Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

Energy Technology Data Exchange (ETDEWEB)

Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve [Unite mixte CNRS/Saint Gobain Saint Gobain Recherche, BP135, 93303 Aubervilliers (France); Berthier, Serge [Institut des Nanosciences de Paris, UMR 7588, CNRS, Universite Pierre et Marie Curie-Paris 6, 140 rue Lourmel, 75015 Paris (France)], E-mail: cperoz@lbl.gov

2008-12-01

An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C.

Structural evolution of nanoporous silica thin films studied by positron annihilation spectroscopy and Fourier transform infrared spectroscopy

International Nuclear Information System (INIS)

Patel, N; Mariazzi, S; Toniutti, L; Checchetto, R; Miotello, A; Dire, S; Brusa, R S

2007-01-01

Three series of silica thin films with thicknesses in the 300 nm range were deposited by spin coating on Si substrates using different compositions of the sol precursors. Film samples were thermally treated in static air at temperatures ranging from 300 to 900 deg. C. The effect of sol precursors and thermal treatment temperature on the film porosity was analysed by Fourier transform infrared (FTIR) spectroscopy, depth profiling with positron annihilation spectroscopy (DP-PAS) and the analysis of the capacitance-voltage (C-V) characteristic. The maximum of the total porosity was found to occur at a temperature of 600 deg. C when removal of porogen and OH groups was completed. Film densification due to the collapsing of the pores was observed after drying at 900 deg. C. DP-PAS provides evidence that the increase in the total porosity is related to a progressive increase in the pore size. The increase in the pore size never gives rise to the onset of connected porosity. In the silica film samples prepared using a low acidity sol precursor, the pore size is always lower than 1 nm. By increasing the acid catalyst ratio in the sol, larger pores are formed. Pores with size larger than 2.3 nm can be obtained by adding porogen to the sol. In each series of silica film samples the shift of the antisymmetric Si-O-Si transversal optical (TO 3 ) mode upon thermal treatment correlates with a change of the pore size as evidenced by DP-PAS analysis. The pore microstructure of the three series of silica films is different at all the examined treatment temperatures and depends on the composition of the precursor sol

Structural evolution of nanoporous silica thin films studied by positron annihilation spectroscopy and Fourier transform infrared spectroscopy

Science.gov (United States)

Patel, N.; Mariazzi, S.; Toniutti, L.; Checchetto, R.; Miotello, A.; Dirè, S.; Brusa, R. S.

2007-09-01

Three series of silica thin films with thicknesses in the 300 nm range were deposited by spin coating on Si substrates using different compositions of the sol precursors. Film samples were thermally treated in static air at temperatures ranging from 300 to 900 °C. The effect of sol precursors and thermal treatment temperature on the film porosity was analysed by Fourier transform infrared (FTIR) spectroscopy, depth profiling with positron annihilation spectroscopy (DP-PAS) and the analysis of the capacitance-voltage (C-V) characteristic. The maximum of the total porosity was found to occur at a temperature of 600 °C when removal of porogen and OH groups was completed. Film densification due to the collapsing of the pores was observed after drying at 900 °C. DP-PAS provides evidence that the increase in the total porosity is related to a progressive increase in the pore size. The increase in the pore size never gives rise to the onset of connected porosity. In the silica film samples prepared using a low acidity sol precursor, the pore size is always lower than 1 nm. By increasing the acid catalyst ratio in the sol, larger pores are formed. Pores with size larger than 2.3 nm can be obtained by adding porogen to the sol. In each series of silica film samples the shift of the antisymmetric Si-O-Si transversal optical (TO3) mode upon thermal treatment correlates with a change of the pore size as evidenced by DP-PAS analysis. The pore microstructure of the three series of silica films is different at all the examined treatment temperatures and depends on the composition of the precursor sol.

Silica doped with lanthanum sol-gel thin films for corrosion protection

Energy Technology Data Exchange (ETDEWEB)

Abuin, M. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Serrano, A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); Llopis, J. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Garcia, M.A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); IMDEA Nanoscience, Fco. Tomas y Valiente 7, 28049 Madrid (Spain); Carmona, N., E-mail: n.carmona@fis.ucm.es [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain)

2012-06-01

We present here anticorrosive silica coatings doped with lanthanum ions for the protection of metallic surfaces as an alternative to chromate (VI)-based conversion coatings. The coatings were synthesized by the sol-gel method starting from silicon alkoxides and two different lanthanum precursors: La (III) acetate hydrate and La (III) isopropoxide. Artificial corrosion tests in acid and alkaline media showed their effectiveness for the corrosion protection of AA2024 aluminum alloy sheets for coating prepared with both precursors. The X-ray absorption Near Edge Structure and X-ray Absorption Fine Structure analysis of the coatings confirmed the key role of lanthanum in the structural properties of the coating determining its anticorrosive properties. - Highlights: Black-Right-Pointing-Pointer Silica sol-gel films doped with lanthanum ions were synthesized. Black-Right-Pointing-Pointer Films from lanthanum-acetate and La-alkoxide were prepared for comparison purposes. Black-Right-Pointing-Pointer La-acetate is an affordable chemical reactive preferred for the industry. Black-Right-Pointing-Pointer Films properties were explored by scanning electron microscopy and X-Ray absorption spectroscopy. Black-Right-Pointing-Pointer An alternative to anticorrosive pre-treatments for metallic surfaces is suggested.

Hydrophobic and optical characteristics of graphene and graphene oxide films transferred onto functionalized silica particles deposited glass surface

Science.gov (United States)

Yilbas, B. S.; Ibrahim, A.; Ali, H.; Khaled, M.; Laoui, T.

2018-06-01

Hydrophobic and optical transmittance characteristics of the functionalized silica particles on the glass surface prior and after transfer of graphene and graphene oxide films on the surface are examined. Nano-size silica particles are synthesized and functionalized via chemical grafting and deposited onto a glass surface. Graphene film, grown on copper substrate, was transferred onto the functionalized silica particles surface through direct fishing method. Graphene oxide layer was deposited onto the functionalized silica particles surface via spin coating technique. Morphological, hydrophobic, and optical characteristics of the functionalized silica particles deposited surface prior and after graphene and graphene oxide films transfer are examined using the analytical tools. It is found that the functionalized silica particles are agglomerated at the surface forming packed structures with few micro/nano size pores. This arrangement gives rise to water droplet contact angle and contact angle hysteresis in the order of 163° and 2°, respectively, and remains almost uniform over the entire surface. Transferring graphene and depositing graphene oxide films over the functionalized silica particles surface lowers the water droplet contact angle slightly (157-160°) and increases the contact angle hysteresis (4°). The addition of the graphene and graphene oxide films onto the surface of the deposited functionalized silica particles improves the optical transmittance.

Colloidal silica films for high-capacity DNA arrays

Science.gov (United States)

Glazer, Marc Irving

The human genome project has greatly expanded the amount of genetic information available to researchers, but before this vast new source of data can be fully utilized, techniques for rapid, large-scale analysis of DNA and RNA must continue to develop. DNA arrays have emerged as a powerful new technology for analyzing genomic samples in a highly parallel format. The detection sensitivity of these arrays is dependent on the quantity and density of immobilized probe molecules. We have investigated substrates with a porous, "three-dimensional" surface layer as a means of increasing the surface area available for the synthesis of oligonucleotide probes, thereby increasing the number of available probes and the amount of detectable bound target. Porous colloidal silica films were created by two techniques. In the first approach, films were deposited by spin-coating silica colloid suspensions onto flat glass substrates, with the pores being formed by the natural voids between the solid particles (typically 23nm pores, 35% porosity). In the second approach, latex particles were co-deposited with the silica and then pyrolyzed, creating films with larger pores (36 nm), higher porosity (65%), and higher surface area. For 0.3 mum films, enhancements of eight to ten-fold and 12- to 14-fold were achieved with the pure silica films and the films "templated" with polymer latex, respectively. In gene expression assays for up to 7,000 genes using complex biological samples, the high-capacity films provided enhanced signals and performed equivalently or better than planar glass on all other functional measures, confirming that colloidal silica films are a promising platform for high-capacity DNA arrays. We have also investigated the kinetics of hybridization on planar glass and high-capacity substrates. Adsorption on planar arrays is similar to ideal Langmuir-type adsorption, although with an "overshoot" at high solution concentration. Hybridization on high-capacity films is

Preparing hydrophobic nanocellulose-silica film by a facile one-pot method.

Science.gov (United States)

Le, Duy; Kongparakul, Suwadee; Samart, Chanatip; Phanthong, Patchiya; Karnjanakom, Surachai; Abudula, Abuliti; Guan, Guoqing

2016-11-20

Hydrophobic nanocellulose-silica film was successfully prepared by a facile one-pot method using tetraethoxysilane (TEOS) and dodecyl triethoxylsilane (DTES). Morphological characterization of the hydrophobic nanocellulose-silica (NC-SiO2-DTES) film showed well self-assembled DTES modified silica spherical nanoparticles with the particle sizes in the range of 88-126nm over the nanocellulose film. The hydrophobicity of the NC-SiO2-DTES film was achieved owing to the improvement of roughness of the nanocellulose film by coating dodecyl- terminated silica nanoparticles. An increase in DTES loading amount and reaction time increased the hydrophobicity of the film, and the optimum condition for NC-SiO2-DTES film preparation was achieved at DTES/TEOS molar ratio of 2.0 for 8h reaction time. Besides, the NC-SiO2-DTES film performed superoleophilic property with octane and hexadecane contact angles of 0°. It also showed an excellent hydrophobic property over all pH values ranged from 1 to 14. Copyright © 2016 Elsevier Ltd. All rights reserved.

Thickness controlled sol-gel silica films for plasmonic bio-sensing devices

Energy Technology Data Exchange (ETDEWEB)

Figus, Cristiana, E-mail: cristiana.figus@dsf.unica.it; Quochi, Francesco, E-mail: cristiana.figus@dsf.unica.it; Artizzu, Flavia, E-mail: cristiana.figus@dsf.unica.it; Saba, Michele, E-mail: cristiana.figus@dsf.unica.it; Marongiu, Daniela, E-mail: cristiana.figus@dsf.unica.it; Mura, Andrea; Bongiovanni, Giovanni [Dipartimento di Fisica - University of Cagliari, S.P. Km 0.7, I-09042 Monserrato (Canada) (Italy); Floris, Francesco; Marabelli, Franco; Patrini, Maddalena; Fornasari, Lucia [Dipartimento di Fisica - University of Pavia, Via Agostino Bassi 6, I-27100 Pavia (PV) (Italy); Pellacani, Paola; Valsesia, Andrea [Plasmore S.r.l. -Via Grazia Deledda 4, I-21020 Ranco (Vatican City State, Holy See) (Italy)

2014-10-21

Plasmonics has recently received considerable interest due to its potentiality in many fields as well as in nanobio-technology applications. In this regard, various strategies are required for modifying the surfaces of plasmonic nanostructures and to control their optical properties in view of interesting application such as bio-sensing, We report a simple method for depositing silica layers of controlled thickness on planar plasmonic structures. Tetraethoxysilane (TEOS) was used as silica precursor. The control of the silica layer thickness was obtained by optimizing the sol-gel method and dip-coating technique, in particular by properly tuning different parameters such as pH, solvent concentration, and withdrawal speed. The resulting films were characterized via atomic force microscopy (AFM), Fourier-transform (FT) spectroscopy, and spectroscopic ellipsometry (SE). Furthermore, by performing the analysis of surface plasmon resonances before and after the coating of the nanostructures, it was observed that the position of the resonance structures could be properly shifted by finely controlling the silica layer thickness. The effect of silica coating was assessed also in view of sensing applications, due to important advantages, such as surface protection of the plasmonic structure.

Evaluation of optical properties of the amorphous carbon film on fused silica

International Nuclear Information System (INIS)

Baydogan, Nilguen Dogan

2004-01-01

Deposition was done using a pulsed filtered cathodic arc with a graphite cathode. The carbon plasma is fully ionised and condenses on the substrate, forming diamond-like material but with amorphous structure. Optical properties of amorphous carbon films on fused-silica glass were investigated and the curves of optical density have a characteristic band at approximately 950 nm. Changes of the colourimetric quantities were evaluated and compared to uncoated fused silica glass. These changes were investigated as a function of the applied substrate bias voltage using the CIE and CIELAB colour systems. It is suggested that the mechanism of absorption is related to an allowed direct transition at the amorphous carbon films on fused silica glass. The optical energy gap of the amorphous carbon film depends on the bias voltage applied to the substrate holder. The optical colour parameters and optical band gap indicated that there is a relation between the dominant wavelength of the reflectance in the visible range and the wavelength of the optical band gap

Physical Characteristics of Chitosan Based Film Modified With Silica and Polyethylene Glycol

Directory of Open Access Journals (Sweden)

F. Widhi Mahatmanti

2014-07-01

Full Text Available Recently, development of film materials is focused on finding the films with high chemical and physical stabilities. Organic based material such as chitosan produces films with low physical stability, and hence addition of inorganic materials necessary. In this research, the effect of silica and polyethylene glycol (PEG addition on the properties of chitosan based films has been investigated. Precursors used to produce films included chitosan with the deacetylation degree of 83% and sodium silicate solution as the silica source. A simple synthesis in a one-pot process was carried out by mixing 1%(w of chitosan solution in 2%(v/v acetate acid and sodium silicate solution (27% SiO2 in various composition ratios and casting the solution on a glass dish. The tensile strength and percentage of elongation decrease with increasing the silica content. The tensile strength tends to decline with addition of PEG, but the elongation percentage of the film increases. Hydrophilicity of the film decreases with the addition of silica and increases with the addition of PEG. The addition of silica and PEG does not change significantly the morphology of the film and functional groups indicating the domination of physical interaction among active sites in the film components.

Hydrophobicity of silica thin films: The deconvolution and interpretation by Fourier-transform infrared spectroscopy

Science.gov (United States)

Saputra, Riza Eka; Astuti, Yayuk; Darmawan, Adi

2018-06-01

This work investigated the synthesis of dimethoxydimethylsilane:tetraethoxysilane (DMDMS:TEOS) silica thin films as well as the effect of DMDMS:TEOS molar ratios and calcination temperature on hydrophobic properties of silica thin films and its correlation with the FTIR spectra behaviour. The silica thin films were synthesized by sol-gel method using combination of DMDMS and TEOS as silica precursors, ethanol as solvent and ammonia as catalyst, with DMDMS and TEOS molar ratio of 10:90, 25:75, 50:50, 75:25 and 90:10. The results showed that DMDMS:TEOS molar ratio had significant impact on the hydrophobic properties of silica thin films coated on a glass surface. Furthermore, the correlation between water contact angle (WCA) and DMDMS:TEOS molar ratio was found to be in a parabolic shape. Concurrently, the maximum apex of the parabola obtained was observed on the DMDMS:TEOS molar ratio of 50:50 for all calcination temperature. It was clearly observed that the silica xerogel exhibiting notable change in relative peak intensities showed FTIR peak splitting of υasymmetric Si-O-Si. To uncover what happened at the FTIR peak, the deconvolution was conducted in Gaussian approach. It was established that the changes in the Gaussian peak component were related to DMDMS:TEOS molar ratios and the calcination temperature that allowed us to tailor the DMDMS:TEOS silica polymer structure model based on the peak intensity ratios. With the increase of DMDMS:TEOS molar ratio, the ratio of (cyclic Si-O-Si)/(linear Si-O-Si) decreased, whilst the ratio of (C-H)/(linear Si-O-Si) increased. Both ratios intersected at DMDMS:TEOS molar ratio of 50:50 with contribution factor ratio of 1:16 and 1:50 for silica xerogel calcined at 300 °C and 500 °C respectively. The importance of this research is the DMDMS:TEOS molar ratio plays an important role in determining the hydrophobic properties of thin films.

Hydrophobicity of silica thin films: The deconvolution and interpretation by Fourier-transform infrared spectroscopy.

Science.gov (United States)

Saputra, Riza Eka; Astuti, Yayuk; Darmawan, Adi

2018-03-14

This work investigated the synthesis of dimethoxydimethylsilane:tetraethoxysilane (DMDMS:TEOS) silica thin films as well as the effect of DMDMS:TEOS molar ratios and calcination temperature on hydrophobic properties of silica thin films and its correlation with the FTIR spectra behaviour. The silica thin films were synthesized by sol-gel method using combination of DMDMS and TEOS as silica precursors, ethanol as solvent and ammonia as catalyst, with DMDMS and TEOS molar ratio of 10:90, 25:75, 50:50, 75:25 and 90:10. The results showed that DMDMS:TEOS molar ratio had significant impact on the hydrophobic properties of silica thin films coated on a glass surface. Furthermore, the correlation between water contact angle (WCA) and DMDMS:TEOS molar ratio was found to be in a parabolic shape. Concurrently, the maximum apex of the parabola obtained was observed on the DMDMS:TEOS molar ratio of 50:50 for all calcination temperature. It was clearly observed that the silica xerogel exhibiting notable change in relative peak intensities showed FTIR peak splitting of υ asymmetric Si-O-Si. To uncover what happened at the FTIR peak, the deconvolution was conducted in Gaussian approach. It was established that the changes in the Gaussian peak component were related to DMDMS:TEOS molar ratios and the calcination temperature that allowed us to tailor the DMDMS:TEOS silica polymer structure model based on the peak intensity ratios. With the increase of DMDMS:TEOS molar ratio, the ratio of (cyclic Si-O-Si)/(linear Si-O-Si) decreased, whilst the ratio of (C-H)/(linear Si-O-Si) increased. Both ratios intersected at DMDMS:TEOS molar ratio of 50:50 with contribution factor ratio of 1:16 and 1:50 for silica xerogel calcined at 300°C and 500°C respectively. The importance of this research is the DMDMS:TEOS molar ratio plays an important role in determining the hydrophobic properties of thin films. Copyright © 2018 Elsevier B.V. All rights reserved.

A simple three step method for selective placement of organic groups in mesoporous silica thin films

Energy Technology Data Exchange (ETDEWEB)

Franceschini, Esteban A. [Gerencia Química, Centro Atómico Constituyentes, Comisión Nacional de Energía Atómica, Av. Gral Paz 1499 (B1650KNA) San Martín, Buenos Aires (Argentina); Llave, Ezequiel de la; Williams, Federico J. [Departamento de Química Inorgánica, Analítica y Química Física and INQUIMAE-CONICET, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria, Pabellón II, C1428EHA Buenos Aires (Argentina); Soler-Illia, Galo J.A.A., E-mail: galo.soler.illia@gmail.com [Departamento de Química Inorgánica, Analítica y Química Física and INQUIMAE-CONICET, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria, Pabellón II, C1428EHA Buenos Aires (Argentina); Instituto de Nanosistemas, Universidad Nacional de General San Martín, 25 de Mayo y Francia (1650) San Martín, Buenos Aires (Argentina)

2016-02-01

Selective functionalization of mesoporous silica thin films was achieved using a three step method. The first step consists in an outer surface functionalization, followed by washing off the structuring agent (second step), leaving the inner surface of the pores free to be functionalized in the third step. This reproducible method permits to anchor a volatile silane group in the outer film surface, and a second type of silane group in the inner surface of the pores. As a concept test we modified the outer surface of a mesoporous silica film with trimethylsilane (–Si–(CH{sub 3}){sub 3}) groups and the inner pore surface with propylamino (–Si–(CH{sub 2}){sub 3}–NH{sub 2}) groups. The obtained silica films were characterized by Environmental Ellipsometric Porosimetry (EEP), EDS, XPS, contact angle and electron microscopy. The selectively functionalized silica (SF) shows an amount of surface amino functions 4.3 times lower than the one-step functionalized (OSF) silica samples. The method presented here can be extended to a combination of silane chlorides and alkoxides as functional groups, opening up a new route toward the synthesis of multifunctional mesoporous thin films with precisely localized organic functions. - Highlights: • Selective functionalization of mesoporous silica thin films was achieved using a three step method. • A volatile silane group is anchored by evaporation on the outer film surface. • A second silane is deposited in the inner surface of the pores by post-grafting. • Contact angle, EDS and XPS measurements show different proportions of amino groups on both surfaces. • This method can be extended to a combination of silane chlorides and alkoxides functional groups.

Dielectric breakdown in silica-amorphous polymer nanocomposite films: the role of the polymer matrix.

Science.gov (United States)

Grabowski, Christopher A; Fillery, Scott P; Westing, Nicholas M; Chi, Changzai; Meth, Jeffrey S; Durstock, Michael F; Vaia, Richard A

2013-06-26

The ultimate energy storage performance of an electrostatic capacitor is determined by the dielectric characteristics of the material separating its conductive electrodes. Polymers are commonly employed due to their processability and high breakdown strength; however, demands for higher energy storage have encouraged investigations of ceramic-polymer composites. Maintaining dielectric strength, and thus minimizing flaw size and heterogeneities, has focused development toward nanocomposite (NC) films; but results lack consistency, potentially due to variations in polymer purity, nanoparticle surface treatments, nanoparticle size, and film morphology. To experimentally establish the dominant factors in broad structure-performance relationships, we compare the dielectric properties for four high-purity amorphous polymer films (polymethyl methacrylate, polystyrene, polyimide, and poly-4-vinylpyridine) incorporating uniformly dispersed silica colloids (up to 45% v/v). Factors known to contribute to premature breakdown-field exclusion and agglomeration-have been mitigated in this experiment to focus on what impact the polymer and polymer-nanoparticle interactions have on breakdown. Our findings indicate that adding colloidal silica to higher breakdown strength amorphous polymers (polymethyl methacrylate and polyimide) causes a reduction in dielectric strength as compared to the neat polymer. Alternatively, low breakdown strength amorphous polymers (poly-4-vinylpyridine and especially polystyrene) with comparable silica dispersion show similar or even improved breakdown strength for 7.5-15% v/v silica. At ∼15% v/v or greater silica content, all the polymer NC films exhibit breakdown at similar electric fields, implying that at these loadings failure becomes independent of polymer matrix and is dominated by silica.

Hybrid thin films derived from UV-curable acrylate-modified waterborne polyurethane and monodispersed colloidal silica

Directory of Open Access Journals (Sweden)

C. H. Yang

2012-01-01

Full Text Available Hybrid thin films containing nano-sized inorganic domains were synthesized from UV-curable acrylate-modified waterborne polyurethane (WPU-AC and monodispersed colloidal silica with coupling agent. The coupling agent, 3-(trimethoxysilylpropyl methacrylate (MSMA, was bonded onto colloidal silica first, and then mixed with WPU-AC to form a precursor solution. This precursor was spin coated, dried and UV-cured to generate the hybrid films. The silica content in the hybrid thin films was varied from 0 to 30 wt%. Experimental results showed the aggregation of silica particles in the hybrid films. Thus, the silica domain in the hybrid films was varied from 30 to 50 nm by the different ratios of MSMAsilica to WPU-AC. The prepared hybrid films from the crosslinked WPU-AC/MSMA-silica showed much better thermal stability and mechanical properties than pure WPU-AC.

Structural and optical studies of nano-structure silica gel doped with different rare earth elements, prepared by two different sol -gel techniques

International Nuclear Information System (INIS)

Battisha, I.K.; El Beyally, A.; Seliman, S.I.; El Nahrawi, A.S.

2005-01-01

Structural and optical characteristics of pure silica gel (silica-xerogel, SiO 2 ) and doped with different concentrations ranging from 1 up to 6% of some rare earth (REEs) ions such as, praseodymium Pr +3 ,and Europium Eu +3 , Erbium Er +3 and Holmium Ho +3 , ions, in the form of thin film and monolith materials were prepared by sol - gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural and optical features of sol-gel derived monolith and thin films are analyzed and compared, namely the structure of nano-particle monolith and thin film silica-gel samples, based on X-ray diffraction (XRD). The types of structural information obtainable are compared in detail. It is show that the XRD spectra of a-cristobalite are obtained for the two type materials and even by doping with the four REEs ions. Optical measurements of monolith and thin films were also studied and compared, the normal transmission and specular reflection were measured. The refractive index were calculated and discussed

Micropatterned Silica Films with Nanohydroxyapatite for Y-TZP Implants.

Science.gov (United States)

Miranda, R B P; Grenho, L; Carvalho, A; Fernandes, M H; Monteiro, F J; Cesar, P F

2018-03-01

This investigation aimed at developing micropatterned silica thin films (MSTFs) containing nanohydroxyapatite (nano-HA) microaggregates that were not completely covered by silica so that they could directly interact with the surrounding cells. The objectives were 1) to evaluate the effect of the presence of 2 films (MSTF with or without nano-HA addition) on the characteristic strength (σ 0 ) and Weibull modulus ( m) of a yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) and 2) to evaluate the effect of these 2 films, as applied onto the Y-TZP surface, on the morphology, orientation, and proliferation of MG63 cells. Sol-gel process and soft lithography were used to apply the MSTF onto the Y-TZP specimens. Three experimental groups were produced: Y-TZP, Y-TZP + MSTF, and Y-TZP + MSTF + sprayed nano-HA. All surfaces were characterized by scanning electron microscopy and energy-dispersive X-ray spectroscopy and tested for 4-point flexural strength ( n = 30) in water at 37 °C. Weibull analysis was used to determine m and σ 0 (maximum likelihood method). In vitro biological behavior was performed with human osteoblast-like cells (MG63). Y-TZP was successfully coated with MSFT and MSFT + nano-HA. Scanning electron microscopy micrographs indicated that the microaggregates of nano-HA were not entirely covered by the silica. There was no statistically significant difference among the experimental groups for σ 0 and m. In the groups containing the films, the cells were elongated and aligned along the lines. The MSFT + nano-HA group showed significantly higher cell metabolic activity than that obtained for the Y-TZP group at day 7. This investigation was successful in producing an MSTF containing nano-HA microaggregates that remained exposed to the environment. The developed films did not jeopardize the structural reliability of a commercial Y-TZP, as confirmed by the Weibull statistics. The MG63 cells seeded over the films became elongated and aligned along the

Improvement of RVNRL film properties by adding fumed silica and hydroxy apatite

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Adul Thiangchanya

2003-01-01

Full Text Available The effect of adding fumed silica and hydroxy apatite to Radiation Vulcanized Natural Rubber Latex (RVNRL for improving tear strength, aging properties, degradability and water-soluble protein content of rubber films has been investigated. The addition of fumed silica and hydroxy apatite in RVNRL improves tear strength and aging properties of rubber films, whereas tensile strength and degradability of rubber films were unchanged during storage at room temperature. The water-soluble protein content in rubber films was reduced by immobilization of the fumed silica and hydroxy apatite and enhanced by addition of ZnO. This may reduce allergy problems of natural rubber latex products caused by water-soluble protein. The MST of the RVNRL with fumed silica and hydroxy apatite indicated that the latex must be used within two months after mixing because of its stability.

Flexible, cathodoluminescent and free standing mesoporous silica films with entrapped quasi-2D perovskites

Science.gov (United States)

Vassilakopoulou, Anastasia; Papadatos, Dionysios; Koutselas, Ioannis

2017-04-01

The effective entrapment of hybrid organic-inorganic semiconductors (HOIS) into mesoporous polymer-silica hybrid matrices, formed as free standing flexible films, is presented for the first time. A blend of quasi-2D HOIS, simply synthesized by mixing two-dimensional (2D) and three dimensional (3D) HOIS, exhibiting strong photoluminescence, is embedded into porous silica matrices during the sol-gel synthesis, using tetraethylorthosilicate as precursor and Pluronic F-127 triblock copolymer as structure directing agent, under acidic conditions. The final nanostructure hybrid forms flexible, free standing films, presenting high cathodoluminescence and long stable excitonic luminescence, indicating the protective character of the hybrid matrix towards the entrapped perovskite. A significant result is that the photoluminescence of the entrapped HOIS is not affected even after films' prolonged exposure to water.

Addition of silica nanoparticles to tailor the mechanical properties of nanofibrillated cellulose thin films.

Science.gov (United States)

Eita, Mohamed; Arwin, Hans; Granberg, Hjalmar; Wågberg, Lars

2011-11-15

Over the last decade, the use of nanocellulose in advanced technological applications has been promoted both due the excellent properties of this material in combination with its renewability. In this study, multilayered thin films composed of nanofibrillated cellulose (NFC), polyvinyl amine (PVAm) and silica nanoparticles were fabricated on polydimethylsiloxane (PDMS) using a layer-by-layer adsorption technique. The multilayer build-up was followed in situ by quartz crystal microbalance with dissipation, which indicated that the PVAm-SiO(2)-PVAm-NFC system adsorbs twice as much wet mass material compared to the PVAm-NFC system for the same number of bilayers. This is accompanied with a higher viscoelasticity for the PVAm-SiO(2)-PVAm-NFC system. Ellipsometry indicated a dry-state thickness of 2.2 and 3.4 nm per bilayer for the PVAm-NFC system and the PVAm-SiO(2)-PVAm-NFC system, respectively. Atomic force microscopy height images indicate that in both systems, a porous network structure is achieved. Young's modulus of these thin films was determined by the Strain-Induced Elastic Buckling Instability for Mechanical Measurements (SIEBIMM) technique. The Young's modulus of the PVAm/NFC films was doubled, from 1 to 2 GPa, upon incorporation of silica nanoparticles in the films. The introduction of the silica nanoparticles lowered the refractive index of the films, most probably due to an increased porosity of the films. Copyright © 2011 Elsevier Inc. All rights reserved.

Characterization of transparent silica films deposited on polymeric materials

International Nuclear Information System (INIS)

Teshima, K.; Sugimura, H.; Inoue, Y.; Takai, O.

2002-01-01

Silica films were synthesized by capacitively coupled RF PECVD using mixtures of organo-silane and oxygen as a source. The chemical bonding states and compositions of the films deposited were evaluated with FTIR and XPS. Film surfaces and cross-sections were observed by SEM. Oxygen transmission rates (OTR) of the films coated on polyethylene terephthalate (PET) substrates were measured by an isopiestic method. (Authors)

Action of colloidal silica films on different nano-composites

Directory of Open Access Journals (Sweden)

S. Abdalla

Full Text Available Nano-composite films have been the subject of extensive work to develop the energy-storage efficiency of electrostatic capacitors. Factors such as polymer purity, nano-particles size, and film morphology drastically affect the electrostatic efficiency of the dielectric material that form an insulating film between conductive electrodes of a capacitor. This in turn affects the energy storage performance of the capacitor. In the present work, we have studied the dielectric properties of 4 high pure amorphous polymer films: polymethylmethacrylate (PMMA, polystyrene, polyimide and poly-4-vinylpyridine. Comparison between the dielectric properties of these polymers has revealed that the higher break down performance is a character of polyimide PI and PMMA. Also, our experimental data shows that adding colloidal silica to PMMA and PI leads to a net decrease in the dielectric properties compared to the pure polymer. Keywords: Dielectric break down, Polymers, Nano-composite, Colloidal silica

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.

High-coercivity FePt nanoparticle assemblies embedded in silica thin films

International Nuclear Information System (INIS)

Yan, Q; Purkayastha, A; Singh, A P; Li, H; Ramanath, G; Li, A; Ramanujan, R V

2009-01-01

The ability to process assemblies using thin film techniques in a scalable fashion would be a key to transmuting the assemblies into manufacturable devices. Here, we embed FePt nanoparticle assemblies into a silica thin film by sol-gel processing. Annealing the thin film composite at 650 deg. C transforms the chemically disordered fcc FePt phase into the fct phase, yielding magnetic coercivity values H c >630 mT. The positional order of the particles is retained due to the protection offered by the silica host. Such films with assemblies of high-coercivity magnetic particles are attractive for realizing new types of ultra-high-density data storage devices and magneto-composites.

Easy approach to assembling a biomimetic color film with tunable structural colors.

Science.gov (United States)

Wang, Wentao; Tang, Bingtao; Ma, Wei; Zhang, Jian; Ju, Benzhi; Zhang, Shufen

2015-06-01

The self-assembly of silica microspheres into a close-packed array is a simple method of fabricating three-dimensional photonic crystal structural color films. However, the color is very dull because of the interferences of scattering and background light. In this study, we added a small quantity of surface-modified carbon black (CB) to the system of colloidal silica in n-propanol. The use of n-propanol as a dispersant is beneficial to the rapid development of photonic crystal films during the process of dip-coating. The doping of CB into silica microspheres can absorb background and scattering light, resulting in vivid structural colors.

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)

Low temperature mechanical dissipation of an ion-beam sputtered silica film

International Nuclear Information System (INIS)

Martin, I W; Craig, K; Bassiri, R; Hough, J; Robie, R; Rowan, S; Nawrodt, R; Schwarz, C; Harry, G; Penn, S; Reid, S

2014-01-01

Thermal noise arising from mechanical dissipation in oxide mirror coatings is an important limit to the sensitivity of future gravitational wave detectors, optical atomic clocks and other precision measurement systems. Here, we present measurements of the temperature dependence of the mechanical dissipation of an ion-beam sputtered silica film between 10 and 300 K. A dissipation peak was observed at 20 K and the low temperature dissipation was found to have significantly different characteristics than observed for bulk silica and silica films deposited by alternative techniques. These results are important for better understanding the underlying mechanisms of mechanical dissipation, and thus thermal noise, in the most commonly-used reflective coatings for precision measurements. (paper)

Ageing-induced enhancement of open porosity of mesoporous silica films studied by positron annihilation spectroscopy

International Nuclear Information System (INIS)

He Chunqing; Muramatsu, Makoto; Oshima, Nagayasu; Ohdaira, Toshiyuki; Kinomura, Atsushi; Suzuki, Ryoichi

2006-01-01

We show that ageing of the silica sol in a closed vessel enhanced the open porosity of calcined mesoporous silica film studied by positron. Positron annihilation lifetime spectroscopy (PALS) based on a pulsed slow positron beam was used to estimate the mesopore size. 2-dimensional PALS (2D-PALS) and ortho-positronium time-of-flight (Ps-TOF) were used to evaluate the open porosity, interconnectivity and tortuosity of mesopores in the silica films. Results revealed that little change in pore size but significant enhancement of open porosity and/or pore interconnectivity occurred in the silica film deposited after the precursor solution aged for a relative longer time

High-quality substrate for fluorescence enhancement using agarose-coated silica opal film.

Science.gov (United States)

Xu, Ming; Li, Juan; Sun, Liguo; Zhao, Yuanjin; Xie, Zhuoying; Lv, Linli; Zhao, Xiangwei; Xiao, Pengfeng; Hu, Jing; Lv, Mei; Gu, Zhongze

2010-08-01

To improve the sensitivity of fluorescence detection in biochip, a new kind of substrates was developed by agarose coating on silica opal film. In this study, silica opal film was fabricated on glass substrate using the vertical deposition technique. It can provide stronger fluorescence signals and thus improve the detection sensitivity. After coating with agarose, the hybrid film could provide a 3D support for immobilizing sample. Comparing with agarose-coated glass substrate, the agarose-coated opal substrates could selectively enhance particular fluorescence signals with high sensitivity when the stop band of the silica opal film in the agarose-coated opal substrate overlapped the fluorescence emission wavelength. A DNA hybridization experiment demonstrated that fluorescence intensity of special type of agarose-coated opal substrates was about four times that of agarose-coated glass substrate. These results indicate that the optimized agarose-coated opal substrate can be used for improving the sensitivity of fluorescence detection with high quality and selectivity.

Reinforcement of LENRA film by in-situ generated silica produced by sol gel process

International Nuclear Information System (INIS)

Mahathir Mohamed; Eda Yuhana Ariffin; Dahlan Mohd; Ibrahim Abdullah

2008-08-01

Liquid epoxidised natural rubber acrylate (LENRA) film was reinforced with silica-siloxane structures formed in-situ via sol gel process. Combination of these two components produces organic-inorganic composites. Tetraethylorthosilicate (TEOS) was used as precursor material for silica generation. Sol gel reaction was carried out at different concentrations of TEOS i.e. between 10 and 50 phr. Instrumental analysis was carried out by dynamic mechanical analysis (DMA), thermogravimetry analysis (TGA) and FTIR. It was found that miscibility between organic and inorganic components improved with the presence of silanol groups (Si-OH) and polar solvent i.e. THF, via hydrogen bonding formation between siloxane and LENRA. In this work, the effects of TEOS composition on mechanical properties and interaction that occurs between fillers and matrix have also been studied. It was observed that increasing the concentration of TEOS improved the scratch and stress properties of the film. Morphology study by the scanning electron microscopy (SEM) showed in-situ generated silica particles were homogenous and well dispersed at low concentrations of TEOS. (Author)

Characterization of fluorinated silica thin films with ultra-low refractive index deposited at low temperature

Energy Technology Data Exchange (ETDEWEB)

Abbasi-Firouzjah, Marzieh [Semnan Science and Technology Park, 3614933578, Shahrood (Iran, Islamic Republic of); Shokri, Babak, E-mail: b-shokri@sbu.ac.ir [Laser & Plasma Research Institute, Shahid Beheshti University, G.C., Evin, Tehran 1983963113 (Iran, Islamic Republic of); Physics Department, Shahid Beheshti University, G.C., Evin, Tehran 1983963113 (Iran, Islamic Republic of)

2015-02-27

Structural and optical properties of low refractive index fluorinated silica (SiO{sub x}C{sub y}F{sub z}) films were investigated. The films were deposited on p-type silicon and polycarbonate substrates by radio frequency plasma enhanced chemical vapor deposition method at low temperatures. A mixture of tetraethoxysilane vapor, oxygen, and CF{sub 4} was used for deposition of the films. The influence of oxygen flow rate on the elemental compositions, chemical bonding states and surface roughness of the films was studied using energy dispersive X-ray analyzer, Fourier transform infrared spectroscopy in reflectance mode and atomic force microscopy, respectively. Effects of chemical bonds of the film matrix on optical properties and chemical stability were discussed. Energy dispersive spectroscopy showed high fluorine content in the SiO{sub x}C{sub y}F{sub z} film matrix which is in the range of 7.6–11.3%. It was concluded that in fluorine content lower than a certain limit, chemical stability of the film enhances, while higher contents of fluorine heighten moisture absorption followed by increasing refractive index. All of the deposited films were highly transparent. Finally, it was found that the refractive index of the SiO{sub x}C{sub y}F{sub z} film was continuously decreased with the increase of the O{sub 2} flow rate down to the minimum value of 1.16 ± 0.01 (at 632.8 nm) having the most ordered and nano-void structure and the least organic impurities. This sample also had the most chemical stability against moisture absorption. - Highlights: • Low deposition temperature and organic precursor led to higher film fluorination. • High fluorine and nanovoid structure led to drastic decrease in the refractive index. • Silica based thin film with ultralow refractive index of 1.16 was produced. • The produced ultralow-n film is highly stable against moisture absorption.

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.

Biodegradable Starch/Copolyesters Film Reinforced with Silica Nanoparticles: Preparation and Characterization

Science.gov (United States)

Lima, Roberta A.; Oliveira, Rene R.; Wataya, Célio H.; Moura, Esperidiana A. B.

Biodegradable starch/copolyesters/silica nanocomposite films were prepared by melt extrusion, using a twin screw extruder machine and blown extrusion process. The influence of the silica nanoparticle addition on mechanical and thermal properties of nanocomposite films was investigated by tensile tests; X-rays diffraction (XRD), differential scanning calorimetry (DSC) and Scanning electron microscopy (SEM) analysis and the correlation between properties was discussed. The results showed that incorporation of 2 % (wt %) of SiO2 nanoparticle in the blend matrix of PBAT/Starch, resulted in a gain of mechanical properties of blend.

Sol-gel-derived mesoporous silica films with low dielectric constants

Energy Technology Data Exchange (ETDEWEB)

Seraji, S.; Wu, Yun; Forbess, M.; Limmer, S.J.; Chou, T.; Cao, Guozhong [Washington Univ., Seattle, WA (United States). Dept. of Materials Science and Engineering

2000-11-16

Mesoporous silica films with low dielectric constants and possibly closed pores have been achieved with a multiple step sol-gel processing technique. Crack-free films with approximately 50% porosity and 0.9 {mu}m thicknesses were obtained, a tape-test revealing good adhesion between films and substrates or metal electrodes. Dielectric constants remained virtually unchanged after aging at room temperature at 56% humidity over 6 days. (orig.)

Preparation of silane-functionalized silica films via two-step dip coating sol–gel and evaluation of their superhydrophobic properties

International Nuclear Information System (INIS)

Ramezani, Maedeh; Vaezi, Mohammad Reza; Kazemzadeh, Asghar

2014-01-01

Highlights: • Superhydrophobic silica film was prepared by sol–gel process. • The surfaces exhibited superhydrophobicity with water contact angle greater than 150°. • AFM images showed the roughness increases with increasing the percentage of silylation agent. • Before and after modification, the particle size of silica was lower than 50 nm. - Graphical abstract: Schematic illustration of the surface modification of the silica nanoparticle by iso-OTMS on the glass substrate. - Abstract: In this paper, we study the two-step dip coating via a sol–gel process to prepare superhydrophobic silica films on the glass substrate. The water repellency of the silica films was controlled by surface silylation method using isooctyltrimethoxysilane (iso-OTMS) as a surface modifying agent. Silica alcosol was synthesized by keeping the molar ratio of ethyltriethoxysilane (ETES) precursor, ethanol (EtOH) solvent, water (H 2 O) was kept constant at 1:36:6.6 respectively, with 6 M NH 4 OH throughout the experiment and the percentages of hydrophobic agent in hexane bath was varied from 0 to 15 vol.%. The static water contact angle values of the silica films increased from 108° to 160° with an increase in the vol.% of iso-OTMS. At 15 vol%. of iso-OTMS, the silica film shows static water contact angle as high as 160°. The superhydrophobic silica films are thermally stable up to 440 °C and above this temperature, the silica films lose superhydrophobicity. By controlling the primer particle size of SiO 2 about 26 nm, leading to decrease the final size of silica nanoparticles after modification of nanoparticles by isooctyltrimethoxysilane about 42 nm. The films are transparent and have uniform size on the surface. The silica films have been characterized by atomic force microscopy (AFM), fourier transform infrared spectroscopy (FT-IR), transparency, contact angle measurement (CA), Zeta-potential, Thermal stability by TG–DTA analysis

Atomic Structure Control of Silica Thin Films on Pt(111)

KAUST Repository

Crampton, Andrew S; Ridge, Claron J.; Rö tzer, Marian David; Zwaschka, Gregor; Braun, Thomas; D'Elia, Valerio; Basset, Jean-Marie; Schweinberger, Florian Frank; Gü nther, Sebastian; Heiz, Ueli

2015-01-01

Metal oxide thin films grown on metal single crystals are commonly used to model heterogeneous catalyst supports. The structure and properties of thin silicon dioxide films grown on metal single crystals have only recently been thoroughly

TiO2 and SiC nanostructured films, organized CNT structures

Indian Academy of Sciences (India)

sized nanostructured TiO2 films through hydrolysis of titanium tetra-isopropoxide. (TTIP) [9 ... structured TiO2 as a photocatalyst is as follows [15]:. TiO2(ns) ... The deposited films were easily detached from the silica tube and subjected to. SEM.

Biomimetic Cationic Nanoparticles Based on Silica: Optimizing Bilayer Deposition from Lipid Films

Directory of Open Access Journals (Sweden)

Rodrigo T. Ribeiro

2017-10-01

Full Text Available The optimization of bilayer coverage on particles is important for a variety of biomedical applications, such as drug, vaccine, and genetic material delivery. This work aims at optimizing the deposition of cationic bilayers on silica over a range of experimental conditions for the intervening medium and two different assemblies for the cationic lipid, namely, lipid films or pre-formed lipid bilayer fragments. The lipid adsorption on silica in situ over a range of added lipid concentrations was determined from elemental analysis of carbon, hydrogen, and nitrogen and related to the colloidal stability, sizing, zeta potential, and polydispersity of the silica/lipid nanoparticles. Superior bilayer deposition took place from lipid films, whereas adsorption from pre-formed bilayer fragments yielded limiting adsorption below the levels expected for bilayer adsorption.

Photochemical oxygen reduction by zinc phthalocyanine and silver/gold nanoparticle incorporated silica thin films

Energy Technology Data Exchange (ETDEWEB)

Pal, Manas; Ganesan, Vellaichamy, E-mail: velganesh@yahoo.com; Azad, Uday Pratap

2012-12-15

Silver or gold nanoparticles are synthesized using a borohydride reduction method and are anchored simultaneously into/onto the mercaptopropyl functionalized silica. Later, zinc phthalocyanine is adsorbed onto the above materials. Thin films of these materials are prepared by coating an aqueous colloidal suspension of the respective material onto glass plates. Visible light irradiation of these films in oxygen saturated, stirred aqueous solutions effectively reduces oxygen to hydrogen peroxide. The photocatalytic reduction of oxygen is explained on the basis of the semiconducting properties of the silica films. The back electron transfer reaction is largely prevented by means of a sacrificial electron donor, triethanolamine. - Highlights: Black-Right-Pointing-Pointer Zinc phthalocyanine adsorbed silica materials were prepared. Black-Right-Pointing-Pointer Thin films of these materials photocatalytically reduce oxygen. Black-Right-Pointing-Pointer The photocatalysis is explained based on semiconductor properties of the materials. Black-Right-Pointing-Pointer Metal nanoparticles increase the photocatalytic efficiency of the materials.

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.

Quantum dots/silica/polymer nanocomposite films with high visible light transmission and UV shielding properties.

Science.gov (United States)

Mumin, Md Abdul; Xu, William Z; Charpentier, Paul A

2015-08-07

The dispersion of light-absorbing inorganic nanomaterials in transparent plastics such as poly(ethylene-co-vinyl acetate) (PEVA) is of enormous current interest in emerging solar materials, including photovoltaic (PV) modules and commercial greenhouse films. Nanocrystalline semiconductor or quantum dots (QDs) have the potential to absorb UV light and selectively emit visible light, which can control plant growth in greenhouses or enhance PV panel efficiencies. This work provides a new and simple approach for loading mesoporous silica-encapsulated QDs into PEVA. Highly luminescent CdS and CdS-ZnS core-shell QDs with 5 nm size were synthesized using a modified facile approach based on pyrolysis of the single-molecule precursors and capping the CdS QDs with a thin layer of ZnS. To make both the bare and core-shell structure QDs more resistant against photochemical reactions, a mesoporous silica layer was grown on the QDs through a reverse microemulsion technique based on hydrophobic interactions. By careful experimental tuning, this encapsulation technique enhanced the quantum yield (∼65%) and photostability compared to the bare QDs. Both the encapsulated bare and core-shell QDs were then melt-mixed with EVA pellets using a mini twin-screw extruder and pressed into thin films with controlled thickness. The results demonstrated for the first time that mesoporous silica not only enhanced the quantum yield and photostability of the QDs but also improved the compatibility and dispersibility of QDs throughout the PEVA films. The novel light selective films show high visible light transmission (∼90%) and decreased UV transmission (∼75%).

Synthesis and electrical characterization of low-temperature thermal-cured epoxy resin/functionalized silica hybrid-thin films for application as gate dielectrics

Energy Technology Data Exchange (ETDEWEB)

Na, Moonkyong, E-mail: nmk@keri.re.kr [HVDC Research Division, Korea Electrotechnology Research Institute, Changwon, 642-120 (Korea, Republic of); System on Chip Chemical Process Research Center, Department of Chemical Engineering, Pohang University of Science and Technology (POSTECH), Pohang, 790-784 (Korea, Republic of); Kang, Young Taec [Creative and Fundamental Research Division, Korea Electrotechnology Research Institute, Changwon, 642-120 (Korea, Republic of); Department of Polymer Science and Engineering, Pusan National University, Busan, 609-735 (Korea, Republic of); Kim, Sang Cheol [HVDC Research Division, Korea Electrotechnology Research Institute, Changwon, 642-120 (Korea, Republic of); Kim, Eun Dong [Creative and Fundamental Research Division, Korea Electrotechnology Research Institute, Changwon, 642-120 (Korea, Republic of)

2013-07-31

Thermal-cured hybrid materials were synthesized from homogenous hybrid sols of epoxy resins and organoalkoxysilane-functionalized silica. The chemical structures of raw materials and obtained hybrid materials were characterized using Fourier transform infrared spectroscopy. The thermal resistance of the hybrids was enhanced by hybridization. The interaction between epoxy matrix and the silica particles, which caused hydrogen bonding and van der Waals force was strengthened by organoalkoxysilane. The degradation temperature of the hybrids was improved by approximately 30 °C over that of the parent epoxy material. The hybrid materials were formed into uniformly coated thin films of about 50 nm-thick using a spin coater. An optimum mixing ratio was used to form smooth-surfaced hybrid films. The electrical property of the hybrid film was characterized, and the leakage current was found to be well below 10{sup −6} A cm{sup −2}. - Highlights: • Preparation of thermal-curable hybrid materials using epoxy resin and silica. • The thermal stability was enhanced through hybridization. • The insulation property of hybrid film was investigated as gate dielectrics.

