directory of Open Access Journals (Sweden)

    Sang Woo Lee

    2016-01-01

    Full Text Available In this study, we investigate power generation by reverse electrodialysis in a dense silica membrane that is between two NaCl solutions with various combinations of concentrations. Each silica membrane is fabricated by depositing a silica layer on a porous alumina substrate via chemical vapor deposition. The measured potential-current (V-I characteristics of the silica membrane are used to obtain the transference number, diffusion potential, and electrical resistance. We develop empirical correlations for the transference number and the area-specific resistance, and present the results of power generation by reverse electrodialysis using the fabricated silica membranes. The highest measured power density is 0.98 mW/m2. In addition, we develop a contour map of the power density as a function of NaCl concentrations on the basis of the empirical correlations. The contour map shows that a power output density of 1.2 mW/m2 is achievable with the use of silica membranes and is sufficient to drive nanofluidic and microfluidic systems. The dense silica membrane has the potential for use in micro power generators in nanofluidic and microfluidic systems.

  16. Control of silicification by genetically engineered fusion proteins: silk-silica binding peptides.

    Science.gov (United States)

    Zhou, Shun; Huang, Wenwen; Belton, David J; Simmons, Leo O; Perry, Carole C; Wang, Xiaoqin; Kaplan, David L

    2015-03-01

    In the present study, an artificial spider silk gene, 6mer, derived from the consensus sequence of Nephila clavipes dragline silk gene, was fused with different silica-binding peptides (SiBPs), A1, A3 and R5, to study the impact of the fusion protein sequence chemistry on silica formation and the ability to generate a silk-silica composite in two different bioinspired silicification systems: solution-solution and solution-solid. Condensed silica nanoscale particles (600-800 nm) were formed in the presence of the recombinant silk and chimeras, which were smaller than those formed by 15mer-SiBP chimeras, revealing that the molecular weight of the silk domain correlated to the sizes of the condensed silica particles in the solution system. In addition, the chimeras (6mer-A1/A3/R5) produced smaller condensed silica particles than the control (6mer), revealing that the silica particle size formed in the solution system is controlled by the size of protein assemblies in solution. In the solution-solid interface system, silicification reactions were performed on the surface of films fabricated from the recombinant silk proteins and chimeras and then treated to induce β-sheet formation. A higher density of condensed silica formed on the films containing the lowest β-sheet content while the films with the highest β-sheet content precipitated the lowest density of silica, revealing an inverse correlation between the β-sheet secondary structure and the silica content formed on the films. Intriguingly, the 6mer-A3 showed the highest rate of silica condensation but the lowest density of silica deposition on the films, compared with 6mer-A1 and -R5, revealing antagonistic crosstalk between the silk and the SiBP domains in terms of protein assembly. These findings offer a path forward in the tailoring of biopolymer-silica composites for biomaterial related needs. Copyright © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  17. Silica nanoparticle stability in biological media revisited.

    Science.gov (United States)

    Yang, Seon-Ah; Choi, Sungmoon; Jeon, Seon Mi; Yu, Junhua

    2018-01-09

    The stability of silica nanostructure in the core-silica shell nanomaterials is critical to understanding the activity of these nanomaterials since the exposure of core materials due to the poor stability of silica may cause misinterpretation of experiments, but unfortunately reports on the stability of silica have been inconsistent. Here, we show that luminescent silver nanodots (AgNDs) can be used to monitor the stability of silica nanostructures. Though relatively stable in water and phosphate buffered saline, silica nanoparticles are eroded by biological media, leading to the exposure of AgNDs from AgND@SiO 2 nanoparticles and the quenching of nanodot luminescence. Our results reveal that a synergistic effect of organic compounds, particularly the amino groups, accelerates the erosion. Our work indicates that silica nanostructures are vulnerable to cellular medium and it may be possible to tune the release of drug molecules from silica-based drug delivery vehicles through controlled erosion.

