Study of Catalyst, Aging Time and Surfactant Effects on Silica Inorganic Polymer Characteristics

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M. Pakizeh

2007-06-01

Full Text Available In the present study the sol-gel method is used for synthesis of amorphous nanostructure silica polymer using tetraethoxysilane (TEOS as silicon source. This polymer can be used in manufacturing of nanoporous asymmetricmembranes. The effect of catalyst on silica particle size has been studied under acidic and basic conditions.زAcid-catalyzed reaction leads to the formation of fine particles while the base-catalyzed reaction produceslarger particles. The presence of cationic template surfactant namely cetyl pyridinium bromide (CPBزdirects the structural formation of the polymer by preventing the highly branched polymeric clusters. This will increase the effective area of the produced silica membrane. Nitrogen physisorption tests by Brunaver- Emmett-Teller (BET and Barrett-Joyner-Halenda (BJH methods revealed that the surface area of the membrane increases significantly around 5-folds when acid-catalyzed reaction is used. 29Si-NMR test is also used to study the aging time effect on the level of silica polymer branching. The results show that in acidic condition, aging time up to three weeks can still affect branching. The calcinations process in which the organic materials and CPB (surfactant are burned and released from the silica particles, is studied on template free silica materials as well as templated silica materials using TGA and DTA techniques.

Use of ground clay brick as a pozzolanic material to reduce the alkali-silica reaction

International Nuclear Information System (INIS)

Turanli, L.; Bektas, F.; Monteiro, P.J.M.

2003-01-01

The objective of this experimental study was to use ground clay brick (GCB) as a pozzolanic material to minimize the alkali-silica reaction expansion. Two different types of clay bricks were finely ground and their activity indices were determined. ASTM accelerated mortar bar tests were performed to investigate the effect of GCB when used to replace cement mass. The microstructure of the mortar was investigated using scanning electron microscopy (SEM). The results showed that the GCBs meet the strength activity requirements of ASTM. In addition, the GCBs were found to be effective in suppressing the alkali-silica reaction expansion. The expansion decreased as the amount of GCBs in the mortar increased

Electrochemical redox reactions in solvated silica sol-gel glass

International Nuclear Information System (INIS)

Opallo, M.

2002-01-01

The studies of electrochemical redox reactions in solvated silica sol-gel glass were reviewed. The methodology of the experiments with emphasis on the direct preparation of the solid electrolyte and the application ultra microelectrodes was described. Generally, the level of the electrochemical signal is not much below that observed in liquid electrolyte. The current depends on time elapsed after gelation, namely the longer time, the smaller current. The differences between electrochemical behaviour of the redox couples in monoliths and thin layers were described. (author)

The effects of supplementary cementitious materials on alkali-silica reaction.

Science.gov (United States)

2015-07-01

The Kansas Department of Transportation (KDOT) has controlled alkali-silica reaction (ASR) for more than : 70 years through the use of selected aggregates. Sand and gravel sources had to be tested using Kansas Test Method : KTMR-23 (1999), Wetting an...

Ordered mesoporous silica prepared by quiescent interfacial growth method - effects of reaction chemistry

Science.gov (United States)

2013-01-01

Acidic interfacial growth can provide a number of industrially important mesoporous silica morphologies including fibers, spheres, and other rich shapes. Studying the reaction chemistry under quiescent (no mixing) conditions is important for understanding and for the production of the desired shapes. The focus of this work is to understand the effect of a number of previously untested conditions: acid type (HCl, HNO3, and H2SO4), acid content, silica precursor type (TBOS and TEOS), and surfactant type (CTAB, Tween 20, and Tween 80) on the shape and structure of products formed under quiescent two-phase interfacial configuration. Results show that the quiescent growth is typically slow due to the absence of mixing. The whole process of product formation and pore structuring becomes limited by the slow interfacial diffusion of silica source. TBOS-CTAB-HCl was the typical combination to produce fibers with high order in the interfacial region. The use of other acids (HNO3 and H2SO4), a less hydrophobic silica source (TEOS), and/or a neutral surfactant (Tweens) facilitate diffusion and homogenous supply of silica source into the bulk phase and give spheres and gyroids with low mesoporous order. The results suggest two distinct regions for silica growth (interfacial region and bulk region) in which the rate of solvent evaporation and local concentration affect the speed and dimension of growth. A combined mechanism for the interfacial bulk growth of mesoporous silica under quiescent conditions is proposed. PMID:24237719

Alkali silica reaction (ASR) in cement free alkali activated sustainable concrete.

Science.gov (United States)

2016-12-19

This report summarizes the findings of an experimental evaluation into alkali silica : reaction (ASR) in cement free alkali-activated slag and fly ash binder concrete. The : susceptibility of alkali-activated fly ash and slag concrete binders to dele...

Alkali-silica reaction of aggregates in real concrete and mortar specimen

Czech Academy of Sciences Publication Activity Database

Lukschová, Šárka

-, č. 18 (2009), s. 75-78 ISSN 1214-9691 Institutional research plan: CEZ:AV0Z30460519 Keywords : alkali-silica reaction * concrete * mocroscopy Subject RIV: DB - Geology ; Mineralogy www.irsm.cas.cz/?Lang=CZE&Menu=25,29,0,0

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

Energy Technology Data Exchange (ETDEWEB)

Somorjai, G.A.

2009-09-14

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

Synthesis and application of silica gel modified with alkoxyalcohols. Alkoxyalcohol shushoku silica gel no gosei to riyo

Energy Technology Data Exchange (ETDEWEB)

Moriguchi, T.; Ishiguro, H.; Matsubara, Y.; Yoshihara, M.; Maeshima, T.; Ito, S. (Kinki University, Osaka (Japan). Faculty of Science and Engineering)

1991-08-20

Several kinds of silica gel modified by alkoxyalcohols were synthesized by refluxing and dehyration and the organic reactions were studied when these silica gels were used as the catalyst. It could be confirmed by FT-IR spectra, DTA and elementary analysis that alkoxylalcohols adhere to the surface of silica gels without any decomposition. The acetate was produced by using alkyl halides. It was found that the modified silica gels had clearly the catalytic action for the reaction with n-hexyl bromide and dibromoethane although unmodified silica gels did not show the catalytic action. The reducing reaction of carbonyl compounds was carried out. The reaction proceeded at 25 centigrade for acetophenone, cyclohexanone, 1-indanone and 2-octanone to produce the corresponding reduction products. 11 refs., 5 figs., 4 tabs.

Silica Gel-Mediated Organic Reactions under Organic Solvent-Free Conditions

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Satoaki Onitsuka

2012-09-01

Full Text Available Silica gel was found to be an excellent medium for some useful organic transformations under organic solvent-free conditions, such as (1 the Friedel-Crafts-type nitration of arenes using commercial aqueous 69% nitric acid alone at room temperature, (2 one-pot Wittig-type olefination of aldehydes with activated organic halides in the presence of tributyl- or triphenylphosphine and Hunig’s base, and (3 the Morita-Baylis-Hillman reaction of aldehydes with methyl acrylate. After the reactions, the desired products were easily obtained in good to excellent yields through simple manipulation.

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.

Polymer-silica hybrids for separation of CO2 and catalysis of organic reactions

Science.gov (United States)

Silva Mojica, Ernesto

Porous materials comprising polymeric and inorganic segments have attracted interest from the scientific community due to their unique properties and functionalities. The physical and chemical characteristics of these materials can be effectively exploited for adsorption applications. This dissertation covers the experimental techniques for fabrication of poly(vinyl alcohol) (PVA) and silica (SiO2) porous supports, and their functionalization with polyamines for developing adsorbents with potential applications in separation of CO2 and catalysis of organic reactions. The supports were synthesized by processes involving (i) covalent cross-linking of PVA, (ii) hydrolysis and poly-condensation of silica precursors (i,e,. sol-gel synthesis), and formation of porous structures via (iii) direct templating and (iv) phase inversion techniques. Their physical structure was controlled by the proper combination of the preparation procedures, which resulted in micro-structured porous materials in the form of micro-particles, membranes, and pellets. Their adsorption characteristics were tailored by functionalization with polyethyleneimine (PEI), and their physicochemical properties were characterized by vibrational spectroscopy (FTIR, UV-vis), microscopy (SEM), calorimetry (TGA, DSC), and adsorption techniques (BET, step-switch adsorption). Spectroscopic investigations of the interfacial cross-linking reactions of PEI and PVA with glutaraldehyde (GA) revealed that PEI catalyzes the cross-linking reactions of PVA in absence of external acid catalysts. In-situ IR spectroscopy coupled with a focal plane array (FPA) image detector allowed the characterization of a gradient interface on a PEI/PVA composite membrane and the investigation of the cross-linking reactions as a function of time and position. The results served as a basis to postulate possible intermediates, and propose the reaction mechanisms. The formulation of amine-functionalized CO2 capture sorbents was based on the

The effects of supplementary cementitious materials on alkali-silica reaction : [technical summary].

Science.gov (United States)

2015-07-01

The Kansas Department of Transportation (KDOT) has controlled alkali-silica : reaction (ASR) for more than 70 years through the use of selected aggregates. : Sand and gravel sources had to be tested using Kansas Test Method KTMR- : 23 (1999), Wetting...

SiC Conversion Coating Prepared from Silica-Graphite Reaction

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Back-Sub Sung

2017-01-01

Full Text Available The β-SiC conversion coatings were successfully synthesized by the SiO(v-graphite(s reaction between silica powder and graphite specimen. This paper is to describe the effects on the characteristics of the SiC conversion coatings, fabricated according to two different reaction conditions. FE-SEM, FE-TEM microstructural morphologies, XRD patterns, pore size distribution, and oxidation behavior of the SiC-coated graphite were investigated. In the XRD pattern and SAD pattern, the coating layers showed cubic SiC peak as well as hexagonal SiC peak. The SiC coatings showed somewhat different characteristics with the reaction conditions according to the position arrangement of the graphite samples. The SiC coating on graphite, prepared in reaction zone (2, shows higher intensity of beta-SiC main peak (111 in XRD pattern as well as rather lower porosity and smaller main pore size peak under 1 μm.

Automated Detection of Alkali-silica Reaction in Concrete using Linear Array Ultrasound Data

Energy Technology Data Exchange (ETDEWEB)

Santos-Villalobos, Hector J [ORNL; Clayton, Dwight A [ORNL; Ezell, N Dianne Bull [ORNL; Clayton, Joseph A [ORNL; Baba, Justin S [ORNL

2017-01-01

Alkali-silica reaction (ASR) is a chemical reaction in either concrete or mortar between hydroxyl ions of the alkalis (sodium and potassium) from hydraulic cement (or other sources), and certain siliceous minerals present in some aggregates. The reaction product, an alkali-silica gel, is hygroscopic having a tendency to absorb water and swell, which under certain circumstances, leads to abnormal expansion and cracking of the concrete. This phenomenon affects the durability and performance of concrete structures severely since it can cause significant loss of mechanical properties. Developing reliable methods and tools that can evaluate the degree of the ASR damage in existing structures, so that informed decisions can be made toward mitigating ASR progression and damage, is important to the long term operation of nuclear power plants especially if licenses are extended beyond 60 years. This paper examines an automated method of determining the extent of ASR damage in fabricated concrete specimens.

Alkali Silica Reaction In The Presence Of Metakaolin - The Significant Role of Calcium Hydroxide

Science.gov (United States)

Zapała-Sławeta, Justyna

2017-10-01

Reducing the internal corrosion, which is the result of reactions between alkalis and reactive aggregates is especially important in ensuring durability properties of concrete. One of the methods of inhibiting the reaction is using some mineral additives which have pozzolanic properties. This paper presents the efficacy of high-reactivity metakaolin in reducing expansion due to alkali-silica reaction. It was demonstrated that metakaolin in the amount from 5% to 20% by mass of Portland cement reduce linear expansion of mortar bars with opal aggregate. Nevertheless, the safe expansion level in the specimens, classified as non-destructive to concrete, was recorded for the mortars prepared with 20% addition of metakaolin. Depletion of free calcium hydroxide content was considered as one of the most beneficial effects of metakaolin in controlling alkali silica reaction. Based on thermogravimetric analysis (TGA) performed on mortar bars with and without metakaolin the differences in portlandite content were determined. Microstructural observation of the specimens containing metakaolin indicated the presence of a reaction products but fewer in number than those forming in the mortars without mineral additives.

In-situ reactions in hybrid aluminum alloy composites during incorporating silica sand in aluminum alloy melts

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Benjamin F. Schultz

2016-07-01

Full Text Available In order to gain a better understanding of the reactions and strengthening behavior in cast aluminum alloy/silica composites synthesized by stir mixing, experiments were conducted to incorporate low cost foundry silica sand into aluminum composites with the use of Mg as a wetting agent. SEM and XRD results show the conversion of SiO2 to MgAl2O4 and some Al2O3 with an accompanying increase in matrix Si content. A three-stage reaction mechanism proposed to account for these changes indicates that properties can be controlled by controlling the base Alloy/SiO2/Mg chemistry and reaction times. Experimental data on changes of composite density with increasing reaction time and SiO2 content support the three-stage reaction model. The change in mechanical properties with composition and time is also described.

Thermogravimetric analyses and mineralogical study of polymer modified mortar with silica fume

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Alessandra Etuko Feuzicana de Souza Almeida

2006-09-01

Full Text Available Mineral and organic additions are often used in mortars to improve their properties. Microstructural investigation concerning the effects of styrene acrylic polymer and silica fume on the mineralogical composition of high-early-strength portland cement pastes after 28 days of hydration are presented in this paper. Thermogravimetry and derivative thermogravimetry were used to study the interaction between polymers and cement, as well as the extent of pozzolanic reaction of the mortars with silica fume. Differential scanning calorimetry and X ray diffraction were used to investigate the cement hydration and the effect of the additions. The results showed that the addition of silica fume and polymer reduces the portlandite formation due to delaying of Portland cement hydration and pozzolanic reaction.

Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

Science.gov (United States)

Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

2017-09-01

Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

Relation of expansion due to alkali silica reaction to the degree of reaction measured by SEM image analysis

International Nuclear Information System (INIS)

Haha, M. Ben; Gallucci, E.; Guidoum, A.; Scrivener, K.L.

2007-01-01

Scanning Electron Microscopy Image Analysis (SEM-IA) was used to quantify the degree of alkali silica reaction in affected microbars, mortar and concrete prisms. It was found that the degree of reaction gave a unique correlation with the macroscopic expansion for three different aggregates, stored at three temperatures and with two levels of alkali. The relationships found for the concretes and the mortars overlap when normalised by the aggregate content. This relationship seems to be linear up to a critical reaction degree which coincides with crack initiation within the reactive aggregates

A test on reactive force fields for the study of silica dimerization reactions

Energy Technology Data Exchange (ETDEWEB)

Moqadam, Mahmoud; Riccardi, Enrico; Trinh, Thuat T.; Åstrand, Per-Olof; Erp, Titus S. van, E-mail: titus.van.erp@ntnu.no [Department of Chemistry, Norwegian University of Science and Technology (NTNU), Høgskoleringen 5, Realfagbygget D3-117, 7491 Trondheim (Norway)

2015-11-14

We studied silica dimerization reactions in the gas and aqueous phase by density functional theory (DFT) and reactive force fields based on two parameterizations of ReaxFF. For each method (both ReaxFF force fields and DFT), we performed constrained geometry optimizations, which were subsequently evaluated in single point energy calculations using the other two methods. Standard fitting procedures typically compare the force field energies and geometries with those from quantum mechanical data after a geometry optimization. The initial configurations for the force field optimization are usually the minimum energy structures of the ab initio database. Hence, the ab initio method dictates which structures are being examined and force field parameters are being adjusted in order to minimize the differences with the ab initio data. As a result, this approach will not exclude the possibility that the force field predicts stable geometries or low transition states which are realistically very high in energy and, therefore, never considered by the ab initio method. Our analysis reveals the existence of such unphysical geometries even at unreactive conditions where the distance between the reactants is large. To test the effect of these discrepancies, we launched molecular dynamics simulations using DFT and ReaxFF and observed spurious reactions for both ReaxFF force fields. Our results suggest that the standard procedures for parameter fitting need to be improved by a mutual comparative method.

Effect of SiO2 concentration in silica sol on interface reaction during titanium alloy investment casting

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Ya-meng Wei

2018-01-01

Full Text Available Using silica sol as a binder for titanium investment casting is very attractive due to its good stability and reasonable cost as compared with yttrium sol and zirconium sol. However, the mechanism of interface reaction in the related system remains unclear. In this investigation, the interface reaction between Y2O3-SiO2 (Y-Si shell mold and titanium alloys was studied. A group of shell molds were prepared by using Y2O3 sand and silica sol with different contents of SiO2. Ti-6Al-4V alloy was cast under vacuum by gravity casting through cold crucible induction melting (CCIM method. Scanning electron microscopy (SEM and energy dispersive x-ray spectroscopy (EDS were employed to characterize the micromorphology and composition of the reaction area, respectively. X-ray photoelectron spectroscopy (XPS was used to confirm the valence state of relevant elements. White light interferometer (WLI was used to obtain the surface topography of Y-Si shells. The results show that the thickness of reaction layers is below 3 μm when the SiO2 content of silica sol is below 20wt.%. Whereas, when the SiO2 content increases to 25wt.%, the thickness of the reaction layer increases sharply to about 15 μm. There is a good balance between chemical inertness and mechanical performance when the SiO2 content is between 15 and 20wt.%. Moreover, it was found that the distribution of SiO2 and the roughness at the surface of the shell are the key factors that determine the level of reaction.

Nondestructive analysis of alkali-silica reaction damage in concrete slabs using shear waves

Science.gov (United States)

Khazanovich, Lev; Freeseman, Katelyn; Salles, Lucio; Clayton, Dwight

2018-04-01

Alkali-silica reaction (ASR) is the chemical reaction that occurs in concrete. It is caused by the interaction of alkalis in Portland cement and silica in aggregates and results in microcracks within the material. This type of damage has been the focus of nondestructive evaluation efforts in recent history, but no work was done on in-situ structures or large-scale samples. To address these limitations, an ultrasonic linear array device, MIRA, was utilized for this research. An experimental investigation was performed on four slabs with various levels of alkali-silica reaction at the Electric Power Research Institute (EPRI) [1]. One-period impulses with a target of 50kHz center frequency were selected in this study. We propose the use of the Hilbert Transform Indicator (HTI) for quantification of ASR damage [2]. A higher HTI value would be indicative of damaged concrete, while a low value represents sound concrete. In general, values below 90 are regarded as an indicator of sound concrete while values above 100 indicate the presence of damage [3]. The ability of the HTI values to distinguish between areas of damaged concrete was evident via the production of color intensity maps. The maps show that the control specimen, was in good condition, while other slabs exhibited higher levels of damage as indicated by the HTI values. It should be noted that extreme damage conditions were not present in any of the slabs. Evaluation of migration-based reconstructions can give a qualitative characterization of large scale or excessive subsurface damage. However, for detection of stochastic damage mechanisms such as freeze-thaw damage, evaluation of the individual time-history data can provide additional information. A comparison of the spatially diverse measurements on several concrete slabs with varying freeze-thaw damage levels is given in this study. Signal characterization scans of different levels of freeze-thaw damage at various transducer spacing is investigated. The

Serpentinization processes: Influence of silica

Science.gov (United States)

Huang, R.; Sun, W.; Ding, X.; Song, M.; Zhan, W.

2016-12-01

Serpentinization systems are highly enriched in molecular hydrogen (H2) and hydrocarbons (e.g. methane, ethane and propane). The production of hydrocarbons results from reactions between H2 and oxidized carbon (carbon dioxide and carbon monoxide), which possibly contribute to climate changes during early history of the Earth. However, the influence of silica on the production of H2 and hydrocarbons was poorly constrained. We performed experiments at 311-500 °C and 3.0 kbar using mechanical mixtures of silica and olivine in ratios ranging from 0 to 40%. Molecular hydrogen (H2), methane, ethane and propane were formed, which were analyzed by gas chromatography. It was found that silica largely decreased H2 production. Without any silica, olivine serpentinization produced 94.5 mmol/kg H2 after 20 days of reaction time. By contrast, with the presence of 20% silica, H2 concentrations decreased largely, 8.5 mmol/kg. However, the influence of silica on the production of hydrocarbons is negligible. Moreover, with the addition of 20%-40% silica, the major hydrous minerals are talc, which was quantified according to an established standard curve calibrated by infrared spectroscopy analyses. It shows that silica greatly enhances olivine hydration, especially at 500 °C. Without any addition of silica, reaction extents were serpentinization at 500 °C and 3.0 kbar. By contrast, with the presence of 50% silica, olivine was completely transformed to talc within 9 days. This study indicates that silica impedes the oxidation of ferrous iron into ferric iron, and that rates of olivine hydration in natural geological settings are much faster with silica supply.

Concrete alkali-silica reaction and nuclear radiation damage

International Nuclear Information System (INIS)

Ichikawa, Tsuneki

2008-01-01

The deterioration of concrete by alkali-silica reaction of aggregates (ASR) and the effect of nuclear radiations on the ASR have been reviewed based on our studies on the mechanism of ASR and the effect of nuclear radiations on the resistivity of minerals to alkaline solution. It has been found that the ASR is initiated by the attack of alkaline solution in concrete to silicious aggregates to convert them into hydrated alkali silicate. The consumption of alkali hydroxide by the aggregates induces the dissolution of Ca 2+ ions into the solution. The alkali silicate surrounding the aggregates then reacts with Ca 2+ ions to convert to insoluble tight and rigid reaction rims. The reaction rim allows the penetration of alkaline solution but prevents the leakage of viscous alkali silicate, so that alkali silicate generated afterward is accumulated in the aggregate to give an expansive pressure enough for cracking the aggregate and the surrounding concrete. The effect of nuclear radiation on the reactivity of quartz and plagioclase, a part of major minerals composing volcanic rocks as popular aggregates, to alkaline solution has been examined for clarifying whether nuclear radiations accelerates the ASR. It has been found that the irradiation of these minerals converts them into alkali-reactive amorphous ones. The radiation dose for plagioclase is as low as 10 8 Gy, which suggests that the ASR of concrete surrounding nuclear reactors is possible to be accelerated by nuclear radiation. (author)

Studies on silica sol-clay particle interactions by small-angle neutron scattering

International Nuclear Information System (INIS)

Moini, A.; Pinnavaia, T.J.; Michigan State Univ., East Lansing; Thiyagarajan, P.; White, J.W.

1988-01-01

SANS data were collected on a series of hydrolyzed silica and silica-clay complexes prepared from a 40 A silica sol and aqueous suspensions of Na + montmorillonite. The hydrolyzed silica product showed a peak centered at Q=0.0856 A -1 corresponding to a distance of 73 A between the sol particles. For such an evaporated gel in which the particles are in close contact, this distance is expected to be very close to the particle diameter indicating partial aggregation of the original spheres. A similar feature was observed in the SANS data for silica-clay products indicating the presence of some unintercalated silica. The intensity of this scattering was found to be dependent on the silica:clay ratio and the reaction time. The SANS data in the region from Q=0.006 to 0.025 A -1 were characteristic of clay scattering and exhibited a power-law behavior. The change in the slope of this curve upon reaction of the clay with the silica sol was interpreted in terms of a separation of clay platelets caused by a binding interaction with the sol particles. (orig.)

Liquid Phase Deposition of Silica on the Hexagonally Close-Packed Monolayer of Silica Spheres

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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.

Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction

International Nuclear Information System (INIS)

Xu, Wei; Li, Yani; Yu, Bo; Yang, Jindou; Zhang, Ying; Chen, Xi; Zhang, Guofang; Gao, Ziwei

2015-01-01

A successive anchoring of Ti(NMe 2 ) 4 , cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on silica was conducted by SOMC strategy in moderate conditions. The silica, monitored by in-situ Fourier transform infrared spectroscopy (in-situ FT-IR), was pretreated at different temperatures (200, 500 and 800 °C). The ligand tailored silica-supported titanium complexes were characterized by in-situ FT-IR, 13 C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), X-ray absorption near edge structure (XANES) and elemental analysis in detail, verifying that the surface titanium species are single sited. The catalytic activity of the ligand tailored single-site silica supported titanium complexes was evaluated by a cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the dehydroxylation temperatures of silica and the configuration of the ligands. - Graphical abstract: The ligand-tailored silica supported “single site” titanium complexes were synthesized by SOMC strategy and fully characterized. Their catalytic activity were evaluated by benzaldehyde silylcyanation. - Highlights: • Single-site silica supported Ti active species was prepared by SOMC technique. • O-donor ligand tailored Ti surface species was synthesized. • The surface species was characterized by XPS, 13 C CP-MAS NMR, XANES etc. • Catalytic activity of the Ti active species in silylcyanation reaction was evaluated

Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction

Energy Technology Data Exchange (ETDEWEB)

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

2015-01-15

A successive anchoring of Ti(NMe{sub 2}){sub 4}, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on silica was conducted by SOMC strategy in moderate conditions. The silica, monitored by in-situ Fourier transform infrared spectroscopy (in-situ FT-IR), was pretreated at different temperatures (200, 500 and 800 °C). The ligand tailored silica-supported titanium complexes were characterized by in-situ FT-IR, {sup 13}C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), X-ray absorption near edge structure (XANES) and elemental analysis in detail, verifying that the surface titanium species are single sited. The catalytic activity of the ligand tailored single-site silica supported titanium complexes was evaluated by a cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the dehydroxylation temperatures of silica and the configuration of the ligands. - Graphical abstract: The ligand-tailored silica supported “single site” titanium complexes were synthesized by SOMC strategy and fully characterized. Their catalytic activity were evaluated by benzaldehyde silylcyanation. - Highlights: • Single-site silica supported Ti active species was prepared by SOMC technique. • O-donor ligand tailored Ti surface species was synthesized. • The surface species was characterized by XPS, {sup 13}C CP-MAS NMR, XANES etc. • Catalytic activity of the Ti active species in silylcyanation reaction was evaluated.

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)

Particle size effect of redox reactions for Co species supported on silica

International Nuclear Information System (INIS)

Chotiwan, Siwaruk; Tomiga, Hiroki; Katagiri, Masaki; Yamamoto, Yusaku; Yamashita, Shohei; Katayama, Misaki; Inada, Yasuhiro

2016-01-01

Conversions of chemical states during redox reactions of two silica-supported Co catalysts, which were prepared by the impregnation method, were evaluated by using an in situ XAFS technique. The addition of citric acid into the precursor solution led to the formation on silica of more homogeneous and smaller Co particles, with an average diameter of 4 nm. The supported Co 3 O 4 species were reduced to metallic Co via the divalent CoO species during a temperature-programmed reduction process. The reduced Co species were quantitatively oxidized with a temperature-programmed oxidation process. The higher observed reduction temperature of the smaller CoO particles and the lower observed oxidation temperature of the smaller metallic Co particles were induced by the higher dispersion of the Co oxide species, which apparently led to a stronger interaction with supporting silica. The redox temperature between CoO and Co 3 O 4 was found to be independent of the particle size. - Graphical abstract: Chemical state conversions of SiO 2 -supported Co species and the particle size effect have been analyzed by means of in situ XAFS technique. The small CoO particles have endurance against the reduction and exist in a wide temperature range. Display Omitted - Highlights: • The conversions of the chemical state of supported Co species during redox reaction are evaluated. • In operando XAFS technique were applied to measure redox properties of small Co particles. • A small particle size affects to the redox temperatures of cobalt catalysts.

Characterization of alkali silica reaction gels using Raman spectroscopy

International Nuclear Information System (INIS)

Balachandran, C.; Muñoz, J.F.; Arnold, T.

2017-01-01

The ability of Raman spectroscopy to characterize amorphous materials makes this technique ideal to study alkali silica reaction (ASR) gels. The structure of several synthetic ASR gels was thoroughly characterized using Raman Spectroscopy. The results were validated with additional techniques such as Fourier transmission infrared spectroscopy, X-ray powder diffraction and thermogravimetric analysis. The Raman spectra were found to have two broad bands in the 800 to 1200 cm −1 range and the 400 to 700 cm −1 range indicating the amorphous nature of the gel. Important information regarding the silicate polymerization was deduced from both of these spectral regions. An increase in alkali content of the gels caused a depolymerization in the silicate framework which manifested in the Raman spectra as a gradual shift of predominant peaks in both regions. The trends in silicate depolymerization were in agreement with results from a NMR spectroscopy study on similar synthetic ASR gels.

Interfacial interaction between the epoxidized natural rubber and silica in natural rubber/silica composites

Energy Technology Data Exchange (ETDEWEB)

Xu, Tiwen [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510640 (China); Jia, Zhixin, E-mail: zxjia@scut.edu.cn [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510640 (China); Luo, Yuanfang; Jia, Demin [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510640 (China); Peng, Zheng [Agricultural Product Processing Research Institute, Chinese Academy of Tropical Agriculture Sciences, Zhanjiang 524001 (China)

2015-02-15

Highlights: • Substantiate the ring open reaction between Si-OH of silica and epoxy groups of ENR. • ENR can act as a bridge between NR and silica to enhance the interfacial interaction. • As a modifier, ENR gets the potential to be used in the tread of green tire for improving the wet skid resistance apparently. - Abstract: The epoxidized natural rubber (ENR) as an interfacial modifier was used to improve the mechanical and dynamical mechanical properties of NR/silica composites. In order to reveal the interaction mechanism between ENR and silica, the ENR/Silica model compound was prepared by using an open mill and the interfacial interaction of ENR with silica was investigated by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), X-ray diffraction (XRD) and stress–strain testing. The results indicated that the ring-opening reaction occurs between the epoxy groups of ENR chains and Si-OH groups on the silica surfaces and the covalent bonds are formed between two phases, which can improve the dispersion of silica in the rubber matrix and enhance the interfacial combination between rubber and silica. The ring-opening reaction occurs not only in vulcanization process but also in mixing process, meanwhile, the latter seems to be more important due to the simultaneous effects of mechanical force and temperature.

Distinct metamorphic evolution of alternating silica-saturated and silica-deficient microdomains within garnet in ultrahigh-temperature granulites: An example from Sri Lanka

Directory of Open Access Journals (Sweden)

P.L. Dharmapriya

2017-09-01

Full Text Available Here we report the occurrence of garnet porphyroblasts that have overgrown alternating silica-saturated and silica deficient microdomains via different mineral reactions. The samples were collected from ultrahigh-temperature (UHT metapelites in the Highland Complex, Sri Lanka. In some of the metapelites, garnet crystals have cores formed via a dehydration reaction, which had taken place at silica-saturated microdomains and mantle to rim areas formed via a dehydration reaction at silica-deficient microdomains. In contrast, some other garnets in the same rock cores had formed via a dehydration reaction which occurred at silica-deficient microdomains while mantle to rim areas formed via a dehydration reaction at silica-saturated microdomains. Based on the textural observations, we conclude that the studied garnets have grown across different effective bulk compositional microdomains during the prograde evolution. These microdomains could represent heterogeneous compositional layers (paleobedding/laminations in the precursor sediments or differentiated crenulation cleavages that existed during prograde metamorphism. UHT metamorphism associated with strong ductile deformation, metamorphic differentiation and crystallization of locally produced melt may have obliterated the evidence for such microdomains in the matrix. The lack of significant compositional zoning in garnet probably due to self-diffusion during UHT metamorphism had left mineral inclusions as the sole evidence for earlier microdomains with contrasting chemistry.

Continuing studies of alkali-aggregate reactions in concrete

International Nuclear Information System (INIS)

Gilliot, J.E.; Beddoes, R.J.

1981-01-01

Studies are continuing into the nature of the different forms of the alkali-aggregate reaction. No general agreement exists as to the detailed nature of the expansive mechanisms. Alkali is known to react internally with opaline silica because of its microporous nature whereas reaction at the external surface is thought to be relatively more important in the case of quartz. A combination of Fourier shape and surface texture analysis, microscopy and osmotic studies is being used to obtain information on the relative importance of these two forms of alkaline attack on silica. Analytical methods are much more rapid than dimensional change tests and it is hoped that a better understanding of the expansion mechanism will lead to more certain recognition of potentially alkali expansive aggregates

Effect of alkali–silica reaction on the shear strength of reinforced concrete structural members. A numerical and statistical study

Energy Technology Data Exchange (ETDEWEB)

Saouma, Victor E.; Hariri-Ardebili, Mohammad Amin [Department of Civil Engineering, University of Colorado, Boulder, CO 80305 (United States); Le Pape, Yann, E-mail: lepapeym@ornl.gov [Oak Ridge National Laboratory, One Bethel Valley Road, Oak Ridge, TN 37831 (United States); Balaji, Rajagopalan [Department of Civil Engineering, University of Colorado, Boulder, CO 80305 (United States)

2016-12-15

Highlights: • Alkali–silica reaction (ASR) affects reinforced structures shear strength. • Statistical analysis indicates large scattering of post-ASR strength losses/gains. • Competitive structural and materials mechanisms affect the residual shear strength. - Abstract: The residual structural shear resistance of concrete members without shear reinforcement and subject to alkali–aggregate reaction (ASR) is investigated by finite element analysis. A parametric numerical study of 648 analyses considering various structural members’ geometries, boundary conditions, ASR-induced losses of materials properties, ASR expansions and reinforcement ratios is conducted. As a result of competitive mechanisms (e.g., ASR-induced prestressing caused by the longitudinal reinforcement) and loss of concrete materials properties, important scatter in terms of gain or loss of shear strength is observed: about 50% of the studied configurations lead to a degradation of structural performance. The range of variation in terms of post-ASR shear resistance is extremely scattered, in particular, when ASR results in out-of-plane expansion only. Influencing factors are derived by two methods: (i) visual inspection of boxplots and probability distributions, and (ii) information criteria within multiple-linear regression analysis.

Elastic modulus of the alkali-silica reaction rim in a simplified calcium-alkali-silicate system determined by nano-indentation

NARCIS (Netherlands)

Zheng, Kunpeng; Lukovic, M.; De Schutter, Geert; Ye, G.; Taerwe, Luc

2016-01-01

This work aims at providing a better understanding of the mechanical properties of the reaction rim in the alkali-silica reaction. The elastic modulus of the calcium alkali silicate constituting the reaction rim, which is formed at the interface between alkali silicate and Ca(OH)2 in a

Interfacial interaction between the epoxidized natural rubber and silica in natural rubber/silica composites

Science.gov (United States)

Xu, Tiwen; Jia, Zhixin; Luo, Yuanfang; Jia, Demin; Peng, Zheng

2015-02-01

The epoxidized natural rubber (ENR) as an interfacial modifier was used to improve the mechanical and dynamical mechanical properties of NR/silica composites. In order to reveal the interaction mechanism between ENR and silica, the ENR/Silica model compound was prepared by using an open mill and the interfacial interaction of ENR with silica was investigated by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), X-ray diffraction (XRD) and stress-strain testing. The results indicated that the ring-opening reaction occurs between the epoxy groups of ENR chains and Si-OH groups on the silica surfaces and the covalent bonds are formed between two phases, which can improve the dispersion of silica in the rubber matrix and enhance the interfacial combination between rubber and silica. The ring-opening reaction occurs not only in vulcanization process but also in mixing process, meanwhile, the latter seems to be more important due to the simultaneous effects of mechanical force and temperature.

Alumina plate containing photosystem I reaction center complex oriented inside plate-penetrating silica nanopores.

Science.gov (United States)

Kamidaki, Chihiro; Kondo, Toru; Noji, Tomoyasu; Itoh, Tetsuji; Yamaguchi, Akira; Itoh, Shigeru

2013-08-22

The photosynthetic photosystem I reaction center complex (PSI-RC), which has a molecular diameter of 21 nm with 100 pigments, was incorporated into silica nanopores with a 100-nm diameter that penetrates an alumina plate of 60-μm thickness to make up an inorganic-biological hybrid photocell. PSI-RCs, purified from a thermophilic cyanobacterium, were stable inside the nanopores and rapidly photoreduced a mediator dye methyl viologen. The reduced dye was more stable inside nanopores suggesting the decrease of dissolved oxygen. The analysis by a cryogenic electron spin paramagnetic resonance indicated the oriented arrangement of RCs inside the 100-nm nanopores, with their surface parallel to the silica wall and perpendicular to the plane of the alumina plate. PSI RC complex in the semicrystalline orientation inside silica nanopores can be a new type of light energy conversion unit to supply strong reducing power selectively to other molecules inside or outside nanopores.