Tailoring of the Nanotexture of Mesoporous Silica Films and their Functionalized Derivatives for Selectively Harvesting Low Molecular Weight Protein

Science.gov (United States)

Hu, Ye; Bouamrani, Ali; Tasciotti, Ennio; Li, Li; Liu, Xuewu; Ferrari, Mauro

2010-01-01

We present a fast, efficient and reliable system based on mesoporous silica chips to specifically fractionate and enrich the low molecular weight proteome. Mesoporous silica thin films with tunable features at the nanoscale were fabricated using the triblock copolymer template pathway. Using different templates and concentrations in the precursor solution, various pore size distributions, pore structures and connectivity were obtained and applied for selective recovery of low mass proteins. In combination with mass spectrometry and statistic analysis, we demonstrated the correlation between the nanophase characteristics of the mesoporous silica thin films and the specificity and efficacy of low mass proteome harvesting. In addition, to overcome the limitations of the pre-functionalization method in polymer selection, plasma ashing was used for the first time for the treatment of the mesoporous silica surface prior to chemical modification. Surface charge modifications by different functional groups resulted in a selective capture of the low molecular weight proteins from serum sample. In conclusion our study demonstrates that the ability to tune the physico-chemical properties of mesoporous silica surfaces, for a selective enrichment of the low molecular weight proteome from complex biological fluids, has the potential to promote proteomic biomarker discovery. PMID:20014864

Gold Incorporated Mesoporous Silica Thin Film Model Surface as a Robust SERS and Catalytically Active Substrate

Directory of Open Access Journals (Sweden)

Anandakumari Chandrasekharan Sunil Sekhar

2016-05-01

Full Text Available Ultra-small gold nanoparticles incorporated in mesoporous silica thin films with accessible pore channels perpendicular to the substrate are prepared by a modified sol-gel method. The simple and easy spin coating technique is applied here to make homogeneous thin films. The surface characterization using FESEM shows crack-free films with a perpendicular pore arrangement. The applicability of these thin films as catalysts as well as a robust SERS active substrate for model catalysis study is tested. Compared to bare silica film our gold incorporated silica, GSM-23F gave an enhancement factor of 103 for RhB with a laser source 633 nm. The reduction reaction of p-nitrophenol with sodium borohydride from our thin films shows a decrease in peak intensity corresponding to –NO2 group as time proceeds, confirming the catalytic activity. Such model surfaces can potentially bridge the material gap between a real catalytic system and surface science studies.

Development of pore interconnectivity/morphology in porous silica films investigated by cyclic voltammetry and slow positron annihilation spectroscopy

International Nuclear Information System (INIS)

Tang, Xiuqin; Xiong, Bangyun; Li, Qichao; Mao, Wenfeng; Xiao, Wei; Fang, Pengfei; He, Chunqing

2015-01-01

Highlights: •Porous silica films were studied by cyclic voltammetry and positron annihilation. •Highly interconnected pores were formed in the film fabricated with more CTAB. •Aligned nanochannels were observed in the porous flim prepared with 25 wt.% CTAB. •I − and Ps diffusion in the films was governed by pore interconnectivity/morphology. •Cyclic voltammetry is feasible to explore pore interconnectivity/morphology. -- Abstract: Cyclic voltammetry and positronium (Ps) 3γ-annihilation spectroscopy were applied to investigate pore interconnectivity/morphology of porous silica films fabricated with various loading of cetyltrimethyl ammonium bromide (CTAB). With increasing the ratio of CTAB up to 15 wt.%, the total charge Q, resulted from I − diffusion across the silica films, increased remarkably, indicative of formation of highly interconnected pores in the films prepared with more porogen. However, it decreased dramatically with further loading CTAB of 25 wt.%. Interestingly, 3γ-annihilation fraction I 3γ due to a triplet-state Ps (ortho-positronium, o-Ps) emission from the silica films showed a similar behavior as a function of CTAB loading. The abnormal decrement in Q and I 3γ in the film fabricated with 25 wt.% CTAB was well explained by formation of long nanochannels aligning parallel to the film surface. The results indicated that the total charge Q and Ps 3γ-annihilation fraction were closely associated with I − and Ps diffusion governed by the pore interconnectivity/morphology of the silica films, which made cyclic voltammetry possible to be a feasible tool to characterize pore interconnectivity/morphology of porous thin films

A Robust Fiber Bragg Grating Hydrogen Gas Sensor Using Platinum-Supported Silica Catalyst Film

OpenAIRE

Marina Kurohiji; Seiji Ichiriyama; Naoki Yamasaku; Shinji Okazaki; Naoya Kasai; Yusuke Maru; Tadahito Mizutani

2018-01-01

A robust fiber Bragg grating (FBG) hydrogen gas sensor for reliable multipoint-leakage monitoring has been developed. The sensing mechanism is based on shifts of center wavelength of the reflection spectra due to temperature change caused by catalytic combustion heat. The sensitive film which consists of platinum-supported silica (Pt/SiO2) catalyst film was obtained using sol-gel method. The precursor solution was composed of hexachloroplatinic acid and commercially available silica precursor...

Optical and electrical properties of boron doped diamond thin conductive films deposited on fused silica glass substrates

Energy Technology Data Exchange (ETDEWEB)

Ficek, M.; Sobaszek, M.; Gnyba, M. [Department of Metrology and Optoelectronics, Gdansk University of Technology, 11/12G. Narutowicza St., 80-233 Gdansk (Poland); Ryl, J. [Department of Electrochemistry, Corrosion and Material Engineering, Gdansk University of Technology, 11/12 Narutowicza St., 80-233 Gdansk (Poland); Gołuński, Ł. [Department of Metrology and Optoelectronics, Gdansk University of Technology, 11/12G. Narutowicza St., 80-233 Gdansk (Poland); Smietana, M.; Jasiński, J. [Institute of Microelectronics and Optoelectronics, Warsaw University of Technology, 75 Koszykowa St., 00-662 Warsaw (Poland); Caban, P. [Institute of Electronic Materials Technology, 133 Wolczynska St., 01-919 Warsaw (Poland); Bogdanowicz, R., E-mail: rbogdan@eti.pg.gda.pl [Department of Metrology and Optoelectronics, Gdansk University of Technology, 11/12G. Narutowicza St., 80-233 Gdansk (Poland); Materials and Process Simulation Center, California Institute of Technology, Pasadena, CA 91125 (United States)

2016-11-30

Highlights: • Growth of 60% of transmittance diamond films with resistivity as low as 48 Ω cm. • Two step seeding process of fused silica: plasma hydrogenation and wet seeding. • Nanodiamond seeding density of 2 × 10{sup 10} cm{sup −2} at fused silica substrates. • High refractive index (2.4 @550 nm) was achieved for BDD films deposited at 500 °C. - Abstract: This paper presents boron-doped diamond (BDD) film as a conductive coating for optical and electronic purposes. Seeding and growth processes of thin diamond films on fused silica have been investigated. Growth processes of thin diamond films on fused silica were investigated at various boron doping level and methane admixture. Two step pre-treatment procedure of fused silica substrate was applied to achieve high seeding density. First, the substrates undergo the hydrogen plasma treatment then spin-coating seeding using a dispersion consisting of detonation nanodiamond in dimethyl sulfoxide with polyvinyl alcohol was applied. Such an approach results in seeding density of 2 × 10{sup 10} cm{sup −2}. The scanning electron microscopy images showed homogenous, continuous and polycrystalline surface morphology with minimal grain size of 200 nm for highly boron doped films. The sp{sup 3}/sp{sup 2} ratio was calculated using Raman spectra deconvolution method. A high refractive index (range of 2.0–2.4 @550 nm) was achieved for BDD films deposited at 500 °C. The values of extinction coefficient were below 0.1 at λ = 550 nm, indicating low absorption of the film. The fabricated BDD thin films displayed resistivity below 48 Ohm cm and transmittance over 60% in the visible wavelength range.

Mesoporous silica films as catalyst support for microstructured reactors: preparation and characterization

NARCIS (Netherlands)

Muraza, O.; Kooyman, P.J.; Lafont, U.; Albouy, P.A.; Khimyak, T.; Rebrov, E.V.; Croon, de M.H.J.M.; Schouten, J.C.

2008-01-01

Mesoporous silica thin films with hexagonal and cubic mesostructure have been deposited by the evaporation induced self-assembly assisted sol–gel route on microchannels etched in a Pyrex® 7740 borosilicate glass substrate. Prior to the synthesis, a 50 nm TiO2 film has been deposited on the substrate

Preparation and Properties of Nano Dy/TiO2 Films Supported on High Silica Fiber

Directory of Open Access Journals (Sweden)

HUANG Feng-ping

2017-07-01

Full Text Available In order to improve the photocatalytic degradation performance and stability of nano TiO2, Dy doped TiO2 supported on high silica glass fiber was prepared by microwave-sol method combined with dip-coating method. The samples were analyzed by XRD,SEM,PL,EDS,XPS and other equipments for phase composition of films,surface topography, surface elements and the stability of films. And the effects of pretreatment solution and coating method on the high-silica fiber film were investigated.In addition, the photocatalytic performance of the sample has been investigated by degrading methylene blue. The results show that the catalytic stability of Dy doping TiO2 nanofilms supported on high silica glass fiber can be improved and the degradation of methyl orange can reach 94% in 30min after 5 times of coating treatment.

Large third-order optical nonlinearity in vertically oriented mesoporous silica thin films embedded with Ag nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Tan, Min; Liu, Qiming, E-mail: qmliu@whu.edu.cn [Wuhan University, Key Laboratory of Artificial Micro- and Nano-structures of Ministry of Education, School of Physics and Technology (China)

2016-12-15

Taking advantage of the channel confinement of mesoporous films to prevent the agglomeration of Ag nanoparticles to achieve large third-order optical nonlinearity in amorphous materials, Ag-loaded composite mesoporous silica film was prepared by the electrochemical deposition method on ITO substrate. Ag ions were firstly transported into the channels of mesoporous film by the diffusion and binding force of channels, which were reduced to nanoparticles by applying suitable voltage. The existence and uniform distribution of Ag nanoparticles ranging in 1–10 nm in the mesoporous silica thin films were exhibited by UV spectrophotometer, X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) measurements. The third-order optical nonlinearity induced by Ag nanoparticles was studied by the Z-scan technique. Due to the local field surface plasmon resonance, the maximum third-order nonlinear optical susceptibility of Ag-loaded composite mesoporous silica film is 1.53×10{sup −10} esu, which is 1000 times larger than that of the Ag-contained chalcogenide glasses which showed large nonlinearity in amorphous materials.

Nanotexture Optimization by Oxygen Plasma of Mesoporous Silica Thin Film for Enrichment of Low Molecular Weight Peptides Captured from Human Serum

Science.gov (United States)

Hu, Ye; Peng, Yang; Brousseau, Louis; Bouamrani, Ali; Liu, Xuewu; Ferrari, Mauro

2010-01-01

This study investigated the optimization of mesoporous silica thin films by nanotexturing using oxygen plasma versus thermal oxidation. Calcination in oxygen plasma provides superior control over pore formation with regard to the pore surface and higher fidelity to the structure of the polymer template. The resulting porous film offers an ideal substrate for the selective partitioning of peptides from complex mixtures. The improved chemico-physical characteristics of porous thin films (pore size distribution, nanostructure, surface properties and pore connectivity) were systematically characterized with XRD, Ellipsometry, FTIR, TEM and N2 adsorption/desorption. The enrichment of low molecular weight proteins captured from human serum on mesoporous silica thin films fabricated by both methodologies were investigated by comparison of their MALDI-TOF MS profiles. This novel on-chip fractionation technology offers advantages in recovering the low molecular weight peptides from human serum, which has been recognized as an informative resource for early diagnosis of cancer and other diseases. PMID:21179395

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.

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.

Growth of ordered silver nanoparticles in silica film mesostructured with a triblock copolymer PEO-PPO-PEO

International Nuclear Information System (INIS)

Bois, L.; Chassagneux, F.; Parola, S.; Bessueille, F.; Battie, Y.; Destouches, N.; Boukenter, A.; Moncoffre, N.; Toulhoat, N.

2009-01-01

Elaboration of mesostructured silica films with a triblock copolymer polyethylene oxide-polypropylene oxide-polyethylene oxide, (PEO-PPO-PEO) and controlled growth of silver nanoparticles in the mesostructure are described. The films are characterized using UV-visible optical absorption spectroscopy, TEM, AFM, SEM, X-ray diffraction (XRD) and Rutherford backscattering spectrometry (RBS). Organized arrays of spherical silver nanoparticles with diameter between 5 and 8 nm have been obtained by NaBH 4 reduction. The size and the repartition of silver nanoparticles are controlled by the film mesostructure. The localization of silver nanoparticles exclusively in the upper-side part of the silica-block copolymer film is evidenced by RBS experiment. On the other hand, by using a thermal method, 40 nm long silver sticks can be obtained, by diffusion and coalescence of spherical particles in the silica-block copolymer layer. In this case, migration of silver particles toward the glass substrate-film interface is shown by the RBS experiment. - Graphical abstract: Growth of silver nanoparticles in a mesostructured block copolymer F127-silica film is performed either by a chemical route involving NaBH 4 reduction or by a thermal method. An array of spherical silver nanoparticles with 10 nm diameter on the upper-side of the mesostructured film or silver sticks long of 40 nm with a preferential orientation are obtained according to the method used. a: TEM image of the Fag5SiNB sample illustrating the silver nanoparticles array obtained by the chemical process; b: HR-TEM image of the Fag20Sid2 sample illustrating the silver nanosticks obtained by the thermal process.

Reversible Surface Properties of Polybenzoxazine/Silica Nanocomposites Thin Films

Directory of Open Access Journals (Sweden)

Wei-Chen Su

2013-01-01

Full Text Available We report the reversible surface properties (hydrophilicity, hydrophobicity of a polybenzoxazine (PBZ thin film through simple application of alternating UV illumination and thermal treatment. The fraction of intermolecularly hydrogen bonded O–H⋯O=C units in the PBZ film increased after UV exposure, inducing a hydrophilic surface; the surface recovered its hydrophobicity after heating, due to greater O–H⋯N intramolecular hydrogen bonding. Taking advantage of these phenomena, we prepared a PBZ/silica nanocomposite coating through two simple steps; this material exhibited reversible transitions from superhydrophobicity to superhydrophilicity upon sequential UV irradiation and thermal treatment.

Controlling pore morphology and properties of nanoporous silica films using the different architecture PS-b-P2VP as a template.

Science.gov (United States)

Yu, Yang-Yen; Chien, Wen-Chen; Chen, Shih-Ting

2010-07-01

Nanoporous silica films were prepared through the templating of amphiphilic block copolymer, poly(styrene-2-vinyl pyridine) (PS-b-P2VP), and monodispersed colloidal silica nanoparticles. The experimental and theoretical studies suggested that the intermolecular hydrogen bonding existes between the colloidal silica nanoparticles and PS-b-P2VP. The effects of the loading ratio and P2VP chain length on the morphology and properties of the prepared nanoporous silica films were investigated. TEM and AFM studies showed that the uniform pore size could be achieved and the pore size increased with increasing porogen loading. The refractive index and dielectric constant of the prepared nanoporous films decreased with an increase in PS-b-P2VP loading. On the other hand, the porosity increased with an increasing PS-b-P2VP loading. This study demonstrated a methodology to control pore morphology and properties of the nanoporous silica films through the templating of PS-b-P2VP.

Organized mesoporous silica films as templates for the elaboration of organized nanoparticle networks

International Nuclear Information System (INIS)

Gacoin, T; Besson, S; Boilot, J P

2006-01-01

Tremendous work achieved in the last 20 years on nanoparticle synthesis has allowed us to study many new physical properties that are found in the nanometre size range. New developments are now expected when considering assemblies of nanoparticles such as 2D or 3D organized arrays. These systems are indeed expected to exhibit original physical properties resulting from particle-particle interactions. Studies in this field are clearly dependent on the elaboration of materials with controlled particle size, organization and interparticle distance. This paper presents a strategy of elaboration that is based on the use of organized mesoporous silica films as templates. These films are made by sol-gel polymerization around surfactant assemblies and further elimination of the surfactant. This provides porous matrices with a pore organization that is the almost perfect replica of the initial micellar structure. The use of such films for the elaboration of organized arrays of nanoparticles is detailed in the case of CdS and Ag particles. The formation of particles inside the pores is achieved through impregnation with precursors that are allowed to diffuse inside the pores. This leads to particles with a size and a spatial arrangement that is directly related to the initial pore structure of the films. This process opens a wide range of investigations due to the relative ease of fabrication over large surfaces and the numerous possibilities offered by the elaboration of porous films with different pore sizes and organizations

Bidisperse silica nanoparticles close-packed monolayer on silicon substrate by three step spin method

Science.gov (United States)

Khanna, Sakshum; Marathey, Priyanka; Utsav, Chaliawala, Harsh; Mukhopadhyay, Indrajit

2018-05-01

We present the studies on the structural properties of monolayer Bidisperse silica (SiO2) nanoparticles (BDS) on Silicon (Si-100) substrate using spin coating technique. The Bidisperse silica nanoparticle was synthesised by the modified sol-gel process. Nanoparticles on the substrate are generally assembled in non-close/close-packed monolayer (CPM) form. The CPM form is obtained by depositing the colloidal suspension onto the silicon substrate using complex techniques. Here we report an effective method for forming a monolayer of bidisperse silica nanoparticle by three step spin coating technique. The samples were prepared by mixing the monodisperse solutions of different particles size 40 and 100 nm diameters. The bidisperse silica nanoparticles were self-assembled on the silicon substrate forming a close-packed monolayer film. The scanning electron microscope images of bidisperse films provided in-depth film structure of the film. The maximum surface coverage obtained was around 70-80%.

Two-dimensional silica opens new perspectives

Science.gov (United States)

Büchner, Christin; Heyde, Markus

2017-12-01

In recent years, silica films have emerged as a novel class of two-dimensional (2D) materials. Several groups succeeded in epitaxial growth of ultrathin SiO2 layers using different growth methods and various substrates. The structures consist of tetrahedral [SiO4] building blocks in two mirror symmetrical planes, connected via oxygen bridges. This arrangement is called a silica bilayer as it is the thinnest 2D arrangement with the stoichiometry SiO2 known today. With all bonds saturated within the nano-sheet, the interaction with the substrate is based on van der Waals forces. Complex ring networks are observed, including hexagonal honeycomb lattices, point defects and domain boundaries, as well as amorphous domains. The network structures are highly tuneable through variation of the substrate, deposition parameters, cooling procedure, introducing dopants or intercalating small species. The amorphous networks and structural defects were resolved with atomic resolution microscopy and modeled with density functional theory and molecular dynamics. Such data contribute to our understanding of the formation and characteristic motifs of glassy systems. Growth studies and doping with other chemical elements reveal ways to tune ring sizes and defects as well as chemical reactivities. The pristine films have been utilized as molecular sieves and for confining molecules in nanocatalysis. Post growth hydroxylation can be used to tweak the reactivity as well. The electronic properties of silica bilayers are favourable for using silica as insulators in 2D material stacks. Due to the fully saturated atomic structure, the bilayer interacts weakly with the substrate and can be described as quasi-freestanding. Recently, a mm-scale film transfer under structure retention has been demonstrated. The chemical and mechanical stability of silica bilayers is very promising for technological applications in 2D heterostacks. Due to the impact of this bilayer system for glass science

Effect of structure on nonlinear optical properties in CaCu{sub 3}Ti{sub 4}O{sub 12} films

Energy Technology Data Exchange (ETDEWEB)

Ning, Tingyin [School of Physics and Electronics, Shandong Normal University, Jinan 250014 (China); Zhou, Yueliang, E-mail: ylzhou@iphy.ac.cn [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190 (China)

2015-12-21

We report the third-order nonlinear optical properties of CaCu{sub 3}Ti{sub 4}O{sub 12} films with different preferred growth orientations on MgO and fused silica substrates. The films have (310)- and (220)-orientation on MgO and fused silica, respectively, due to the lattice-mismatch. Raman spectra further indicate different atom-bonding states in the films. The nonlinear optical measurements show the films possess the same self-defocusing behavior but with different values of nonlinear refraction, and changed signs of nonlinear absorption. The difference of optical nonlinearity in CaCu{sub 3}Ti{sub 4}O{sub 12} films is ascribed to different lattice parameters and intermediate levels induced by structure.

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.

A Robust Fiber Bragg Grating Hydrogen Gas Sensor Using Platinum-Supported Silica Catalyst Film

Directory of Open Access Journals (Sweden)

Marina Kurohiji

2018-01-01

Full Text Available A robust fiber Bragg grating (FBG hydrogen gas sensor for reliable multipoint-leakage monitoring has been developed. The sensing mechanism is based on shifts of center wavelength of the reflection spectra due to temperature change caused by catalytic combustion heat. The sensitive film which consists of platinum-supported silica (Pt/SiO2 catalyst film was obtained using sol-gel method. The precursor solution was composed of hexachloroplatinic acid and commercially available silica precursor solution. The atom ratio of Si : Pt was fixed at 13 : 1. A small amount of this solution was dropped on the substrate and dried at room temperature. After that, the film was calcined at 500°C in air. These procedures were repeated and therefore thick hydrogen-sensitive films were obtained. The catalytic film obtained by 20-time coating on quartz glass substrate showed a temperature change 75 K upon exposure to 3 vol.% H2. For realizing robust sensor device, this catalytic film was deposited and FBG portion was directly fixed on titanium substrate. The sensor device showed good performances enough to detect hydrogen gas in the concentration range below lower explosion limit at room temperature. The enhancement of the sensitivity was attributed to not only catalytic combustion heat but also related thermal strain.

Bragg gratings in air-silica structured fibers

NARCIS (Netherlands)

Groothoff, N.; Canning, J.; Buckley, E.; Lyttikainen, K.; Zagari, J.

2003-01-01

We report on grating writing in air-silica structured optical fibers with pure silica cores by use of two-photon absorption at 193 nm. A decrease in propagation loss with irradiation was observed. The characteristic growth curves were obtained. © 2003 Optical Society of America.

Structure and Properties of LENRA/ Silica Composite

International Nuclear Information System (INIS)

Mahathir Mohamed; Dahlan Mohd

2010-01-01

The sol-gel reaction using tetra ethoxysilane (TEOS) was conducted for modified natural rubber (NR) matrix to obtain in situ generated NR/ silica composite. The present of acrylate group in the modified NR chain turns the composite into radiation-curable. The maximum amount of silica generated in the matrix was 50 p hr by weight. During the sol-gel process the inorganic mineral was deposited in the rubber matrix forming hydrogen bonding between organic and inorganic phases. The composites obtained were characterized by various techniques including thermogravimetric analysis and infrared spectrometry to study their molecular structure. The increase in mechanical properties was observed for low silica contents ( 30 p hr) where more silica were generated, agglomerations were observed at the expense of the mechanical properties. From the DMTA data, it shows an increase of the interaction between the rubber and silica phases up to 30 p hr TEOS. Structure and morphology of the heterogeneous system were analyzed by transmission electron microscopy. The average particle sizes of between 150 nm to 300 nm were achieved for the composites that contain less than 20 p hr of TEOS. (author)

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

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.

Selective porous gates made from colloidal silica nanoparticles

Directory of Open Access Journals (Sweden)

Roberto Nisticò

2015-11-01

Full Text Available Highly selective porous films were prepared by spin-coating deposition of colloidal silica nanoparticles on an appropriate macroporous substrate. Silica nanoparticles very homogenous in size were obtained by sol–gel reaction of a metal oxide silica precursor, tetraethyl orthosilicate (TEOS, and using polystyrene-block-poly(ethylene oxide (PS-b-PEO copolymers as soft-templating agents. Nanoparticles synthesis was carried out in a mixed solvent system. After spin-coating onto a macroporous silicon nitride support, silica nanoparticles were calcined under controlled conditions. An organized nanoporous layer was obtained characterized by a depth filter-like structure with internal porosity due to interparticle voids. Permeability and size-selectivity were studied by monitoring the diffusion of probe molecules under standard conditions and under the application of an external stimulus (i.e., electric field. Promising results were obtained, suggesting possible applications of these nanoporous films as selective gates for controlled transport of chemical species in solution.

Steady state and time resolved fluorescence studies of azadioxatriangulenium (ADOTA) fluorophore in silica and PVA thin films

DEFF Research Database (Denmark)

Chib, Rahul; Raut, Sangram; Shah, Sunil

2015-01-01

A cationic azadioxatriangulenium dye was entrapped in silica thin films obtained by the sol-gel process and in poly (vinyl) alcohol (PVA) thin films. Azadioxatriangulenium is a red emitting fluorophore with a long fluorescence lifetime of ∼20 ns. The fluorescent properties of azadioxatriangulenium...

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

Facile method to fabricate raspberry-like particulate films for superhydrophobic surfaces.

Science.gov (United States)

Tsai, Hui-Jung; Lee, Yuh-Lang

2007-12-04

A facile method using layer-by-layer assembly of silica particles is proposed to prepare raspberry-like particulate films for the fabrication of superhydrophobic surfaces. Silica particles 0.5 microm in diameter were used to prepare a surface with a microscale roughness. Nanosized silica particles were then assembled on the particulate film to construct a finer structure on top of the coarse one. After surface modification with dodecyltrichlorosilane, the advancing and receding contact angles of water on the dual-sized structured surface were 169 and 165 degrees , respectively. The scale ratio of the micro/nano surface structure and the regularity of the particulate films on the superhydrophobic surface performance are discussed.

Ordered mesoporous silica materials with complicated structures

KAUST Repository

Han, Yu

2012-05-01

Periodically ordered mesoporous silicas constitute one of the most important branches of porous materials that are extensively employed in various chemical engineering applications including adsorption, separation and catalysis. This short review gives an introduction to recently developed mesoporous silicas with emphasis on their complicated structures and synthesis mechanisms. In addition, two powerful techniques for solving complex mesoporous structures, electron crystallography and electron tomography, are compared to elucidate their respective strength and limitations. Some critical issues and challenges regarding the development of novel mesoporous structures as well as their applications are also discussed. © 2011 Elsevier Ltd.

Organic-Inorganic Hydrophobic Nanocomposite Film with a Core-Shell Structure

Directory of Open Access Journals (Sweden)

Peng Liu

2016-12-01

Full Text Available A method to prepare novel organic-inorganic hydrophobic nanocomposite films was proposed by a site-specific polymerization process. The inorganic part, the core of the nanocomposite, is a ternary SiO2–Al2O3–TiO2 nanoparticles, which is grafted with methacryloxy propyl trimethoxyl silane (KH570, and wrapped by fluoride and siloxane polymers. The synthesized samples are characterized by transmission electron microscopy (TEM, Fourier transform infrared (FTIR spectrscopy, X-ray diffractometry (XRD, contact angle meter (CA, and scanning electron microscope (SEM. The results indicate that the novel organic-inorganic hydrophobic nanocomposite with a core-shell structure was synthesized successfully. XRD analysis reveals the nanocomposite film has an amorphous structure, and FTIR analysis indicates the nanoparticles react with a silane coupling agent (methacryloxy propyl trimethoxyl silane KH570. Interestingly, the morphology of the nanoparticle film is influenced by the composition of the core. Further, comparing with the film synthesized by silica nanoparticles, the film formed from SiO2–Al2O3–TiO2 nanoparticles has higher hydrophobic performance, i.e., the contact angle is greater than 101.7°. In addition, the TEM analysis reveals that the crystal structure of the particles can be changed at high temperatures.

Structure and dynamics of a silica melt in neutral confinement

Science.gov (United States)

Geske, Julian; Drossel, Barbara; Vogel, Michael

2017-04-01

We analyze the effects of spatial confinement on viscous silica using molecular dynamics simulations. For this purpose, we prepare a silica melt in a cylindrical pore, which is produced by pinning appropriate fractions of silicon and oxygen atoms in a bulk system after an equilibration period. In this way, the structure of the confined silica melt remains unaffected, while the confinement has a strong impact on the dynamics. We find that the structural relaxation of viscous silica is slowed down according to a double exponential law when approaching the pore wall. Moreover, we observe that static density correlations exist in the vicinity of the pore wall. Based on these effects, we determine dynamical and structural length scales of the silica melt. Both length scales show a similar increase upon cooling, with values on the order of the next-neighbor distances in the studied temperature range. Interestingly, we find no evidence that the growth of the length scales is affected by a fragile-to-strong transition of the silica melt. This observation casts serious doubts on the relevance of these length scales for the structural relaxation, at least for the studied glass former.

Defect prevention in silica thin films synthesized using AP-PECVD for flexible electronic encapsulation

NARCIS (Netherlands)

Elam, F.M.; Starostin, S.A.; Meshkova, A.S.; Van Der Velden-Schuermans, B.C.A.M.; Van De Sanden, M.C.M.; De Vries, H.W.

2017-01-01

Industrially and commercially relevant roll-to-roll atmospheric pressure-plasma enhanced chemical vapour deposition was used to synthesize smooth, 80 nm silica-like bilayer thin films comprising a dense 'barrier layer' and comparatively porous 'buffer layer' onto a flexible polyethylene 2,6

Supramolecular structures on silica surfaces and their adsorptive properties.

Science.gov (United States)

Belyakov, Vladimir N; Belyakova, Lyudmila A; Varvarin, Anatoly M; Khora, Olexandra V; Vasilyuk, Sergei L; Kazdobin, Konstantin A; Maltseva, Tetyana V; Kotvitskyy, Alexey G; Danil de Namor, Angela F

2005-05-01

The study of adsorptive and chemical immobilization of beta-cyclodextrin on a surface of hydroxylated silicas with various porous structure is described. Using IR spectroscopy, thermal gravimetrical analysis with a programmed heating, and chemical analysis of the silica surface, it is shown that the process of adsorption-desorption of beta-cyclodextrin depends on the porous structure of the silica. The reaction of esterification was used for chemical grafting of beta-cyclodextrin on the surface of hydroxylated silicas. Hydrolytic stability of silicas chemically modified by beta-cyclodextrin apparently is explained by simultaneous formation of chemical and hydrogen bonds between surface silanol groups and hydroxyl groups of beta-cyclodextrin. The uptake of the cations Cu(II), Cd(II), and Pb(II) and the anions Cr(VI) and As(V) by silicas modified with beta-cyclodextrin is investigated as a function of equilibrium ion concentrations. The increase of ion uptake and selectivity of ion extraction in comparison with starting silicas is established. It is due to the formation of surface inclusion complexes of the "host-guest" type in which one molecule of beta-cyclodextrin interacts simultaneously with several ions.

Sol-gel approach to the novel organic-inorganic hybrid composite films with ternary europium complex covalently bonded with silica matrix

International Nuclear Information System (INIS)

Dong Dewen; Yang Yongsheng; Jiang Bingzheng

2006-01-01

Novel organic-inorganic hybrid composite films with ternary lanthanide complex covalently bonded with silica matrix were prepared in situ via co-ordination of N-(3-propyltriethoxysilane)-4-carboxyphthalimide (TAT) and 1,10-phenanthroline (Phen) with europium ion (Eu 3+ ) during a sol-gel approach and characterized by the means of spectrofluorimeter, phosphorimeter and infrared spectrophotometer (FTIR). The resulting transparent films showed improved photophysical properties, i.e. increased luminescence intensity and longer luminescence lifetime, compared with the corresponding binary composite films without Phen. All the results revealed that the intense luminescence of the composite film was attributed to the efficient energy transfer from ligands, especially Phen, to chelated Eu 3+ and the reduced non-radiation through the rigid silica matrix and 'site isolation'

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.)

Preparation of mesoporous silica thin films by photocalcination method and their adsorption abilities for various proteins

Energy Technology Data Exchange (ETDEWEB)

Kato, Katsuya, E-mail: katsuya-kato@aist.go.jp [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya 463-8560 (Japan); Nakamura, Hitomi [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya 463-8560 (Japan); Yamauchi, Yoshihiro; Nakanishi, Kazuma; Tomita, Masahiro [Department of Chemistry for Materials, Graduate School of Engineering, Mie University, 1577 Kurimamachiya-cho, Tsu, Mie 514-8570 (Japan)

2014-07-01

Mesoporous silica (MPS) thin film biosensor platforms were established. MPS thin films were prepared from tetraethoxysilane (TEOS) via using sol–gel and spin-coating methods using a poly-(ethylene oxide)-block-poly-(propylene oxide)-block-poly-(ethylene oxide) triblock polymer, such as P123 ((EO){sub 20}(PO){sub 70}(EO){sub 20}) or F127 ((EO){sub 106}(PO){sub 70}(EO){sub 106}), as the structure-directing agent. The MPS thin film prepared using P123 as the mesoporous template and treated via vacuum ultraviolet (VUV) irradiation to remove the triblock copolymer had a more uniform pore array than that of the corresponding film prepared via thermal treatment. Protein adsorption and enzyme-linked immunosorbent assay (ELISA) on the synthesized MPS thin films were also investigated. VUV-irradiated MPS thin films adsorbed a smaller quantity of protein A than the thermally treated films; however, the human immunoglobulin G (IgG) binding efficiency was higher on the former. In addition, protein A–IgG specific binding on MPS thin films was achieved without using a blocking reagent; i.e., nonspecific adsorption was inhibited by the uniform pore arrays of the films. Furthermore, VUV-irradiated MPS thin films exhibited high sensitivity for ELISA testing, and cytochrome c adsorbed on the MPS thin films exhibited high catalytic activity and recyclability. These results suggest that MPS thin films are attractive platforms for the development of novel biosensors. - Highlights: • VUV-treated MPS thin films with removed polymer had uniform pore. • VUV-treated MPS thin films exhibited high sensitivity by ELISA. • Cytochrome c showed the catalytic activity and recyclability on synthesized films.

Preparation of mesoporous silica thin films by photocalcination method and their adsorption abilities for various proteins

International Nuclear Information System (INIS)

Kato, Katsuya; Nakamura, Hitomi; Yamauchi, Yoshihiro; Nakanishi, Kazuma; Tomita, Masahiro

2014-01-01

Mesoporous silica (MPS) thin film biosensor platforms were established. MPS thin films were prepared from tetraethoxysilane (TEOS) via using sol–gel and spin-coating methods using a poly-(ethylene oxide)-block-poly-(propylene oxide)-block-poly-(ethylene oxide) triblock polymer, such as P123 ((EO) 20 (PO) 70 (EO) 20 ) or F127 ((EO) 106 (PO) 70 (EO) 106 ), as the structure-directing agent. The MPS thin film prepared using P123 as the mesoporous template and treated via vacuum ultraviolet (VUV) irradiation to remove the triblock copolymer had a more uniform pore array than that of the corresponding film prepared via thermal treatment. Protein adsorption and enzyme-linked immunosorbent assay (ELISA) on the synthesized MPS thin films were also investigated. VUV-irradiated MPS thin films adsorbed a smaller quantity of protein A than the thermally treated films; however, the human immunoglobulin G (IgG) binding efficiency was higher on the former. In addition, protein A–IgG specific binding on MPS thin films was achieved without using a blocking reagent; i.e., nonspecific adsorption was inhibited by the uniform pore arrays of the films. Furthermore, VUV-irradiated MPS thin films exhibited high sensitivity for ELISA testing, and cytochrome c adsorbed on the MPS thin films exhibited high catalytic activity and recyclability. These results suggest that MPS thin films are attractive platforms for the development of novel biosensors. - Highlights: • VUV-treated MPS thin films with removed polymer had uniform pore. • VUV-treated MPS thin films exhibited high sensitivity by ELISA. • Cytochrome c showed the catalytic activity and recyclability on synthesized films

Defect prevention in silica thin films synthesized using AP-PECVD for flexible electronic encapsulation

NARCIS (Netherlands)

Elam, F. M.; Starostin, S. A.; Meshkova, A. S.; van der Velden, B. C. A. M.; van de Sanden, M. C. M.; de Vries, H. W.

2017-01-01

Industrially and commercially relevant roll-to-roll atmospheric pressure-plasma enhanced chemical vapour deposition was used to synthesize smooth, 80 nm silica-like bilayer thin films comprising a dense ‘barrier layer’ and comparatively porous ‘buffer layer’ onto a flexible polyethylene 2,6

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.

Effects of annealing time on the structure, morphology, and stress of gold–chromium bilayer film

International Nuclear Information System (INIS)

Zhang Hong; Wang Hu; Huang Hao-Peng; Jin Yun-Xia; Kong Fang-Yu; Cui Yun

2016-01-01

In this work, a 200-nm-thick gold film with a 10-nm-thick chromium layer used as an adhesive layer is fabricated on fused silica by the electron beam evaporation method. The effects of annealing time at 300 °C on the structure, morphology and stress of the film are studied. We find that chromium could diffuse to the surface of the film by formatting a solid solution with gold during annealing. Meanwhile, chromium is oxidized on the surface and diffused downward along the grain grooves in the gold film. The various operant mechanisms that change the residual stresses of gold films for different annealing times are discussed. (paper)

Positron and positronium annihilation in silica-based thin films studied by a pulsed positron beam

International Nuclear Information System (INIS)

Suzuki, R.; Ohdaira, T.; Kobayashi, Y.; Ito, K.; Shioya, Y.; Ishimaru, T.

2003-01-01

Positron and positronium annihilation in silica-based thin films has been investigated by means of measurement techniques with a monoenergetic pulsed positron beam. The age-momentum correlation study revealed that positron annihilation in thermally grown SiO 2 is basically the same as that in bulk amorphous SiO 2 while o-Ps in the PECVD grown SiCOH film predominantly annihilate with electrons of C and H at the microvoid surfaces. We also discuss time-dependent three-gamma annihilation in porous low-k films by two-dimensional positron annihilation lifetime spectroscopy

Relaxation of excited surface states of thin Ge-implanted silica films probed by OSEE spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Zatsepin, A.F., E-mail: a.f.zatsepin@urfu.ru [Ural Federal University, Mira Street 19, 620002 Ekaterinburg (Russian Federation); Buntov, E.A.; Mikhailovich, A.P.; Slesarev, A.I. [Ural Federal University, Mira Street 19, 620002 Ekaterinburg (Russian Federation); Schmidt, B. [Research Center Dresden-Rossendorf, Institute of Ion Beam Physics and Materials Research, P.O. Box 510119, D-01314 Dresden (Germany); Czarnowski, A. von; Fitting, Hans-Joachim [Institute of Physics, University of Rostock, Universitätsplatz 3, D-18051 Rostock (Germany)

2016-01-15

As an example of thin silica films, 30 nm SiO{sub 2}–Si heterostructures implanted with Ge{sup +} ions (10{sup 16} cm{sup −2} fluence) and rapid thermally annealed (RTA) at 950 °C are studied by means of optically stimulated electron emission (OSEE) in the spectral region of optical transparency for bulk silica. Quartz glass samples were used as references. Experimental data revealed a strong dependence between electron emission spectral features and RTA annealing time. The spectral contributions of both surface band tail states and interband transitions were clearly distinguished. The application of emission Urbach rule as well as Kane and Pässler equations allowed to analyze the OSEE spectra at different optical excitation energy ranges and to retrieve the important microstructural and energy parameters. The observed correlations between parameter values of Urbach- and Kane-related models suggest the implantation-induced conversion of both the vibrational subsystem and energy band of surface and interface electronic states. - Highlights: • Peculiarities of electron emission from excited surface states of SiO{sub 2}:Ge structures are studied. • Spectral contributions of surface band tails and interband transitions are distinguished. • Urbach and Kane models allow to examine photo-thermal emission mechanism. • Surface energy gap and structural disorder parameters are determined.

Ordered and disordered evolution of the pore mesostructure in hybrid silica anti-reflective films obtained by one-pot self-assembly method

Energy Technology Data Exchange (ETDEWEB)

Ghazzal, Mohamed N., E-mail: g_nawfel@yahoo.fr; Debecker, Damien P.; Gaigneaux, Eric M.

2016-07-29

Hybrid mesoporous silica films were prepared in acid-catalysed medium using a one-pot self-assembly method. A gradual content of methyl groups was introduced into the inorganic framework by co-condensation of tetraethyl orthosilicate and methyltriethoxysilane. To better understand how the ordered and disordered transition occurs in mesoporous hybrid organosilica sytem as function of the MTES molar ratio in the starting solution, textural, chemical and optical properties of the films were studied by transmission electronic microscopy (TEM), grazing-incident small angle X-ray scattering (GISAXS), transmission Fourier transformed infrared (FTIR) and UV–visible spectroscopy. Increasing the loading of the incorporated organic groups (up to 40% in the starting solution) led simultaneously to a disorganization of the pore mesostructure and a reduction in the pore diameter. Concomitantly, a disordered domain of the silica rings in the walls was observed, which created bond strains in the silica wall contributing also to the disorganization of the pore mesostructure. Furthermore, an optimal MTES content was identified in order to obtain antireflection coatings, exhibiting low reflection in the visible range. - Highlights: • Mesoporous hybrid silica films where prepared by one-pot co-condensation of MTES and TEOS. • Ordered and disordered mesostructures were studied as function as variable MTES molar ratio. • A rearrangement of the silica cyclic species occurred as the molar ratio of MTES increases. • Transmittance of the silica coatings is affected by the MTES molar ratio.

Characterization of electron beam deposited thin films of HfO2 and binary thin films of (HfO2:SiO2) by XRD and EXAFS measurements

International Nuclear Information System (INIS)

Das, N.C.; Sahoo, N.K.; Bhattacharyya, D.; Thakur, S.; Kamble, N.M.; Nanda, D.; Hazra, S.; Bal, J.K.; Lee, J.F.; Tai, Y.L.; Hsieh, C.A.

2009-10-01

In this report, we have discussed the microstructure and the local structure of composite thin films having varying hafnia and silica compositions and prepared by reactive electron beam evaporation. XRD and EXAFS studies have confirmed that the pure hafnium oxide thin film has crystalline microstructure whereas the films with finite hafnia and silica composition are amorphous. The result of EXAFS analysis has shown that the bond lengths as well as coordination numbers around hafnium atom change with the variation of hafnia and silica compositions in the thin film. Finally, change of bond lengths has been correlated with change of refractive index and band gap of the composite thin films. (author)

SEM and Raman studies of CNT films on porous Si

Science.gov (United States)

Belka, R.; Keczkowska, J.; Suchańska, M.; Firek, P.; Wronka, H.; Kozłowski, M.; Radomska, J.; Czerwosz, E.; Craciunoiu, F.

2017-08-01

Carbon nanotube (CNT) films deposited on different porous silica substrates were studied by Scanning Electron Microscopy (SEM) and Raman Spectroscopy (RS). The films samples were prepared by a two-step method consisting of PVD and CVD processes. In the first step the nanocomposite Ni-C film was obtained by evaporation in dynamic vacuum from two separated sources of fullerenes and nickel acetate. Those films were deposited on porous silica and DLC/porous silica substrates. Analysis of SEM imaging showed that the obtained film are composed of carbon nanotubes, the distribution, size and quality of which depend on the type of substrate. The CNT films were studied by RS method to determine the influence of the substrate type on disordering of carbonaceous structure and quality of CNT in deposited films.

Nanoscale assembly of lanthanum silica with dense and porous interfacial structures.

Science.gov (United States)

Ballinger, Benjamin; Motuzas, Julius; Miller, Christopher R; Smart, Simon; Diniz da Costa, João C

2015-02-03

This work reports on the nanoscale assembly of hybrid lanthanum oxide and silica structures, which form patterns of interfacial dense and porous networks. It was found that increasing the molar ratio of lanthanum nitrate to tetraethyl orthosilicate (TEOS) in an acid catalysed sol-gel process alters the expected microporous metal oxide silica structure to a predominantly mesoporous structure above a critical lanthanum concentration. This change manifests itself by the formation of a lanthanum silicate phase, which results from the reaction of lanthanum oxide nanoparticles with the silica matrix. This process converts the microporous silica into the denser silicate phase. Above a lanthanum to silica ratio of 0.15, the combination of growth and microporous silica consumption results in the formation of nanoscale hybrid lanthanum oxides, with the inter-nano-domain spacing forming mesoporous volume. As the size of these nano-domains increases with concentration, so does the mesoporous volume. The absence of lanthanum hydroxide (La(OH)3) suggests the formation of La2O3 surrounded by lanthanum silicate.

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

Phosphorus-doped thin silica films characterized by magic-angle spinning nuclear magnetic resonance spectroscopy

DEFF Research Database (Denmark)

Jacobsen, H.J.; Skibsted, J.; Kristensen, Martin

2001-01-01

Magic-angle spinning nuclear magnetic resonance spectra of 31P and 29Si have been achieved for a thin silica film doped with only 1.8% 31P and deposited by plasma enhanced chemical vapor deposition on a pure silicon wafer. The observation of a symmetric 31P chemical shift tensor is consistent...

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-03-15

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

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

International Nuclear Information System (INIS)

Hou Aiqin; Chen Huawei

2010-01-01

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

Unraveling the atomic structure of biogenic silica: evidence of the structural association of Al and Si in diatom frustules

Science.gov (United States)

Gehlen, M.; Beck, L.; Calas, G.; Flank, A.-M.; Van Bennekom, A. J.; Van Beusekom, J. E. E.

2002-05-01

We used X-ray absorption spectroscopy at the Al K-edge to investigate the atomic structure of biogenic silica and to assess the effect of Al on its crystal chemistry. Our study provides the first direct evidence for a structural association of Al and Si in biogenic silica. In samples of cultured diatoms, Al is present exclusively in fourfold coordination. The location and relative intensity of X-ray absorption near-edge structure (XANES) features suggests the structural insertion of tetrahedral Al inside the silica framework synthesized by the organism. In diatom samples collected in the marine environment, Al is present in mixed six- and fourfold coordination. The relative intensity of XANES structures indicates the coexistence of structural Al with a clay component, which most likely reflects sample contamination by adhering mineral particles. Extended X-ray absorption fine structure spectroscopy has been used to get Al-O distances in biogenic silica of cultured diatoms, confirming a tetrahedral coordination. Because of its effect on solubility and reaction kinetics of biogenic silica, the structural association between Al and biogenic silica at the stage of biosynthesis has consequences for the use of sedimentary biogenic silica as an indicator of past environmental conditions.

Perhydropolysilazane-derived silica-polymethylmethacrylate hybrid thin films highly doped with spiropyran: Effects of polymethylmethacrylate on the hardness, chemical durability and photochromic properties

International Nuclear Information System (INIS)

Yamano, Akihiro; Kozuka, Hiromitsu

2011-01-01

Polymethylmethacrylate (PMMA)-perhydropolysilazane (PHPS) hybrid thin films doped with spiropyran were prepared by spin-coating, which were then converted into 0.26-1.7 μm thick, spiropyran-doped PMMA-silica hybrid films by exposure treatment over aqueous ammonia. The spiropyran/(spiropyran + PHPS + PMMA) mass ratio was fixed at a high value of 0.2 so that the films exhibit visual photochromic changes in color, while the PMMA/(PMMA + PHPS) mass ratio, r, was varied. The spiropyran molecules in the as-prepared films were in merocyanine (MC) and spiro (SP) forms, with and without an optical absorption at 500 nm, at low (r ≤ 0.2) and high (r ≥ 0.4) PMMA contents, respectively. When PMMA content r was increased from 0 to 0.2, the degree of the MC-to-SP conversion on vis light illumination was enhanced, while at higher r's the spiropyran molecules underwent photodegradation. When the silica film (r = 0) was soaked in xylene under vis light, the spiropyran molecules were almost totally leached out, while not on soaking in the dark. On the other hand, no leaching occurred for the film of r = 0.2 either in the presence or absence of vis light. These suggest that the introduction of PMMA is effective in improving the chemical durability of the films, while the silica film (r = 0) is an interesting material with a photoresponsive controlled-release ability. The pencil hardness of the films decreased with increasing PMMA content, but remained over 9H at r ≤ 0.4.

Surface texture modification of spin-coated SiO2 xerogel thin films ...

Indian Academy of Sciences (India)

hydrolysis and condensation of tetraethylorthosilicate (TEOS) with ethanol as a solvent. Further, the deposited thin films were ... termed as hydrolysis and condensation that occur simultane- ously in the formation of silica films. ... rial leads to capillary tensions, which destroy the structure of silica (Naik and Ghosh 2009).