  18. Development of silica RO membranes

    International Nuclear Information System (INIS)

    Ikeda, Ayumi; Kawamoto, Takashi; Matsuyama, Emi; Utsumi, Keisuke; Nomura, Mikihiro; Sugimoto, Masaki; Yoshikawa, Masato

    2012-01-01

    Silica based membranes have been developed by using a counter diffusion CVD method. Effects of alkyl groups in the silica precursors and deposition temperatures had investigated in order to control pore sizes of the silica membranes. In this study, this type of a silica membrane was applied for RO separation. Effects of silica sources, deposition temperatures and post treatments had been investigated. Tetramethoxysilane (TMOS), Ethyltrimethoxysilane (ETMOS) and Phenyltrimethoxysilane (PhTMOS) were used as silica precursors. A counter diffusion CVD method was carried out for 90 min at 270 - 600degC on γ-alumina capillary substrates (effective length: 50 mm, φ: 4 nm: NOK Co.). O 3 or O 2 was introduced into the inside of the substrate at the O 2 rate of 0.2 L min -1 . Ion beam irradiation was carried out for a post treatment using Os at 490 MeV for 1.0 x 10 10 ions cm -2 or 3.0 x 10 10 ions cm -2 . Single gas permeance was measured by using H 2 , N 2 and SF 6 . RO tests were employed at 3.0 or 5.4 MPa for 100 mg L -1 of feed NaCl solution. First, effects of the silica sources were investigated. The total fluxes increased by increasing N 2 permeance through the silica membrane deposited by ETMOS. The maximum NaCl rejection was 28.2% at 12.2 kg m -2 h -1 of the total flux through the membrane deposited at 270degC. N 2 permeance was 9.6 x 10 -9 mol m -2 s -1 Pa -1 . While, total fluxes through the membrane deposited by using PhTMOS were smaller than those through the ETMOS membranes. The phenyl groups for the PhTMOS membrane must be important for the hydrophobic properties through the membrane. Next, effects of ion beam irradiation were tested for the TMOS membranes. Water is difficult to permeate through the TMOS membranes due to the low N 2 permeance through the membrane (3.1 x 10 -11 mol m -2 s -1 Pa -1 ). N 2 permeance increased to 7.3 x 10 -9 mol m -2 s -1 Pa -1 by the irradiation. Irradiation amounts had little effects on N 2 permeance. However, NaCl rejections

  19. Niobia-silica and silica membranes for gas separation

    NARCIS (Netherlands)

    Boffa, V.

    2008-01-01

    This thesis describes the development of ceramic membranes suitable for hydrogen separation and CO2 recovery from gaseous streams. The research work was focused on the three different parts of which gas selective ceramic membranes are composed, i.e., the microporous gas selective silica layer, the

  20. The strength and failure of silica optical fibers

    International Nuclear Information System (INIS)

    Yan, C; Bai, R X; Yu, H; Canning, J; Law, S

    2010-01-01

    The mechanical strength and failure behavior of conventional and microstructured silica optical fibers was investigated using a tensile test and fracture mechanics and numerical analyses. The effect of polymer coating on failure behavior was also studied. The results indicate that all these fibers fail in a brittle manner and failure normally starts from fiber surfaces. The failure loads observed in coated fibers are higher than those in bare fibers. The introduction of air holes reduces fiber strength and their geometrical arrangements have a remarkable effect on stress distribution in the longitudinal direction. These results are potentially useful for the design, fabrication and evaluation of optical fibers for a wide range of applications.