Effect of support on hydro-metathesis of propene: A comparative study of W(CH 3 ) 6 anchored to silica vs. silica-alumina

KAUST Repository

Tretiakov, Mykyta

2018-03-27

Hydro-metathesis of propene was carried out by using well-defined W(CH3)6 supported on silica and silica-alumina. It was observed that W(CH3)6 supported silica-alumina catalyst is much better (TON 4577) than the silica supported catalyst (TON 2104). We demonstrated that the present catalysts are much better than the previously reported (tantalum hydride/KCC-1, TON 786) catalyst. For the first time, we observed the formation of n-decane from propene, which enables us to think of using cheaper raw materials and converting them to petroleum range alkanes using hydro-metathesis reaction.

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)

Synthesis of hybrid interfacial silica-based nanospheres composite as a support for ultra-small palladium nanoparticle and application of PdNPs/HSN in Mizoroki-Heck reaction

Science.gov (United States)

Rostamnia, Sadegh; Kholdi, Saba

2017-12-01

The silica based hollow nanosphere (silica-HNS) containing polymer of polyaniline was synthesized and chosen as a promising support for PdNPs. Then it was applied as a green catalyst in the reaction of Heck coupling with high yield. TEM and SEM-EDX/mapping images were used to study the structure and morphology. FT-IR spectroscopy, Thermal gravimetry analysis (TGA), and BET were used to characterize and investigate the catalyst. Also, the amounts of Pd loading were characterized by ICP-AES technique. Catalyst recyclability showed 5 successful runs for the reaction.

Water adsorption on amorphous silica surfaces: a Car-Parrinello simulation study

International Nuclear Information System (INIS)

Mischler, Claus; Horbach, Juergen; Kob, Walter; Binder, Kurt

2005-01-01

A combination of classical molecular dynamics (MD) and ab initio Car-Parrinello molecular dynamics (CPMD) simulations is used to investigate the adsorption of water on a free amorphous silica surface. From the classical MD, SiO 2 configurations with a free surface are generated which are then used as starting configurations for the CPMD. We study the reaction of a water molecule with a two-membered ring at the temperature T = 300 K. We show that the result of this reaction is the formation of two silanol groups on the surface. The activation energy of the reaction is estimated and it is shown that the reaction is exothermic

Pilot-scale study of the radiation-induced silica removal from underground brackish water in Saudi Arabia

Energy Technology Data Exchange (ETDEWEB)

Aljohani, Mohammed S. [King Abdulaziz Univ., Jeddah (Saudi Arabia). Nuclear Engineering Dept.

2017-08-01

Silica scaling deposition in industrial water systems is one of the biggest challenges facing the water treatment industry due the low solubility of the scalants in the feed waters. In this preliminary work, we investigated the effectiveness of the ionizing radiation induced removal of silica in water sample from the Salbukh, Saudi Arabia, water treatment plant by using metallic iron as the source of ferric hydroxide to co-precipitate the silica. The influence of several reaction parameters, i.e. iron powder dosage, radiation dose, initial pH and equilibrium pH effect were investigated. In the optimum conditions, up to 75% of silica was removed. This preliminary study showed that this environmentally friendly process is effective in silica removal from underground water.

Preparation of silica nanoparticles through microwave-assisted acid-catalysis.

Science.gov (United States)

Lovingood, Derek D; Owens, Jeffrey R; Seeber, Michael; Kornev, Konstantin G; Luzinov, Igor

2013-12-16

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan δ solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials' morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by Stöber's methods, which have smooth surfaces.

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.

Vulcanization characteristics and dynamic mechanical behavior of natural rubber reinforced with silane modified silica.

Science.gov (United States)

Chonkaew, Wunpen; Minghvanish, Withawat; Kungliean, Ulchulee; Rochanawipart, Nutthaya; Brostow, Witold

2011-03-01

Two silane coupling agents were used for hydrolysis-condensation reaction modification of nanosilica surfaces. The surface characteristics were analyzed using Fourier transform infrared spectroscopy (FTIR). The vulcanization kinetics of natural rubber (NR) + silica composites was studied and compared to behavior of the neat NR using differential scanning calorimetry (DSC) in the dynamic scan mode. Dynamic mechanical analysis (DMA) was performed to evaluate the effects of the surface modification. Activation energy E(a) values for the reaction are obtained. The presence of silica, modified or otherwise, inhibits the vulcanization reaction of NR. The neat silica containing system has the lowest cure rate index and the highest activation energy for the vulcanization reaction. The coupling agent with longer chains causes more swelling and moves the glass transition temperature T(g) downwards. Below the glass transition region, silica causes a lowering of the dynamic storage modulus G', a result of hindering the cure reaction. Above the glass transition, silica-again modified or otherwise-provides the expected reinforcement effect.

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.

Direct synthesis of acid-base bifunctionalized hexagonal mesoporous silica and its catalytic activity in cascade reactions.

Science.gov (United States)

Shang, Fanpeng; Sun, Jianrui; Wu, Shujie; Liu, Heng; Guan, Jingqi; Kan, Qiubin

2011-03-01

A series of efficient acid-base bifunctionalized hexagonal mesoporous silica (HMS) catalysts contained aminopropyl and propanesulfonic acid have been synthesized through a simple co-condensation by protection of amino group. The results of small-angle XRD, TEM, and N(2) adsorption-desorption measurements show that the resultant materials have mesoscopic structures. X-ray photoelectron spectroscopies, elemental analysis (EA), back titration, (29)Si NMR and (13)C NMR confirm that the organosiloxanes were condensed as a part of the silica framework. The resultant catalysts exhibit excellent acid-basic properties, which make them possess high activity for one-pot deacetalization-Knoevenagel and deacetalization-nitroaldol (Henry) reactions. Copyright © 2010 Elsevier Inc. All rights reserved.

Study of silica sol-gel materials for sensor development

Science.gov (United States)

Lei, Qiong

in disrupting R6G/silica attraction. Similar post-grafting method was applied to highly hydrated silica hydrogel monoliths. Rhodamine 6G (R6G) and fluorescein (Fl) molecules were used as probes to monitor the surface modification inside silica hydrogel by measuring anisotropy values of doped dyes. Due to the larger pore sizes, pore surface modification inside hydrogel was more effective than in alcogel. Surface modification by chemical reactions of 3-Aminopropyltrimethoxysilane (APTS) and methyltriethoxysilane (MTES) showed dramatic effect on guest molecule mobility, whereas surface modification by physical method, that is to increase ionic strength by using 1.0 M sodium chloride or to neutralize pore surfaces by adding pH 2.0 hydrochloric acid, barely showed any effect. Charge-reversal by APTS is a more effective way to modify pore surfaces in hydrogel than hydrophobic capping from MTES. The ease of tracking surface modification inside hydrogel by simply locating R6G dye band, and the negligible pore fluid effect on R6G in modified hydrogel makes R6G a better probe than Fl to monitor the pore surface modification process in silica hydrogel monoliths. During the study of post-grafting on silica alcogel thin film, a new approach to produce stable silica hydrogel-like thin films was discovered. Homogeneous thin film hydrogel-like samples with thickness between 100 nm and 300 nm were produced, and they showed a very hydrophilic surface, high dye loading capacity, and the support of molecular diffusion. The reactive stage of starting silica gel matrix was elongated by increasing environmental humidity, the reproducibility of sample preparation was greatly improved by controlling environmental humidity, and the dye loading capacity of samples was improved more than ten times by using phosphate buffer solutions (PBS). The concentration of R6G trapped inside hydrogel-like thin film could reach as high as 900 times of its saturated aqueous solution. Dye encapsulation can

Volcanic Aggregates from Azores and Madeira Archipelagos (Portugal): An Overview Regarding the Alkali Silica Reactions

Science.gov (United States)

Medeiros, Sara; Ramos, Violeta; Fernandes, Isabel; Nunes, João Carlos; Fournier, Benoit; Santos Silva, António; Soares, Dora

2017-12-01

Alkali-silica reaction (ASR) is a type of deterioration that has been causing serious expansion, cracking and durability/operational issues in concrete structures worldwide. The presence of sufficient moisture, high alkali content in the cement paste and reactive forms of silica in the aggregates are the required conditions for this reaction to occur. Reactive aggregates of volcanic nature have been reported in different countries such as Japan, Iceland and Turkey, among others. The presence of silica minerals and SiO2-rich volcanic glass is regarded as the main cause for the reactivity of volcanic rocks. In Portugal, volcanic aggregates are mainly present in Azores and Madeira Archipelagos and, for several years, there was no information regarding the potential alkali-reactivity of these rocks. Since the beginning of this decade some data was obtained by the work of Medeiros (2011) and Ramos (2013) and by the national research projects ReAVA, (Characterization of potential reactivity of the volcanic aggregates from the Azores Archipelago: implications on the durability of concrete structures) and IMPROVE (Improvement of performance of aggregates in the inhibition of alkali-aggregate reactions in concrete), respectively. In order to investigate the potential alkali-reactivity of aggregates from both archipelagos, a total of sixteen aggregates were examined under the optical microscope and, some of them, also under the Scanning Electron Microscope with Energy Dispersive X-ray Spectroscopy. A set of geochemical analyses and laboratory expansion tests were also performed on those volcanic aggregates. The main results showed that the presence of volcanic glass is rare in both archipelagos and that the samples of Madeira Archipelago contain clay minerals (mainly from scoria/tuff formations inter-layered with the lava flows), which can play a role in concrete expansion. The results of the laboratory tests showed that one of the samples performed as potentially reactive

Photooxidation of ethylene over Cu-modified and unmodified silica

OpenAIRE

Ichihashi, Yuichi; Matsumura, Yasuyuki

2003-01-01

Silica catalyzes photooxidation of ethylene to carbon dioxide and modification of copper on silica results in the lower reaction rate and partial production of ethylene oxide. The reaction does not proceed by the light irradiation through a color filter (λ>280 nm). ESR measurement indicates that radical oxygen species assignable T-shape Si − O3− can be produced on silica by UV irradiation at 77 K. The same species are also found on silica modified with copper by UV irradiation whi...

Sonochemical synthesis of silica particles and their size control

Energy Technology Data Exchange (ETDEWEB)

Kim, Hwa-Min [Advanced Materials and Chemical Engineering, Catholic University of Daegu, Gyeongbuk 38430 (Korea, Republic of); Lee, Chang-Hyun [Electronic and Electrical Engineering, Catholic University of Daegu, Gyeongbuk 38430 (Korea, Republic of); Kim, Bonghwan, E-mail: bhkim@cu.ac.kr [Electronic and Electrical Engineering, Catholic University of Daegu, Gyeongbuk 38430 (Korea, Republic of)

2016-09-01

Graphical abstract: - Highlights: • Silica particles were easily prepared by an ultrasound-assisted sol–gel method. • The particle size was controlled by the ammonium hydroxide/water molar ratio. • The size-controlled diameter of silica particles ranged from 40 to 400 nm. • The particles were formed in a relatively short reaction time. - Abstract: Using an ultrasound-assisted sol–gel method, we successfully synthesized very uniformly shaped, monodisperse, and size-controlled spherical silica particles from a mixture of ethanol, water, and tetraethyl orthosilicate in the presence of ammonia as catalyst, at room temperature. The diameters of the silica particles were distributed in the range from 40 to 400 nm; their morphology was well characterized by scanning electron microscopy. The silica particle size could be adjusted by choosing suitable concentrations of ammonium hydroxide and water, which in turn determined the nucleation and growth rates of the particles during the reaction. This sonochemical-based silica synthesis offers an alternative way to produce spherical silica particles in a relatively short reaction time. Thus, we suggest that this simple, low-cost, and efficient method of preparing uniform silica particles of various sizes will have practical and wide-ranging industrial applicability.

Effect of Alkali-Silica Reaction on Shear Strength of Reinforced Concrete Structural Members

Energy Technology Data Exchange (ETDEWEB)

Hariri-Ardebili, Mohammad [Univ. of Colorado, Boulder, CO (United States); Saouma, Victor [Univ. of Colorado, Boulder, CO (United States); Le Pape, Yann [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2015-10-01

Alkali-silica reaction (ASR) was discovered in the early 40s by Stanton (1940) of the California Division of Highways. Since, it has been recognized as a major degradation mechanism for concrete dams and transportation infrastructures. Sometimes described as the ’cancer of concrete’, this internal swelling mechanism causes expansion, cracking and loss of mechanical properties. There are no known economically viable solutions applicable to massive concrete to prevent the reaction once initiated. The e ciency of the mitigation strategies for ASR subjected structures is limited. Several cases of ASR in nuclear generating stations have been disclosed in Japan (Takatura et al. 2005), Canada at Gentilly 2 NPP (Tcherner and Aziz 2009) 1, and more recently, in the United States for which the U.S. Nuclear Regulatory Commission issued Information Notice (IN) 2011-20, ’Concrete Degradation by Alkali Silica Reaction,’ on November 18, 2011, to provide the industry with information related to the ASR identified at Seabrook. Considering that US commercial reactors in operation enter the age when ASR degradation can be visually detected and that numerous non nuclear infrastructures (transportation, energy production) have already experienced ASR in a large majority of the States (e.g., Department of Transportation survey reported by Touma (Touma 2000)), the susceptibility and significance of ASR for nuclear concrete structures must be addressed in the perspective of license renewal and long-term operation beyond 60 years. The aim of this report is to perform an extensive parametric series of 3D nonlinear finite element analyses of three di erent “beam-like” geometries, including two di erent depths, three di erent types of boundary conditions, and four other parameters: namely, the ASR volumetric expansion, the reinforcement ratio, the loss of elastic modulus induced by ASR and the loss of tensile strength caused by ASR.

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.

Kinetics of silica-phase transitions

International Nuclear Information System (INIS)

Duffy, C.J.

1993-07-01

In addition to the stable silica polymorph quartz, several metastable silica phases are present in Yucca Mountain. The conversion of these phases to quartz is accompanied by volume reduction and a decrease in the aqueous silica activity, which may destabilize clinoptilolite and mordenite. The primary reaction sequence for the silica phases is from opal or glass to disordered opal-CT, followed by ordering of the opal-CT and finally by the crystallization of quartz. The ordering of opal-CT takes place in the solid state, whereas the conversion of opal-CT takes place through dissolution-reprecipitation involving the aqueous phase. It is proposed that the rate of conversion of opal-CT to quartz is controlled by diffusion of defects out of a disordered surface layer formed on the crystallizing quartz. The reaction rates are observed to be dependent on temperature, pressure, degree of supersaturation, and pH. Rate equations selected from the literature appear to be consistent with observations at Yucca Mountain

Effect of silica nanoparticles on polyurethane foaming process and foam properties

International Nuclear Information System (INIS)

Francés, A B; Bañón, M V Navarro

2014-01-01

Flexible polyurethane foams (FPUF) are commonly used as cushioning material in upholstered products made on several industrial sectors: furniture, automotive seating, bedding, etc. Polyurethane is a high molecular weight polymer based on the reaction between a hydroxyl group (polyol) and isocyanate. The density, flowability, compressive, tensile or shearing strength, the thermal and dimensional stability, combustibility, and other properties can be adjusted by the addition of several additives. Nanomaterials offer a wide range of possibilities to obtain nanocomposites with specific properties. The combination of FPUF with silica nanoparticles could develop nanocomposite materials with unique properties: improved mechanical and thermal properties, gas permeability, and fire retardancy. However, as silica particles are at least partially surface-terminated with Si-OH groups, it was suspected that the silica could interfere in the reaction of poyurethane formation.The objective of this study was to investigate the enhancement of thermal and mechanical properties of FPUF by the incorporation of different types of silica and determining the influence thereof during the foaming process. Flexible polyurethane foams with different loading mass fraction of silica nanoparticles (0-1% wt) and different types of silica (non treated and modified silica) were synthesized. PU/SiO 2 nanocomposites were characterized by FTIR spectroscopy, TGA, and measurements of apparent density, resilience and determination of compression set. Addition of silica nanoparticles influences negatively in the density and compression set of the foams. However, resilience and thermal stability of the foams are improved. Silica nanoparticles do not affect to the chemical structure of the foams although they interfere in the blowing reaction

A proposed aging management program for alkali silica reactions in a nuclear power plant

Energy Technology Data Exchange (ETDEWEB)

Saouma, Victor E., E-mail: saouma@colorado.edu; Hariri-Ardebili, Mohammad A.

2014-10-01

Drawing from publicly available information, this paper addresses the alkali silica reaction management of Seabrook nuclear power plant. The essence of the reaction is first examined, followed by a summary of findings, current and planned work. Then, the authors draw on their experience in ASR to first comment on the current work, and then complete the paper with what they would recommend. An important observation is that ASR constitutes a major challenge to the nuclear industry, and a thorough understanding of the State of the Art is essential before a holistic approach is undertaken. It is neither a simple nor an inexpensive challenge, yet a most critical one that industry and regulators must confront. This paper is only a breach into such an effort.

A proposed aging management program for alkali silica reactions in a nuclear power plant

International Nuclear Information System (INIS)

Saouma, Victor E.; Hariri-Ardebili, Mohammad A.

2014-01-01

Drawing from publicly available information, this paper addresses the alkali silica reaction management of Seabrook nuclear power plant. The essence of the reaction is first examined, followed by a summary of findings, current and planned work. Then, the authors draw on their experience in ASR to first comment on the current work, and then complete the paper with what they would recommend. An important observation is that ASR constitutes a major challenge to the nuclear industry, and a thorough understanding of the State of the Art is essential before a holistic approach is undertaken. It is neither a simple nor an inexpensive challenge, yet a most critical one that industry and regulators must confront. This paper is only a breach into such an effort

Effect of Dissolved Silica on Immobilization of Boron by Magnesium Oxide

Directory of Open Access Journals (Sweden)

Shoko Nozawa

2018-02-01

Full Text Available The effect of silica on the immobilization reaction of boron by magnesium oxide was investigated by laboratory experiments. In the absence of silica, due to dissolution of the magnesium oxide, boron was removed from solutions by the precipitation of multiple magnesium borates. In the presence of silica, magnesium silica hydrate (M-S-H was formed as a secondary mineral, which takes up boron. Here 11B magic-angle spinning nuclear magnetic resonance (MAS-NMR and Fourier transform infrared spectrometer (FT-IR data show that a part of the boron would be incorporated into M-S-H structures by isomorphic substitution of silicon. Another experiment where magnesium oxide and amorphous silica were reacted beforehand and boron was added later showed that the shorter the reaction time of the preceding reaction, the higher the sorption ratio of boron. That is, boron was incorporated into the M-S-H mainly by coprecipitation. The experiments in the study here show that the sorption of boron in the presence of silica is mainly due to the incorporation of boron during the formation of the M-S-H structure, which suggests that boron would not readily leach out, and that stable immobilization of boron can be expected.

Moessbauer spectroscopic characterisation of catalysts obtained by interaction between tetra-n-butyl-tin and silica or silica supported rhodium

International Nuclear Information System (INIS)

Millet, J.M.M.; Toyir, J.; Didillon, B.; Candy, J.P.; Nedez, C.; Basset, J.M.

1997-01-01

Moessbauer spectroscopy at 78 K was used to study the interaction between tetra-n-butyl-tin and the surfaces of silica or silica supported rhodium. At room temperature, the tetra-n-butyl-tin was physically adsorbed on the surfaces. After reaction under hydrogen at 373 K, the formation of grafted organometallic fragments on the Rh surface was confirmed whereas with pure silica, ≡SiO-Sn(n-C 4 H 9 ) 3 moieties were observed. After treatment at 523 K, the rhodium grafted organometallic species was completely decomposed and there was formation of a defined bimetallic RhSn compound

Fluorescent proteins as efficient tools for evaluating the surface PEGylation of silica nanoparticles

Science.gov (United States)

Zhang, Wei; Ma, Minyan; Zhang, Xiao-ai; Zhang, Ze-yu; Saleh, Sayed M.; Wang, Xu-dong

2017-06-01

Surface PEGylation is essential for preventing non-specific binding of biomolecules when silica nanoparticles are utilized for in vivo applications. Methods for installing poly(ethylene glycol) on a silica surface have been widely explored but varies from study to study. Because there is a lack of a satisfactory method for evaluating the properties of silica surface after PEGylation, the prepared nanoparticles are not fully characterized before use. In some cases, even non-PEGylated silica nanoparticles were produced, which is unfortunately not recognized by the end-user. In this work, a fluorescent protein was employed, which acts as a sensitive material for evaluating the surface protein adsorption properties of silica nanoparticles. Eleven different methods were systematically investigated for their reaction efficiency towards surface PEGylation. Results showed that both reaction conditions (including pH, catalyst) and surface functional groups of parent silica nanoparticles play critical roles in producing fully PEGylated silica nanoparticles. Great care needs to be taken in choosing the proper coupling chemistry for surface PEGylation. The data and method shown here will guarantee high-quality PEGylated silica nanoparticles to be produced and guide their applications in biology, chemistry, industry and medicine.

Grafting of polymer onto silica surface in the presence of γ-ray irradiated silica

International Nuclear Information System (INIS)

Tsuchida, A.; Yokoyama, R.; Takami, M.; Chen, J.; Ohta, M.; Tsubokawa, N.

2002-01-01

Complete text of publication follows. We have reported the graft polymerization of vinyl monomers initiated by surface radicals formed by the decomposition of azo and peroxide groups previously introduced onto the surface. In addition, the grafting of polymers onto carbon black has been reported by the reaction of polymer radicals with the surface. On the other hand, it is well known that the relatively stable radicals are generated on the surface by the γ-ray irradiation. In this paper, the grafting of polystyrene onto silica surface during the thermal polymerization of styrene in the presence of γ-ray irradiated silica, grafting mechanism and thermal stability of grafted polymer will be discussed. The grafting of polymers onto silica surface by irradiation of polymer-adsorbed silica was also investigated. Silica obtained from Mitsubishi Chemical Co., Japan was used after pulverization: the particle size was 0.037-0.088 mm. Irradiation was performed in Cs-137 source at room temperature. The silica was irradiated at 50 Gy with dose rate of 3.463 Gy/min. Into a polymerization tube, styrene and irradiated silica was charged and the polymerization was carried out under argon under stirring. The percentage of polystyrene grafting was determined from weight loss when polystyrene-grafted silica was heated at 600 deg C by a thermal analyzer. Untreated silica did not affect the thermal polymerization of styrene. On the contrary, the thermal polymerization of styrene was remarkably retarded in the presence of the irradiated silica at 60 deg C. Similar tendency was reported during the polymerization of vinyl monomers in the presence of carbon black. In the initial stage of the polymerization in the presence of the irradiated silica below 50 deg C, the polymerization was accelerated. During the polymerization in the presence of irradiated silica, polystyrene was grafted onto the surface: the percentage of grafting was 5-11%. The amount of polystyrene grafted onto silica

Interim solidification of SRP waste with silica, bentonite, or phosphoric acid

International Nuclear Information System (INIS)

Thompson, G.H.

1976-03-01

One option for interim waste management at the Savannah River Plant is in-tank solidification of the liquid waste solutions. This would reduce the mobility of these highly radioactive solutions until techniques for their long-term immobilization and storage are developed and implemented. Interim treatments must permit eventual retrieval of waste and subsequent incorporation into a high-integrity form. This study demonstrated the solidification of simulated alkaline waste solutions by reaction with silica, bentonite, and phosphoric acid. Alkaline waste can be solidified by reaction with silica gel, silica flour, or sodium silicate solution. Solidified products containing waste salt can be retrieved by slurrying with water. Alkaline supernate (solution in equilibrium with alkaline sludge in SRP waste tanks) can be solidified by reaction with bentonite to form cancrinite powder. The solidified waste can be retrieved by slurrying with water. Alkaline supernate can be solidified by partial evaporation and reaction with phosphoric acid. Water is incorporated into hydrated complexes of trisodium phosphate. The product is soluble, but actual plant waste would not solidify completely because of decay heat. Reaction of simulated alkaline waste solutions with silica gel, silica flour, or bentonite increases the volume by a factor of approximately 6 over that of evaporated waste; reaction with phosphoric acid results in a volume 1.5 times that of evaporated waste. At present, the best method for in-tank solidification is by evaporation, a method that contributes no additional solids to the waste and does not compromise any waste management options

Fibrous nano-silica (KCC-1)-supported palladium catalyst: Suzuki coupling reactions under sustainable conditions

KAUST Repository

Fihri, Aziz; Cha, Dong Kyu; Bouhrara, Mohamed; Al Mana, Noor; Polshettiwar, Vivek

2011-01-01

Noble amines recycled: Fibrous high-surface-area nano-silica functionalized with aminopropyl groups and loaded with well-dispersed Pd nanoparticles is evaluated for the Suzuki coupling of aromatic halides. It is active for the reaction of a range of aryl bromides and iodides as well as chlorides with aryl boronic acids in good to excellent yields. The catalyst can be recovered and reused for a number of cycles with negligible loss in activity. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fibrous nano-silica (KCC-1)-supported palladium catalyst: Suzuki coupling reactions under sustainable conditions

KAUST Repository

Fihri, Aziz

2011-11-15

Noble amines recycled: Fibrous high-surface-area nano-silica functionalized with aminopropyl groups and loaded with well-dispersed Pd nanoparticles is evaluated for the Suzuki coupling of aromatic halides. It is active for the reaction of a range of aryl bromides and iodides as well as chlorides with aryl boronic acids in good to excellent yields. The catalyst can be recovered and reused for a number of cycles with negligible loss in activity. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Pd-bound functionalized mesoporous silica as active catalyst for Suzuki coupling reaction: Effect of OAcˉ, PPh3 and Clˉ ligands on catalytic activity

Science.gov (United States)

Das, Trisha; Uyama, Hiroshi; Nandi, Mahasweta

2018-04-01

Three new palladium catalysts, PdCat-I, PdCat-II and PdCat-III, immobilized over heterogeneous silica support have been synthesized using different ligands attached to the palladium precursor. The ligands that have been used in this study are acetate, triphenylphosphine and chloride in PdCat-I, PdCat-II and PdCat-III, respectively. The ligands have different effect on stability of the compounds and impart different oxidation states to the metal center. The materials have been characterized by powder X-ray diffraction, nitrogen adsorption-desorption studies, transmission electron microscopy, thermal analysis, and different spectroscopic techniques. The Pd-content of the samples have been determined by ICP-AES analysis. The materials have been used as catalysts for Suzuki coupling reaction of aryl halides with phenylboronic acid under mild conditions. A comparative study has been carried out to ascertain the effect of the nature of different ligands on the outcome of the catalytic reactions. Products have been identified and estimated by 1H NMR and gas chromatography. The results show that the best yields are obtained with the catalyst containing triphenylphosphine as the ligand in methanol. Such type of work to study the effect of ligand on Suzuki coupling reaction over functionalized mesoporous silica heterogeneous catalysts have not been carried out so far.

Thermogravimetric study on the hydration of reactive magnesia and silica mixture at room temperature

International Nuclear Information System (INIS)

Jin, Fei; Al-Tabbaa, Abir

2013-01-01

Highlights: • The characteristics of reactive MgO vary significantly in terms of their impurity content and reactivity depending on their sources and calcination conditions. • The synthesis of magnesium silicate hydrate (MSH) is affected by the characteristics of the precursors, i.e., MgO and silica. • The reaction process in the MgO–SiO 2 –H 2 O system can be followed by TGA, and is essential to develop MSH-based materials. - Abstract: The synthesis of magnesium silicate hydrate (MSH), which has wide applications in both construction and environmental fields, has been studied for decades. However, it is known that the characteristics of magnesia (MgO) vary significantly depending on their calcination conditions, which is expected to affect their performance in the MgO–SiO 2 –H 2 O system. This paper investigated the effect of different MgO and silica sources on the formation of magnesium silicate hydrate (MSH) at room temperature. The hydration process was studied by mixing commercial reactive MgO and silica powders with water and curing for 1, 7 and 28 days. The hydration products were analysed with the help of X-ray diffraction (XRD) and thermogravimatric analysis (TGA). The results showed the continuous consumption of MgO and the existence of MSH and brucite and other minor phases such as magnesite and calcite. It is found that the Mg and Si sources have significant effect on the hydration process of MgO–SiO 2 –H 2 O system. The reaction degree is controlled by the availability of dissolved Mg and Si in the solution. The former is determined by the reactivity of MgO and the latter is related to the reactivity of the silica as well as the pH of the system

Monitoring, Modeling, and Diagnosis of Alkali-Silica Reaction in Small Concrete Samples

Energy Technology Data Exchange (ETDEWEB)

Agarwal, Vivek [Idaho National Lab. (INL), Idaho Falls, ID (United States); Cai, Guowei [Idaho National Lab. (INL), Idaho Falls, ID (United States); Gribok, Andrei V. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Mahadevan, Sankaran [Idaho National Lab. (INL), Idaho Falls, ID (United States)

2015-09-01

Assessment and management of aging concrete structures in nuclear power plants require a more systematic approach than simple reliance on existing code margins of safety. Structural health monitoring of concrete structures aims to understand the current health condition of a structure based on heterogeneous measurements to produce high-confidence actionable information regarding structural integrity that supports operational and maintenance decisions. This report describes alkali-silica reaction (ASR) degradation mechanisms and factors influencing the ASR. A fully coupled thermo-hydro-mechanical-chemical model developed by Saouma and Perotti by taking into consideration the effects of stress on the reaction kinetics and anisotropic volumetric expansion is presented in this report. This model is implemented in the GRIZZLY code based on the Multiphysics Object Oriented Simulation Environment. The implemented model in the GRIZZLY code is randomly used to initiate ASR in a 2D and 3D lattice to study the percolation aspects of concrete. The percolation aspects help determine the transport properties of the material and therefore the durability and service life of concrete. This report summarizes the effort to develop small-size concrete samples with embedded glass to mimic ASR. The concrete samples were treated in water and sodium hydroxide solution at elevated temperature to study how ingress of sodium ions and hydroxide ions at elevated temperature impacts concrete samples embedded with glass. Thermal camera was used to monitor the changes in the concrete sample and results are summarized.

Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

International Nuclear Information System (INIS)

Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A.

2013-01-01

In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na 2 SiO 3 ) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO 2 molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO 2 molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

Energy Technology Data Exchange (ETDEWEB)

Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A., E-mail: ivan_melendez380@hotmail.com [Centro de Investigacion en Quimica Aplicada, Bldv. Enrique Reyna Hermosillo No. 140, Saltillo 25294, Coahuila (Mexico)

2013-08-01

In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na{sub 2}SiO{sub 3}) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO{sub 2} molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO{sub 2} molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

Assessment of concrete bridge decks with alkali silica reactions

DEFF Research Database (Denmark)

Eriksen, Kirsten; Jansson, Jacob; Geiker, Mette Rica

2008-01-01

Based on investigations of concrete from an approximately 40 years old bridge a procedure to support the management of maintenance and repair of alkali silica damaged bridges is proposed. Combined petrography and accelerated expansion testing were undertaken on cores from the Bridge at Skovdiget......, Bagsværd, Denmark to provide information on the damage condition as well as the residual reactivity of the concrete. The Danish Road Directory’s guidelines for inspection and assessment of alkali silica damaged bridges will be briefly presented, and proposed modifications will be describe...

Study on the influence of Alkali-Silica reaction on structural behavior of reinforced concrete members

International Nuclear Information System (INIS)

Murazumi, Y.; Watanabe, Y.; Matsumoto, N.; Mitsugi, S.; Takiguchi, K.; Masuda, Y.

2005-01-01

Expansion produced by alkali-silica reaction (ASR) has been observed in the turbine generator foundation of the unit 1, Ikata nuclear power station, Japan. The foundation is a reinforced concrete frame structure. This paper, as a part of the series of investigation and experiments, discusses tests on structural behavior of concrete members affected by ASR. The purpose of the study is to obtain experimental results on the effects of ASR on bending and shear behavior of reinforced concrete beams and shear walls, and compare with the calculated results by present evaluation methods for normal concrete structures For the experiments on bending/shear behavior of beam, bending test models with a small amount of rebar and shear test models with larger amount were made of concrete in which ASR was induced by adding alkali or concrete without ASR. It was found from the results that bending strength of the bending test models and shear strength of the shear test models did not fall, nor was it lower than the calculated strength for concrete members without ASR. In the shear wall test, the two test models were made of either concrete with ASR or one without it. Horizontal load was applied with actuators on the test model fixed on the test floor, while vertical load was applied with oil jacks. The results did not indicate that ASR lowered the stiffness or strength of the wall test models, showing the strength was able to be calculated with the same formula for reinforced concrete wall without ASR. (authors)

SOMC-Designed Silica Supported Tungsten Oxo Imidazolin-2-iminato Methyl Precatalyst for Olefin Metathesis Reactions

KAUST Repository

Qureshi, Ziyauddin

2017-01-05

Synthesis, structure, and olefin metathesis activity of a surface complex [(≡Si-O-)W(═O)(CH3)2-ImDippN] (4) (ImDipp = 1,3-bis(2,6-diisopropylphenyl)imidazolin-2-iminato) supported on silica by a surface organometallic chemistry (SOMC) approach are reported. The reaction of N-silylated 2-iminoimidazoline with tungsten(VI) oxytetrachloride generated the tungsten oxo imidazolin-2-iminato chloride complex [ImDippNW(═O)Cl3] (2). This was grafted on partially dehydroxylated silica pretreated at 700 °C (SiO2-700) to afford a well-defined monopodal surface complex [(≡Si-O-)W(═O)Cl2-ImDippN] (3). 3 underwent alkylation by ZnMe2 to produce [(≡Si-O-)W(═O)(CH3)2-ImDippN] (4). The alkylated surface complex was thoroughly characterized by solid-state NMR, elemental microanalysis, Raman, FT-IR spectroscopies, and XAS analysis. 4 proved to be an active precatalyst for self-metathesis of terminal olefins such as propylene and 1-hexene.

SOMC-Designed Silica Supported Tungsten Oxo Imidazolin-2-iminato Methyl Precatalyst for Olefin Metathesis Reactions

KAUST Repository

Qureshi, Ziyauddin; Hamieh, Ali Imad Ali; Barman, Samir; Maity, Niladri; Samantaray, Manoja; Ould-Chikh, Samy; Abou-Hamad, Edy; Falivene, Laura; D’ Elia, Valerio; Rothenberger, Alexander; Llorens, Isabelle; Hazemann, Jean-Louis; Basset, Jean-Marie

2017-01-01

Synthesis, structure, and olefin metathesis activity of a surface complex [(≡Si-O-)W(═O)(CH3)2-ImDippN] (4) (ImDipp = 1,3-bis(2,6-diisopropylphenyl)imidazolin-2-iminato) supported on silica by a surface organometallic chemistry (SOMC) approach are reported. The reaction of N-silylated 2-iminoimidazoline with tungsten(VI) oxytetrachloride generated the tungsten oxo imidazolin-2-iminato chloride complex [ImDippNW(═O)Cl3] (2). This was grafted on partially dehydroxylated silica pretreated at 700 °C (SiO2-700) to afford a well-defined monopodal surface complex [(≡Si-O-)W(═O)Cl2-ImDippN] (3). 3 underwent alkylation by ZnMe2 to produce [(≡Si-O-)W(═O)(CH3)2-ImDippN] (4). The alkylated surface complex was thoroughly characterized by solid-state NMR, elemental microanalysis, Raman, FT-IR spectroscopies, and XAS analysis. 4 proved to be an active precatalyst for self-metathesis of terminal olefins such as propylene and 1-hexene.

The study of diffusion mechanism in network-forming liquid: Silica liquid

Directory of Open Access Journals (Sweden)

P. K. Hung

2016-12-01

Full Text Available Molecular dynamics simulation is employed to investigate the diffusion mechanism in silica melt, a typical network-forming liquid. From the analysis of SiOx→SiOx±1 and OSiy→OSiy±1 reactions we reveal two moving modes: fast hopping and slow collective moving. Accordingly the atoms diffuse in the melt by simple hopping or through displacing of super-molecule (SM. A cluster analysis is performed for several of atom sets. It is shown that the melt exhibits non-uniform spatial distribution of reaction which causes the dynamics heterogeneity (DH. Further, the network structure of the melt consists of main subnet and large defective subnets. These subnets differ strongly in local environment, chemical composition and atomic density. This result evidences two distinct phases, the structure heterogeneity in silica melt and supports the polymorphism of network-forming liquid. We also find out that the node transformation spreads non-uniformly through the network structure. It takes place mainly in large defective subnet. The strong localization of node transformation is responsible for dynamical slowdown.