Investigation of structural properties associated with alkali-silica reaction by means of macro- and micro-structural analysis

International Nuclear Information System (INIS)

Mo Xiangyin; Fournier, Benoit

2007-01-01

Structural properties associated with alkali-silica reaction were systematically investigated by means of macro-structural accelerated mortar prism expansion levels testing, combined with micro-structural analysis. One part of this study is to determine the reactivity of the aggregate by means of accelerated mortar bar tests, and also to evaluate perlite aggregate constituents, especially the presence of deleterious components and find main causes of the alkali-silica reaction, which was based on the petrographic studies by optical microscope and the implication of X-ray diffraction on the aggregate. Results implied that the aggregate was highly alkali-silica reactive and the main micro-crystalline quartz-intermediate character and matrix that is mainly composed of chalcedony are potentially suitable for alkali-silica reaction. The other part is to study the long-term effect of lithium salts against alkali-silica reaction by testing accelerated mortar prism expansion levels. The macro-structural results were also consistent with the micro-structural mechanisms of alkali-silica reaction of mortar prisms containing this aggregate and the effect of chemical admixtures by means of the methods of scanning electron microscope-X-ray energy-dispersive spectroscopy and X-ray diffraction. It was indicated by these techniques that lithium salts, which were introduced into concrete containing reactive aggregate at the mixing stage, suppressed the alkali-silica reaction by producing non-expansive crystalline materials

Stability of erbium and silver implanted in silica-titania sol-gel films

International Nuclear Information System (INIS)

Ramos, A.R.; Marques, C.; Alves, E.; Marques, A.C.; Almeida, R.M.

2005-01-01

We implanted silica-titania sol-gel films with 3 x 10 15 at./cm 2 , 180 keV Er + and 6 x 10 16 at./cm 2 , 140 keV Ag + ions. The energies were chosen so that the profiles of Ag and Er overlap. RBS and ERDA were used to study the behaviour of Ag, Er and H during the heat treatments used to density the films. Implantation causes H depletion at the film surface and an increase in H concentration just beneath the implanted Ag and Er profiles. The total H content decreases by 27% to 75% during implantation. During annealing the H content decreases, with an almost complete H loss after annealing for 35 min at 800 deg. C. The Ag profile remains stable up to 600 deg. C. Above 700 deg. C Ag becomes increasingly mobile. Annealing at 800 deg. C for 35 min results in a nearly constant Ag distribution in the film. The Er profile remains unchanged with heat treatment up to the maximum temperature used (800 deg. C)

Voltammetric Determination of Lead (II) and Cadmium (II) Using a Bismuth Film Electrode Modified with Mesoporous Silica Nanoparticles

International Nuclear Information System (INIS)

Yang, Die; Wang, Liang; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

2014-01-01

A new chemically modified glassy carbon electrode based on bismuth film coated mesoporous silica nanoparticles was developed and evaluated for reliable quantification of trace Pb 2+ and Cd 2+ by anodic stripping square wave voltammetry in natural water samples. Compared with conventional bismuth film electrodes or bismuth nanoparticles modified electrodes, this electrode exhibited significantly improved sensitivity and stability for Pb 2+ and Cd 2+ detection. The key experimental parameters related to the fabrication of the electrode and the voltammetric measurements were optimized on the basis of the stripping signals, where the peak currents increased linearly with the metal concentrations in a range of 2-150 μg L −1 with a detect limit of 0.2 μg L −1 for Pb 2+ , and 0.6 μg L −1 for Cd 2+ for 120s deposition. Good reproducibility was achieved on both single and equally prepared electrodes. In addition, scanning electron microscopy reveals that fibril-like bismuth structures were formed on silica nanoparticles, which could be responsible for the improved voltammetric performance due to the enhanced surface area. Finally, the developed electrode was applied to determine Pb 2+ and Cd 2+ in water samples, indicating that this electrode was sensitive, reliable and effective for the simultaneous determination of Pb 2+ and Cd 2+

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.

Structural refinement of vitreous silica bilayers

Science.gov (United States)

Sadjadi, Mahdi; Wilson, Mark; Thorpe, M. F.

The importance of glasses resides not only in their applications but in fundamental questions that they put forth. The continuous random network model can successfully describe the glass structure, but determining details, like ring statistics, has always been difficult using only diffraction data. But recent atomic images of 2D vitreous silica bilayers can offer valuable new insights which are hard to be observed directly in 3D silica models/experiments (for references see). However, the experimental results are prone to uncertainty in atomic positions, systematic errors, and being finite. We employ special boundary conditions developed for such networks to refine the experimental structures. We show the best structure can be found by using various potentials to maximize information gained from the experimental samples. We find a range of densities, the so-called flexibility window, in which tetrahedra are perfect. We compare results from simulations using harmonic potentials, MD with atomic polarizabilities included and DFT. We should thank David Drabold and Bishal Bhattarai for useful discussions. Support through NSF Grant # DMS 1564468 is gratefully acknowledged.

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.

Study of the spectra of silica colloidal crystals with assembled silver obtained from a photolysis method

Science.gov (United States)

Li, Wenjiang; He, Jinglong; He, Sailing

2005-02-01

The colorful artificial 3D silica colloidal crystals (opal) were prepared through self-assembly of silica spheres in the visible frequency range. We directly synthesized nano silver particles in the void of the silica artificial opal film using the photolysis of silver nitrate under UV light, nano silver particles were self-deposited around the surface of silica sphere. The shifts of the stop band of the artificial crystals after exposing different time under UV light were studied. Synthetic silica opal with three-dimensional (3D) structure is potentially useful for the development of diffractive optical devices, micro mechanical systems, and sensory elements because photonic band gaps obtained from self-assembled closely packed periodic structures.

Low molecular weight protein enrichment on mesoporous silica thin films for biomarker discovery.

Science.gov (United States)

Fan, Jia; Gallagher, James W; Wu, Hung-Jen; Landry, Matthew G; Sakamoto, Jason; Ferrari, Mauro; Hu, Ye

2012-04-17

The identification of circulating biomarkers holds great potential for non invasive approaches in early diagnosis and prognosis, as well as for the monitoring of therapeutic efficiency.(1-3) The circulating low molecular weight proteome (LMWP) composed of small proteins shed from tissues and cells or peptide fragments derived from the proteolytic degradation of larger proteins, has been associated with the pathological condition in patients and likely reflects the state of disease.(4,5) Despite these potential clinical applications, the use of Mass Spectrometry (MS) to profile the LMWP from biological fluids has proven to be very challenging due to the large dynamic range of protein and peptide concentrations in serum.(6) Without sample pre-treatment, some of the more highly abundant proteins obscure the detection of low-abundance species in serum/plasma. Current proteomic-based approaches, such as two-dimensional polyacrylamide gel-electrophoresis (2D-PAGE) and shotgun proteomics methods are labor-intensive, low throughput and offer limited suitability for clinical applications.(7-9) Therefore, a more effective strategy is needed to isolate LMWP from blood and allow the high throughput screening of clinical samples. Here, we present a fast, efficient and reliable multi-fractionation system based on mesoporous silica chips to specifically target and enrich LMWP.(10,11) Mesoporous silica (MPS) thin films with tunable features at the nanoscale were fabricated using the triblock copolymer template pathway. Using different polymer templates and polymer concentrations in the precursor solution, various pore size distributions, pore structures, connectivity and surface properties were determined and applied for selective recovery of low mass proteins. The selective parsing of the enriched peptides into different subclasses according to their physicochemical properties will enhance the efficiency of recovery and detection of low abundance species. In combination with mass

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.

Silica promoted self-assembled mesoporous aluminas. Impact of the silica precursor on the structural, textural and acidic properties

NARCIS (Netherlands)

Perez, Lidia Lopez; Zarubina, Valeriya; Mayoral, Alvaro; Melian-Cabrera, Ignacio

2015-01-01

This paper investigates the effect of silica addition on the structural, textural and acidic properties of an evaporation induced self-assembled (EISA) mesoporous alumina. Two silica addition protocols were applied while maintaining the EISA synthesis route. The first route is based on the addition

Alkali passivation mechanism of sol-gel derived TiO2-SiO2 films coated on soda-lime-silica glass substrates

Energy Technology Data Exchange (ETDEWEB)

Matsuda, A; Matsuno, Y; Katayama, S; Tsuno, T [Nippon Steel Glass Co. Ltd., Tokyo (Japan); Toge, N; Minami, T [University of Osaka Prefecture, Osaka (Japan). College of Engineering

1992-09-01

TiO2-SiO2 films prepared by the sol-gel method serves as an effective alkali passivation layer on a soda-lime-silica glass substrate and the film is superior to a sol-gel derived pure SiO2 film from the view point of weathering resistance improvement. To clarify the reason, alkali passivation mechanism of sol-gel derived TiO2-SiO2 glass films with different TiO2 contents coated on a soda-lime-silica glass substrate was studied by SIMS (secondary ion mass spectroscopy) and XPS (X-ray photoelectron spectroscopy) analyses, and compared with the results of a sol-gel derived pure SiO2 film. As a result, the following conclusions were obtained: An increase in TiO2 content in the TiO2 SiO2 film increases the sodium concentration in the film, which was induced by sodium migration from the glass substrate during the heat-treatment. Because of the presence of sodium the TiO2 -SiO2 films serve not as a barrier but as an effective getter of alkali ions and thereby effectively improve the weathering resistance Of the glass substrate. 10 refs., 6 figs.

Electrochemical lithium migration to mitigate alkali-silica reaction in existing concrete structures

NARCIS (Netherlands)

Silva De Souza, L.M.

2016-01-01

Alkali-silica reaction (ASR) is a deterioration process that affects the durability of concrete structures worldwide. During the reaction, hydroxyl and alkali ions present in the pore solution react with reactive silica from the aggregate, forming a hygroscopic ASR gel. Alternatively, the silica

A Thin Film Nanocomposite Membrane with MCM-41 Silica Nanoparticles for Brackish Water Purification

Directory of Open Access Journals (Sweden)

Mohammed Kadhom

2016-12-01

Full Text Available Thin film nanocomposite (TFN membranes containing MCM-41 silica nanoparticles (NPs were synthesized by the interfacial polymerization (IP process. An m-phenylenediamine (MPD aqueous solution and an organic phase with trimesoyl chloride (TMC dissolved in isooctane were used in the IP reaction, occurring on a nanoporous polysulfone (PSU support layer. Isooctane was introduced as the organic solvent for TMC in this work due to its intermediate boiling point. MCM-41 silica NPs were loaded in MPD and TMC solutions in separate experiments, in a concentration range from 0 to 0.04 wt %, and the membrane performance was assessed and compared based on salt rejection and water flux. The prepared membranes were characterized via scanning electron microscopy (SEM, transmission electron microscopy (TEM, contact angle measurement, and attenuated total reflection Fourier transform infrared (ATR FT-IR analysis. The results show that adding MCM-41 silica NPs into an MPD solution yields slightly improved and more stable results than adding them to a TMC solution. With 0.02% MCM-41 silica NPs in the MPD solution, the water flux was increased from 44.0 to 64.1 L/m2·h, while the rejection virtually remained the same at 95% (2000 ppm NaCl saline solution, 25 °C, 2068 kPa (300 psi.

A Thin Film Nanocomposite Membrane with MCM-41 Silica Nanoparticles for Brackish Water Purification.

Science.gov (United States)

Kadhom, Mohammed; Yin, Jun; Deng, Baolin

2016-12-06

Thin film nanocomposite (TFN) membranes containing MCM-41 silica nanoparticles (NPs) were synthesized by the interfacial polymerization (IP) process. An m -phenylenediamine (MPD) aqueous solution and an organic phase with trimesoyl chloride (TMC) dissolved in isooctane were used in the IP reaction, occurring on a nanoporous polysulfone (PSU) support layer. Isooctane was introduced as the organic solvent for TMC in this work due to its intermediate boiling point. MCM-41 silica NPs were loaded in MPD and TMC solutions in separate experiments, in a concentration range from 0 to 0.04 wt %, and the membrane performance was assessed and compared based on salt rejection and water flux. The prepared membranes were characterized via scanning electron microscopy (SEM), transmission electron microscopy (TEM), contact angle measurement, and attenuated total reflection Fourier transform infrared (ATR FT-IR) analysis. The results show that adding MCM-41 silica NPs into an MPD solution yields slightly improved and more stable results than adding them to a TMC solution. With 0.02% MCM-41 silica NPs in the MPD solution, the water flux was increased from 44.0 to 64.1 L/m²·h, while the rejection virtually remained the same at 95% (2000 ppm NaCl saline solution, 25 °C, 2068 kPa (300 psi)).

Polymer-Silica nanoparticles composite films as protective coatings for stone-based monuments

Energy Technology Data Exchange (ETDEWEB)

Manoudis, P [Department of Chemical Engineering, Aristotle University of Thessaloniki, 54124, Thessaloniki (Greece); Papadopoulou, S [Department of Chemical Engineering, Aristotle University of Thessaloniki, 54124, Thessaloniki (Greece); Karapanagiotis, I [' Ormylia' Art Diagnosis Centre, Ormylia, Chalkidiki, 63071 (Greece); Tsakalof, A [Medical Department, University of Thessaly, Larissa, 41222 (Greece); Zuburtikudis, I [Department of Industrial Design Engineering, TEI of Western Macedonia, Kozani, 50100 (Greece); Panayiotou, C [Department of Chemical Engineering, Aristotle University of Thessaloniki, 54124, Thessaloniki (Greece)

2007-04-15

The decrease of surface energy of mineral substrates similar to those used in many stone monuments of cultural heritage by the application of protective polymer coatings along with the simultaneous increase of their surface roughness can increase their ability to repel water substantially. In this work, the effect of artificially induced roughness on the water repellency of mineral substrates coated with protective polymer films was investigated. Natural marble samples or home made calcium carbonate blocks were tried as the mineral substrates. The roughness increase was achieved by mineral chemical etching or by creation of nanoscale binary composition film on the substrate surface. PMMA and PFPE were the polymers used, while different-sized silica nanoparticles were employed for the production of the nanocomposite films. Examination of the coated and uncoated surfaces with profilometry and AFM and measurements of water contact angles reveal a pronounced effect of the surface roughness on water repellency. Especially in the case of nanocomposite coatings, the surfaces become super-hydrophobic. This result indicates that the nanoscale binary composition film scheme, which is characterized by its simplicity and low cost, is a suitable candidate for the water protection of stone-based monuments on large scale.

Polymer-Silica nanoparticles composite films as protective coatings for stone-based monuments

International Nuclear Information System (INIS)

Manoudis, P; Papadopoulou, S; Karapanagiotis, I; Tsakalof, A; Zuburtikudis, I; Panayiotou, C

2007-01-01

The decrease of surface energy of mineral substrates similar to those used in many stone monuments of cultural heritage by the application of protective polymer coatings along with the simultaneous increase of their surface roughness can increase their ability to repel water substantially. In this work, the effect of artificially induced roughness on the water repellency of mineral substrates coated with protective polymer films was investigated. Natural marble samples or home made calcium carbonate blocks were tried as the mineral substrates. The roughness increase was achieved by mineral chemical etching or by creation of nanoscale binary composition film on the substrate surface. PMMA and PFPE were the polymers used, while different-sized silica nanoparticles were employed for the production of the nanocomposite films. Examination of the coated and uncoated surfaces with profilometry and AFM and measurements of water contact angles reveal a pronounced effect of the surface roughness on water repellency. Especially in the case of nanocomposite coatings, the surfaces become super-hydrophobic. This result indicates that the nanoscale binary composition film scheme, which is characterized by its simplicity and low cost, is a suitable candidate for the water protection of stone-based monuments on large scale

Preparation of thick silica coatings on carbon fibers with fine-structured silica nanotubes induced by a self-assembly process

Directory of Open Access Journals (Sweden)

Benjamin Baumgärtner

2017-05-01

Full Text Available A facile method to coat carbon fibers with a silica shell is presented in this work. By immobilizing linear polyamines on the carbon fiber surface, the high catalytic activity of polyamines in the sol–gel-processing of silica precursors is used to deposit a silica coating directly on the fiber’s surface. The surface localization of the catalyst is achieved either by attaching short-chain polyamines (e.g., tetraethylenepentamine via covalent bonds to the carbon fiber surface or by depositing long-chain polyamines (e.g., linear poly(ethylenimine on the carbon fiber by weak non-covalent bonding. The long-chain polyamine self-assembles onto the carbon fiber substrate in the form of nanoscopic crystallites, which serve as a template for the subsequent silica deposition. The silicification at close to neutral pH is spatially restricted to the localized polyamine and consequently to the fiber surface. In case of the linear poly(ethylenimine, silica shells of several micrometers in thickness can be obtained and their morphology is easily controlled by a considerable number of synthesis parameters. A unique feature is the hierarchical biomimetic structure of the silica coating which surrounds the embedded carbon fiber by fibrillar and interconnected silica fine-structures. The high surface area of the nanostructured composite fiber may be exploited for catalytic applications and adsorption purposes.

Structural, optical and mechanical properties of amorphous and crystalline alumina thin films

Energy Technology Data Exchange (ETDEWEB)

Nayar, Priyanka [Department of Physics, Guru Nanak Dev University, Amritsar 143005 (India); Khanna, Atul, E-mail: akphysics@yahoo.com [Department of Physics, Guru Nanak Dev University, Amritsar 143005 (India); Kabiraj, D.; Abhilash, S.R. [Inter University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi 110067 (India); Beake, Ben D.; Losset, Yannick [Micro Materials Limited, Unit 3, Wrexham Technology Park, Wrexham LL13 7YP (United Kingdom); Chen, Banghao [Chemistry and Biochemistry Department, Florida State University, Tallahassee 32306 (United States)

2014-10-01

Thin films of amorphous alumina of thickness 350 nm were deposited on fused silica substrates by electron beam evaporation. Amorphous films were annealed at several temperatures in the range: 400–1130 °C and changes in film crystallinity, short-range structure, optical and mechanical properties were studied. X-ray diffraction studies found that crystallization starts at 800 °C and produces γ and δ-alumina, the latter phase grows with heat treatment and the sample was mostly δ and θ-alumina after annealing at 1130 °C. The as-deposited amorphous alumina films have low hardness of 5 to 8 GPa, which increases to 11 to 12 GPa in crystalline sample. {sup 27}Al Magic Angle Spinning Nuclear Magnetic Resonance was used to study the short-range order of amorphous and crystalline alumina films and it was found that amorphous alumina film contains AlO{sub 5} and AlO{sub 4} structural units in the ratio of 1:2. The concentration of AlO{sub 5} was significantly suppressed in crystalline film, which contains 48% of Al{sup 3+} ions in AlO{sub 6}, 7% in AlO{sub 5} and 45% in AlO{sub 4} units. - Highlights: • Structure–property correlations in alumina films grown by electron-beam evaporation • Amorphous films crystallize into γ and δ-alumina on annealing in air at 800 °C. • δ and θ-alumina films are stable up to 1130 °C and do not transform to α-phase. • Amorphous alumina films contain {sup [5]}Al and {sup [4]}Al structural units in the ratio of 1:2. • {sup [5]}Al decreases whereas {sup [6]}Al concentration increases on crystallization.

Patternable Poly(chloro-p-xylylene Film with Tunable Surface Wettability Prepared by Temperature and Humidity Treatment on a Polydimethylsiloxane/Silica Coating

Directory of Open Access Journals (Sweden)

Yonglian Yu

2018-03-01

Full Text Available Poly(chloro-p-xylylene (PPXC film has a water contact angle (WCA of only about 84°. It is necessary to improve its hydrophobicity to prevent liquid water droplets from corroding or electrically shorting metallic circuits of semiconductor devices, sensors, microelectronics, and so on. Herein, we reported a facile approach to improve its surface hydrophobicity by varying surface pattern structures under different temperature and relative humidity (RH conditions on a thermal curable polydimethylsiloxane (PDMS and hydrophobic silica (SiO2 nanoparticle coating. Three distinct large-scale surface patterns were obtained mainly depending on the contents of SiO2 nanoparticles. The regularity of patterns was mainly controlled by the temperature and RH conditions. By changing the pattern structures, the surface wettability of PPXC film could be improved and its WCA was increased from 84° to 168°, displaying a superhydrophobic state. Meanwhile, it could be observed that water droplets on PPXC film with superhydrophobicity were transited from a “Wenzel” state to a “Cassie” state. The PPXC film with different surface patterns of 200 μm × 200 μm and the improved surface hydrophobicity showed wide application potentials in self-cleaning, electronic engineering, micro-contact printing, cell biology, and tissue engineering.

Ceramic Composite Thin Films

Science.gov (United States)

Ruoff, Rodney S. (Inventor); Stankovich, Sasha (Inventor); Dikin, Dmitriy A. (Inventor); Nguyen, SonBinh T. (Inventor)

2013-01-01

A ceramic composite thin film or layer includes individual graphene oxide and/or electrically conductive graphene sheets dispersed in a ceramic (e.g. silica) matrix. The thin film or layer can be electrically conductive film or layer depending the amount of graphene sheets present. The composite films or layers are transparent, chemically inert and compatible with both glass and hydrophilic SiOx/silicon substrates. The composite film or layer can be produced by making a suspension of graphene oxide sheet fragments, introducing a silica-precursor or silica to the suspension to form a sol, depositing the sol on a substrate as thin film or layer, at least partially reducing the graphene oxide sheets to conductive graphene sheets, and thermally consolidating the thin film or layer to form a silica matrix in which the graphene oxide and/or graphene sheets are dispersed.

Fabrication of semi-transparent superoleophobic thin film from fabrics and nanoparticle-based hierarchical structure

Directory of Open Access Journals (Sweden)

Nishizawa S.

2013-08-01

Full Text Available Superoleophobic thin films have many potential applications including fluid transfer, fluid power systems, stain resistant and antifouling materials, and microfluidics among others. Transparency is also desired with superhydrophobicity for their numerous applications; however transparency and oleophobicity are almost incompatible relationship with each other in the point of surface structure. Because oleophobicity required rougher structure at nano-micro scale than hydrophobicity, and these rough structure brings light scattering. So far, there is very few report of the compatible of transparency and superoleophobicity. In this report, we proposed the see-through type fabrics using the nanoparticle-based hierarchical structure thin film for improving both of oleophobicity and transparency. The vacant space between fibrils of fabrics has two important roles: the one is to through the light, another one is to introduce air layer to realize Cassie state of liquid droplet on thin film. To realize the low surface energy and nanoscale rough structure surface on fibrils, we used the spray method with perfluoroalkyl methacrylic copolymer (PMC, silica nano particles and volatile solvent. From the SEM image, the hierarchical structures of nanoparticle were formed uniformly on the fabrics. The transparency of thin film obtained was approximately 61% and the change of transparency between pre-coated fabrics and coated was 11%. From investigation of the surface wettability, the contact angles of oils (rapeseed oil and hexadecane and water droplet on the fabricated film were over 150 degree.

In Situ Growth of Mesoporous Silica with Drugs on Titanium Surface and Its Biomedical Applications.

Science.gov (United States)

Wan, Mimi; Zhang, Jin; Wang, Qi; Zhan, Shuyue; Chen, Xudong; Mao, Chun; Liu, Yuhong; Shen, Jian

2017-06-07

Mesoporous silica has been developed for the modification of titanium surfaces that are used as implant materials. Yet, the traditional modification methods failed to effectively construct mesoporous silica on the titanium surface evenly and firmly, in which the interaction between mesoporous silica and titanium was mainly physical. Here, in situ growth of mesoporous silica on a titanium surface was performed using a simple evaporation-induced self-assembly strategy. Meantime, in situ introduction of drugs (heparin and vancomycin) to mesoporous silica was also adopted to improve the drug-loading amount. Both the above-mentioned processes were completed at the same time. Transmission electron microscopy, N 2 adsorption-desorption isotherms, Fourier transform infrared spectroscopy, scanning electron microscopy, and water contact angle measurements were used to characterize the structure of the mesoporous silica film. Results indicated that the mesoporous silica film that in situ grew on the titanium surface was smooth, thin, transparent, and stable. Cytotoxicity, proliferation performance of osteoblast cells, and in vitro and in vivo studies of the antibacterial activity of the coating were tested. This is the first study to modify the titanium surface by the in situ growth of a mesoporous silica coating with two kinds of drugs. The stability of the mesoporous silica coating can be attributed to the chemical bonding between dopamine and silicon hydroxyl of the mesoporous silica coating, and the smooth surface of mesoporous silica is a result of the method of in situ growth. The large amount of drug-loading also could be ascribed to the in situ introduction of drugs during the synthetic process. The strategy proposed in this work will bring more possibilities for the preparation of advanced functional materials based on the combination of mesoporous structure and metallic materials.

Hybrid silica luminescent materials based on lanthanide-containing lyotropic liquid crystal with polarized emission

Energy Technology Data Exchange (ETDEWEB)

Selivanova, N.M., E-mail: natsel@mail.ru [Kazan National Research Technological University, 68 Karl Marx Str., Kazan 420015 (Russian Federation); Vandyukov, A.E.; Gubaidullin, A.T. [A.E. Arbuzov Institute of Organic and Physical Chemistry of the Kazan Scientific Center of the Russian Academy of Sciences, 8 Acad. Arbuzov Str., Kazan 420088 (Russian Federation); Galyametdinov, Y.G. [Kazan National Research Technological University, 68 Karl Marx Str., Kazan 420015 (Russian Federation)

2014-11-14

This paper represents the template method for synthesis of hybrid silica films based on Ln-containing lyotropic liquid crystal and characterized by efficient luminescence. Luminescence films were prepared in situ by the sol–gel processes. Lyotropic liquid crystal (LLC) mesophases C{sub 12}H{sub 25}O(CH{sub 2}CH{sub 2}O){sub 10}H/Ln(NO{sub 3}){sub 3}·6H{sub 2}O/H{sub 2}O containing Ln (III) ions (Dy, Tb, Eu) were used as template. Polarized optical microscopy, X-ray powder diffraction, and FT-IR-spectroscopy were used for characterization of liquid crystal mesophases and hybrid films. The morphology of composite films was studied by the atomic force microscopy method (AFM). The optical properties of the resulting materials were evaluated. It was found that hybrid silica films demonstrate significant increase of their lifetime in comparison with an LLC system. New effects of linearly polarized emission revealed for Ln-containing hybrid silica films. Polarization in lanthanide-containing hybrid composites indicates that silica precursor causes orientation of emitting ions. - Highlights: • We suggest a new simple approach for creating luminescence hybrid silica films. • Ln-containing hybrid silica films demonstrate yellow, green and red emissions. • Tb(III)-containing hybrid film have a high lifetime. • We report effects of linearly polarized emission in hybrid film.

Effect of Addition of Colloidal Silica to Films of Polyimide, Polyvinylpyridine, Polystyrene, and Polymethylmethacrylate Nano-Composites

Directory of Open Access Journals (Sweden)

Soliman Abdalla

2016-02-01

Full Text Available Nano-composite films have been the subject of extensive work for developing the energy-storage efficiency of electrostatic capacitors. Factors such as polymer purity, nanoparticle size, and film morphology drastically affect the electrostatic efficiency of the dielectric material that forms the insulating film between the conductive electrodes of a capacitor. This in turn affects the energy storage performance of the capacitor. In the present work, we have studied the dielectric properties of four highly pure amorphous polymer films: polymethyl methacrylate (PMMA, polystyrene, polyimide and poly-4-vinylpyridine. Comparison between the dielectric properties of these polymers has revealed that the higher breakdown performance is a character of polyimide (PI and PMMA. Also, our experimental data shows that adding colloidal silica to PMMA and PI leads to a net decrease in the dielectric properties compared to the pure polymer.

Highly Aminated Mesoporous Silica Nanoparticles with Cubic Pore Structure

KAUST Repository

Suteewong, Teeraporn; Sai, Hiroaki; Cohen, Roy; Wang, Suntao; Bradbury, Michelle; Baird, Barbara; Gruner, Sol M.; Wiesner, Ulrich

2011-01-01

Mesoporous silica with cubic symmetry has attracted interest from researchers for some time. Here, we present the room temperature synthesis of mesoporous silica nanoparticles possessing cubic Pm3n symmetry with very high molar ratios (>50%) of 3-aminopropyl triethoxysilane. The synthesis is robust allowing, for example, co-condensation of organic dyes without loss of structure. By means of pore expander molecules, the pore size can be enlarged from 2.7 to 5 nm, while particle size decreases. Adding pore expander and co-condensing fluorescent dyes in the same synthesis reduces average particle size further down to 100 nm. After PEGylation, such fluorescent aminated mesoporous silica nanoparticles are spontaneously taken up by cells as demonstrated by fluorescence microscopy.

Highly Aminated Mesoporous Silica Nanoparticles with Cubic Pore Structure

KAUST Repository

Suteewong, Teeraporn

2011-01-19

Mesoporous silica with cubic symmetry has attracted interest from researchers for some time. Here, we present the room temperature synthesis of mesoporous silica nanoparticles possessing cubic Pm3n symmetry with very high molar ratios (>50%) of 3-aminopropyl triethoxysilane. The synthesis is robust allowing, for example, co-condensation of organic dyes without loss of structure. By means of pore expander molecules, the pore size can be enlarged from 2.7 to 5 nm, while particle size decreases. Adding pore expander and co-condensing fluorescent dyes in the same synthesis reduces average particle size further down to 100 nm. After PEGylation, such fluorescent aminated mesoporous silica nanoparticles are spontaneously taken up by cells as demonstrated by fluorescence microscopy.

In situ crystallization of b-oriented MFI films on plane and curved substrates coated with a mesoporous silica layer

KAUST Repository

Deng, Zhiyong

2013-05-01

A simple and reproducible method is presented for preparing b-oriented MFI films on plane (disc) and curved (hollow fiber) supports by in situ hydrothermal synthesis. A mesoporous silica (sub-)layer was pre-coated on the supports by dip coating followed by a rapid thermal calcination step (973 K during 1 min) to reduce the number of grain boundaries while keeping the hydrophilic behavior of silica. The role of the silica sub-layer is not only to smoothen the substrate surface, but also to provide a silica source to promote the nucleation and growth of zeolite crystals via a heterogeneous nucleation mechanism (zeolitization), and adsorb zeolite moieties generated in the synthesis solution via a homogeneous nucleation mechanism. A monolayer of b-oriented MFI crystals was obtained on both supports after 3 h synthesis time with a moderate degree of twinning on the surface. © 2013 Elsevier Ltd.

Facile and tunable synthesis of hierarchical mesoporous silica materials ranging from flower structure with wrinkled edges to hollow structure with coarse surface

Energy Technology Data Exchange (ETDEWEB)

Hao, Nanjing, E-mail: nanjing.hao@dartmouth.edu [Dartmouth College, Thayer School of Engineering (United States); Li, Laifeng; Tang, Fangqiong, E-mail: tangfq@mail.ipc.ac.cn [Chinese Academy of Sciences, Technical Institute of Physics and Chemistry (China)

2016-11-15

Mesoporous silica materials have attracted great attention in many fields. However, facile and tunable synthesis of hierarchical mesoporous silica structures is still a big challenge, and thus the development of them still lags behind. Herein, well-defined mesoporous silica flower structure with wrinkled edges and mesoporous silica hollow structure with coarse surface were synthesized simply by using poly(vinylpyrrolidone) and hexadecylamine as cotemplates in different water/ethanol solvent systems. The shape evolution from flower to hollow can be easily realized by tuning the volume ratio of water to ethanol, and the yields of both materials can reach gram scale. The formation mechanisms of mesoporous silica flower and hollow structures were also experimentally investigated and discussed. These novel hierarchical structures having unique physicochemical properties may bring many interesting insights into scientific research and technological application.

Facile fabrication of superhydrophobic films with fractal structures using epoxy resin microspheres

Energy Technology Data Exchange (ETDEWEB)

Quan, Yun-Yun; Zhang, Li-Zhi, E-mail: lzzhang@scut.edu.cn

2014-02-15

A simple method has been developed to fabricate superhydrophobic surfaces with fractal structures with epoxy resin microspheres (ERMs). The ERMs is produced by phase separation in an epoxy-amine curing system with a silica sol (SS) dispersant. The transparent epoxy solution becomes cloudy and turns into epoxy suspension (ES) in this process. The fractal structure (two tier structure) generated by synthetic epoxy resin microspheres (ERMs) and deposited nanoincrutations on the surfaces of these ERMs, which have been observed by scanning electron microscope (SEM). The curing time of ES is an important condition to obtain films with good comprehensive performances. Superhydrophobic films can be prepared by adding extra SS into ES with a curing time longer than 5 h. The optimal curing time is 10 h to fabricate a film with good mechanical stability and high superhydrophobicity. In addition, a surface with anti-wetting property of impacting microdroplets can be fabricated by prolonging the curing time of ES to 24 h. The gradually decreased hydrophilic groups resulted from a longer curing time enable the surface to have smaller surface adhesions to water droplets, which is the main reason to keep its superhydrophobicity under impacting conditions. The coated surface is highly hydrophobic and the impacting water droplets are bounced off from the surface.

Facile fabrication of superhydrophobic films with fractal structures using epoxy resin microspheres

Science.gov (United States)

Quan, Yun-Yun; Zhang, Li-Zhi

2014-02-01

A simple method has been developed to fabricate superhydrophobic surfaces with fractal structures with epoxy resin microspheres (ERMs). The ERMs is produced by phase separation in an epoxy-amine curing system with a silica sol (SS) dispersant. The transparent epoxy solution becomes cloudy and turns into epoxy suspension (ES) in this process. The fractal structure (two tier structure) generated by synthetic epoxy resin microspheres (ERMs) and deposited nanoincrutations on the surfaces of these ERMs, which have been observed by scanning electron microscope (SEM). The curing time of ES is an important condition to obtain films with good comprehensive performances. Superhydrophobic films can be prepared by adding extra SS into ES with a curing time longer than 5 h. The optimal curing time is 10 h to fabricate a film with good mechanical stability and high superhydrophobicity. In addition, a surface with anti-wetting property of impacting microdroplets can be fabricated by prolonging the curing time of ES to 24 h. The gradually decreased hydrophilic groups resulted from a longer curing time enable the surface to have smaller surface adhesions to water droplets, which is the main reason to keep its superhydrophobicity under impacting conditions. The coated surface is highly hydrophobic and the impacting water droplets are bounced off from the surface.

Luminescent hybrid films obtained by covalent grafting of terbium complex to silica network

International Nuclear Information System (INIS)

Liu Fengyi; Fu Lianshe; Wang Jun; Liu Ze; Li Huanrong; Zhang Hongjie

2002-01-01

Luminescent hybrid thin films consisting of terbium complex covalently bonded to a silica-based network have been obtained in situ via a sol-gel approach. A new monomer, N-(4-benzoic acid-yl), N'-(propyltriethoxysilyl)urea (PABI), has been synthesized by grafting isocyanatopropyltriethoxysilane (ICPTES) to p-aminobenzoic acid and characterized by 1 H NMR, IR and MS. The monomer acts as a ligand for Tb 3+ ion and as a sol-gel precursor. Band emission from Tb 3+ ion due to an efficient ligand-to-metal energy transfer was observed by UV excitation. The decay curves of Tb 3+ in the hybrid films were measured. The energy difference between the triplet state energy of PABI and the 5 D 4 level of Tb 3+ ion falls in the exciting range to sensitize Tb 3+ ion fluorescence

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.

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.

Preparation and characterization of silica/fluorinated acrylate copolymers hybrid films and the investigation of their icephobicity

International Nuclear Information System (INIS)

Huang Yanfen; Hu Mingjie; Yi Shengping; Liu Xinghai; Li Houbin; Huang Chi; Luo Yunbai; Li Yan

2012-01-01

Inexpensive hydrophobic and icephobic coatings and films were obtained by a simple method. These coatings were prepared by mixing silica sol and fluorinated acrylate copolymers. There was a phase separation process in the film-forming which can provide the excellent performance. Small amount (about 2 wt.%) of fluorinated (methyl) acrylate was used in all of these coatings. The coatings were eco-friendly by using ethanol as the solvent system. Scanning electron microscopy, atomic force microscope, energy dispersive X-ray fluorescence spectrometer, water contact angle, thermal gravimetric analysis and tests of adhesion and hardness had been performed to characterize the morphological feature, chemical composition, hydrophobicity and icephobicity of the surface, thermal stability and mechanical properties of the coatings. The results showed that the films had good hydrophobicity, high thermal stability and excellent mechanical properties of adhesion strength and pencil hardness. Furthermore, by testing their properties of delaying water droplet from icing, it was found that ice formation was delayed for 90 min compared with the glass surface at − 5.6 °C. The hybrid coatings may be suitable for large-scale and practical application owing to its flexibility and simplicity. - Highlights: ► Coatings were prepared by mixing fluorinated acrylate copolymer and silica. ► Mechanical properties and anti-icing performance of the coatings were examined. ► Water contact angle increased with raising SiO 2 (sol)/monomers weight ratio. ► Ice formation was delayed for 90 min at − 5.6 °C.

The Structure and Properties of Silica Glass Nanostructures using Novel Computational Systems

Science.gov (United States)

Doblack, Benjamin N.

The structure and properties of silica glass nanostructures are examined using computational methods in this work. Standard synthesis methods of silica and its associated material properties are first discussed in brief. A review of prior experiments on this amorphous material is also presented. Background and methodology for the simulation of mechanical tests on amorphous bulk silica and nanostructures are later presented. A new computational system for the accurate and fast simulation of silica glass is also presented, using an appropriate interatomic potential for this material within the open-source molecular dynamics computer program LAMMPS. This alternative computational method uses modern graphics processors, Nvidia CUDA technology and specialized scientific codes to overcome processing speed barriers common to traditional computing methods. In conjunction with a virtual reality system used to model select materials, this enhancement allows the addition of accelerated molecular dynamics simulation capability. The motivation is to provide a novel research environment which simultaneously allows visualization, simulation, modeling and analysis. The research goal of this project is to investigate the structure and size dependent mechanical properties of silica glass nanohelical structures under tensile MD conditions using the innovative computational system. Specifically, silica nanoribbons and nanosprings are evaluated which revealed unique size dependent elastic moduli when compared to the bulk material. For the nanoribbons, the tensile behavior differed widely between the models simulated, with distinct characteristic extended elastic regions. In the case of the nanosprings simulated, more clear trends are observed. In particular, larger nanospring wire cross-sectional radii (r) lead to larger Young's moduli, while larger helical diameters (2R) resulted in smaller Young's moduli. Structural transformations and theoretical models are also analyzed to identify

Mesoporous Structure Control of Silica in Room-Temperature Synthesis under Basic Conditions

Directory of Open Access Journals (Sweden)

Jeong Wook Seo

2015-01-01

Full Text Available Various types of mesoporous silica, such as continuous cubic-phase MCM-48, hexagonal-phase MCM-41, and layer-phase spherical silica particles, have been synthesized at room temperature using cetyltrimethylammonium bromide as a surfactant, ethanol as a cosurfactant, tetraethyl orthosilicate as a silica precursor, and ammonia as a condensation agent. Special care must be taken both in the filtering of the resultant solid products and in the drying process. In the drying process, further condensation of the silica after filtering was induced. As the surfactant and cosurfactant concentrations in the reaction mixture increased and the NH3 concentration decreased, under given conditions, continuous cubic MCM-48 and layered silica became the dominant phases. A cooperative synthesis mechanism, in which both the surfactant and silica were involved in the formation of mesoporous structures, provided a good explanation of the experimental results.

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.

Silica-Coated Liposomes for Insulin Delivery

OpenAIRE

Neelam Dwivedi; M. A. Arunagirinathan; Somesh Sharma; Jayesh Bellare

2010-01-01

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 evid...

Two-dimensional silica: Structural, mechanical properties, and strain-induced band gap tuning

Energy Technology Data Exchange (ETDEWEB)

Gao, Enlai; Xie, Bo [Applied Mechanics Laboratory, Department of Engineering Mechanics, and Center for Nano and Micro Mechanics, Tsinghua University, Beijing 100084 (China); Xu, Zhiping, E-mail: xuzp@tsinghua.edu.cn [Applied Mechanics Laboratory, Department of Engineering Mechanics, and Center for Nano and Micro Mechanics, Tsinghua University, Beijing 100084 (China); State Key Laboratory of Mechanics and Control of Mechanical Structures, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China)

2016-01-07

Two-dimensional silica is of rising interests not only for its practical applications as insulating layers in nanoelectronics, but also as a model material to understand crystals and glasses. In this study, we examine structural and electronic properties of hexagonal and haeckelite phases of silica bilayers by performing first-principles calculations. We find that the corner-sharing SiO{sub 4} tetrahedrons in these two phases are locally similar. The robustness and resilience of these tetrahedrons under mechanical perturbation allow effective strain engineering of the electronic structures with band gaps covering a very wide range, from of that for insulators, to wide-, and even narrow-gap semiconductors. These findings suggest that the flexible 2D silica holds great promises in developing nanoelectronic devices with strain-tunable performance, and lay the ground for the understanding of crystalline and vitreous phases in 2D, where bilayer silica provides an ideal test-bed.

Molecular Structure and Dynamics in Thin Water Films at the Silica and Graphite Surfaces

Energy Technology Data Exchange (ETDEWEB)

Argyris, Dr. Dimitrios [University of Oklahoma; Tummala, Dr. Naga Rajesh [University of Oklahoma; StrioloDr., A [Vanderbilt University; Cole, David R [ORNL

2008-01-01

The structure and dynamic properties of interfacial water at the graphite and silica solid surfaces were investigated using molecular dynamics simulations. The effect of surface properties on the characteristics of interfacial water was quantified by computing density profiles, radial distribution functions, surface density distributions, orientation order parameters, and residence and reorientation correlation functions. In brief, our results show that the surface roughness, chemical heterogeneity, and surface heterogeneous charge distribution affect the structural and dynamic properties of the interfacial water molecules, as well as their rate of exchange with bulk water. Most importantly, our results indicate the formation of two distinct water layers at the SiO2 surface covered by a large density of hydroxyl groups. Further analysis of the data suggests a highly confined first layer where the water molecules assume preferential hydrogen-down orientation and a second layer whose behavior and characteristics are highly dependent on those of the first layer through a well-organized hydrogen bond network. The results suggest that water-water interactions, in particular hydrogen bonds, may be largely responsible for macroscopic interfacial properties such as adsorption and contact angle.

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.

Effect of adjustable molecular chain structure and pure silica zeolite nanoparticles on thermal, mechanical, dielectric, UV-shielding and hydrophobic properties of fluorinated copolyimide composites

Science.gov (United States)

Li, Qing; Liao, Guangfu; Zhang, Shulai; Pang, Long; Tong, Hao; Zhao, Wenzhe; Xu, Zushun

2018-01-01

A series of polyimide (PI) films, polyimide/pure silica zeolite nanoparticles (PSZN) blend films and polyimide/amine-functionalized pure silica zeolite nanoparticles (APSZN) composite films were successfully prepared by random copolycondensation. Thereinto, PSZN were synthesized by hydrothermal method. The polyimides were derived from 4,4‧-diaminodiphenyl ether (ODA), and three adjustable molar ratios (3:1, 1:1, 1:3) of 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl] propane dianhydride (BPADA) and 4,4‧-(hexafluoroisopropylidene) diphthalic anhydride (6FDA). The effects of PSZN, APSZN and different chain structure on PI films were specifically evaluated in terms of morphology, thermal, mechanical, dielectric and UV-shielding properties, etc. Comparison was given among pure PI flims, PI/PSZN blend films and PI/APSZN composite flims. The results showed that the thermal and mechanical properties of PI films were drastically impaired after adding PSZN. On the contrary, the strength, toughness and thermal stability were improved after adding APSZN. Moreover, the dielectric constants of the PI/APSZN composite flims were lowered but UV-shielding properties were enhanced. Interestingly, we found that the greatest effects were obtained through introducing APSZN in PI derived by the 1:1 ratio of BPADA:6FDA. The corresponding PI/APSZN composite flim exhibited the most reinforced and toughened properties, the largest decrement of dielectric constant and the best UV-shielding efficiency, which made the composite flim be used as ultraviolet shielding material in outer space filled with high temperature and intensive ultraviolet light. Meanwhile, this work also provided a facile way to synthesize composite materials with adjustable performance.

Metal induced crystallization of amorphous silicon thin films studied by x-ray absorption fine structure spectroscopy

International Nuclear Information System (INIS)

Naidu, K Lakshun; Mohiddon, Md Ahamad; Dalba, G; Krishna, M Ghanashyam; Rocca, F

2013-01-01

The role of thin metallic layer (Chromium or Nickel) in the crystallization of a-Si film has been studied using X-ray absorption fine structure spectroscopy (XAFS). The films were grown at different substrate temperatures in two different geometrical structures : (a) a 200 nm metal layer (Cr or Ni) was deposited on fused silica (FS) followed by 400 nm of a-Si and (b) the 400 nm a-Si layer was deposited on FS followed by 200 nm of metal layer. XAFS measurements at Cr K-edge and Ni K-edge were done at BM08 – GILDA beamline of the European Synchrotron Research Facility (ESRF, Grenoble, F) in fluorescence mode. To understand the evolution of the local structure of Cr/Ni diffusing from bottom to top and from top to bottom, total reflection and higher incidence angles were employed. The relative content of metal, metal oxide and metal silicides compounds on the upper surface and/or in the bulk of different films has been evaluated as a function of thermal treatment.

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.

Synthesis of Novel Mesoporous Silica Materials with Hierarchical Pore Structures

Energy Technology Data Exchange (ETDEWEB)

Yoon, Suk Bon; Choi, Wang Kyu; Choi, Byung Seon; Moon, Jei Kwon [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2012-05-15

Porous materials with various pore sizes in the range of micropore (< 2 nm), mesopore (2-50 nm), and macropore (> 50 nm) are attractive due to their many emerging applications such as catalysts, separation systems, and low dielectric constant materials. The discovery of new M41S mesoporous silica families with pore sizes larger than 2 nm in diameter in 1992 extended the applications into much wider pore ranges, bringing in a new prosperous era in porous material research. The synthesis of these silica materials has been mainly accomplished through a self-assembly between surfactant molecules and inorganic species under various pH conditions. Recently, core-shell nanoparticles with a silica core and mesoporous shell under basic conditions were synthesized using the silica nanoparticles as a core, and a silica precursor (TEOS) and cationic surfactant (CTABr) as a material for the formation of the mesoporous shell. The resultant materials were very monodispersive in size and showed a narrow pore size distribution in the range of ca 2-3 nm in diameter, depending on the alkyl-chain length of the surfactants used. In this work, the mesoporous shell coated-fumed silicas (denoted as MS M-5s) were synthesized by using fumed silica instead of the silica nanoparticle as a core based on previous reports. Also, the structural properties of the MS M-5s such as the specific surface area and pore volume were easily controlled by varying the amount of the silica precursor and surfactant. The resultant materials exhibited a BET surface area of ca 279-446 m{sup 2}/g and total pore volume of ca 0.64-0.74 cm{sup 3}/g and showed a narrow pore size distribution (PSD) due to the removal of the organic surfactant molecules

Effects of Silica Nanostructures in Poly(ethylene oxide)-Based Composite Polymer Electrolytes.

Science.gov (United States)

Mohanta, Jagdeep; Anwar, Shahid; Si, Satyabrata

2016-06-01

The present work describes the synthesis of some poly(ethylene oxide)-based nanocomposite polymer electrolyte films using various silica nanostructures as the inorganic filler by simple solution mixing technique, in which the nature of the silica nanostructures play a vital role in modulating their electrochemical performances at room temperature. The silica nanostructures are prepared by ammonical hydrolysis of tetraethyl orthosilicate following the modified St6ber method. The resulting films are characterized by X-ray diffraction and differential scanning calorimeter to study their crystallinity. Room temperature AC impedance spectroscopy is utilized to determine the Li+ ion conductivity of the resulting films. The observed conductivity values of various NCPE films depend on the nature of silica filling as well as on their surface characteristics and also on the varying PEO-Li+ ratio, which is observed to be in the order of 10(-7)-10(-6) S cm(-1).