  1. Sonochemical coating of magnetite nanoparticles with silica.

    Science.gov (United States)

    Dang, Feng; Enomoto, Naoya; Hojo, Junichi; Enpuku, Keiji

    2010-01-01

    Magnetite nanoparticles were coated with silica through the hydrolysis and condensation of tetraethyl orthosilicate (TEOS) under ultrasonic irradiation. The ultrasonic irradiation was used to prevent the agglomeration of the magnetite particles and accelerate the hydrolysis and condensation of TEOS. TEM, DLS, XRF, VSM, TG and sedimentation test were used to characterize the silica-coated magnetite particles. The dispersibility of silica-coated magnetite particles in aqueous solution was improved significantly and the agglomerate particle size was decreased to 110 nm. It was found that the agglomerate particle size of silica-coated magnetite particles was mainly decided by the coating temperature and the pH value in the silica-coating process. The weight ratio of silica in silica-coated magnetite particles was mainly decided by the pH value in the silica-coating process. The dispersibility of silica-coated magnetite particles was mainly decided by the agglomerate particle size of the suspension. The oxidation of magnetite particles in air was limited through the coated silica. The magnetism of silica-coated magnetite particles decreased slightly after silica-coating.

  2. 21 CFR 584.700 - Hydrophobic silicas.

    Science.gov (United States)

    2010-04-01

    ...) Product. Amorphous fumed hydrophobic silica or precipitated hydrophobic silica (CAS Reg. No. 68611-0944... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Hydrophobic silicas. 584.700 Section 584.700 Food... DRUGS, FEEDS, AND RELATED PRODUCTS FOOD SUBSTANCES AFFIRMED AS GENERALLY RECOGNIZED AS SAFE IN FEED AND...

  3. Silica supported palladium nanoparticles for the decarboxylation of high-acid feedstocks: Design, deactivation and regeneration

    Science.gov (United States)

    Ping, Eric Wayne

    2011-12-01

    The major goals of this thesis were to (1) design and synthesize a supported catalyst with well-defined monodisperse palladium nanoparticles evenly distributed throughout an inorganic oxide substrate with tunable porosity characteristics, (2) demonstrate the catalytic activity of this material in the decarboxylation of long chain fatty acids and their derivatives to make diesel-length hydrocarbons, (3) elucidate the deactivation mechanism of supported palladium catalysts under decarboxylation conditions via post mortem catalyst characterization and develop a regeneration methodology thereupon, and (4) apply this catalytic system to a real low-value biofeedstock. Initial catalyst designs were based on the SBA-15 silica support, but in an effort to maximize loading and minimize mass transfer limitations, silica MCF was synthesized as catalyst support. Functionalization with various silane ligands yielded a surface that facilitated even distribution of palladium precursor salts throughout the catalyst particle, and, after reduction, monodisperse palladium nanoparticles approximately 2 nm in diameter. Complete characterization was performed on this Pd-MCF catalyst. The Pd-MCF catalyst showed high one-time activity in the decarboxylation of fatty acids to hydrocarbons in dodecane at 300°C. Hydrogen was found to be an unnecessary reactant in the absence of unsaturations, but was required in their presence---full hydrogenation of the double bonds occurs before any decarboxylation can take place. The Pd-MCF also exhibited good activity for alkyl esters and glycerol, providing a nice hypothetical description of a stepwise reaction pathway for catalytic decarboxylation of acids and their derivatives. As expected, the Pd-MCF catalyst experienced severe deactivation after only one use. Substantial effort was put into elucidating the nature of this deactivation via post mortem catalyst characterization. H2 chemisorption confirmed a loss of active surface area, but TEM and

  4. Fabricated Elastin.

    Science.gov (United States)

    Yeo, Giselle C; Aghaei-Ghareh-Bolagh, Behnaz; Brackenreg, Edwin P; Hiob, Matti A; Lee, Pearl; Weiss, Anthony S