Effect of silica fume on reaction products of uranium (VI) with portland cement

International Nuclear Information System (INIS)

Tan Hongbin; Shaanxi Univ. of Technology, Hanzhong; Li Yuxiang

2005-01-01

Simulation of radioactive waste of U(VI) by uranyl nitrate and the effects of different additive quantities (12%, 20%, 30%, 35%, 40%) of silica fume on the products of U(VI) with Portland cement were studied at a hydrothermal condition of 180 degree C for a duration of one week. The X-ray powder diffraction examination results showed that the calcium uranate would be transformed into uranophane when the cement contained 30% silica fume. (authors)

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.

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

International Nuclear Information System (INIS)

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

2017-01-01

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

Clean Chlorination of Silica Surfaces by a Single-site Substitution Approach

KAUST Repository

Maity, Niladri; Barman, Samir; Abou-Hamad, Edy; D'Elia, Valerio; Basset, Jean-Marie

2018-01-01

A chlorination method for the selective substitution of well-defined isolated silanol groups of the silica surface has been developed using the catalytic Appel reaction. Spectroscopic analysis, complemented by elemental microanalysis studies, reveals that a quantitative chlorination could be achieved with highly dehydroxylated silica materials that exclusively possess non-hydrogen bonded silanol groups. The employed method did not leave any carbon or phosphorous residue on the silica surface and can be regarded as a promising tool for the future functionalization of metal oxide surfaces.

Clean Chlorination of Silica Surfaces by a Single-site Substitution Approach

KAUST Repository

Maity, Niladri

2018-02-12

A chlorination method for the selective substitution of well-defined isolated silanol groups of the silica surface has been developed using the catalytic Appel reaction. Spectroscopic analysis, complemented by elemental microanalysis studies, reveals that a quantitative chlorination could be achieved with highly dehydroxylated silica materials that exclusively possess non-hydrogen bonded silanol groups. The employed method did not leave any carbon or phosphorous residue on the silica surface and can be regarded as a promising tool for the future functionalization of metal oxide surfaces.

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)

Investigation of safety margin for turbine generator foundation affected by Alkali Silica reaction based on non-linear structure analysis

International Nuclear Information System (INIS)

Shimizu, H.; Asai, Y.; Hosokawa, T.; Sekimoto, H.; Sato, K.; Oshima, R.; Takiguchi, K.; Masuda, Y.; Nishiguchi, I.

2005-01-01

A turbine generator foundation is a reinforced concrete structure having a table deck and columns to support equipments. After operation of the plant, the expansion of the table deck in turbine longitudinal axis has been observed. By investigation of concrete material properties, it was found that the expansion has been caused by alkali-silica reaction. This study has been performed to evaluate the safety allowance of strength capacity of the turbine generator foundation by nonlinear analysis using beam element model with elongation, rebar strain and material properties data which have been measured for almost 30 years in actual foundation. (authors)

Functionalized mesoporous silica materials for molsidomine adsorption: Thermodynamic study

International Nuclear Information System (INIS)

Alyoshina, Nonna A.; Parfenyuk, Elena V.

2013-01-01

A series of unmodified and organically modified mesoporous silica materials was prepared. The unmodified mesoporous silica was synthesized via sol–gel synthesis in the presence of D-glucose as pore-forming agent. The functionalized by phenyl, aminopropyl and mercaptopropyl groups silica materials were prepared via grafting. The fabricated adsorbent materials were characterized by Fourier transform infrared spectroscopy (FTIR) analysis, N 2 adsorption/desorption and elemental analysis methods. Then their adsorption properties for mesoionic dug molsidomine were investigated at 290–313 K and physiological pH value. Thermodynamic parameters of molsidomine adsorption on the synthesized materials have been calculated. The obtained results showed that the adsorption process of molsidomine on the phenyl modified silica is the most quantitatively and energetically favorable. The unmodified and mercaptopropyl modified silica materials exhibit significantly higher adsorption capacities and energies for molsidomine than the aminopropyl modified sample. The effects are discussed from the viewpoint of nature of specific interactions responsible for the adsorption. - Graphical abstract: Comparative analysis of the thermodynamic characteristics of molsidomine adsorption showed that the adsorption process on mesoporous silica materials is controlled by chemical nature of surface functional groups. Molsidomine adsorption on the phenyl modified silica is the most quantitatively and energetically favorable. Taking into account ambiguous nature of mesoionic compounds, it was found that molsidomine is rather aromatic than dipolar. Display Omitted - Highlights: • Unmodified and organically modified mesoporous silica materials were prepared. • Molsidomine adsorption on the silica materials was studied. • Phenyl modified silica shows the highest adsorption capacity and favorable energy. • Molsidomine exhibits the lowest affinity to aminopropyl modified silica

Viability for controlling long-term leaching of radionuclides from HLW glass by amorphous silica additives

International Nuclear Information System (INIS)

Inagaki, Y.; Uehara, S.

2004-01-01

Dissolution and deterioration experiments in coexistence system of amorphous silica and vitrified wastes have been executed in order to evaluating the effects of amorphous silica addition to high level radioactive vitrified waste (HLW glass) on suppression of nuclide leaching. Geo-chemical reaction mechanism among the vitrified waste, the amorphous silica and water was also evaluated. Dissolution of the silica network was suppressed by addition of the amorphous silica. However, the leaching of soluble nuclides like B proceeded depending on the hydration deterioration reaction. (A. Hishinuma)

Amorphous silica in ultra-high performance concrete: First hour of hydration

Energy Technology Data Exchange (ETDEWEB)

Oertel, Tina, E-mail: tina.oertel@isc.fraunhofer.de [Fraunhofer-Institute for Silicate Research ISC, Neunerplatz 2, 97082 Würzburg (Germany); Chair for Inorganic Chemistry I, Universität Bayreuth, Universitätsstr. 30, 95440 Bayreuth (Germany); Hutter, Frank [Fraunhofer-Institute for Silicate Research ISC, Neunerplatz 2, 97082 Würzburg (Germany); Helbig, Uta, E-mail: uta.helbig@th-nuernberg.de [Chair for Crystallography and X-ray Methods, Technische Hochschule Nürnberg Georg Simon Ohm, Wassertorstraße 10, 90489 Nürnberg (Germany); Sextl, Gerhard [Fraunhofer-Institute for Silicate Research ISC, Neunerplatz 2, 97082 Würzburg (Germany); Chair for Chemical Technology of Advanced Materials, Julius Maximilian Universität, Röntgenring 11, 97070 Würzburg (Germany)

2014-04-01

Amorphous silica in the sub-micrometer size range is widely used to accelerate cement hydration. Investigations including properties of silica which differ from the specific surface area are rare. In this study, the reactivity of varying types of silica was evaluated based on their specific surface area, surface silanol group density, content of silanol groups and solubility in an alkaline suspension. Pyrogenic silica, silica fume and silica synthesized by hydrolysis and condensation of alkoxy silanes, so-called Stoeber particles, were employed. Influences of the silica within the first hour were further examined in pastes with water/cement ratios of 0.23 using in-situ X-ray diffraction, cryo scanning electron microscopy and pore solution analysis. It was shown that Stoeber particles change the composition of the pore solution. Na{sup +}, K{sup +}, Ca{sup 2+} and silicate ions seem to react to oligomers. The extent of this reaction might be highest for Stoeber particles due to their high reactivity.

Prestressing of reinforcing bars in concrete slabs due to concrete expansion induced by Alkali-Silica Reaction

DEFF Research Database (Denmark)

Gustenhoff Hansen, Søren; Antonio Barbosa, Ricardo; Hoang, Linh Cao

2017-01-01

Alkali-silica reactions (ASR) in concrete bridges have been a major concern worldwide for many decades. In Denmark, several bridges are severely damaged due to ASR and over 600 bridges have the potential to develop ASR in the future. The majority of these bridges are slab-bridges. Despite the many...... cases, experimental research on structural safety and residual load carrying capacity of ASR-damaged bridges is limited. As ASR causes severe cracks in the concrete, which may affect the concrete compressive and tensile strength, concerns have been directed towards the residual shear capacity. Yet...

Functionalized mesoporous silica materials for molsidomine adsorption: Thermodynamic study

Energy Technology Data Exchange (ETDEWEB)

Alyoshina, Nonna A.; Parfenyuk, Elena V., E-mail: evp@iscras.ru

2013-09-15

A series of unmodified and organically modified mesoporous silica materials was prepared. The unmodified mesoporous silica was synthesized via sol–gel synthesis in the presence of D-glucose as pore-forming agent. The functionalized by phenyl, aminopropyl and mercaptopropyl groups silica materials were prepared via grafting. The fabricated adsorbent materials were characterized by Fourier transform infrared spectroscopy (FTIR) analysis, N{sub 2} adsorption/desorption and elemental analysis methods. Then their adsorption properties for mesoionic dug molsidomine were investigated at 290–313 K and physiological pH value. Thermodynamic parameters of molsidomine adsorption on the synthesized materials have been calculated. The obtained results showed that the adsorption process of molsidomine on the phenyl modified silica is the most quantitatively and energetically favorable. The unmodified and mercaptopropyl modified silica materials exhibit significantly higher adsorption capacities and energies for molsidomine than the aminopropyl modified sample. The effects are discussed from the viewpoint of nature of specific interactions responsible for the adsorption. - Graphical abstract: Comparative analysis of the thermodynamic characteristics of molsidomine adsorption showed that the adsorption process on mesoporous silica materials is controlled by chemical nature of surface functional groups. Molsidomine adsorption on the phenyl modified silica is the most quantitatively and energetically favorable. Taking into account ambiguous nature of mesoionic compounds, it was found that molsidomine is rather aromatic than dipolar. Display Omitted - Highlights: • Unmodified and organically modified mesoporous silica materials were prepared. • Molsidomine adsorption on the silica materials was studied. • Phenyl modified silica shows the highest adsorption capacity and favorable energy. • Molsidomine exhibits the lowest affinity to aminopropyl modified silica.

Characterization and Curing Kinetics of Epoxy/Silica Nano-Hybrids

Science.gov (United States)

Yang, Cheng-Fu; Wang, Li-Fen; Wu, Song-Mao; Su, Chean-Cheng

2015-01-01

The sol-gel technique was used to prepare epoxy/silica nano-hybrids. The thermal characteristics, curing kinetics and structure of epoxy/silica nano-hybrids were studied using differential scanning calorimetry (DSC), 29Si nuclear magnetic resonance (NMR) and transmission electron microscopy (TEM). To improve the compatibility between the organic and inorganic phases, a coupling agent was used to modify the diglycidyl ether of bisphenol A (DGEBA) epoxy. The sol-gel technique enables the silica to be successfully incorporated into the network of the hybrids, increasing the thermal stability and improving the mechanical properties of the prepared epoxy/silica nano-hybrids. An autocatalytic mechanism of the epoxy/SiO2 nanocomposites was observed. The low reaction rate of epoxy in the nanocomposites is caused by the steric hindrance in the network of hybrids that arises from the consuming of epoxide group in the network of hybrids by the silica. In the nanocomposites, the nano-scale silica particles had an average size of approximately 35 nm, and the particles were well dispersed in the epoxy matrix, according to the TEM images. PMID:28793616

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.

Study of radon transport through concrete modified with silica fume

International Nuclear Information System (INIS)

Chauhan, R.P.; Kumar, Amit

2013-01-01

The concentration of radon in soil usually varies between a few kBq/m 3 and tens or hundreds of kBq/m 3 depending upon the geographical region. This causes the transport of radon from the soil to indoor environments by diffusion and advection through the pore space of concrete. To reduce indoor radon levels, the use of concrete with low porosity and a low radon diffusion coefficient is recommended. A method of reducing the radon diffusion coefficient through concrete and hence the indoor radon concentration by using silica fume to replace an optimum level of cement was studied. The diffusion coefficient of the concrete was reduced from (1.63 ± 0.3) × 10 −7 to (0.65 ± 0.01) × 10 −8 m 2 /s using 30% substitution of cement with silica fume. The compressive strength of the concrete increased as the silica-fume content increased, while radon exhalation rate and porosity of the concrete decreased. This study suggests a cost-effective method of reducing indoor radon levels. -- Highlights: • Radon diffusion study through silica fume modified concrete was carried out. • Radon diffusion coefficient of concrete decreased with increase of silica fume contents. • Compressive strength increased with increase of silica fume. • Radon exhalation rates and porosity of samples decreased with addition of silica fume. • Radon diffusion coefficient decreased to 2.6% by 30% silica fume substitution

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)

The chemistry of the carbothermal synthesis of β-SiC : reaction mechanism, reaction rate and grain growth

NARCIS (Netherlands)

van Dijen, F.K.; Metselaar, R.

1991-01-01

Evidence is given that in the present case the reaction mechanism of ß-SiC formation from silica and carbon is a direct solid-state reaction in which silica migrates over the silicon carbide surface to the carbon. A high value (440 kJ/mol) of activation energy is obtained for this reaction. This

In situ polymerization of L-Lactide in the presence of fumed silica

International Nuclear Information System (INIS)

Prebe, A.; Alcouffe, P.; Cassagnau, Ph.; Gerard, J.F.

2010-01-01

Chemiorheology, i.e. rheological changes during the polymerization, of a biosourced monomer, i.e. L-Lactide, containing fumed silica have been studied. For that purpose, the reaction was proceeded in situ between the plates of a dynamic rheometer. The polymerization kinetics was followed from the variation of the complex shear modulus versus reaction time. Moreover, at temperatures lower than the crystallization temperature, it was possible to follow the crystallization process while the polymerization takes place. Adding fumed silica particles into the monomer leads to the formation of a physical (percolated) network from particle-particle interactions, i.e. silica, in the L-Lactide probably hydrophilic interactions. The gel-like structure was kept while the polymerization as long as the strain remains low indicating that the silica particle network remains weak. Furthermore, the mechanism of the break down of the gel structure under large deformation as well as the recovery was discussed. It seems that the non-linearity effect of the nanocomposites stems in the silica inter-particle interactions. It was found that silica particles do not have any effect on the temperature of crystallization - molar mass relation but could act as nucleating agent. In situ polymerization of L-Lactide in the presence of 5 wt.% of modified fumed silica was carried out in a reactor. It was found that fumed hydrophilic silica leaded to a microcomposite with highly dense agglomerates in the polymer matrix whereas with a less hydrophilic silica it was possible to decrease the size of the agglomerates increasing the dispersion. The finest dispersion state was achieved with the 'initiating' functionalized silica leading to a 'grafting from' polymerization of the L-Lactide. Such functionalized silica leads to a nanoscale dispersion in a one-step bulk polymerization with only a few small agglomerates.

In situ polymerization of L-Lactide in the presence of fumed silica

Energy Technology Data Exchange (ETDEWEB)

Prebe, A. [Universite de Lyon, F-69361, Lyon (France); CNRS, UMR 5223, Ingenierie des Materiaux Polymeres, F-69622, Villeurbanne (France); Universite Claude Bernard Lyon 1, F-69622, Villeurbanne (France); INSA Lyon, F-69621, Villeurbanne (France); Alcouffe, P. [Universite de Lyon, F-69361, Lyon (France); CNRS, UMR 5223, Ingenierie des Materiaux Polymeres, F-69622, Villeurbanne (France); Universite Claude Bernard Lyon 1, F-69622, Villeurbanne (France); Cassagnau, Ph., E-mail: philippe.cassagnau@univ-lyon1.fr [Universite de Lyon, F-69361, Lyon (France); CNRS, UMR 5223, Ingenierie des Materiaux Polymeres, F-69622, Villeurbanne (France); Universite Claude Bernard Lyon 1, F-69622, Villeurbanne (France); Gerard, J.F. [Universite de Lyon, F-69361, Lyon (France); CNRS, UMR 5223, Ingenierie des Materiaux Polymeres, F-69622, Villeurbanne (France); INSA Lyon, F-69621, Villeurbanne (France)

2010-11-01

Chemiorheology, i.e. rheological changes during the polymerization, of a biosourced monomer, i.e. L-Lactide, containing fumed silica have been studied. For that purpose, the reaction was proceeded in situ between the plates of a dynamic rheometer. The polymerization kinetics was followed from the variation of the complex shear modulus versus reaction time. Moreover, at temperatures lower than the crystallization temperature, it was possible to follow the crystallization process while the polymerization takes place. Adding fumed silica particles into the monomer leads to the formation of a physical (percolated) network from particle-particle interactions, i.e. silica, in the L-Lactide probably hydrophilic interactions. The gel-like structure was kept while the polymerization as long as the strain remains low indicating that the silica particle network remains weak. Furthermore, the mechanism of the break down of the gel structure under large deformation as well as the recovery was discussed. It seems that the non-linearity effect of the nanocomposites stems in the silica inter-particle interactions. It was found that silica particles do not have any effect on the temperature of crystallization - molar mass relation but could act as nucleating agent. In situ polymerization of L-Lactide in the presence of 5 wt.% of modified fumed silica was carried out in a reactor. It was found that fumed hydrophilic silica leaded to a microcomposite with highly dense agglomerates in the polymer matrix whereas with a less hydrophilic silica it was possible to decrease the size of the agglomerates increasing the dispersion. The finest dispersion state was achieved with the 'initiating' functionalized silica leading to a 'grafting from' polymerization of the L-Lactide. Such functionalized silica leads to a nanoscale dispersion in a one-step bulk polymerization with only a few small agglomerates.

Surface modification of silica nanoparticles by UV-induced graft polymerization of methyl methacrylate.

Science.gov (United States)

Kim, Sooyeon; Kim, Eunhye; Kim, Sungsoo; Kim, Woosik

2005-12-01

In this study we modified the surface of silica nanoparticles with methyl methacrylate by UV-induced graft polymerization. It is a surface-initiated polymerization reaction induced by ultraviolet irradiation. The resulting organic-inorganic nanocomposites were near-monodisperse and fabricated without homopolymerization of the monomer. Substantial increase in mean particle size was observed by SEM image analysis after UV-induced grafting of methyl methacrylate onto pure silica particles. FT-Raman spectroscopy and X-ray photoelectron spectroscopy studies of these materials revealed the successful grafting of methyl methacrylate onto the silica surface. The formation of a covalent bond between the grafted PMMA chains and silica surface was indicated by FT-Raman spectra. Thermogravimetric analysis of the PMMA-grafted silica particles indicated the polymer contents in good agreement with SEM photographs.

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.

Influence of alkali-silica reaction on the physical, mechanical, and structural behaviour of reinforced concrete

DEFF Research Database (Denmark)

Barbosa, Ricardo Antonio

Alkali-silica reaction (ASR) is one of the major concrete deterioration mechanisms in the world. Cracking in concrete structures due to ASR has been observed worldwide. In Denmark numerous concrete structures have been built with a critical amount of ASR-reactive aggregate, mostly as porous opaline...... and porous calcareous opaline flint in the fine aggregate fraction. During the last few decades, an increasing number of bridges in Denmark have been severely damaged due to ASR. In the most severe cases, the ASR-damaged bridges have been demolished and reconstructed due to uncertainty about their residual...... following features in common: (a) significant amount of ASR cracks were observed on and inside the slabs, (b) the ASR cracks were oriented parallel to the plane of the slabs, and (c) ASR occurred in the fine aggregate fraction. In this PhD study, both the compressive strength and tensile strength of drilled...

Synthesis and characterization of titanium oxide supported silica materials

Science.gov (United States)

Schrijnemakers, Koen

2002-01-01

Titania-silica materials are interesting materials for use in catalysis, both as a catalyst support as well as a catalyst itself. Titania-silica materials combine the excellent support and photocatalytic properties of titania with the high thermal and mechanical stability of silica. Moreover, the interaction of titania with silica leads to new active sites, such as acid and redox sites, that are not found on the single oxides. In this Ph.D. two recently developed deposition methods were studied and evaluated for their use to create titanium oxide supported silica materials, the Chemical Surface Coating (CSC) and the Molecular Designed Dispersion (MDD). These methods were applied to two structurally different silica supports, an amorphous silica gel and the highly ordered MCM-48. Both methods are based on the specific interaction between a titanium source and the functional groups on the silica surface. With the CSC method high amounts of titanium can be obtained. However, clustering of the titania phase is observed in most cases. The MDD method allows much lower titanium amounts to be deposited without the formation of crystallites. Only at the highest Ti loading very small crystallites are formed after calcination. MCM-48 and silica gel are both pure SiO2 materials and therefore chemically similar to each other. However, they possess a different morphology and are synthesized in a different way. As such, some authors have reported that the MCM-48 surface would be more reactive than the surface of silica gel. In our experiments however no differences could be observed that confirmed this hypothesis. In the CSC method, the same reactions were observed and similar amounts of Ti and Cl were deposited. In the case of the MDD method, no difference in the reaction mechanism was observed. However, due to the lower thermal and hydrothermal stability of the MCM-48 structure compared to silica gel, partial incorporation of Ti atoms in the pore walls of MCM-48 took place

Studies on the Potential of Waste Soda Lime Silica Glass in Glass Ionomer Cement Production

Directory of Open Access Journals (Sweden)

V. W. Francis Thoo

2013-01-01

Full Text Available Glass ionomer cements (GIC are produced through acid base reaction between calcium-fluoroaluminosilicate glass powder and polyacrylic acid (PAA. Soda lime silica glasses (SLS, mainly composed of silica (SiO2, have been utilized in this study as the source of SiO2 for synthesis of Ca-fluoroaluminosilicate glass. Therefore, the main objective of this study was to investigate the potential of SLS waste glass in producing GIC. Two glasses, GWX 1 (analytical grade SiO2 and GWX 2 (replacing SiO2 with waste SLS, were synthesized and then characterized using X-ray diffraction (XRD and energy dispersive X-ray (EDX. Synthesized glasses were then used to produce GIC, in which the properties were characterized using Fourier transform infrared spectroscopy (FT-IR and compressive test (from 1 to 28 days. XRD results showed that amorphous glass was produced by using SLS waste glass (GWX 2, which is similar to glass produced using analytical grade SiO2 (GWX 1. Results from FT-IR showed that the setting reaction of GWX 2 cements is slower compared to cement GWX 1. Compressive strengths for GWX 1 cements reached up to 76 MPa at 28 days, whereas GWX 2 cements showed a slightly higher value, which is 80 MPa.

Radiation enhances silica translocation to the pulmonary interstitium and increases fibrosis in mice

International Nuclear Information System (INIS)

Adamson, I.Y.R.

1992-01-01

The effects of whole body irradiation (WBR) on particle clearance and the development of pulmonary fibrosis have been investigated. Using carbon, clearance is accomplished by polymorphonuclear leukocytes (PMN) and alveolar macrophages (AM), and only a few particles reach the interstitum. However, in preirradiated mice, the usual eflux of inflammatory cells is much delayed so that more free carbon remains in the alveoli, and by 1 week, many particles cross the epithelium to be phagocytized by interstitial macrophages. Carbon is found in the peribronchiolar interstitium 6 months later with no evidence of fibrosis. In the present study, mice received 1 mg silica intratracheally 2 days after 6.5 Gy WBR when the white blood cell count was low. A much-reduced Am and PMN response was found in the following 2 weeks compared to the reaction to silica alone, and many silica particles reached interstitial macrophages. In this case, macrophage activation by silica was associated with fibroblast proliferation, and by 16 weeks, much more pulmonary fibrosis was produced than after silica or irradiation only. This was measured biochemically and correlated with a large increase in retained silica in the irradiation-silica group. The results indicate that radiation inhibits the inflammatory response to particle instillation, resulting in greater translocation of free particles to the pulmonary interstitium. In the case of silica, the greater, prolonged interaction with interstitial macrophages leads to a much exaggerated fibrotic reaction. 17 refs., 11 figs

Potential of sub- and supercritical CO_2 reaction media for sol-gel deposition of silica-based molecular sieve membranes

International Nuclear Information System (INIS)

Durand, Veronique; Duchateau, Maxime; Drobek, Martin; Julbe, Anne; Hertz, Audrey; Ruiz, Jean-Christophe; Sarrade, Stephane

2014-01-01

A new eco-friendly method recently developed in our group has been further investigated for the preparation of gas selective silica-based molecular sieve membranes on/in macroporous tubular ceramic supports without any intermediate layer. The synthesis protocol under sub- and supercritical conditions was based on an 'On-Stream Supercritical Fluid Deposition method' (OS-SFD) applying supercritical carbon dioxide (scCO_2) as an attractive 'green' solvent with easily adjustable properties enabling a controlled solubilisation/reaction of precursors and their transport to the ceramic support. Parameters influencing the final membrane characteristics such as permeates flow rate, calcination treatment and deposition steps have been examined for a selected reaction mixture, transmembrane pressure and defined deposition temperatures. On-line monitoring of the membrane formation process (deposition signature curve) was used in this process. Membrane characteristics are discussed in correlation with their gas permeation properties. The optimized crack-free silica membranes prepared at 50 C have a compact microstructure but a thermal stability limited to 400 C. A second deposition run allowed a recovery of the molecular sieving behaviour with a thermally activated transport for He up to 350 C. These promising results demonstrate the potential of this novel method for the preparation of uniform molecular sieve membranes deposited directly on macroporous supports with virtually zero waste. (authors)

11C-radioisotope study of methanol co-reaction with ethanol over Ni-MCM-41 silica-alumina and Ni-alumina

International Nuclear Information System (INIS)

Sarkadi-Priboczki, E.; Kovacs, Z.; Tsoncheva, T.; Kumar, N.; Murzin, D.Yu.

2009-01-01

Complete text of publication follows. The Ni modifies the properties of acidic alumina and light acidic MCM-41 silica-alumina supports. The radioisotopic method is a suitable tool for distinction of the 11 Cradioisotopic methanol and its co-derivates from derivates of non-radioactive ethanol on these catalysts. Experimental. The Ni/A l 2O 3 (5 wt % Ni) is commercially available while H-MCMN-41 (Si/Al=20) and Ni-ion-exchanged MCM-41 silica-alumina (5 wt % Ni) were prepared and characterized in previous works. Before catalysis the Ni/Al 2 O 3 and Ni-MCM-41 were pre-reduced. The 11 C-methanol was formed by a radiochemical process from 11 C-carbon dioxide produced at cyclotron (T 1/2 = 20.4 min). The mixture of equivalent volume of radioactive methanol and non-radioactive ethanol was introduced into glass tube micro-flow reactor at ambient temperature. After adsorption, the valves were closed and the catalyst was heated up to the required temperatures. The desorption rate of the remaining 11 C-derivatives on catalysts were continuously followed by radiodetectors and the derivatives of methanol with ethanol were analyzed by Radio/FID-gas chromatography (FID is coupled on-line with a radiodetector). The ethanol and its derivates were identified by FID while the 11 C-methanol and its co-derivates (with ethanol) were detected by both of FID and radiodetector. Results The 11 C-dimethyl ether was the common product of the single 11 C-methanol transformation on H-MCM-41, Ni-MCM-41 and Ni- Al 2 O 3 at low temperature (200-280 degC) due to middle strong acid sites. At higher temperature (280-350 degC), the dimethyl ether and hydrocarbons were the dominant products on H-MCM-41 while dimethyl ether selectivity decreased on Ni-alumina and Ni-MCM-41 in favor of methane. The selectivities of methanol to formaldehyde and methane were the highest on Ni-MCM-41. During co-reaction of 11 C-methanol with non-radioactive ethanol, the 11 C-labeled coethers, namely 11 C-methyl ethyl ether

Influence of the silica fillers on the ageing of epoxy resins under irradiations

International Nuclear Information System (INIS)

Benard, F.

2004-01-01

Various studies were carried out on the ageing of epoxy resins under irradiations. In all cases, pure polymers were studied. The aim of our work managed by the CEA and the CNRS consists on studying the part of fillers and particularly the part of silica on ageing process under electron beam irradiations. Because of their wide use in industrial applications and especially in nuclear environment, the DGEBA-TETA resins (Diglycidylether of Bisphenol A - Triethylenetetramine) were chosen. Those epoxy resins are difficult to analyse because of their insolubility. Some pure and nano-metric silica filled chemical models which chemical structure very close to the one the DGEBA/TETA resin were synthesized and analysed with classical methods in organic chemistry. A major phenomenon of rupture of the C-O and C-N chemical bonds with creation of phenolic extremities, methylketone extremities, of primary and tertiary amines and notably enamine functions were revealed by the analyses. The quantitative 1 H and 13 C NMR analyses revealed the screen effect due to the silica and the reactions between the chemical species created by the irradiations and the silica surface. Thermic and thermodynamic analyses of the different epoxy resins in function of the irradiation dose and of the kind of silica showed the decrease of the glass transition temperature, of the relaxation temperature and of the crosslink density confirming the major phenomenon of bond ruptures during irradiations. With silica, the decrease of the crosslink density is slowed. This phenomenon can be explained with interactions between the nano-metric silica surface and the epoxy resin offsetting the effect of the chain rupture on the resin mechanical properties. The 13 C solid state NMR analyses confirmed the choice of the chemical models and permitted to detect the chemical species created by the irradiations. The analyse of the polarization transfers with 13 C CP-MAS NMR spectroscopy revealed the stiffening of the nano

Styrene grafted natural rubber reinforced by in situ silica generated via sol–gel technique

Energy Technology Data Exchange (ETDEWEB)

Sittiphan, Torpong [Program of Petrochemistry and Polymer Sciences, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Prasassarakich, Pattarapan [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Poompradub, Sirilux, E-mail: sirilux.p@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand)

2014-02-15

Highlights: • Sol–gel reaction by NR latex was the absence of use of organic solvent and base catalyst. • Well dispersed in situ formed silica particles in the rubber matrix were obtained. • In situ silica was better to improve mechanical properties of rubber vulcanizates. -- Abstract: The filling of styrene graft natural rubber (ST-GNR) with in situ formed silica was performed using the sol–gel reaction via the latex solution method. The mechanical properties of ST-GNR/NR vulcanizate were improved when using the in situ formed silica to levels higher than those obtained with the commercial ex situ formed silica filled ST-GNR/NR vulcanizates at a comparable silica content of 12 parts by weight per hundred parts of rubber. Transmission electron microscopy analysis revealed that the in situ silica particles were small (∼40 nm diameter) and well dispersed, while the commercial silica particles were larger (∼60 nm diameter) and markedly agglomerated in the rubbery matrix. The mechanical properties of the composites prepared via both the solid rubber and latex solution methods were comparable.

Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction

Science.gov (United States)

Xu, Wei; Li, Yani; Yu, Bo; Yang, Jindou; Zhang, Ying; Chen, Xi; Zhang, Guofang; Gao, Ziwei

2015-01-01

A successive anchoring of Ti(NMe2)4, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1‧-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on silica was conducted by SOMC strategy in moderate conditions. The silica, monitored by in-situ Fourier transform infrared spectroscopy (in-situ FT-IR), was pretreated at different temperatures (200, 500 and 800 °C). The ligand tailored silica-supported titanium complexes were characterized by in-situ FT-IR, 13C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), X-ray absorption near edge structure (XANES) and elemental analysis in detail, verifying that the surface titanium species are single sited. The catalytic activity of the ligand tailored single-site silica supported titanium complexes was evaluated by a cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the dehydroxylation temperatures of silica and the configuration of the ligands.

Polar silica-based stationary phases. Part II- Neutral silica stationary phases with surface bound maltose and sorbitol for hydrophilic interaction liquid chromatography.

Science.gov (United States)

Rathnasekara, Renuka; El Rassi, Ziad

2017-07-28

Two neutral polyhydroxylated silica bonded stationary phases, namely maltose-silica (MALT-silica) and sorbitol-silica (SOR-silica), have been introduced and chromatographically characterized in hydrophilic interaction liquid chromatography (HILIC) for a wide range of polar compounds. The bonding of the maltose and sorbitol to the silica surface was brought about by first converting bare silica to an epoxy-activated silica surface via reaction with γ-glycidoxypropyltrimethoxysilane (GPTMS) followed by attaching maltose and sorbitol to the epoxy surface in the presence of the Lewis acid catalyst BF 3 .ethereate. Both silica based columns offered the expected retention characteristics usually encountered for neutral polar surface. The retention mechanism is majorly based on solute' differential partitioning between an organic rich hydro-organic mobile phase (e.g., ACN rich mobile phase) and an adsorbed water layer on the surface of the stationary phase although additional hydrogen bonding was also responsible in some cases for solute retention. The MALT-silica column proved to be more hydrophilic and offered higher retention, separation efficiency and resolution than the SOR-silica column among the tested polar solutes such as derivatized mono- and oligosaccharides, weak phenolic acids, cyclic nucleotide monophosphate and nucleotide-5'-monophosphates, and weak bases, e.g., nucleobases and nucleosides. Copyright © 2017 Elsevier B.V. All rights reserved.

A polyacrylonitrile copolymer-silica template for three-dimensional hierarchical porous carbon as a Pt catalyst support for the oxygen reduction reaction.

Science.gov (United States)

Liu, Minmin; Li, Jian; Cai, Chao; Zhou, Ziwei; Ling, Yun; Liu, Rui

2017-08-01

Herein, we report a novel route to construct a hierarchical three-dimensional porous carbon (3DC) through a copolymer-silica assembly. In the synthesis, silica acts as a hard template and leads to the formation of an interconnected 3D macropore, whereas styrene-co-acrylonitrile polymer has been used as both a carbon source and a soft template for micro- and meso-pores. The obtained 3DC materials possess a large surface area (∼550.5 m 2 g -1 ), which facilitates high dispersion of Pt nanoparticles on the carbon support. The 3DC-supported Pt electrocatalyst shows excellent performance in the oxygen reduction reaction (ORR). The easy processing ability along with the characteristics of hierarchical porosity offers a new strategy for the preparation of carbon nanomaterials for energy application.

POLYETHYLENEIMINE (PEI ON SILICA AS CATALYST IN KNOEVENAGEL AND MICHAEL REACTIONS

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FATIHA ZAOUI

2017-03-01

Full Text Available After the synthesis of polyethylenimine supported on silica, it has been used as a new and efficient catalyst in Knoevenagel and Michael condensations. The presence of the polyethylenimine in the catalytic system together with silica displays an acido-basic character allows a better catalytic activity in the condensations. Carried out under microwave irradiation, without organic solvent and during short time, the syntheses are respectful towards green chemistry. The solid catalyst can be easily reused. This catalyst has the acido-basic character at the same time.

One-pot and efficient synthesis of triazolo[1,2-a]indazole-triones via reaction of arylaldehydes with urazole and dimedone catalyzed by silica nanoparticles prepared from rice husk.

Science.gov (United States)

Hamidian, Hooshang; Fozooni, Samieh; Hassankhani, Asadollah; Mohammadi, Sayed Zia

2011-10-26

A novel synthesis of triazolo[1,2-a]indazole-1,3,8-trione derivatives by reaction of urazole, dimedone and aromatic aldehydes under conventional heating and microwave irradiation and solvent-free conditions using silica nanoparticles prepared from rice husk ash as catalyst is described. The new method features high yields, multicomponent reactions and environmental friendliness.

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....

The mechanism of cesium immobilization in densified silica-fume blended cement pastes

International Nuclear Information System (INIS)

Bar-Nes, G.; Katz, A.; Peled, Y.; Zeiri, Y.