Structural characterization of ZnO thin films grown on various substrates by pulsed laser deposition

International Nuclear Information System (INIS)

Novotný, M; Bulíř, J; Lančok, J; Čížek, J; Kužel, R; Connolly, J; McCarthy, E; Krishnamurthy, S; Mosnier, J-P; Anwand, W; Brauer, G

2012-01-01

ZnO thin films were grown by pulsed laser deposition on three different substrates: sapphire (0 0 0 1), MgO (1 0 0) and fused silica (FS). The structure and morphology of the films were characterized by x-ray diffraction and scanning electron microscopy and defect studies were carried out using slow positron implantation spectroscopy (SPIS). Films deposited on all substrates studied in this work exhibit the wurtzite ZnO structure and are characterized by an average crystallite size of 20-100 nm. However, strong differences in the microstructure of films deposited on various substrates were found. The ZnO films deposited on MgO and sapphire single-crystalline substrates exhibit local epitaxy, i.e. a well-defined relation between film crystallites and the substrate. Domains with different orientation relationships with the substrate were found in both films. On the other hand, the film deposited on the FS substrate exhibits fibre texture with random lateral orientation of crystallites. Extremely high compressive in-plane stress of σ ∼ 14 GPa was determined in the film deposited on the MgO substrate, while the film deposited on sapphire is virtually stress-free, and the film deposited on the FS substrate exhibits a tensile in-plane stress of σ ∼ 0.9 GPa. SPIS investigations revealed that the concentration of open-volume defects in the ZnO films is substantially higher than that in a bulk ZnO single crystal. Moreover, the ZnO films deposited on MgO and sapphire single-crystalline substrates exhibit a significantly higher density of defects than the film deposited on the amorphous FS substrate. (paper)

Influence of Nano Silica on Alkyd Films

DEFF Research Database (Denmark)

Nikolic, Miroslav

. The present work centers on the reinforcement of alkyd binders emulsified in water and used in exterior wood coatings with nano silica. Raman spectroscopy was used throughout the study to maintain the reproducibility of results as it was found that colloidal nano silica can increase or decrease the speed...... of alkyd curing affecting the tested mechanical properties. Hydrophilic, colloidal nano silica was seen to have limited effect in improving the mechanical properties due to problems in properly dispersing and attaining good surface interactions with the hydrophobic alkyd polymer. Efforts in increasing...... the interactions with the alkyd polymer while keeping the nano filler stable in the water phase did not show further improvements of mechanical properties. The best results in respect to mechanical properties, as measured under static and dynamic loading, were obtained with the use of hexamethyldisilazane treated...

Diffusion structural analysis study of titania films deposited by sol-gel technique on silica glass

Czech Academy of Sciences Publication Activity Database

Balek, V.; Mitsuhashi, T.; Bountseva, I.M.; Haneda, H.; Málek, Z.; Šubrt, Jan

2003-01-01

Roč. 26, 1-3 (2003), s. 185-189 ISSN 0928-0707. [International Workshop on Glasses, Ceramics, Hybrids and Nanocomposites from Gels /11./. Abano Terme, 16.09.2001-21.09.2001] Institutional research plan: CEZ:AV0Z4032918 Keywords : titania film * diffusion structural analysis * sol-gel Subject RIV: CA - Inorganic Chemistry Impact factor: 1.546, year: 2003

Fractal Structures on Silica Aerogels Containing Titanium: A Small Angle Neutron Scattering Study

International Nuclear Information System (INIS)

Widya Sari; Dian Fitriyani; Abdul Aziz Mohamed; Noordin Ibrahim

2009-01-01

Full text: The fractal structure of silica aerogels containing titanium has been investigated by means of small-angle neutron scattering (SANS) technique. The SANS experiments were conducted using a 36 meter SANS BATAN spectrometer (SMARTer) in Serpong, Indonesia in the range of momentum transfer Q, 0.006 -1 ) < 0.3. The power-law for a fractal object scattering Q-D observed from all measured samples. The Fourier transform of pattern I(Q) a pair correlation model function was implemented in analyzing the structure factor from the power-law scattering profiles. The results are showing that the silica aerogels containing titanium has a mass fractal where its dimension DM is larger than the pure silica aerogels. The mass fractal dimension of silica aerogels containing titanium is relatively constant between 2.23 to 2.40 with the decrease of acid concentrations during a sol-gel process and formed a nanometer size of aggregate. Those fractal structures were simulated using a Delphi language and the results are presented in this paper. (author)

Plasma Polymerization of Acetylene onto silica: and Approach to control the distribution of silica in single elastomers and immiscible blends

NARCIS (Netherlands)

Tiwari, M.; Noordermeer, Jacobus W.M.; Ooij, W.J.; Dierkes, Wilma K.

2008-01-01

Surface modification of silica by acetylene plasma polymerization is applied in order to improve the dispersion in and compatibility with single rubbers and their blends. Silica, used as a reinforcing filler for elastomers, is coated with a polyacetylene (PA) film under vacuum conditions. Water

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....

Study of the structure of 3D-ordered macroporous GaN-ZnS:Mn nanocomposite films

Energy Technology Data Exchange (ETDEWEB)

Kurdyukov, D. A., E-mail: kurd@gvg.ioffe.ru; Shishkin, I. I.; Grudinkin, S. A.; Sitnikova, A. A.; Zamoryanskaya, M. V.; Golubev, V. G. [Russian Academy of Sciences, Ioffe Physical-Technical Institute (Russian Federation)

2015-05-15

A film-type 3D-ordered macroporous GaN-ZnS:Mn nanocomposite with the structure of an inverted opal is fabricated. Structural studies of the nanocomposite are performed, and it is shown that GaN and ZnS:Mn introduced into the pores of the silica opal are nanocrystallites misoriented with respect to each other. It is shown that the nanocomposite is a structurally perfect 3D photonic crystal. The efficiency of using a buffer of GaN crystallites to preclude interaction between the surface of the spherical a-SiO{sub 2} particles forming the opal matrix and chemically active substances introduced into the pores is demonstrated.

Solvothermal growth of a ruthenium metal-organic framework featuring HKUST-1 structure type as thin films on oxide surfaces.

Science.gov (United States)

Kozachuk, Olesia; Yusenko, Kirill; Noei, Heshmat; Wang, Yuemin; Walleck, Stephan; Glaser, Thorsten; Fischer, Roland A

2011-08-14

Phase-pure crystalline thin films of a mixed-valence Ru(2)(II,III) metal-organic framework with 1,3,5-benzenetricarboxylate (btc) as a linker were solvothermally grown on amorphous alumina and silica surfaces. Based on the Rietveld refinement, the structure of Ru-MOF was assigned to be analogous to [Cu(3)(btc)(2)] (HKUST-1). This journal is © The Royal Society of Chemistry 2011

Structural and Luminescence Properties of Lu2O3:Eu3+ F127 Tri-Block Copolymer Modified Thin Films Prepared by Sol-Gel Method

Science.gov (United States)

de Jesus Morales Ramírez, Angel; Hernández, Margarita García; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Palmerin, Joel Moreno; Velazquez, Dulce Yolotzin Medina; Jota, María Luz Carrera

2013-01-01

Lu2O3:Eu3+ transparent, high density, and optical quality thin films were prepared using the sol-gel dip-coating technique, starting with lutetium and europium nitrates as precursors and followed by hydrolysis in an ethanol-ethylene glycol solution. Acetic acid and acetylacetonate were incorporated in order to adjust pH and as a sol stabilizer. In order to increment the thickness of the films and orient the structure, F127 Pluronic acid was incorporated during the sol formation. Structural, morphological, and optical properties of the films were investigated for different F127/Lu molar ratios (0–5) in order to obtain high optical quality films with enhanced thickness compared with the traditional method. X-ray diffraction (XRD) shows that the films present a highly oriented cubic structure beyond 1073 K for a 3-layer film, on silica glass substrates. The thickness, density, porosity, and refractive index evolution of the films were investigated by means of m-lines microscopy along with the morphology by scanning electron microscope (SEM) and luminescent properties. PMID:28809336

Experimental collaboration for thick concrete structures with alkali-silica reaction

Science.gov (United States)

Ezell, N. Dianne Bull; Hayes, Nolan; Lenarduzzi, Roberto; Clayton, Dwight; Ma, Z. John; Le Pape, Sihem; Le Pape, Yann

2018-04-01

Alkali-Silica Reaction (ASR) is a reaction that occurs over time in concrete between alkaline cement paste and reactive, non-crystalline silica in aggregates. An expansive gel is formed within the aggregates which results in micro-cracks in aggregates and adjacent cement paste. The reaction requires the presence of water and has been predominantly detected in groundwater-impacted portions of below grade structures, with limited impact to exterior surfaces in above grade structures. ASR can potentially affect concrete properties and performance characteristics such as compressive strength, modulus of elasticity, shear strength, and tensile strength. Since ASR degradation often takes significant amounts of time, developing ASR detection techniques is important to the sustainability and extended operation lifetimes of nuclear power plants (NPPs). The University of Tennessee, Knoxville (UTK) in collaboration with Oak Ridge National Laboratory (ORNL) designed and built an experiment representative of typical NPP structures to study ASR in thick concrete structures.

Mesoporous silicas with covalently immobilized β-cyclodextrin moieties: synthesis, structure, and sorption properties

Science.gov (United States)

Roik, Nadiia V.; Belyakova, Lyudmila A.; Trofymchuk, Iryna M.; Dziazko, Marina O.; Oranska, Olena I.

2017-09-01

Mesoporous silicas with chemically attached macrocyclic moieties were successfully prepared by sol-gel condensation of tetraethyl orthosilicate and β-cyclodextrin-silane in the presence of a structure-directing agent. Introduction of β-cyclodextrin groups into the silica framework was confirmed by the results of IR spectral, thermogravimetric, and quantitative chemical analysis of surface compounds. The porous structure of the obtained materials was characterized by nitrogen adsorption-desorption measurements, powder X-ray diffraction, transmission electron microscopy, and dynamic light scattering. It was found that the composition of the reaction mixture used in β-cyclodextrin-silane synthesis significantly affects the structural parameters of the resulting silicas. The increase in (3-aminopropyl)triethoxysilane as well as the coupling agent content in relation to β-cyclodextrin leads ultimately to the lowering or complete loss of hexagonal arrangement of pore channels in the synthesized materials. Formation of hexagonally ordered mesoporous structure was observed at molar composition of the mixture 0.049 TEOS:0.001 β-CD-silane:0.007 CTMAB:0.27 NH4OH:7.2 H2O and equimolar ratio of components in β-CD-silane synthesis. The sorption of alizarin yellow on starting silica and synthesized materials with chemically attached β-cyclodextrin moieties was studied in phosphate buffer solutions with pH 7.0. Experimental results of the dye equilibrium sorption were analyzed using Langmuir, Freundlich, and Redlich-Peterson isotherm models. It was proved that the Redlich-Peterson isotherm model is the most appropriate for fitting the equilibrium sorption of alizarin yellow on parent silica with hexagonally arranged mesoporous structure as well as on modified one with chemically immobilized β-cyclodextrin groups. [Figure not available: see fulltext.

Preparation of novel film-forming armoured latexes using silica nanoparticles as a pickering emulsion stabiliser.

Science.gov (United States)

Shiraz, Hana; Peake, Simon J; Davey, Tim; Cameron, Neil R; Tabor, Rico F

2018-05-15

Film-forming polymer latex particles of diameter acrylate (BA) as co-monomers, potassium persulphate (KPS) as an initiator and a commercially available colloidal nano-silica (Ludox®-TM40). It was found that pH control before polymerisation using methacrylic acid (MAA) facilitated the formation of armoured latexes, and mechanistic features of this process are discussed. An alternative, more robust protocol was developed whereby addition of vinyltriethoxysilane (VTES) to control wettability resulted in latexes completely armoured in colloidal nano-silica. The latexes were characterised using SEM, cryo-TEM and AFM imaging techniques. The mechanism behind the adsorption was investigated through surface pressure and contact angle measurements to understand the factors that influence this irreversible adsorption. Results indicate that nanoparticle attachment (but intriguingly not latex size) is dependent on particle wettability, providing new insight into the formation of nanoparticle-armoured latexes, along with opportunities for further development of diversely functionalized inorganic/organic polymer composite particles. Copyright © 2018 Elsevier Inc. All rights reserved.

Structural effect of monomer type on properties of copolyimides and copolyimide-silica hybrid materials

Directory of Open Access Journals (Sweden)

Kizilkaya Canan

2015-01-01

Full Text Available In this work, the effect of two different diamine monomers, containing phosphine oxide, on thermal, mechanical and morphological properties of copolyimides and their hybrid materials was investigated. Gas separation properties of the synthesized copolyimides were also analysed. Two different diamine monomers with phosphine oxide were bis(3-aminophenyl phenylphosphine oxide (BAPPO and bis(3-aminophenoxy-4-phenyl phenylphosphine oxide (m-BAPPO. In the synthesis of copolyimides 3,3’-diamino-diphenyl sulfone (DDS was also used as the diamine, as well as 2,2’-bis(3,4-dicarboxyphenylhexafluoropropane dianhydride (6FDA. Copolyimide films were prepared by thermal imidization. Hybrid materials containing 5 % SiO2 were synthesised further by sol-gel technique. The Fourier-transform infrared spectroscopy (FTIR, Nuclear magnetic resonance spectroscopy (NMR confirmed the expected structure. Dynamic mechanical analysis (DMA demonstrated that m-BAPPO based copolyimides had lower glass transition temperatures (Tg than BAPPO based copolyimides. m-BAPPO containing copolyimide without silica shifted the thermal decomposition temperature to a higher value. The moduli and strength values of BAPPO diamine containing copolyimide and its hybrid were higher than those of m-BAPPO containing materials. The contact angle measurements showed the hydrophobicity. Scanning electron microscope (SEM analysis exhibited the silica particles dispersion in the copolyimides. These copolyimides may be used in the coating industry. The CO2 permeability and the permselectivity were the highest among the other values in this study, when m-BAPPO containing copolyimide in the absence of silica was used. The gas permeabilities obtained from this work were in this decreasing order: PCO2 > PO2 > PN2.

Engineering the internal structure of magnetic silica nanoparticles by thermal control

KAUST Repository

Song, Hyon Min

2014-09-30

Calcination of hydrated iron salts in the pores of both spherical and rod-shaped mesoporous silica nanoparticles (NPs) changes the internal structure from an ordered 2D hexagonal structure into a smaller number of large voids in the particles with sizes ranging from large hollow cores down to ten nanometer voids. The voids only form when the heating rate is rapid at a rate of 30 °C min-1. The sizes of the voids are controlled reproducibly by the final calcination temperature; as the temperature is decreased the number of voids decreases as their size increases. The phase of the iron oxide NPs is α-Fe2O3 when annealed at 500 °C, and Fe3O4 when annealed at lower temperatures. The water molecules in the hydrated iron (III) chloride precursor salts appear to play important roles by hydrolyzing Si-O-Si bonding, and the resulting silanol is mobile enough to affect the reconstruction into the framed hollow structures at high temperature. Along with hexahydrates, trivalent Fe3+ ions are assumed to contribute to the structure disruption of mesoporous silica by replacing tetrahedral Si4+ ions and making Fe-O-Si bonding. Volume fraction tomography images generated from transmission electron microscopy (TEM) images enable precise visualization of the structures. These results provide a controllable method of engineering the internal shapes in silica matrices containing superparamagnetic NPs.

Engineering the internal structure of magnetic silica nanoparticles by thermal control

KAUST Repository

Song, Hyon Min; Zink, Jeffrey I.; Khashab, Niveen M.

2014-01-01

Calcination of hydrated iron salts in the pores of both spherical and rod-shaped mesoporous silica nanoparticles (NPs) changes the internal structure from an ordered 2D hexagonal structure into a smaller number of large voids in the particles with sizes ranging from large hollow cores down to ten nanometer voids. The voids only form when the heating rate is rapid at a rate of 30 °C min-1. The sizes of the voids are controlled reproducibly by the final calcination temperature; as the temperature is decreased the number of voids decreases as their size increases. The phase of the iron oxide NPs is α-Fe2O3 when annealed at 500 °C, and Fe3O4 when annealed at lower temperatures. The water molecules in the hydrated iron (III) chloride precursor salts appear to play important roles by hydrolyzing Si-O-Si bonding, and the resulting silanol is mobile enough to affect the reconstruction into the framed hollow structures at high temperature. Along with hexahydrates, trivalent Fe3+ ions are assumed to contribute to the structure disruption of mesoporous silica by replacing tetrahedral Si4+ ions and making Fe-O-Si bonding. Volume fraction tomography images generated from transmission electron microscopy (TEM) images enable precise visualization of the structures. These results provide a controllable method of engineering the internal shapes in silica matrices containing superparamagnetic NPs.

Sol-gel preparation of Ag-silica nanocomposite with high electrical conductivity

Science.gov (United States)

Ma, Zhijun; Jiang, Yuwei; Xiao, Huisi; Jiang, Bofan; Zhang, Hao; Peng, Mingying; Dong, Guoping; Yu, Xiang; Yang, Jian

2018-04-01

Sol-gel derived noble-metal-silica nanocomposites are very useful in many applications. Due to relatively low price, higher conductivity, and higher chemical stability of silver (Ag) compared with copper (Cu), Ag-silica has gained much more research interest. However, it remains a significant challenge to realize high loading of Ag content in sol-gel Ag-silica composite with high structural controllability and nanoparticles' dispersity. Different from previous works by using multifunctional silicon alkoxide to anchor metal ions, here we report the synthesis of Ag-silica nanocomposite with high loading of Ag nanoparticles by employing acetonitrile bi-functionally as solvent and metal ions stabilizer. The electrical conductivity of the Ag-silica nanocomposite reached higher than 6800 S/cm. In addition, the Ag-silica nanocomposite could simultaneously possess high electrical conductivity and positive conductivity-temperature coefficient by properly controlling the loading content of Ag. Such behavior is potentially advantageous for high-temperature devices (like phosphoric acid fuel cells) and inhibiting the thermal-induced increase of devices' internal resistance. The strategy proposed here is also compatible with block-copolymer directed self-assembly of mesoporous material, spin-coating of film and electrospinning of nanofiber, making it more charming in various practical applications.

Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials.

Science.gov (United States)

Hesemann, Peter; Nguyen, Thy Phung; Hankari, Samir El

2014-04-11

The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS) recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA), mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the "anionic templating" strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches.

Basic evaluation of typical nanoporous silica nanoparticles in being drug carrier: Structure, wettability and hemolysis.

Science.gov (United States)

Li, Jing; Guo, Yingyu

2017-04-01

Herein, the present work devoted to study the basic capacity of nanoporous silica nanoparticles in being drug carrier that covered structure, wettability and hemolysis so as to provide crucial evaluation. Typical nanoporous silica nanoparticles that consist of nanoporous silica nanoparticles (NSN), amino modified nanoporous silica nanoparticles (amino-NSN), carboxyl modified nanoporous silica nanoparticles (carboxyl-NSN) and hierachical nanoporous silica nanoparticles (hierachical-NSN) were studied. The results showed that their wettability and hemolysis were closely related to structure and surface modification. Basically, wettability became stronger as the amount of OH on the surface of NSN was higher. Both large nanopores and surface modification can reduce the wettability of NSN. Furthermore, NSN series were safe to be used when they circulated into the blood in low concentration, while if high concentration can not be avoided during administration, high porosity or amino modification of NSN were safer to be considered. It is believed that the basic evaluation of NSN can make contribution in providing scientific instruction for designing drug loaded NSN systems. Copyright © 2016 Elsevier B.V. All rights reserved.

Investigation of durability of silica fume concretes in coastal structures within tidal zone

International Nuclear Information System (INIS)

Ganjian, E.; Sadeghi Pouya, H.

2003-01-01

In recent decade use of silica fume has been become greater in coastal concrete structures in the persona gulf, to increase durability of those establishments. In this research the durability of cement passers and concrete cubes with use of 7 and 10 percent of silica fume as a cement replacement have been investigated in three curing conditions (fresh water, coast of sea and simulation bonds) by measuring compressive strengths and capillary absorption. Silica fume specimens under wetting and drying condition showed more strength loss after 180 days compare to samples without silica fume or cured in the fresh water. In addition the greater silica fume amount in specimens cured within tidal zone and under wetting and drying simulation, the more water absorption by capillary. According to the results, good correspondence between simulated condition and real site exposure was obtained

Functionalization of silica nanoparticles for polypropylene nanocomposites applications

International Nuclear Information System (INIS)

Bracho, Diego; Palza, Humberto; Quijada, Raul; Dougnac, Vivianne

2011-01-01

Synthetic silica nanospheres of different diameters produced via the sol-gel method were used in order to enhance the barrier properties of the polypropylene-silica nanocomposites. Modification of the silica surface by reaction with organic chlorosilanes was performed in order to improve the particles interaction with the polypropylene matrix and its dispersion. Unmodified and modified silica nanoparticles were characterized using electronic microscopy (TEM), elemental analysis, thermo gravimetric analysis (TGA), and solid state nuclear magnetic resonance (NMR) spectroscopy. Preliminary permeability tests of the polymer-silica nanocomposite films showed no significant change at low particles load (3 wt%) regardless its size or surface functionality, mainly because of the low aspect ratio of the silica nanospheres. However, it is expected that at a higher concentration of silica particles differences will be observed. (author)

Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials

Directory of Open Access Journals (Sweden)

Peter Hesemann

2014-04-01

Full Text Available The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA, mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the “anionic templating” strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches.

Ce+3-and Tb+3-luminescence in glasses. Ce+3-activated bulk silica and silica thin films. An α-particle detector based on a Ce+3-activated silica thin film. A Ce+3-Tb+3-energy transfer in a high melting point phosphate glass

International Nuclear Information System (INIS)

Heindl, R.; Loriers, J.; Sella, J.C.; Robert, A.

1984-07-01

While many Ce +3 -activated glasses of different type emit strongly under UV (253,7 nm) and β-ray excitation, only the commercial silicate glass NE 905 shows an useful emission when exposed to α-particles. Only phosphate glasses have give the green Tb +3 -emission, when doped by it, under UV and α and β radiation. Sputtered films of Ce +3 -activated silica have appropriate luminescence properties, adherence to the substrate and a perfect chemical resistance to hot nitric acid. An α-particle detector has been built which has permitted the quantitative detection of plutonium in the presence of other radiative ions

Processing, adhesion and electrical properties of silicon steel having non-oriented grains coated with silica and alumina sol-gel

International Nuclear Information System (INIS)

Vasconcelos, D.C.L.; Orefice, R.L.; Vasconcelos, W.L.

2007-01-01

Silicon steels having non-oriented grains are usually coated with a series of inorganic or organic films to be used in electrical applications. However, the commercially available coatings have several disadvantages that include poor adhesion to the substrates, low values of electrical resistance and degradation at higher temperatures. In this work, silica and alumina sol-gel films were deposited onto silicon steel in order to evaluate the possibility of replacing the commercially available coatings by these sol-gel derived materials. Silica and alumina sol-gel coatings were prepared by dipping silicon steel samples into hydrolyzed silicon or aluminum alkoxides. Samples coated with sol-gel films were studied by scanning electron microscopy, energy dispersive spectroscopy and infrared spectroscopy. Adhesion between silicon steel and sol-gel films was measured by using several standard adhesion tests. Electrical properties were evaluated by the Franklin method. Results showed that homogeneous sol-gel films can be deposited onto silicon steel. Thicknesses of the films could be easily managed by altering the speed of deposition. The structure of the films could also be tailored by introducing additives, such as nitric acid and N,N-dimethyl formamide. Adhesion tests revealed a high level of adhesion between coatings and metal. The Franklin test showed that sol-gel films can produce coated samples with electrical resistances suitable for electrical applications. Electrical properties of the coated samples could also be manipulated by altering the structure of the sol-gel films or by changing the thickness of them

Effect of various structure directing agents on the physicochemical properties of the silica aerogels prepared at an ambient pressure

KAUST Repository

Sarawade, Pradip

2013-12-01

We studied the effects of various surfactants on the textural properties (BET surface area, pore size, and pore volume) of the silica aerogels prepared at an ambient pressure. A simple surface modification of silica gel prepared at an ambient pressure through hydrolysis and polycondensation of TEOS as asilica precursor was conducted using various structure directing agents. The treatment was found to induce a significant difference in the porosity of the silica aerogel. Highly porous silica aerogels with bimodal porous structures were prepared by modifying the surface of the silica wet-gel (alcogel) with trimethylchlorosilane (TMCS) in order to preserve its porosity. The samples were analyzed by small-angle X-ray scattering and nitrogen adsorption. In this work, a possible new type of highly porous hydrophobic silica aerogel with a bimodal porous structure is presented. A hydrophilic extremely porous (high surface area and large pore volume) silica aerogel was obtained by heating the as-synthesized hydrophobic silica aerogel at 400°C for 1 h. There was a significant effect of structure directing agent on the textural properties, such as specific surface area, pore size distribution and cumulative pore volume of the silicaaerogels. © 2013 Elsevier B.V. All rights reserved.

Effect of various structure directing agents on the physicochemical properties of the silica aerogels prepared at an ambient pressure

KAUST Repository

Sarawade, Pradip; Shao, Godlistennamwel; Quang, Dangviet; Kim, Heetaik

2013-01-01

We studied the effects of various surfactants on the textural properties (BET surface area, pore size, and pore volume) of the silica aerogels prepared at an ambient pressure. A simple surface modification of silica gel prepared at an ambient pressure through hydrolysis and polycondensation of TEOS as asilica precursor was conducted using various structure directing agents. The treatment was found to induce a significant difference in the porosity of the silica aerogel. Highly porous silica aerogels with bimodal porous structures were prepared by modifying the surface of the silica wet-gel (alcogel) with trimethylchlorosilane (TMCS) in order to preserve its porosity. The samples were analyzed by small-angle X-ray scattering and nitrogen adsorption. In this work, a possible new type of highly porous hydrophobic silica aerogel with a bimodal porous structure is presented. A hydrophilic extremely porous (high surface area and large pore volume) silica aerogel was obtained by heating the as-synthesized hydrophobic silica aerogel at 400°C for 1 h. There was a significant effect of structure directing agent on the textural properties, such as specific surface area, pore size distribution and cumulative pore volume of the silicaaerogels. © 2013 Elsevier B.V. All rights reserved.

Laser ablation of toluene liquid for surface micro-structuring of silica glass

International Nuclear Information System (INIS)

Niino, H.; Kawaguchi, Y.; Sato, T.; Narazaki, A.; Gumpenberger, T.; Kurosaki, R.

2006-01-01

Microstructures with well-defined micropatterns were fabricated on the surfaces of silica glass using a laser-induced backside wet etching (LIBWE) method by diode-pumped solid state (DPSS) UV laser at the repetition rate of 10 kHz. For a demonstration of flexible rapid prototyping as mask-less exposure system, the focused laser beam was directed to the sample by galvanometer-based point scanning system. Additionally, a diagnostics study of plume propagation in the ablated products of toluene solid film was carried out with an intensified CCD (ICCD) camera

Successful implementation of the stepwise layer-by-layer growth of MOF thin films on confined surfaces: Mesoporous silica foam as a first case study

KAUST Repository

Shekhah, Osama; Fu, Lei; Sougrat, Rachid; Belmabkhout, Youssef; Cairns, Amy; Giannelis, Emmanuel P.; Eddaoudi, Mohamed

2012-01-01

Here we report the successful growth of highly crystalline homogeneous MOF thin films of HKUST-1 and ZIF-8 on mesoporous silica foam, by employing a layer-by-layer (LBL) method. The ability to control and direct the growth of MOF thin films on confined surfaces, using the stepwise LBL method, paves the way for new prospective applications of such hybrid systems. © 2012 The Royal Society of Chemistry.

Hydrophobic silica nanoparticles as reinforcing filler for poly (lactic acid polymer matrix

Directory of Open Access Journals (Sweden)

Pilić Branka M.

2016-01-01

Full Text Available Properties of poly (lactic acid (PLA and its nanocomposites, with silica nanoparticles (SiO2, as filler were investigated. Neat PLA films and PLA films with different percentage of hydrophobic fumed silica nanoparticles (0.2, 0.5, 1, 2, 3 and 5 wt. % were prepared by solution casting method. Several tools were used to characterize the influence of different silica content on crystalline behavior, and thermal, mechanical and barrier properties of PLA/SiO2 nanocomposites. Results from scanning electron microscope (SEM showed that the nanocomposite preparation and selection of specific hydrophobic spherical nano filler provide a good dispersion of the silica nanoparticles in the PLA matrix. Addition of silica nanoparticles improved mechanical properties, the most significant improvement being observed for lowest silica content (0.2wt.%. Barrier properties were improved for all measured gases at all loadings of silica nanoparticles. The degree of crystallinity for PLA slightly increased by adding 0.2 and 0.5 wt. % of nano filler. [Projekat Ministarstva nauke Republike Srbije, br. III46001

Influence of acetone extract from natural rubber on the structure and interface interaction in NR/silica composites

Science.gov (United States)

Xu, Tiwen; Jia, Zhixin; Wu, Lianghui; Chen, Yongjun; Luo, Yuanfang; Jia, Demin; Peng, Zheng

2017-11-01

It is well known that the coupling reagents as the additional modifiers were often used to improve the reinforcement effect of silica filled natural rubber. Actually, the commercial raw NR is a mixture consisting of polyisoprene and non-isoprene, where the latter one might have impact on the properties of NR/silica composites as an inartificial modifier inside. Thus, investigating the effect of non-isoprene compounds on the structure and properties of NR/silica composites is a novel approach to disclose the peculiarity of NR, which is meaningful to the assessment of NR quality. In this paper, the influences of acetone extract (AE) from natural rubber on the structure and mechanical properties of NR/silica composites were studied. Then the interfacial interactions between AE and silica were also illustrated through Fourier transform infrared spectroscopy (FTIR), thermogravimetic analysis (TGA), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Results demonstrated the existence of hydrogen bond between silica and AE, also the covalent bond induced by esterification reaction between sbnd COOH and Sisbnd OH, which resulted in an increase of constrained regions around silica surface leading to the promotions on mechanical and dynamical properties of NR/silica composites significantly.

Structural Characterization of Silica Particles Extracted from Grass Stenotaphrum secundatum: Biotransformation via Annelids

Directory of Open Access Journals (Sweden)

A. Espíndola-Gonzalez

2014-01-01

Full Text Available This study shows the structural characterization of silica particles extracted from Stenotaphrum secundatum (St. Augustine grass using an annelid-based biotransformation process. This bioprocess starts when St. Augustine grass is turned into humus by vermicompost, and then goes through calcination and acid treatment to obtain silica particles. To determine the effect of the bioprocess, silica particles without biotransformation were extracted directly from the sample of grass. The characterization of the silica particles was performed using Infrared (FTIR and Raman spectroscopy, Transmission Electron Microscopy (TEM, X-ray Diffraction (XRD, Dynamic Light Scattering (DLS, and Energy Dispersion Spectroscopy (EDS. Both types of particles showed differences in morphology and size. The particles without biotransformation were essentially amorphous while those obtained via annelids showed specific crystalline phases. The biological relationship between the metabolisms of worms and microorganisms and the organic-mineral matter causes changes to the particles' properties. The results of this study are important because they will allow synthesis of silica in cheaper and more ecofriendly ways.

Structure and Properties of Silica Glass Densified in Cold Compression and Hot Compression

Science.gov (United States)

Guerette, Michael; Ackerson, Michael R.; Thomas, Jay; Yuan, Fenglin; Bruce Watson, E.; Walker, David; Huang, Liping

2015-10-01

Silica glass has been shown in numerous studies to possess significant capacity for permanent densification under pressure at different temperatures to form high density amorphous (HDA) silica. However, it is unknown to what extent the processes leading to irreversible densification of silica glass in cold-compression at room temperature and in hot-compression (e.g., near glass transition temperature) are common in nature. In this work, a hot-compression technique was used to quench silica glass from high temperature (1100 °C) and high pressure (up to 8 GPa) conditions, which leads to density increase of ~25% and Young’s modulus increase of ~71% relative to that of pristine silica glass at ambient conditions. Our experiments and molecular dynamics (MD) simulations provide solid evidences that the intermediate-range order of the hot-compressed HDA silica is distinct from that of the counterpart cold-compressed at room temperature. This explains the much higher thermal and mechanical stability of the former than the latter upon heating and compression as revealed in our in-situ Brillouin light scattering (BLS) experiments. Our studies demonstrate the limitation of the resulting density as a structural indicator of polyamorphism, and point out the importance of temperature during compression in order to fundamentally understand HDA silica.

Metal-silica sol-gel materials

Science.gov (United States)

Stiegman, Albert E. (Inventor)

2002-01-01

The present invention relates to a single phase metal-silica sol-gel glass formed by the co-condensation of a transition metal with silicon atoms where the metal atoms are uniformly distributed within the sol-gel glass as individual metal centers. Any transition metal may be used in the sol-gel glasses. The present invention also relates to sensor materials where the sensor material is formed using the single phase metal-silica sol-gel glasses. The sensor materials may be in the form of a thin film or may be attached to an optical fiber. The present invention also relates to a method of sensing chemicals using the chemical sensors by monitoring the chromatic change of the metal-silica sol-gel glass when the chemical binds to the sensor. The present invention also relates to oxidation catalysts where a metal-silica sol-gel glass catalyzes the reaction. The present invention also relates to a method of performing oxidation reactions using the metal-silica sol-gel glasses. The present invention also relates to organopolymer metal-silica sol-gel composites where the pores of the metal-silica sol-gel glasses are filled with an organic polymer polymerized by the sol-gel glass.

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).

Structural changes in femtosecond laser modified regions inside fused silica

International Nuclear Information System (INIS)

Juodkazis, Saulius; Kohara, Shinji; Ohishi, Yasuo; Hirao, Norihisa; Vailionis, Arturas; Mizeikis, Vygantas; Saito, Akira; Rode, Andrei

2010-01-01

Structural characterization of photomodified microvolumes formed by tightly focused femtosecond laser pulses inside silica glass was carried out using synchrotron x-ray diffraction. The observed distinct separation between the O–O and Si–Si pair correlation peaks can be interpreted as a phase separation induced by microexplosions at the focal volume. The mechanisms of structural transitions induced by femtosecond laser pulses inside dielectrics are discussed

Oxide ultrathin films science and technology

CERN Document Server

Pacchioni, Gianfranco

2012-01-01

A wealth of information in one accessible book. Written by international experts from multidisciplinary fields, this in-depth exploration of oxide ultrathin films covers all aspects of these systems, starting with preparation and characterization, and going on to geometrical and electronic structure, as well as applications in current and future systems and devices. From the Contents: Synthesis and Preparation of Oxide Ultrathin Films Characterization Tools of Oxide Ultrathin Films Ordered Oxide Nanostructures on Metal Surfaces Unusual Properties of Oxides and Other Insulators in the Ultrathin Limit Silica and High-K Dielectrics Thin Films in Microelectronics Oxide Passive Films and Corrosion Protection Oxide Films as Catalytic Materials and as Models of Real Catalysts Oxide Films in Spintronics Oxide Ultrathin Films in Solid Oxide Fuel Cells Transparent Conducting and Chromogenic Oxide Films as Solar Energy Materials Oxide Ultrathin Films in Sensor Applications Ferroelectricity in Ultrathin Film Capacitors T...

A facile and efficient method of enzyme immobilization on silica particles via Michael acceptor film coatings: immobilized catalase in a plug flow reactor.

Science.gov (United States)

Bayramoglu, Gulay; Arica, M Yakup; Genc, Aysenur; Ozalp, V Cengiz; Ince, Ahmet; Bicak, Niyazi

2016-06-01

A novel method was developed for facile immobilization of enzymes on silica surfaces. Herein, we describe a single-step strategy for generating of reactive double bonds capable of Michael addition on the surfaces of silica particles. This method was based on reactive thin film generation on the surfaces by heating of impregnated self-curable polymer, alpha-morpholine substituted poly(vinyl methyl ketone) p(VMK). The generated double bonds were demonstrated to be an efficient way for rapid incorporation of enzymes via Michael addition. Catalase was used as model enzyme in order to test the effect of immobilization methodology by the reactive film surface through Michael addition reaction. Finally, a plug flow type immobilized enzyme reactor was employed to estimate decomposition rate of hydrogen peroxide. The highly stable enzyme reactor could operate continuously for 120 h at 30 °C with only a loss of about 36 % of its initial activity.

Fluctuations and structure of amphiphilic films; Fluctuations et structure de films d`amphiphiles

Energy Technology Data Exchange (ETDEWEB)

Gourier, CH

1996-07-01

This thesis is divided in three parts.The first part exposes in a theoretical point of view, how the fluctuations spectrum of an amphiphilic film is governed by its properties and its bidimensional characteristics.The measurements of fluctuations spectra of an interface are accessible with the measurement of intensity that interface diffuses out of the specular angle, we present in the second chapter the principles of the X rays diffusion by a real interface and see how the diffuse diffusion experiments allow to determine the fluctuations spectrum of an amphiphilic film. The second part is devoted to the different experimental techniques that have allowed to realize the study of fluctuation as well as the structural study.The third part is devoted to experimental results concerning the measurements of fluctuations spectra and to the study of the structure of amphiphilic films. We show that it is possible by using an intense source of X rays (ESRF: European Synchrotron Radiation Facility) to measure the water and amphiphilic films fluctuations spectra until molecular scales. The last chapter is devoted to the structural study and film fluctuations made of di-acetylenic molecules. (N.C.)

The effects of surface roughness on low haze ultrathin nanocomposite films

Energy Technology Data Exchange (ETDEWEB)

Kanniah, Vinod [Chemical and Materials Engineering, 177 F. Paul Anderson Tower, University of Kentucky, Lexington, KY 40506 (United States); Tru Vue, Inc. 9400 West, 55th St, McCook, IL 60525 (United States); Grulke, Eric A., E-mail: eric.grulke@uky.edu [Chemical and Materials Engineering, 177 F. Paul Anderson Tower, University of Kentucky, Lexington, KY 40506 (United States); Druffel, Thad [Vision Dynamics LLC, 1950 Production Court, Louisville, KY 40299 (United States); Conn Center for Renewable Energy Research, University of Louisville, Ernst Hall Room 102A, Louisville, KY 40292 (United States)

2013-07-31

Control of surface roughness in optical applications can have a large impact on haze. This work compares surface roughness and haze for self-assembled experimental surface structures as well as simulated surface structures for ultrathin nanocomposite films. Ultrathin nanocomposite films were synthesized from an acrylate monomer as the continuous phase with monodisperse or bidisperse mixtures of silica nanoparticles as the dispersed phase. An in-house spin coating deposition technique was used to make thin nanocomposite films on hydrophilic (glass) and hydrophobic (polycarbonate) substrates. Manipulating the size ratios of the silica nanoparticle mixtures generated multimodal height distributions, varied the average surface roughness (σ) and changed lateral height–height correlations (a). For the simulated surfaces, roughness was estimated from their morphologies, and haze was calculated using simplified Rayleigh scattering theory. Experimental data for haze and morphologies of nanocomposite films corresponded well to these properties for simulated tipped pyramid surfaces. A correlation based on simple Rayleigh scattering theory described our experimental data well, but the exponent on the parameter, σ/λ (λ is the wavelength of incident light), does not have the expected value of 2. A scalar scattering model and a prior Monte Carlo simulation estimated haze values similar to those of our experimental samples. - Highlights: • Bidisperse nanoparticle mixtures created structured surfaces on thin films. • Monodisperse discrete phases created unimodal structure distributions. • Bidisperse discrete phases created multimodal structure distributions. • Multimodal structures had maximum heights ≤ 1.5 D{sub large} over our variable range. • Simplified Rayleigh scattering theory linked roughness to haze and contact angle.

Effect of nitrogen incorporation on the structural, optical and dielectric properties of reactive sputter grown ITO films

Energy Technology Data Exchange (ETDEWEB)

Gartner, M.; Stroescu, H. [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Marin, A., E-mail: alexmarin@icf.ro [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Osiceanu, P. [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Anastasescu, M., E-mail: manastasescu@icf.ro [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Stoica, M.; Nicolescu, M.; Duta, M.; Preda, S. [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Aperathitis, E.; Pantazis, A.; Kampylafka, V. [FORTH-IESL, Crete (Greece); Modreanu, M. [Tyndall National Institute, University College Cork, Cork (Ireland); Zaharescu, M. [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania)

2014-09-15

Highlights: • Graded optical model for ITON films is presented. • ITON thin films retain an amorphous structure even after RTA at 500 °C in N{sub 2} ambient. • The lowest resistivity was 2 × 10{sup −3} Ω cm for films deposited in 75%N{sub 2} and RTA at 500 °C. • Films deposited in 75% N{sub 2} and RTA at 500 °C have degenerate semiconductor behavior. • Chemical composition before and after RTA has been analyzed by XPS depth profiling. - Abstract: The changes in the optical, microstructural and electrical properties, following the nitrogen incorporation into indium tin oxide thin films are investigated. The films are formed by r.f. sputtering from an indium-tin-oxide (80% In{sub 2}O{sub 3}–20% SnO{sub 2}) target in a mixture of Ar and N{sub 2} plasma (75% N{sub 2}–25% Ar and 100% N{sub 2} respectively) on fused silica glass substrate. The impact of rapid thermal annealing (up to 500 °C, in N{sub 2} ambient) on the properties of indium tin oxynitride (ITON) thin films is also reported. The UV–vis–NIR ellipsometry (SE) characterization of ITON films was performed assuming several realistic approaches based on various oscillator models, using a chemical composition gradient depth profiling, in agreement with the X-ray photoelectron spectroscopy measurements. The Hall measurements show that the ITON films prepared by r.f. sputtering in 75% N{sub 2} and annealed at 500 °C behave as degenerate semiconductors. X-ray diffraction analysis proved that ITON thin films retain an amorphous structure even after RTA at 500 °C in N{sub 2} ambient and atomic force microscopy showed the formation of continuous and smooth ITON thin films, with a morphology consisting in quasispherical nanometric particles.

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

Thermally induced structural modifications and O2 trapping in highly porous silica nanoparticles

International Nuclear Information System (INIS)

Alessi, A.; Agnello, S.; Iovino, G.; Buscarino, G.; Melodia, E.G.; Cannas, M.; Gelardi, F.M.

2014-01-01

In this work we investigate by Raman spectroscopy the effect of isochronal (2 h) thermal treatments in air in the temperature range 200–1000 °C of amorphous silicon dioxide porous nanoparticles with diameters ranging from 5 up to 15 nm and specific surface 590–690 m 2 /g. Our results indicate that the amorphous structure changes similarly to other porous systems previously investigated, in fact superficial SiOH groups are removed, Si–O–Si linkages are created and the ring statistic is modified, furthermore these data evidence that the three membered rings do not contribute significantly to the Raman signal detected at about 495 cm −1 . In addition, after annealing at 900 and 1000 °C we noted the appearance of the O 2 emission at 1272 nm, absent in the not treated samples. The measure of the O 2 emission has been combined with electron paramagnetic resonance measurements of the γ irradiation induced HO · 2 radicals to investigate the O 2 content per mass unit of thin layers of silica. Our data reveal that the porous nanoparticles have a much lower ability to trap O 2 molecules per mass units than nonporous silica supporting a model by which O 2 trapping inside a surface layer of about 1 nm of silica is always limited. - Highlights: • O 2 emission and HO · 2 electron paramagnetic resonance signals are investigated. • Silica surface ability to trap O 2 molecules is explored by thermal treatments. • Raman study of thermally induced structural changes in porous silica nanoparticles. • Raman signal attributable to the three membered rings in silica

Structure and dynamics of spin-labeled insulin entrapped in a silica matrix by the sol-gel method.

Science.gov (United States)

Vanea, E; Gruian, C; Rickert, C; Steinhoff, H-J; Simon, V

2013-08-12

The structure and conformational dynamics of insulin entrapped into a silica matrix was monitored during the sol to maturated-gel transition by electron paramagnetic resonance (EPR) spectroscopy. Insulin was successfully spin-labeled with iodoacetamide and the bifunctional nitroxide reagent HO-1944. Room temperature continuous wave (cw) EPR spectra of insulin were recorded to assess the mobility of the attached spin labels. Insulin conformation and its distribution within the silica matrix were studied using double electron-electron resonance (DEER) and low-temperature cw-EPR. A porous oxide matrix seems to form around insulin molecules with pore diameters in the order of a few nanometers. Secondary structure of the encapsulated insulin investigated by Fourier transform infrared spectroscopy proved a high structural integrity of insulin even in the dried silica matrix. The results show that silica encapsulation can be used as a powerful tool to effectively isolate and functionally preserve biomolecules during preparation, storage, and release.

Structure and spectral properties of the silver-containing high-silica glasses

International Nuclear Information System (INIS)

Girsova, M A; Golovina, G F; Anfimova, I N; Antropova, T V; Arsent'ev, M Yu

2016-01-01

Silver-containing high-silica glasses were synthesized by an impregnation of the silica porous glasses (PGs) first with AgNO 3 aqueous solution (with or without the presence of the sensitizers, such as Cu(NO 3 ) 2 or Ce(NO 3 ) 3 ), next in the mixed halide salt (NH 4 Cl, KBr, KI) solution. Then some part of the samples was sintered at the temperatures from 850 to 900°C up to closing of the pores. The structure of glasses was studied by UV-VIS-NIR and IR spectroscopy and X-ray diffraction (XRD) techniques. According to XRD data the silver-containing high-silica glasses contain the AgBr, AgI, Ag 3 PO 4 , (CuBr) 0.75 (CuI) 0.25 phases. IR spectra confirmed B-O-B, Si- O-Si, P-O-P, O-P-O, O-B-O bonds, (PO 4 ) 3- and P-O - groups in glasses. (paper)

Facile synthesis of mesoporous silica sublayer with hierarchical pore structure on ceramic membrane using anionic polyelectrolyte.

Science.gov (United States)

Kang, Taewook; Oh, Seogil; Kim, Honggon; Yi, Jongheop

2005-06-21

A facile method for introducing mesoporous silica sublayer onto the surface of a ceramic membrane for use in liquid-phase separation is described. To reduce the electrostatic repulsion between the mesoporous silica sol and the ceramic membrane in highly acidic conditions (pH ceramic membrane, as confirmed by experimental titration data. Consistent with the titration results, the amount of mesoporous silica particles on the surface of the ceramic membrane was low, in the absence of PSS- treatment, whereas mesoporous silica sublayer with hierarchical pore structure was produced, when 1 wt % PSS- was used. The results show that mesoporous silica grows in the confined surface, eventually forming a multistacked surface architecture. The mesoporous silica sublayer contained uniform, ordered (P6 mm) mesopores of ca. 7.5 nm from mesoporous silica as well as macropores ( approximately mum) from interparticle voids, as evidenced by transmission electron microscopy and scanning electron microscopy analyses. The morphologies of the supported mesoporous silica could be manipulated, thus permitting the generation of uniform needlelike forms or uniform spheroid particles by varying the concentration of PSS-.

Infrared characterization of strontium titanate thin films

International Nuclear Information System (INIS)

Almeida, B.G.; Pietka, A.; Mendes, J.A.

2004-01-01

Strontium titanate thin films have been prepared at different oxygen pressures with various post-deposition annealing treatments. The films were deposited by pulsed laser ablation at room temperature on Si(0 0 1) substrates with a silica buffer layer. Infrared reflectance measurements were performed in order to determine relevant film parameters such as layer thicknesses and chemical composition. The infrared reflectance spectra were fitted by using adequate dielectric function forms for each layer. The fitting procedure provided the extraction of the dielectric functions of the strontium titanate film, the silica layer and the substrate. The as-deposited films are found to be amorphous, and their infrared spectra present peaks corresponding to modes with high damping constants. As the annealing time and temperature increases the strontium titanate layer becomes more ordered so that it can be described by its SrTiO 3 bulk mode parameters. Also, the silica layer grows along with the ordering of the strontium titanate film, due to oxidation during annealing

Photocrosslinked nanocomposite hydrogels from PEG and silica nanospheres: Structural, mechanical and cell adhesion characteristics

International Nuclear Information System (INIS)

Gaharwar, Akhilesh K.; Rivera, Christian; Wu, Chia-Jung; Chan, Burke K.; Schmidt, Gudrun

2013-01-01

Photopolymerized hydrogels are extensively investigated for various tissue engineering applications, primarily due to their ability to form hydrogels in a minimally invasive manner. Although photocrosslinkable hydrogels provide necessary biological and chemical characteristics to mimic cellular microenvironments, they often lack sufficient mechanical properties. Recently, nanocomposite approaches have demonstrated potential to overcome these deficits by reinforcing the hydrogel network with. In this study, we investigate some physical, chemical, and biological properties of photocrosslinked poly(ethylene glycol) (PEG)-silica hydrogels. The addition of silica nanospheres significantly suppresses the hydration degree of the PEG hydrogels, indicating surface interactions between the silica nanospheres and the polymer chains. No significant change in hydrogel microstructure or average pore size due to the addition of silica nanospheres was observed. However, addition of silica nanospheres significantly increases both the mechanical strength and the toughness of the hydrogel networks. The biological properties of these nanocomposite hydrogels were evaluated by seeding fibroblast cells on the hydrogel surface. While the PEG hydrogels showed minimum cell adhesion, spreading and proliferation, the addition of silica nanospheres enhanced initial cell adhesion, promoted cell spreading and increased the metabolic activity of the cells. Overall, results indicate that the addition of silica nanospheres improves the mechanical stiffness and cell adhesion properties of PEG hydrogels and can be used for biomedical applications that required controlled cell adhesion. - Graphical abstract: Structural, mechanical and biological properties of photocrosslinked nanocomposite hydrogels from silica and poly(ethylene oxide) are investigated. Silica reinforce the hydrogel network and improved mechanical strength. Addition of induces cell adhesion characteristic properties for various

Synthesis, structural characterization and in vitro testing of dysprosium containing silica particles as potential MRI contrast enhancing agents

International Nuclear Information System (INIS)

Chiriac, L.B.; Trandafir, D.L.; Turcu, R.V.F.; Todea, M.; Simon, S.