    2015-11-18

    The mechanical stability, elasticity, inherent bioactivity, and self-assembly properties of elastin make it a highly attractive candidate for the fabrication of versatile biomaterials. The ability to engineer specific peptide sequences derived from elastin allows the precise control of these physicochemical and organizational characteristics, and further broadens the diversity of elastin-based applications. Elastin and elastin-like peptides can also be modified or blended with other natural or synthetic moieties, including peptides, proteins, polysaccharides, and polymers, to augment existing capabilities or confer additional architectural and biofunctional features to compositionally pure materials. Elastin and elastin-based composites have been subjected to diverse fabrication processes, including heating, electrospinning, wet spinning, solvent casting, freeze-drying, and cross-linking, for the manufacture of particles, fibers, gels, tubes, sheets and films. The resulting materials can be tailored to possess specific strength, elasticity, morphology, topography, porosity, wettability, surface charge, and bioactivity. This extraordinary tunability of elastin-based constructs enables their use in a range of biomedical and tissue engineering applications such as targeted drug delivery, cell encapsulation, vascular repair, nerve regeneration, wound healing, and dermal, cartilage, bone, and dental replacement. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Catalytic partial oxidation of methane over porous silica supported VO{sub x} catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Pirovano, C.; Schoenborn, E.; Kalevaru, V.N.; Wohlrab, S.; Luecke, B.; Martin, A. [University Rostock e.V., Rostock (Germany). Leibniz Inst. for Catalysis

    2011-07-01

    High surface area mesoporous siliceous MCM-41 and SBA-15 materials have been used as supports to disperse vanadium oxide species using wet impregnation and incipient wetness impregnation methods. These materials were used as catalysts for the partial oxidation of methane (POM) to formaldehyde. The physico-chemical properties of the solids were studied by means of BET, DR-UV/Vis spectroscopy, Py-FTIR and TEM. The influence of support and the preparation method on the dispersion of VOx is also investigated. The catalytic properties of the catalysts were examined in a fixed bed stainless steel reactor at 923 K. So far a maximum production of formaldehyde can be detected on SBA-15 supported VOx-catalysts prepared by incipient wetness impregnation. On this V/SBA-15 material a covalent attachment of catalytic active molecular vanadium species dominates, which in turn leads to a lower activation temperature and thereby reduced over-oxidation. From the best case, the space time yield of HCHO could be reached close to 775 g{sub HCHO} Kg{sub cat}{sup -1} h{sup -1}. (orig.)

  6. Poling of Planar Silica Waveguides

    DEFF Research Database (Denmark)

    Arentoft, Jesper; Kristensen, Martin; Jensen, Jesper Bo

    1999-01-01

    UV-written planar silica waveguides are poled using two different poling techniques, thermal poling and UV-poling. Thermal poling induces an electro-optic coefficient of 0.067 pm/V. We also demonstrate simultaneous UV-writing and UV-poling. The induced electro-optic effect shows a linear dependence...

  7. Functionalized silica materials for electrocatalysis

    Indian Academy of Sciences (India)

    To increase the efficiency of the electrocatalytic process and to increase the electrochemical accessibility of the immobilized electrocatalysts, functionalized and non-functionalized mesoporous organo-silica (MCM41-type-materials) are used in this study. These materials possess several suitable properties to be durable ...

  8. Incorporation of polyoxotungstate complexes in silica spheres and in situ formation of tungsten trioxide nanoparticles.

    Science.gov (United States)

    Zhao, Yuanyuan; Fan, Haimei; Li, Wen; Bi, Lihua; Wang, Dejun; Wu, Lixin

    2010-09-21

    In this paper, we demonstrated a new convenient route for in situ fabrication of well separated small sized WO(3) nanoparticles in silica spheres, through a predeposition of surfactant encapsulated polyoxotungates as tungsten source, and followed by a calcination process. In a typical procedure, selected polyoxotungates with different charges were enwrapped with dioctadecyldimethylammonium cations through electrostatic interaction. Elemental analysis, thermogravimetric analysis, and spectral characterization confirmed the formation of prepared complexes with the anticipated chemical structure. The complexes were then phase-transferred into aqueous solution that predissolved surfactant cetyltrimethylammonium bromide, and finally incorporated into silica spheres through a joint sol-gel reaction with tetraethyl orthosilicate in a well dispersed state under the protection of organic layer for polyoxotungates from the alkaline reaction condition. Transmission electron microscopic images illustrated the well dispersed WO(3) nanoparticles in the size range of ca. 2.2 nm in the silica spheres after the calcination at 465 °C. The sizes of both the silica spheres and WO(3) nanoparticles could be adjusted independently through changing the doping content to a large extent. Meanwhile, the doped polyoxotungate complexes acted as the template for the mesoporous structure in silica spheres after the calcination. Along with the increase of doping content and surfactant, the mesopore size changed little (2.0-2.9 nm), but the specific surface areas increased quite a lot. Importantly, the WO(3)-nanoparticle-doped silica spheres displayed an interesting photovoltaic property, which is favorable for the funtionalization of these nanomaterials.