2008-01-01

The role of silica-fume agglomerates, found in densified silica-fume (DSF) pastes, in the immobilization mechanism of Cs ions was studied. Samples of cementitious pastes containing two different forms of silica fume - DSF and raw silica fume (RSF) - were prepared. Leaching experiments showed that both additives reduced the leachability of the metal ion, but the effect of the DSF paste was much stronger. Scanning Electron Microscopy, together with Differential Thermal Analysis, proved that no agglomerated particles were present in the RSF pastes and that the extent of pozzolanic reactivity was higher. We therefore believe that unreacted silica within the DSF agglomerates adsorbs Cs ions and consequently increases their immobilization. Furthermore, this work suggests that during the pozzolanic reaction, a hydrated rim develops around the agglomerate that acts as an additional diffusion barrier for the Cs ions, resulting in an increased efficiency of Cs immobilization

Mesoporous Silica from Rice Husk Ash

Directory of Open Access Journals (Sweden)

S.A. Mandavgane

2010-12-01

Full Text Available Mesoporous silica is used as a raw material in several areas: in preparation of catalysts, in inks, as aconcrete hardening accelerator, as a component of detergents and soaps, as a refractory constituent etc.Sodium silicate is produced by reacting rice hull ash (RHA with aqueous NaOH and silica is precipitatedfrom the sodium silicate by acidification. In the present work, conversion of about 90% of silica containedin RHA into sodium silicate was achieved in an open system at temperatures of about 100 °C. The resultsshowed that silica obtained from RHA is mesoporous, has a large surface area and small particle size.Rice Husk is usually mixed with coal and this mixture is used for firing boilers. The RHA therefore, usuallycontains carbon particles. Activated carbon embedded on silica has been prepared using the carbon alreadypresent in RHA. This carbon shows good adsorption capacity. ©2010 BCREC UNDIP. All rights reserved(Received: 25th April 2010, Revised: 17th June 2010, Accepted: 24th June 2010[How to Cite: V.R. Shelke, S.S. Bhagade, S.A. Mandavgane. (2010. Mesoporous Silica from Rice Husk Ash. Bulletin of Chemical Reaction Engineering and Catalysis, 5 (2: 63-67. doi:10.9767/bcrec.5.2.793.63-67

One-Pot and Efficient Synthesis of Triazolo[1,2-a]indazole-triones via Reaction of Arylaldehydes with Urazole and Dimedone Catalyzed by Silica Nanoparticles Prepared from Rice Husk

Directory of Open Access Journals (Sweden)

Asadollah Hassankhani

2011-10-01

Full Text Available A novel synthesis of triazolo[1,2-a]indazole-1,3,8-trione derivatives by reaction of urazole, dimedone and aromatic aldehydes under conventional heating and microwave irradiation and solvent-free conditions using silica nanoparticles prepared from rice husk ash as catalyst is described. The new method features high yields, multicomponent reactions and environmental friendliness.

UV-cured methacrylic-silica hybrids: Effect of oxygen inhibition on photo-curing kinetics

International Nuclear Information System (INIS)

Corcione, C. Esposito; Striani, R.; Frigione, M.

2014-01-01

Highlights: • The kinetic behavior of novel photopolymerizable organic–inorganic hybrid system was studied as a function of the composition and of the atmosphere for reactions. • The UV-curing reaction of the hybrid mixture was found fast and complete. • The combined presence of thiol monomer and nanostructured silica allows to reduce the effect of inhibition of oxygen towards the radical photopolymerization. - Abstract: The kinetic behavior of innovative photopolymerizable UV-cured methacrylic–silica hybrid formulations, previously developed, was studied and compared to that of a reference control system. The organic–inorganic (O–I) hybrids proposed in this study are obtained from organic precursors with a high siloxane content mixed with tetraethoxysilane (TEOS) in such a way to produce co-continuous silica nano-domains dispersed within a cross-linked organic phase, as a result of the hydrolysis and condensation reactions. The kinetics of the radical photopolymerization mechanism induced by UV-radiations, in presence of a suitable photoinitiator, was studied by calorimetric, FTIR and Raman spectroscopic analyses, by varying the composition of the mixtures and the atmosphere for reactions. The well known effect of oxygen on the kinetic mechanism of the free radical photopolymerization of the methacrylic–siloxane based monomers was found to be strongly reduced in the hybrid system, especially when a proper thiol was used. The experimental calorimetric data were fitted using a simple kinetic model for radical photopolymerization reactions, obtaining a good agreement between the experimental data and the theoretical model. From the comparison of the kinetic constants calculated for control and hybrid systems, it was possible to assess the effect of the composition, as well as of the atmosphere used during the photo-polymerization process, on the kinetic of photopolymerization reaction

Microwave-assisted combustion synthesis of nano iron oxide/iron-coated activated carbon, anthracite, cellulose fiber, and silica, with arsenic adsorption studies

Science.gov (United States)

Combustion synthesis of iron oxide/iron coated carbons such as activated carbon, anthracite, cellulose fiber and silica is described. The reactions were carried out in alumina crucibles using a Panasonic kitchen microwave with inverter technology, and the reaction process was com...

Supramolecular Complex Antioxidant Consisting of Vitamins C, E and Hydrophilic-Hydrophobic Silica Nanoparticles

Science.gov (United States)

Laguta, I. V.; Kuzema, P. O.; Stavinskaya, O. N.; Kazakova, O. A.

Samples with varied amount of surface trimethylsilyl groups were obtained via gas-phase chemical modification of silica nanoparticles. The biocompatibility tests conducted in erythrocyte suspension have shown that hydrophobization of silica decreases its damaging effect to the cells. Being wettable in aqueous media, partially silylated silicas have higher affinity to hydrophobic bioactive molecules in comparison with the initial silica. Novel antioxidant consisting of vitamins C and E and silica with 40% of surface trimethylsilyl groups was formulated. It was found that supramolecular complexes are formed on the silica surface due to the affinity of water- and fat-soluble antioxidants to hydrophilic silanol and hydrophobic trimethylsilyl groups, respectively. Test reactions (total phenolic index determination, DPPH test) and in vitro studies (spectral analysis of erythrocyte suspensions undergoing UV irradiation) revealed the correlation between antioxidant activity of the complex antioxidant and the vitamins’ content. The antioxidant remained active during long-term storage under standard conditions.

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

International Nuclear Information System (INIS)

Liao Yufeng; Li Wenjiang; He Sailing

2007-01-01

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

A study of some fundamental physicochemical variables on the morphology of mesoporous silica nanoparticles MCM-41 type

Science.gov (United States)

Beltrán-Osuna, Ángela A.; Gómez Ribelles, José L.; Perilla, Jairo E.

2017-12-01

All variables affecting the morphology of mesoporous silica nanoparticles (MSN) should be carefully analyzed in order to truly tailored design their mesoporous structure according to their final use. Although complete control on MCM-41 synthesis has been already claimed, reproducibility and repeatability of results remain a big issue due to the lack of information reported in literature. Stirring rate, reaction volume, and system configuration (i.e., opened or closed reactor) are three variables that are usually omitted, making the comparison of product characteristics difficult. Specifically, the rate of solvent evaporation is seldom disclosed, and its influence has not been previously analyzed. These variables were systematically studied in this work, and they were proven to have a fundamental impact on final particle morphology. Hence, a high degree of circularity ( C = 0.97) and monodispersed particle size distributions were only achieved when a stirring speed of 500 rpm and a reaction scale of 500 mL were used in a partially opened system, for a 2 h reaction at 80 °C. Well-shaped spherical mesoporous silica nanoparticles with a diameter of 95 nm, a pore size of 2.8 nm, and a total surface area of 954 m2 g-1 were obtained. Final characteristics made this product suitable to be used in biomedicine and nanopharmaceutics, especially for the design of drug delivery systems.

Mass spectrometric investigation of synthetic glycoside of muramyl dipeptide immobilized on fumed silica surface

Energy Technology Data Exchange (ETDEWEB)

Kulik, Tetiana V., E-mail: tanyakulyk@gala.net [O.O. Chuiko Institute of Surface Chemistry, National Academy of Sciences of Ukraine, 17 Generala Naumova Str., Kyiv 03164 (Ukraine); Azizova, Liana R., E-mail: liana_azizova@ukr.net [O.O. Chuiko Institute of Surface Chemistry, National Academy of Sciences of Ukraine, 17 Generala Naumova Str., Kyiv 03164 (Ukraine); Palyanytsya, Borys B. [O.O. Chuiko Institute of Surface Chemistry, National Academy of Sciences of Ukraine, 17 Generala Naumova Str., Kyiv 03164 (Ukraine); Zemlyakov, Alexander E.; Tsikalova, Victoria N. [Vernadsky Tauric National University, pr. Akademika Vernadskogo 4, Simferopol, 95007 (Ukraine)

2010-05-25

N-Acetylmuramyl-L-alanyl-D-isoglutamine or muramyl dipeptide is a cleavage product of peptidoglycan by lysozyme. This study explored the use of the temperature-programmed desorption mass spectrometry (TPDMS) in analysis of glycoside of muramyl dipeptide: O-{l_brace}(4-tert-butylcyclohexyl)-2-acetamido-2, 3-dideoxy-{beta}-D-glucopyranoside-3-yl{r_brace}-D-lactoyl-L-alanyl-D-isoglutamine (MDP) on the surface of fumed silica. Stages of pyrolysis of MDP in condensed state and on the silica surface have been determined. Three stages have been clear identified under pyrolysis of MDP on the silica surface. Kinetic parameters of thermal reactions on the fumed silica surface and in the condensed state have been calculated.

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

Directory of Open Access Journals (Sweden)

Wang Y

2013-10-01

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

XAFS study on silica glasses irradiated in a nuclear reactor

International Nuclear Information System (INIS)

Yoshida, Tomoko; Yoshida, Hisao; Hara, Takanobu; Ii, Tatsuya; Okada, Tomohisa; Tanabe, Tetsuo

2000-01-01

X-ray absorption technique (XANES and EXAFS) was applied to study the local structures of silica glasses before and after the irradiation in a nuclear reactor. Although our separate photoluminescence (PL) measurements clearly showed the different aspects about oxygen vacancies in these samples, i.e., at least the B 2β type oxygen-deficient center exists as an intrinsic defect in the fused silica glass while another type B 2α center is formed in the synthesized silica glass, such differences did not directly reflect on the X-ray absorption spectra (XANES and EXAFS). However, the curve-fitting analysis of EXAFS showed that the number of oxygen atoms coordinated to Si relatively increased after the irradiation. This result may indicate the occurrence of the structural relaxation in the irradiated samples, that is, a slightly distorted SiO 4 tetrahedra in silica glasses relaxed to the regular SiO 4 tetrahedra due to the break of some connections between SiO 4 units in the silica glasses. Thus, the X-ray absorption technique gave the important information of the in-reactor irradiated silica glasses which complements the results obtained from PL measurements

Performance of Portland cement mixes containing silica fume and mixed with lime-water

Directory of Open Access Journals (Sweden)

Metwally A.A. Abd Elaty

2014-12-01

Test results show that using lime-water in mixing enhances consistency degree compared to the corresponding control mixes. Furthermore, it delays both initial and final setting times compared with traditional water due to the common ion effect principles. Moreover, combined use of lime-water and silica fume enhances the pozzolanic reaction that was identified by the strength development at both early and later ages. The existence of CH crystals for higher percentages of silica fume (up to 30% for further reaction at later ages was observed by XRD results. Moreover, combined use of silica fume and lime-water ensures a high alkaline media around steel bars from the moment of ingredients mixing as long as later ages despite of pozzolanic reaction that was identified from results of chloride attack.

Nanoengineering of methylene blue loaded silica encapsulated magnetite nanospheres and nanocapsules for photodynamic therapy

Energy Technology Data Exchange (ETDEWEB)

Andhariya, Nidhi [Bhavnagar University, Department of Physics (India); Chudasama, Bhupendra, E-mail: bnchudasama@gmail.com [Thapar University, School of Physics and Materials Science (India); Mehta, R. V. [Bhavnagar University, Department of Physics (India); Upadhyay, R. V. [Charotar University of Science and Technology, P.D. Patel Institute of Applied Sciences (India)

2011-09-15

Core-shell nanostructures have emerged as an important class of functional materials with potential applications in diverse fields, especially in health sciences. In this article, nanoengineering of novel magnetic colloidal dispersion containing surface modifiable silica with a core of single domain magnetite nanoparticles loaded with photosensitizer (PS) drug 'Methylene blue' (MB) has been described. Magnetite core is produced by the well-established chemical coprecipitation technique and silica shell is formed over it by the modified hydrolysis and condensation of TEOS (tetraethyl orthosilicate). Conditions for reaction kinetics have been established to tailor the core-shell structures in the form of nanospheres and nanocapsules. MB is loaded into the nanostructures by demethylation reaction. The major conclusion drawn from this study is that the synthesis route yields stable, non-aggregated MB loaded superparamagnetic magnetite-silica nanostructures with tailored morphology, tunable loading, and excellent magnetic properties.

Mesoporous Silica from Rice Husk Ash

Directory of Open Access Journals (Sweden)

V.R. Shelke

2011-01-01

Full Text Available Mesoporous silica is used as a raw material in several areas: in preparation of catalysts, in inks, as a concrete hardening accelerator, as a component of detergents and soaps, as a refractory constituent etc. Sodium silicate is produced by reacting rice hull ash (RHA with aqueous NaOH and silica is precipitated from the sodium silicate by acidification. In the present work, conversion of about 90% of silica contained in RHA into sodium silicate was achieved in an open system at temperatures of about 100 °C. The results showed that silica obtained from RHA is mesoporous, has a large surface area and small particle size. Rice Husk is usually mixed with coal and this mixture is used for firing boilers. The RHA therefore, usually contains carbon particles. Activated carbon embedded on silica has been prepared using the carbon already present in RHA. This carbon shows good adsorption capacity. ©2010 BCREC UNDIP. All rights reserved(Received: 25th April 2010, Revised: 17th June 2010, Accepted: 24th June 2010[How to Cite: V.R. Shelke, S.S. Bhagade, S.A. Mandavgane. (2010. Mesoporous Silica from Rice Husk Ash. Bulletin of Chemical Reaction Engineering and Catalysis, 5 (2: 63-67. doi:10.9767/bcrec.5.2.793.63-67][DOI: http://dx.doi.org/10.9767/bcrec.5.2.793.63-67

A Silica-Supported Monoalkylated Tungsten Dioxo Complex Catalyst for Olefin Metathesis

KAUST Repository

Maity, Niladri

2018-02-15

A well-defined silica-supported monoalkylated tungsten dioxo complex [(Si-O-)W(=O)(CH-Bu)] was prepared by treatment of highly dehydroxylated silica (SiO: silica treated at 700 °C under high vacuum) with an ionic precursor complex [NEt][W(=O)(CH-Bu)]. The identity of the resulting neutral monoalkylated tungsten dioxo surface complex was established by means of elemental microanalysis and spectroscopic studies (IR, solid-state NMR, Raman, and X-ray absorption spectroscopies). The supported tungsten complex was found to act as a precatalyst for the self-metathesis of 1-octene in a batch reactor. The mechanistic implications of this reaction are discussed with the support of DFT calculations highlighting the potential occurrence of thus-far unexplored mechanistic pathways.

A Silica-Supported Monoalkylated Tungsten Dioxo Complex Catalyst for Olefin Metathesis

KAUST Repository

Maity, Niladri; Barman, Samir; Minenkov, Yury; Ould-Chikh, Samy; Abou-Hamad, Edy; Ma, Tao; Qureshi, Ziyauddin; Cavallo, Luigi; D'Elia, Valerio; Gates, Bruce C.; Basset, Jean-Marie

2018-01-01

A well-defined silica-supported monoalkylated tungsten dioxo complex [(Si-O-)W(=O)(CH-Bu)] was prepared by treatment of highly dehydroxylated silica (SiO: silica treated at 700 °C under high vacuum) with an ionic precursor complex [NEt][W(=O)(CH-Bu)]. The identity of the resulting neutral monoalkylated tungsten dioxo surface complex was established by means of elemental microanalysis and spectroscopic studies (IR, solid-state NMR, Raman, and X-ray absorption spectroscopies). The supported tungsten complex was found to act as a precatalyst for the self-metathesis of 1-octene in a batch reactor. The mechanistic implications of this reaction are discussed with the support of DFT calculations highlighting the potential occurrence of thus-far unexplored mechanistic pathways.

A study of positron properties in quartz crystals and synthetic silica glass

International Nuclear Information System (INIS)

Anwand, W.; Brauer, G.; Hesegawa, M.; Dersch, O.; Rauch, F.

2001-01-01

The monoenergetic positron beamline 'SPONSOR' at Rossendorf has been used to investigate the positron behaviour in a naturally grown Brasilian quartz, two synthetic quartz crystals of different origin, and synthetic silica glass. The measurements allow us to obtain the positron diffusion length of free positrons and Bloch para-positronium, if formed, in these materials. In addition, hydrothermal treatment of a synthetic quartz has been used to introduce hydrogen into the crystal up to a certain depth. The presence of hydrogen is found to influence the formation of para-positronium. The depth distribution of hydrogen has been measured independently by the nuclear reaction analysis, and will be discussed in comparison with the results deduced from the positron studies. (author)

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

Well-Defined Silica Grafted Molybdenum Bis(imido) Catalysts for Imine Metathesis Reactions

KAUST Repository

Barman, Samir

2017-04-06

Novel site-isolated tetracoordinated molybdenum complexes possessing bis(imido) ligands, [(≡Si–O)2Mo(═NR)2] (R = t-Bu, 2,6-C6H3-i-Pr2), were immobilized on partially dehydroxylated silica (SiO2-200) by a rigorous surface organometallic chemistry protocol. The newly developed materials adorned with bis(imido) functional units, which were previously exploited mainly as spectator ligands on silica-supported olefin metathesis molybdenum catalysts, are found to be efficient heterogeneous catalytic systems for imine cross metathesis under mild conditions.

Well-Defined Silica Grafted Molybdenum Bis(imido) Catalysts for Imine Metathesis Reactions

KAUST Repository

Barman, Samir; Merle, Nicolas; Minenkov, Yury; De Mallmann, Aimery; Samantaray, Manoja; Le Qué mé ner, Fré dé ric; Szeto, Kai C.; Abou-Hamad, Edy; Cavallo, Luigi; Taoufik, Mostafa; Basset, Jean-Marie

2017-01-01

Novel site-isolated tetracoordinated molybdenum complexes possessing bis(imido) ligands, [(≡Si–O)2Mo(═NR)2] (R = t-Bu, 2,6-C6H3-i-Pr2), were immobilized on partially dehydroxylated silica (SiO2-200) by a rigorous surface organometallic chemistry protocol. The newly developed materials adorned with bis(imido) functional units, which were previously exploited mainly as spectator ligands on silica-supported olefin metathesis molybdenum catalysts, are found to be efficient heterogeneous catalytic systems for imine cross metathesis under mild conditions.

Effects of nano-silica on mechanical performance and microstructure of ultra-high performance concrete

Energy Technology Data Exchange (ETDEWEB)

Mendes, T. M., E-mail: thiagomendes@utfpr.edu.br [Universidade Tecnologica Federal do Parana (UTFPR), Londrina, PR (Brazil). Departamento de Engenharia Ambiental; Repette, W.L., E-mail: wellington.repette@gmail.br [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil). Dept. de Engenharia Civil; Reis, P.J., E-mail: pjlondrina@yahoo.com.br [Univeridade Estadual de Londrina (UEL), PR (Brazil). Lab. de Fisica Nuclear Aplicada

2017-07-15

The use of nanoparticles in ultra-high strength concretes can result in a positive effect on mechanical performance of these cementitious materials. This study evaluated mixtures containing 10 and 20 wt% of silica fume, for which the optimum nano-silica content was determined, i.e. the quantity of nano-silica that resulted on the higher gain of strength. The physical characterization of raw materials was done in terms of particle size distribution, density and specific surface area. Chemical and mineralogical compositions of materials were obtained through fluorescence and X-ray diffraction. The mechanical performance was evaluated by compressive strength, flexural strength and dynamic elastic modulus measurements. The microstructural analysis of mixtures containing nano-silica was performed by X-ray diffraction, thermogravimetry, mercury intrusion porosimetry and scanning electron microscopy. Obtained results indicate an optimum content of nano-silica of 0.62 wt%, considering compressive and flexural strengths. This performance improvement was directly related to two important microstructural aspects: the packing effect and pozzolanic reaction of nano-silica. (author)

Effects of nano-silica on mechanical performance and microstructure of ultra-high performance concrete

International Nuclear Information System (INIS)

Mendes, T. M.; Repette, W.L.; Reis, P.J.

2017-01-01

The use of nanoparticles in ultra-high strength concretes can result in a positive effect on mechanical performance of these cementitious materials. This study evaluated mixtures containing 10 and 20 wt% of silica fume, for which the optimum nano-silica content was determined, i.e. the quantity of nano-silica that resulted on the higher gain of strength. The physical characterization of raw materials was done in terms of particle size distribution, density and specific surface area. Chemical and mineralogical compositions of materials were obtained through fluorescence and X-ray diffraction. The mechanical performance was evaluated by compressive strength, flexural strength and dynamic elastic modulus measurements. The microstructural analysis of mixtures containing nano-silica was performed by X-ray diffraction, thermogravimetry, mercury intrusion porosimetry and scanning electron microscopy. Obtained results indicate an optimum content of nano-silica of 0.62 wt%, considering compressive and flexural strengths. This performance improvement was directly related to two important microstructural aspects: the packing effect and pozzolanic reaction of nano-silica. (author)

a study on silica sand quality in yazaram and mugulbu deposits

African Journals Online (AJOL)

ENGR. G A DUVUNA

A STUDY ON SILICA SAND QUALITY IN YAZARAM AND MUGULBU ... the lowest percentage of silica content of 77.60% and the grain morphology was found to be angular with specific ..... things.com/articles/glass colouring.html, accessed.

Study of cross-linking reactions induced by gamma rays in hybrid membranes of Bisphenol-A-Polysulfone and precipitated silica

International Nuclear Information System (INIS)

Furtado Filho, Acacio Antonio M.; Gomes, Ailton de S.; Lopes, Lea; Benzi, Marcia R.

2011-01-01

In this work the bisphenol-A-polysulfone (PSF) was sulfonated using trimethyl silyl chlorosulfonate [(CH 3 ) 3 SiSO 3 Cl] as a mild sulfonating agent in a homogeneous solution of dichloroethane. The sulfonation reaction was confirmed by acid-base titration and FTIR-spectroscopy analysis. The hybrid membranes were obtained by casting the sulfonated bisphenol-A-polysulfone (SPSF) and precipitated silica Tixosil R 333 solutions in N-N-dimethylacetamide. Cross-linking in the hybrid membranes was obtained by irradiation, with doses ranging from 5 to 30 kGy using gamma ray from a 60 Co source. The water uptake and the swelling of the membranes were estimated by measuring the change in weight between dry and wet conditions. The conductivity of the membranes in acid form was measured with the ac impedance technique using a PGSTAT30 frequency response analyzer. The hybrid cross-linked membranes have conductivity close to 10-1 S.cm -1 at 100% RH and 80 deg C. Electrochemical performances, thermo-mechanical stability and low cost make this cross-linked SPSF hybrid membrane an attractive material for fuel cells using a proton exchange membrane. (author)

Quantitative assessment of alkali silica reaction potential of quartz-rich aggregates: comparison of chemical test and accelerated mortar bar test improved by SEM-PIA

Czech Academy of Sciences Publication Activity Database

Šachlová, Š.; Kuchařová, A.; Pertold, Z.; Přikryl, R.; Fridrichová, Michaela

2017-01-01

Roč. 76, č. 1 (2017), s. 133-144 ISSN 1435-9529 R&D Projects: GA ČR(CZ) GAP104/12/0915 Institutional support: RVO:67985831 Keywords : accelerated mortar bar test * Alkali silica reaction * chemical test * electron microscopy * petrographic image analysis Subject RIV: DD - Geochemistry OBOR OECD: Environmental and geological engineering , geotechnics Impact factor: 1.901, year: 2016

Influence of colloidal nano-silica on alkyd autoxidation

DEFF Research Database (Denmark)

Nikolic, Miroslav; Sanadi, Anand Ramesh; Löf, David

2017-01-01

Nanoparticles are often added to coatings in order to improve their mechanical properties. However, nanoparticles can also influence the cross-linking reaction of polymers and overall curing kinetics, and from this follows that properties of interest are further impacted. In research studies...... on alkyd-based coatings, only the physical drying stage during the first 24 h has been studied in this respect until now. In this study, it was shown with the use of Raman spectroscopy that colloidal nano-silica can change the rate of alkyd autoxidation and how this effect is reflected on the tensile...... properties of the coating. One of the consequences of the influence of nano-silica on curing kinetics is that, contrary to implicit assumptions of common testing methods, the real effect of nanoparticles on mechanical properties can emerge much later in the coating lifetime....

The Effect of Titanium Tetrahedral Coordination of Silica-Titania Catalyst on the Physical Properties of Biodiesel

Science.gov (United States)

Nizar, U. K.; Hidayatul, J.; Sundari, R.; Bahrizal, B.; Amran, A.; Putra, A.; Latisma DJ, L.; Dewata, I.

2018-04-01

This study investigates the correlation of the number of titanium tetrahedral coordination and biodiesel production. The solid-state method has been used to synthesis of silica-titania catalyst for biodiesel production, which the precursors, i.e. silica and titania commercials were heated in the temperature range of 450 - 550°C. The characterization of the prepared silica-titania has been studied by FTIR and DR UV-Vis in order to identify and calculate the presence of titanium tetrahedral coordination in silica-titania catalyst. A very small peak at around 950 cm-1 indicated the presence of titanium tetrahedral coordination through Si–O–Ti bonds. Deconvolution of DR UV-Vis spectra showed the coordination of titanium in silica-titania is more octahedral. However, the number of titanium tetrahedral coordination of the prepared silica-titania is found higher than that of TiO2 commercial. The increasing of titanium tetrahedral fraction in silica-titania affects the physical properties of biodiesel in terms of boiling point, viscosity and density, which is produced by the reaction of methanol and palm oil.

Some Durability Characteristics of Micro Silica and Nano Silica Contained Concrete

Directory of Open Access Journals (Sweden)

Mohammed Salah Nasr

2016-12-01

Full Text Available This paper aims to investigate the influence of replacement of cement with nano and micro silica admixtures on some durability properties of concrete such as water absorption, chloride content and pH tests. Three replacement ratios (5%,10%,15% of micro silica and four replacement proportions (0.5%,1.5%,3%,5% for nano silica were used in this study. Two exposure conditions were considered for chloride content test: wetting-drying and full immersing exposure in 6% of chloride ions solution, NaCl type. Results showed that mixes of %5 micro silica and 5% nano silica had lower content of chloride (about 0.19% and 0.18% for wetting-drying and full immersing exposure respectively. For water absorption test, all mixes incorporated micro and nano silica, except for %5 micro silica mix, showed lower absorption than control mixes. For pH test, results indicated that the adding of nano and micro silica didn’t affect adversely the alkalinity of concrete.

A coupled mechanical and chemical damage model for concrete affected by alkali–silica reaction

Energy Technology Data Exchange (ETDEWEB)

Pignatelli, Rossella, E-mail: rossellapignatelli@gmail.com [Department of Civil and Environmental Engineering, Politecnico di Milano, Piazza L. da Vinci 32, 20133 Milano (Italy); Lombardi Ingegneria S.r.l., Via Giotto 36, 20145 Milano (Italy); Comi, Claudia, E-mail: comi@stru.polimi.it [Department of Civil and Environmental Engineering, Politecnico di Milano, Piazza L. da Vinci 32, 20133 Milano (Italy); Monteiro, Paulo J.M., E-mail: monteiro@ce.berkeley.edu [Department of Civil and Environmental Engineering, University of California, Berkeley, CA 94720 (United States)

2013-11-15

To model the complex degradation phenomena occurring in concrete affected by alkali–silica reaction (ASR), we formulate a poro-mechanical model with two isotropic internal variables: the chemical and the mechanical damage. The chemical damage, related to the evolution of the reaction, is caused by the pressure generated by the expanding ASR gel on the solid concrete skeleton. The mechanical damage describes the strength and stiffness degradation induced by the external loads. As suggested by experimental results, degradation due to ASR is considered to be localized around reactive sites. The effect of the degree of saturation and of the temperature on the reaction development is also modeled. The chemical damage evolution is calibrated using the value of the gel pressure estimated by applying the electrical diffuse double-layer theory to experimental values of the surface charge density in ASR gel specimens reported in the literature. The chemo-damage model is first validated by simulating expansion tests on reactive specimens and beams; the coupled chemo-mechanical damage model is then employed to simulate compression and flexure tests results also taken from the literature. -- Highlights: •Concrete degradation due to ASR in variable environmental conditions is modeled. •Two isotropic internal variables – chemical and mechanical damage – are introduced. •The value of the swelling pressure is estimated by the diffuse double layer theory. •A simplified scheme is proposed to relate macro- and microscopic properties. •The chemo-mechanical damage model is validated by simulating tests in literature.

Spectroscopic and chromatographic characterisation of a pentafluorophenylpropyl silica phase end-capped in supercritical carbon dioxide as a reaction solvent.

Science.gov (United States)

Ashu-Arrah, Benjamin A; Glennon, Jeremy D; Albert, Klaus

2013-07-12

This research uses solid-state nuclear magnetic resonance (NMR) spectroscopy to characterise the nature and amount of different surface species, and chromatography to evaluate phase properties of a pentafluorophenylpropyl (PFPP) bonded silica phase prepared and end-capped using supercritical carbon dioxide (sc-CO2) as a reaction solvent. Under sc-CO2 reaction conditions (at temperature of 100 °C and pressure of 414 bar), a PFPP silica phase was prepared using 3-[(pentafluorophenyl)propyldimethylchlorosilane] within 1h. The bonded PFPP phase was subsequently end-capped with bis-N,O-trimethylsilylacetamide (BSA), hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) within 1h under the same sc-CO2 reaction conditions (100 °C/4141 bar). Elemental microanalysis, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM) were used to provide support data to solid-state NMR and chromatographic evaluation. Results revealed a surface coverage of 2.2 μmol/m(2) for the non-end-capped PFPP silica phase while the PFPP phase end-capped with BSA gave a higher surface coverage (3.9 μmol/m(2)) compared to HMDS (2.9 μmol/m(2)) and TMCS (2.8 μmol/m(2)). (29)Si CP/MAS NMR analysis of the PFPP end-capped with BSA shows a significant decrease in the amount of Q(3) (free silanols) and Q(4) (siloxane groups) species, coupled with the absence of the most reactive Q(2) (geminal silanols) in addition to increased amount of a single resonance peak centred at +13 ppm (MH) corresponding to -Si-O-*Si-CH3 bond. (13)C CP/MAS NMR shows the resonance corresponding to the propyl linkage (CH3CH2CH2-) and methyl groups (Si(CH3)n) confirming successful silanisation and endcapping reactions in sc-CO2. Chromatographic evaluation of the BSA end-capped PFPP phase with Neue text mixture revealed improved chromatographic separation as evidenced in the enhanced retention of hydrophobic markers and decreased retention for basic solutes. Moreover, chromatography revealed a change in

Cu(II) recognition materials: Fluorophores grafted on mesoporous silica supports

International Nuclear Information System (INIS)

Kledzik, Krzysztof; Orlowska, Maja; Patralska, Dorota; Gwiazda, Marcin; Jezierska, Julia; Pikus, Stanislaw; Ostaszewski, Ryszard; Klonkowski, Andrzej M.

2007-01-01

There were designed and synthesized naphthalene and pyrene derivatives consisting of fluorophore group and of receptor fragment with donor N and O atoms. These fluorosensors were covalently attached by grafting carboxyl group to surfaces of silica xerogel or mesoporous silicas (MCM-41 and MCM-48) functionalized either with 3-aminopropyl or 3-glycidoxypropyl groups. The pyrene derivatives 2 and 3 covalently grafted on MCM-48 silica functionalized with 3-aminopropyl groups are potential recognition elements of a fluorescence chemical sensor. Fluorescence emission of the prepared recognition materials is quenched specifically owing to photoinduced electron transfer (PET) effect after coordination reactions with Cu(II) ions. Moreover, both the materials exhibit selectivity for Cu(II) ions in aqueous solutions in presence of such metal ions as: alkali, alkaline earth and transition. During UV irradiation the studied recognition elements undergo slowly photochemical degradation

Organic inorganic hybrid coating (poly(methyl methacrylate)/monodisperse silica)

Science.gov (United States)

Rubio, E.; Almaral, J.; Ramírez-Bon, R.; Castaño, V.; Rodríguez, V.

2005-04-01

Polymethylmethacrylate-silica hybrid coatings were prepared from methyl methacrylate and monodisperse colloidal silica prepared by the Stöber method. The surfaces of the spheres were successfully modified by chemical reaction with 3-(trimethoxysilyl) propyl methacrylate (TMSPM) to compatibilise the organic and inorganic components of the precursor solution mixture. The coatings were deposited by dip-coating on glass substrates. They result with good properties of homogeneity, optical transparence, hardness and adhesion.

Novel titration method for surface-functionalised silica

Energy Technology Data Exchange (ETDEWEB)

Hofen, Kai; Weber, Siegfried [Department of Biotechnology, University of Applied Sciences, Mannheim (Germany); Chan, Chiu Ping Candace [School of Advanced Manufacturing and Mechanical Engineering, Mawson Institute, University of South Australia, Mawson Lakes Blvd, Mawson Lakes 5095 (Australia); Majewski, Peter, E-mail: peter.majewski@unisa.edu.au [School of Advanced Manufacturing and Mechanical Engineering, Mawson Institute, University of South Australia, Mawson Lakes Blvd, Mawson Lakes 5095 (Australia)

2011-01-15

This paper describes three inexpensive and fast analytical methods to characterise grafted particle surfaces. The reaction of silica with (3-aminopropyl)triethoxysilane, (3-mercaptopropyl)trimethoxysilane and N-(phosphonomethyl)iminodiacetic acid hydrate, respectively, leads to NH{sub 2}-, SO{sub 3}H- or COOH-functionalised silica, which were characterised by X-ray photoelectron spectrometry and titration in nonaqueous media as well as with two titration methods in a water-based environment. In the work presented, factors influencing the titrations are pointed out and solutions are presented to overcome these limiting factors are shown.

Novel titration method for surface-functionalised silica

International Nuclear Information System (INIS)

Hofen, Kai; Weber, Siegfried; Chan, Chiu Ping Candace; Majewski, Peter

2011-01-01

This paper describes three inexpensive and fast analytical methods to characterise grafted particle surfaces. The reaction of silica with (3-aminopropyl)triethoxysilane, (3-mercaptopropyl)trimethoxysilane and N-(phosphonomethyl)iminodiacetic acid hydrate, respectively, leads to NH 2 -, SO 3 H- or COOH-functionalised silica, which were characterised by X-ray photoelectron spectrometry and titration in nonaqueous media as well as with two titration methods in a water-based environment. In the work presented, factors influencing the titrations are pointed out and solutions are presented to overcome these limiting factors are shown.

Acid-base equilibria inside amine-functionalized mesoporous silica.

Science.gov (United States)

Yamaguchi, Akira; Namekawa, Manato; Kamijo, Toshio; Itoh, Tetsuji; Teramae, Norio

2011-04-15

Acid-base equilibria and effective proton concentration inside a silica mesopore modified with a trimethyl ammonium (TMAP) layer were studied by steady-state fluorescence experiments. The mesoporous silica with a dense TMAP layer (1.4 molecules/nm(2)) was prepared by a post grafting of N-trimethoxysilylpropyl-N,N,N-trimethylammonium at surfactant-templated mesoporous silica (diameter of silica framework =3.1 nm). The resulting TMAP-modified mesoporous silica strongly adsorbed of anionic fluorescence indicator dyes (8-hydroxypyrene-1,3,6-trisulfonate (pyranine), 8-aminopyrene-1,3,6-trisulfonate (APTS), 5,10,15,20-tetraphenyl-21H,23H-porphinetetrasulfonic acid disulfuric acid (TPPS), 2-naphthol-3,6-disulfonate (2NT)) and fluorescence excitation spectra of these dyes within TMAP-modified mesoporous silica were measured by varying the solution pH. The fluorescence experiments revealed that the acid-base equilibrium reactions of all pH indicator dyes within the TMAP-modified silica mesopore were quite different from those in bulk water. From the analysis of the acid-base equilibrium of pyranine, the following relationships between solution pH (pH(bulk)) and the effective proton concentration inside the pore (pH(pore)) were obtained: (1) shift of pH(pore) was 1.8 (ΔpH(pore)=1.8) for the pH(bulk) change from 2.1 to 9.1 (ΔpH(bulk)=7.0); (2) pH(pore) was not simply proportional to pH(bulk); (3) the inside of the TMAP-modified silica mesopore was suggested to be in a weak acidic or neutral condition when pH(bulk) was changed from 2.0 to 9.1. Since these relationships between pH(bulk) and pH(pore) could explain the acid-base equilibria of other pH indicator dyes (APTS, TPPS, 2NT), these relationships were inferred to describe the effective proton concentration inside the TMAP-modified silica mesopore. © 2011 American Chemical Society

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.