2016-01-01

Highlights: • Dysprosium containing silica microparticles obtained by freeze and spray drying. • Higher structural units interconnection achieved in freeze vs. spray dried samples. • Dy occurance on the outermost layer of the microparticles evidenced by XPS. • Enhanced MRI contrast observed for freeze dried samples with 5% mol Dy_2O_3. - Abstract: The work is focused on synthesis and structural characterization of novel dysprosium-doped silica particles which could be considered as MRI contrast agents. Sol-gel derived silica rich particles obtained via freeze-drying and spray-drying processing methods were structurally characterized by XRD, "2"9Si MAS-NMR and XPS methods. The occurrence of dysprosium on the outermost layer of dysprosium containing silica particles was investigated by XPS analysis. The MRI contrast agent characteristics have been tested using RARE-T_1 and RARE-T_2 protocols. The contrast of MRI images delivered by the investigated samples was correlated with their local structure. Dysprosium disposal on microparticles with surface structure characterised by decreased connectivity of the silicate network units favours dark T_2-weighted MRI contrast properties.

The structural coloration of textile materials using self-assembled silica nanoparticles.

Science.gov (United States)

Gao, Weihong; Rigout, Muriel; Owens, Huw

2017-01-01

The work presented investigates how to produce structural colours on textile materials by applying a surface coating of silica nanoparticles (SNPs). Uniform SNPs with particle diameters in a controlled micron size range (207-350 nm) were synthesized using a Stöber-based solvent varying (SV) method which has been reported previously. Photonic crystals (PCs) were formed on the surface of a piece of textile fabric through a process of natural sedimentation self-assembly of the colloidal suspension containing uniform SNPs. Due to the uniformity and a particular diameter range of the prepared SNPs, structural colours were observed from the fabric surface due to the Bragg diffraction of white light with the ordered structure of the silica PCs. By varying the mean particle diameter, a wide range of spectral colours from red to blue were obtained. The comparison of structural colours on fabrics and on glasses suggests that a smooth substrate is critical when producing materials with high colour intensity and spatial uniformity. This work suggested a promising approach to colour textile materials without the need for traditional dyes and/or pigments. Graphical abstract.

Fracture properties of hydrogenated amorphous silicon carbide thin films

International Nuclear Information System (INIS)

Matsuda, Y.; King, S.W.; Bielefeld, J.; Xu, J.; Dauskardt, R.H.

2012-01-01

The cohesive fracture properties of hydrogenated amorphous silicon carbide (a-SiC:H) thin films in moist environments are reported. Films with stoichiometric compositions (C/Si ≈ 1) exhibited a decreasing cohesive fracture energy with decreasing film density similar to other silica-based hybrid organic–inorganic films. However, lower density a-SiC:H films with non-stoichiometric compositions (C/Si ≈ 5) exhibited much higher cohesive fracture energy than the films with higher density stoichiometric compositions. One of the non-stoichiometric films exhibited fracture energy (∼9.5 J m −2 ) greater than that of dense silica glasses. The increased fracture energy was due to crack-tip plasticity, as demonstrated by significant pileup formation during nanoindentation and a fracture energy dependence on film thickness. The a-SiC:H films also exhibited a very low sensitivity to moisture-assisted cracking compared with other silica-based hybrid films. A new atomistic fracture model is presented to describe the observed moisture-assisted cracking in terms of the limited Si-O-Si suboxide bond formation that occurs in the films.

Hydrogen absorption in thin ZnO films prepared by pulsed laser deposition

OpenAIRE

Meilkhova, O.; Čížek, J.; Lukáč,, F.; Vlček, M.; Novotný, M.; Bulíř, J.; Lančok, J.; Anwand, W.; Brauer, G.; Connolly, J.; McCarthy, E.; Krishnamurthy, S.; Mosnier, J.-P.

2013-01-01

ZnO films with thickness of ~80 nm were grown by pulsed laser deposition (PLD) on MgO (1 0 0) single crystal and amorphous fused silica (FS) substrates. Structural studies of ZnO films and a high quality reference ZnO single crystal were performed by slow positron implantation spectroscopy (SPIS). It was found that ZnO films exhibit significantly higher density of defects than the reference ZnO crystal. Moreover, the ZnO film deposited on MgO substrate exhibits higher concentration of defects...

Nano-structured silica coated mesoporous carbon micro-granules for potential application in water filtration

Science.gov (United States)

Das, Avik; Sen, D.; Mazumder, S.; Ghosh, A. K.

2017-05-01

A novel nano-composite spherical micro-granule has been synthesized using a facile technique of solvent evaporation induced assembly of nanoparticles for potential application in water filtration. The spherical micro-granule is comprised of nano-structured shell of hydrophilic silica encapsulating a hydrophobic mesoporous carbon at the core. Hierarchical structure of such core-shell micro-granules has been rigorously characterized using small-angle neutron and X-ray scattering techniques and complemented with scanning electron microscopy. The hydrophilic silica envelope around the carbon core helps in incorporation of such granules into the hydrophilic polymeric ultra-filtration membrane. The interstitial micro-pores present in the silica shell can serve as water transport channels and the mesoporus carbon core enhances the separation performance due its well adsorption characteristics. It has been found that the incorporation of such granules inside the ultra-filtration membrane indeed enhances the water permeability as well as the separation performance in a significant way.

Magnetic core-shell silica particles

NARCIS (Netherlands)

Claesson, E.M.

2007-01-01

This thesis deals with magnetic silica core-shell colloids and related functionalized silica structures. Synthesis routes have been developed and optimized. The physical properties of these colloids have been investigated, such as the magnetic dipole moment, dipolar structure formation and

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...

The Effect of Various Acids to the Gelation Process to the Silica Gel Characteristic Using Organic Silica

Science.gov (United States)

Rahman, NA; Widiyastuti, W.; Sigit, D.; Ajiza, M.; Sujana, W.

2018-01-01

Bagasse ash is solid waste of cane sugar industry which contain of silica more than 51%. Some previous study of silica gel from bagasse ash have been conducted often and been applied. This study concerns about the effect of various acid used in the process of gelation to the characteristic of silica gel produced. Then, this silica gel will be used as adsorbent. As that, the silica gel must fulfill the requirements of adsorbent, as have good pores characteristics, fit in mesoporous size so that adsorbent diffusion process is not disturbed. A fitted pores size of silica gel can be prepared by managing acid concentration used. The effect of acid, organic acid (tartaric acid) and inorganic acid (hydrochloric acid), is investigated in detail. The acid is added into sodium silicate solution in that the gel is formed, the pores structures can be investigated with BET, the crystal form is analyzed with XRD and the pore structure is analyzed visually with SEM. By managing the acid concentration added, it gets the effect of acid to the pore structure of silica gel. The bigger concentration is, the bigger the pore’s size of silica gel produced.

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

Synthesis, structural characterization and in vitro testing of dysprosium containing silica particles as potential MRI contrast enhancing agents

Energy Technology Data Exchange (ETDEWEB)

Chiriac, L.B.; Trandafir, D.L. [Faculty of Physics & National Magnetic Resonance Center, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Interdisciplinary Research Institute on Bio-Nano-Sciences & Faculty of Physics, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Turcu, R.V.F. [Faculty of Physics & National Magnetic Resonance Center, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Todea, M. [Interdisciplinary Research Institute on Bio-Nano-Sciences & Faculty of Physics, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Simon, S., E-mail: simons@phys.ubbcluj.ro [Faculty of Physics & National Magnetic Resonance Center, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania); Interdisciplinary Research Institute on Bio-Nano-Sciences & Faculty of Physics, Babeş-Bolyai University, Cluj-Napoca, RO-400084 (Romania)

2016-11-01

Highlights: • Dysprosium containing silica microparticles obtained by freeze and spray drying. • Higher structural units interconnection achieved in freeze vs. spray dried samples. • Dy occurance on the outermost layer of the microparticles evidenced by XPS. • Enhanced MRI contrast observed for freeze dried samples with 5% mol Dy{sub 2}O{sub 3}. - Abstract: The work is focused on synthesis and structural characterization of novel dysprosium-doped silica particles which could be considered as MRI contrast agents. Sol-gel derived silica rich particles obtained via freeze-drying and spray-drying processing methods were structurally characterized by XRD, {sup 29}Si MAS-NMR and XPS methods. The occurrence of dysprosium on the outermost layer of dysprosium containing silica particles was investigated by XPS analysis. The MRI contrast agent characteristics have been tested using RARE-T{sub 1} and RARE-T{sub 2} protocols. The contrast of MRI images delivered by the investigated samples was correlated with their local structure. Dysprosium disposal on microparticles with surface structure characterised by decreased connectivity of the silicate network units favours dark T{sub 2}-weighted MRI contrast properties.

Adsorption-Induced Deformation of Hierarchically Structured Mesoporous Silica-Effect of Pore-Level Anisotropy.

Science.gov (United States)

Balzer, Christian; Waag, Anna M; Gehret, Stefan; Reichenauer, Gudrun; Putz, Florian; Hüsing, Nicola; Paris, Oskar; Bernstein, Noam; Gor, Gennady Y; Neimark, Alexander V

2017-06-06

The goal of this work is to understand adsorption-induced deformation of hierarchically structured porous silica exhibiting well-defined cylindrical mesopores. For this purpose, we performed an in situ dilatometry measurement on a calcined and sintered monolithic silica sample during the adsorption of N 2 at 77 K. To analyze the experimental data, we extended the adsorption stress model to account for the anisotropy of cylindrical mesopores, i.e., we explicitly derived the adsorption stress tensor components in the axial and radial direction of the pore. For quantitative predictions of stresses and strains, we applied the theoretical framework of Derjaguin, Broekhoff, and de Boer for adsorption in mesopores and two mechanical models of silica rods with axially aligned pore channels: an idealized cylindrical tube model, which can be described analytically, and an ordered hexagonal array of cylindrical mesopores, whose mechanical response to adsorption stress was evaluated by 3D finite element calculations. The adsorption-induced strains predicted by both mechanical models are in good quantitative agreement making the cylindrical tube the preferable model for adsorption-induced strains due to its simple analytical nature. The theoretical results are compared with the in situ dilatometry data on a hierarchically structured silica monolith composed by a network of mesoporous struts of MCM-41 type morphology. Analyzing the experimental adsorption and strain data with the proposed theoretical framework, we find the adsorption-induced deformation of the monolithic sample being reasonably described by a superposition of axial and radial strains calculated on the mesopore level. The structural and mechanical parameters obtained from the model are in good agreement with expectations from independent measurements and literature, respectively.

Thermally induced structural modifications and O{sub 2} trapping in highly porous silica nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Alessi, A., E-mail: antonino.alessi@unipa.it; Agnello, S.; Iovino, G.; Buscarino, G.; Melodia, E.G.; Cannas, M.; Gelardi, F.M.

2014-12-15

In this work we investigate by Raman spectroscopy the effect of isochronal (2 h) thermal treatments in air in the temperature range 200–1000 °C of amorphous silicon dioxide porous nanoparticles with diameters ranging from 5 up to 15 nm and specific surface 590–690 m{sup 2}/g. Our results indicate that the amorphous structure changes similarly to other porous systems previously investigated, in fact superficial SiOH groups are removed, Si–O–Si linkages are created and the ring statistic is modified, furthermore these data evidence that the three membered rings do not contribute significantly to the Raman signal detected at about 495 cm{sup −1}. In addition, after annealing at 900 and 1000 °C we noted the appearance of the O{sub 2} emission at 1272 nm, absent in the not treated samples. The measure of the O{sub 2} emission has been combined with electron paramagnetic resonance measurements of the γ irradiation induced HO{sup ·}{sub 2} radicals to investigate the O{sub 2} content per mass unit of thin layers of silica. Our data reveal that the porous nanoparticles have a much lower ability to trap O{sub 2} molecules per mass units than nonporous silica supporting a model by which O{sub 2} trapping inside a surface layer of about 1 nm of silica is always limited. - Highlights: • O{sub 2} emission and HO{sup ·}{sub 2} electron paramagnetic resonance signals are investigated. • Silica surface ability to trap O{sub 2} molecules is explored by thermal treatments. • Raman study of thermally induced structural changes in porous silica nanoparticles. • Raman signal attributable to the three membered rings in silica.

Magnetic structure of Tb-Fe films with an artificially layered structure

International Nuclear Information System (INIS)

Yamauchi, K.; Habu, K.; Sato, N.

1988-01-01

The magnetic structure of Tb-Fe films with an artificially layered structure has been investigated by measuring the temperature dependence of the magnetization of the films. Ferrimagnetic coupling between Tb and Fe through the interface was explicitly observed up to about 9-A Tb and 10-A Fe layers. Films with thinner Tb and Fe layers than these thicknesses are composed of only ferrimagnetically coupled Tb-Fe regions. Films with thicker layers of Tb and Fe are composed of ferrimagnetically coupled Tb-Fe, ferromagnetic Fe, ferromagnetic Tb, and/or magnetically compensated Tb regions. The Tb-Fe films exhibit various temperature dependencies of the magnetization corresponding to these magnetic structures

A study on the silica removal in primary system using the membrane process

International Nuclear Information System (INIS)

Kim, Bong Jin; Lee, Sang Jin; Yang, Ho Yeon; Kim, Kyung Duk; Jung, Hee Chul; Jo, Hang Rae

2005-01-01

Silica in primary system combines with an alkali grammatical particle metal and forms the zeolite layer which is hindering the heat transfer on the surface of the cladding. Zeolite layer becomes the cause of the damage in this way. The problems of the NPP's primary system have been issued steadily by EPRI. Through a series of experiments of the laboratory scale, we confirmed the applicability of NF membrane for silica removal, as silica rejection rate of NF membrane is about 60 ∼ 70% and boron rejection rate is about 10 ∼ 20%. We accomplished a site experiment about four NF membranes manufactured by FilmTec and Osmonics Inc. In experiment using 400L of SFP water, when operation pressure is 10kg f /cm 2 , we confirmed that the silica rejection rate of NF90-2540 manufactured by FilmTec Inc. is about 98%, boron rejection rate is about 43%. The silica rejection rate of NF270-2540 is about 38%, boron rejection rate is about 3.5%. Afterward, through additional experiments, such as long term characteristic experiments, we are going to design a optimum NF membrane system for silica removal

A study on the silica removal in primary system using the membrane process

Energy Technology Data Exchange (ETDEWEB)

Kim, Bong Jin; Lee, Sang Jin; Yang, Ho Yeon; Kim, Kyung Duk [Korea Hydro and Nuclear Power Co., LTD., Taejeon (Korea, Republic of); Jung, Hee Chul; Jo, Hang Rae [Korea Hydro and Nuclear Power Co., LTD., Uljin (Korea, Republic of)

2005-06-15

Silica in primary system combines with an alkali grammatical particle metal and forms the zeolite layer which is hindering the heat transfer on the surface of the cladding. Zeolite layer becomes the cause of the damage in this way. The problems of the NPP's primary system have been issued steadily by EPRI. Through a series of experiments of the laboratory scale, we confirmed the applicability of NF membrane for silica removal, as silica rejection rate of NF membrane is about 60 {approx} 70% and boron rejection rate is about 10 {approx} 20%. We accomplished a site experiment about four NF membranes manufactured by FilmTec and Osmonics Inc. In experiment using 400L of SFP water, when operation pressure is 10kg{sub f}/cm{sup 2}, we confirmed that the silica rejection rate of NF90-2540 manufactured by FilmTec Inc. is about 98%, boron rejection rate is about 43%. The silica rejection rate of NF270-2540 is about 38%, boron rejection rate is about 3.5%. Afterward, through additional experiments, such as long term characteristic experiments, we are going to design a optimum NF membrane system for silica removal.

A methodology for the preparation of nanoporous polyimide films with low dielectric constants

International Nuclear Information System (INIS)

Jiang Lizhong; Liu Jiugui; Wu Dezhen; Li Hangquan; Jin Riguang

2006-01-01

A method to generate nanoporous polyimide films with low dielectric constants was proposed. The preparation consisted of two steps. Firstly, a polyimide/silica hybrid film was prepared via sol-gel process. Secondly, the hybrid film was treated with hydrofluoric acid to remove the dispersed silica particles, leaving pores with diameters between 20 and 120 nm, depending on the size of silica particles. Both hybrid and porous films were subjected to a variety of characterizations including transmission electron microscopy observation, dielectric constant measurement and tensile strength measurement

Study of thin insulating films using secondary ion emission

International Nuclear Information System (INIS)

Hilleret, Noel

1973-01-01

Secondary ion emission from insulating films was investigated using a CASTAING-SLODZIAN ion analyzer. Various different aspects of the problem were studied: charge flow across a silica film; the mobilization of sodium during ion bombardment; consequences of the introduction of oxygen on the emission of secondary ions from some solids; determination of the various characteristics of secondary ion emission from silica, silicon nitride and silicon. An example of measurements made using this type of operation is presented: profiles (concentration as a function of depth) of boron introduced by diffusion or implantation in thin films of silica on silicon or silicon nitride. Such measurements have applications in microelectronics. The same method of operation was extended to other types of insulating film, and in particular, to the metallurgical study of passivation films formed on the surface of stainless steels. (author) [fr

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.

Electronic structure of semiconductor quantum films

International Nuclear Information System (INIS)

Zhang, S.B.; Yeh, C.; Zunger, A.

1993-01-01

The electronic structure of thin (≤30 A) free-standing ideal films of Si(001), Si(110), and GaAs(110) is calculated using a plane-wave pseudopotential description. Unlike the expectation based on the simple effective-mass model, we find the following. (i) The band gaps of (001) quantum films exhibit even-odd oscillation as a function of the number N of monolayers. (ii) In addition to sine-type envelope functions which vanish at the film boundaries, some states have cosine envelope functions with extrema at boundaries. (iii) Even-layer Si(001) films exhibit at the valence-band maximum a state whose energy does not vary with the film thickness. Such zero confinement states have constant envelope throughout the film. (iv) Optical transitions in films exhibit boundary-imposed selection rules. Furthermore, oscillator strengths for pseudodirect transitions in the vicinity of forbidden direct transitions can be enhanced by several orders of magnitude. These findings, obtained in direct supercell calculations, can be explained in terms of a truncated crystal (TC) analysis. In this approach the film's wave functions are expanded in terms of pairs of bulk wave functions exhibiting a destructive interference at the boundaries. This maps the eigenvalue spectra of a film onto the bulk band structure evaluated at special k points which satisfy the boundary conditions. We find that the TC representation reproduces accurately the above-mentioned results of direct diagonalization of the film's Hamiltonian. This provides a simple alternative to the effective-mass model and relates the properties of quantum structures to those of the bulk material

ZnO based transparent conductive oxide films with controlled type of conduction

Energy Technology Data Exchange (ETDEWEB)

Zaharescu, M., E-mail: mzaharescu@icf.ro [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Mihaiu, S., E-mail: smihaiu@icf.ro [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Toader, A. [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Atkinson, I., E-mail: irinaatkinson@yahoo.com [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Calderon-Moreno, J.; Anastasescu, M.; Nicolescu, M.; Duta, M.; Gartner, M. [Institute of Physical Chemistry “Ilie Murgulescu”, Romanian Academy, 202 Splaiul Independentei, 060021 Bucharest (Romania); Vojisavljevic, K.; Malic, B. [Institute Jožef Stefan, Ljubljana (Slovenia); Ivanov, V.A.; Zaretskaya, E.P. [State Scientific and Production Association “Scientific-Practical Materials Research Center of the National Academy of Science Belarus, P. Brovska str.19, 220072, Minsk (Belarus)

2014-11-28

The transparent conductive oxide films with controlled type of conduction are of great importance and their preparation is intensively studied. In our work, the preparation of such films based on doped ZnO was realized in order to achieve controlled type of conduction and high concentration of the charge carriers. Sol–gel method was used for films preparation and several dopants were tested (Sn, Li, Ni). Multilayer deposition was performed on several substrates: SiO{sub 2}/Si wafers, silica-soda-lime and/or silica glasses. The structural and morphological characterization of the obtained films were done by scanning electron microscopy, X-ray diffraction, X-ray fluorescence, X-ray photoelectron spectroscopy and atomic force microscopy respectively, while spectroscopic ellipsometry and transmittance measurements were done for determination of optical properties. The selected samples with the best structural, morphological and optical properties were subjected to electrical measurement (Hall and Seebeck effect). In all studied cases, samples with good adherence and homogeneous morphology as well as monophasic wurtzite type structure were obtained. The optical constants (refractive index and extinction coefficient) were calculated from spectroscopic ellipsometry data using Cauchy model. Films with n- or p-type conduction were obtained depending on the composition, number of deposition and thermal treatment temperature. - Highlights: • Transparent conductive ZnO based thin films were prepared by the sol–gel method. • Controlled type of conduction is obtained in (Sn, Li) doped and Li-Ni co-doped ZnO films. • Hall and Seebeck measurements proved the p-type conductivity for Li-Ni co-doped ZnO films. • The p-type conductivity was maintained even after 4-months of storage. • Influence of dopant- and substrate-type on the ZnO films properties was established.

Structural determinants for protein adsorption/non-adsorption to silica surface

International Nuclear Information System (INIS)

Mathe, Christelle; Devineau, Stephanie; Aude, Jean-Christophe; Lagniel, Gilles; Chedin, Stephane; Legros, Veronique; Mathon, Marie-Helene; Renault, Jean-Philippe; Pin, Serge; Boulard, Yves; Labarre, Jean

2013-01-01

The understanding of the mechanisms involved in the interaction of proteins with inorganic surfaces is of major interest in both fundamental research and applications such as nano-technology. However, despite intense research, the mechanisms and the structural determinants of protein/surface interactions are still unclear. We developed a strategy consisting in identifying, in a mixture of hundreds of soluble proteins, those proteins that are adsorbed on the surface and those that are not. If the two protein subsets are large enough, their statistical comparative analysis must reveal the physicochemical determinants relevant for adsorption versus non-adsorption. This methodology was tested with silica nanoparticles. We found that the adsorbed proteins contain a higher number of charged amino acids, particularly arginine, which is consistent with involvement of this basic amino acid in electrostatic interactions with silica. The analysis also identified a marked bias toward low aromatic amino acid content (phenylalanine, tryptophan, tyrosine and histidine) in adsorbed proteins. Structural analyses and molecular dynamics simulations of proteins from the two groups indicate that non-adsorbed proteins have twice as many p-p interactions and higher structural rigidity. The data are consistent with the notion that adsorption is correlated with the flexibility of the protein and with its ability to spread on the surface. Our findings led us to propose a refined model of protein adsorption. (authors)

Structural determinants for protein adsorption/non-adsorption to silica surface.

Directory of Open Access Journals (Sweden)

Christelle Mathé

Full Text Available The understanding of the mechanisms involved in the interaction of proteins with inorganic surfaces is of major interest in both fundamental research and applications such as nanotechnology. However, despite intense research, the mechanisms and the structural determinants of protein/surface interactions are still unclear. We developed a strategy consisting in identifying, in a mixture of hundreds of soluble proteins, those proteins that are adsorbed on the surface and those that are not. If the two protein subsets are large enough, their statistical comparative analysis must reveal the physicochemical determinants relevant for adsorption versus non-adsorption. This methodology was tested with silica nanoparticles. We found that the adsorbed proteins contain a higher number of charged amino acids, particularly arginine, which is consistent with involvement of this basic amino acid in electrostatic interactions with silica. The analysis also identified a marked bias toward low aromatic amino acid content (phenylalanine, tryptophan, tyrosine and histidine in adsorbed proteins. Structural analyses and molecular dynamics simulations of proteins from the two groups indicate that non-adsorbed proteins have twice as many π-π interactions and higher structural rigidity. The data are consistent with the notion that adsorption is correlated with the flexibility of the protein and with its ability to spread on the surface. Our findings led us to propose a refined model of protein adsorption.

Encapsulation of dye molecules into mesoporous polymer resin and mesoporous polymer-silica films by an evaporation-induced self-assembly method

Energy Technology Data Exchange (ETDEWEB)

Chi Yue; Li Nan; Tu Jinchun; Zhang Yujie [School of Material Science and Engineering, Key Laboratory of Automobile Materials of Ministry of Education, Jilin University, Changchun 130012 (China); Li Xiaotian, E-mail: xiaotianli@jlu.edu.c [School of Material Science and Engineering, Key Laboratory of Automobile Materials of Ministry of Education, Jilin University, Changchun 130012 (China); Shao Changlu, E-mail: clshao@nenu.edu.c [Center for Advanced Optoelectronic Functional Materials Research, Northeast Normal University, Changchun 130024 (China)

2010-03-15

Polymer resin and polymer-silica films with highly ordered mesostructure have been used as host materials to encapsulate DCM (4-(dicyanomethylene) -2-methyl-6-(4-dimethylaminostyryl)-4h-pyran), a kind of fluorescent dye, through evaporation-induced self-assembly method (EISA). After encapsulation, the composites show significant blue-shift in photoluminescence (PL) spectra. Particularly, by changing the excitation wavelength, the samples show different emission bands. These phenomena are related to the mesostructure and the positions of DCM molecules in the host.

The Pozzolanic reaction of silica fume

DEFF Research Database (Denmark)

Jensen, Ole Mejlhede

2012-01-01

Silica fume is a very important supplementary cementitious binder in High-Performance and Ultra High-Performance Concretes. Through its pozzolanic reaction the silica fume densifies the concrete micro-structure, in particular it strengthens the paste-aggregate interfacial transition zone. In the ......Silica fume is a very important supplementary cementitious binder in High-Performance and Ultra High-Performance Concretes. Through its pozzolanic reaction the silica fume densifies the concrete micro-structure, in particular it strengthens the paste-aggregate interfacial transition zone....... In the present paper different aspects of the pozzolanic reaction of silica fume are investigated. These include chemical shrinkage, isothermal heat development and strength development. Key data for these are given and compared with theoretical calculations, and based on presented measurements the energy...

Encapsulating Silica/Antimony into Porous Electrospun Carbon Nanofibers with Robust Structure Stability for High-Efficiency Lithium Storage.

Science.gov (United States)

Wang, Hongkang; Yang, Xuming; Wu, Qizhen; Zhang, Qiaobao; Chen, Huixin; Jing, Hongmei; Wang, Jinkai; Mi, Shao-Bo; Rogach, Andrey L; Niu, Chunming

2018-04-24

To address the volume-change-induced pulverization problems of electrode materials, we propose a "silica reinforcement" concept, following which silica-reinforced carbon nanofibers with encapsulated Sb nanoparticles (denoted as SiO 2 /Sb@CNFs) are fabricated via an electrospinning method. In this composite structure, insulating silica fillers not only reinforce the overall structure but also contribute to additional lithium storage capacity; encapsulation of Sb nanoparticles into the carbon-silica matrices efficiently buffers the volume changes during Li-Sb alloying-dealloying processes upon cycling and alleviates the mechanical stress; the porous carbon nanofiber framework allows for fast charge transfer and electrolyte diffusion. These advantageous characteristics synergistically contribute to the superior lithium storage performance of SiO 2 /Sb@CNF electrodes, which demonstrate excellent cycling stability and rate capability, delivering reversible discharge capacities of 700 mA h/g at 200 mA/g, 572 mA h/g at 500 mA/g, and 468 mA h/g at 1000 mA/g each after 400 cycles. Ex situ as well as in situ TEM measurements confirm that the structural integrity of silica-reinforced Sb@CNF electrodes can efficiently withstand the mechanical stress induced by the volume changes. Notably, the SiO 2 /Sb@CNF//LiCoO 2 full cell delivers high reversible capacities of ∼400 mA h/g after 800 cycles at 500 mA/g and ∼336 mA h/g after 500 cycles at 1000 mA/g.

Influence of the ammonium hydroxide concentration in morphological control of meso porous silica particles

International Nuclear Information System (INIS)

Yoon, Sukbon; Jung, Chonghun; Yoon, Inho; Kim, Changki; Choi, Wangkyu; Moon, Jeikwon

2012-01-01

The discovery of new M41S meso porous silica families in 1992 extended the applications into much wider pore ranges, bringing in a new prosperous era in porous material research. The synthesis of these meso porous silicas has been mainly accomplished through a self-assembly between surfactant molecules and inorganic species under various pH conditions. Meanwhile, many studies have been conducted on the application as catalysts, adsorbents, and packing materials for separation columns due to their unique properties such as high specific surface area, large pore volume, tuneable pore size, and narrow pore size distribution. The pore sizes of these materials can be easily controlled by changing the alkyl-chain length of the surfactant used. However, the control of the morphology and the pore structure is not so common. The morphological control of these materials in particular is one of the major challenges for their industrial application. Recently, the meso porous silica materials with various shapes such as fibers, films, polyhedral particles, and spheres have been reported. In our previous study, the core-shell nanoparticles with a silica core and a meso porous shell under basic conditions were synthesized using the silica nanoparticles as a core and tetraethyl orthosilicate (TEOS)-cetyltrimethylammonium bromide (CTABr)-NH 4 OH-H 2 O-C 2 H 5 OH system. In this work, we report the synthesis of the most well known hexagonal MCM-41 among three main mesophases in the M41S families using TEOS-CTABr-NH 4 OH-H 2 O system. Also, in the control of the morphology and pore structure of the meso porous silica materials, the influence of the NH 4 OH concentration was investigated

Thermally stable silica-coated hydrophobic gold nanoparticles.

Science.gov (United States)

Kanehara, Masayuki; Watanabe, Yuka; Teranishi, Toshiharu

2009-01-01

We have successfully developed a method for silica coating on hydrophobic dodecanethiol-protected Au nanoparticles with coating thickness ranging from 10 to 40 nm. The formation of silica-coated Au nanoparticles could be accomplished via the preparation of hydrophilic Au nanoparticle micelles by cationic surfactant encapsulation in aqueous phase, followed by hydrolysis of tetraethylorthosilicate on the hydrophilic surface of gold nanoparticle micelles. Silica-coated Au nanoparticles exhibited quite high thermal stability, that is, no agglomeration of the Au cores could be observed after annealing at 600 degrees C for 30 min. Silica-coated Au nanoparticles could serve as a template to derive hollow nanoparticles. An addition of NaCN solution to silica-coated Au nanoparticles led the formation of hollow silica nanoparticles, which were redispersible in deionized water. The formation of the hollow silica nanoparticles results from the mesoporous structures of the silica shell and such a mesoporous structure is applicable to both catalyst support and drug delivery.

Effect of nano silica based modifying agent for hydrophobic coating application

International Nuclear Information System (INIS)

Nurul Huda Mudri; Nik Ghazali Nik Salleh; Mek Zah Salleh

2016-01-01

Hydrophobic coatings find wide application in industry due to their unique features such as water repellent and self-cleaning properties. In this study, modifying agent was synthesized by way of nano silica particles dispersion in polydimethyl siloxane with addition of surfactant, catalyst and stabilizer using high speed distemper. The modifying agent was added into coating formulation and cured under UV exposure. Scanning Electron Microscopy image of the film found that the nano silica particles were distributed well on substrate. Contact angle measurement gave the highest reading of 116 degree for 20 % wt of the modifying agent. The optical properties of the film were evaluated via transmission and haze test. (author)

Coaxial carbon plasma gun deposition of amorphous carbon films

Science.gov (United States)

Sater, D. M.; Gulino, D. A.; Rutledge, S. K.

1984-01-01

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.

Coaxial carbon plasma gun deposition of amorphous carbon films

International Nuclear Information System (INIS)

Sater, D.M.; Gulino, D.A.

1984-03-01

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented

Preparation of resveratrol-loaded nanoporous silica materials with different structures

International Nuclear Information System (INIS)

Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

2014-01-01

Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol

Preparation of resveratrol-loaded nanoporous silica materials with different structures

Energy Technology Data Exchange (ETDEWEB)

Popova, Margarita, E-mail: mpopova@orgchem.bas.bg [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria); Szegedi, Agnes [Research Centre for Natural Sciences, Institute of Materials and Environmental Chemistry, Hungarian Academy of Sciences, 1117 Budapest, Magyar tudósok körútja 2. (Hungary); Mavrodinova, Vesselina [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria); Novak Tušar, Natasa [National Institute of Chemistry, Ljubljana (Slovenia); Mihály, Judith; Klébert, Szilvia [Research Centre for Natural Sciences, Institute of Materials and Environmental Chemistry, Hungarian Academy of Sciences, 1117 Budapest, Magyar tudósok körútja 2. (Hungary); Benbassat, Niko; Yoncheva, Krassimira [Faculty of Pharmacy, 2 Dunav Str., 1000 Sofia (Bulgaria)

2014-11-15

Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol.

Polymer-Silica Nanocomposites: A Versatile Platform for Multifunctional Materials

Science.gov (United States)

Chiu, Chi-Kai

Solution sol-gel synthesis is a versatile approach to create polymer-silica nanocomposite materials. The solution-to-solid transformation results in a solid consisting of interconnected nanoporous structure in 3D space, making it the ideal material for filtration, encapsulation, optics, electronics, drug release, and biomaterials, etc. Although the pore between nano and meso size may be tunable using different reaction conditions, the intrinsic properties such as limited diffusion within pore structure, complicated interfacial interactions at the pore surfaces, shrinkage and stress-induced cracking and brittleness have limited the applications of this material. To overcome these problems, diffusion, pore size, shrinkage and stress-induced defects need further investigation. Thus, the presented thesis will address these important questions such as whether these limitations can be utilized as the novel method to create new materials and lead to new applications. First, the behaviors of polymers such as poly(ethylene glycol) inside the silica pores are examined by studying the nucleation and growth of AgCl at the surface of the porous matrix. The pore structure and the pressure induced by the shrinkage affect have been found to induce the growth of AgCl nanocrystals. When the same process is carried out at 160 °C, silver metallization is possible. Due to the shrinkage-induced stresses, the polymer tends to move into open crack spaces and exterior surfaces, forming interconnected silver structure. This interconnected silver structure is very unique because its density is not related to the size scale of nanopore structures. These findings suggest that it is possible to utilize defect surface of silica material as the template to create interconnected silver structure. When the scale is small, polymer may no longer be needed if the diffusion length of Ag is more than the size of silica particles. To validate our assumption, monoliths of sol-gel sample containing AgNO3

Structural and Chemical Characterization of Silica Spheres before and after Modification by Silanization for Trypsin Immobilization

Directory of Open Access Journals (Sweden)

Eduardo F. Barbosa

2017-01-01

Full Text Available In the last decades, silica particles of a variety of sizes and shapes have been characterized and chemically modified for several applications, from chromatographic separation to dental supplies. The present study proposes the use of aminopropyl triethoxysilane (APTS silanized silica particles to immobilize the proteolytic enzyme trypsin for the development of a bioreactor. The major advantage of the process is that it enables the polypeptides hydrolysis interruption simply by removing the silica particles from the reaction bottle. Silanized silica surfaces showed significant morphological changes at micro- and nanoscale level. Chemical characterization showed changes in elemental composition, chemical environment, and thermal degradation. Their application as supports for trypsin immobilization showed high immobilization efficiency at reduced immobilization times, combined with more acidic conditions. Indirect immobilization quantification by reversed-phase ultrafast high performance liquid chromatography proved to be a suitable approach due to its high linearity and sensitivity. Immobilized trypsin activities on nonmodified and silanized silica showed promising features (e.g., selective hydrolysis for applications in proteins/peptides primary structure elucidation for proteomics. Silanized silica system produced some preferential targeting peptides, probably due to the hydrophobicity of the nanoenvironment conditioned by silanization.

Synthesis and Gas Transport Properties of Hyperbranched Polyimide–Silica Hybrid/Composite Membranes

Directory of Open Access Journals (Sweden)

Masako Miki

2013-12-01

Full Text Available Hyperbranched polyimide–silica hybrids (HBPI–silica HBDs and hyperbranched polyimide–silica composites (HBPI–silica CPTs were prepared, and their general and gas transport properties were investigated to clarify the effect of silica sources and preparation methods. HBPI–silica HBDs and HBPI–silica CPTs were synthesized by two-step polymerization of A2 + B3 monomer system via polyamic acid as precursor, followed by hybridizing or blending silica sources. Silica components were incorporated by the sol-gel reaction with tetramethoxysilane (TMOS or the addition of colloidal silica. In HBPI-silica HBDs, the aggregation of silica components is controlled because of the high affinity of HBPI and silica caused by the formation of covalent bonds between HBPI and silica. Consequently, HBPI-silica HBDs had good film formability, transparency, and mechanical properties compared with HBPI-silica CPTs. HBPI-silica HBD and CPT membranes prepared via the sol-gel reaction with TMOS showed specific gas permeabilities and permselectivities for CO2/CH4 separation, that is, both CO2 permeability and CO2/CH4 selectivity increased with increasing silica content. This result suggests that gas transport can occur through a molecular sieving effect of the porous silica network derived from the sol-gel reaction and/or through the narrow interfacial region between the silica networks and the organic matrix.

Film-thickness dependence of structure formation in ultra-thin polymer blend films

CERN Document Server

Gutmann, J S; Stamm, M

2002-01-01

We investigated the film-thickness dependence of structure formation in ultra-thin polymer blend films prepared from solution. As a model system we used binary blends of statistical poly(styrene-co-p-bromostyrene) copolymers of different degrees of bromination. Ultra-thin-film samples differing in miscibility and film thickness were prepared via spin coating of common toluene solutions onto silicon (100) substrates. The resulting morphologies were investigated with scanning force microscopy, reflectometry and grazing-incidence scattering techniques using both X-rays and neutrons in order to obtain a picture of the sample structure at and below the sample surface. (orig.)

Nanodrilling of fused silica using nanosecond laser radiation

Energy Technology Data Exchange (ETDEWEB)

Lorenz, P., E-mail: pierre.lorenz@iom-leipzig.de; Zajadacz, J.; Bayer, L.; Ehrhardt, M.; Zimmer, K.

2015-10-01

Graphical abstract: - Highlights: • Low-fluence irradiation of 10 nm Mo on SiO{sub 2} results in the formation of Mo droplets. • High-fluence irradiation of droplets results in the formation of holes in the SiO{sub 2}. • The process allows the formation of randomly distributed and periodic holes. • The randomly distributed hole density ρ{sub h} depends on the fluence (ρ{sub h} ≤ 1.3 μm{sup −2}). • The interaction of the laser beam with Mo/SiO{sub 2} was simulated by FEM. - Abstract: The fast laser drilling of dielectric surfaces with hole diameters in the sub-μm range and a high aspect ratio is a challenge for laser methods. In this study, a novel laser structuring method for the production of randomly and periodically distributed holes in a fused silica surface will be presented using a self-assembling process. A fused silica surface was covered with a 10 nm thick magnetron-sputtered molybdenum film. The metal film was irradiated by a KrF excimer laser (wavelength λ = 248 nm, pulse duration Δt{sub p} = 25 ns) with low laser fluences (Φ < 1 J/cm{sup 2}) and the laser-induced heating resulting in a melting of the metal film and finally in a self-assembled formation of randomly distributed metal droplets due to the surface tension of the metal liquid phase using a top hat beam profile. Furthermore, the usage of a periodically modulated laser beam profile allows the fabrication of periodically distributed droplet pattern. The multi-pulse irradiation of the laser-generated metal droplets with higher laser fluences results in a stepwise evaporation of the metal and in a partial evaporation of the fused silica near the metal droplets. Finally, the laser-induced stepwise evaporation process results in a formation of cone-like holes in the fused silica surface where the resultant holes are dependent on the size of the generated metal droplets and on the laser parameters. The “drilling” process allows the fabrication of holes with a depth up to 1 �

Preparation of resveratrol-loaded nanoporous silica materials with different structures

Science.gov (United States)

Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

2014-11-01

Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound.

Synthesis of Various Silica Nanoparticles for Foam Stability

International Nuclear Information System (INIS)

Yoon, Suk Bon; Yoon, Inho; Jung, Chonghun; Kim, Chorong; Choi, Wangkyu; Moon, Jeikwon

2013-01-01

The synthesis of the non-porous silica nanoparticles with uniform sizes has been reported through the Sto ber method, the synthesis of meso porous silica nanoparticles with a specific morphology such as core-shell, rod-like, and hexagonal shapes is not so common. As a synthetic strategy for controlling the particle size, shape, and porosity, the synthesis of core-shell silicas with meso porous shells formed on silica particle cores through the self-assembly of silica precursor and organic templates or spherical meso porous silicas using modified Sto ber method was also reported. Recently, in an effort to reduce the amount of radioactive waste and enhance the decontamination efficiency during the decontamination process of nuclear facilities contaminated with radionuclides, a few research for the preparation of the decontamination foam containing solid nanoparticles has been reported. In this work, the silica nanoparticles with various sizes, shapes, and structures were synthesized based on the previous literatures. The resulting silica nanoparticles were used to investigate the effect of the nanoparticles on the foam stability. In a study on the foam stability using various silica nanoparticles, the results showed that the foam volume and liquid volume in foam was enhanced when using a smaller size and lower density of the silica nanoparticles. Silica nanoparticles with various sizes, shapes, and structures such as a non-porous, meso porous core-shell, and meso porous silica were synthesized to investigate the effect of the foam stability. The sizes and structural properties of the silica nanoparticles were easily controlled by varying the amount of silica precursor, surfactant, and ammonia solution as a basic catalyst. The foam prepared using various silica nanoparticles showed that foam the volume and liquid volume in the foam were enhanced when using a smaller size and lower density of the silica nanoparticles

Synthesis of poly(ethylene oxide)-silica hybrids

International Nuclear Information System (INIS)

Ishak Manaf

2002-01-01

A hybrid material incorporating silica networks in poly (ethylene oxide) was produced using the sol-gel process from solution mixtures of poly (ethylene oxide) dissolved in water and partially polymerized tetraethylorthosilicate (TEOS) with and without compatibilisation agent. These mixtures were converted into films by solvent evaporation and drying them in an air-circulating oven at 60 degree C. Depending on the alkoxysilane solution composition and several mixing parameters, different morphologies were obtained, varying from semi-interpenetrating networks of PEO within highly cross linked silica chains, to finely dispersed heterogeneous system exhibiting either co-continuous or particulate microstructure. The influence of pH, type of solvents, mixing temperatures and time, as well as the nature of compatibiliser was found to be extremely important in controlling the morphology and properties of the fine hybrid films. It was found that compatibilisation of PEO-SiO 2 hybrid system is achieved exclusively with the use of γ-glycidyloxypropyltrimethoxysilane (GOTMS) coupling agent. (Author)

Fluctuations and structure of amphiphilic films

International Nuclear Information System (INIS)

Gourier, CH.

1996-01-01

This thesis is divided in three parts.The first part exposes in a theoretical point of view, how the fluctuations spectrum of an amphiphilic film is governed by its properties and its bidimensional characteristics.The measurements of fluctuations spectra of an interface are accessible with the measurement of intensity that interface diffuses out of the specular angle, we present in the second chapter the principles of the X rays diffusion by a real interface and see how the diffuse diffusion experiments allow to determine the fluctuations spectrum of an amphiphilic film. The second part is devoted to the different experimental techniques that have allowed to realize the study of fluctuation as well as the structural study.The third part is devoted to experimental results concerning the measurements of fluctuations spectra and to the study of the structure of amphiphilic films. We show that it is possible by using an intense source of X rays (ESRF: European Synchrotron Radiation Facility) to measure the water and amphiphilic films fluctuations spectra until molecular scales. The last chapter is devoted to the structural study and film fluctuations made of di-acetylenic molecules. (N.C.)

Water-insoluble Silk Films with Silk I Structure

Energy Technology Data Exchange (ETDEWEB)

Lu, Q.; Hu, X; Wang, X; Kluge, J; Lu, S; Cebe, P; Kaplan, D

2010-01-01

Water-insoluble regenerated silk materials are normally produced by increasing the {beta}-sheet content (silk II). In the present study water-insoluble silk films were prepared by controlling the very slow drying of Bombyx mori silk solutions, resulting in the formation of stable films with a predominant silk I instead of silk II structure. Wide angle X-ray scattering indicated that the silk films stabilized by slow drying were mainly composed of silk I rather than silk II, while water- and methanol-annealed silk films had a higher silk II content. The silk films prepared by slow drying had a globule-like structure at the core surrounded by nano-filaments. The core region was composed of silk I and silk II, surrounded by hydrophilic nano-filaments containing random turns and {alpha}-helix secondary structures. The insoluble silk films prepared by slow drying had unique thermal, mechanical and degradative properties. Differential scanning calorimetry results revealed that silk I crystals had stable thermal properties up to 250 C, without crystallization above the T{sub g}, but degraded at lower temperatures than silk II structure. Compared with water- and methanol-annealed films the films prepared by slow drying had better mechanical ductility and were more rapidly enzymatically degraded, reflecting the differences in secondary structure achieved via differences in post processing of the cast silk films. Importantly, the silk I structure, a key intermediate secondary structure for the formation of mechanically robust natural silk fibers, was successfully generated by the present approach of very slow drying, mimicking the natural process. The results also point to a new mode of generating new types of silk biomaterials with enhanced mechanical properties and increased degradation rates, while maintaining water insolubility, along with a low {beta}-sheet content.

Anomalous enthalpy relaxation in vitreous silica

DEFF Research Database (Denmark)

Yue, Yuanzheng

2015-01-01

scans. It is known that the liquid fragility (i.e., the speed of the viscous slow-down of a supercooled liquid at its Tg during cooling) has impact on enthalpy relaxation in glass. Here, we find that vitreous silica (as a strong system) exhibits striking anomalies in both glass transition and enthalpy...... relaxation compared to fragile oxide systems. The anomalous enthalpy relaxation of vitreous silica is discovered by performing the hyperquenching-annealing-calorimetry experiments. We argue that the strong systems like vitreous silica and vitreous Germania relax in a structurally cooperative manner, whereas...... the fragile ones do in a structurally independent fashion. We discuss the origin of the anomalous enthalpy relaxation in the HQ vitreous silica....

Synthesis and properties of highly dispersed ionic silica-poly(ethylene oxide) nanohybrids.

KAUST Repository

Fernandes, Nikhil J; Akbarzadeh, Johanna; Peterlik, Herwig; Giannelis, Emmanuel P

2013-01-01

We report an ionic hybrid based on silica nanoparticles as the anion and amine-terminated poly(ethylene oxide) (PEO) as a cation. The charge on the nanoparticle anion is carried by the surface hydroxyls. SAXS and TEM reveal an exceptional degree of dispersion of the silica in the polymer and high degree of order in both thin film and bulk forms. In addition to better dispersion, the ionic hybrid shows improved flow characteristics compared to silica/PEO mixtures in which the ionic interactions are absent.

Synthesis and properties of highly dispersed ionic silica-poly(ethylene oxide) nanohybrids.

KAUST Repository

Fernandes, Nikhil J

2013-02-04

We report an ionic hybrid based on silica nanoparticles as the anion and amine-terminated poly(ethylene oxide) (PEO) as a cation. The charge on the nanoparticle anion is carried by the surface hydroxyls. SAXS and TEM reveal an exceptional degree of dispersion of the silica in the polymer and high degree of order in both thin film and bulk forms. In addition to better dispersion, the ionic hybrid shows improved flow characteristics compared to silica/PEO mixtures in which the ionic interactions are absent.

Effects of film thickness on scintillation characteristics of columnar CsI:Tl films exposed to high gamma radiation doses

Energy Technology Data Exchange (ETDEWEB)

Shinde, Seema; Singh, S.G.; Sen, S.; Gadkari, S.C., E-mail: gadkari@barc.gov.in

2016-02-21

Oriented columnar films of Tl doped CsI (CsI:Tl) of varying thicknesses from 50 µm to 1000 µm have been deposited on silica glass substrates by a thermal evaporation technique. The SEM micrographs confirmed the columnar structure of the film while the powder X-ray diffraction pattern recorded for the films revealed a preferred orientation of the grown columns along the <200> direction. Effects of high energy gamma exposure up to 1000 Gy on luminescence properties of the films were investigated. Results of radio-luminescence, photo-luminescence and scintillation studies on the films are compared with those of a CsI:Tl single crystal with similar thickness. A possible correlation between the film thicknesses and radiation damage in films has been observed. - Highlights: • CsI:Tl films of different thicknesses deposited for γ and α detection. • Pulse-height spectra found to degrade with increasing thickness. • Radiation damage is found more in films than single crystal of comparable thickness. • Detection efficiency increases for γ while it is invariant for α beyond 50 µm.

Effects of film thickness on scintillation characteristics of columnar CsI:Tl films exposed to high gamma radiation doses

International Nuclear Information System (INIS)

Shinde, Seema; Singh, S.G.; Sen, S.; Gadkari, S.C.