  9. Radiation hardening in sol-gel derived Er3+-doped silica glasses

    International Nuclear Information System (INIS)

    Hari Babu, B.; León Pichel, Mónica; Ollier, Nadège; El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed; Poumellec, Bertrand; Lancry, Matthieu; Ibarra, Angel

    2015-01-01

    The aim of the present paper is to report the effect of radiation on the Er 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 3+ -doped sol-gel silica is found to increase with erbium content. Electron paramagnetic resonance studies reveal the presence of E′ 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 3+ to Er 2+ ions. This process occurs in association with the formation of aluminum oxygen hole centers and different intrinsic point defects

  10. On the PEEK composites reinforced by surface-modified nano-silica

    International Nuclear Information System (INIS)

    Lai, Y.H.; Kuo, M.C.; Huang, J.C.; Chen, M.

    2007-01-01

    The nano-sized silica fillers reinforced poly(ether ether ketone) (PEEK) composites were fabricated by means of compression molding technique. The nano-sized silica, measuring 30 nm in size, was firstly modified by surface pretreatment with stearic acid. The performances and properties of the resulting PEEK/SiO 2 nanocomposites were examined in terms of tensile loading, hardness, dynamic mechanical analysis (DMA), thermomechanical analysis (TMA), thermogravimetry analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The modified nano-silica was seen to disperse more uniformly than the unmodified counterpart. The XRD patterns of the modified silica reinforced PEEK composites reveal a systematic shift toward higher angles, suggesting the smaller d-spacing of the PEEK crystallites. The coefficient of thermal expansion (CTE) becomes lowered when the content of the nano-silica increases. Furthermore, the CTE of the modified silica filled PEEK nanocomposites shows the higher CTE values. A logic model is proposed. The increment of the dynamic modulus for the PEEK nanocomposites is up to 40% at elevated temperatures from 100 to 250 deg. C, indicating the apparent improvement of elevated temperature mechanical properties

  11. Silica-Coated Liposomes for Insulin Delivery

    Directory of Open Access Journals (Sweden)

    Neelam Dwivedi

    2010-01-01

    Full Text Available Liposomes coated with silica were explored as protein delivery vehicles for their enhanced stability and improved encapsulation efficiency. Insulin was encapsulated within the fluidic phosphatidylcholine lipid vesicles by thin film hydration at pH 2.5, and layer of silica was formed above lipid bilayer by acid catalysis. The presence of silica coating and encapsulated insulin was identified using confocal and electron microscopy. The native state of insulin present in the formulation was evident from Confocal Micro-Raman spectroscopy. Silica coat enhances the stability of insulin-loaded delivery vehicles. In vivo study shows that these silica coated formulations were biologically active in reducing glucose levels.

  12. Phosphate-core silica-clad Er/Yb-doped optical fiber and cladding pumped laser.

    Science.gov (United States)

    Egorova, O N; Semjonov, S L; Velmiskin, V V; Yatsenko, Yu P; Sverchkov, S E; Galagan, B I; Denker, B I; Dianov, E M

    2014-04-07

    We present a composite optical fiber with a Er/Yb co-doped phosphate-glass core in a silica glass cladding as well as cladding pumped laser. The fabrication process, optical properties, and lasing parameters are described. The slope efficiency under 980 nm cladding pumping reached 39% with respect to the absorbed pump power and 28% with respect to the coupled pump power. Due to high doping level of the phosphate core optimal length was several times shorter than that of silica core fibers.