Microwave-Assisted Combustion Synthesis of Nano Iron Oxide/Iron-Coated Activated Carbon, Anthracite, Cellulose Fiber, and Silica, with Arsenic Adsorption Studies

Directory of Open Access Journals (Sweden)

Mallikarjuna N. Nadagouda

2011-01-01

Full Text Available Combustion synthesis of iron oxide/iron coated carbons such as activated carbon, anthracite, cellulose fiber, and silica is described. The reactions were carried out in alumina crucibles using a Panasonic kitchen microwave with inverter technology, and the reaction process was completed within a few minutes. The method used no additional fuel and nitrate, which is present in the precursor itself, to drive the reaction. The obtained samples were then characterized with X-ray mapping, scanning electron microscopy (SEM, energy dispersive X-ray analysis (EDS, selected area diffraction pattern (SAED, transmission electron microscopy (TEM, X-ray diffraction (XRD, and inductively coupled plasma (ICP spectroscopy. The size of the iron oxide/iron nanoparticle-coated activated carbon, anthracite, cellulose fiber, and silica samples were found to be in the nano range (50–400 nm. The iron oxide/iron nanoparticles mostly crystallized into cubic symmetry which was confirmed by SAED. The XRD pattern indicated that iron oxide/iron nano particles existed in four major phases. That is, γ-Fe2O3, α-Fe2O3, Fe3O4, and Fe. These iron-coated activated carbon, anthracite, cellulose fiber, and silica samples were tested for arsenic adsorption through batch experiments, revealing that few samples had significant arsenic adsorption.

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.

Synthesis of silica nanosphere from homogeneous and ...

Indian Academy of Sciences (India)

WINTEC

avoid it, reaction in heterogeneous system using CTABr was carried out. Nanosized silica sphere with ... Homogeneous system contains a mixture of ethanol, water, aqueous ammonia and ... heated to 823 K (rate, 1 K/min) in air and kept at this.

Extraction of metal ions using chemically modified silica gel: a PIXE analysis.

Science.gov (United States)

Jal, P K; Dutta, R K; Sudarshan, M; Saha, A; Bhattacharyya, S N; Chintalapudi, S N; K Mishra, B

2001-08-30

Organic ligand with carboxyhydrazide functional group was immobilised on the surface of silica gel and the metal binding capacity of the ligand-embedded silica was investigated. The functional group was covalently bonded to the silica matrix through a spacer of methylene groups by sequential reactions of silica gel with dibromobutane, malonic ester and hydrazine in different media. Surface area value of the modified silica was determined. The changes in surface area were correlated with the structural change of the silica surface due to chemical modifications. A mixture solution of metal ions [K(I),Cr(III),Co(II),Ni(II),Cu(II),Zn(II),Hg(II) and U(VI)] was treated with the ligand-embedded silica in 10(-3) M aqueous solution. The measurement of metal extraction capacity of the silica based ligand was done by multielemental analysis of the metal complexes thus formed by using Proton Induced X-ray Emission (PIXE) technique.

Functionalized silica aerogels for gas-phase purification, sensing, and catalysis: A review

Energy Technology Data Exchange (ETDEWEB)

Amonette, James E.; Matyáš, Josef

2017-09-01

Silica aerogels have a rich history and a unique, fascinating gas-phase chemistry that has lent them to many diverse applications. This review starts with a brief discussion of the fundamental issues driving the movement of gases in silica aerogels and then proceeds to provide an overview of the work that has been done with respect to the purification of gases, sensing of individual gases, and uses of silica aerogels as catalysts for gas-phase reactions. Salient features of the research behind these different applications are presented, and, where appropriate, critical aspects that affect the practical use of the aerogels are noted. Specific sections under the gas-purification category focus on the removal of airborne nanoparticles, carbon dioxide, volatile organic compounds, sulfur gases and radioactive iodine from gas streams. The use of silica aerogels as sensors for humidity, oxygen, hydrocarbons, volatile acids and bases, various non-ammoniacal nitrogen gases, and viral particles is discussed. With respect to catalysis, the demonstrated use of silica aerogels as supports for oxidation, Fischer-Tropsch, alkane isomerization, and hydrogenation reactions is reviewed, along with a section on untested catalytic formulations involving silica aerogels. A short section focuses on recent developments in thermomolecular Knudsen compressor pumps using silica aerogel membranes. The review continues with an overview of the production methods, locations of manufacturing facilities globally, and a brief discussion of the economics before concluding with a few remarks about the present and future trends revealed by the work presented.

Study of interaction in silica glass via model potential approach

Science.gov (United States)

Mann, Sarita; Rani, Pooja

2016-05-01

Silica is one of the most commonly encountered substances in daily life and in electronics industry. Crystalline SiO2 (in several forms: quartz, cristobalite, tridymite) is an important constituent of many minerals and gemstones, both in pure form and mixed with related oxides. Cohesive energy of amorphous SiO2 has been investigated via intermolecular potentials i.e weak Van der Waals interaction and Morse type short-range interaction. We suggest a simple atom-atom based Van der Waals as well as Morse potential to find cohesive energy of glass. It has been found that the study of silica structure using two different model potentials is significantly different. Van der Waals potential is too weak (P.E =0.142eV/molecule) to describe the interaction between silica molecules. Morse potential is a strong potential, earlier given for intramolecular bonding, but if applied for intermolecular bonding, it gives a value of P.E (=-21.92eV/molecule) to appropriately describe the structure of silica.

Effect of Molecular Weight on the Properties of Liquid Epoxidized Natural Rubber Acrylate (LENRA)/ Silica Hybrid Composites

International Nuclear Information System (INIS)

Eda Yuhana Ariffin; Azizan Ahmad; Dahlan Mohd; Mahathir Mohamed

2011-01-01

This paper reports on the effect of molecular weight on the morphological and mechanical properties of liquid epoxidized natural rubber acrylate (LENRA)/ silica hybrid composites prepared by sol-gel technique. The sol-gel reaction was conducted at different concentration of tetraethyl orthosilicate (TEOS), used as a precursor of silica. TEOS were introduced in 10, 20, 30, 40 and 50 parts per hundred rubber (phr) in the composites. Two different molecular weights of ENR were used to study the effect of molecular weight on the mechanical and morphological properties of the compounds. These compounds were cured by ultraviolet (UV) irradiation. The mechanical properties were studied through pendulum hardness and scratch tests. Higher molecular weight of ENR showed better mechanical properties than lower molecular weight. Transmission electron microscope was used to determine the silica size and to study the distribution and dispersion of the silica particles. High molecular weight showed greater distribution and dispersion of silica particles with diameter of 13 - 256 nm. Morphological and mechanical properties of LENRA/ silica hybrid composites were improved by using high molecular weight of ENR. (author)

Mesoporous silica nanoparticles for biomedical and catalytical applications

Energy Technology Data Exchange (ETDEWEB)

Sun, Xiaoxing [Iowa State Univ., Ames, IA (United States)

2011-01-01

Mesoporous silica materials, discovered in 1992 by the Mobile Oil Corporation, have received considerable attention in the chemical industry due to their superior textual properties such as high surface area, large pore volume, tunable pore diameter, and narrow pore size distribution. Among those materials, MCM-41, referred to Mobile Composition of Matter NO. 41, contains honeycomb liked porous structure that is the most common mesoporous molecular sieve studied. Applications of MCM-41 type mesoporous silica material in biomedical field as well as catalytical field have been developed and discussed in this thesis. The unique features of mesoporous silica nanoparticles were utilized for the design of delivery system for multiple biomolecules as described in chapter 2. We loaded luciferin into the hexagonal channels of MSN and capped the pore ends with gold nanoparticles to prevent premature release. Luciferase was adsorbed onto the outer surface of the MSN. Both the MSN and the gold nanoparticles were protected by poly-ethylene glycol to minimize nonspecific interaction of luciferase and keep it from denaturating. Controlled release of luciferin was triggered within the cells and the enzymatic reaction was detected by a luminometer. Further developments by varying enzyme/substrate pairs may provide opportunities to control cell behavior and manipulate intracellular reactions. MSN was also served as a noble metal catalyst support due to its large surface area and its stability with active metals. We prepared MSN with pore diameter of 10 nm (LP10-MSN) which can facilitate mass transfer. And we successfully synthesized an organo silane, 2,2'-Bipyridine-amide-triethoxylsilane (Bpy-amide-TES). Then we were able to functionalize LP10-MSN with bipyridinyl group by both post-grafting method and co-condensation method. Future research of this material would be platinum complexation. This Pt (II) complex catalyst has been reported for a C-H bond activation reaction as an

Fluorescence lifetime studies of MeV erbium implanted silica glass

International Nuclear Information System (INIS)

Lidgard, A.; Polman, A.; Jacobsen, D.C.; Blonder, G.E.; Kistler, R.; Poate, J.M.; Becker, P.C.

1991-01-01

MeV erbium ion implantation into various SiO 2 glasses has been studied with the aim of incorporating the rare-earth dopant as an optically active ion in the silica network. The lifetime of the excited state ranges from 1.6 to 12.8 ms, depending on base material and implantation fluence. These results have positive implications for silica-based integrated optical technology. (Author)

Fluorescence lifetime studies of MeV erbium implanted silica glass

Energy Technology Data Exchange (ETDEWEB)

Lidgard, A.; Polman, A.; Jacobsen, D.C.; Blonder, G.E.; Kistler, R.; Poate, J.M.; Becker, P.C. (AT and T Bell Labs., Murray Hill, NJ (USA))

1991-05-23

MeV erbium ion implantation into various SiO{sub 2} glasses has been studied with the aim of incorporating the rare-earth dopant as an optically active ion in the silica network. The lifetime of the excited state ranges from 1.6 to 12.8 ms, depending on base material and implantation fluence. These results have positive implications for silica-based integrated optical technology. (Author).

Chromo- and fluorophoric water-soluble polymers and silica particles by nucleophilic substitution reaction of poly(vinyl amine

Directory of Open Access Journals (Sweden)

Katja Hofmann

2010-07-01

Full Text Available Novel chromophoric and fluorescent carbonitrile-functionalized poly(vinyl amine (PVAm and PVAm/silica particles were synthesized by means of nucleophilic aromatic substitution of 8-oxo-8H-acenaphtho[1,2-b]pyrrol-9-carbonitrile (1 with PVAm in water. The water solubility of 1 has been mediated by 2,6-O-β-dimethylcyclodextrin or by pre-adsorption onto silica particles. Furthermore, 1 was converted with isopropylamine into the model compound 1-M. All new compounds were characterized by NMR, FTIR, UV–vis and fluorescence spectroscopy. The solvent-dependent UV–vis absorption and fluorescence emission band positions of the model compound and the carbonitrile-functionalized PVAm were studied and interpreted using the empirical Kamlet–Taft solvent parameters π* (dipolarity/polarizability, α (hydrogen-bond donating capacity and β (hydrogen-accepting ability in terms of the linear solvation energy relationship (LSER. The solvent-independent regression coefficients a, b and s were determined using multiple linear correlation analysis. It is shown, that the chains of the polymer have a significant influence on the solvatochromic behavior of 1-P. The structure of the carbonitrile 1-Si bound to polymer-modified silica particles was studied by means of X-ray photoelectron spectroscopy (XPS and Brunauer–Emmett–Teller (BET measurements. Fluorescent silica particles were obtained as shown by fluorescence spectroscopy with a diffuse reflectance technique.

Catalytic reduction of organic dyes at gold nanoparticles impregnated silica materials: influence of functional groups and surfactants

International Nuclear Information System (INIS)

Azad, Uday Pratap; Ganesan, Vellaichamy; Pal, Manas

2011-01-01

Gold nanoparticles (Au NPs) in three different silica based sol–gel matrixes with and without surfactants are prepared. They are characterized by UV–vis absorbance and transmission electron microscopic (TEM) studies. The size and shape of Au NPs varied with the organo-functional group present in the sol–gel matrix. In the presence of mercaptopropyl functionalized organo-silica, large sized (200–280 nm) spherical Au NPs are formed whereas in the presence of aminopropyl functionalized organo-silica small sized (5–15 nm) Au NPs are formed inside the tube like organo-silica. Further, it is found that Au NPs act as efficient catalyst for the reduction of organic dyes. The catalytic rate constant is evaluated from the decrease in absorbance of the dye molecules. Presence of cationic or anionic surfactants greatly influences the catalytic reaction. The other factors like hydrophobicity of the organic dyes, complex formation of the dyes with anionic surfactants, repulsion between dyes and cationic surfactant, adsorption of dyes on the Au NPs also play important role on the reaction rate.

Catalytic reduction of organic dyes at gold nanoparticles impregnated silica materials: influence of functional groups and surfactants

Energy Technology Data Exchange (ETDEWEB)

Azad, Uday Pratap; Ganesan, Vellaichamy, E-mail: velganesh@yahoo.com; Pal, Manas [Banaras Hindu University, Department of Chemistry, Faculty of Science (India)

2011-09-15

Gold nanoparticles (Au NPs) in three different silica based sol-gel matrixes with and without surfactants are prepared. They are characterized by UV-vis absorbance and transmission electron microscopic (TEM) studies. The size and shape of Au NPs varied with the organo-functional group present in the sol-gel matrix. In the presence of mercaptopropyl functionalized organo-silica, large sized (200-280 nm) spherical Au NPs are formed whereas in the presence of aminopropyl functionalized organo-silica small sized (5-15 nm) Au NPs are formed inside the tube like organo-silica. Further, it is found that Au NPs act as efficient catalyst for the reduction of organic dyes. The catalytic rate constant is evaluated from the decrease in absorbance of the dye molecules. Presence of cationic or anionic surfactants greatly influences the catalytic reaction. The other factors like hydrophobicity of the organic dyes, complex formation of the dyes with anionic surfactants, repulsion between dyes and cationic surfactant, adsorption of dyes on the Au NPs also play important role on the reaction rate.

Quantifying Silica Reactivity in Subsurface Environments: Reaction Affinity and Solute Matrix Controls on Quartz and SiO2 Glass Dissolution Kinetics

International Nuclear Information System (INIS)

Dove, Patricia M.

2000-01-01

During the three years of this project, Professor Dove's laboratory made tremendous progress in understanding controls on amorphous silica dissolution kinetics in aqueous solutions. Our findings have already received considerable attention. In hydrothermal and low temperature studies, the work focused on determining quantitative and mechanistic controls on the most abundant silica polymorphs in Earth environments--quartz and amorphous silica. Our studies achieved goals set forth in the original proposal to establish a new quantitative understanding of amorphous silica dissolution. This support has resulted in 10 journal, 12 abstracts and 2 thesis publications. The PI and students were also recognized with 6 awards during this period. The 1998 EMSP conference in Chicago was an important meeting for our project. The symposium, enabled P.I. Dove to establish valuable contacts with ''users'' having specific needs for the findings of our EMSP project related to the urgency of problems in the Tanks Focus Area (TFA). Since that time, our working relations developed as Dove interacted with TFA scientists and engineers on the problems of waste glass properties. These interactions refined our experimental objectives to better meet their needs. Dove presented the results of EMSP research findings to a TFA subgroup at a Product Acceptance Workshop held in Salt Lake City during December 1998. The travel costs to attend this unanticipated opportunity were paid from EMSP project funds. In January 2000, Dove also attended a similar meeting in Atlanta with PNNL, SRL and BNF scientists/engineers to discuss new issues and make another level of decisions on the Product Acceptance goals. Our EMSP-funded research interfaced very well with the ongoing studies of Dr. Pete McGrail and colleagues in the Applied Geochemistry Group at PNNL. The value of our work to ''users'' was further demonstrated when Dove's EMSP-funded Postdoc, Dr. Jonathan Icenhower was hired by the same PNNL group. With

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

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.

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.

Contribution to the study of the mechanism of crack in amorphous silica: study by the molecular dynamics of crack in amorphous silica

International Nuclear Information System (INIS)

Van Brutzel, L.

2000-01-01

The aim of this thesis was to understand the mechanism which occurs during the crack at the atomic scale in amorphous silica. The difficulties of the experimental observations at this length scale lead us to use numerical studies by molecular dynamics to access to the dynamical and the thermodynamical informations. We have carried out large simulations with 500000 atoms and studied the structure of the amorphous silica before to studying their behaviours under an imposed strain. The structure of this simulated amorphous silica settled in three length scales. In small length scale between 0 and 5 angstrom glass is composed of tetrahedra, this is close to the crystalline structure. In intermediate length scale between 3 and 10 angstrom tetrahedra are connected together and build rings of different sizes composed in majority between 5 and 7 tetrahedra. In bigger length scale between 15 and 60 angstrom, areas with high density of rings are surrounded by areas with low density of rings. These structural considerations play an important role in initiation and propagation of a crack. Indeed. in this length scale. crack propagates by growth and coalescence of some small cavities which appear in area with low density of rings behind the crack tip. The cavities dissipate the stress with carries away a delay to propagation of the crack. This phenomenons seems ductile and leads to non linear elastic behaviour near the crack tip. We have also shown that the addition of alkali in the amorphous silica changes the structure by creation of nano-porosities and leads to enhance the ductility during the crack propagation. (author)

Crystalline Silica Primer

Science.gov (United States)

,

1992-01-01

Crystalline silica is the scientific name for a group of minerals composed of silicon and oxygen. The term crystalline refers to the fact that the oxygen and silicon atoms are arranged in a threedimensional repeating pattern. This group of minerals has shaped human history since the beginning of civilization. From the sand used for making glass to the piezoelectric quartz crystals used in advanced communication systems, crystalline silica has been a part of our technological development. Crystalline silica's pervasiveness in our technology is matched only by its abundance in nature. It's found in samples from every geologic era and from every location around the globe. Scientists have known for decades that prolonged and excessive exposure to crystalline silica dust in mining environments can cause silicosis, a noncancerous lung disease. During the 1980's, studies were conducted that suggested that crystalline silica also was a carcinogen. As a result of these findings, crystalline silica has been regulated under the Occupational Safety and Health Administration's (OSHA) Hazard Communication Standard (HCS). Under HCS, OSHAregulated businesses that use materials containing 0.1% or more crystalline silica must follow Federal guidelines concerning hazard communication and worker training. Although the HCS does not require that samples be analyzed for crystalline silica, mineral suppliers or OSHAregulated

Pulmonary hypertension and vascular remodeling in mice exposed to crystalline silica.

Science.gov (United States)

Zelko, Igor N; Zhu, Jianxin; Ritzenthaler, Jeffrey D; Roman, Jesse

2016-11-28

Occupational and environmental exposure to crystalline silica may lead to the development of silicosis, which is characterized by inflammation and progressive fibrosis. A substantial number of patients diagnosed with silicosis develop pulmonary hypertension. Pulmonary hypertension associated with silicosis and with related restrictive lung diseases significantly reduces survival in affected subjects. An animal model of silicosis has been described previously however, the magnitude of vascular remodeling and hemodynamic effects of inhaled silica are largely unknown. Considering the importance of such information, this study investigated whether mice exposed to silica develop pulmonary hypertension and vascular remodeling. C57BL6 mice were intratracheally injected with either saline or crystalline silica at doses 0.2 g/kg, 0.3 g/kg and 0.4 g/kg and then studied at day 28 post-exposure. Pulmonary hypertension was characterized by changes in right ventricular systolic pressure and lung histopathology. Mice exposed to saline showed normal lung histology and hemodynamic parameters while mice exposed to silica showed increased right ventricular systolic pressure and marked lung pathology characterized by a granulomatous inflammatory reaction and increased collagen deposition. Silica-exposed mice also showed signs of vascular remodeling with pulmonary artery muscularization, vascular occlusion, and medial thickening. The expression of pro-inflammatory genes such as TNF-α and MCP-1 was significantly upregulated as well as the expression of the pro-remodeling genes collagen type I, fibronectin and the metalloproteinases MMP-2 and TIMP-1. On the other hand, the expression of several vasculature specific genes involved in the regulation of endothelial function was significantly attenuated. We characterized a new animal model of pulmonary hypertension secondary to pulmonary fibrosis induced by crystalline silica. Our data suggest that silica promotes the damage of the

sup(60)Co hot atom chemistry of tris(acetylacetonato) cobalt(III) adsorbed on silica gel

International Nuclear Information System (INIS)

Nishioji, H.; Sakai, Y.; Tominaga, T.

1985-01-01

The sup(60)Co hot atom reactions were studied in tris(acetylacetonato)cobalt(III) adsorbed on silica gel surface. sup(57)Fe Moessbauer spectra of tris(acetylacetonato)iron(III) in the corresponding system were also measured in order to examine the state of dispersion of complex molecules on silica gel. The retention formation processes were discussed in terms of the dependence of sup(60)Co retention on the adsorbed amount (concentration) of cobalt(III) complexes. (author)

Synthesis Characterization and Photocatalytic Studies of Cobalt Ferrite-Silica-Titania Nanocomposites

Directory of Open Access Journals (Sweden)

David Greene

2014-04-01

Full Text Available In this work, CoFe2O4@SiO2@TiO2 core-shell magnetic nanostructures have been prepared by coating of cobalt ferrite nanoparticles with the double SiO2/TiO2 layer using metallorganic precursors. The Transmission Electron Microscopy (TEM, Energy Dispersive X-Ray Analysis (EDX, Vibrational Sample Magnetometer (VSM measurements and Raman spectroscopy results confirm the presence both of the silica and very thin TiO2 layers. The core-shell nanoparticles have been sintered at 600 °C and used as a catalyst in photo-oxidation reactions of methylene blue under UV light. Despite the additional non-magnetic coatings result in a lower value of the magnetic moment, the particles can still easily be retrieved from reaction mixtures by magnetic separation. This retention of magnetism was of particular importance allowing magnetic recovery and re-use of the catalyst.

Hydrothermal synthesis of silica rich zeolites and microporous martials

International Nuclear Information System (INIS)

Durrani, S.K.; Chughtai, N.A.; Akhtar, J.; Arif, M.; Ahmed, M.

1999-01-01

A fast crystallization method for synthesis of silica rich aluminosilicate and ferro silicate zeotype materials has been reported. The method also permits for the complete crystallization of silico alumino phosphate microporous materials. Aluminosilicate and ferro silicate silica rich zeotype materials and silico alumino phosphate microporous materials have been synthesized from the reaction mixture of colloidal silica sol, reactive aluminum, ferrous and phosphorous salts, and the essential organic templates at 373-473 K and were characterized by TG/DTA/DSC, X-ray diffraction, scanning electron microscopy and other analytical techniques. Crystallinity and unit cell parameters of the synthesized materials were found to be the function of Al and Fe content of zeolites. (author)

Patchy micelles based on coassembly of block copolymer chains and block copolymer brushes on silica particles.

Science.gov (United States)

Zhu, Shuzhe; Li, Zhan-Wei; Zhao, Hanying

2015-04-14

Patchy particles are a type of colloidal particles with one or more well-defined patches on the surfaces. The patchy particles with multiple compositions and functionalities have found wide applications from the fundamental studies to practical uses. In this research patchy micelles with thiol groups in the patches were prepared based on coassembly of free block copolymer chains and block copolymer brushes on silica particles. Thiol-terminated and cyanoisopropyl-capped polystyrene-block-poly(N-isopropylacrylamide) block copolymers (PS-b-PNIPAM-SH and PS-b-PNIPAM-CIP) were synthesized by reversible addition-fragmentation chain transfer polymerization and chemical modifications. Pyridyl disulfide-functionalized silica particles (SiO2-SS-Py) were prepared by four-step surface chemical reactions. PS-b-PNIPAM brushes on silica particles were prepared by thiol-disulfide exchange reaction between PS-b-PNIPAM-SH and SiO2-SS-Py. Surface micelles on silica particles were prepared by coassembly of PS-b-PNIPAM-CIP and block copolymer brushes. Upon cleavage of the surface micelles from silica particles, patchy micelles with thiol groups in the patches were obtained. Dynamic light scattering, transmission electron microscopy, and zeta-potential measurements demonstrate the preparation of patchy micelles. Gold nanoparticles can be anchored onto the patchy micelles through S-Au bonds, and asymmetric hybrid structures are formed. The thiol groups can be oxidized to disulfides, which results in directional assembly of the patchy micelles. The self-assembly behavior of the patchy micelles was studied experimentally and by computer simulation.

Synthesis of Polyurethane/Silica Modified Epoxy Polymer Based on 1,3-Propanediol for Coating Application

Directory of Open Access Journals (Sweden)

Lutviasari Nuraini

2017-11-01

Full Text Available Studies on the synthesis of polyurethane/silica modified epoxy polymer using 1,3-propanediol has been conducted. Synthesis of polymers made by reaction of tolonate and 1,3-propanediol (ratio NCO/OH=2.5 as the building blocks of polyurethane with diglycidyl ether bisphenol A (DGEBA epoxy and catalyst dibutyltin dilaurate (DBTL.The total weight of the polyurethane used was 20% (w/w of the total epoxy. Based on Fourier Transform Infrared (FTIR and 1H-Nuclear Magnetic Resonance (1H-NMR spectra indicated the existence of a new bond that is formed from the reaction of isocyanate group and hydroxyl group, where the hydroxyl groups derived from epoxy and 1,3-propanediol. The addition of silica (5, 10, and 15% w/w to epoxy into the epoxy-modified polyurethane has been carried out through sol-gel reaction of tetraethyl orthosilicate (TEOS. The isocyanate conversion rate for the addition of silica 5, 10, and 15% are 95.69; 100, and 100%, respectively. The morphology and element identification by Scanning Electron Microscopy/Energy Dispersive X-Ray Analysis (SEM/EDX, showed that Si element has been successfully added in the polymer. From the tensile strength and elongation analysis, also thermal stability analysis using Thermal Gravimetric Analyzer (TGA, the increase of silica amount into the polyurethane modified epoxy did not significantly affect to thermal properties, but decrease the tensile strength of the polymer.

Synthesis, characterization and antimicrobial studies of bio silica ...

Indian Academy of Sciences (India)

2018-05-16

May 16, 2018 ... Cynodon dactylon; green approach; silica nanoparticles; characterization; antimicrobial studies. 1. .... The obtained powder was well-ground with a mortar and ..... Inhalation of SiCl4 fumes irritates nose, throat and lungs.

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

Science.gov (United States)

Wang, Shengnan; Wang, David K.; Smart, Simon; Diniz da Costa, João C.

2015-01-01

A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification. PMID:26411484

Charge Transfer Mechanism in Titanium-Doped Microporous Silica for Photocatalytic Water-Splitting Applications

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Wendi Sapp

2016-02-01

Full Text Available Solar energy conversion into chemical form is possible using artificial means. One example of a highly-efficient fuel is solar energy used to split water into oxygen and hydrogen. Efficient photocatalytic water-splitting remains an open challenge for researchers across the globe. Despite significant progress, several aspects of the reaction, including the charge transfer mechanism, are not fully clear. Density functional theory combined with density matrix equations of motion were used to identify and characterize the charge transfer mechanism involved in the dissociation of water. A simulated porous silica substrate, using periodic boundary conditions, with Ti4+ ions embedded on the inner pore wall was found to contain electron and hole trap states that could facilitate a chemical reaction. A trap state was located within the silica substrate that lengthened relaxation time, which may favor a chemical reaction. A chemical reaction would have to occur within the window of photoexcitation; therefore, the existence of a trapping state may encourage a chemical reaction. This provides evidence that the silica substrate plays an integral part in the electron/hole dynamics of the system, leading to the conclusion that both components (photoactive materials and support of heterogeneous catalytic systems are important in optimization of catalytic efficiency.

Adsorption of benzyldimethylhexadecylammonium chloride at the hydrophobic silica-water interface studied by total internal reflection Raman spectroscopy: effects of silica surface properties and metal salt addition.

Science.gov (United States)

Grenoble, Zlata; Baldelli, Steven

2013-08-29

The adsorption of the cationic surfactant benzyldimethylhexadecylammonium (BDMHA(+)) chloride was studied at an octadecyltrichlorosilane (OTS)-monolayer-modified silica-water interface by Raman spectroscopy in total internal reflection (TIR) geometry. The present study demonstrates the capabilities of this spectroscopic technique to evaluate thermodynamic and kinetic BDMHA(+)Cl(-) adsorption properties at the hydrophobic silica surface. The surface coverage of BDMHA(+) decreased by 50% at the hydrophobic OTS-silica surface relative to the surface coverage on bare silica; the dominating driving mechanisms for surfactant adsorption were identified as hydrophobic effects and head group charge screening by the electrolyte counterions. Addition of magnesium metal salt (MgCl2) to the aqueous solution (∼ neutral pH) lowered the surface coverage and moderately increased the Langmuir adsorption constants relative to those of the pure surfactant. These trends were previously observed at the hydrophilic, negatively charged silica surface but with a smaller change in the Gibbs free energy of adsorption at the hydrophobic silica surface. The hydrophobic OTS-silica surface properties resulted in shorter times for the surfactant to reach steady-state adsorption conditions compared to the slow adsorption kinetics previously seen with the surfactant at the hydrophilic surface. Adsorption isotherms, based on Raman signal intensities from spectral analysis, were developed according to the Langmuir adsorption model for the pure surfactant at the OTS-silica-water interface; the modified Langmuir model was applied to the surfactant adsorption in the presence of 5, 10, 50, and 100 mM magnesium chloride. Spectral analysis of the Raman scattering intensities and geometric considerations suggests a hemimicelle-type surface aggregate as the most likely surfactant structure at the OTS-silica surface. The different kinetics observed at the hydrophilic versus the hydrophobic silica surface

Study of interaction in silica glass via model potential approach

Energy Technology Data Exchange (ETDEWEB)

Mann, Sarita, E-mail: saritaiitr2003@gmail.com [Department of Physics, Panjab University, Chandigarh-160014 (India); Rani, Pooja [D.A.V. College, Sec-10, Chandigarh-160010 (India)

2016-05-06

Silica is one of the most commonly encountered substances in daily life and in electronics industry. Crystalline SiO{sub 2} (in several forms: quartz, cristobalite, tridymite) is an important constituent of many minerals and gemstones, both in pure form and mixed with related oxides. Cohesive energy of amorphous SiO{sub 2} has been investigated via intermolecular potentials i.e weak Van der Waals interaction and Morse type short-range interaction. We suggest a simple atom-atom based Van der Waals as well as Morse potential to find cohesive energy of glass. It has been found that the study of silica structure using two different model potentials is significantly different. Van der Waals potential is too weak (P.E =0.142eV/molecule) to describe the interaction between silica molecules. Morse potential is a strong potential, earlier given for intramolecular bonding, but if applied for intermolecular bonding, it gives a value of P.E (=−21.92eV/molecule) to appropriately describe the structure of silica.

Studies of Immobilized Homogeneous Metal Catalysts on Silica Supports

Energy Technology Data Exchange (ETDEWEB)

Stanger, Keith James [Iowa State Univ., Ames, IA (United States)

2003-01-01

The tethered, chiral, chelating diphosphine rhodium complex, which catalyzes the enantioselective hydrogenation of methyl-α-acetamidocinnamate (MAC), has the illustrated structure as established by ³¹P NMR and IR studies. Spectral and catalytic investigations also suggest that the mechanism of action of the tethered complex is the same as that of the untethered complex in solution. The rhodium complexes, [Rh(COD)H]₄, [Rh(COD)₂]⁺BF₄^-, [Rh(COD)Cl]₂, and RhCl₃• 3H₂O, adsorbed on SiO₂ are optimally activated for toluene hydrogenation by pretreatment with H₂ at 200 C. The same complexes on Pd-SiO₂ are equally active without pretreatments. The active species in all cases is rhodium metal. The catalysts were characterized by XPS, TEM, DRIFTS, and mercury poisoning experiments. Rhodium on silica catalyzes the hydrogenation of fluorobenzene to produce predominantly fluorocyclohexane in heptane and 1,2-dichloroethane solvents. In heptane/methanol and heptane/water solvents, hydrodefluorination to benzene and subsequent hydrogenation to cyclohexane occurs exclusively. Benzene inhibits the hydrodefluorination of fluorobenzene. In DCE or heptane solvents, fluorocyclohexane reacts with hydrogen fluoride to form cyclohexene. Reaction conditions can be chosen to selectively yield fluorocyclohexane, cyclohexene, benzene, or cyclohexane. The oxorhenium(V) dithiolate catalyst [-S(CH₂)₃s-]Re(O)(Me)(PPh₃) was modified by linking it to a tether that could be attached to a silica support. Spectroscopic investigation and catalytic oxidation reactivity showed the heterogenized catalyst's structure and reactivity to be similar to its homogeneous analog. However, the immobilized catalyst offered additional advantages of recyclability, extended stability, and increased resistance to deactivation.

Optimization of o-phtaldialdehyde/2-mercaptoethanol postcolumn reaction for the hydrophilic interaction liquid chromatography determination of memantine utilizing a silica hydride stationary phase.

Science.gov (United States)

Douša, Michal; Pivoňková, Veronika; Sýkora, David

2016-08-01

A rapid procedure for the determination of memantine based on hydrophilic interaction chromatography with fluorescence detection was developed. Fluorescence detection after postcolumn derivatization with o-phtaldialdehyde/2-mercaptoethanol was performed at excitation and emission wavelengths of 345 and 450 nm, respectively. The postcolumn reaction conditions such as reaction temperature, derivatization reagent flow rate, and reagents concentration were studied due to steric hindrance of amino group of memantine. The derivatization reaction was applied for the hydrophilic interaction liquid chromatography method which was based on Cogent Silica-C stationary phase with a mobile phase consisting of a mixture of 10 mmol/L citric acid and 10 mmol/L o-phosphoric acid (pH 6.0) with acetonitrile using an isocratic composition of 2:8 v/v. The benefit of the reported approach consists in a simple sample pretreatment and a quick and sensitive hydrophilic interaction chromatography method. The developed method was validated in terms of linearity, accuracy, precision, and selectivity according to the International Conference on Harmonisation guidelines. The developed method was successfully applied for the analysis of commercial memantine tablets. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Exchange reaction between hydrogen and deuterium. I. Importance of surface reactions in the steady-state mechanism

Energy Technology Data Exchange (ETDEWEB)

Marteau, C; Gaillard-Cusin, F; James, H [Centre National de la Recherche Scientifique, 45 - Orleans-la-Source (France). Centre de Recherches sur la Chimie de Combustion et des Hautes Temperatures

1978-05-01

Investigation of heterogeneous initiation process of gas phase linear chain reactions is carried out through the study of H/sub 2/-D/sub 2/ exchange reaction. Experimental data under study concern mainly the stationary rate of HD formation and the prestationary proceeding. Steady-state method accounts for the first one of these data; it allows to clearly compare the wall process part to the part played by the homogeneous chain reaction towards HD formation. Activation energy of exchange elementary step between chemisorbed hydrogen (on silica) and gaseous deuterium has been evaluated: Esub(e1)=52+-1 Kcal/mole.

Preparation and Physicochemical Properties of Functionalized Silica/Octamethacryl-Silsesquioxane Hybrid Systems

Directory of Open Access Journals (Sweden)

Karolina Szwarc-Rzepka

2013-01-01

Full Text Available Alkoxysilane-grafted silica/polyhedral oligomeric silsesquioxane with methacryl substituents (SiO2/silane/POSS hybrid material was synthesized according to hydrolyzation and condensation reactions in the so-called “bifunctionalization process.” It is a new attractive system because of its physicochemical, especially thermal and structural, properties. This innovative method of preparation as well as specific physicochemical and useful properties determine the potential applications of such products in many industries. The structure and physicochemical parameters of obtained hybrid systems were characterized using infrared spectroscopy (FTIR, 13C and 29Si solid-state nuclear magnetic resonance (CP MAS NMR, and thermal analysis. The mechanism of bifunctionalization reaction was proposed. The chemical immobilization of silane coupling agent and Methacryl POSS onto silica support surface was noted during the study. Those changes caused a significant increase in the hydrophobic character of fillers obtained. Moreover, changes in thermal stability of SiO2/silane/POSS hybrid systems in comparison to pure POSS modifier were also observed.

Multimodality Imaging with Silica-Based Targeted Nanoparticle Platforms

International Nuclear Information System (INIS)

Lewis, Jason S.