2016-01-01

Oriented columnar films of Tl doped CsI (CsI:Tl) of varying thicknesses from 50 µm to 1000 µm have been deposited on silica glass substrates by a thermal evaporation technique. The SEM micrographs confirmed the columnar structure of the film while the powder X-ray diffraction pattern recorded for the films revealed a preferred orientation of the grown columns along the direction. Effects of high energy gamma exposure up to 1000 Gy on luminescence properties of the films were investigated. Results of radio-luminescence, photo-luminescence and scintillation studies on the films are compared with those of a CsI:Tl single crystal with similar thickness. A possible correlation between the film thicknesses and radiation damage in films has been observed. - Highlights: • CsI:Tl films of different thicknesses deposited for γ and α detection. • Pulse-height spectra found to degrade with increasing thickness. • Radiation damage is found more in films than single crystal of comparable thickness. • Detection efficiency increases for γ while it is invariant for α beyond 50 µm.

Synthesis of multilayered structure of nano-dimensional silica glass/reduced graphene oxide for advanced electrochemical applications.

Science.gov (United States)

Ghosh, Arnab; Miah, Milon; Majumder, Chinmoy; Bag, Shekhar; Chakravorty, Dipankar; Saha, Shyamal Kumar

2018-03-28

During the past few years, intensive research has been carried out to design new functional materials for superior electrochemical applications. Due to low storage capacity and low charge transport, silica based glasses have not yet been investigated for their supercapacitive behavior. Therefore, in the present study, a multilayered structure of silica-based nanoglass and reduced graphene oxide has been designed to remarkably enhance the specific capacitance by exploiting the porosity, large surface area, sufficient dangling bonds in the nanoglass and high electrical conductivity of rGO. The charge transport in the composite structure is also investigated to understand the electrochemical properties. It is found that Simmons tunneling or direct tunneling is the dominant mechanism of charge conduction between the graphene layers via the potential barrier of silica nanoglass phase. We believe that this study will open up a new area in the design of glass-based two-dimensional nanocomposites for superior supercapacitor applications.

Structural and magnetic study of CoCr{sub 2}O{sub 4} thin films obtained by employing the sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Del Toro, A.D.; Garcia, R.P.; Davila, Y.G.; Gomes, J.L.; Goncalves, L.P.; Hernandez, E.P. [Universidade Federal de Pernambuco (UFPE), PE (Brazil)

2016-07-01

Full text: In this work we made a study about the structural and magnetic properties of cobalt chromite. We obtained samples in a film format and also in chromite nanopowder. Both, the powder and films were fabricated by the sol-gel chemical method, the film were deposited by the spin coating technique followed by an appropriate heat treatment at 500 °C. The used substrate was glass based on silica and we studied the rotating speed parameter during deposition. The initial aim of the work was the study of the influence of rotating speed on the quality of cromite films. The crystallinity of samples was confirmed by diffraction X-ray (XRD). The lattice parameters were determined using the Rietveld method from which we calculate grain size of 8.6 nm. The scanning electron microscopy (SEM) showed granular films with good homogeneity and we observed the dependence of the rotating speed on the quality of the deposited films. The magnetic properties were measured using a vibrating sample magnetometer (VSM). For powder samples we obtained Curie temperature of 94 K, which is a phase transition from ferrimagnetic to paramagnetic. The applied magnetic field during in the characterization of the film was oriented parallel to the plane of the substrate and we observed a high coercivity. The Curie temperature value for the films was 93 K, similar to the powder samples. (author)

Growth of ZnO nanocrystals in silica by rf co-sputter deposition and post-annealing

International Nuclear Information System (INIS)

Siva Kumar, V.V.; Singh, F.; Kumar, Amit; Avasthi, D.K.

2006-01-01

Thin films with ZnO nanocrystals in silica were synthesized by rf reactive magnetron co-sputter deposition and post-annealing. The films were deposited from a ZnO/Si composite target in an rf oxygen plasma. The deposited films were annealed in air/vacuum at high temperatures to grow ZnO nanocrystals. The deposited and annealed films were characterized by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), uv-vis spectroscopy (UV-VIS) and photoluminescence (PL) measurements. FT-IR results of the films show the vibrational features of Si-O-Si and Zn-O bonds. UV-VIS spectra of the deposited film shows the band edge of ZnO. The XRD results of the films annealed at 750 deg. C and 1000 deg. C indicate the growth of ZnO nanocrystals with average crystallite sizes between 7 nm and 26 nm. PL measurements of the deposited film show a broad visible luminescence peak which can be due to ZnO. These results suggest the growth of ZnO nanocrystals in silica matrix

Improving structural stability of water-dispersed MCM-41 silica nanoparticles through post-synthesis pH aging process

Energy Technology Data Exchange (ETDEWEB)

Varache, Mathieu; Bezverkhyy, Igor [UMR 6303 CNRS-Université Bourgogne Franche-Comté, Laboratoire Interdisciplinaire Carnot de Bourgogne (France); Bouyer, Florence [Inserm U866, Equipe Chimiothérapie, métabolisme des lipides et réponse immunitaire anti-tumorale (France); Chassagnon, Rémi; Baras, Florence; Bouyer, Frédéric, E-mail: frederic.bouyer@u-bourgogne.fr [UMR 6303 CNRS-Université Bourgogne Franche-Comté, Laboratoire Interdisciplinaire Carnot de Bourgogne (France)

2015-09-15

The colloidal and structural stabilities of MCM-41 mesoporous silica nanoparticles (MSNs) are of great importance in order to prepare optimal nanovectors. In this paper, MSNs (approximatively 160 nm in diameter) were synthesized using n-cetyltrimethylammonium bromide as a template and tetraethyl orthosilicate as a silica source under high N{sub 2} flow (MSN/N{sub 2}) to obtain stable dispersions in water. The degradation of the porous nanoparticles was investigated by immersion in water. The morphology and the porous structure were studied by TEM, XRD, N{sub 2} sorption, and {sup 29}Si MAS NMR and were compared to that of MSNs prepared in ambient air (MSN/air). The volumetric properties of the MSN/N{sub 2} after 1 day in water were drastically more decreased than MSN/air (a pore volume decrease of 85 % for MSN/N{sub 2} and 59 % for MSN/air) and the 2D-hexagonal porous structure was totally lost. Furthermore, synthesizing MSNs under a high N{sub 2} flow leads to a decrease in the synthesis yield (45 % MSN/N{sub 2} and 75 % for MSN/air). The lower structural stability of the MSN/N{sub 2} is explained by the lower polycondensation degree of the MSN/N{sub 2} observed by {sup 29}Si MAS NMR (Q{sup 4}/Q{sup 3} = 0.86 for MSN/N{sub 2} and 1.61 for MSN/air) and the lower silica molar ratio in the nanomaterials (SiO{sub 2}/CTA = 3.9 for MSN/N{sub 2} 7.1 for MSN/air). This allows for enhanced solubilization of silica in water. Four strategies were hence evaluated in order to reinforce the porous structure of the MSNs. Among them, the most efficient route was based on a pH adjustment of the colloidal suspension (pH 7.5) after 2 h of synthesis without any purification and while keeping a N{sub 2} static atmosphere (called MSN/N{sub 2}/7.5). After 1 day in water, the volumetric and structural properties of MSN/N{sub 2}/7.5 were similar to that obtained for MSN/air. The improvement of the stability arose as a result of the increase in the silica condensation (Q{sup 4

Structures of sub-monolayered silicon carbide films

International Nuclear Information System (INIS)

Baba, Y.; Sekiguchi, T.; Shimoyama, I.; Nath, Krishna G.

2004-01-01

The electronic and geometrical structures of silicon carbide thin films are presented. The films were deposited on graphite by ion-beam deposition using tetramethylsilane (TMS) as an ion source. In the Si K-edge near-edge X-ray absorption fine structure (NEXAFS) spectra for sub-monolayered film, sharp peaks due to the resonance from Si 1s to π*-like orbitals were observed, suggesting the existence of Si=C double bonds. On the basis of the polarization dependencies of the Si 1s → π* peak intensities, it is elucidated that the direction of the π*-like orbitals is just perpendicular to the surface. We conclude that the sub-monolayered SiC x film has a flat-lying hexagonal structure of which configuration is analogous to the single sheet of graphite

Characterization of silica particles prepared via urease-catalyzed urea hydrolysis and activity of urease in sol–gel silica matrix

International Nuclear Information System (INIS)

Kato, Katsuya; Nishida, Masakazu; Ito, Kimiyasu; Tomita, Masahiro

2012-01-01

Highlights: ► Silica precipitation occurred via urease-catalytic reactions. ► Higher urease activity for silica synthesis enables mesostructure of silica–urease composites. ► Urease encapsulating in silica matrix retained high activity. - Abstract: Urease templated precipitation of silica synthesized by sol–gel chemistry produces a composite material allowing high urease activity. This study investigates the structural properties of the composite material that allow for the retention of the urease hydrolysis activity. Scanning (SEM) and transmission (TEM) electron microscopy reveal that the composite has a mesoporous structure composed of closely packed spherical structures ∼20–50 nm in diameter. Brunauer–Emmett–Teller (BET) analysis revealed that the surface area and pore volume of the composite prepared under the conditions of 50 mM urea and 25 °C is relatively high (324 m 2 /g and 1.0 cm 3 /g). These values are equivalent to those of usual mesoporous silica materials synthesized from the self-assembly of triblock copolymers as organic templates. In addition, after encapsulating in a sol–gel silica matrix, urease retained high activity (∼90% of the activity compared with native urease). Our results suggest a new method for synthesizing mesoporous silica materials with highly tunable pore sizes and shapes under mild conditions.

Nonionic Fluorinated Surfactant Removal from Mesoporous Film Using sc-CO2.

Science.gov (United States)

Chavez Panduro, Elvia A; Assaker, Karine; Beuvier, Thomas; Blin, Jean-Luc; Stébé, Marie-José; Konovalov, Oleg; Gibaud, Alain

2017-01-25

Surfactant templated silica thin films were self-assembled on solid substrates by dip-coating using a partially fluorinated surfactant R 8 F (EO) 9 as the liquid crystal template. The aim was 2-fold: first we checked which composition in the phase diagram was corresponding to a 2D rectangular highly ordered crystalline phase and second we exposed the films to sc-CO 2 to foster the removal of the surfactant. The films were characterized by in situ X-ray reflectivity (XRR) and grazing incidence small angle X-ray scattering (GISAXS) under CO 2 pressure from 0 to 100 bar at 34 °C. GISAXS patterns reveal the formation of a 2-D rectangular structure at a molar ratio R 8 F (EO) 9 /Si equal to 0.1. R 8 F (EO) 9 micelles have a cylindrical shape, which have a core/shell structure ordered in a hexagonal system. The core contains the R 8 F part and the shell is a mixture of (EO) 9 embedded in the silica matrix. We further evidence that the extraction of the template using supercritical carbon dioxide can be successfully achieved. This can be attributed to both the low solubility parameter of the surfactants and the fluorine and ethylene oxide CO 2 -philic groups. The initial 2D rectangular structure was well preserved after depressurization of the cell and removal of the surfactant. We attribute the very high stability of the rinsed film to the large value of the wall thickness relatively to the small pore size.

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.

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.

Alternative nano-structured thin-film materials used as durable thermal nanoimprint lithography templates

Science.gov (United States)

Bossard, M.; Boussey, J.; Le Drogoff, B.; Chaker, M.

2016-02-01

Nanoimprint templates made of diamond-like carbon (DLC) and amorphous silicon carbide (SiC) thin films and fluorine-doped associated materials, i.e. F-DLC and F-SiC were investigated in the context of thermal nanoimprint lithography (NIL) with respect to their release properties. Their performances in terms of durability and stability were evaluated and compared to those of conventional silicon or silica molds coated with antisticking molecules applied as a self-assembled monolayer. Plasma-enhanced chemical vapor deposition parameters were firstly tuned to optimize mechanical and structural properties of the DLC and SiC thin films. The impact of the amount of fluorine dopant on the deposited thin films properties was then analyzed. A comparative analysis of DLC, F-DLC as well as SiC and F-SiC molds was then carried out over multiple imprints, performed into poly (methyl methacrylate) (PMMA) thermo-plastic resist. The release properties of un-patterned films were evaluated by the measurement of demolding energies and surface energies, associated with a systematic analysis of the mold surface contamination. These analyses showed that the developed materials behave as intrinsically easy-demolding and contamination-free molds over series of up to 40 imprints. To our knowledge, it is the first time that such a large number of imprints has been considered within an exhaustive comparative study of materials for NIL. Finally, the developed materials went through standard e-beam lithography and plasma etching processes to obtain nanoscale-patterned templates. The replicas of those patterned molds, imprinted into PMMA, were shown to be of high fidelity and good stability after several imprints.

Silica Nanoparticles Functionalized with Zwitterionic Sulfobetaine Siloxane for Application as a Versatile Antifouling Coating System.

Science.gov (United States)

Knowles, Brianna R; Wagner, Pawel; Maclaughlin, Shane; Higgins, Michael J; Molino, Paul J

2017-06-07

The growing need to develop surfaces able to effectively resist biological fouling has resulted in the widespread investigation of nanomaterials with potential antifouling properties. However, the preparation of effective antifouling coatings is limited by the availability of reactive surface functional groups and our ability to carefully control and organize chemistries at a materials' interface. Here, we present two methods of preparing hydrophilic low-fouling surface coatings through reaction of silica-nanoparticle suspensions and predeposited silica-nanoparticle films with zwitterionic sulfobetaine (SB). Silica-nanoparticle suspensions were functionalized with SB across three pH conditions and deposited as thin films via a simple spin-coating process to generate hydrophilic antifouling coatings. In addition, coatings of predeposited silica nanoparticles were surface functionalized via exposure to zwitterionic solutions. Quartz crystal microgravimetry with dissipation monitoring was employed as a high throughput technique for monitoring and optimizing reaction to the silica-nanoparticle surfaces. Functionalization of nanoparticle films was rapid and could be achieved over a wide pH range and at low zwitterion concentrations. All functionalized particle surfaces presented a high degree of wettability and resulted in large reductions in adsorption of bovine serum albumin protein. Particle coatings also showed a reduction in adhesion of fungal spores (Epicoccum nigrum) and bacteria (Escherichia coli) by up to 87 and 96%, respectively. These results indicate the potential for functionalized nanosilicas to be further developed as versatile fouling-resistant coatings for widespread coating applications.

Concentration of small ring structures in vitreous silica from a first-principles analysis of the Raman spectrum.

Science.gov (United States)

Umari, P; Gonze, Xavier; Pasquarello, Alfredo

2003-01-17

Using a first-principles approach, we calculate Raman spectra for a model structure of vitreous silica. We develop a perturbational method for calculating the dielectric tensor in an ultrasoft pseudopotential scheme and obtain Raman coupling tensors by finite differences with respect to atomic displacements. For frequencies below 1000 cm(-1), the parallel-polarized Raman spectrum of vitreous silica is dominated by oxygen bending motions, showing a strong sensitivity to the intermediate range structure. By modeling the Raman coupling, we derive estimates for the concentrations of three- and four-membered rings from the experimental intensities of the Raman defect lines.

Growth, structure, and optical properties of carbon-reinforced silica fibers

International Nuclear Information System (INIS)

Zhang, Z. J.; Ajayan, P. M.; Ramanath, G.; Vacik, J.; Xu, Y. H.

2001-01-01

We report the synthesis of carbon-reinforced silica fibers by methane exposure of metallocene-treated oxidized-Si(001) substrates at 1100 degree C. The SiO 2 cap layer transforms into silica fibers reinforced by glassy carbon in the core during methane exposure. High-resolution electron microscopy and spatially resolved spectroscopy measurements of the fibers reveal an amorphous structure without a hollow, and domains of glassy carbon embedded at the fiber core. The carbon-reinforced fibers are optically transparent and have an optical band gap of ≅3.1 eV. These fibers are organized in radial patterns that vary for different metallocene species. On nickelocene-treated substrates, the fibers originate from the circumference of the circular templates and grow outwards, forming radial patterns. On ferrocene-treated substrates, randomly oriented fibers grow within as well as slightly outside the perimeter of the templates, forming wreath-like patterns. Aligned growth of such fibers could be useful for fabricating optoelectronics devices and reinforced composites. [copyright] 2001 American Institute of Physics

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.

Nanoporous silica membranes with high hydrothermal stability

DEFF Research Database (Denmark)

Boffa, Vittorio; Magnacca, Giualiana; Yue, Yuanzheng

to improve the stability of nanoporous silica structure. This work is a quantitative study on the impact of type and concentration of transition metal ions on the microporous structure and stability of amorphous silica-based membranes, which provides information on how to design chemical compositions...

Construction of proton exchange membranes under ultrasonic irradiation based on novel fluorine functionalizing sulfonated polybenzimidazole/cellulose/silica bionanocomposite.

Science.gov (United States)

Esmaielzadeh, Sheida; Ahmadizadegan, Hashem

2018-03-01

Novel sulfonated polybenzimidazole (s-PBI)/cellulose/silica bionanocomposite membranes were prepared from fluorine-containing s-PBI copolymer with a cellulose/silica precursor and a bonding agent. The introduction of the bonding agent results in the reinforcing interfacial interaction between s-PBI chains and the cellulose/silica nanoparticles. Commercially available silica nanoparticles were modified with biodegradable nanocellolose through ultrasonic irradiation technique. Transmission electron microscopy (TEM) analyses showed that the cellulose/silica composites were well dispersed in the s-PBI matrix on a nanometer scale. The mechanical properties and the methanol barrier ability of the s-PBI films were improved by the addition of cellulose/silica. The modulus of the s-PBI/10 wt% cellulose/silica nanocomposite membranes had a 45% increase compared to the pure s-PBI films, and the methanol permeability decreased by 62% with respect to the pure s-PBI membranes. The conductivities of the s-PBI/cellulose/silica nanocomposites were slightly lower than the pure s-PBI. The antibacterial activity of (s-PBI)/cellulose/silica was investigated against Gram-positive bacteria, ie, Staphylococcus aureus and methicillin-resistant S. aureus and Gram-negative bacteria, ie, Escherichia coli, E. coli O157:H7 and Pseudomonas aeruginosa by the disc diffusion method using Mueller Hinton agar at different sizes of cellulose/silica. All of the synthesized (s-PBI)/cellulose/silica were found to have high antibacterial activity. Copyright © 2017 Elsevier B.V. All rights reserved.

Influence of organic solvents on interfacial water at surfaces of silica gel and partially silylated fumed silica

International Nuclear Information System (INIS)

Turov, V.V.; Gun'ko, V.M.; Tsapko, M.D.; Bogatyrev, V.M.; Skubiszewska-Zieba, J.; Leboda, R.; Ryczkowski, J.

2004-01-01

The effects of organic solvents (dimethylsulfoxide-d 6 (DMSO-d 6 ), chloroform-d, acetone-d 6 , and acetonitrile-d 3 ) on the properties of interfacial water at surfaces of silica gel Si-40 and partially silylated fumed silica A-380 were studied by means of the 1 H NMR spectroscopy with freezing-out of adsorbed water at 180 1 H NMR investigations were also analysed on the basis of the structural characteristics of silicas and quantum chemical calculations of the chemical shifts δ H and solvent effects. DMSO-d 6 and acetonitrile-d 3 are poorly miscible with water in silica gel pores in contrast to the bulk liquids. DMSO-d 6 and chloroform-d affect the structure of the interfacial water weaker than acetone-d 6 and acetonitrile-d 3 at amounts of liquids greater than the pore volume. Acetone-d 6 and acetonitrile-d 3 can displace water from pores under this condition. The chemical shift of protons in water adsorbed on silica gel is 3.5-6.5 ppm, which corresponds to the formation of two to four hydrogen bonds per molecule. Water adsorbed on partially silylated fumed silica has two 1 H NMR signals at 5 and 1.1-1.7 ppm related to different structures (droplets and small clusters) of the interfacial water

Spectroscopic studies of organic-inorganic composite film cured by low energy electron beam

International Nuclear Information System (INIS)

Mahathir Mohamed; Dahlan Mohd; Ibrahim Abdullah; Eda Yuhana Ariffin

2009-01-01

Liquid epoxidized natural rubber acrylate (LENRA) film was reinforced with silica particles formed in-situ via sol gel process. Combination of these two components produces organic-inorganic composites. Tetraethyl orthosilicate (TEOS) was used as precursor material for silica generation. Sol gel reactions was carried out at different concentrations of TEOS i.e. between 10 and 50 phr. The compounds that contain silica were crosslinked by electron beam. Structural properties studies were carried out by Fourier Transform Infrared Spectrometer (FTIR). It was found that miscibility between organic and inorganic components improved with the presence of silanol groups (Si-OH) and polar solvent i.e. THF, via hydrogen bonding formation between siloxane and LENRA. Morphology study by the transmission electron microscopy (TEM) and scanning electron microscopy (SEM) showed in-situ generated silica particles were homogenous and well dispersed at any concentrations of TEOS. (author)

Structural and optical characterization of the propolis films

Energy Technology Data Exchange (ETDEWEB)

Drapak, S.I. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine)]. E-mail: drapak@unicom.cv.ua; Bakhtinov, A.P. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine); Gavrylyuk, S.V. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine); Drapak, I.T. [Chernivtsi National University, 2 Kotsyubynskii Str., 58012 Chernivtsi (Ukraine); Kovalyuk, Z.D. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine)

2006-10-31

We have performed structural and optical characterizations of the propolis (an organic entity of biological nature) films grown on various non-organic substrates. The films were grown from a propolis melt or a propolis alcohol solution. The crystal structure has been observed in the films precipitated from the solution onto substrates such as an amorphous glass and sapphire or semiconductor indium monoselenide. For any growth method, the propolis film is a semiconductor with the bandgap of 3.07 eV at 300 K that is confirmed by a maximum in photoluminescence spectra at 2.86 eV. We argue that propolis films might be used in various optoelectronic device applications.

Significance of Alkali-Silica reaction in nuclear safety-related concrete structures

International Nuclear Information System (INIS)

Le Pape, Y.; Field, K.G.; Mattus, C.H.; Naus, D.J.; Busby, J.T.; Saouma, V.; Ma, Z.J.; Cabage, J.V.; Guimaraes, M.

2015-01-01

Nuclear Power Plant license renewal up to 60 years and possible life extension beyond has established a renewed focus on long-term aging of nuclear generating stations materials, and particularly, on concrete. Large irreplaceable sections of most nuclear generating stations include concrete components. The Expanded Materials Degradation Analysis, jointly performed by the Department of Energy, the U.S. Nuclear Regulatory Commission, the Academia and the Power Generation Industry, identified the need to develop a consistent knowledge base of alkali-silica reaction (ASR) within concrete as an urgent priority (Graves et al., 2014). ASR results in an expansion of Concrete produced by the reaction between alkali (generally from cement), reactive aggregate (like amorphous silica) and water absorption. ASR causes expansion, cracking and loss of mechanical properties. Considering that US commercial reactors in operation enter the age when ASR distress can be potentially observed and that numerous non-nuclear infrastructures (transportation, energy production) in a majority of the States have already experienced ASR-related concrete degradation, the susceptibility and significance of ASR for nuclear concrete structures must be addressed. This paper outlines an on-going research program including the investigation of the possibility of ASR in nuclear power plants, and the assessment of the residual shear bearing capacity of ASR-subjected nuclear structures. (authors)

Orientationally ordered ridge structures of aluminum films on hydrogen terminated silicon

DEFF Research Database (Denmark)

Quaade, Ulrich; Pantleon, Karen

2006-01-01

Films of aluminum deposited onto Si(100) substrates show a surface structure of parallel ridges. On films deposited on oxidized silicon substrates the direction of the ridges is arbitrary, but on films deposited on hydrogen-terminated Si(100) the ridges are oriented parallel to the < 110 > direct......Films of aluminum deposited onto Si(100) substrates show a surface structure of parallel ridges. On films deposited on oxidized silicon substrates the direction of the ridges is arbitrary, but on films deposited on hydrogen-terminated Si(100) the ridges are oriented parallel to the ... > directions on the silicon substrate. The ridge structure appears when the film thickness is above 500 nm, and increasing the film thickness makes the structure more distinct. Anodic oxidation enhances the structure even further. X-ray diffraction indicates that grains in the film have mostly (110) facets...

Optical Degradation of Colloidal Eu-Complex Embedded in Silica Glass Film Using Reprecipitation and Sol-Gel Methods.

Science.gov (United States)

Fukuda, Takeshi; Kurabayashi, Tomokazu; Yamaki, Tatsuki

2016-04-01

A reprecipitation method has been investigated for fabricating colloidal nanoparticles using Eu-complex. Herein, we investigated optical degradation characteristics of (1,10-phenanthroline)tris [4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedionato]europium(III) colloidal nanoparticles, which were embedded into a silica glass film fabricated by a conventional sol-gel process. At first, we tried several types of good solvents for the reprecipitation method, and dimethyl sulfoxide (DMSO) is found to be a suitable solvent for realizing the small diameter and the high long-term stability against the ultraviolet irradiation even though the boing point of DMSO is higher than that of water used as a poor solvent. By optimizing the good solvent and the concentration of Eu-complex, the relative photoluminescence intensity of 0.96 was achieved even though the ultraviolet light was continuously irradiated for 90 min. In addition, the average diameter of 106 nm was achieved when DMSO was used as a good solvent, resulting in the high transmittance at a visible wavelength region. Therefore, we can achieve the transparent emissive thin film with a center wavelength of 612 nm, and the optical degradation was drastically reduced by forming nanoparticles.

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.

Infrared Spectroscopic Study on Structural Change and Interfacial Interaction in Rubber Composites Filled with Silica-Kaolin Hybrid Fillers

Science.gov (United States)

Chen, Y.; Guan, J.; Hu, H.; Gao, H.; Zhang, L.

2016-07-01

A series of natural rubber/styrene butadiene rubber/polybutadiene rubber composites was prepared with nanometer silica and micron kaolin by a dry modification process, mechanical compounding, and mold vulcanization. Fourier transform infrared spectroscopy and a scanning electron microscope were used to investigate the structural changes and interfacial interactions in composites. The results showed that the "seesaw" structure was formed particularly with the incorporation of silica particles in the preparation process, which would be beneficial to the dispersibility of fillers in the rubber matrix. The kaolinite platelets were generally arranged in directional alignment. Kaolinite with smaller particle size and low-defect structure was more stable in preparation, but kaolinite with larger particle size and high defect structure tended to change the crystal structure. The composite prepared in this research exhibited excellent mechanical and thermal properties.

Reaction kinetics for preparation of silica film with Stoeber method

International Nuclear Information System (INIS)

Shang Mengying; Jiang Xiaodong; Liu Miao; Luo Xuan; Tang Yongjian; Cao Linhong

2013-01-01

A new formula was proposed to investigate the relationship between reaction time and tetraethylorthosilicate (TEOS) conversion rate for preparation of silica sol with Stöber method, by studying the reaction kinetics of TEOS hydrolytic process. An appropriate conversion rate was then determined and used to calculate the theoretical optimal reaction time. Meanwhile, silica sols were prepared by sol-gel process using TEOS as precursor and ammonia as catalyst. It was found that the reaction time decreases with an increasing amount of ammonia and water. The values of experimental optimal reaction time were obtained, and agree with the theoretical results (the errors are within 5%), which shows good applicability of our formula. (authors)

Pressure dependence of the interfacial structure of potassium chloride films on iron

International Nuclear Information System (INIS)

Olson, Dustin; Gao, Hongyu; Tang, Chun; Tysoe, Wilfred T.; Martini, Ashlie

2015-01-01

Potassium chloride films on a clean iron surface are used as a model system to explore the interfacial structure of the films and the dependence of that structure on film thickness and pressure. The interfacial structure of one-, two-, three- and four-layer films is measured experimentally using low-energy electron diffraction. Those findings are then complemented by molecular dynamics simulations in which the atomic interaction between the film and substrate is tuned to match film thickness-dependent sublimation activation energy obtained from temperature-programmed desorption measurements. The resultant simulation reliably predicts the structure of thicker films and is then used to study the effect of pressure on the distribution of the lattice constant within and between each layer of the potassium chloride films. Findings indicate that both film thickness and pressure affect the structure within the films as well as the degree of registry between the film and adjacent substrate. - Highlights: • KCl films on an Fe surface are used as a model system to explore interfacial structure • Thin film structure is measured using low-energy electron diffraction • An empirical potential is tuned to match sublimation activation energy • Simulations reveal the effect of pressure on the lattice constant within the KCl films • Pressure affects the film structure and registry between film and substrate

Pressure dependence of the interfacial structure of potassium chloride films on iron

Energy Technology Data Exchange (ETDEWEB)

Olson, Dustin [Department of Chemistry and Laboratory for Surface Studies, University of Wisconsin—Milwaukee, Milwaukee, WI 53211 (United States); Gao, Hongyu; Tang, Chun [School of Engineering, University of California Merced, Merced CA 95343 (United States); Tysoe, Wilfred T. [Department of Chemistry and Laboratory for Surface Studies, University of Wisconsin—Milwaukee, Milwaukee, WI 53211 (United States); Martini, Ashlie [School of Engineering, University of California Merced, Merced CA 95343 (United States)

2015-10-30

Potassium chloride films on a clean iron surface are used as a model system to explore the interfacial structure of the films and the dependence of that structure on film thickness and pressure. The interfacial structure of one-, two-, three- and four-layer films is measured experimentally using low-energy electron diffraction. Those findings are then complemented by molecular dynamics simulations in which the atomic interaction between the film and substrate is tuned to match film thickness-dependent sublimation activation energy obtained from temperature-programmed desorption measurements. The resultant simulation reliably predicts the structure of thicker films and is then used to study the effect of pressure on the distribution of the lattice constant within and between each layer of the potassium chloride films. Findings indicate that both film thickness and pressure affect the structure within the films as well as the degree of registry between the film and adjacent substrate. - Highlights: • KCl films on an Fe surface are used as a model system to explore interfacial structure • Thin film structure is measured using low-energy electron diffraction • An empirical potential is tuned to match sublimation activation energy • Simulations reveal the effect of pressure on the lattice constant within the KCl films • Pressure affects the film structure and registry between film and substrate.

Structural and magnetic studies of Cr doped nickel ferrite thin films

International Nuclear Information System (INIS)

Panwar, Kalpana; Heda, N. L.; Tiwari, Shailja; Bapna, Komal; Ahuja, B. L.; Choudhary, R. J.; Phase, D. M.

2016-01-01

We have studied the structural and magnetic properties of Cr doped nickel ferrite thin films deposited on Si (100) and Si (111) using pulsed laser deposition technique. The films were deposited under vacuum and substrate temperature was kept at 700°C. X-ray diffraction analysis revealed that films on both substrates have single phase cubic spinel structure. However, the film grown on Si (111) shows better crystalline behavior. Fourier transform infrared spectroscopy suggests that films on both substrates have mixed spinel structure. These films show magnetic hysteresis behavior and magnetization value of film on Si (100) is larger than that on Si (111). It turns out that structural and magnetic properties of these two films are correlated.

Adhesion and friction in polymer films on solid substrates: conformal sites analysis and corresponding surface measurements.

Science.gov (United States)

An, Rong; Huang, Liangliang; Mineart, Kenneth P; Dong, Yihui; Spontak, Richard J; Gubbins, Keith E

2017-05-21

In this work, we present a statistical mechanical analysis to elucidate the molecular-level factors responsible for the static and dynamic properties of polymer films. This analysis, which we term conformal sites theory, establishes that three dimensionless parameters play important roles in determining differences from bulk behavior for thin polymer films near to surfaces: a microscopic wetting parameter, α wx , defined as the ratio of polymer-substrate interaction to polymer-polymer interaction; a dimensionless film thickness, H*; and dimensionless temperature, T*. The parameter α wx introduced here provides a more fundamental measure of wetting than previous metrics, since it is defined in terms of intermolecular forces and the atomic structure of the substrate, and so is valid at the nanoscale for gas, liquid or solid films. To test this theoretical analysis, we also report atomic force microscopy measurements of the friction coefficient (μ), adhesion force (F A ) and glass transition temperature (T g ) for thin films of two polymers, poly(methyl methacrylate) (PMMA) and polystyrene (PS), on two planar substrates, graphite and silica. Both the friction coefficient and the glass transition temperature are found to increase as the film thickness decreases, and this increase is more pronounced for the graphite than for the silica surface. The adhesion force is also greater for the graphite surface. The larger effects encountered for the graphite surface are attributed to the fact that the microscopic wetting parameter, α wx , is larger for graphite than for silica, indicating stronger attraction of polymer chains to the graphite surface.

Structural changes in irreversibly densified fused silica: implications for the chemical resistance of high level nuclear waste glasses

International Nuclear Information System (INIS)

Susman, S.; Volin, K.J.; Liebermann, R.C.; Gwanmesia, G.D.; Yanbin Wang

1990-01-01

Energetic photons and energetic particles create changes in the structure of nuclear waste glasses. These can be observed as changes in the average bulk physical properties. For example, exposure of fused silica to high doses of neutron bombardment leads to a maximum average compaction of 3%. However, this does not reveal the true extent of the densification that takes place at a microscopic level. Recent advances in high pressure technology have yielded large samples of fused silica which have been permanently densified under pressure and whose bulk density has been increased by 20%. These specimens have an overall structure that replicates the microstructure of a radiation damaged glass. Measurements have been made for the first time of the structural changes in this pressure densified vitreous silica using neutron diffraction and infrared absorption spectrometry. Extensive alterations in intermediate range order have been observed with consequent anticipated changes in chemical reactivity. The resistance of high level waste glasses to leaching by groundwater must be considered in light of these experimental findings. (author)

Detecting alkali-silica reaction in thick concrete structures using linear array ultrasound

Science.gov (United States)

Bull Ezell, N. Dianne; Albright, Austin; Clayton, Dwight; Santos-Villalobos, Hector

2018-03-01

Commercial nuclear power plants (NPPs) depend heavily on concrete structures, making the long-term performance of these structures crucial for safe operation, especially with license period extensions to 60 years and possibly beyond. Alkali-silica reaction (ASR) is a reaction that occurs over time in concrete between alkaline cement paste and reactive, noncrystalline silica (aggregates). In the presence of water, an expansive gel is formed within the aggregates, which results in microcracks in aggregates and adjacent cement paste. ASR can potentially affect concrete properties and performance characteristics such as compressive strength, modulus of elasticity, flexural stiffness, shear strength, and tensile strength. Currently, no nondestructive evaluation methods have proven effective in identifying ASR before surface cracks form. ASR is identified visibly or by petrographic analysis. Although ASR definitely impacts concrete material properties, the performance of concrete structures exhibiting ASR depends on whether or not the concrete is unconfined or confined with reinforcing bars. Confinement by reinforcing bars restrainsthe expansion of ASR-affected concrete, similar to prestressing, thus improving the performance of a structure. Additionally, there is no direct correlation between the mechanical properties of concrete sample cores and the in-situ properties of the concrete. The University of Tennessee-Knoxville, Oak Ridge National Laboratory, and a consortium of universities have developed an accelerated ASR experiment. Three large concrete specimens, representative of NPP infrastructure, were constructed containing both embedded and surface instruments. This paper presents preliminary analysis of these specimens using a frequency-banded synthetic aperture focusing technique.

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.

Enhanced microcontact printing of proteins on nanoporous silica surface

Energy Technology Data Exchange (ETDEWEB)

Blinka, Ellen; Hu Ye; Gopal, Ashwini; Hoshino, Kazunori; Lin, Kevin; Zhang, John X J [Department of Biomedical Engineering, University of Texas at Austin, Austin, TX 78758 (United States); Loeffler, Kathryn; Liu Xuewu; Ferrari, Mauro, E-mail: John.Zhang@engr.utexas.edu [Department of Nanomedicine and Biomedical Engineering, University of Texas Health Science Service, Houston, TX 77031 (United States)

2010-10-15

We demonstrate porous silica surface modification, combined with microcontact printing, as an effective method for enhanced protein patterning and adsorption on arbitrary surfaces. Compared to conventional chemical treatments, this approach offers scalability and long-term device stability without requiring complex chemical activation. Two chemical surface treatments using functionalization with the commonly used 3-aminopropyltriethoxysilane (APTES) and glutaraldehyde (GA) were compared with the nanoporous silica surface on the basis of protein adsorption. The deposited thickness and uniformity of porous silica films were evaluated for fluorescein isothiocyanate (FITC)-labeled rabbit immunoglobulin G (R-IgG) protein printed onto the substrates via patterned polydimethlysiloxane (PDMS) stamps. A more complete transfer of proteins was observed on porous silica substrates compared to chemically functionalized substrates. A comparison of different pore sizes (4-6 nm) and porous silica thicknesses (96-200 nm) indicates that porous silica with 4 nm diameter, 57% porosity and a thickness of 96 nm provided a suitable environment for complete transfer of R-IgG proteins. Both fluorescence microscopy and atomic force microscopy (AFM) were used for protein layer characterizations. A porous silica layer is biocompatible, providing a favorable transfer medium with minimal damage to the proteins. A patterned immunoassay microchip was developed to demonstrate the retained protein function after printing on nanoporous surfaces, which enables printable and robust immunoassay detection for point-of-care applications.

Investigation of structural integrity for turbine generator foundation affected by alkali-silica reaction

International Nuclear Information System (INIS)

Ryo Fujimoto; Hiroshi Shimizu; Hisashi Sekimoto; Yuichi Watanabe; Tatsuya Ishikawa

2005-01-01

Turbine Generator Foundation is a reinforced concrete structure having a table deck to support equipments and columns to support the table deck. After operation of the plant, the expansion of the table deck in turbine longitudinal axis in the structure has been observed. By investigation of concrete material property, it is found that the expansion has been caused by alkali-silica reaction (ASR). In this study, we evaluate the material properties of the structure affected by ASR and safety margin of capacity of the structure by nonlinear analysis using beam element model with those material properties. (authors)

Evidence of coexistence of micro and nanoporosity of organo-silica polymeric films deposited on silicon by plasma deposition

International Nuclear Information System (INIS)

Purohit, Viswas; Mielczarski, Ela; Mielczarski, Jerzy A.; Akesso, Laurent

2013-01-01

A range of hybrid, SiOCH films were deposited on silicon substrates within a radio frequency plasma reactor using hexamethyldisiloxane (HMDSO) as a precursor. The plasma polymerized films were deposited at various HMDSO/argon/oxygen ratios. The composition and structure, at microscopic and nanoscopic levels, of the deposited films were determined by external reflection and transmission Fourier Transform Infrared (FTIR) spectroscopy as well as by X-Ray Photoelectron Spectroscopy (XPS). The content of carbon and oxygen in films were found to be inversely proportional to each other. XPS results showed that the outermost surface of the deposited films are nanoporous and coexist with microporosity which was revealed by electron microscopy. The structure of deposited coatings is anisotropic as was documented by polarized external reflection FTIR spectroscopy. Several correlations between the film chemical composition, surface structure, and macroscopic properties of the films such as: hydrophobicity and hydrophilicity were established. - Highlights: • Hybrid organo-polymer silicon films deposited by RF plasma on silicon substrates. • FTIR and XPS reveal porosity by interpreting bonding between Si and –O. • Quantification of nano and microporosity are identified with bonding of Si with –O

Evidence of coexistence of micro and nanoporosity of organo-silica polymeric films deposited on silicon by plasma deposition

Energy Technology Data Exchange (ETDEWEB)

Purohit, Viswas, E-mail: vishwas.purohit@gmail.com [Laboratoire Environnment et Mineralurgie, UMR 7569 CNRS, INPL-ENSG, BP.40, 54501 Vandoeuvre-les-Nancy (France); Mielczarski, Ela; Mielczarski, Jerzy A. [Laboratoire Environnment et Mineralurgie, UMR 7569 CNRS, INPL-ENSG, BP.40, 54501 Vandoeuvre-les-Nancy (France); Akesso, Laurent [Teer Coatings Ltd., Droitwich, Worcestershire WR9 9AS (United Kingdom)

2013-09-16

A range of hybrid, SiOCH films were deposited on silicon substrates within a radio frequency plasma reactor using hexamethyldisiloxane (HMDSO) as a precursor. The plasma polymerized films were deposited at various HMDSO/argon/oxygen ratios. The composition and structure, at microscopic and nanoscopic levels, of the deposited films were determined by external reflection and transmission Fourier Transform Infrared (FTIR) spectroscopy as well as by X-Ray Photoelectron Spectroscopy (XPS). The content of carbon and oxygen in films were found to be inversely proportional to each other. XPS results showed that the outermost surface of the deposited films are nanoporous and coexist with microporosity which was revealed by electron microscopy. The structure of deposited coatings is anisotropic as was documented by polarized external reflection FTIR spectroscopy. Several correlations between the film chemical composition, surface structure, and macroscopic properties of the films such as: hydrophobicity and hydrophilicity were established. - Highlights: • Hybrid organo-polymer silicon films deposited by RF plasma on silicon substrates. • FTIR and XPS reveal porosity by interpreting bonding between Si and –O. • Quantification of nano and microporosity are identified with bonding of Si with –O.

Influence of organic solvents on interfacial water at surfaces of silica gel and partially silylated fumed silica

Energy Technology Data Exchange (ETDEWEB)

Turov, V.V.; Gun' ko, V.M.; Tsapko, M.D.; Bogatyrev, V.M.; Skubiszewska-Zieba, J.; Leboda, R.; Ryczkowski, J

2004-05-15

The effects of organic solvents (dimethylsulfoxide-d{sub 6} (DMSO-d{sub 6}), chloroform-d, acetone-d{sub 6}, and acetonitrile-d{sub 3}) on the properties of interfacial water at surfaces of silica gel Si-40 and partially silylated fumed silica A-380 were studied by means of the {sup 1}H NMR spectroscopy with freezing-out of adsorbed water at 180structural characteristics of silicas and quantum chemical calculations of the chemical shifts {delta}{sub H} and solvent effects. DMSO-d{sub 6} and acetonitrile-d{sub 3} are poorly miscible with water in silica gel pores in contrast to the bulk liquids. DMSO-d{sub 6} and chloroform-d affect the structure of the interfacial water weaker than acetone-d{sub 6} and acetonitrile-d{sub 3} at amounts of liquids greater than the pore volume. Acetone-d{sub 6} and acetonitrile-d{sub 3} can displace water from pores under this condition. The chemical shift of protons in water adsorbed on silica gel is 3.5-6.5 ppm, which corresponds to the formation of two to four hydrogen bonds per molecule. Water adsorbed on partially silylated fumed silica has two {sup 1}H NMR signals at 5 and 1.1-1.7 ppm related to different structures (droplets and small clusters) of the interfacial water.

Biomimetic synthesized chiral mesoporous silica: Structures and controlled release functions as drug carrier

Energy Technology Data Exchange (ETDEWEB)

Li, Jing; Xu, Lu, E-mail: xl2013109@163.com; Yang, Baixue; Bao, Zhihong; Pan, Weisan; Li, Sanming, E-mail: li_sanming2013@163.com

2015-10-01

This work initially illustrated the formation mechanism of chiral mesoporous silica (CMS) in a brand new insight named biomimetic synthesis. Three kinds of biomimetic synthesized CMS (B-CMS, including B-CMS1, B-CMS2 and B-CMS3) were prepared using different pH or stirring rate condition, and their characteristics were tested with transmission electron microscope and small angle X-ray diffraction. The model drug indomethacin was loaded into B-CMS and drug loading content was measured using ultraviolet spectroscopy. The result suggested that pH condition influenced energetics of self-assembly process, mainly packing energetics of the surfactant, while stirring rate was the more dominant factor to determine particle length. In application, indomethacin loading content was measured to be 35.3%, 34.8% and 35.1% for indomethacin loaded B-CMS1, indomethacin loaded B-CMS2 and indomethacin loaded B-CMS3. After loading indomethacin into B-CMS carriers, surface area, pore volume and pore diameter of B-CMS carriers were reduced. B-CMS converted crystalline state of indomethacin to amorphous state, leading to the improved indomethacin dissolution. B-CMS1 controlled drug release without burst-release, while B-CMS2 and B-CMS3 released indomethacin faster than B-CMS1, demonstrating that the particle length, the ordered lever of multiple helixes, the curvature degree of helical channels and pore diameter greatly contributed to the release behavior of indomethacin loaded B-CMS. - Highlights: • Chiral mesoporous silica was synthesized using biomimetic method. • pH influenced energetics of self-assembly process of chiral mesoporous silica. • Stirring rate determined the particle length of chiral mesoporous silica. • Controlled release behaviors of chiral mesoporous silica varied based on structures.

Biomimetic synthesized chiral mesoporous silica: Structures and controlled release functions as drug carrier

International Nuclear Information System (INIS)

Li, Jing; Xu, Lu; Yang, Baixue; Bao, Zhihong; Pan, Weisan; Li, Sanming

2015-01-01

This work initially illustrated the formation mechanism of chiral mesoporous silica (CMS) in a brand new insight named biomimetic synthesis. Three kinds of biomimetic synthesized CMS (B-CMS, including B-CMS1, B-CMS2 and B-CMS3) were prepared using different pH or stirring rate condition, and their characteristics were tested with transmission electron microscope and small angle X-ray diffraction. The model drug indomethacin was loaded into B-CMS and drug loading content was measured using ultraviolet spectroscopy. The result suggested that pH condition influenced energetics of self-assembly process, mainly packing energetics of the surfactant, while stirring rate was the more dominant factor to determine particle length. In application, indomethacin loading content was measured to be 35.3%, 34.8% and 35.1% for indomethacin loaded B-CMS1, indomethacin loaded B-CMS2 and indomethacin loaded B-CMS3. After loading indomethacin into B-CMS carriers, surface area, pore volume and pore diameter of B-CMS carriers were reduced. B-CMS converted crystalline state of indomethacin to amorphous state, leading to the improved indomethacin dissolution. B-CMS1 controlled drug release without burst-release, while B-CMS2 and B-CMS3 released indomethacin faster than B-CMS1, demonstrating that the particle length, the ordered lever of multiple helixes, the curvature degree of helical channels and pore diameter greatly contributed to the release behavior of indomethacin loaded B-CMS. - Highlights: • Chiral mesoporous silica was synthesized using biomimetic method. • pH influenced energetics of self-assembly process of chiral mesoporous silica. • Stirring rate determined the particle length of chiral mesoporous silica. • Controlled release behaviors of chiral mesoporous silica varied based on structures

Ion beam-based characterization of multicomponent oxide thin films and thin film layered structures

International Nuclear Information System (INIS)

Krauss, A.R.; Rangaswamy, M.; Lin, Yuping; Gruen, D.M.; Schultz, J.A.; Schmidt, H.K.; Chang, R.P.H.

1992-01-01

Fabrication of thin film layered structures of multi-component materials such as high temperature superconductors, ferroelectric and electro-optic materials, and alloy semiconductors, and the development of hybrid materials requires understanding of film growth and interface properties. For High Temperature Superconductors, the superconducting coherence length is extremely short (5--15 Angstrom), and fabrication of reliable devices will require control of film properties at extremely sharp interfaces; it will be necessary to verify the integrity of thin layers and layered structure devices over thicknesses comparable to the atomic layer spacing. Analytical techniques which probe the first 1--2 atomic layers are therefore necessary for in-situ characterization of relevant thin film growth processes. However, most surface-analytical techniques are sensitive to a region within 10--40 Angstrom of the surface and are physically incompatible with thin film deposition and are typically restricted to ultra high vacuum conditions. A review of ion beam-based analytical methods for the characterization of thin film and multi-layered thin film structures incorporating layers of multicomponent oxides is presented. Particular attention will be paid to the use of time-of-flight techniques based on the use of 1- 15 key ion beams which show potential for use as nondestructive, real-time, in-situ surface diagnostics for the growth of multicomponent metal and metal oxide thin films

Effect of thermal history on the structure of chemically and vapor deposited silver films on glass

International Nuclear Information System (INIS)

Shelby, J.E.; Nichols, M.C.; Smith, D.K. Jr.; Vitko, J. Jr.