  13. Amine-functionalized magnetic mesoporous silica nanoparticles for DNA separation

    Energy Technology Data Exchange (ETDEWEB)

    Sheng, Wei; Wei, Wei; Li, Junjian; Qi, Xiaoliang; Zuo, Gancheng; Chen, Qi; Pan, Xihao; Dong, Wei, E-mail: weidong@njust.edu.cn

    2016-11-30

    Highlights: • Fe{sub 3}O{sub 4}@SiO{sub 2}@EDPS with uniform size and good dispersity is prepared. • We fabricated MMSN@EDPS with distinct core-shell–shell triple-layer composition. • DNA adsorption capacity of MMSN@EDPS is considerable. - Abstract: We report a modified approach for the functionalized magnetic mesoporous silica nanoparticles (MMSN) using polymer microspheres incorporated with magnetic nanoparticles in the presence of cetyltrimethylammonium bromide (CTAB) and the core-shell magnetic silica nanoparticles (MSN). These particles were functionalized with amino groups via the addition of aminosilane directly to the particle sol. We then evaluate their DNA separation abilities and find the capacity of DNA binding significantly increased (210.22 μg/mg) compared with normal magnetic silica spheres (138.44 μg/mg) by using an ultraviolet and visible spectrophotometer (UV). The morphologies, magnetic properties, particle size, pore size, core-shell structure and Zeta potential are characterized by Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM), Transmission electron microscopy (TEM), Powder X-ray diffraction (XRD), and dynamic light scattering (DLS). This work demonstrates that our MMSN own an excellent potential application in bioseparation and drug delivery.

  14. High strength fused silica flexures manufactured by femtosecond laser

    Science.gov (United States)

    Bellouard, Yves; Said, Ali A.; Dugan, Mark; Bado, Philippe

    2009-02-01

    Flexures are mechanical elements used in micro- and precision-engineering to precisely guide the motion of micro-parts. They consist of slender bodies that deform elastically upon the application of a force. Although counter-intuitive at first, fused silica is an attractive material for flexure. Pending that the machining process does not introduce surface flaws that would lead to catastrophic failure, the material has a theoretically high ultimate tensile strength of several GPa. We report on high-aspect ratio fused silica flexures manufactured by femtosecond laser combined with chemical etching. Notch-hinges with thickness as small as twenty microns and aspect ratios comparable to aspect ratios obtained by Deep- Reactive-Ion-Etching (DRIE) were fabricated and tested under different loading conditions. Multiple fracture tests were performed for various loading conditions and the cracks morphologies were analyzed using Scanning Electron Microscopy. The manufactured elements show outstanding mechanical properties with flexural strengths largely exceeding those obtained with other technologies and materials. Fused silica flexures offer a mean to combine integrated optics with micro-mechanics in a single monolithic substrate. Waveguides and mechanical elements can be combined in a monolithic devices opening new opportunities for integrated opto-mechatronics devices.

  15. Designer silica layers for advanced applications: Processing and properties

    Science.gov (United States)

    Anderson, Adam

    Recently, as scientists have investigated the application of conventional MEMS devices to biological systems, the exciting fields of bio-MEMS and microfluidics have emerged. Due to their small size, bio-MEMS and microfluidics devices offer the advantage of requiring only small sample and reagent volumes, in a potentially low-cost, integrated package. Such devices have the potential to significantly advance point-of-care diagnostics devices and improve overall patient care. However, due to the extremely small feature size, the large surface area-to-volume ratio in these devices makes controlling surface interactions of critical importance. Recently, there has been a shift to polymeric materials for fabrication of microfluidics devices due to their lower cost, ease of device fabrication by various processes, varied and favorable material properties, and, in some cases, pre-existing regulatory agency approvals. As a result, various surface modification strategies for polymeric surfaces have been proposed, but with only limited success. The proven success of organosilicon-based precursors in a wide variety of surface modification strategies has been demonstrated, with a body of knowledge on the general subject dating back nearly fifty years. However, these proven methodologies cannot be transferred to many important polymeric materials due to a lack of sufficient reactive groups on the surface. If any polymer surface could be made reactive by some intermediate treatment, the wide body of knowledge of organosilicon-based surface modification chemistries could be leveraged to advance the state-of-the-art in surface modification for microfluidics applications, where polymeric substrates are commonly encountered. This thesis reports on the processing properties and chemical properties of a vapor deposited silica layer, which is formed from the vapor phase hydrolysis of silicon tetrachloride. This layer can be deposited at low temperatures to a wide variety of substrates