2012-01-01

Objectives: To synthesize and characterize a C-Dot silica-based nanoparticle containing 'clickable' groups for the subsequent attachment of targeting moieties (e.g., peptides) and multiple contrast agents (e.g., radionuclides with high specific activity) (1,2). These new constructs will be tested in suitable tumor models in vitro and in vivo to ensure maintenance of target-specificity and high specific activity. Methods: Cy5 dye molecules are cross-linked to a silica precursor which is reacted to form a dye-rich core particle. This core is then encapsulated in a layer of pure silica to create the core-shell C-Dot (Figure 1) (2). A 'click' chemistry approach has been used to functionalize the silica shell with radionuclides conferring high contrast and specific activity (e.g. 64Cu and 89Zr) and peptides for tumor targeting (e.g. cRGD and octreotate) (3). Based on the selective Diels-Alder reaction between tetrazine and norbornene, the reaction is bioorthogonal, highyielding, rapid, and water-compatible. This radiolabeling approach has already been employed successfully with both short peptides (e.g. octreotate) and antibodies (e.g. trastuzumab) as model systems for the ultimate labeling of the nanoparticles (1). Results: PEGylated C-Dots with a Cy5 core and labeled with tetrazine have been synthesized (d = 55 nm, zeta potential = -3 mV) reliably and reproducibly and have been shown to be stable under physiological conditions for up to 1 month. Characterization of the nanoparticles revealed that the immobilized Cy5 dye within the C-Dots exhibited fluorescence intensities over twice that of the fluorophore alone. The nanoparticles were successfully radiolabeled with Cu-64. Efforts toward the conjugation of targeting peptides (e.g. cRGD) are underway. In vitro stability, specificity, and uptake studies as well as in vivo imaging and biodistribution investigations will be presented. Conclusions: C-Dot silica-based nanoparticles offer a robust, versatile, and multi

Bioconjugated fluorescent silica nanoparticles for the rapid detection of Entamoeba histolytica.

Science.gov (United States)

Hemadi, Ahmad; Ekrami, Alireza; Oormazdi, Hormozd; Meamar, Ahmad Reza; Akhlaghi, Lame; Samarbaf-Zadeh, Ali Reza; Razmjou, Elham

2015-05-01

Rapid detection of Entamoeba histolytica based on fluorescent silica nanoparticle (FSNP) indirect immunofluorescence microscopy was evaluated. Silica nanoparticles were synthesized using Stöber's method, with their surface activated to covalently bind to, and immobilize, protein A. For biolabeling, FSNP was added to conjugated E. histolytica trophozoites with monoclonal anti-E. histolytica IgG1 for microscopic observation of fluorescence. Fluorescent silica nanoparticle sensitivity was determined with axenically cultured E. histolytica serially diluted to seven concentrations. Specificity was evaluated using other intestinal protozoa. Fluorescent silica nanoparticles detected E. histolytica at the lowest tested concentration with no cross-reaction with Entamoeba dispar, Entamoeba moshkovskii, Blastocystis sp., or Giardia lamblia. Visualization of E. histolytica trophozoites with anti-E. histolytica antibody labeled with fluorescein isothiocyanate (FITC) was compared with that using anti-E. histolytica antibody bioconjugated FSNP. Although FITC and FSNP produced similar results, the amount of specific antibody required for FITC to induce fluorescence of similar intensity was fivefold that for FSNP. Fluorescent silica nanoparticles delivered a rapid, simple, cost-effective, and highly sensitive and specific method of detecting E. histolytica. Further study is needed before introducing FSNP for laboratory diagnosis of amoebiasis. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and Characterization of Hybrid Nanocomposite of Polyacrylamide/Silica-Nanoparticles

Directory of Open Access Journals (Sweden)

Ahmad Rabiee

2013-01-01

Full Text Available Polyacrylamides are water soluble macromolecules. These polymers are widely used for flocculation, separation and treatment of solid-liquid phase materials. In this research, organic-inorganic hybrid of polyacrylamide/silica nanoparticle is prepared via radical polymerization. First, the silica nanoparticle surfaces were modified by 3-methacryloxypropyltrimethoxysilane as coupling agent using a sol-gel technique in aqueous media in acidic condition. Afterwards, the modified nanoparticles are copolymerized by acrylamide monomer in presence of a peroxide initiator during a free radical polymerization. The chemical structure of the prepared modified nano-silica as well as polyacrylamide nanocomposite was studied and confirmed by FTIR spectroscopy technique. The morphology of nanocomposite was investigated by scanning electron microscopy. The SEM micrograph showed that the surface of the composite did not display any phase separation. Nanoparticles distribution was investigated by SEM-EDX technique. The results showed a uniform distribution of particles throughout the polymer bulk. TEM analysis showed the presence of silica nanoparticles in bulk of polymer which is an indicative of suitable dispersion of nanoparticles. The thermal stability of hybrid nanocomosite with that of polyacrylamide was compared by TGA technique. The higher thermal stability of hybrid nanocomposite with respect to homopolymer is indicative of a reaction between the modified nanoparticles and polyacrylamide chain. The presence of silica particles in copolymer was also confirmed with EDX analysis in ash content of hybrid nanocomposite.

Synthesis of silicon carbide by carbothermal reduction of silica

International Nuclear Information System (INIS)

Abel, Joao Luis

2009-01-01

The production of silicon carbide (SiC) in an industrial scale still by carbothermal reduction of silica. This study aims to identify, in a comparative way, among the common reducers like petroleum coke, carbon black, charcoal and graphite the carbothermal reduction of silica from the peat. It is shown, that the peat, also occurs in nature together with high purity silica sand deposits, where the proximity of raw materials and their quality are key elements that determine the type, purity and cost of production of SiC. Tests were running from samples produced in the electric resistance furnace with controlled atmosphere at temperatures of 1550 degree C, 1600 degree C and 1650 degree C, both the precursors and products of reaction of carbothermal reduction were characterized by applying techniques of X-ray diffraction, scanning electron microscopy (SEM) and Energy-Dispersive X-ray analysis Spectroscopy (EDS). The results showed the formation of SiC for all common reducers, as well as for peat, but it was not possible to realize clearly the difference between them, being necessary, specific tests. (author)

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.

Understanding the Hydro-metathesis Reaction of 1-decene by Using Well-defined Silica Supported W, Mo, Ta Carbene/Carbyne Complexes

KAUST Repository

Saidi, Aya

2017-12-21

Direct conversion of 1-decene to petroleum range alkanes was obtained using hydro-metathesis reaction. To understand this reaction we employed three different well-defined single site catalysts precursors; [(≡Si-O-)W(CH3)5] 1, [(≡Si-O-)Mo(≡CtBu)(CH2tBu)2] 2 and [(≡Si-O)Ta(=CHtBu)(CH2tBu)2] 3. We witnessed that in our conditions olefin metathesis/isomerization of 1-decene occurs much faster followed by reduction of the newly formed olefins rather than reduction of the 1-decene to decane, followed by metathesis of decane. We found that Mo-based catalyst favors 2+2 cycloaddition of 1-decene forming metallocarbene, followed by reduction of the newly formed olefins to alkanes. However, in the case of W and Ta-based catalysts, a rapid isomerization (migration) of the double bond followed by olefin metathesis and reduction of the newly formed olefins were observed. We witnessed that silica supported W catalyst precursor 1 and Mo catalyst precursor 2 are better catalysts for hydro-metathesis reaction with TONs of 818 and 808 than Ta-based catalyst 3 (TON of 334). This comparison of the catalysts provides us a better understanding that, if a catalyst is efficient in olefin metathesis reaction it would be a better catalyst for hydro-metathesis reaction.

Removal mechanism of tritium by variously pretreated silica gel

International Nuclear Information System (INIS)

Nakashima, M.; Tachikawa, E.; Saeki, M.; Aratono, Y.

1981-01-01

Removal mechanisms of HTO from variously pretreated and non-pretreated silica gel columns were investigated with pulse-loading with tritiated water vapor. With non-pretreated silica gel, the HTO physisorbed on the upper part of the column comes into contact with surface hydroxyl groups while passing downward the column, so that in each equilibration a part of the tritium is incorporated into hydroxyl groups by H/T isotopic exchange reactions. With the silica gel pretreated at a temperature below 400 0 C, most of tritium in the applied HTO is easily incorporated into surface hydroxyl groups in the upper part of the column either by H/T isotopic exchange reactions or by rehydration of the dehydrated surface (siloxyl linkage). In the pretreatment above 400 0 C, essentially all the tritium is trapped by siloxyl groups of various stabilities. The ease of rehydration of siloxyl groups by applied HTO depends on their stabilities, which, in turn, depend on the pretreatment temperature. As a general trend, treatment at higher temperature promotes annealing of the constrained siloxyl groups and thus the rate of rehydration becomes slower. (author)

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.

Preparation of Silica Nanoparticles and Its Beneficial Role in Cementitious Materials

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S. Ahalawat

2011-07-01

Full Text Available Spherical silica nanoparticles (n‐SiO2 with controllable size have been synthesized using tetraethoxysilane as starting material and ethanol as solvent by sol‐gel method. Morphology and size of the particles was controlled through surfactants. Sorbitan monolaurate, sorbitain monopalmitate and sorbitain monostearate produced silica nanoparticles of varying sizes (80‐150 nm, indicating the effect of chain length of the surfactant. Increase in chain length of non‐ionic surfactant resulted in decreasing particle size of silica nanoparticles. Further, the size of silica particles was also controlled using NH3 as base catalyst. These silica nanoparticles were incorporated into cement paste and their role in accelerating the cementitious reactions was investigated. Addition of silica nanoparticles into cement paste improved the microstructure of the paste and calcium leaching is significantly reduced as n‐SiO2 reacts with calcium hydroxide and form additional calcium‐ silicate‐hydrate (C‐S‐H gel. It was found that calcium hydroxide content in silica nanoparticles incorporated cement paste reduced ~89% at 1 day and up to ~60% at 28 days of hydration process. Synthesized silica particles and cement paste samples were characterized using scanning electron microscopy (SEM, powder X‐ray diffraction (XRD, infrared spectroscopy (IR and thermogravimetric analysis (TGA.

Characterisation of silica nanoparticles prior to in vitro studies: from primary particles to agglomerates

International Nuclear Information System (INIS)

Orts-Gil, Guillermo; Natte, Kishore; Drescher, Daniela; Bresch, Harald; Mantion, Alexandre; Kneipp, Janina; Österle, Werner

2011-01-01

The size, surface charge and agglomeration state of nanoparticles under physiological conditions are fundamental parameters to be determined prior to their application in toxicological studies. Although silica-based materials are among the most promising candidates for biomedical applications, more systematic studies concerning the characterisation before performing toxicological studies are necessary. This interest is based on the necessity to elucidate the mechanisms affecting its toxicity. We present here TEM, SAXS and SMPS as a combination of methods allowing an accurate determination of single nanoparticle sizes. For the commercial material, Ludox TM50 single particle sizes around 30 nm were found in solution. DLS measurements of single particles are rather affected by polydispersity and particles concentration but this technique is useful to monitor their agglomeration state. Here, the influence of nanoparticle concentration, ionic strength (IS), pH and bath sonication on the agglomeration behaviour of silica particles in solution has been systematically investigated. Moreover, the colloidal stability of silica particles in the presence of BSA has been investigated showing a correlation between silica and protein concentrations and the formation of agglomerates. Finally, the colloidal stability of silica particles in standard cell culture medium has been tested, concluding the necessity of surface modification in order to preserve silica as primary particles in the presence of serum. The results presented here have major implications on toxicity investigations because silica agglomeration will change the probability and uptake mechanisms and thereby may affect toxicity.

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.

Effect of support on hydro-metathesis of propene: A comparative study of W(CH 3 ) 6 anchored to silica vs. silica-alumina

KAUST Repository

Tretiakov, Mykyta; Samantaray, Manoja; Saidi, Aya; Basset, Jean-Marie

2018-01-01

Hydro-metathesis of propene was carried out by using well-defined W(CH3)6 supported on silica and silica-alumina. It was observed that W(CH3)6 supported silica-alumina catalyst is much better (TON 4577) than the silica supported catalyst (TON 2104

Water Contact Angle Dependence with Hydroxyl Functional Groups on Silica Surfaces under CO2 Sequestration Conditions.

Science.gov (United States)

Chen, Cong; Zhang, Ning; Li, Weizhong; Song, Yongchen

2015-12-15

Functional groups on silica surfaces under CO2 sequestration conditions are complex due to reactions among supercritical CO2, brine and silica. Molecular dynamics simulations have been performed to investigate the effects of hydroxyl functional groups on wettability. It has been found that wettability shows a strong dependence on functional groups on silica surfaces: silanol number density, space distribution, and deprotonation/protonation degree. For neutral silica surfaces with crystalline structure (Q(3), Q(3)/Q(4), Q(4)), as silanol number density decreases, contact angle increases from 33.5° to 146.7° at 10.5 MPa and 318 K. When Q(3) surface changes to an amorphous structure, water contact angle increases 20°. Water contact angle decreases about 12° when 9% of silanol groups on Q(3) surface are deprotonated. When the deprotonation degree increases to 50%, water contact angle decreases to 0. The dependence of wettability on silica surface functional groups was used to analyze contact angle measurement ambiguity in literature. The composition of silica surfaces is complicated under CO2 sequestration conditions, the results found in this study may help to better understand wettability of CO2/brine/silica system.

Stellate macroporous silica nanospheres in bio-macromolecules encapsulation and delivery

Science.gov (United States)

Chi, Hao-Hsin

This project focused on using mesoporous silica as a solid support to encapsulate enzymes for operating a highly economic, and recyclable biomass processing system. The main objective is to turn non-food biomass sources into food products. Enzymes are macromolecules with the structural backbone of proteins or ribonucleic acid sequences (RNAs) which work as catalysts in living organisms. Enzymes have the advantage of being the least contaminating catalyst due to normal catalyst might generate toxic by-product, and preferable to organic and inorganic catalysts, especially when used for product related to human used, which require biocompatibility of final product. However, there are several disadvantages in enzyme utilization. Their fabrication is time-consuming and requires elaborated molecular biology processes. Most of the enzymes need well-defined reaction conditions to be functional and operate at high yield. Unfortunately, although they are reusable as normal catalysts, it proves difficult to extract or reuse the enzymes from a reaction. Also, enzyme molecules are easily degradable and demand proper storage. To overcome some of the disadvantages, especially regarding stability to degradation, recovery, and reusability, immobilization of enzyme on solid support has become a thriving methodology. In recent years, mesoporous silica nanomaterials(MSN) have been at the forefront of enzyme immobilization given their extensive surface area, which provides capability to increase enzyme loading and for their demonstrate ability to protect enzyme from degradation, thus enabling high recyclability. Mesoporous silica is biocompatible and has already been used for several applications included. Catalysis, drug delivery, and Bio-imaging. Previously published research utilized mesoporous silica to deliver drugs, DNAs, RNAs or encapsulate single enzyme. The objective of this research is completed to develop a new porous silica platform that is unique in its porosity structure

Silica-Immobilized Enzyme Reactors; Application to Cholinesterase-Inhibition Studies

National Research Council Canada - National Science Library

Luckarift, Heather R; Johnson, Glenn R; Spain, Jim C

2006-01-01

...) using silica-encapsulated equine butyrycholinestearse (BuChE) as a model system. Peptide-mediated silica formation was used to encapsulate BuChE, directly immobilizing the enzyme within a commercial pre-packed column...

Formation of quartz veins by local dissolution and transport of silica

Energy Technology Data Exchange (ETDEWEB)

Wangen, Magnus; Munz, Ingrid Anne

2004-08-01

A simple model is proposed for the (often) thick quartz veins observed in the Modum Complex in Southern Norway. The formation of these veins cannot easily be explained by silica imported by hot ascending fluids. The proposed model has dissolution in the host rock adjacent to the veins as the source for silica. The suggested process for vein formation is represented by a reaction-diffusion equation, and the process is studied in terms of a Damkoehler number. Estimates for the growth rate of quartz cement are derived. The estimates for the growth rate can be used to constrain poorly known parameters of the vein formation process, like for instance, the degree of supersaturation in the host rock. (Author)

Reduction and aggregation of silver in aqueous gelatin and silica suspensions

International Nuclear Information System (INIS)

Kapoor, S.; Lawless, D.; Kennepohl, P.; Meisel, D.; Serpone, N.

1994-01-01

The investigation of silver reduction and aggregation processes are of specific interest to the photographic industry, which relies heavily on photochemical equivalents of these reactions. Mechanistic insights into the formation of small silver clusters in aqueous solution have been obtained from both pulse and γ-radiolytic studies. This paper examines the reduction of silver ions and the subsequent formation of silver clusters in aqueous gelatin solutions and on colloidal silica particles using the pulse radiolysis technique. The aggregation processes are compared with the parallel reactions in aqueous solutions

Thermodynamics of the silica-steam system

Energy Technology Data Exchange (ETDEWEB)

Krikorian, Oscar H [Lawrence Radiation Laboratory, University of California, Livermore, CA (United States)

1970-05-01

In most nuclear cratering and cavity formation applications, the working fluid in the expanding cavity consists primarily of vaporized silica and steam. The chemical reaction products of silica and steam under these conditions are not known, although it is known that silica is very volatile in the presence of high-pressure steam under certain geologic conditions and in steam turbines. A review is made of work on the silica-steam system in an attempt to determine the vapor species that exist, and to establish the associated thermo-dynamic data. The review indicates that at 600-900 deg K and 1-100 atm steam pressure, Si(OH){sub 4} is the most likely silicon-containing gaseous species. At 600-900 deg. K and 100-1000 atm steam, Si{sub 2}O(OH){sub 6} is believed to predominate, whereas at 1350 deg K and 2000-9000 atm, a mixture of Si(OH){sub 4} and Si{sub 2}O(OH){sub 6} is consistent with the observed volatilities. In work at 1760 deg. K in which silica was reacted either with steam at 0.5 and 1 atm, or with gaseous mixtures of H{sub 2}/H{sub 2}O and O{sub 2}/H{sub 2}O at 1 atm total pressure, only part of the volatility could be accounted for by Si(OH){sub 4}. Hydrogen was found to greatly enhance the volatility of silica, and oxygen to suppress it. The species most likely to explain this behavior is believed to be SiO(OH). A number of other species may also be significant under these conditions. Thermodynamic data have been estimated for all species considered. The Si-OH bond dissociation energy is found to be {approx}117 kcal/mole in both Si(OH){sub 4} and Si{sub 2}O(OH){sub 6}. (author)

Dedolomitization and Alkali Reactions in Ohio-sourced Dolstone Aggregates

Science.gov (United States)

2017-11-01

Concrete samples produced using NW-Ohio sourced aggregates were evaluated for susceptibility to degradation and premature failure due to cracks formed by the volume expansion during hydration of silica gels produced by alkali-silica reactions between...

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

Directory of Open Access Journals (Sweden)

F. Alrouh

2017-02-01

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

STUDY ON SILICA INFUSED RECYCLED AGGREGATE CONCRETE USING DESIGN OF EXPERIMENTS

Directory of Open Access Journals (Sweden)

P. M. MRUDUL

2017-04-01

Full Text Available Recycled Aggregate (RA generated from the construction industry is used as a material for sustainable construction. The old mortar attached to these aggregates makes it porous and are generally used for low-grade applications. However, by infusing with silica fumes, the properties of recycled aggregate concrete (RAC can be improved, as the silica fumes get infused into the pores of old mortar attached to it. In this study, the optimum percentage of recycled aggregate that can be used in fresh concrete for higher grade applications was found out. Design of experiments (DoE was used to optimize percentage of silica fumes and recycled aggregate to achieve optimum properties of concrete. Equations to predict the properties of concrete were also modelled using regression analysis.

Effect of colloidal nano-silica on the mechanical and physical behaviour of waste-glass cement mortar

International Nuclear Information System (INIS)

Aly, M.; Hashmi, M.S.J.; Olabi, A.G.; Messeiry, M.; Abadir, E.F.; Hussain, A.I.

2012-01-01

Highlights: → Glass powder (GP) and nano-silica (CS) were used as a partial cement replacement in cement mortar (CM). → No damaging effect can be detected due to the reaction between GP and CM with particle size up to 75 μm. → Hybrid combination of GP/CS greatly improved mechanical properties and microstructure of CM. -- Abstract: This paper presents a laboratory study of the properties of colloidal nano-silica (CS)/waste glass cement composites. The microstructure, alkali-silica reaction (ASR), and the mechanical properties of cement mortars containing waste glass powder (WG) as a cement replacement with and without CS are investigated and compared with plain mortar. In addition, the hydration of cement compounds was followed by differential thermal analysis (DTA), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). The results show that incorporation of WG has a positive effect on the mechanical properties of cement mortars especially when CS is presented. In addition, the DTA/TGA results and XRD analysis show a reduction in the calcium hydroxide (CH) content in mortars with both WG and a hybrid combination of WG and CS. This confirms the improvement of mechanical properties and the occurrence of the pozzolanic reaction after 28 days of hydration.

PVP-Stabilized Palladium Nanoparticles in Silica as Effective Catalysts for Hydrogenation Reactions

Directory of Open Access Journals (Sweden)

Caroline Pires Ruas

2013-01-01

Full Text Available Palladium nanoparticles stabilized by poly (N-vinyl-2-pyrrolidone (PVP can be synthesized by corresponding Pd(acac2 (acac = acetylacetonate as precursor in methanol at 80°C for 2 h followed by reduction with NaBH4 and immobilized onto SiO2 prepared by sol-gel process under acidic conditions (HF or HCl. The PVP/Pd molar ratio is set to 6. The effect of the sol-gel catalyst on the silica morphology and texture and on Pd(0 content was investigated. The catalysts prepared (ca. 2% Pd(0/SiO2/HF and ca. 0,3% Pd(0/SiO2/HCl were characterized by TEM, FAAS, and SEM-EDS. Palladium nanoparticles supported in silica with a size 6.6 ± 1.4 nm were obtained. The catalytic activity was tested in hydrogenation of alkenes.

Sensing behavior study of silica-coated Ag nanoparticles deposited on glassy carbon toward nitrobenzene

Energy Technology Data Exchange (ETDEWEB)

Devi, Pooja; Reddy, Pramod [CSIR, Sector-30C, Central Scientific Instruments Organization (India); Arora, Swati [Shri Mata Vaishno Devi University (India); Singh, Suman; Ghanshyam, C.; Singla, M. L., E-mail: singla_min@yahoo.co.in [CSIR, Sector-30C, Central Scientific Instruments Organization (India)

2012-10-15

In this study, we report the synthesis and characterization of silica-coated silver core/shell nanostructures (NSs) and their sensing behavior when deposited on glassy carbon (GC) electrode for nitrobenzene (NB) detection. Synthesized silica-coated silver core/shell NSs were characterized for their chemical, structural and morphological properties. TEM analysis confirmed that the silica-coated silver nanoparticles (size {approx}200 nm) are spherical in shape and the core diameter is {approx}38 nm. FT-IR spectra also confirmed the coating of silica on the surface of silver nanoparticles. Cyclic voltammetry studies of NB with silica-coated silver core-shell nanoparticles-modified GC electrodes revealed two cathodic peaks at -0.74 V (C{sub 1}) and -0.34 V (C{sub 2}) along with two anodic peaks at -0.64 V (A{sub 1}) and -0.2 V (A{sub 2}). Enhanced cathodic peak current (C{sub 1}, I{sub P}) of the core-shell NSs-modified electrode is observed relative to bare and silica-modified electrodes. Amperometric studies revealed a very high current sensitivity (114 nA/nM) and linearly dependent reduction current with NB amount in the low concentration range and a detection limit of 25 nM. Moreover, the core-shell NSs-modified electrode showed good reproducibility and selectivity toward NB in the presence of many cationic, anionic, and organic interferents.

Sensing behavior study of silica-coated Ag nanoparticles deposited on glassy carbon toward nitrobenzene

International Nuclear Information System (INIS)

Devi, Pooja; Reddy, Pramod; Arora, Swati; Singh, Suman; Ghanshyam, C.; Singla, M. L.

2012-01-01

In this study, we report the synthesis and characterization of silica-coated silver core/shell nanostructures (NSs) and their sensing behavior when deposited on glassy carbon (GC) electrode for nitrobenzene (NB) detection. Synthesized silica-coated silver core/shell NSs were characterized for their chemical, structural and morphological properties. TEM analysis confirmed that the silica-coated silver nanoparticles (size ∼200 nm) are spherical in shape and the core diameter is ∼38 nm. FT-IR spectra also confirmed the coating of silica on the surface of silver nanoparticles. Cyclic voltammetry studies of NB with silica-coated silver core–shell nanoparticles-modified GC electrodes revealed two cathodic peaks at −0.74 V (C 1 ) and −0.34 V (C 2 ) along with two anodic peaks at −0.64 V (A 1 ) and −0.2 V (A 2 ). Enhanced cathodic peak current (C 1 , I P ) of the core–shell NSs-modified electrode is observed relative to bare and silica-modified electrodes. Amperometric studies revealed a very high current sensitivity (114 nA/nM) and linearly dependent reduction current with NB amount in the low concentration range and a detection limit of 25 nM. Moreover, the core–shell NSs-modified electrode showed good reproducibility and selectivity toward NB in the presence of many cationic, anionic, and organic interferents.

A new surface catalytic model for silica-based thermal protection material for hypersonic vehicles

Directory of Open Access Journals (Sweden)

Li Kai

2015-10-01

Full Text Available Silica-based materials are widely employed in the thermal protection system for hypersonic vehicles, and the investigation of their catalytic characteristics is crucially important for accurate aerothermal heating prediction. By analyzing the disadvantages of Norman’s high and low temperature models, this paper combines the two models and proposes an eight-reaction combined surface catalytic model to describe the catalysis between oxygen and silica surface. Given proper evaluation of the parameters according to many references, the recombination coefficient obtained shows good agreement with experimental data. The catalytic mechanisms between oxygen and silica surface are then analyzed. Results show that with the increase of the wall temperature, the dominant reaction contributing to catalytic coefficient varies from Langmuir–Hinshelwood (LH recombination (TW  1350 K. The surface coverage of chemisorption areas varies evidently with the dominant reactions in the high temperature (HT range, while the surface coverage of physisorption areas varies within quite low temperature (LT range (TW < 250 K. Recommended evaluation of partial parameters is also given.

Tunable pores in mesoporous silica films studied using a pulsed slow positron beam

International Nuclear Information System (INIS)

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

2007-01-01

Positron annihilation lifetime spectroscopy (PALS) based on a pulsed slow positron beam was applied to study mesoporous silica films, synthesized using amphiphilic PEO-PPO-PEO triblock copolymers as structure-directing agents. The pore size depends on the loading of different templates. Larger pores were formed in silica films templated by copolymers with higher molecular-weights. Using 2-dimensional PALS, open porosity of silica films was also found to be influenced by the molecular-weight as well as the ratio of hydrophobic PPO moiety of the templates

Antidegradation and reinforcement effects of phenyltrimethoxysilane- or N-[3-(trimethoxysilyl)propyl]aniline-modified silica particles in natural rubber composites

Energy Technology Data Exchange (ETDEWEB)

Tunlert, Apinya [Program in Petrochemistry and Polymer Science, Chulalongkorn University, Bangkok 10330 (Thailand); Prasassarakich, Pattarapan [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Poompradub, Sirilux, E-mail: sirilux.p@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Center for Petroleum, Petrochemical and Advanced Material, Chulalongkorn University Bangkok 10330 (Thailand)

2016-04-15

The modification of silica particles with phenyltrimethoxysilane or N-[3-(trimethoxysilyl)propyl]aniline via a sol–gel reaction was performed in order to improve the dispersion of silica and antidegradation in natural rubber (NR). The functional groups on the modified silica surface were characterized by Fourier transform infrared spectroscopy, while the morphology was evaluated by scanning and transmission electron microscopy. The surface properties and antioxidant activity of the modified silica particles were determined by the water contact angle and 2, 2-diphenyl-1-picrylhydrazyl assay, respectively. The modified silica particles exhibited a higher hydrophobicity and a decreased interfacial adhesion energy compared with the unmodified silica particles. The modified silica particles were then incorporated into NR. The better dispersion of the modified silica particles than the unmodified ones in the NR matrix resulted in improved mechanical properties in terms of the modulus at 300% elongation (2.9 ± 0.02 MPa), hardness (52.5 ± 0.2 Shore A), abrasion resistance (241 ± 8 mm{sup 3}) and compression set (20.2 ± 0.6%). In addition, the inclusion of the modified silica particles in the NR matrix gave a high initial temperature of decomposition and retarded the ozone-induced degradation compared with the NR filled with unmodified silica particles. - Highlights: • Silica was surface modified with PhTMS or ATMS via a sol–gel reaction. • Modified silica showed a decreased interfacial adhesion energy. • Modified silica showed an enhanced free radical scavenging activity. • Modified silica improved the mechanical properties, thermal stability and ozone resistance in NR vulcanizates.

Microscopy and Cathodoluminescence Spectroscopy Characterization of Quartz Exhibiting Different Alkali-Silica Reaction Potential.

Science.gov (United States)

Kuchařová, Aneta; Götze, Jens; Šachlová, Šárka; Pertold, Zdeněk; Přikryl, Richard

2016-02-01

Different quartz types from several localities in the Czech Republic and Sweden were examined by polarizing microscopy combined with cathodoluminescence (CL) microscopy, spectroscopy, and petrographic image analysis, and tested by use of an accelerated mortar bar test (following ASTM C1260). The highest alkali-silica reaction potential was indicated by very fine-grained chert, containing significant amounts of fine-grained to cryptocrystalline matrix. The chert exhibited a dark red CL emission band at ~640 nm with a low intensity. Fine-grained orthoquartzites, as well as fine-grained metamorphic vein quartz, separated from phyllite exhibited medium expansion values. The orthoquartzites showed various CL of quartz grains, from blue through violet, red, and brown. Two CL spectral bands at ~450 and ~630 nm, with various intensities, were detected. The quartz from phyllite displayed an inhomogeneous dark red CL with two CL spectral bands of low intensities at ~460 and ~640 nm. The massive coarse-grained pegmatite quartz from pegmatite was assessed to be nonreactive and displayed a typical short-lived blue CL (~480 nm). The higher reactivity of the fine-grained hydrothermal quartz may be connected with high concentrations of defect centers, and probably with amorphized micro-regions in the quartz, respectively; indicated by a yellow CL emission (~570 nm).

Perhydropolysilazane derived silica coating protecting Kapton from atomic oxygen attack

Energy Technology Data Exchange (ETDEWEB)

Hu Longfei [China Academy of Aerospace Aerodynamics, Beijing 100074 (China); Li Meishuan, E-mail: mshli@imr.ac.cn [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Xu Caihong; Luo Yongming [Institute of Chemistry, Chinese Academy of Sciences, Beijing 100080 (China)

2011-11-30

By using surface sol-gel method with perhydropolysilazane (PHPS) as a precursor, a silica coating was prepared on a Kapton substrate as an atomic oxygen (AO) protective coating. The AO exposure tests were conducted in a ground-based simulator. It is found that the erosion yield of Kapton decreases by about three orders of magnitude after the superficial application of the coating. After AO exposure, the surface of the coating is smooth and uniform, no surface shrinkage induced cracks or undercutting erosion are observed. This is because that during AO exposure the PHPS is oxidized directly to form SiO{sub 2} without through intermediate reaction processes, the surface shrinkage and cracking tendency are prohibited. Meanwhile, this PHPS derived silica coating also presents self-healing effect due to the oxidation of free Si. Compared with other kinds of silica or organic polymer coatings, this PHPS derived silica coating exhibits a superior AO erosion resistance.

Perhydropolysilazane derived silica coating protecting Kapton from atomic oxygen attack

International Nuclear Information System (INIS)

Hu Longfei; Li Meishuan; Xu Caihong; Luo Yongming

2011-01-01

By using surface sol–gel method with perhydropolysilazane (PHPS) as a precursor, a silica coating was prepared on a Kapton substrate as an atomic oxygen (AO) protective coating. The AO exposure tests were conducted in a ground-based simulator. It is found that the erosion yield of Kapton decreases by about three orders of magnitude after the superficial application of the coating. After AO exposure, the surface of the coating is smooth and uniform, no surface shrinkage induced cracks or undercutting erosion are observed. This is because that during AO exposure the PHPS is oxidized directly to form SiO 2 without through intermediate reaction processes, the surface shrinkage and cracking tendency are prohibited. Meanwhile, this PHPS derived silica coating also presents self-healing effect due to the oxidation of free Si. Compared with other kinds of silica or organic polymer coatings, this PHPS derived silica coating exhibits a superior AO erosion resistance.

Multimodality Imaging with Silica-Based Targeted Nanoparticle Platforms

Energy Technology Data Exchange (ETDEWEB)

Jason S. Lewis

2012-04-09

Objectives: To synthesize and characterize a C-Dot silica-based nanoparticle containing 'clickable' groups for the subsequent attachment of targeting moieties (e.g., peptides) and multiple contrast agents (e.g., radionuclides with high specific activity) [1,2]. These new constructs will be tested in suitable tumor models in vitro and in vivo to ensure maintenance of target-specificity and high specific activity. Methods: Cy5 dye molecules are cross-linked to a silica precursor which is reacted to form a dye-rich core particle. This core is then encapsulated in a layer of pure silica to create the core-shell C-Dot (Figure 1) [2]. A 'click' chemistry approach has been used to functionalize the silica shell with radionuclides conferring high contrast and specific activity (e.g. 64Cu and 89Zr) and peptides for tumor targeting (e.g. cRGD and octreotate) [3]. Based on the selective Diels-Alder reaction between tetrazine and norbornene, the reaction is bioorthogonal, highyielding, rapid, and water-compatible. This radiolabeling approach has already been employed successfully with both short peptides (e.g. octreotate) and antibodies (e.g. trastuzumab) as model systems for the ultimate labeling of the nanoparticles [1]. Results: PEGylated C-Dots with a Cy5 core and labeled with tetrazine have been synthesized (d = 55 nm, zeta potential = -3 mV) reliably and reproducibly and have been shown to be stable under physiological conditions for up to 1 month. Characterization of the nanoparticles revealed that the immobilized Cy5 dye within the C-Dots exhibited fluorescence intensities over twice that of the fluorophore alone. The nanoparticles were successfully radiolabeled with Cu-64. Efforts toward the conjugation of targeting peptides (e.g. cRGD) are underway. In vitro stability, specificity, and uptake studies as well as in vivo imaging and biodistribution investigations will be presented. Conclusions: C-Dot silica-based nanoparticles offer a robust

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.

Histological and histomorphometrical analysis of a silica matrix embedded nanocrystalline hydroxyapatite bone substitute using the subcutaneous implantation model in Wistar rats

Energy Technology Data Exchange (ETDEWEB)

Ghanaati, Shahram; Orth, Carina; Barbeck, Mike; Kirkpatrick, Charles James [Institute of Pathology, University Medical Center of the Johannes Gutenberg University Mainz, Langenbeckstrasse 1, 55101 Mainz (Germany); Willershausen, Ines [Institute for Dental Material Sciences and Technology, University Medical Center of the Johannes Gutenberg University Mainz, Anselm-Franz-von-Bentzel-Weg 14, 55128 Mainz (Germany); Thimm, Benjamin W [Institute for Biomechanics, ETH Zuerich, Wolfgang-Pauli-Str.10, 8093 Zuerich (Switzerland); Booms, Patrick [Leeds Institute of Molecular Medicine, Section of Medicine, Surgery and Anaesthesia, University of Leeds (United Kingdom); Stuebinger, Stefan; Landes, Constantin; Sader, Robert Anton, E-mail: ghanaati@uni-mainz.d [Department for Oral, Cranio-Maxillofacial and Facial Plastic Surgery, Medical Center of the Goethe University Frankfurt, Theodor-Stein-Kai 7, 60596 Frankfurt am Main (Germany)

2010-06-01

The clinical suitability of a bone substitute material is determined by the ability to induce a tissue reaction specific to its composition. The aim of this in vivo study was to analyze the tissue reaction to a silica matrix-embedded, nanocrystalline hydroxyapatite bone substitute. The subcutaneous implantation model in Wistar rats was chosen to assess the effect of silica degradation on the vascularization of the biomaterial and its biodegradation within a time period of 6 months. Already at day 10 after implantation, histomorphometrical analysis showed that the vascularization of the implantation bed reached its peak value compared to all other time points. Both vessel density and vascularization significantly decreased until day 90 after implantation. In this time period, the bone substitute underwent a significant degradation initiated by TRAP-positive and TRAP-negative multinucleated giant cells together with macrophages and lymphocytes. Although no specific tissue reaction could be related to the described silica degradation, the biomaterial was close to being fully degraded without a severe inflammatory response. These characteristics are advantageous for bone regeneration and remodeling processes.