1981-01-01

The observation of silver agglomeration in second surface mirrors used for solar applications has emphasized consideration of the effect of thermal history on the optical properties of mirrors. Thermal history effects may arise from the processing of mirrors, the application of protective coatings, or from outdoor exposure. Mirrors may be subject to elevated temperatures (T less than or equal to 400 0 C) for short periods of time, or to low temperatures (T less than or equal to 60 0 C) for long (less than or equal to 30 years) periods of time. Although a significant amount of work has been done on thermally driven agglomeration of silver films, most of these studies have been restricted to vapor deposited films on vitreous silica. Large area reflectors, such as those used in heliostats, will almost certainly be deposited by commercial chemical methods on substrates of soda-lime-silicate or other glasses which differ considerably from vitreous silica in composition and properties. The present study addresses the effect of this change in deposition technique and substrate on silver agglomeration. These problems were studied by optical and scanning electron microscopy, reflectometry, and x-ray diffraction. The results indicate that both the method used to deposit the silver and the type of glass affect the agglomeration process and the character of the reflective film

A new parameter-free soft-core potential for silica and its application to simulation of silica anomalies

Energy Technology Data Exchange (ETDEWEB)

Izvekov, Sergei, E-mail: sergiy.izvyekov.civ@mail.mil; Rice, Betsy M. [Weapons and Materials Research Directorate, U.S. Army Research Laboratory, Aberdeen Proving Ground, Maryland 21005 (United States)

2015-12-28

A core-softening of the effective interaction between oxygen atoms in water and silica systems and its role in developing anomalous thermodynamic, transport, and structural properties have been extensively debated. For silica, the progress with addressing these issues has been hampered by a lack of effective interaction models with explicit core-softening. In this work, we present an extension of a two-body soft-core interatomic force field for silica recently reported by us [S. Izvekov and B. M. Rice, J. Chem. Phys. 136(13), 134508 (2012)] to include three-body forces. Similar to two-body interaction terms, the three-body terms are derived using parameter-free force-matching of the interactions from ab initio MD simulations of liquid silica. The derived shape of the O–Si–O three-body potential term affirms the existence of repulsion softening between oxygen atoms at short separations. The new model shows a good performance in simulating liquid, amorphous, and crystalline silica. By comparing the soft-core model and a similar model with the soft-core suppressed, we demonstrate that the topology reorganization within the local tetrahedral network and the O–O core-softening are two competitive mechanisms responsible for anomalous thermodynamic and kinetic behaviors observed in liquid and amorphous silica. The studied anomalies include the temperature of density maximum locus and anomalous diffusivity in liquid silica, and irreversible densification of amorphous silica. We show that the O–O core-softened interaction enhances the observed anomalies primarily through two mechanisms: facilitating the defect driven structural rearrangements of the silica tetrahedral network and modifying the tetrahedral ordering induced interactions toward multiple characteristic scales, the feature which underlies the thermodynamic anomalies.

Nanostructured antistatic and antireflective thin films made of indium tin oxide and silica over-coat layer

Science.gov (United States)

Cho, Young-Sang; Hong, Jeong-Jin; Yang, Seung-Man; Choi, Chul-Jin

2010-08-01

Stable dispersion of colloidal indium tin oxide nanoparticles was prepared by using indium tin oxide nanopowder, organic solvent, and suitable dispersants through attrition process. Various comminution parameters during the attrition step were studied to optimize the process for the stable dispersion of indium tin oxide sol. The transparent and conductive films were fabricated on glass substrate using the indium tin oxide sol by spin coating process. To obtain antireflective function, partially hydrolyzed alkyl silicate was deposited as over-coat layer on the pre-fabricated indium tin oxide film by spin coating technique. This double-layered structure of the nanostructured film was characterized by measuring the surface resistance and reflectance spectrum in the visible wavelength region. The final film structure was enough to satisfy the TCO regulations for EMI shielding purposes.

Study of electron-beam-evaporated MgO films using electron diffraction, optical absorption and cathodoluminescence

Energy Technology Data Exchange (ETDEWEB)

Aboelfotoh, M.O.; Ramsey, J.N.

1982-05-21

Reflection high energy electron diffraction, optical absorption and cathodoluminescence were used to study MgO films deposited onto fused silica, single-crystal silicon and LiF substrates at various temperatures. Results showed that some of the same optical absorption and emission bands observed in X- or UV-irradiated, additively colored or mechanically deformed MgO crystals were observed in evaporated MgO films. The peak positions and the relative peak intensities of the optical absorption and emission bands depended on the substrate temperature during film deposition as well as on the structure of the film. The effect of heating the films in air and vacuum on the optical absorption and emission bands is also discussed.

Structural study of TiO2-based transparent conducting films

International Nuclear Information System (INIS)

Hitosugi, T.; Yamada, N.; Nakao, S.; Hatabayashi, K.; Shimada, T.; Hasegawa, T.

2008-01-01

We have investigated microscopic structures of sputter and pulsed laser deposited (PLD) anatase Nb-doped TiO 2 transparent conducting films, and discuss what causes the degradation of resistivity in sputter-deposited films. Cross-sectional transmission electron microscope and polarized optical microscope images show inhomogeneous intragrain structures and small grains of ∼10 μm in sputter-deposited films. From comparison with PLD films, these results suggest that homogeneous film growth is the important factor to obtain highly conducting sputter-deposited film

Ordered mesoporous silica materials with complicated structures

KAUST Repository

Han, Yu; Zhang, Daliang

2012-01-01

Periodically ordered mesoporous silicas constitute one of the most important branches of porous materials that are extensively employed in various chemical engineering applications including adsorption, separation and catalysis. This short review

Hybrid AC EL structures with thin protective ZnO film

International Nuclear Information System (INIS)

Tsvetkova, E; Dikov, H; Kolentsov, K; Yourukova, L; Zhechev, D; Steflekova, V

2008-01-01

Alternating current hybrid electroluminescent Al/SnO 2 /ZnS: Cu/ZnO/Al structures with blue emission have been prepared. In these ZnO films are used as protective layers. The optical properties of different RF magnetron sputtered ZnO films have been studied. The voltage - brightness characteristics of AC EL structures with a ZnO protective film and conventional structures with a TiO 2 protective layer are compared. The investigation shows that the brightness of the structures with a ZnO protective film is higher. The improved characteristics of these new hybrid structures could be used in preparing various systems for representation of permanent or variable light information

Addition of Silica Fume to Improve Strength of Cement Paste

Science.gov (United States)

Chen, Jiajian; Chen, Hongniao; Li, Gu

2018-03-01

This study measured the packing densities of 0 to 30% silica fume (SF) added cementitious materials and strength of the cementitious pastes with various water content. The results revealed that addition of silica fume up to a certain level has great effects on packing density and strength. In-depth analysis illustrated that a lower W/CM ratio would not always result in a higher cube strength, and the range between 0.05 and 0.07 µm would be the amount of water film thickness (WFT) for muximum strength.

Structures and properties of fluorinated amorphous carbon films

Science.gov (United States)

Huang, K. P.; Lin, P.; Shih, H. C.

2004-07-01

Fluorinated amorphous carbon (a-C:F) films were deposited by radio frequency bias assisted microwave plasma electron cyclotron resonance chemical vapor deposition with tetrafluoromethane (CF4) and acetylene (C2H2) as precursors. The deposition process was performed at two flow ratios R=0.90 and R=0.97, where R=CF4/(CF4+C2H2). The samples were annealed at 300 °C for 30 min. in a N2 atmosphere. Both Fourier transform infrared and electron spectroscopy for chemical analyzer were used to characterize the a-C:F film chemical bond and fluorine concentration, respectively. A high resolution electron energy loss spectrometer was applied to detect the electronic structure. The higher CF4 flow ratio (R=0.97) produced more sp3 linear structure, and it made the a-C:F film smoother and softer. A lifetime of around 0.34 μs and an energy gap of ˜2.75 eV were observed in both the as-deposited and after annealing conditions. The short carriers lifetime in the a-C:F film made the photoluminescence peak blueshift. The annealing changed both the structure and composition of the a-C:F film. The type of fluorocarbon bond and electronic structure characterized the mechanical and physical properties of a-C:F film.

IR-spectroscopical investigations on the glass structure of porous and sintered compacts of colloidal silica gels

Science.gov (United States)

Clasen, Rolf; Hornfeck, M.; Theiss, Wolfgang

1991-08-01

The forming and sintering of fumed silica powders is an interesting route for the preparation of large, very pure or doped silica glasses with a precise geometry. The processing from the shaping of a porous compact to the sintering of transparent silica glass can be successfully investigated with optical spectroscopy. As only the dielectric function DF (a dielectric function is the square root of the complex refractive index) characterizes the material, the vibrational bands were calculated from reflectance measurements. In compacts of fine particles, the topology cannot be neglected. Therefore, the models describing topological effects are briefly reviewed. With these model calculations it could be proven that new bands in the compacts and the significant shifts in the reflectance spectra during sintering are mainly caused by topological effects and that changes in the glass structure play only a secondary role.

Structural and mechanical properties of glassy water in nanoscale confinement.

Science.gov (United States)

Lombardo, Thomas G; Giovambattista, Nicolás; Debenedetti, Pablo G

2009-01-01

We investigate the structure and mechanical properties of glassy water confined between silica-based surfaces with continuously tunable hydrophobicity and hydrophilicity by computing and analyzing minimum energy, mechanically stable configurations (inherent structures). The structured silica substrate imposes long-range order on the first layer of water molecules under hydrophobic confinement at high density (p > or = 1.0 g cm(-3)). This proximal layer is also structured in hydrophilic confinement at very low density (p approximately 0.4 g cm(-3)). The ordering of water next to the hydrophobic surface greatly enhances the mechanical strength of thin films (0.8 nm). This leads to a substantial stress anisotropy; the transverse strength of the film exceeds the normal strength by 500 MPa. The large transverse strength results in a minimum in the equation of state of the energy landscape that does not correspond to a mechanical instability, but represents disruption of the ordered layer of water next to the wall. In addition, we find that the mode of mechanical failure is dependent on the type of confinement. Under large lateral strain, water confined by hydrophilic surfaces preferentially forms voids in the middle of the film and fails cohesively. In contrast, water under hydrophobic confinement tends to form voids near the walls and fails by loss of adhesion.

Deformation analysis of a film-overlapped micro-pump membrane structure

International Nuclear Information System (INIS)

Lee, Fu-Shin; Wang, Pi-Wen; Chen, Chih-Hsiung

2008-01-01

A novel approach is developed to study a film-overlapped membrane structure. Meanwhile, the established model is employed to design the micro-pump membrane structure and to evaluate its pumping efficiency. Two-dimensional coupling effects between the overlapping actuator films and the deformable membrane are thoroughly investigated, including the influences on the membrane from the overlapping films' elongation effects, Poisson's ratio effects and shear strain effects. Overall deformations and interactions for the three-layer membrane structures are accurately calculated through exercising the developed model, in contrast to what difficulties are usually encountered in carrying out FEM methods with very thin elements meshed for the actuator films. Furthermore, this study demonstrates that the high stiffness of the actuating metal films needs to be reflected in the equivalent stiffness of the membrane structures, especially when the sizes of the actuator films become compatible with the sizes of the membranes. Hence, the optimal micro-pumping efficiency of a membrane structure is acquired upon exercising the developed model, and larger sizes of the actuating films do not definitely obtain larger pumping efficiencies for the electromagnetically actuated micro-pumps

Lanthanoid titanate film structure deposited at different temperatures in vacuum

International Nuclear Information System (INIS)

Kushkov, V.D.; Zaslavskij, A.M.; Mel'nikov, A.V.; Zverlin, A.V.; Slivinskaya, A.Eh.

1991-01-01

Influence of deposition temperature on the structure of lanthanoid titanate films, prepared by the method of high-rate vacuum condensation. It is shown that formation of crystal structure, close to equilibrium samples, proceeds at 1100-1300 deg C deposition temperatures. Increase of temperature in this range promotes formation of films with higher degree of structural perfection. Amorphous films of lanthanoid titanates form at 200-1000 deg C. Deposition temperature shouldn't exceed 1400 deg C to prevent the formation of perovskite like phases in films

Preparation of superhydrophobic poly(methyl methacrylate)-silicon dioxide nanocomposite films

International Nuclear Information System (INIS)

Wang Jinyan; Chen Xinhua; Kang Yingke; Yang Guangbin; Yu Laigui; Zhang Pingyu

2010-01-01

Superhydrophobic poly(methyl methacrylate)-SiO 2 (coded as PMMA-SiO 2 ) nanocomposite films with micro-nanohierarchical structure were prepared via a simple approach in the absence of low surface-energy compounds. By spin-coating the suspension of hydrophobic silica (SiO 2 ) nanoparticles dispersed in PMMA solution, target nanocomposite films were obtained on glass slides. The wetting behavior of PMMA-SiO 2 nanocomposite films was investigated in relation to the dosage of SiO 2 nanoparticles dispersed in PMMA solution. It was found that hydrophilic PMMA film was transferred to superhydrophobic PMMA-SiO 2 nanocomposite films when hydrophobic SiO 2 nanoparticles were introduced into the PMMA solution at a high enough dosage (0.2 g and above). Resultant PMMA-SiO 2 nanocomposite films had a static water contact angle of above 162 o , showing promising applications in selfcleaning and waterproof for outer wall of building, outer covering for automobile, sanitary wares, and so forth.

Converting Water Adsorption and Capillary Condensation in Usable Forces with Simple Porous Inorganic Thin Films.

Science.gov (United States)

Boudot, Mickael; Elettro, Hervé; Grosso, David

2016-11-22

This work reports an innovative humidity-driven actuation concept based on conversion of chemical energy of adsorption/desorption using simple nanoporous sol-gel silica thin films as humidity-responsive materials. Bilayer-shaped actuators, consisting of a humidity-sensitive active nanostructured silica film deposited on a polymeric substrate (Kapton), were demonstrated as an original mean to convert water molecule adsorption and capillary condensation in usable mechanical work. Reversible solvation stress changes in silica micropores by water adsorption and energy produced by the rigid silica film contraction, induced by water capillary condensation in mesopores, were finely controlled and used as energy sources. The influence of the film nanostructure (microporosity, mesoporosity) and thickness and the polymeric substrate thickness on actuation force, on movement speed and on displacement amplitude are clearly evidenced and discussed. We show that the global mechanical response of such silica-based actuators can easily be adjusted to fabricate tailor-made actuation systems triggered by humidity variation. This study provides insight into hard ceramic stimulus-responsive materials that seem to be a promising alternative to traditional soft organic materials for surface-chemistry-driven actuation systems.

Structural study of Ge/GaAs thin films

International Nuclear Information System (INIS)

Lazarov, V K; Lari, L; Lytvyn, P M; Kholevchuk, V V; Mitin, V F

2012-01-01

Ge/GaAs heterostructure research is largely motivated by the application of this material in solar cells, metal-oxide-semiconductor field-effect transistors, mm-wave mixer diodes, temperature sensors and photodetectors. Therefore, understanding of how the properties of Ge/GaAs heterostructure depend on its preparation (growth) is of importance for various high-efficiency devices. In this work, by using thermal Ge evaporation on GaAs(100), we studied structural properties of these films as a function of the deposition rate. Film grains size and morphology show strong dependence of the deposition rate. Low deposition rates results in films with large crystal grains and rough surface. At high deposition rates films become flatter and their crystal grains size decreases, while at very high deposition rates films become amorphous. Cross-sectional TEM of the films show that the Ge films are granular single crystal epitaxially grown on GaAs. The Ge/GaAs interface is atomically abrupt and free from misfit dislocations. Stacking faults along the [111] directions that originate at the interface were also observed. Finally by using the Kelvin probe microscopy we show that work function changes are related to the grain structure of the film.

Fractal dimensions of silica gels generated using reactive molecular dynamics simulations

International Nuclear Information System (INIS)

Bhattacharya, Sudin; Kieffer, John

2005-01-01

We have used molecular dynamics simulations based on a three-body potential with charge transfer to generate nanoporous silica aerogels. Care was taken to reproduce the sol-gel condensation reaction that forms the gel backbone as realistically as possible and to thereby produce credible gel structures. The self-similarity of aerogel structures was investigated by evaluating their fractal dimension from geometric correlations. For comparison, we have also generated porous silica glasses by rupturing dense silica and computed their fractal dimension. The fractal dimension of the porous silica structures was found to be process dependent. Finally, we have determined that the effect of supercritical drying on the fractal nature of condensed silica gels is not appreciable

Micropore structure stabilization in organosilica membranes by gaseous catalyst post-treatment

NARCIS (Netherlands)

Dral, A. Petra; van Eck, Ernst R.H.; Winnubst, Louis; ten Elshof, Johan E.

2018-01-01

A post-treatment involving repeated exposure to gaseous HCl alternated with heating is demonstrated to strongly accelerate the recently reported structural evolution in organically bridged silica networks. Films, powders and membranes derived from 1,2-bis(triethoxysilyl)ethane were exposed to

Laccase immobilized on methylene blue modified mesoporous silica MCM-41/PVA

International Nuclear Information System (INIS)

Xu Xinhua; Lu Ping; Zhou Yumei; Zhao Zhenzhen; Guo Meiqing

2009-01-01

The mesoporous silica sieve MCM-41 containing methylene blue (MB) provides a suitable immobilization of biomolecule matrix due to its uniform pore structure, high surface areas, good biocompatibility and nice conductivity. Based on this, a facilely fabricated amperometric biosensor by entrapping laccase into the MB modified MCM-41/PVA composite film has been developed. Laccase from Trametes versicolor is assembled on a composite film of MCM-41 containing MB/PVA modified Au electrode and the electrode is characterized with respect to transmission electron microscopy (TEM) and scanning electron microscopic (SEM), Cyclic voltammetry (CV), response time, detection limit, linear range and activity of laccase. The laccase modified electrode remains good redox behavior in pH 4.95 acetate buffer solution, at room temperature in present of 0.1 mM catechol. The response time (t 90% ) of the modified electrode is less than 4 s for catechol. The detection limit is 0.331 μM and the linear detect range is about from 4.0 μM to 87.98 μM for catechol with a correlation coefficient of 0.99913(S/N = 3). The apparent Michaelis-Menten (K M app ) is estimated using the Lineweaver-Burk equation and the K M app value is about 0.256 mM. This work demonstrated that the mesoporous silica MCM-41 containing MB provides a novel support for laccase immobilization and the construction of biosensors with a faster response and better bioactivity.

Surface structure of ultrathin metal films deposited on copper single crystals

International Nuclear Information System (INIS)

Butterfield, M.T.

2000-04-01

Ultrathin films of Cobalt, Iron and Manganese have been thermally evaporated onto an fcc Copper (111) single crystal substrate and investigated using a variety of surface structural techniques. The small lattice mismatch between these metals and the Cu (111) substrate make them an ideal candidate for the study of the phenomena of pseudomorphic film growth. This is important for the understanding of the close relationship between film structure and magnetic properties. Growing films with the structure of their substrate rather than their bulk phase may provide an opportunity to grow materials with novel physical and magnetic properties, and hence new technological applications. Both Cobalt and Iron have been found to initially maintain a registry with the fcc Cu (111) surface in a manner consistent with pseudomorphic growth. This growth is complicated by island rather than layer by layer growth in the initials stages of the film. In both cases a change in the structure of the film seems to occur at a point where the coalescence of islands in the film may be expected to occur. When the film does change structure they do not form a perfect overlayer with the structure of their bulk counterpart. The films do contain a number of features representative of the bulk phase but also contain considerable disorder and possibly remnants of fcc (111) structure. The order present in these films can be greatly improved by annealing. Manganese appears to grow with an fcc Mn (111) lattice spacing and there is no sign of a change in structure in films of up to 4.61 ML thick. The gradual deposition and annealing of a film to 300 deg. C, with a total deposition time the same as that for a 1 ML thick film, causes a surface reconstruction to occur that is apparent in a R30 deg. (√3 x √3) LEED pattern. This is attributed to the formation of a surface alloy, which is also supported by the local expansion of the Cu lattice in the (111) direction. (author)

Template-mediated, Hierarchical Engineering of Ordered Mesoporous Films and Powders

Science.gov (United States)

Tian, Zheng

Hierarchical control over pore size, pore topology, and meso/mictrostructure as well as material morphology (e.g., powders, monoliths, thin films) is crucial for meeting diverse materials needs among applications spanning next generation catalysts, sensors, batteries, sorbents, etc. The overarching goal of this thesis is to establish fundamental mechanistic insight enabling new strategies for realizing such hierarchical textural control for carbon materials that is not currently achievable with sacrificial pore formation by 'one-pot' surfactant-based 'soft'-templating or multi-step inorganic 'hard-templating. While 'hard'-templating is often tacitly discounted based upon its perceived complexity, it offers potential for overcoming key 'soft'-templating challenges, including bolstering pore stability, accommodating a more versatile palette of replica precursors, realizing ordered/spanning porosity in the case of porous thin films, simplifying formation of bi-continuous pore topologies, and inducing microstructure control within porous replica materials. In this thesis, we establish strategies for hard-templating of hierarchically porous and structured carbon powders and tunable thin films by both multi-step hard-templating and a new 'one-pot' template-replica precursor co-assembly process. We first develop a nominal hard-templating technique to successfully prepare three-dimensionally ordered mesoporous (3DOm) and 3DOm-supported microporous carbon thin films by exploiting our ability to synthesize and assemble size-tunable silica nanoparticles into scalable, colloidal crystalline thin film templates of tunable mono- to multi-layer thickness. This robust thin film template accommodates liquid and/or vapor-phase infiltration, polymerization, and pyrolysis of various carbon sources without pore contraction and/or collapse upon template sacrifice. The result is robust, flexible 3DOm or 3DOm-supported ultra-thin microporous films that can be transferred by stamp

P-type CuxS thin films: Integration in a thin film transistor structure

International Nuclear Information System (INIS)

Nunes de Carvalho, C.; Parreira, P.; Lavareda, G.; Brogueira, P.; Amaral, A.

2013-01-01

Cu x S thin films, 80 nm thick, are deposited by vacuum thermal evaporation of sulfur-rich powder mixture, Cu 2 S:S (50:50 wt.%) with no intentional heating of the substrate. The process of deposition occurs at very low deposition rates (0.1–0.3 nm/s) to avoid the formation of Cu or S-rich films. The evolution of Cu x S films surface properties (morphology/roughness) under post deposition mild annealing in air at 270 °C and their integration in a thin film transistor (TFT) are the main objectives of this study. Accordingly, Scanning Electron Microscopy studies show Cu x S films with different surface morphologies, depending on the post deposition annealing conditions. For the shortest annealing time, the Cu x S films look to be constructed of grains with large dimension at the surface (approximately 100 nm) and consequently, irregular shape. For the longest annealing time, films with a fine-grained surface are found, with some randomly distributed large particles bound to this fine-grained surface. Atomic Force Microscopy results indicate an increase of the root-mean-square roughness of Cu x S surface with annealing time, from 13.6 up to 37.4 nm, for 255 and 345 s, respectively. The preliminary integration of Cu x S films in a TFT bottom-gate type structure allowed the study of the feasibility and compatibility of this material with the remaining stages of a TFT fabrication as well as the determination of the p-type characteristic of the Cu x S material. - Highlights: • Surface properties of annealed Cu x S films. • Variation of conductivity with annealing temperatures of Cu x S films. • Application of evaporated Cu x S films in a thin film transistor (TFT) structure. • Determination of Cu x S p-type characteristic from TFT behaviour

Arrays of Hollow Silica Half-Nanospheres Via the Breath Figure Approach

KAUST Repository

Gao, Yangqin; Hou, Yuanfang; Beaujuge, Pierre

2015-01-01

Breath figures (BFs) are patterns of liquid droplets that usually form upon condensation on a cold surface. Earlier work has shown that BFs can be used to produce continuous films of porous honeycomb-structured patterns on various types of materials, paving the path to a number of important applications such as the manufacturing of highly ordered nano- and micron-sized templates, micro lenses, and superhydrophobic coatings. It is worth noting, however, that few new findings have been reported in this area in recent years, limiting pursuits of novel architectures and key applications. In this report, an alternative method is described by which arrays of hollow silica half-nanospheres can be produced via BF templates. In the present method, a chemical vapor deposition (CVD) protocol performed while the BF is formed on a glass substrate yields a nanostructured pattern of silica half-spheres, which size (100-700 nm) and density across the glass surface vary with substrate modification and with the relative rates of water condensation and hydrolysis from silica precursors (a process carried out at room temperature). This method of forming arrays of hollow half-nanospheres via the BF approach may be applicable to various other oxides and a broad range of substrates including large-area flexible plastics. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Arrays of Hollow Silica Half-Nanospheres Via the Breath Figure Approach

KAUST Repository

Gao, Yangqin

2015-04-21

Breath figures (BFs) are patterns of liquid droplets that usually form upon condensation on a cold surface. Earlier work has shown that BFs can be used to produce continuous films of porous honeycomb-structured patterns on various types of materials, paving the path to a number of important applications such as the manufacturing of highly ordered nano- and micron-sized templates, micro lenses, and superhydrophobic coatings. It is worth noting, however, that few new findings have been reported in this area in recent years, limiting pursuits of novel architectures and key applications. In this report, an alternative method is described by which arrays of hollow silica half-nanospheres can be produced via BF templates. In the present method, a chemical vapor deposition (CVD) protocol performed while the BF is formed on a glass substrate yields a nanostructured pattern of silica half-spheres, which size (100-700 nm) and density across the glass surface vary with substrate modification and with the relative rates of water condensation and hydrolysis from silica precursors (a process carried out at room temperature). This method of forming arrays of hollow half-nanospheres via the BF approach may be applicable to various other oxides and a broad range of substrates including large-area flexible plastics. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The ionic conductivity, mechanical performance and morphology of two-phase structural electrolytes based on polyethylene glycol, epoxy resin and nano-silica

Energy Technology Data Exchange (ETDEWEB)

Feng, Qihang; Yang, Jiping, E-mail: jyang08@163.com; Yu, Yalin; Tian, Fangyu; Zhang, Boming; Feng, Mengjie; Wang, Shubin

2017-05-15

Highlights: • Structural electrolytes based on PEG-epoxy resins were prepared. • Factors of influencing ionic conductivity and mechanical properties were studied. • Co-continuous morphology was benefit for improved structural electrolyte property. • Efficiently optimized multifunctional electrolyte performance was achieved. - Abstract: As one of significant parts of structural power composites, structural electrolytes have desirable mechanical properties like structural resins while integrating enough ionic conductivity to work as electrolytes. Here, a series of polyethylene glycol (PEG)-epoxy-based electrolytes filled with nano-silica were prepared. The ionic conductivity and mechanical performance were studied as functions of PEG content, lithium salt concentration, nano-silica content and different curing agents. It was found that, PEG-600 and PEG-2000 content in the epoxy electrolyte system had a significant effect on their ionic conductivity. Furthermore, increasing the nano-silica content in the system induced increased ionic conductivity, decreased glass transition temperature and mechanical properties, and more interconnected irregular network in the cured systems. The introduction of rigid m-xylylenediamine resulted in enhanced mechanical properties and reasonably decreased ionic conductivity. As a result, these two-phase epoxy structural electrolytes have great potential to be used in the multifunctional energy storage devices.

The influence of the matrix structure on the oxidation of aniline in a silica sol-gel composite

International Nuclear Information System (INIS)

Widera, J.; Kijak, A.M.; Ca, D.V.; Pacey, G.E.; Taylor, R.T.; Perfect, H.; Cox, J.A.

2005-01-01

Mesoporous and microporous silica matrices were formed on indium tin oxide electrodes for liquid-phase voltammetry and as monoliths for solid-state voltammetry of aniline. The pore structure, which was verified by scanning probe microscopy and by surface area measurement, was directed by either control of pH during sol-gel processing or by inclusion of a templating agent. Whether aniline was included as a dopant in the sol-gel or as a component of the contacting liquid, the pore size influenced the coupling of the product of its electrochemical oxidation. With microporous silica, the dominant products were dimers and related short-chain products whereas with mesoporous silica, polymerization was suggested. As a step toward the formation of polyaniline (PANI) that is covalently anchored to the sol-gel, the electrochemistry of aniline was investigated using composites prepared from sols comprising tetraethyl orthosilicate (TEOS), 3-aminophenyl-[3-triethoxylsilyl)-propyl] urea (ormosil), and aniline in various ratios. Combinatorial chemistry identified that the optimum combination of silica precursors in terms of obtaining PANI was a 1:12 mole ratio of ormosil:TEOS

Soft magnetic properties and damping parameter of (FeCo-Al alloy thin films

Directory of Open Access Journals (Sweden)

Isao Kanada

2017-05-01

Full Text Available For high frequency device applications, a systematic study of the soft magnetic properties and magnetization dynamics of (FeCo-Al alloy thin films has been carried out. A low effective damping parameter αeff of 0.002 and a high saturation magnetization of about 1,800 emu/cc are obtained at y=0.2∼0.3 for (Fe1-yCoy98Al2 alloy thin films deposited onto fused silica and MgO(100 at an ambient temperature during deposition. Those films are of the bcc structure with the orientation normal to the film plane. They possess a columnar structure, grown along the film normal. The column width is found to be about 20 nm for y=0.25. It is concluded that the (FeCo-Al thin films with a damping parameter as low as 0.002 and high saturation magnetization of about 1,800 emu/cc have been successfully fabricated, and that they are potential for future high frequency device applications.

Structural modification of silica glass by laser scanning

International Nuclear Information System (INIS)

Zhao Jian; Sullivan, James; Zayac, John; Bennett, Ted D.

2004-01-01

The thermophysical nature of rapid CO 2 laser heating of silica glass is explored using a numerical simulation that considers the structural state of the glass, as characterized by the fictive temperature. The fictive temperature reflects the thermodynamic temperature at which the glass structure would be in equilibrium. To demonstrate that the thermophysical model can accurately predict the structural change in the glass, the fictive temperature is measured experimentally utilizing the fact that the fictive temperature change corresponds to a change of glass properties that can be revealed through wet chemical etching. The relationship between the etch rate and the fictive temperature is determined by preparing and etching samples of known fictive temperature. Wet chemical etching is used to measure the fictive temperature over the entire laser affected zone and the results are found to compare favorably with the results of the thermophysical model. The model and experimental measurements demonstrate that rapid laser processing results in an increased fictive temperature near the surface of the glass. The fictive temperature increase is about 1000 K and is uniform to within 5% over the laser affected zone. Near the boundary of this zone, the fictive temperature transitions abruptly to the value of the surrounding untreated glass

Chitosan-silica complex membranes from sulfonic acid functionalized silica nanoparticles for pervaporation dehydration of ethanol-water solutions.

Science.gov (United States)

Liu, Ying-Ling; Hsu, Chih-Yuan; Su, Yu-Huei; Lai, Juin-Yih

2005-01-01

Nanosized silica particles with sulfonic acid groups (ST-GPE-S) were utilized as a cross-linker for chitosan to form a chitosan-silica complex membranes, which were applied to pervaporation dehydration of ethanol-water solutions. ST-GPE-S was obtained from reacting nanoscale silica particles with glycidyl phenyl ether, and subsequent sulfonation onto the attached phenyl groups. The chemical structure of the functionalized silica was characterized with FTIR, (1)H NMR, and energy-dispersive X-ray. Homogeneous dispersion of the silica particles in chitosan was observed with electronic microscopies, and the membranes obtained were considered as nanocomposites. The silica nanoparticles in the membranes served as spacers for polymer chains to provide extra space for water permeation, so as to bring high permeation rates to the complex membranes. With addition of 5 parts per hundred of functionalized silica into chitosan, the resulting membrane exhibited a separation factor of 919 and permeation flux of 410 g/(m(2) h) in pervaporation dehydration of 90 wt % ethanol aqueous solution at 70 degrees C.

Measurement and modelization of silica opal optical properties

OpenAIRE

Avoine , Amaury; Ngoc Hong , Phan; Frederich , Hugo; Aregahegn , Kifle; Bénalloul , Paul; Coolen , Laurent; Schwob , Catherine; Thu Nga , Pham; Gallas , Bruno; Maître , Agnès

2014-01-01

International audience; We present the synthesis process and optical characterization of artificial silica opals. The specular reflection spectra are analyzed and compared to band structure calculations and finite difference time domain (FDTD) simulations. The silica optical index is a key parameter to correctly describe an opal and is usually not known and treated as a free parameter. Here we propose a method to infer the silica index, as well as the silica spheres diameter, from the reflect...

Highly transparent, stable, and superhydrophobic coatings based on gradient structure design and fast regeneration from physical damage

International Nuclear Information System (INIS)

Chen, Zao; Liu, Xiaojiang; Wang, Yan; Li, Jun; Guan, Zisheng

2015-01-01

Graphical abstract: - Highlights: • Highly transparent, stable, and superhydrophobic PET film was fabricated by dip-coating way. • The gradient structure is beneficial to both hydrophobicity and transparency. • The superhydrophobic PET film after physical damage can quickly regain by one-step spary. • The fabrication method is available for various substrates and large-scale production. - Abstract: Optical transparency, mechanical flexibility, and fast regeneration are important factors to expand the application of superhydrophobic surfaces. Herein, we fabricated highly transparent, stable, and superhydrophobic coatings through a novel gradient structure design by versatile dip-coating of silica colloid particles (SCPs) and diethoxydimethysiliane cross-linked silica nanoparticles (DDS-SNPs) on polyethylene terephthalate (PET) film and glass, followed by the modification of octadecyltrichlorosiliane (OTCS). When the DDS concentration reached 5 wt%, the modified SCPs/DDS-SNPs coating exhibited a water contact angle (WCA) of 153° and a sliding angle (SA) <5°. Besides, the average transmittance of this superhydrophobic coating on PET film and glass was increased by 2.7% and 1% in the visible wavelength, respectively. This superhydrophobic coating also showed good robustness and stability against water dropping impact, ultrasonic damage, and acid solution. Moreover, the superhydrophobic PET film after physical damage can quickly regain the superhydrophobicity by one-step spray regenerative solution of dodecyltrichlorosilane (DTCS) modified silica nanoparticles at room temperature. The demonstrated method for the preparation and regeneration of superhydrophobic coating is available for different substrates and large-scale production at room temperature.

Structure and oxygen incorporation in low pressure sputtered YBCO films

International Nuclear Information System (INIS)

Chaudhary, S.; Pandya, D. K.; Kashyap, S. C.

2002-01-01

Thin films of YBa 2 Cu 3 O 7- δ (YBCO) have been successfully grown by reactive RF-magnetron sputtering technique at low pressure. The oxygen partial pressure of 0.95 mTorr, a total pressure (argon and oxygen) of 1.9 mTorr, and a substrate temperature of 775 grad C resulted in good quality films with T C (R=0) = 85.3 K and J Cmag (4.2 K) ≅ 2x10 7 A/cm 2 . The incorporation of oxygen in the as-grown films has been controlled by using different ambient - oxygen, air or argon during in-situ cooling. The superconducting behaviour of the films was studied using resistance-temperature and low field ac-susceptibility measurements and correlated with their structure. All the films exhibited metallic conduction in the normal state. The oxygen- and air- cooled films were superconducting, possessing the usual orthorhombic structure. The argon-cooled films were non-superconducting possessing the tetragonal structure, thus implying that the structure of the film during deposition is tetragonal which transforms to either of the oxygen rich orthorhombic-I or -II phases depending upon the oxygen/air ambient. The 'δ' values of 0.14, 0.32 and 0.70 and higher 'c'-parameters of 1.1785, 1.180 and 1.183 nm have been obtained for oxygen, air and argon cooled films respectively. (Authors)

Non-iridescent structural colors from uniform-sized SiO2 colloids

Science.gov (United States)

Topçu, Gökhan; Güner, Tuğrul; Demir, Mustafa M.

2018-05-01

Structural colors have recently attracted interest from diverse fields of research due to their ease of fabrication and eco-friendliness. These types of colors are, in principle, achieved by periodically arranged submicron-diameter colloidal particles. The interaction of light with a structure containing long-range ordered colloidal particles leads to coloration; this usually varies depending on the angle of observation (iridescence). However, the majority of the applications demand constant color that is independent of the viewing angle (non-iridescence). In this work, silica colloids were obtained using the Stöber method at different sizes from 150 to 300 nm in an alcoholic dispersion. The casting of the dispersion on a substrate leaves behind a photonic crystal showing a colorful iridescent film. However, centrifugation and redispersion of the SiO2 particles into fresh solvent may cause the formation of small, aggregated silica domains in the new dispersion. The casting of this dispersion allows for the development of photonic glass, presumably due to the accumulation of aggregates showing stable colloidal film independent of viewing angle. Moreover, depending on the size of the silica colloids, non-iridescent photonic glasses with various colors (violet, blue, green, and orange) are obtained.

Role of surface functionality on the formation of raspberry-like polymer/silica composite particles: Weak acid–base interaction and steric effect

International Nuclear Information System (INIS)

Wang, Lan; Song, LinYong; Chao, ZhiYin; Chen, PengPeng; Nie, WangYan; Zhou, YiFeng

2015-01-01

Graphical abstract: - Highlights: • Core–shell structured polymer/SiO 2 was obtained with carboxylic-functionalized templates. • Raspberry-like structure was observed with carboxylic and poly(ethylene glycol) hybrid-functionalized polymer microspheres. • Carboxylic groups contributed to the nucleation and the poly(ethylene glycol) chains was used to control the growth of silica particles. • Super-hydrophobic surface was obtained and the contact angle of water on the dual-sized structured surface was up to 160°. - Abstract: The surface functionality of polymer microspheres is the crucial factor to determine the nucleation and growth of silica particles and to construct the organic/inorganic hierarchical structures. The objective of this work was to evaluate the surface functionality and hierarchical morphology relationship via in situ sol–gel reaction. Carboxylic-functionalized poly (styrene-co-maleic anhydride) [P(S-co-MA)], poly(ethylene glycol)-functionalized poly(styrene-co-poly(ethylene glycol) methacrylate) [P(S-co-PEGMA)], and hybrid functionalized poly(styrene-co-maleic anhydride-co-poly(ethylene glycol) methacrylate) [P(S-co-MA-co-PEGMA)] microspheres were synthesized by emulsifier-free polymerization and used as templates. The morphologies of the composite particles were observed by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results showed that core–shell structure was obtained with P(S-co-MA) as templates; raspberry-like structure was observed by using P(S-co-MA-co-PEGMA) as templates; and no silica particles were attached onto the surface of P(S-co-PEGMA) microspheres. These results indicated that the carboxylic groups on the surface formed by hydrolysis of anhydride groups were the determinate factor to control the nucleation of silica nanoparticles, and the PEG chains on the surface can affect the growth of silica particles. In addition, the particulate films were constructed by assembling these

The structural and optical characterizations of tetraphenylporphyrin thin films

Energy Technology Data Exchange (ETDEWEB)

Makhlouf, M.M., E-mail: m_makhlof@hotmail.com [Physics Department, Faculty of Applied Medical Science at Turabah branch, Taif University, Turabah, 21995 (Saudi Arabia); Department of Physics, Faculty of Science at New Damietta, Damietta University, New Damietta 34517 (Egypt); El-Denglawey, A. [Physics Department, Faculty of Applied Medical Science at Turabah branch, Taif University, Turabah, 21995 (Saudi Arabia); Physics Department, Faculty of Science, South Valley University, Qena 83523 (Egypt); Zeyada, H.M. [Department of Physics, Faculty of Science at New Damietta, Damietta University, New Damietta 34517 (Egypt); El-Nahass, M.M. [Physics Department, Faculty of Education, Ain Shams University, Cairo (Egypt)

2014-03-15

X-rays diffraction and scanning electron microscope were used to investigate the structural properties of tetraphenylporphyrin, TPP, which is polycrystalline in a synthesized condition. It turns to amorphous structure upon thermal deposition. Annealing temperature ranging from 295 to 473 K does not influence the amorphous structure of films. The optical properties of TPP were investigated using spectrophotometric measurements of the transmittance and reflectance at normal incidence in the wavelength range of 200–2200 nm. The absorption spectra were recorded in UV–visible region of spectra for the as-deposited and annealed samples show different absorption bands, namely four bands labeled as Q-band in visible region of spectra and a more intense band termed as the Soret band in near UV region of spectra. The Soret band shows its splitting (Davydov splitting). Two other bands labeled N and M appear in UV region. The film thickness has no influence on optical properties of films while annealing temperatures have a slight influence on optical properties of TPP films. The type of optical transition in as deposited and annealed conditions of films was found to be indirect allowed band-gap. Both fundamental and onset energy gap decreases upon annealing. -- Highlights: • Tetraphenylporphyrin (TPP) is polycrystalline in powder form, while the as-deposited and annealed TPP thin films have amorphous structure. • The absorption spectra of TPP in UV–visible region consists of Q-bands, Soret band and two other bands labeled N and M. • The optical parameters of TPP thin film were measured. • Thermal annealing influences optical properties of TPP thin films.

The structural and optical characterizations of tetraphenylporphyrin thin films

International Nuclear Information System (INIS)

Makhlouf, M.M.; El-Denglawey, A.; Zeyada, H.M.; El-Nahass, M.M.

2014-01-01

X-rays diffraction and scanning electron microscope were used to investigate the structural properties of tetraphenylporphyrin, TPP, which is polycrystalline in a synthesized condition. It turns to amorphous structure upon thermal deposition. Annealing temperature ranging from 295 to 473 K does not influence the amorphous structure of films. The optical properties of TPP were investigated using spectrophotometric measurements of the transmittance and reflectance at normal incidence in the wavelength range of 200–2200 nm. The absorption spectra were recorded in UV–visible region of spectra for the as-deposited and annealed samples show different absorption bands, namely four bands labeled as Q-band in visible region of spectra and a more intense band termed as the Soret band in near UV region of spectra. The Soret band shows its splitting (Davydov splitting). Two other bands labeled N and M appear in UV region. The film thickness has no influence on optical properties of films while annealing temperatures have a slight influence on optical properties of TPP films. The type of optical transition in as deposited and annealed conditions of films was found to be indirect allowed band-gap. Both fundamental and onset energy gap decreases upon annealing. -- Highlights: • Tetraphenylporphyrin (TPP) is polycrystalline in powder form, while the as-deposited and annealed TPP thin films have amorphous structure. • The absorption spectra of TPP in UV–visible region consists of Q-bands, Soret band and two other bands labeled N and M. • The optical parameters of TPP thin film were measured. • Thermal annealing influences optical properties of TPP thin films

Rupture of thin liquid films on structured surfaces.

Science.gov (United States)

Ajaev, Vladimir S; Gatapova, Elizaveta Ya; Kabov, Oleg A

2011-10-01

We investigate stability and breakup of a thin liquid film on a solid surface under the action of disjoining pressure. The solid surface is structured by parallel grooves. Air is trapped in the grooves under the liquid film. Our mathematical model takes into account the effect of slip due to the presence of menisci separating the liquid film from the air inside the grooves, the deformation of these menisci due to local variations of pressure in the liquid film, and nonuniformities of the Hamaker constant which measures the strength of disjoining pressure. Both linear stability and strongly nonlinear evolution of the film are analyzed. Surface structuring results in decrease of the fastest growing instability wavelength and the rupture time. It is shown that a simplified description of film dynamics based on the standard formula for effective slip leads to significant deviations from the behavior seen in our simulations. Self-similar decay over several orders of magnitude of the film thickness near the rupture point is observed. We also show that the presence of the grooves can lead to instability in otherwise stable films if the relative groove width is above a critical value, found as a function of disjoining pressure parameters.

Elaboration of colloidal silica sols in aqueous medium: functionalities, optical properties and chemical detection of coating

International Nuclear Information System (INIS)

Le Guevel, X.

2006-03-01

The aim of this work was to study surface reactivity of silica nanoparticles through physical and chemical properties of sols and coatings. Applications are numerous and they are illustrated in this work by optical coating preparation for laser components and chemical gas sensor development for nitroaromatics detection. On one hand, protocol synthesis of colloidal silica sols has been developed in water medium using sol-gel process (0 to 100 w%). These sols, so-called BLUESIL, are time-stable during at least one year. Homogeneous coatings having thickness fixed to 200 nm, have been prepared on silica substrate and show high porosity and high transparence. Original films have been developed using catalytic curing in gas atmosphere (ammonia curing) conferring good abrasive resistance to the coating without significant properties modification. In order to reduce film sensitivity to molecular adsorption (water, polluting agents... ), specific BLUESIL coatings have been prepared showing hydrophobic property due to apolar species grafting onto silica nanoparticles. Using this route, coatings having several functional properties such as transparence, hydrophobicity, high porosity and good abrasive resistance have been elaborated. On the other hand, we show that colloidal silica is a material specifically adapted to the detection of nitro aromatic vapors (NAC). Indeed, the use of colloidal silica as chemical gas sensor reveals very high sensitivity, selectivity to NAC compared to Volatile Organic Compound (V.O.C) and good detection performances during one year. Moreover, chemical sensors using functionalized colloidal silica have exhibited good results of detection, even in high humidity medium (≥70 %RH). (author)

Silica-coated flexible liposomes as a nanohybrid delivery system for enhanced oral bioavailability of curcumin

Directory of Open Access Journals (Sweden)

Li C

2012-12-01

Full Text Available Chong Li, Yan Zhang, Tingting Su, Lianlian Feng, Yingying Long, Zhangbao ChenKey Laboratory on Luminescence and Real-Time Analysis, Ministry of Education, College of Pharmaceutical Sciences, Southwest University, Chongqing, ChinaAbstract: We investigated flexible liposomes as a potential oral drug delivery system. However, enhanced membrane fluidity and structural deformability may necessitate liposomal surface modification when facing the harsh environment of the gastrointestinal tract. In the present study, silica-coated flexible liposomes loaded with curcumin (CUR-SLs having poor water solubility as a model drug were prepared by a thin-film method with homogenization, followed by the formation of a silica shell by the sol-gel process. We systematically investigated the physical properties, drug release behavior, pharmacodynamics, and bioavailability of CUR-SLs. CUR-SLs had a mean diameter of 157 nm and a polydispersity index of 0.14, while the apparent entrapment efficiency was 90.62%. Compared with curcumin-loaded flexible liposomes (CUR-FLs without silica-coatings, CUR-SLs had significantly higher stability against artificial gastric fluid and showed more sustained drug release in artificial intestinal fluid as determined by in vitro release assays. The bioavailability of CUR-SLs and CUR-FLs was 7.76- and 2.35-fold higher, respectively, than that of curcumin suspensions. Silica coating markedly improved the stability of flexible liposomes, and CUR-SLs exhibited a 3.31-fold increase in bioavailability compared with CUR-FLs, indicating that silica-coated flexible liposomes may be employed as a potential carrier to deliver drugs with poor water solubility via the oral route with improved bioavailability.Keywords: silica, flexible liposome, oral bioavailability, curcumin

Crystal structure and thin film morphology of BBL ladder polymer

Energy Technology Data Exchange (ETDEWEB)

Song, H H [Department of Macromolecular Science, Han Nam University, Taejon (Korea, Republic of); Fratini, A V [Department of Chemistry, University of Dayton, Dayton, OH (United States); Chabinyc, M [Department of Chemistry, University of Dayton, Dayton, OH (United States); Price, G E [University of Dayton Research, Dayton, OH (United States); Agrawal, A K [Systran Corporation, Dayton, OH (United States); Wang, C S [University of Dayton Research, Dayton, OH (United States); Burkette, J [University of Dayton Research, Dayton, OH (United States); Dudis, D S [Materials Directorate, Wright Laboratory, Wright-Patterson Air Force Base, OH (United States); Arnold, F E [Materials Directorate, Wright Laboratory, Wright-Patterson Air Force Base, OH (United States)

1995-03-01

Crystal structure and morphology of poly[7-oxo-7H-benz(d,e)imidazo(4`,5`:5,6)-benzimidazo(2,1-a)isoquinoline-3,4:10,11-tetrayl-10-carbonyl] (BBL) ladder-like polymer were studied. The polymer forms a two-dimensional lattice of nematic liquid crystalline structure. An orthorhombic unit cell with cell parameters of a=7.87 b=3.37 c=11.97A was determined from the fiber diffraction pattern. In thin films, the rigid chains spontaneously form a layered structure across the film thickness, but in a very unusual manner, i.e. the very large molecular plane is standing perpendicularly to the film surface plane. The results are identical to our recent results of poly(p-phenylene benzobisthiazole) (PBT) film [7]. The polymer, however, lost its anisotropic order upon extrusion into a film and resulted in a fiber-like structure. (orig.)

Bioinspired Non-iridescent Structural Color from Polymer Blend Thin Films

Science.gov (United States)

Nallapaneni, Asritha; Shawkey, Matthew; Karim, Alamgir

Colors exhibited in biological species are either due to natural pigments, sub-micron structural variation or both. Structural colors thus exhibited can be iridescent (ID) or non-iridescent (NID) in nature. NID colors originate due to interference and coherent scattering of light with quasi-ordered micro- and nano- structures. Specifically, in Eastern Bluebird (Sialia sialis) these nanostructures develop as a result of phase separation of β-keratin from cytoplasm present in cells. We replicate these structures via spinodal blend phase separation of PS-PMMA thin films. Colors of films vary from ultraviolet to blue. Scattering of UV-visible light from selectively leeched phase separated blends are studied in terms of varying domain spacing (200nm to 2 μm) of film. We control these parameters by tuning annealing time and temperature. Angle-resolved spectroscopy studies suggest that the films are weakly iridescent and scattering from phase-separated films is more diffused when compared to well-mixed films. This study offers solutions to several color-based application in paints and coatings industry.