  16. Process for manufacturing hollow fused-silica insulator cylinder

    Science.gov (United States)

    Sampayan, Stephen E.; Krogh, Michael L.; Davis, Steven C.; Decker, Derek E.; Rosenblum, Ben Z.; Sanders, David M.; Elizondo-Decanini, Juan M.

    2001-01-01

    A method for building hollow insulator cylinders that can have each end closed off with a high voltage electrode to contain a vacuum. A series of fused-silica round flat plates are fabricated with a large central hole and equal inside and outside diameters. The thickness of each is related to the electron orbit diameter of electrons that escape the material surface, loop, and return back. Electrons in such electron orbits can support avalanche mechanisms that result in surface flashover. For example, the thickness of each of the fused-silica round flat plates is about 0.5 millimeter. In general, the thinner the better. Metal, such as gold, is deposited onto each top and bottom surface of the fused-silica round flat plates using chemical vapor deposition (CVD). Eutectic metals can also be used with one alloy constituent on the top and the other on the bottom. The CVD, or a separate diffusion step, can be used to defuse the deposited metal deep into each fused-silica round flat plate. The conductive layer may also be applied by ion implantation or gas diffusion into the surface. The resulting structure may then be fused together into an insulator stack. The coated plates are aligned and then stacked, head-to-toe. Such stack is heated and pressed together enough to cause the metal interfaces to fuse, e.g., by welding, brazing or eutectic bonding. Such fusing is preferably complete enough to maintain a vacuum within the inner core of the assembled structure. A hollow cylinder structure results that can be used as a core liner in a dielectric wall accelerator and as a vacuum envelope for a vacuum tube device where the voltage gradients exceed 150 kV/cm.

  17. Deep reactive ion etching of fused silica using a single-coated soft mask layer for bio-analytical applications

    International Nuclear Information System (INIS)

    Ray, Tathagata; Zhu, Haixin; Meldrum, Deirdre R

    2010-01-01

    In this note, we present our results from process development and characterization of reactive ion etching (RIE) of fused silica using a single-coated soft masking layer (KMPR® 1025, Microchem Corporation, Newton, MA). The effects of a number of fluorine-radical-based gaseous chemistries, the gas flow rate, RF power and chamber pressure on the etch rate and etching selectivity of fused silica were studied using factorial experimental designs. RF power and pressure were found to be the most important factors in determining the etch rate. The highest fused silica etch rate obtained was about 933 Å min −1 by using SF 6 -based gas chemistry, and the highest etching selectivity between the fused silica and KMPR® 1025 was up to 1.2 using a combination of CF 4 , CHF 3 and Ar. Up to 30 µm deep microstructures have been successfully fabricated using the developed processes. The average area roughness (R a ) of the etched surface was measured and results showed it is comparable to the roughness obtained using a wet etching technique. Additionally, near-vertical sidewalls (with a taper angle up to 85°) have been obtained for the etched microstructures. The processes developed here can be applied to any application requiring fabrication of deep microstructures in fused silica with near-vertical sidewalls. To our knowledge, this is the first note on deep RIE of fused silica using a single-coated KMPR® 1025 masking layer and a non-ICP-based reactive ion etcher. (technical note)

  18. Silica aerogel and space astrophysics

    International Nuclear Information System (INIS)

    Koch-Miramond, L.

    1985-09-01

    Silica aerogels have been produced in large and transparent bloc