Histological and histomorphometrical analysis of a silica matrix embedded nanocrystalline hydroxyapatite bone substitute using the subcutaneous implantation model in Wistar rats

International Nuclear Information System (INIS)

Ghanaati, Shahram; Orth, Carina; Barbeck, Mike; Kirkpatrick, Charles James; Willershausen, Ines; Thimm, Benjamin W; Booms, Patrick; Stuebinger, Stefan; Landes, Constantin; Sader, Robert Anton

2010-01-01

The clinical suitability of a bone substitute material is determined by the ability to induce a tissue reaction specific to its composition. The aim of this in vivo study was to analyze the tissue reaction to a silica matrix-embedded, nanocrystalline hydroxyapatite bone substitute. The subcutaneous implantation model in Wistar rats was chosen to assess the effect of silica degradation on the vascularization of the biomaterial and its biodegradation within a time period of 6 months. Already at day 10 after implantation, histomorphometrical analysis showed that the vascularization of the implantation bed reached its peak value compared to all other time points. Both vessel density and vascularization significantly decreased until day 90 after implantation. In this time period, the bone substitute underwent a significant degradation initiated by TRAP-positive and TRAP-negative multinucleated giant cells together with macrophages and lymphocytes. Although no specific tissue reaction could be related to the described silica degradation, the biomaterial was close to being fully degraded without a severe inflammatory response. These characteristics are advantageous for bone regeneration and remodeling processes.

An exsolution silica-pump model for the origin of myrmekite

Science.gov (United States)

Castle, R.O.; Lindsley, D.H.

1993-01-01

Myrmekite, as defined here, is the microscopic intergrowth between vermicular quartz and modestly anorthitic plagioclase (calcic albite-oligoclase), intimately associated with potassium feldspar in plutonic rocks of granitic composition. Hypotheses previously invoked in explanation of myrmekite include: (1) direct crystallization; (2) replacement; (3) exsolution. The occurrence of myrmekite in paragneisses and its absence in rocks devold of discrete grains of potassium feldspar challenge those hypotheses based on direct crystallization or replacement. However, several lines of evidence indicate that myrmekite may in fact originate in response to kinetic effects associated with the exsolution of calcic alkali feldspar into discrete potassium feldspar and plagioclase phases. Exsolution of potassium feldspar system projected from [AlSi2O8] involves the exchange CaAlK-1Si-1, in which the AlSi-1 tetrahedral couple is resistant to intracrystalline diffusion. By contrast, diffusion of octahedral K proceeds relatively easily where it remains uncoupled to the tetrahedral exchange. We suggest here that where the ternary feldspar system is open to excess silica, the exchange reaction that produces potassium feldspar in the ternary plane is aided by the net-transfer reaction K+Si=Orthoclase, leaving behind indigenous Si that reports as modal quartz in the evolving plagioclase as the CaAl component is concomitantly incorporated in this same phase. Thus silica is "pumped" into the reaction volume from a "silica reservoir", a process that enhances redistribution of both Si and Al through the exsolving ternary feldspar. ?? 1993 Springer-Verlag.

Larnite powders and larnite/silica aerogel composites as effective agents for CO{sub 2} sequestration by carbonation

Energy Technology Data Exchange (ETDEWEB)

Santos, A., E-mail: alberto.santos@uca.es [Departamento de Ciencias de la Tierra, Universidad de Cadiz, Puerto Real, 11510 Cadiz (Spain); Ajbary, M.; Morales-Florez, V. [Departamento de Fisica de la Materia Condensada, Universidad de Cadiz, Puerto Real, 11510 Cadiz (Spain); Kherbeche, A. [Universite Sidi Mohamed Ben Abdellah, Ecole Superieure de Technologie, Fes (Morocco); Pinero, M. [Departamento de Fisica Aplicada, Universidad de Cadiz, Puerto Real, 11510 Cadiz (Spain); Esquivias, L. [Departamento de Fisica de la Materia Condensada, Facultad de Fisica, Instituto de Ciencias de Materiales de Sevilla (CSIC), Universidad de Sevilla, 41012 Sevilla (Spain)

2009-09-15

This paper presents the results of the carbonation reaction of two sample types: larnite (Ca{sub 2}SiO{sub 4}) powders and larnite/silica aerogel composites, the larnite acting as an active phase in a process of direct mineral carbonation. First, larnite powders were synthesized by the reaction of colloidal silica and calcium nitrate in the presence of ethylene glycol. Then, to synthesize the composites, the surface of the larnite powders was chemically modified with 3-aminopropyltriethoxysilane (APTES), and later this mixture was added to a silica sol previously prepared from tetraethylorthosilicate (TEOS). The resulting humid gel was dried in an autoclave under supercritical conditions for the ethanol. The textures and chemical compositions of the powders and composites were characterized.The carbonation reaction of both types of samples was evaluated by means of X-ray diffraction and thermogravimetric analysis. Both techniques confirm the high efficiency of the reaction at room temperature and atmospheric pressure. A complete transformation of the silicate into carbonate resulted after submitting the samples to a flow of pure CO{sub 2} for 15 min. This indicates that for this reaction time, 1 t of larnite could eliminate about 550 kg of CO{sub 2}. The grain size, porosity, and specific surface area are the factors controlling the reaction.

Silica Nephropathy

Directory of Open Access Journals (Sweden)

N Ghahramani

2010-06-01

Full Text Available Occupational exposure to heavy metals, organic solvents and silica is associated with a variety of renal manifestations. Improved understanding of occupational renal disease provides insight into environmental renal disease, improving knowledge of disease pathogenesis. Silica (SiO2 is an abundant mineral found in sand, rock, and soil. Workers exposed to silica include sandblasters, miners, quarry workers, masons, ceramic workers and glass manufacturers. New cases of silicosis per year have been estimated in the US to be 3600–7300. Exposure to silica has been associated with tubulointerstitial disease, immune-mediated multisystem disease, chronic kidney disease and end-stage renal disease. A rare syndrome of painful, nodular skin lesions has been described in dialysis patients with excessive levels of silicon. Balkan endemic nephropathy is postulated to be due to chronic intoxication with drinking water polluted by silicates released during soil erosion. The mechanism of silica nephrotoxicity is thought to be through direct nephrotoxicity, as well as silica-induced autoimmune diseases such as scleroderma and systemic lupus erythematosus. The renal histopathology varies from focal to crescentic and necrotizing glomerulonephritis with aneurysm formation suggestive of polyarteritis nodosa. The treatment for silica nephrotoxicity is non-specific and depends on the mechanism and stage of the disease. It is quite clear that further research is needed, particularly to elucidate the pathogenesis of silica nephropathy. Considering the importance of diagnosing exposure-related renal disease at early stages, it is imperative to obtain a thorough occupational history in all patients with renal disease, with particular emphasis on exposure to silica, heavy metals, and solvents.

Vapor Pressure and Evaporation Coefficient of Silicon Monoxide over a Mixture of Silicon and Silica

Science.gov (United States)

Ferguson, Frank T.; Nuth, Joseph A., III

2012-01-01

The evaporation coefficient and equilibrium vapor pressure of silicon monoxide over a mixture of silicon and vitreous silica have been studied over the temperature range (1433 to 1608) K. The evaporation coefficient for this temperature range was (0.007 plus or minus 0.002) and is approximately an order of magnitude lower than the evaporation coefficient over amorphous silicon monoxide powder and in general agreement with previous measurements of this quantity. The enthalpy of reaction at 298.15 K for this reaction was calculated via second and third law analyses as (355 plus or minus 25) kJ per mol and (363.6 plus or minus 4.1) kJ per mol respectively. In comparison with previous work with the evaporation of amorphous silicon monoxide powder as well as other experimental measurements of the vapor pressure of silicon monoxide gas over mixtures of silicon and silica, these systems all tend to give similar equilibrium vapor pressures when the evaporation coefficient is correctly taken into account. This provides further evidence that amorphous silicon monoxide is an intimate mixture of small domains of silicon and silica and not strictly a true compound.

COOH-functionalisation of silica particles

Energy Technology Data Exchange (ETDEWEB)

Majewski, Peter, E-mail: peter.majewski@unisa.edu.au [School of Advanced Manufacturing and Mechanical Engineering, Mawson Institute, University of South Australia, Adelaide (Australia); Albrecht, Trent [Ian Wark Research Institute, University of South Australia, Adelaide (Australia); Weber, Siegfried [Department of Biotechnology, University of Applied Sciences, Mannheim (Germany)

2011-09-01

In this study COOH-functionalised silica is synthesised using phosphonateN-(phosphonomethyl)iminodiacetic acid (PMIDA) in an aqueous solution. The presence of PMIDA on the silica particles was verified using Fourier Transform Infrared Spectroscopy, X-ray Photoelectron Spectroscopy and titration. Experimentally, surface concentrations of COOH functional groups of up to about 3 mmol/g{sub silica} were achieved, whereas theoretical calculation of the maximum COOH functional group concentration gave about 1 mmol/g{sub silica}. The discrepancy may be caused by PMIDA multilayer formation on the particle.

Control the Morphologies and the Pore Architectures of Meso porous Silicas through a Dual-Templating Approach

International Nuclear Information System (INIS)

Wang, H.; Chen, H.; Xu, Z.; Wang, S.; Li, B.; Li, Y.

2012-01-01

Meso porous silica nanospheres were prepared using a chiral cationic low-molecular-weight amphiphile and organic solvents such as toluene, cyclohexane, and tetrachlorocarbon through a dual-templating approach. X-ray diffraction, nitrogen sorption, field emission scanning electron microscopy, and transmission electron microscopy techniques have been used to characterize the meso porous silicas. The volume ratio of toluene to water plays an important role in controlling the morphologies and the pore architectures of the meso porous silicas. It was also found that meso porous silica nano flakes can be prepared by adding tetrahydrofuran to the reaction mixtures.

Thermal transformation of bioactive caffeic acid on fumed silica seen by UV-Vis spectroscopy, thermogravimetric analysis, temperature programmed desorption mass spectrometry and quantum chemical methods.

Science.gov (United States)

Kulik, Tetiana V; Lipkovska, Natalia O; Barvinchenko, Valentyna M; Palyanytsya, Borys B; Kazakova, Olga A; Dudik, Olesia O; Menyhárd, Alfréd; László, Krisztina

2016-05-15

Thermochemical studies of hydroxycinnamic acid derivatives and their surface complexes are important for the pharmaceutical industry, medicine and for the development of technologies of heterogeneous biomass pyrolysis. In this study, structural and thermal transformations of caffeic acid complexes on silica surfaces were studied by UV-Vis spectroscopy, thermogravimetric analysis, temperature programmed desorption mass spectrometry (TPD MS) and quantum chemical methods. Two types of caffeic acid surface complexes are found to form through phenolic or carboxyl groups. The kinetic parameters of the chemical reactions of caffeic acid on silica surface are calculated. The mechanisms of thermal transformations of the caffeic chemisorbed surface complexes are proposed. Thermal decomposition of caffeic acid complex chemisorbed through grafted ester group proceeds via three parallel reactions, producing ketene, vinyl and acetylene derivatives of 1,2-dihydroxybenzene. Immobilization of phenolic acids on the silica surface improves greatly their thermal stability. Copyright © 2016 Elsevier Inc. All rights reserved.

Preparation and characterization of hybrid Nafion/silica and Nafion/silica/PTA membranes for redox flow batteries

Energy Technology Data Exchange (ETDEWEB)

Glibin, V.; Pupkevich, V.; Svirko, L.; Karamanev, D. [Western Ontario Univ., London, ON (Canada). Dept. of Biochemical and Chemical Engineering

2008-07-01

Redox flow batteries are both efficient and cost-effective. However, the long-term stability of most ion-exchange membranes is limited as a result of the high oxidation rates of ions with high redox potentials. A method of synthesizing multi-component Nafion-silica and Nafion-silica-PTA membranes was presented in this study, which also investigated the electrochemical and ion transport properties of the membranes. Membranes were cast from dimethylformamide (DMFA) solution. The iron ion diffusion kinetics of the Nafion-silica and Nafion-silica PTA membranes were studied by dialysis. Results of the investigation demonstrated that the introduction of silica and phosphotungstic acid (PTA) into the Nafion membrane composition resulted in a significant decrease of ion transfer through the membrane. The addition of PTA also increased membrane permeability to ferric ions. The low iron diffusion coefficient and high ionic conductivity of the Nafion-silica membrane makes it a promising material for use in redox flow batteries. 4 refs., 1 tab., 1 fig.

Gas Separation through Bilayer Silica, the Thinnest Possible Silica Membrane.

Science.gov (United States)

Yao, Bowen; Mandrà, Salvatore; Curry, John O; Shaikhutdinov, Shamil; Freund, Hans-Joachim; Schrier, Joshua

2017-12-13

Membrane-based gas separation processes can address key challenges in energy and environment, but for many applications the permeance and selectivity of bulk membranes is insufficient for economical use. Theory and experiment indicate that permeance and selectivity can be increased by using two-dimensional materials with subnanometer pores as membranes. Motivated by experiments showing selective permeation of H 2 /CO mixtures through amorphous silica bilayers, here we perform a theoretical study of gas separation through silica bilayers. Using density functional theory calculations, we obtain geometries of crystalline free-standing silica bilayers (comprised of six-membered rings), as well as the seven-, eight-, and nine-membered rings that are observed in glassy silica bilayers, which arise due to Stone-Wales defects and vacancies. We then compute the potential energy barriers for gas passage through these various pore types for He, Ne, Ar, Kr, H 2 , N 2 , CO, and CO 2 gases, and use the data to assess their capability for selective gas separation. Our calculations indicate that crystalline bilayer silica, which is less than a nanometer thick, can be a high-selectivity and high-permeance membrane material for 3 He/ 4 He, He/natural gas, and H 2 /CO separations.

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.

Heating ability and biocompatibility study of silica-coated magnetic ...

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science; Volume 38; Issue 6. Heating ability and biocompatibility study of silica-coated magnetic nanoparticles as heating mediators for magnetic hyperthermia and magnetically triggered drug delivery systems. Meysam Soleymani Mohammad Edrissi. Volume 38 Issue 6 October 2015 ...

Quantitative diagnosis and prognosis framework for concrete degradation due to alkali-silica reaction

Science.gov (United States)

Mahadevan, Sankaran; Neal, Kyle; Nath, Paromita; Bao, Yanqing; Cai, Guowei; Orme, Peter; Adams, Douglas; Agarwal, Vivek

2017-02-01

This research is seeking to develop a probabilistic framework for health diagnosis and prognosis of aging concrete structures in nuclear power plants that are subjected to physical, chemical, environment, and mechanical degradation. The proposed framework consists of four elements: monitoring, data analytics, uncertainty quantification, and prognosis. The current work focuses on degradation caused by ASR (alkali-silica reaction). Controlled concrete specimens with reactive aggregate are prepared to develop accelerated ASR degradation. Different monitoring techniques — infrared thermography, digital image correlation (DIC), mechanical deformation measurements, nonlinear impact resonance acoustic spectroscopy (NIRAS), and vibro-acoustic modulation (VAM) — are studied for ASR diagnosis of the specimens. Both DIC and mechanical measurements record the specimen deformation caused by ASR gel expansion. Thermography is used to compare the thermal response of pristine and damaged concrete specimens and generate a 2-D map of the damage (i.e., ASR gel and cracked area), thus facilitating localization and quantification of damage. NIRAS and VAM are two separate vibration-based techniques that detect nonlinear changes in dynamic properties caused by the damage. The diagnosis results from multiple techniques are then fused using a Bayesian network, which also helps to quantify the uncertainty in the diagnosis. Prognosis of ASR degradation is then performed based on the current state of degradation obtained from diagnosis, by using a coupled thermo-hydro-mechanical-chemical (THMC) model for ASR degradation. This comprehensive approach of monitoring, data analytics, and uncertainty-quantified diagnosis and prognosis will facilitate the development of a quantitative, risk informed framework that will support continuous assessment and risk management of structural health and performance.

Immobilization of Beauveria bassiana Lipase on Silica Gel by Physical Adsorption

Directory of Open Access Journals (Sweden)

Vanessa Hitomi Sugahara

2014-12-01

Full Text Available Extracellular lipase from Beauveria bassianastrain CG481 was immobilized by using thirteen different immobilization protocols. Silica gel was chosen as the most suitable adsorbent with 94.8% of activity yield. The adsorption on silica gel did not change the optimum pH (8.5 and temperature (45ºC values of the free lipase (FL for lipolytic activity, and it showed higher activities in extreme conditions (pH 9.0 to 10.5, 60ºC. The lipase immobilized on silica gel (ILS showed enhanced stability at pH 7.0 after 120 h incubation (69.0% when compared to FL (33.3%. The thermal stability was also enhanced by immobilization at 60ºC in aqueous (64.6% and organic medium (95.1%, while FL showed only 40.6% of residual activity in aqueous medium and exhibited no activity for esterification reaction in n-heptane. The treatment of ILS with 0.8 M NaCl prevented lipase desorption while Triton X-100 (0.1% resulted the enzyme leakage. The ILS was reused for four times for esterification reaction with 80.8% of initial activity.

Incorporation of polyoxotungstate complexes in silica spheres and in situ formation of tungsten trioxide nanoparticles.

Science.gov (United States)

Zhao, Yuanyuan; Fan, Haimei; Li, Wen; Bi, Lihua; Wang, Dejun; Wu, Lixin

2010-09-21

In this paper, we demonstrated a new convenient route for in situ fabrication of well separated small sized WO(3) nanoparticles in silica spheres, through a predeposition of surfactant encapsulated polyoxotungates as tungsten source, and followed by a calcination process. In a typical procedure, selected polyoxotungates with different charges were enwrapped with dioctadecyldimethylammonium cations through electrostatic interaction. Elemental analysis, thermogravimetric analysis, and spectral characterization confirmed the formation of prepared complexes with the anticipated chemical structure. The complexes were then phase-transferred into aqueous solution that predissolved surfactant cetyltrimethylammonium bromide, and finally incorporated into silica spheres through a joint sol-gel reaction with tetraethyl orthosilicate in a well dispersed state under the protection of organic layer for polyoxotungates from the alkaline reaction condition. Transmission electron microscopic images illustrated the well dispersed WO(3) nanoparticles in the size range of ca. 2.2 nm in the silica spheres after the calcination at 465 °C. The sizes of both the silica spheres and WO(3) nanoparticles could be adjusted independently through changing the doping content to a large extent. Meanwhile, the doped polyoxotungate complexes acted as the template for the mesoporous structure in silica spheres after the calcination. Along with the increase of doping content and surfactant, the mesopore size changed little (2.0-2.9 nm), but the specific surface areas increased quite a lot. Importantly, the WO(3)-nanoparticle-doped silica spheres displayed an interesting photovoltaic property, which is favorable for the funtionalization of these nanomaterials.

Diels-Alder reactions in confined spaces: the influence of catalyst structure and the nature of active sites for the retro-Diels-Alder reaction.

Science.gov (United States)

Cantín, Ángel; Gomez, M Victoria; de la Hoz, Antonio

2016-01-01

Diels-Alder cycloaddition between cyclopentadiene and p -benzoquinone has been studied in the confined space of a pure silica zeolite Beta and the impact on reaction rate due to the concentration effect within the pore and diffusion limitations are discussed. Introduction of Lewis or Brønsted acid sites on the walls of the zeolite strongly increases the reaction rate. However, contrary to what occurs with mesoporous molecular sieves (MCM-41), Beta zeolite does not catalyse the retro-Diels-Alder reaction, resulting in a highly selective catalyst for the cycloaddition reaction.

An Active Alkali-Exchanged Faujasite Catalyst for p-Xylene Production via the One-Pot Diels-Alder Cycloaddition/Dehydration Reaction of 2,5-Dimethylfuran with Ethylene.

Science.gov (United States)

Rohling, Roderigh Y; Uslamin, Evgeny; Zijlstra, Bart; Tranca, Ionut C; Filot, Ivo A W; Hensen, Emiel J M; Pidko, Evgeny A

2018-02-02

The one-pot Diels-Alder cycloaddition (DAC)/dehydration (D) tandem reaction between 2,5-dimethylfuran and ethylene is a potent pathway toward biomass-derived p -xylene. In this work, we present a cheap and active low-silica potassium-exchanged faujasite (KY, Si/Al = 2.6) catalyst. Catalyst optimization was guided by a computational study of the DAC/D reaction mechanism over different alkali-exchanged faujasites using periodic density functional theory calculations complemented by microkinetic modeling. Two types of faujasite models were compared, i.e., a high-silica alkali-exchanged faujasite model representing isolated active cation sites and a low-silica alkali-exchanged faujasite in which the reaction involves several cations in the proximity. The mechanistic study points to a significant synergetic cooperative effect of the ensemble of cations in the faujasite supercage on the DAC/D reaction. Alignment of the reactants by their interactions with the cationic sites and stabilization of reaction intermediates contribute to the high catalytic performance. Experiments confirmed the prediction that KY is the most active catalyst among low-silica alkali-exchanged faujasites. This work is an example of how the catalytic reactivity of zeolites depends on multiple interactions between the zeolite and reagents.

Cellular membrane trafficking of mesoporous silica nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Fang, I-Ju [Iowa State Univ., Ames, IA (United States)

2012-01-01

This dissertation mainly focuses on the investigation of the cellular membrane trafficking of mesoporous silica nanoparticles. We are interested in the study of endocytosis and exocytosis behaviors of mesoporous silica nanoparticles with desired surface functionality. The relationship between mesoporous silica nanoparticles and membrane trafficking of cells, either cancerous cells or normal cells was examined. Since mesoporous silica nanoparticles were applied in many drug delivery cases, the endocytotic efficiency of mesoporous silica nanoparticles needs to be investigated in more details in order to design the cellular drug delivery system in the controlled way. It is well known that cells can engulf some molecules outside of the cells through a receptor-ligand associated endocytosis. We are interested to determine if those biomolecules binding to cell surface receptors can be utilized on mesoporous silica nanoparticle materials to improve the uptake efficiency or govern the mechanism of endocytosis of mesoporous silica nanoparticles. Arginine-glycine-aspartate (RGD) is a small peptide recognized by cell integrin receptors and it was reported that avidin internalization was highly promoted by tumor lectin. Both RGD and avidin were linked to the surface of mesoporous silica nanoparticle materials to investigate the effect of receptor-associated biomolecule on cellular endocytosis efficiency. The effect of ligand types, ligand conformation and ligand density were discussed in Chapter 2 and 3. Furthermore, the exocytosis of mesoporous silica nanoparticles is very attractive for biological applications. The cellular protein sequestration study of mesoporous silica nanoparticles was examined for further information of the intracellular pathway of endocytosed mesoporous silica nanoparticle materials. The surface functionality of mesoporous silica nanoparticle materials demonstrated selectivity among the materials and cancer and normal cell lines. We aimed to determine

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

Science.gov (United States)

Kapusuz, Derya; Durucan, Caner

2017-07-01

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

Synthesis of monodisperse silica microspheres and modification with diazoresin for mixed-mode ultra high performance liquid chromatography separations.

Science.gov (United States)

Cong, Hailin; Yu, Bing; Tian, Chao; Zhang, Shuai; Yuan, Hua

2017-11-01

Monodisperse silica particles with average diameters of 1.9-2.9 μm were synthesized by a modified Stöber method, in which tetraethyl orthosilicate was continuously supplied to the reaction mixture containing KCl electrolyte, water, ethanol, and ammonia. The obtained silica particles were modified by self-assembly with positively charged photosensitive diazoresin on the surface. After treatment with ultraviolet light, the ionic bonding between silica and diazoresin was converted into covalent bonding through a unique photochemistry reaction of diazoresin. Depending on the chemical structure of diazoresin and mobile phase composition, the diazoresin-modified silica stationary phase showed different separation mechanisms, including reversed phase and hydrophilic interactions. Therefore, a variety of baseline separation of benzene analogues and organic acids was achieved by using the diazoresin-modified silica particles as packing materials in ultra high performance liquid chromatography. According to the π-π interactional difference between carbon rings of fullerenes and benzene rings of diazoresin, C 60 and C 70 were also well separated by ultra-high performance liquid chromatography. Because it has a small size, the ∼2.5 μm monodisperse diazoresin-modified silica stationary phase shows ultra-high efficiency compared with the commercial C 18 -silica high-performance liquid chromatography stationary phase with average diameters of ∼5 μm. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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

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.

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

KAUST Repository

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

2013-01-01

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

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

KAUST Repository

Bouhrara, Mohamed

2013-09-03

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-08-15

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

Molecular imprinting at walls of silica nanotubes for TNT recognition.

Science.gov (United States)

Xie, Chenggen; Liu, Bianhua; Wang, Zhenyang; Gao, Daming; Guan, Guijian; Zhang, Zhongping

2008-01-15

This paper reports the molecular imprinting at the walls of highly uniform silica nanotubes for the recognition of 2,4,6-trinitrotoluene (TNT). It has been demonstrated that TNT templates were efficiently imprinted into the matrix of silica through the strong acid-base pairing interaction between TNT and 3-aminopropyltriethoxysilane (APTS). TNT-imprinted silica nanotubes were synthesized by the gelation reaction between APTS and tetraethylorthosilicate (TEOS), selectively occurring at the porous walls of APTS-modified alumina membranes. The removal of the original TNT templates leaves the imprinted cavities with covalently anchored amine groups at the cavity walls. A high density of recognition sites with molecular selectivity to the TNT analyte was created at the wall of silica nanotubes. Furthermore, most of these recognition sites are situated at the inside and outside surfaces of tubular walls and in the proximity of the two surfaces due to the ultrathin wall thickness of only 15 nm, providing a better site accessibility and lower mass-transfer resistance. Therefore, greater capacity and faster kinetics of uptaking target species were achieved. The silica nanotube reported herein is an ideal form of material for imprinting various organic or biological molecules toward applications in chemical/biological sensors and bioassay.

Influence of silica fume and fly ash on hydration, microstructure and strength of cement based mixtures

Energy Technology Data Exchange (ETDEWEB)

Weng, Kaimao

1992-10-01

The influence of fly ash and silica fume on the hydration, microstructure and strength of cement-based mixtures was investigated. A literature review of the hydration processes, compressive strength development, and microstructure of Portland cement is presented, followed by description of materials and specimens preparation and experimental methodology. It was found that silica fume retards cement hydration at low water/concrete ratios. It reduces calcium hydroxide significantly and increases the amount of hydrates at early ages. Fly ash retards hydration more significantly at high water/concrete ratios than at low ratios. The combination of silica fume and fly ash further retards hydration at one day. Silica fume dominates the reaction with calcium hydroxide. Silica fume significantly increases early strength of mortars and concrete, while fly ash reduces early strength. Silica fume can substantially increase strength of fly ash mortar and concrete after 7 days. Silica fume refines pores in the range 100-500 A, while fly ash mortars exhibit gradual pore refinement as hydration proceeds. Silica fume dominates the pore refinement if used with fly ash. 89 refs., 74 figs., 16 tabs.

Silica removal in industrial effluents with high silica content and low hardness.

Science.gov (United States)

Latour, Isabel; Miranda, Ruben; Blanco, Angeles

2014-01-01

High silica content of de-inked paper mill effluents is limiting their regeneration and reuse after membrane treatments such as reverse osmosis (RO). Silica removal during softening processes is a common treatment; however, the effluent from the paper mill studied has a low hardness content, which makes the addition of magnesium compounds necessary to increase silica removal. Two soluble magnesium compounds (MgCl₂∙6H₂O and MgSO₄∙7H₂O) were tested at five dosages (250-1,500 mg/L) and different initial pH values. High removal rates (80-90%) were obtained with both products at the highest pH tested (11.5). With these removal efficiencies, it is possible to work at high RO recoveries (75-85%) without silica scaling. Although pH regulation significantly increased the conductivity of the waters (at pH 11.5 from 2.1 to 3.7-4.0 mS/cm), this could be partially solved by using Ca(OH)₂ instead of NaOH as pH regulator (final conductivity around 3.0 mS/cm). Maximum chemical oxygen demand (COD) removal obtained with caustic soda was lower than with lime (15 vs. 30%). Additionally, the combined use of a polyaluminum coagulant during the softening process was studied; the coagulant, however, did not significantly improve silica removal, obtaining a maximum increase of only 10%.

Kinetics Study of Gas Pollutant Adsorption and Thermal Desorption on Silica Gel

Directory of Open Access Journals (Sweden)

Rong A

2017-06-01

Full Text Available Silica gel is a typical porous desiccant material. Its adsorption performance for gaseous air pollutants was investigated to determine its potential contribution to reducing such pollutants. Three gaseous air pollutants, toluene, carbon dioxide, and methane, were investigated in this paper. A thermogravimetric analyzer was used to obtain the equilibrium adsorption capacity of gases on single silica gel particles. The silica gel adsorption capacity for toluene is much higher than that for carbon dioxide and methane. To understand gas pollutant thermal desorption from silica gel, the thermogravimetric analysis of toluene desorption was conducted with 609 ppm toluene vapor at 313 K, 323 K, and 333 K. The overall regeneration rate of silica gel was strongly dependent on temperature and the enthalpy of desorption. The gas pollutant adsorption performance and thermal desorption on silica gel material may be used to estimate the operating and design parameters for gas pollutant adsorption by desiccant wheels.

Improvement of thermal stability of UV curable pressure sensitive adhesive by surface modified silica nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Pang, Beili; Ryu, Chong-Min; Kim, Hyung-Il, E-mail: hikim@cnu.ac.kr

2013-11-01

Highlights: • Silica nanoparticles were modified to carry the vinyl groups for photo-crosslinking. • Acrylic copolymer was modified to have the vinyl groups for photo-crosslinking. • Strong and extensive interfacial bondings were formed between polymer and silica. • Thermal stability of PSA was improved by forming nanocomposite with modified silica. -- Abstract: Pressure sensitive adhesives (PSAs) with higher thermal stability were successfully prepared by forming composite with the silica nanoparticles modified via reaction with 3-methacryloxypropyltrimethoxysilane. The acrylic copolymer was synthesized as a base resin for PSAs by solution polymerization of 2-EHA, EA, and AA with AIBN as an initiator. The acrylic copolymer was further modified with GMA to have the vinyl groups available for UV curing. The peel strength decreased with the increase of gel content which was dependent on both silica content and UV dose. Thermal stability of the composite PSAs was improved noticeably with increasing silica content and UV dose mainly due to the strong and extensive interfacial bonding between the organic polymer matrix and silica.

Cytotoxicity and fluorescence studies of silica-coated CdSe quantum dots for bioimaging applications

International Nuclear Information System (INIS)

Vibin, Muthunayagam; Vinayakan, Ramachandran; John, Annie; Raji, Vijayamma; Rejiya, Chellappan S.; Vinesh, Naresh S.; Abraham, Annie

2011-01-01

The toxicological effects of silica-coated CdSe quantum dots (QDs) were investigated systematically on human cervical cancer cell line. Trioctylphosphine oxide capped CdSe QDs were synthesized and rendered water soluble by overcoating with silica, using aminopropyl silane as silica precursor. The cytotoxicity studies were conducted by exposing cells to freshly synthesized QDs as a function of time (0–72 h) and concentration up to micromolar level by Lactate dehydrogenase assay, MTT [3-(4,5-Dimethylthiazol-2-yl)-2,5-Diphenyltetrazolium Bromide] assay, Neutral red cell viability assay, Trypan blue dye exclusion method and morphological examination of cells using phase contrast microscope. The in vitro analysis results showed that the silica-coated CdSe QDs were nontoxic even at higher loadings. Subsequently the in vivo fluorescence was also demonstrated by intravenous administration of the QDs in Swiss albino mice. The fluorescence images in the cryosections of tissues depicted strong luminescence property of silica-coated QDs under biological conditions. These results confirmed the role of these luminescent materials in biological labeling and imaging applications.

Cytotoxicity and fluorescence studies of silica-coated CdSe quantum dots for bioimaging applications

Energy Technology Data Exchange (ETDEWEB)

Vibin, Muthunayagam [University of Kerala, Department of Biochemistry (India); Vinayakan, Ramachandran [National Institute for Interdisciplinary Science and Technology (CSIR), Photosciences and Photonics (India); John, Annie [Sree Chitra Tirunal Institute of Medical Sciences and Technology, Biomedical Technology Wing (India); Raji, Vijayamma; Rejiya, Chellappan S.; Vinesh, Naresh S.; Abraham, Annie, E-mail: annieab2@yahoo.co.in [University of Kerala, Department of Biochemistry (India)

2011-06-15

The toxicological effects of silica-coated CdSe quantum dots (QDs) were investigated systematically on human cervical cancer cell line. Trioctylphosphine oxide capped CdSe QDs were synthesized and rendered water soluble by overcoating with silica, using aminopropyl silane as silica precursor. The cytotoxicity studies were conducted by exposing cells to freshly synthesized QDs as a function of time (0-72 h) and concentration up to micromolar level by Lactate dehydrogenase assay, MTT [3-(4,5-Dimethylthiazol-2-yl)-2,5-Diphenyltetrazolium Bromide] assay, Neutral red cell viability assay, Trypan blue dye exclusion method and morphological examination of cells using phase contrast microscope. The in vitro analysis results showed that the silica-coated CdSe QDs were nontoxic even at higher loadings. Subsequently the in vivo fluorescence was also demonstrated by intravenous administration of the QDs in Swiss albino mice. The fluorescence images in the cryosections of tissues depicted strong luminescence property of silica-coated QDs under biological conditions. These results confirmed the role of these luminescent materials in biological labeling and imaging applications.

Silica and lung cancer: a controversial issue.

Science.gov (United States)

Pairon, J C; Brochard, P; Jaurand, M C; Bignon, J

1991-06-01

The role of crystalline silica in lung cancer has long been the subject of controversy. In this article, we review the main experimental and epidemiological studies dealing with this problem. Some evidence for a genotoxic potential of crystalline silica has been obtained in the rare in vitro studies published to date. In vivo studies have shown that crystalline silica is carcinogenic in the rat; the tumour types appear to vary according to the route of administration. In addition, an association between carcinogenic and fibrogenic potency has been observed in various animal species exposed to crystalline silica. An excess of lung cancer related to occupational exposure to crystalline silica is reported in many epidemiological studies, regardless of the presence of silicosis. However, most of these studies are difficult to interpret because they do not correctly take into account associated carcinogens such as tobacco smoke and other occupational carcinogens. An excess of lung cancer is generally reported in studies based on silicosis registers. Overall, experimental and human studies suggest an association between exposure to crystalline silica and an excess of pulmonary malignancies. Although the data available are not sufficient to establish a clear-cut causal relationship in humans, an association between the onset of pneumoconiosis and pulmonary malignancies is probable. In contrast, experimental observations have given rise to a pathophysiological mechanism that might account for a putative carcinogenic potency of crystalline silica.

[Response surface method optimize of nano-silica solid dispersion technology assistant enzymatic hydrolysis preparation genistein].

Science.gov (United States)

Jin, Xin; Zhang, Zhen-Hai; Zhu, Jing; Sun, E; Yu, Dan-Hong; Chen, Xiao-Yun; Liu, Qi-Yuan; Ning, Qing; Jia, Xiao-Bin

2012-04-01

This article reports that nano-silica solid dispersion technology was used to raise genistein efficiency through increasing the enzymatic hydrolysis rate. Firstly, genistin-nano-silica solid dispersion was prepared by solvent method. And differential scanning calorimetry (DSC) and transmission electron microscopy (TEM) were used to verify the formation of solid dispersion, then enzymatic hydrolysis of solid dispersion was done by snailase to get genistein. With the conversion of genistein as criteria, single factor experiments were used to study the different factors affecting enzymatic hydrolysis of genistin and its solid dispersion. And then, response surface method was used to optimize of nano-silica solid dispersion technology assistant enzymatic hydrolysis. The optimum condition to get genistein through enzymatic hydrolysis of genistin-nano-silica solid dispersion was pH 7.1, temperature 52.2 degrees C, enzyme concentration 5.0 mg x mL(-1) and reaction time 7 h. Under this condition, the conversion of genistein was (93.47 +/- 2.40)%. Comparing with that without forming the genistin-nano-silica solid dispersion, the conversion increased 2.62 fold. At the same time, the product of hydrolysis was purified to get pure genistein. The method of enzymatic hydrolysis of genistin-nano-silica solid dispersion by snailase to obtain genistein is simple, efficiency and suitable for the modern scale production.

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.