Plasma-deposited hybrid silica membranes with a controlled retention of organic bridges

Energy Technology Data Exchange (ETDEWEB)

Ngamou, P.H.T.; Creatore, M. [Department of Applied Physics, Eindhoven University of Technology, 5600 MB Eindhoven (Netherlands); Overbeek, J.P.; Kreiter, R.; Van Veen, H.M.; Vente, J.F. [ECN, Energy research Centre of the Netherlands, Petten (Netherlands); Wienk, I.M.; Cuperus, P.F. [SolSep BV, Apeldoorn (Netherlands)

2013-03-05

Hybrid organically bridged silica membranes are suitable for energy-efficient molecular separations under harsh industrial conditions. Such membranes can be useful in organic solvent nanofiltration if they can be deposited on flexible, porous and large area supports. Here, we report the proof of concept for applying an expanding thermal plasma to the synthesis of perm-selective hybrid silica films from an organically bridged monomer, 1,2-bis(triethoxysilyl)ethane. This membrane is the first in its class to be produced by plasma enhanced chemical vapor deposition. By tuning the plasma and process parameters, the organic bridging groups could be retained in the separating layer. This way, a defect free film could be made with pervaporation performances of an n-butanol-water mixture comparable with those of conventional ceramic supported membranes made by sol-gel technology (i.e. a water flux of [similar]1.8 kg m'-{sup 2} h{sup -1}, a water concentration in the permeate higher than 98% and a separation factor of >1100). The obtained results show the suitability of expanding thermal plasma as a technology for the deposition of hybrid silica membranes for molecular separations.

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

Chain and mirophase-separated structures of ultrathin polyurethane films

International Nuclear Information System (INIS)

Kojio, Ken; Yamamoto, Yasunori; Motokucho, Suguru; Furukawa, Mutsuhisa; Uchiba, Yusuke

2009-01-01

Measurements are presented how chain and microphase-separated structures of ultrathin polyurethane (PU) films are controlled by the thickness. The film thickness is varied by a solution concentration for spin coating. The systems are PUs prepared from commercial raw materials. Fourier-transform infrared spectroscopic measurement revealed that the degree of hydrogen bonding among hard segment chains decreased and increased with decreasing film thickness for strong and weak microphase separation systems, respectively. The microphase-separated structure, which is formed from hard segment domains and a surrounding soft segment matrix, were observed by atomic force microscopy. The size of hard segment domains decreased with decreasing film thickness, and possibility of specific orientation of the hard segment chains was exhibited for both systems. These results are due to decreasing space for the formation of the microphase-separated structure.

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.

Crystal structures of sol-gel deposited zirconia thin films

International Nuclear Information System (INIS)

Bell, J.M.; Cheary, R.W.; Rice, M.; Ben-Nissan, B.; Cocking, J.L.; Johnstone, G.R.

1992-01-01

The authors reports on the crystal structure of zirconia thin films by high temperature x-ray diffraction. The films were deposited by sol-gel processing onto polished stainless steel substrates, and dried at 200 deg C. X-ray diffraction at temperatures between 400 deg C and 800 deg C was carried out using an APEX diffractometer with a position sensitive detector. Previous results indicated that there was a transformation between the tetragonal phase and the monoclinic phase at approximately 770 deg C. Two experiments have been carried out: temperature runs, where the structure evolution is studied as a function of temperature; and time evolution of the structure at fixed temperatures. The results for both experiments, including structural analysis of the different phases found in the thin zirconia films and an analysis of the kinetics of the phase transformation(s) from the time evolution work are presented. This will include a comparison with theories of nucleation and crystallisation in single element films. Impurity phases introduced by interaction of the zirconia with the substrate have been observed, and the effect of increasing annealing time on the substrate-film interaction will also be discussed. 17 refs., 1 tab., 3 figs

Micromagnetic study of single-domain FePt nanocrystals overcoated with silica

International Nuclear Information System (INIS)

Hyun, Changbae; Lee, Doh C; Korgel, Brian A; Lozanne, Alex de

2007-01-01

Chemically-synthesized FePt nanocrystals must be annealed at a high temperature (>550 deg. C) to induce the hard ferromagnetic L 1 0 phase. Unfortunately, the organic stabilizer covering these nanocrystals degrades at these temperatures and the nanocrystals sinter, resulting in the loss of control over nanocrystal size and separation in the film. We have developed a silica overcoating strategy to prevent nanocrystal sintering. In this study, 6 nm diameter FePt nanocrystals were coated with 17 nm thick shells of silica using an inverse micelle process. Magnetization measurements of the annealed FePt-SiO 2 nanocrystals indicate ferromagnetism with a high coercivity at room temperature. Magnetic force microscopy (MFM) results show that the film composed of nanocrystals behaves as a dipole after magnetization by an 8 T external field. The individual nanocrystals are modelled as single-domain particles with random crystallographic orientations. We propose that the interparticle magnetic dipole interaction is weaker than the magnetocrystalline energy in the remanent state, leading to an unusual material with no magnetic anisotropy and no domains. Films of these nanoparticles are promising candidates for magnetic media with a data storage density of ∼Tb/in 2

Structural evolution of silica sols modified with formamide

Directory of Open Access Journals (Sweden)

Lenza R.F.S.

2001-01-01

Full Text Available In this work we investigated the influence of formamide on the acid-catalyzed sol-gel process by Fourier transform infrared spectroscopy (FTIR. Three silica sols were studied: Sol catalyzed with nitric acid without formamide, sol catalyzed with nitric acid containing formamide and sol catalyzed with a mixture of nitric acid and hydrofluoric acid and modified with formamide. Following the time evolution of both the Si-(OH stretching vibration at around 950 cm-1 and the Si-O-(Si vibration between 1040 cm-1 and 1200 cm-1 we were able to describe the structural evolution of each sol. The curve of evolution of Si-(OH stretching vibration corresponding to sol A has a simple asymptotic evolution. In the case of formamide containing sol, we observed a two-step structural evolution indicating that for the system containing formamide the polymerization goes through a temporary stabilization of oligomers, which can explain the non-variation of the Si-O(H bond wavenumber for a certain time. Gelation times were of several days for gels without formamide and few hours for gels containing additive. The presence of additive resulted in a highly interconnected gel.

Temperature-dependent structural properties of P3HT films

Energy Technology Data Exchange (ETDEWEB)

Grigorian, S; Joshi, S; Pietsch, U, E-mail: grigorian@physik.uni-siegen.de [Institute of Physics, University Siegen, Walter Flex Strasse 3, D-57068, Siegen (Germany)

2010-11-15

Structural investigations of spin coated and drop cast poly(3-hexylthiophene) P3HT films have been performed under x-ray grazing incidence geometry. Drop cast films revealed to be highly oriented and crystalline and only slightly modify with the temperature. In contrast, spin coated films provided random orientational distribution of nanocrystallites and undergo significant morphological and structural changes during annealing. Interestingly, spin coated films of low and high molecular weight fractions behavior differently as a function of temperature. Crystalline domains of the low molecular weight fractions have been decreased, and, in contrast, we found an improvement of crystallinity of high molecular weight fraction with increase of the temperature.

Temperature-dependent structural properties of P3HT films

International Nuclear Information System (INIS)

Grigorian, S; Joshi, S; Pietsch, U

2010-01-01

Structural investigations of spin coated and drop cast poly(3-hexylthiophene) P3HT films have been performed under x-ray grazing incidence geometry. Drop cast films revealed to be highly oriented and crystalline and only slightly modify with the temperature. In contrast, spin coated films provided random orientational distribution of nanocrystallites and undergo significant morphological and structural changes during annealing. Interestingly, spin coated films of low and high molecular weight fractions behavior differently as a function of temperature. Crystalline domains of the low molecular weight fractions have been decreased, and, in contrast, we found an improvement of crystallinity of high molecular weight fraction with increase of the temperature.

Mesoporous Silica: A Suitable Adsorbent for Amines

Directory of Open Access Journals (Sweden)

Abdollahzadeh-Ghom Sara

2009-01-01

Full Text Available Abstract Mesoporous silica with KIT-6 structure was investigated as a preconcentrating material in chromatographic systems for ammonia and trimethylamine. Its adsorption capacity was compared to that of existing commercial materials, showing its increased adsorption power. In addition, KIT-6 mesoporous silica efficiently adsorbs both gases, while none of the employed commercial adsorbents did. This means that KIT-6 Mesoporous silica may be a good choice for integrated chromatography/gas sensing micro-devices.

Microporous Silica Based Membranes for Desalination

Directory of Open Access Journals (Sweden)

João C. Diniz da Costa

2012-09-01

Full Text Available This review provides a global overview of microporous silica based membranes for desalination via pervaporation with a focus on membrane synthesis and processing, transport mechanisms and current state of the art membrane performance. Most importantly, the recent development and novel concepts for improving the hydro-stability and separating performance of silica membranes for desalination are critically examined. Research into silica based membranes for desalination has focussed on three primary methods for improving the hydro-stability. These include incorporating carbon templates into the microporous silica both as surfactants and hybrid organic-inorganic structures and incorporation of metal oxide nanoparticles into the silica matrix. The literature examined identified that only metal oxide silica membranes have demonstrated high salt rejections under a variety of feed concentrations, reasonable fluxes and unaltered performance over long-term operation. As this is an embryonic field of research several target areas for researchers were discussed including further improvement of the membrane materials, but also regarding the necessity of integrating waste or solar heat sources into the final process design to ensure cost competitiveness with conventional reverse osmosis processes.

Secondary electron emission yield on poled silica based thick films

DEFF Research Database (Denmark)

Braga, D.; Poumellec, B.; Cannas, V.

2004-01-01

Studies on the distribution of the electric field produced by a thermal poling process in a layer of Ge-doped silica on silicon substrate, by using secondary electron emission yield (SEEY) measurements () are presented. Comparing 0 between poled and unpoled areas, the SEEY at the origin of electr...

Defect studies of thin ZnO films prepared by pulsed laser deposition

International Nuclear Information System (INIS)

Vlček, M; Čížek, J; Procházka, I; Novotný, M; Bulíř, J; Lančok, J; Anwand, W; Brauer, G; Mosnier, J-P

2014-01-01

Thin ZnO films were grown by pulsed laser deposition on four different substrates: sapphire (0 0 0 1), MgO (1 0 0), fused silica and nanocrystalline synthetic diamond. Defect studies by slow positron implantation spectroscopy (SPIS) revealed significantly higher concentration of defects in the studied films when compared to a bulk ZnO single crystal. The concentration of defects in the films deposited on single crystal sapphire and MgO substrates is higher than in the films deposited on amorphous fused silica substrate and nanocrystalline synthetic diamond. Furthermore, the effect of deposition temperature on film quality was investigated in ZnO films deposited on synthetic diamond substrates. Defect studies performed by SPIS revealed that the concentration of defects firstly decreases with increasing deposition temperature, but at too high deposition temperatures it increases again. The lowest concentration of defects was found in the film deposited at 450° C.

Amperometric xanthine biosensors using glassy carbon electrodes modified with electrografted porous silica nanomaterials loaded with xanthine oxidase

International Nuclear Information System (INIS)

Saadaoui, Maroua; Sánchez, Alfredo; Díez, Paula; Raouafi, Noureddine; Pingarrón, José M.; Villalonga, Reynaldo

2016-01-01

Glassy carbon electrodes were modified with silica materials such as silica nanoparticles, mesoporous silica nanoparticles and mesoporous silica thin films with the aim to introduce scaffolds suitable for the immobilization of enzymes. Xanthine oxidase was selected as a model enzyme, and xanthine as the target analyte. A comparison of the modified electrodes showed the biosensor prepared with mesoporous silica nanoparticles to perform best. By using the respective biosensor, xanthine can be amperometrically determined (via measurement of enzymatically formed hydrogen peroxide) at a working voltage of 0.7 V (vs. Ag/AgCl) with a 0.28 μM detection limit. The biosensor was evaluated in terms of potential interferences, reproducibility and stability, and applied to the determination of fish freshness via sensing of xanthine. (author)

Simultaneous measurements of top surface and its underlying film surfaces in multilayer film structure.

Science.gov (United States)

Ghim, Young-Sik; Rhee, Hyug-Gyo; Davies, Angela

2017-09-19

With the growth of 3D packaging technology and the development of flexible, transparent electrodes, the use of multilayer thin-films is steadily increasing throughout high-tech industries including semiconductor, flat panel display, and solar photovoltaic industries. Also, this in turn leads to an increase in industrial demands for inspection of internal analysis. However, there still remain many technical limitations to overcome for measurement of the internal structure of the specimen without damage. In this paper, we propose an innovative optical inspection technique for simultaneous measurements of the surface and film thickness corresponding to each layer of multilayer film structures by computing the phase and reflectance over a wide range of wavelengths. For verification of our proposed method, the sample specimen of multilayer films was fabricated via photolithography process, and the surface profile and film thickness of each layer were measured by two different techniques of a stylus profilometer and an ellipsometer, respectively. Comparison results shows that our proposed technique enables simultaneous measurements of the top surface and its underlying film surfaces with high precision, which could not be measured by conventional non-destructive methods.

Electron irradiation effects on partially fluorinated polymer films: Structure-property relationships

International Nuclear Information System (INIS)

Nasef, Mohamed Mahmoud; Dahlan, Khairul Zaman M.

2003-01-01

The effects of electron beam irradiation on two partially fluorinated polymer films i.e. poly(vinylidene fluoride) (PVDF) and poly(ethylene-tetrafluoroethylene) copolymer (ETFE) are studied at doses ranging from 100 to 1200 kGy in air at room temperature. Chemical structure, thermal and mechanical properties of irradiated films are investigated. FTIR show that both PVDF and ETFE films undergo similar changes in their chemical structures including the formation of carbonyl groups and double bonding. The changes in melting and crystallisation temperatures (T m and T c ) in both irradiated films are functions of irradiation dose and reflect the disorder in the chemical structure caused by the competition between crosslinking and chain scission. The heat of melting (ΔH m ) and the degree of crystallinity (X c ) of PVDF films show no significant changes with the dose increase, whereas those of ETFE films are reduced rapidly after the first 100 kGy. The tensile strength of PVDF films is improved by irradiation compared to its rapid deterioration in ETFE films, which stemmed from the degradation prompted by the presence of radiation sensitive tetrafluoroethylene (TFE) comonomer units. The elongation at break of both films drops gradually with the dose increase indicating the formation of predominant crosslinked structures at high doses. However, the response of each polymer to crosslinking and main chain scission at various irradiation doses varies from PVDF to ETFE films

Compositional dependence of absorption coefficient and band-gap for Nb2O5-SiO2 mixture thin films

International Nuclear Information System (INIS)

Sancho-Parramon, Jordi; Janicki, Vesna; Zorc, Hrvoje

2008-01-01

The absorption coefficient of composite films consisting of niobia (Nb 2 O 5 ) and silica (SiO 2 ) mixtures is studied for photon energies around the band gap. The films were deposited by co-evaporation and their composition was varied by changing the ratio of deposition rates of the two materials. Both, as-deposited and thermally annealed films were characterized by different techniques: the absorption coefficient was determined by spectrophotometric measurements and the structural properties were investigated using infrared spectroscopy, transmission electron microscopy and X-ray diffraction. The correlation between the variations of absorption properties and film composition and structure is established. The absorption coefficients determined experimentally are compared with the results derived from effective medium theories in order to evaluate the suitability of these theories for the studied composites

Effect of deposition temperature on the structural, morphological and optical band gap of lead selenide thin films synthesized by chemical bath deposition method

Energy Technology Data Exchange (ETDEWEB)

Hone, Fekadu Gashaw, E-mail: fekeye@gmail.com [Hawassa University, Department of Physics, Hawassa (Ethiopia); Ampong, Francis Kofi [Kwame Nkrumah University of Science and Technology, Department of Physics, Kumasi (Ghana)

2016-11-01

Lead selenide (PbSe) nanocrystalline thin films have been deposited on silica glass substrates by the chemical bath deposition technique. The samples were deposited at the bath temperatures of 60, 75 and 90 °C respectively and characterized by a variety of techniques. The XRD results revealed that the PbSe thin film deposited at 60 °C was amorphous in nature. Films deposited at higher temperatures exhibited sharp and intense diffraction peaks, indicating an improvement in crystallinety. The deposition temperature also had a strong influence on the preferred orientation of the crystallites as well as other structural parameters such as microstrain and dislocation density. From the SEM study it was observed that film deposited at 90 °C had well defined crystallites, uniformly distributed over the entire surface of the substrate. The EDAX study confirmed that the samples deposited at the higher temperature had a better stoichiometric ratio. The optical band gap varied from 2.26 eV to 1.13 eV with increasing deposition temperature. - Highlights: • The crystallinety of the films improved as the deposition temperature increased. • The deposition temperature strongly influenced the preferred orientations. • Microstrain and dislocation density are decreased linearly with deposition temperature. • Band gap decreased from 2.26 eV to 1.13 eV as the deposition temperature increased.

Growth-related magnetic and physical structures in CMR films

Energy Technology Data Exchange (ETDEWEB)

Hawley, M.E.; Brown, G.W.; Hundley, M.F. [and others

1997-09-01

Scanning tunneling microscopy (STM), atomic force microscopy (AFM), and magnetic force microscopy (MFM) have proven to be powerful tools for revealing property-sensitive structures in magnetic materials. With the renewed interest in perovskite films as materials for read-heads in high density magnetic data storage, the same challenges faced by high temperature superconductor (HTS) film fabrication are repeated for these materials. To begin addressing these challenges, we used vapor phase epitaxy to fabricate La (Sr, Ca,) based manganate films on single crystal perovskite substrates under different conditions and characterized them with scanning probe microscopies, x-ray diffraction, and temperature-dependent magnetization and resistivity measurements (M(T) and {rho}(T)). The as-grown films were polygranular with grain sizes increasing with increasing temperature (T). The post-deposition annealed films consisted of coalesced layers with improved transport properties. The room temperature magnetic structure of the Sr-based films appeared to be related to defects and/or strain.

New insight into silica deposition in horsetail (Equisetum arvense

Directory of Open Access Journals (Sweden)

Exley Christopher

2011-07-01

Full Text Available Abstract Background The horsetails (Equisetum sp are known biosilicifiers though the mechanism underlying silica deposition in these plants remains largely unknown. Tissue extracts from horsetails grown hydroponically and also collected from the wild were acid-digested in a microwave oven and their silica 'skeletons' visualised using the fluor, PDMPO, and fluorescence microscopy. Results Silica deposits were observed in all plant regions from the rhizome through to the stem, leaf and spores. Numerous structures were silicified including cell walls, cell plates, plasmodesmata, and guard cells and stomata at varying stages of differentiation. All of the major sites of silica deposition in horsetail mimicked sites and structures where the hemicellulose, callose is known to be found and these serendipitous observations of the coincidence of silica and callose raised the possibility that callose might be templating silica deposition in horsetail. Hydroponic culture of horsetail in the absence of silicic acid resulted in normal healthy plants which, following acid digestion, showed no deposition of silica anywhere in their tissues. To test the hypothesis that callose might be templating silica deposition in horsetail commercially available callose was mixed with undersaturated and saturated solutions of silicic acid and the formation of silica was demonstrated by fluorimetry and fluorescence microscopy. Conclusions The initiation of silica formation by callose is the first example whereby any biomolecule has been shown to induce, as compared to catalyse, the formation of silica in an undersaturated solution of silicic acid. This novel discovery allowed us to speculate that callose and its associated biochemical machinery could be a missing link in our understanding of biosilicification.

Structural and optical properties of nano-structured CdS thin films prepared by chemical bath deposition

Energy Technology Data Exchange (ETDEWEB)

Bai, Rekha, E-mail: rekha.mittal07@gmail.com; Kumar, Dinesh; Chaudhary, Sujeet; Pandya, Dinesh K. [Thin Film Laboratory, Physics Department, Indian Institute of Technology Delhi, New Delhi-110016 (India)

2016-05-06

Cadmium sulfide (CdS) thin films have been deposited on conducting glass substrates by chemical bath deposition (CBD) technique. The effect of precursor concentration on the structural, morphological, compositional, and optical properties of the CdS films has been studied. Crystal structure of these CdS films is characterized by X-ray diffraction (XRD) and it reveals polycrystalline structure with mixture of cubic and wurtzite phases with grain size decreasing as precursor concentration is increased. Optical studies reveal that the CdS thin films have high transmittance in visible spectral region reaching 90% and the films possess direct optical band gap that decreases from 2.46 to 2.39 eV with decreasing bath concentration. Our study suggests that growth is nucleation controlled.

Structural and optical properties of nano-structured CdS thin films prepared by chemical bath deposition

International Nuclear Information System (INIS)

Bai, Rekha; Kumar, Dinesh; Chaudhary, Sujeet; Pandya, Dinesh K.

2016-01-01

Cadmium sulfide (CdS) thin films have been deposited on conducting glass substrates by chemical bath deposition (CBD) technique. The effect of precursor concentration on the structural, morphological, compositional, and optical properties of the CdS films has been studied. Crystal structure of these CdS films is characterized by X-ray diffraction (XRD) and it reveals polycrystalline structure with mixture of cubic and wurtzite phases with grain size decreasing as precursor concentration is increased. Optical studies reveal that the CdS thin films have high transmittance in visible spectral region reaching 90% and the films possess direct optical band gap that decreases from 2.46 to 2.39 eV with decreasing bath concentration. Our study suggests that growth is nucleation controlled.

Preparation of superhydrophobic poly(methyl methacrylate)-silicon dioxide nanocomposite films

Energy Technology Data Exchange (ETDEWEB)

Wang Jinyan [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Jinming Road, Kaifeng, Henan Province 475004 (China); Chen Xinhua [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Jinming Road, Kaifeng, Henan Province 475004 (China); College of Chemistry and Chemical Engineering, Xuchang University, Xuchang 461000 (China); Kang Yingke; Yang Guangbin; Yu Laigui [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Jinming Road, Kaifeng, Henan Province 475004 (China); Zhang Pingyu, E-mail: pingyu@henu.edu.cn [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Jinming Road, Kaifeng, Henan Province 475004 (China)

2010-12-15

Superhydrophobic poly(methyl methacrylate)-SiO{sub 2} (coded as PMMA-SiO{sub 2}) nanocomposite films with micro-nanohierarchical structure were prepared via a simple approach in the absence of low surface-energy compounds. By spin-coating the suspension of hydrophobic silica (SiO{sub 2}) nanoparticles dispersed in PMMA solution, target nanocomposite films were obtained on glass slides. The wetting behavior of PMMA-SiO{sub 2} nanocomposite films was investigated in relation to the dosage of SiO{sub 2} nanoparticles dispersed in PMMA solution. It was found that hydrophilic PMMA film was transferred to superhydrophobic PMMA-SiO{sub 2} nanocomposite films when hydrophobic SiO{sub 2} nanoparticles were introduced into the PMMA solution at a high enough dosage (0.2 g and above). Resultant PMMA-SiO{sub 2} nanocomposite films had a static water contact angle of above 162{sup o}, showing promising applications in selfcleaning and waterproof for outer wall of building, outer covering for automobile, sanitary wares, and so forth.

Synthesis and new structure shaping mechanism of silica particles formed at high pH

International Nuclear Information System (INIS)

Zhang, Henan; Zhao, Yu; Akins, Daniel L.

2012-01-01

For the sol–gel synthesis of silica particles under high pH catalytic conditions (pH>12) in water/ethanol solvent, we have deduced that the competing dynamics of chemical etching and sol–gel process can explain the types of silica particles formed and their morphologies. We have demonstrated that emulsion droplets that are generated by adding tetraethyl orthosilicate (TEOS) to a water–ethanol solution serve as soft templates for hollow spherical silica (1–2 μm). And if the emulsion is converted by the sol–gel process, one finds that suspended solid silica spheres of diameter of ∼900 nm are formed. Moreover, several other factors are found to play fundamental roles in determining the final morphologies of silica particles, such as by variation of the pH (in our case, using OH – ) to a level where condensation dominates; by changing the volume ratios of water/ethanol; and using an emulsifier (specifically, CTAB) - Graphical abstract: “Local chemical etching” and sol–gel process have been proposed to interpret the control of morphologies of silica particles through varying initial pHs in syntheses. Highlights: ► Different initial pHs in our syntheses provides morphological control of silica particles. ► “Local chemical etching” and sol–gel process describes the formation of silica spheres. ► The formation of emulsions generates hollow silica particles.

Three-dimensional structure of Au nanoparticles supported on amorphous silica and carbon substrates

International Nuclear Information System (INIS)

Bruma, A; Li, Z Y

2012-01-01

Scanning Transmission Electron Microscope (STEM) has been employed to study the three-dimensional structure of gold (Au) nanoparticles deposited by means of thermal evaporation in high vacuum on amorphous silica (a-SiO 2 ) and amorphous carbon (a-C) supports. By performing quantitative analysis on the evolution of the high angle annular dark field (HAADF) images, we studied the influence of the nature and the temperature of support on the growth mode of gold nanoparticles.

Structures and Elastic Moduli of Polymer Nanocomposite Thin Films

Science.gov (United States)

Yuan, Hongyi; Karim, Alamgir; University of Akron Team

2014-03-01

Polymeric thin films generally possess unique mechanical and thermal properties due to confinement. In this study we investigated structures and elastic moduli of polymer nanocomposite thin films, which can potentially find wide applications in diverse areas such as in coating, permeation and separation. Conventional thermoplastics (PS, PMMA) and biopolymers (PLA, PCL) were chosen as polymer matrices. Various types of nanoparticles were used including nanoclay, fullerene and functionalized inorganic particles. Samples were prepared by solvent-mixing followed by spin-coating or flow-coating. Film structures were characterized using X-ray scattering and transmission electron microscopy. Elastic moduli were measured by strain-induced elastic buckling instability for mechanical measurements (SIEBIMM), and a strengthening effect was found in certain systems due to strong interaction between polymers and nanoparticles. The effects of polymer structure, nanoparticle addition and film thickness on elastic modulus will be discussed and compared with bulk materials.

Giant basal spicule from the deep-sea glass sponge Monorhaphis chuni: synthesis of the largest bio-silica structure on Earth by silicatein

Science.gov (United States)

Wang, Xiao-hong; Zhang, Xue-hua; Schröder, Heinz C.; Müller, Werner E. G.

2009-09-01

Like all sponges (phylum Porifera), the glass sponges (Hexactinellida) are provided with an elaborate and distinct body plan, which relies on a filigree skeleton. It is constructed by an array of morphologically determined elements, the spicules. Schulze described the largest siliceous hexactinellid sponge on Earth, the up to 3 m high Monorhaphis chuni, collected during the German Deep Sea Expedition "Valdivia" (1898-1899). This species develops an equally large bio-silica structure, the giant basal spicule (3 m × 10 mm). Using these spicules as a model, one can obtain the basic knowledge on the morphology, formation, and development of silica skeletal elements. The silica matrix is composed of almost pure silica, endowing it with unusual optophysical properties, which are superior to those of man-made waveguides. Experiments suggest that the spicules function in vivo as a nonocular photoreception system. The spicules are also provided with exceptional mechanical properties. Like demosponges, the hexactinellids synthesize their silica enzymatically via the enzyme silicatein (27 kDa protein). This enzyme is located in/embedded in the silica layers. This knowledge will surely contribute to a further utilization and exploration of silica in biomaterial/biomedical science.

Two-step excitation structure changes of luminescence centers and strong tunable blue emission on surface of silica nanospheres

Energy Technology Data Exchange (ETDEWEB)

Yang, Lei, E-mail: nanoyang@qq.com; Jiang, Zhongcheng; Dong, Jiazhang; Zhang, Liuqian [Hunan University, College of Materials Science and Engineering (China); Pan, Anlian, E-mail: anlian.pan@gmail.com; Zhuang, Xiujuan [Hunan University, Key Laboratory for Micro-Nano Physics and Technology of Hunan Province (China)

2015-10-15

We report a scheme for investigating two-step stimulated structure change of luminescence centers. Amorphous silica nanospheres with uniform diameter of 9–15 nm have been synthesized by Stöber method. Strong hydroxyl-related infrared-absorption band is observed in infrared spectrum. The surface hydroxyl groups exert great influence on the luminescent behavior of silica. They provide stable and intermediate energy states to accommodate excitation electrons. The existence of these surface states reduces the energy barrier of photochemical reactions, creating conditions for two-step excitation process. By carefully examining excitation and emission process, the nearest excitation band is absent in both optical absorption spectrum and excitation spectrum. This later generated state confirms the generation of new luminescence centers as well as the existence of photochemical reactions. Stimulated by different energies, two-step excitation process impels different photochemical reactions, prompting generation of different lattice defects on surface area of silica. Thereby, tunable luminescence is achieved. After thermal treatment, strong gap excitation band appears with the disappearance of strong surface excitation band. Strong blue luminescence also disappears. The research is significance to precise introducing structural defects and controlling position of luminescence peaks.

Structural and magentic characterization of rare earth and transition metal films grown on epitaxial buffer films on semiconductor substrates

International Nuclear Information System (INIS)

Farrow, R.F.C.; Parkin, S.S.P.; Speriosu, V.S.; Bezinge, A.; Segmuller, A.P.

1989-01-01

Structural and magnetic data are presented and discussed for epitaxial films of rare earth metals (Dy, Ho, Er) on LaF 3 films on the GaAs(TTT) surface and Fe on Ag films on the GaAs(001) surface. Both systems exhibit unusual structural characteristics which influence the magnetic properties of the metal films. In the case of rare earth epitaxy on LaF 3 the authors present evidence for epitaxy across an incommensurate or discommensurate interface. Coherency strain is not transmitted into the metal which behaves much like bulk crystals of the rare earths. In the case of Fe films, tilted epitaxy and long-range coherency strain are confirmed by X- ray diffractometry. Methods of controlling some of these structural effects by modifying the epitaxial structures are presented

Structure of AlN films deposited by magnetron sputtering method

Directory of Open Access Journals (Sweden)

Nowakowska-Langier K.

2015-09-01

Full Text Available AlN films on a Si substrate were synthesized by magnetron sputtering method. A dual magnetron system operating in AC mode was used in the experiment. Processes of synthesis were carried out in the atmosphere of a mixture of Ar/N2. Morphology and phase structure of the AlN films were investigated at different pressures. Structural characterizations were performed by means of SEM and X-ray diffraction methods. Our results show that the use of magnetron sputtering method in a dual magnetron sputtering system is an effective way to produce AlN layers which are characterized by a good adhesion to the silicon substrate. The morphology of the films is strongly dependent on the Ar/N2 gas mixture pressure. An increase of the mixture pressure is accompanied by a columnar growth of the layers. The films obtained at the pressure below 1 Pa are characterized by finer and compacter structure. The AlN films are characterized by a polycrystalline hexagonal (wurtzite structure in which the crystallographic orientation depends on the gas mixture pressure.

On the controlled isotropic shrinkage induced fine-tuning of photo-luminescence in terbium ions embedded silica inverse opal films

Science.gov (United States)

Shrivastava, Vishnu Prasad; Kumar, Jitendra; Sivakumar, Sri

2017-12-01

Tb3+ embedded silica inverse opal structures with different photonic stop bands have been fabricated by annealing the SiO2-polystyrene spheres (diameter 390 nm) opal template at 320-650 oC. The PSB tuning realized in the wavelength range 498 - 600 nm is shown to depend on annealing temperature and impending isotropic shrinkage of silica matrix. The impact of wide PSB shift on four Tb3+ ion emission bands (blue, green, yellow, and red at 486, 545, 580, and 620 nm, respectively) corresponding to 5D4→7Fj (j = 6,5,4,3) transitions have been investigated. The effect amounts to significant suppression of emission bands at 586, 545 and 486 nm in inverse opals, obtained by annealing opal template at 350, 400, and 650 oC, respectively. Further, luminescence lifetime of Tb3+ ion 5D4 state increases with shrinkage induced in inverse opal progressively and get enhanced up to 2.3 times vis-à-vis reference silica. The changes in refractive index caused by thermal annealing of opal template is found to be responsible for the observed improvement in 5D4 state lifetime.

Stability of anti-reflection coatings via the self-assembly encapsulation of silica nanoparticles by diazo-resins

Science.gov (United States)

Metzman, Jonathan S.; Ridley, Jason I.; Khalifa, Moataz B.; Heflin, James R.

2015-12-01

A modified silica nanoparticle (MSNP) solution was formed by the encapsulation of negatively charged silica nanoparticles by the UV-crosslinkable polycation oligomer diazo-resin (DAR). Appropriate DAR encapsulation concentrations were determined by use of zeta-potential and dynamic light scattering measurements. The MSNPs were used in conjunction with poly(styrene sulfonate) (PSS) to grow homogenous ionic self-assembled multilayer anti-reflection coatings. Stability was induced within the films by the exposure of UV-irradiation that allowed for crosslinking of the DAR and PSS. The films were characterized by UV/vis/IR spectroscopy and field emission scanning electron microscopy. The transmission and reflection levels were >98.5% and <0.05%, respectively. The refractive indices resided in the 1.25-1.26 range. The solvent stability was tested by sonication of the films in a ternary solvent (H2O/DMF/ZnCl2 3:5:2 w/w/w).

Electron irradiation effects on partially fluorinated polymer films: Structure-property relationships

CERN Document Server

Nasef, M M

2003-01-01

The effects of electron beam irradiation on two partially fluorinated polymer films i.e. poly(vinylidene fluoride) (PVDF) and poly(ethylene-tetrafluoroethylene) copolymer (ETFE) are studied at doses ranging from 100 to 1200 kGy in air at room temperature. Chemical structure, thermal and mechanical properties of irradiated films are investigated. FTIR show that both PVDF and ETFE films undergo similar changes in their chemical structures including the formation of carbonyl groups and double bonding. The changes in melting and crystallisation temperatures (T sub m and T sub c) in both irradiated films are functions of irradiation dose and reflect the disorder in the chemical structure caused by the competition between crosslinking and chain scission. The heat of melting (DELTA H sub m) and the degree of crystallinity (X sub c) of PVDF films show no significant changes with the dose increase, whereas those of ETFE films are reduced rapidly after the first 100 kGy. The tensile strength of PVDF films is improved b...

Study of the pluronic-silica interaction in synthesis of mesoporous silica under mild acidic conditions.

Science.gov (United States)

Sundblom, Andreas; Palmqvist, Anders E C; Holmberg, Krister

2010-02-02

The interaction between silica and poly(ethylene oxide) (PEO) in water may appear trivial and it is generally stated that hydrogen bonding is responsible for the attraction. However, a literature search shows that there is not a consensus with respect to the mechanism behind the attractive interaction. Several papers claim that only hydrogen bonding is not sufficient to explain the binding. The silica-PEO interaction is interesting from an academic perspective and it is also exploited in the preparation of mesoporous silica, a material of considerable current interest. This study concerns the very early stage of synthesis of mesoporous silica under mild acidic conditions, pH 2-5, and the aim is to shed light on the interaction between silica and the PEO-containing structure directing agent. The synthesis comprises two steps. An organic silica source, tetraethylorthosilicate (TEOS), is first hydrolyzed and Pluronic P123, a poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO) block copolymer, is subsequently added at different time periods following the hydrolysis of TEOS. It is shown that the interaction between the silica and the Pluronic is dependent both on the temperature and on the time between onset of TEOS hydrolysis and addition of the copolymer. The results show that the interaction is mainly driven by entropy. The effect of the synthesis temperature and of the time between hydrolysis and addition of the copolymer on the final material is also studied. The material with the highest degree of mesoorder was obtained when the reaction was performed at 20 degrees C and the copolymer was added 40 h after the start of TEOS hydrolysis. It is claimed that the reason for the good ordering of the silica is that whereas particle formation under these conditions is fast, the rate of silica condensation is relatively low.

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.

Physical phenomena stipulating nucleus formation, growth and structure films

Energy Technology Data Exchange (ETDEWEB)

Aleksandrov, L N [AN SSSR, Novosibirsk. Inst. Fiziki Poluprovodnikov

1975-03-01

This review is concerned with the physical phenomena responsible for the nucleation, growth and structure of films. Emphasis is placed on the study of films of solid-metal systems, semiconductors (In, As, Cd, Se, CdS), and dielectrics. The following problems are discussed in the paper: general regularities of the thermodynamics and kinetics of film formation, methods of obtaining a solid film, the process of film formation, the rate of growth of individual grains. The critical film thickness and its measurement are also considered. The results of investigating the process of formation of mono- and polycrystalline films are discussed. It is concluded, on the basis of studies into the relaxation processes accompanying the growth of films, that an insight into these processes will permits improving film properties.

Multilayered gold/silica nanoparticulate bilayer devices using layer-by-layer self organisation for flexible bending and pressure sensing applications

Energy Technology Data Exchange (ETDEWEB)

Shah Alam, Md. [Department of Electrical and Electronic Engineering, Rajshahi University of Engineering and Technology, Rajshahi 6204 (Bangladesh); Center of Excellence in Nanotechnology, Asian Institute of Technology, 12120 Pathumthani (Thailand); Mohammed, Waleed S., E-mail: waleed.m@bu.ac.th [Center of Research in Optoelectronics, Communication and Control System (BU-CROCCS), School of Engineering, Bangkok University, Pathumthani 12120 (Thailand); Dutta, Joydeep, E-mail: dutta@squ.edu.om [Center of Excellence in Nanotechnology, Asian Institute of Technology, 12120 Pathumthani (Thailand); Chair in Nanotechnology, Water Research Center, Sultan Qaboos University, P.O. Box 33, Al Khoud 123 (Oman)

2014-02-17

A pressure and bending sensor was fabricated using multilayer thin films fabricated on a flexible substrate based on layer-by-layer self-organization of 18 nm gold nanoparticles separated by a dielectric layer of 30 nm silica nanoparticles. 50, 75, and 100 gold-silica bi-layered films were deposited and the device characteristics were studied. A threshold voltage was required for electron conduction which increases from 2.4 V for 50 bi-layers to 3.3 V for 100 bi-layers. Upon bending of the device up to about 52°, the threshold voltage and slope of the I-V curves change linearly. Electrical characterization of the multilayer films was carried out under ambient conditions with different pressures and bending angles in the direct current mode. This study demonstrates that the developed multilayer thin films can be used as pressure as well as bending sensing applications.

Fabrication of polystyrene porous films with gradient pore structures

International Nuclear Information System (INIS)

Yan Hongwei; Zhang Lin; Li Bo; Yin Qiang

2010-01-01

Silica opals and multilayer heterostructures were fabricated by vertical deposition technique. Polystyrene inverse opals and gradient porous structures were obtained by colloidal templating, in order to control the pore microstructure of polymer porous materials. As shown in the scanning electron microscopy images, the polystyrene porous structures are precise replicas of inverse structures of the original templates. After being infiltrated with the polystyrene, the photonic stop-band position of the opal composite is redshifted compared with the original template, and it is blueshifted after the opal template being removed. The filling ratio of polystyrene was calculated according to the Bragg formula. (authors)

Preparation of Ferroelectric Thin Films of Bismuth Layer Structured Compounds

Science.gov (United States)

Watanabe, Hitoshi; Mihara, Takashi; Yoshimori, Hiroyuki; Araujo, Carlos

1995-09-01

Ferroelectric thin films of bismuth layer structured compounds, SrBi2Ta2O9, SrBi2Nb2O9, SrBi4Ti4O15 and their solid solutions, were formed onto a sputtered platinum layer on a silicon substrate using spin-on technique and metal-organic decomposition (MOD) method. X-ray diffraction (XRD) analysis and some electrical measurements were performed on the prepared thin films. XRD results of SrBi2(Ta1- x, Nb x)2O9 films (0≤x≤1) showed that niobium ions substitute for tantalum ions in an arbitrary ratio without any change of the layer structure and lattice constants. Furthermore, XRD results of SrBi2 xTa2O9 films (0≤x≤1.5) indicated that the formation of the bismuth layer structure does not always require an accurate bismuth content. The layer structure was formed above 50% of the stoichiometric bismuth content in the general formula. SrBi2(Ta1- x, Nb x)2O9 films with various Ta/Nb ratios have large enough remanent polarization for nonvolatile memory application and have shown high fatigue resistance against 1011 cycles of full switching of the remanent polarization. Mixture films of the three compounds were also investigated.

D. C. plasma-sprayed coatings of nano-structured alumina-titania-silica

CERN Document Server

Jiang Xian Liang

2002-01-01

nano-crystalline powders of omega(Al sub 2 O sub 3) = 95%, omega(TiO sub 2) = 3%, and omega(SiO sub 2) = 2%, were reprocessed into agglomerated particles for plasma spraying, by using consecutive steps of ball milling, slurry forming, spray drying, and heat treatment. D.C. plasma was used to spray the agglomerated nano-crystalline powders, and resultant coatings were deposited on the substrate of stainless steel. Scanning electron microscopy (SEM) was used to examine the morphology of the agglomerated powders and the cross section of the alumina-titania-silica coatings. Experimental results show that the agglomerated nano-crystalline particles are spherical, with a size from (10-90) mu m. The flow ability of the nano-crystalline powders is greatly improved after the reprocessing. The coatings deposited by the plasma spraying are mainly of nano-structure. Unlike conventional plasma-sprayed coatings, no laminar layer could be found in the nano-structured coatings. Although the nano-structured coatings have a lo...

The structural heterogeneity and optical properties in chalcogenide glass films

International Nuclear Information System (INIS)

Shurgalin, Max; Fuflyigin, Vladimir N; Anderson, Emilia G

2005-01-01

The microscopic structure and optical properties of glassy films prepared by vapour phase deposition process from the germanium-arsenic-selenium family of chalcogenide glasses have been studied. A number of different molecular clusters or domains that can exist in the glass structure are found to play a significant role in determining the absorption characteristics and refractive index of the glass films. Modifications of the glass structure can be described by a variation of relative concentrations of the clusters and can be effected by modifications of film chemical composition and deposition conditions. Changes in absorption spectra are directly correlated with variation in relative concentrations of the structural fragments with different electronic bandgap properties. Experimental results suggest structural heterogeneity and support validity of the cluster structural model for the chalcogenide glasses

Formation of plasma induced surface damage in silica glass etching for optical waveguides

International Nuclear Information System (INIS)

Choi, D.Y.; Lee, J.H.; Kim, D.S.; Jung, S.T.

2004-01-01

Ge, B, P-doped silica glass films are widely used as optical waveguides because of their low losses and inherent compatibility with silica optical fibers. These films were etched by ICP (inductively coupled plasma) with chrome etch masks, which were patterned by reactive ion etching (RIE) using chlorine-based gases. In some cases, the etched surfaces of silica glass were very rough (root-mean square roughness greater than 100 nm) and we call this phenomenon plasma induced surface damage (PISD). Rough surface cannot be used as a platform for hybrid integration because of difficulty in alignment and bonding of active devices. PISD reduces the etch rate of glass and it is very difficult to remove residues on a rough surface. The objective of this study is to elucidate the mechanism of PISD formation. To achieve this goal, PISD formation during different etching conditions of chrome etch mask and silica glass was investigated. In most cases, PISD sources are formed on a glass surface after chrome etching, and metal compounds are identified in theses sources. Water rinse after chrome etching reduces the PISD, due to the water solubility of metal chlorides. PISD is decreased or even disappeared at high power and/or low pressure in glass etching, even if PISD sources were present on the glass surface before etching. In conclusion, PISD sources come from the chrome etching process, and polymer deposition on these sources during the silica etching cause the PISD sources to grow. In the area close to the PISD source there is a higher ion flux, which causes an increase in the etch rate, and results in the formation of a pit

Materials science in microelectronics I the relationships between thin film processing and structure

CERN Document Server

Machlin, Eugene

2005-01-01

Thin films play a key role in the material science of microelectronics, and the subject matter of thin-films divides naturally into two headings: processing / structure relationship, and structure / properties relationship.The first volume of Materials Science in Microelectronics focuses on the first relationship - that between processing and the structure of the thin-film. The state of the thin film's surface during the period that one monolayer exists - before being buried in the next layer - determines the ultimate structure of the thin film, and thus its properties. This

Optical constants and structural properties of thin gold films

DEFF Research Database (Denmark)

Yakubovsky, Dmitry I.; Arsenin, Aleksey V.; Stebunov, Yury V.

2017-01-01

We report a comprehensive experimental study of optical and electrical properties of thin polycrystalline gold films in a wide range of film thicknesses (from 20 to 200 nm). Our experimental results are supported by theoretical calculations based on the measured morphology of the fabricated gold...... rules for thin-film plasmonic and nanophotonic devices....... films. We demonstrate that the dielectric function of the metal is determined by its structural morphology. Although the fabrication process can be absolutely the same for different films, the dielectric function can strongly depend on the film thickness. Our studies show that the imaginary part...

D. C. plasma-sprayed coatings of nano-structured alumina-titania-silica

International Nuclear Information System (INIS)

Jiang Xianliang

2002-01-01

nano-crystalline powders of ω(Al 2 O 3 ) = 95%, ω(TiO 2 ) = 3%, and ω(SiO 2 ) = 2%, were reprocessed into agglomerated particles for plasma spraying, by using consecutive steps of ball milling, slurry forming, spray drying, and heat treatment. D.C. plasma was used to spray the agglomerated nano-crystalline powders, and resultant coatings were deposited on the substrate of stainless steel. Scanning electron microscopy (SEM) was used to examine the morphology of the agglomerated powders and the cross section of the alumina-titania-silica coatings. Experimental results show that the agglomerated nano-crystalline particles are spherical, with a size from (10-90) μm. The flow ability of the nano-crystalline powders is greatly improved after the reprocessing. The coatings deposited by the plasma spraying are mainly of nano-structure. Unlike conventional plasma-sprayed coatings, no laminar layer could be found in the nano-structured coatings. Although the nano-structured coatings have a lower microhardness than conventional microstructured coatings, the toughness of the nano-structured ceramic coatings is significantly improved

Toughening Mechanisms in Silica-Filled Epoxy Nanocomposites

Science.gov (United States)

Patel, Binay S.

Epoxies are widely used as underfill resins throughout the microelectronics industry to mechanically couple and protect various components of flip-chip assemblies. Generally rigid materials largely surround underfill resins. Improving the mechanical and thermal properties of epoxy resins to better match those of their rigid counterparts can help extend the service lifetime of flip-chip assemblies. Recently, researchers have demonstrated that silica nanoparticles are effective toughening agents for lightly-crosslinked epoxies. Improvements in the fracture toughness of silica-filled epoxy nanocomposites have primarily been attributed to two toughening mechanisms: particle debonding with subsequent void growth and matrix shear banding. Various attempts have been made to model the contribution of these toughening mechanisms to the overall fracture energy observed in silica-filled epoxy nanocomposites. However, disparities still exist between experimental and modeled fracture energy results. In this dissertation, the thermal, rheological and mechanical behavior of eight different types of silica-filled epoxy nanocomposites was investigated. Each nanocomposite consisted of up to 10 vol% of silica nanoparticles with particle sizes ranging from 20 nm to 200 nm, with a variety of surface treatments and particle structures. Fractographical analysis was conducted with new experimental approaches in order to accurately identify morphological evidence for each proposed toughening mechanism. Overall, three major insights into the fracture behavior of real world silica-filled epoxy nanocomposites were established. First, microcracking was observed as an essential toughening mechanism in silica-filled epoxy nanocomposites. Microcracking was observed on the surface and subsurface of fractured samples in each type of silica-filled epoxy nanocomposite. The additional toughening contribution of microcracking to overall fracture energy yielded excellent agreement between experimental

Estimation of structural film viscosity based on the bubble rise method in a nanofluid.

Science.gov (United States)

Cho, Heon Ki; Nikolov, Alex D; Wasan, Darsh T

2018-04-15

When a single bubble moves at a very low capillary number (10 -7 ) through a liquid with dispersed nanoparticles (nanofluid) inside a vertical tube/capillary, a film is formed between the bubble surface and the tube wall and the nanoparticles self-layer inside the confined film. We measured the film thickness using reflected light interferometry. We calculated the film structural energy isotherm vs. the film thickness from the film-meniscus contact angle measurements using the reflected light interferometric method. Based on the experimental measurement of the film thickness and the calculated values of the film structural energy barrier, we estimated the structural film viscosity vs. the film thickness using the Frenkel approach. Because of the nanoparticle film self-layering phenomenon, we observed a gradual increase in the film viscosity with the decreasing film thickness. However, we observed a significant increase in the film viscosity accompanied by a step-wise decrease in the bubble velocity when the film thickness decreased from 3 to 2 particle layers due to the structural transition in the film. Copyright © 2018 Elsevier Inc. All rights reserved.