A Pervaporation Study of Ammonia Solutions Using Molecular Sieve Silica Membranes

Directory of Open Access Journals (Sweden)

Xing Yang

2014-02-01

Full Text Available An innovative concept is proposed to recover ammonia from industrial wastewater using a molecular sieve silica membrane in pervaporation (PV, benchmarked against vacuum membrane distillation (VMD. Cobalt and iron doped molecular sieve silica-based ceramic membranes were evaluated based on the ammonia concentration factor downstream and long-term performance. A modified low-temperature membrane evaluation system was utilized, featuring the ability to capture and measure ammonia in the permeate. It was found that the silica membrane with confirmed molecular sieving features had higher water selectivity over ammonia. This was due to a size selectivity mechanism that favoured water, but blocked ammonia. However, a cobalt doped silica membrane previously treated with high temperature water solutions demonstrated extraordinary preference towards ammonia by achieving up to a 50,000 mg/L ammonia concentration (a reusable concentration level measured in the permeate when fed with 800 mg/L of ammonia solution. This exceeded the concentration factor expected by the benchmark VMD process by four-fold, suspected to be due to the competitive adsorption of ammonia over water into the silica structure with pores now large enough to accommodate ammonia. However, this membrane showed a gradual decline in selectivity, suspected to be due to the degradation of the silica material/pore structure after several hours of operation.

Nanoporous Silica-Based Protocells at Multiple Scales for Designs of Life and Nanomedicine

Directory of Open Access Journals (Sweden)

Jie Sun

2015-01-01

Full Text Available Various protocell models have been constructed de novo with the bottom-up approach. Here we describe a silica-based protocell composed of a nanoporous amorphous silica core encapsulated within a lipid bilayer built by self-assembly that provides for independent definition of cell interior and the surface membrane. In this review, we will first describe the essential features of this architecture and then summarize the current development of silica-based protocells at both micro- and nanoscale with diverse functionalities. As the structure of the silica is relatively static, silica-core protocells do not have the ability to change shape, but their interior structure provides a highly crowded and, in some cases, authentic scaffold upon which biomolecular components and systems could be reconstituted. In basic research, the larger protocells based on precise silica replicas of cells could be developed into geometrically realistic bioreactor platforms to enable cellular functions like coupled biochemical reactions, while in translational research smaller protocells based on mesoporous silica nanoparticles are being developed for targeted nanomedicine. Ultimately we see two different motivations for protocell research and development: (1 to emulate life in order to understand it; and (2 to use biomimicry to engineer desired cellular interactions.

Use of Fly Ash in the Mitigation of Alkali-Silica Reaction in Concrete

Science.gov (United States)

2010-11-12

crystallinity of the silica and its solubility. Common reactive minerals susceptible to ASR include strained quartz, cristobalite, opal, obsidian , chert, and... obsidian .[5] Adequate Moisture Adequate moisture, the third and final necessary component for ASR to occur, is one of the key components in the

SCC modification by use of amorphous nano-silica

NARCIS (Netherlands)

Quercia Bianchi, G.; Spiesz, P.R.; Hüsken, G.; Brouwers, H.J.H.

2014-01-01

In this study two different types of nano-silica (nS) were applied in self-compacting concrete (SCC), both having similar particle size distributions (PSD), but produced through two different processes: fumed powder silica and precipitated silica in colloidal suspension. The influence of nano-silica

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

DEFF Research Database (Denmark)

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

2011-01-01

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

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)

The effect of limestone powder, fly ash and silica fume on the ...

Indian Academy of Sciences (India)

water content, high powder volume increases interparticle friction due to ... are cement reactivity with environment, low permeability, diffusion coefficient ... by binding Ca(OH)2 with free silica by a pozzolanic reaction forming a non-soluble CSH.

Determination of diffusion coefficients of hydrogen in fused silica between 296 and 523 K by Raman spectroscopy and application of fused silica capillaries in studying redox reactions

Science.gov (United States)

Shang, L.; Chou, I-Ming; Lu, W.; Burruss, Robert; Zhang, Y.

2009-01-01

Diffusion coefficients (D) of hydrogen in fused silica capillaries (FSC) were determined between 296 and 523 K by Raman spectroscopy using CO2 as an internal standard. FSC capsules (3.25 × 10−4 m OD, 9.9 × 10−5 m ID, and ∼0.01 m long) containing CO2 and H2were prepared and the initial relative concentrations of hydrogen in these capsules were derived from the Raman peak-height ratios between H2 (near 587 cm−1) and CO2 (near 1387 cm−1). The sample capsules were then heated at a fixed temperature (T) at one atmosphere to let H2 diffuse out of the capsule, and the changes of hydrogen concentration were monitored by Raman spectroscopy after quench. This process was repeated using different heating durations at 296 (room T), 323, 375, 430, 473, and 523 K; the same sample capsule was used repeatedly at each temperature. The values of D (in m2 s−1) in FSC were obtained by fitting the observed changes of hydrogen concentration in the FSC capsule to an equation based on Fick’s law. Our D values are in good agreement with the more recent of the two previously reported experimental data sets, and both can be represented by:lnD=-(16.471±0.035)-44589±139RT(R2=0.99991)">lnD=-(16.471±0.035)-44589±139RT(R2=0.99991)where R is the gas constant (8.3145 J/mol K), T in Kelvin, and errors at 1σ level. The slope corresponds to an activation energy of 44.59 ± 0.14 kJ/mol.The D in FSC determined at 296 K is about an order of magnitude higher than that in platinum at 723 K, indicating that FSC is a suitable membrane for hydrogen at temperature between 673 K and room temperature, and has a great potential for studying redox reactions at these temperatures, especially for systems containing organic material and/or sulphur.

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.

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

Directory of Open Access Journals (Sweden)

Isabel Barroso-Martín

2018-05-01

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

Improved Stabilities of Immobilized Glucoamylase on Functionalized Mesoporous Silica Synthesised using Decane as Swelling Agent

Directory of Open Access Journals (Sweden)

Reni George

2013-06-01

Full Text Available Ordered mesoporous silica, with high porosity was used to immobilize glucoamylase via adsorption and covalent binding. Immobilization of glucoamylase within mesoporous silica was successfully achieved, resulting in catalytically high efficiency during starch hydrolysis. In this study, mesoporous silica was functionalized by co-condensation of tetraethoxysilane (TEOS with organosilane (3-aminopropyl triethoxysilane (APTES in a wide range of molar ratios of APTES: TEOS in the presence of triblock copolymer P123 under acidic hydrothermal conditions. The prepared materials were characterized by Small angle XRD, Nitrogen adsorption – desorption and 29Si MAS solid state NMR. N2 desorption studies showed that pore size distribution decreases due to pore blockage after functionalization and enzyme immobilization. Small angle XRD and 29Si MAS NMR study reveals mesophase formation and Si environment of the materials. The main aim of our work was to study the catalytical activity, effect of pH, temperature storage stability and reusability of covalently bound glucoamylase on mesoporous silica support. The result shows that the stability of enzyme can be enhanced by immobilization.  © 2013 BCREC UNDIP. All rights reservedReceived: 3rd December 2012; Revised: 4th April 2013; Accepted: 20th April 2013[How to Cite: George, R., Gopinath, S., Sugunan, S. (2013. Improved Stabilities of Immobilized Glucoamyl-ase on Functionalized Mesoporous Silica Synthesized using Decane as Swelling Agent. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 70-76. (doi:10.9767/bcrec.8.1.4208.70-76][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4208.70-76] | View in  |

Synthesis of highly fluorescent silica nanoparticles in a reverse microemulsion through double-layered doping of organic fluorophores

International Nuclear Information System (INIS)

Yoo, Hyojong; Pak, Joonsung

2013-01-01

Water-soluble, highly fluorescent double-layered silica nanoparticles (FL-DLSN) have been successfully synthesized through a reverse (water-in-oil) microemulsion method. The microemulsion was prepared by mixing a surfactant (Brij35), co-surfactant, organic solvent, water, and fluorescein as an organic fluorophore. The sizes of the silica nanoparticles were successfully controlled in the reverse microemulsion using Brij35 by changing the water-to-Brij35 ratio and by adding HCl. Initially, tetraethylorthosilicate was hydrolyzed by adding NH 4 OH as a catalyst and then polymerized to generate core fluorescent silica nanoparticles with fluorescein. 3-(Aminopropyl)triethoxysilane (APTS) was sequentially added into the reaction mixture, and reacted on the surface of pre-generated core silica nanoparticles to form the second layer in the form of a shell. The second silica layer that was derived from the condensation of APTS effectively protected the fluorescein dye within the silica matrix. This is a novel and simple synthetic approach to generate highly fluorescent, monodispersed silica nanoparticles by doping organic molecules into a silica matrix.Graphical Abstract

Synthesis of highly fluorescent silica nanoparticles in a reverse microemulsion through double-layered doping of organic fluorophores

Energy Technology Data Exchange (ETDEWEB)

Yoo, Hyojong, E-mail: hyojong@hallym.ac.kr; Pak, Joonsung [Hallym University, Department of Chemistry (Korea, Republic of)

2013-05-15

Water-soluble, highly fluorescent double-layered silica nanoparticles (FL-DLSN) have been successfully synthesized through a reverse (water-in-oil) microemulsion method. The microemulsion was prepared by mixing a surfactant (Brij35), co-surfactant, organic solvent, water, and fluorescein as an organic fluorophore. The sizes of the silica nanoparticles were successfully controlled in the reverse microemulsion using Brij35 by changing the water-to-Brij35 ratio and by adding HCl. Initially, tetraethylorthosilicate was hydrolyzed by adding NH{sub 4}OH as a catalyst and then polymerized to generate core fluorescent silica nanoparticles with fluorescein. 3-(Aminopropyl)triethoxysilane (APTS) was sequentially added into the reaction mixture, and reacted on the surface of pre-generated core silica nanoparticles to form the second layer in the form of a shell. The second silica layer that was derived from the condensation of APTS effectively protected the fluorescein dye within the silica matrix. This is a novel and simple synthetic approach to generate highly fluorescent, monodispersed silica nanoparticles by doping organic molecules into a silica matrix.Graphical Abstract.

Multifunctional nanomedicine with silica: Role of silica in nanoparticles for theranostic, imaging, and drug monitoring.

Science.gov (United States)

Chen, Fang; Hableel, Ghanim; Zhao, Eric Ruike; Jokerst, Jesse V

2018-07-01

The idea of multifunctional nanomedicine that enters the human body to diagnose and treat disease without major surgery is a long-standing dream of nanomaterials scientists. Nanomaterials show incredible properties that are not found in bulk materials, but achieving multi-functionality on a single material remains challenging. Integrating several types of materials at the nano-scale is critical to the success of multifunctional nanomedicine device. Here, we describe the advantages of silica nanoparticles as a tool for multifunctional nano-devices. Silica nanoparticles have been intensively studied in drug delivery due to their biocompatibility, degradability, tunable morphology, and ease of modification. Moreover, silica nanoparticles can be integrated with other materials to obtain more features and achieve theranostic capabilities and multimodality for imaging applications. In this review, we will first compare the properties of silica nanoparticles with other well-known nanomaterials for bio-applications and describe typical routes to synthesize and integrate silica nanoparticles. We will then highlight theranostic and multimodal imaging application that use silica-based nanoparticles with a particular interest in real-time monitoring of therapeutic molecules. Finally, we will present the challenges and perspective on future work with silica-based nanoparticles in medicine. Copyright © 2018 Elsevier Inc. All rights reserved.

Amorphous silica studied by high energy x-ray diffraction

DEFF Research Database (Denmark)

Poulsen, H.F.; Neuefeind, J.; Neumann, H.B.

1995-01-01

-ray and neutron data. A feasibility study of amorphous silica has been performed at 95 keV, using a wiggler synchrotron beam-line at HASYLAB and a cylindrical sample, 3 mm in diameter. The range of Q between 0.8 and 32 Angstrom(-1) was covered. A thorough discussion of the experimental challenges is given...

Study of silica coatings degradation under laser irradiation and in controlled environment

International Nuclear Information System (INIS)

Becker, S.

2006-11-01

Performances of optical components submitted to high laser intensities are usually determined by their laser-induced damage threshold. This value represents the highest density of energy (fluence) sustainable by the component before its damage. When submitted to laser fluences far below this threshold, optical performances may also decrease with time. The degradation processes depend on laser characteristics, optical materials, and environment around the component. Silica being the most used material in optics, the aim of this study was to describe and analyse the physical-chemical mechanisms responsible for laser-induced degradation of silica coatings in controlled environment. Experimental results show that degradation is due to the growth of a carbon deposit in the irradiated zone. From these results, a phenomenological model has been proposed and validated with numerical simulations. Then, several technological solutions have been tested in order to reduce the laser-induced contamination of silica coatings. (author)

Preparation, purification, and characterization of aminopropyl-functionalized silica sol.

Science.gov (United States)

Pálmai, Marcell; Nagy, Lívia Naszályi; Mihály, Judith; Varga, Zoltán; Tárkányi, Gábor; Mizsei, Réka; Szigyártó, Imola Csilla; Kiss, Teréz; Kremmer, Tibor; Bóta, Attila

2013-01-15

A new, simple, and "green" method was developed for the surface modification of 20 nm diameter Stöber silica particles with 3-aminopropyl(diethoxy)methylsilane in ethanol. The bulk polycondensation of the reagent was inhibited and the stability of the sol preserved by adding a small amount of glacial acetic acid after appropriate reaction time. Centrifugation, ultrafiltration, and dialysis were compared in order to choose a convenient purification technique that allows the separation of unreacted silylating agent from the nanoparticles without destabilizing the sol. The exchange of the solvent to acidic water during the purification yielded a stable colloid, as well. Structural and morphological analysis of the obtained aminopropyl silica was performed using transmission electron microscopy (TEM), dynamic light scattering (DLS) and zeta potential measurements, Fourier-transform infrared (FTIR), (13)C and (29)Si MAS nuclear magnetic resonance (NMR) spectroscopies, as well as small angle X-ray scattering (SAXS). Our investigations revealed that the silica nanoparticle surfaces were partially covered with aminopropyl groups, and multilayer adsorption followed by polycondensation of the silylating reagent was successfully avoided. The resulting stable aminopropyl silica sol (ethanolic or aqueous) is suitable for biomedical uses due to its purity. Copyright © 2012 Elsevier Inc. All rights reserved.

Effect of temperature on physical and mechanical properties of concrete containing silica fume

International Nuclear Information System (INIS)

Saad, M.; Hanna, G.B.; Abo-El-Enein, S.A.; Kotkata, M.F.

1996-01-01

Heat-resistant materials are usually used for structural purposes. The need for such building materials is particularly important in the chemical and metallurgical industries and for the thermal shieldings of nuclear power plants. Thus the effect of high temperatures on physical and mechanical properties of concrete was investigated. In this study ordinary Portland cement has been partially replaced by ratios of silica fume. The heat treatment temperature varied from 100 to 600 C by increments of 100 C for three hours without any load. Concrete specimens were treated at each temperature level. The specimens were heated under the same condition for each temperature level. Comparison between physical and mechanical properties during heat treatment were investigated. All specimens were moist-cured for 28 days after casting. Tests were carried out on specimens cooled slowly to room temperature after heating. Results of this investigation indicated that the replacement of ordinary Portland cement by 10% silica fume by weight improved the compressive strength by about 64.6%, but replacement of ordinary Portland cement by silica fume by ratios 20 and 30% improved the compressive strength by only 28% at 600 C. This could be attributed to the additional tobermorite gel (CSH phase) which formed due to the reaction of silica fume with Ca(OH) 2

Acoustic emission monitoring of crack formation during alkali silica\

Czech Academy of Sciences Publication Activity Database

Lokajíček, Tomáš; Přikryl, R.; Šachlová, Š.; Kuchařová, A.

2017-01-01

Roč. 220, MAR 30 (2017), s. 175-182 ISSN 0013-7952 R&D Projects: GA ČR(CZ) GAP104/12/0915 Institutional support: RVO:67985831 Keywords : Alkali-silica reaction * accelerated expansion test * ultrasonic sounding * acoustic emission * backscattered electron imaging Subject RIV: JJ - Other Materials OBOR OECD: Materials engineering Impact factor: 2.569, year: 2016

Tuning dipolar magnetic interactions by controlling individual silica coating of iron oxide nanoparticles

Science.gov (United States)

Rivas Rojas, P. C.; Tancredi, P.; Moscoso Londoño, O.; Knobel, M.; Socolovsky, L. M.

2018-04-01

Single and fixed size core, core-shell nanoparticles of iron oxides coated with a silica layer of tunable thickness were prepared by chemical routes, aiming to generate a frame of study of magnetic nanoparticles with controlled dipolar interactions. The batch of iron oxides nanoparticles of 4.5 nm radii, were employed as cores for all the coated samples. The latter was obtained via thermal decomposition of organic precursors, resulting on nanoparticles covered with an organic layer that was subsequently used to promote the ligand exchange in the inverse microemulsion process, employed to coat each nanoparticle with silica. The amount of precursor and times of reaction was varied to obtain different silica shell thicknesses, ranging from 0.5 nm to 19 nm. The formation of the desired structures was corroborated by TEM and SAXS measurements, the core single-phase spinel structure was confirmed by XRD, and superparamagnetic features with gradual change related to dipolar interaction effects were obtained by the study of the applied field and temperature dependence of the magnetization. To illustrate that dipolar interactions are consistently controlled, the main magnetic properties are presented and analyzed as a function of center to center minimum distance between the magnetic cores.

Amorphous silica from rice husk at various temperatures

International Nuclear Information System (INIS)

Javed, S.J.; Feroze, N.; Tajwar, S.

2008-01-01

Rice husk is being used as a source of energy in many heat generating system because of its high calorific value and its availability in many rice producing areas. Rice husk contains approximately 20% silica which is presented in hydrated form. This hydrated silica can be retrieved as amorphous silica under controlled thermal conditions. Uncontrolled burning of rice husk produces crystalline silica which is not reactive silica but can be used as filler in many applications. Amorphous silica is reactive silica which has better market value due to its reactive nature in process industry. The present study deals with the production of amorphous silica at various temperatures from rice husk. Various ashes were prepared in tube furnace by changing the burning temperatures for fixed time intervals and analyzed by XRD. It has been observed that for two hours calculation's of rice husk renders mostly amorphous silica at 650 degree C where as at higher temperatures crystalline silica was obtained. (author)

Worker exposure to silica dust in South African non-mining industries in Gauteng: An exploratory study

CSIR Research Space (South Africa)

Khoza, NN

2012-06-01

Full Text Available %, and sandblasting 2.4%. The overall maximum and minimum exposures were 5.772 and 0.009 mg/m?, respectively. Conclusion: Workers are potentially at high risk of contracting silicosis and other diseases associated with respirable silica dust. Dust control... and monitoring were inadequate in the industries visited. It is recommended that an in-depth study be conducted and that airborne dust-control programmes be implemented. Key words: non-mining industries, silica dust, respirable crystalline silica dust...

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.

High-aluminum-affinity silica is a nanoparticle that seeds secondary aluminosilicate formation.

Directory of Open Access Journals (Sweden)

Ravin Jugdaohsingh

Full Text Available Despite the importance and abundance of aluminosilicates throughout our natural surroundings, their formation at neutral pH is, surprisingly, a matter of considerable debate. From our experiments in dilute aluminum and silica containing solutions (pH ~ 7 we previously identified a silica polymer with an extraordinarily high affinity for aluminium ions (high-aluminum-affinity silica polymer, HSP. Here, further characterization shows that HSP is a colloid of approximately 2.4 nm in diameter with a mean specific surface area of about 1,000 m(2 g(-1 and it competes effectively with transferrin for Al(III binding. Aluminum binding to HSP strongly inhibited its decomposition whilst the reaction rate constant for the formation of the β-silicomolybdic acid complex indicated a diameter between 3.6 and 4.1 nm for these aluminum-containing nanoparticles. Similarly, high resolution microscopic analysis of the air dried aluminum-containing silica colloid solution revealed 3.9 ± 1.3 nm sized crystalline Al-rich silica nanoparticles (ASP with an estimated Al:Si ratio of between 2 and 3 which is close to the range of secondary aluminosilicates such as imogolite. Thus the high-aluminum-affinity silica polymer is a nanoparticle that seeds early aluminosilicate formation through highly competitive binding of Al(III ions. In niche environments, especially in vivo, this may serve as an alternative mechanism to polyhydroxy Al(III species binding monomeric silica to form early phase, non-toxic aluminosilicates.

High-Aluminum-Affinity Silica Is a Nanoparticle That Seeds Secondary Aluminosilicate Formation

Science.gov (United States)

Jugdaohsingh, Ravin; Brown, Andy; Dietzel, Martin; Powell, Jonathan J.

2013-01-01

Despite the importance and abundance of aluminosilicates throughout our natural surroundings, their formation at neutral pH is, surprisingly, a matter of considerable debate. From our experiments in dilute aluminum and silica containing solutions (pH ~ 7) we previously identified a silica polymer with an extraordinarily high affinity for aluminium ions (high-aluminum-affinity silica polymer, HSP). Here, further characterization shows that HSP is a colloid of approximately 2.4 nm in diameter with a mean specific surface area of about 1,000 m2 g-1 and it competes effectively with transferrin for Al(III) binding. Aluminum binding to HSP strongly inhibited its decomposition whilst the reaction rate constant for the formation of the β-silicomolybdic acid complex indicated a diameter between 3.6 and 4.1 nm for these aluminum-containing nanoparticles. Similarly, high resolution microscopic analysis of the air dried aluminum-containing silica colloid solution revealed 3.9 ± 1.3 nm sized crystalline Al-rich silica nanoparticles (ASP) with an estimated Al:Si ratio of between 2 and 3 which is close to the range of secondary aluminosilicates such as imogolite. Thus the high-aluminum-affinity silica polymer is a nanoparticle that seeds early aluminosilicate formation through highly competitive binding of Al(III) ions. In niche environments, especially in vivo, this may serve as an alternative mechanism to polyhydroxy Al(III) species binding monomeric silica to form early phase, non-toxic aluminosilicates. PMID:24349573

Influence of granitic aggregates from Northeast Brazil on the alkali-aggregate reaction

Energy Technology Data Exchange (ETDEWEB)

Gomes Neto, David de Paiva; Santana, Rodrigo Soares de; Barreto, Ledjane Silva, E-mail: pvgomes@uol.com.br [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil). Dept. de Ciencias dos Materiais e Engenharia; Conceicao, Herbert; Lisboa, Vinicios Anselmo Carvalho [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil). Dept. de Geologia

2014-08-15

The alkali-aggregate reaction (AAR) in concrete structures is a problem that has concerned engineers and researchers for decades. This reaction occurs when silicates in the aggregates react with the alkalis, forming an expanded gel that can cause cracks in the concrete and reduce its lifespan. The aim of this study was to characterize three coarse granitic aggregates employed in concrete production in northeastern Brazil, correlating petrographic analysis with the kinetics of silica dissolution and the evolution of expansions in mortar bars, assisted by SEM/EDS, XRD, and EDX. The presence of grains showing recrystallization into individual microcrystalline quartz subgrains was associated with faster dissolution of silica and greater expansion in mortar bars. Aggregates showing substantial deformation, such as stretched grains of quartz with strong undulatory extinction, experienced slower dissolution, with reaction and expansion occurring over longer periods that could not be detected using accelerated tests with mortar bars. (author)

Health hazards due to the inhalation of amorphous silica

Energy Technology Data Exchange (ETDEWEB)

Merget, R.; Bruening, T. [Research Institute for Occupational Medicine (BGFA), Bochum (Germany); Bauer, T. [Bergmannsheil, University Hospital, Department of Internal Medicine, Division of Pneumonology, Allergology and Sleep Medicine, Bochum (Germany); Kuepper, H.U.; Breitstadt, R. [Degussa-Huels Corp., Wesseling (Germany); Philippou, S. [Department of Pathology, Augusta Krankenanstalten, Bochum (Germany); Bauer, H.D. [Research Institute for Hazardous Substances (IGF), Bochum (Germany)

2002-01-01

Occupational exposure to crystalline silica dust is associated with an increased risk for pulmonary diseases such as silicosis, tuberculosis, chronic bronchitis, chronic obstructive pulmonary disease (COPD) and lung cancer. This review summarizes the current knowledge about the health effects of amorphous (non-crystalline) forms of silica. The major problem in the assessment of health effects of amorphous silica is its contamination with crystalline silica. This applies particularly to well-documented pneumoconiosis among diatomaceous earth workers. Intentionally manufactured synthetic amorphous silicas are without contamination of crystalline silica. These synthetic forms may be classified as (1) wet process silica, (2) pyrogenic (''thermal'' or ''fumed'') silica, and (3) chemically or physically modified silica. According to the different physico-chemical properties, the major classes of synthetic amorphous silica are used in a variety of products, e.g. as fillers in the rubber industry, in tyre compounds, as free-flow and anti-caking agents in powder materials, and as liquid carriers, particularly in the manufacture of animal feed and agrochemicals; other uses are found in toothpaste additives, paints, silicon rubber, insulation material, liquid systems in coatings, adhesives, printing inks, plastisol car undercoats, and cosmetics. Animal inhalation studies with intentionally manufactured synthetic amorphous silica showed at least partially reversible inflammation, granuloma formation and emphysema, but no progressive fibrosis of the lungs. Epidemiological studies do not support the hypothesis that amorphous silicas have any relevant potential to induce fibrosis in workers with high occupational exposure to these substances, although one study disclosed four cases with silicosis among subjects exposed to apparently non-contaminated amorphous silica. Since the data have been limited, a risk of chronic bronchitis, COPD or

Health hazards due to the inhalation of amorphous silica

International Nuclear Information System (INIS)

Merget, R.; Bruening, T.; Bauer, T.; Kuepper, H.U.; Breitstadt, R.; Philippou, S.; Bauer, H.D.

2002-01-01

Occupational exposure to crystalline silica dust is associated with an increased risk for pulmonary diseases such as silicosis, tuberculosis, chronic bronchitis, chronic obstructive pulmonary disease (COPD) and lung cancer. This review summarizes the current knowledge about the health effects of amorphous (non-crystalline) forms of silica. The major problem in the assessment of health effects of amorphous silica is its contamination with crystalline silica. This applies particularly to well-documented pneumoconiosis among diatomaceous earth workers. Intentionally manufactured synthetic amorphous silicas are without contamination of crystalline silica. These synthetic forms may be classified as (1) wet process silica, (2) pyrogenic (''thermal'' or ''fumed'') silica, and (3) chemically or physically modified silica. According to the different physico-chemical properties, the major classes of synthetic amorphous silica are used in a variety of products, e.g. as fillers in the rubber industry, in tyre compounds, as free-flow and anti-caking agents in powder materials, and as liquid carriers, particularly in the manufacture of animal feed and agrochemicals; other uses are found in toothpaste additives, paints, silicon rubber, insulation material, liquid systems in coatings, adhesives, printing inks, plastisol car undercoats, and cosmetics. Animal inhalation studies with intentionally manufactured synthetic amorphous silica showed at least partially reversible inflammation, granuloma formation and emphysema, but no progressive fibrosis of the lungs. Epidemiological studies do not support the hypothesis that amorphous silicas have any relevant potential to induce fibrosis in workers with high occupational exposure to these substances, although one study disclosed four cases with silicosis among subjects exposed to apparently non-contaminated amorphous silica. Since the data have been limited, a risk of chronic bronchitis, COPD or emphysema cannot be excluded. There is no

Silica coated ionic liquid templated mesoporous silica nanoparticles ...

African Journals Online (AJOL)

A series of long chain pyridinium based ionic liquids 1-tetradecylpyridinium bromide, 1-hexadecylpyridinium bromide and 1-1-octadecylpyridinium bromide were used as templates to prepare silica coated mesoporous silica nanoparticles via condensation method under basic condition. The effects of alkyl chain length on ...

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

Science.gov (United States)

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

2009-01-01

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

GRIZZLY Model of Multi-Reactive Species Diffusion, Moisture/Heat Transfer and Alkali-Silica Reaction for Simulating Concrete Aging and Degradation

Energy Technology Data Exchange (ETDEWEB)

Huang, Hai [Idaho National Lab. (INL), Idaho Falls, ID (United States); Spencer, Benjamin W. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Cai, Guowei [Vanderbilt Univ., Nashville, TN (United States)

2015-09-01

Concrete is widely used in the construction of nuclear facilities because of its structural strength and its ability to shield radiation. The use of concrete in nuclear power plants for containment and shielding of radiation and radioactive materials has made its performance crucial for the safe operation of the facility. As such, when life extension is considered for nuclear power plants, it is critical to have accurate and reliable predictive tools to address concerns related to various aging processes of concrete structures and the capacity of structures subjected to age-related degradation. The goal of this report is to document the progress of the development and implementation of a fully coupled thermo-hydro-mechanical-chemical model in GRIZZLY code with the ultimate goal to reliably simulate and predict long-term performance and response of aged NPP concrete structures subjected to a number of aging mechanisms including external chemical attacks and volume-changing chemical reactions within concrete structures induced by alkali-silica reactions and long-term exposure to irradiation. Based on a number of survey reports of concrete aging mechanisms relevant to nuclear power plants and recommendations from researchers in concrete community, we’ve implemented three modules during FY15 in GRIZZLY code, (1) multi-species reactive diffusion model within cement materials; (2) coupled moisture and heat transfer model in concrete; and (3) anisotropic, stress-dependent, alkali-silica reaction induced swelling model. The multi-species reactive diffusion model was implemented with the objective to model aging of concrete structures subjected to aggressive external chemical attacks (e.g., chloride attack, sulfate attack, etc.). It considers multiple processes relevant to external chemical attacks such as diffusion of ions in aqueous phase within pore spaces, equilibrium chemical speciation reactions and kinetic mineral dissolution/precipitation. The moisture

Studying the loading effect of acidic type antioxidant on amorphous silica nanoparticle carriers

Science.gov (United States)

Ravinayagam, Vijaya; Rabindran Jermy, B.

2017-06-01

The study investigates the suitable nanosilica carriers to transport acidic type cargo molecules for potential targeted drug delivery application. Using phenolic acidic type antioxidant gallic acid (GA) as model compound, the present study investigates the loading effect of GA (0.3-15.9 mmol GA g-1 support) on textural characteristics of amorphous silica nanoparticles such as Q10 silica (1D), structured two-dimensional Si-MCM-41 (2D), and three-dimensional Si-SBA-16 (3D). The variation in the nature of textures after GA loading was analyzed using X-ray diffraction, N2 adsorption, FT-IR, scanning electron microscopy with energy dispersive X-ray spectroscopy, and high-resolution transmission electron microscopy. Among the nanocarriers, high adsorption of GA was found in the following order: Si-SBA-16 (3D)˜Si-KIT-6 (3D) > Si-MCM-41 (2D) > ultralarge pore FDU-12 (ULPFDU-12; 3D) > Q10 (1D)˜mesostructured cellular silica foam (MSU-F). 3D-type silicas Si-SBA-16 and KIT-6 were shown to maintain structural integrity at acidic condition (pH ˜3) and accommodate GA in non-crystalline form. In the case of ULPFDU-12 and MSU-F cellular foam, only crystalline deposition of GA occurs with a significant variation in the surface area and pore volume. [Figure not available: see fulltext.

Relationship between sol-gel conditions and enzyme stability: a case study with β-galactosidase/silica biocatalyst for whey hydrolysis.

Science.gov (United States)

Escobar, Sindy; Bernal, Claudia; Mesa, Monica

2015-01-01

The sol-gel process has been very useful for preparing active and stable biocatalysts, with the possibility of being reused. Especially those based on silica are well known. However, the study of the enzyme behavior during this process is not well understood until now and more, if the surfactant is involved in the synthesis mixture. This work is devoted to the encapsulation of β-galactosidase from Bacillus circulans in silica by sol-gel process, assisted by non-ionic Triton X-100 surfactant. The correlation between enzyme activity results for the β-galactosidase in three different environments (soluble in buffered aqueous reference solution, in the silica sol, and entrapment on the silica matrix) explains the enzyme behavior under stress conditions offered by the silica sol composition and gelation conditions. A stable β-galactosidase/silica biocatalyst is obtained using sodium silicate, which is a cheap source of silica, in the presence of non-ionic Triton X-100, which avoids the enzyme deactivation, even at 40 °C. The obtained biocatalyst is used in the whey hydrolysis for obtaining high value products from this waste. The preservation of the enzyme stability, which is one of the most important challenges on the enzyme immobilization through the silica sol-gel, is achieved in this study.

Coupling Reagent for UV/vis Absorbing Azobenzene-Based Quantitative Analysis of the Extent of Functional Group Immobilization on Silica.

Science.gov (United States)

Choi, Ra-Young; Lee, Chang-Hee; Jun, Chul-Ho

2018-05-18

A methallylsilane coupling reagent, containing both a N-hydroxysuccinimidyl(NHS)-ester group and a UV/vis absorbing azobenzene linker undergoes acid-catalyzed immobilization on silica. Analysis of the UV/vis absorption band associated with the azobenzene group in the adduct enables facile quantitative determination of the extent of loading of the NHS groups. Reaction of NHS-groups on the silica surface with amine groups of GOx and rhodamine can be employed to generate enzyme or dye-immobilized silica for quantitative analysis.

Hydrolysis of polycarbonate in sub-critical water in fused silica capillary reactor with in situ Raman spectroscopy

Science.gov (United States)

Pan, Z.; Chou, I-Ming; Burruss, R.C.

2009-01-01

The advantages of using fused silica capillary reactor (FSCR) instead of conventional autoclave for studying chemical reactions at elevated pressure and temperature conditions were demonstrated in this study, including the allowance for visual observation under a microscope and in situ Raman spectroscopic characterization of polycarbonate and coexisting phases during hydrolysis in subcritical water.

Electrochemical Studies of Graphene-like materials Synthesized by the Thermolyzed Asphalt Reaction

Science.gov (United States)

Xie, Yuqun

Developing a facile and cost effective synthetic method for producing graphene materials has been an attractive research topic in several disciplines. Chapter 3 demenstrates sheets of multilayered graphene-like paper materials more than 10 cm2 in area were synthesized in the "Thermolyzed Asphalt Reaction (TAR)". TAR is processed within open containers at 650 °C under atmospheric pressure without the need to exclude oxygen, which is the lowest reported temperature for chemical vapor deposition of graphene-based materials. It was found that multilayered graphene-like materials can be grown on amorphous substrates without catalysts. In chapter 4, further studies of the TAR mechanism have allowed sulfur to be identified as an important co-factor in multilayer graphene-like materials formation. Graphene-like material was produced from simple precursors such as elemental sulfur and cyclohexanol. A proposed scheme illustrates sulfur's role in the growth of graphene-like material based on thermogravimetric analyses. We hypothesize that elemental sulfur is involved with the dehydration/dehydrogenation and eventual crosslinking of cyclohexanol between 100-140 °C. In the range of 240-400 °C further dehydrogenation steps occur yielding an unidentified intermediate with a sharp Raman peak at 1450 cm-1 At 550 °C graphene-like Raman D and G bands appear along with the 1450 cm band of the intermediate. At 600 °C and higher temperatures, the intermediate peak is lost with only bands characteristic of graphene-like material being seen in the spectrum of the material synthesized from the University of Idaho Thermolyzed Asphalt Reaction (GUITAR). Sulfur as a key co-factor for GUITAR synthesis is reinforced by results found with other hydrocarbons. Other organics succeeded or failed in GUITAR formation based on melting and boiling considerations. The failure of the compounds with a boiling point below -89°C, melting point above 300°C is reasoned with the volatility of the

Reactive Diazonium-Modified Silica Fillers for High-Performance Polymers.

Science.gov (United States)

Sandomierski, Mariusz; Strzemiecka, Beata; Chehimi, Mohamed M; Voelkel, Adam

2016-11-08

We describe a simple way of modification of three silica-based fillers with in situ generated 4-hydroxymethylbenzenediazonium salt ( + N 2 -C 6 H 4 -CH 2 OH). The rationale for using a hydroxyl-functionalized diazonium salt is that it provides surface-functionalized fillers that can react with phenolic resins. The modification of silica by diazonium salts was assessed using Fourier transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS). FTIR spectroscopy permitted the tracking of benzene ring breathing and C-C. The absence of the characteristic N≡N stretching vibration in the 2200-2300 cm -1 range indicates the loss of the diazonium group. XPS results indicate a higher C/Si atomic ratio after the diazonium modification of fillers and the presence of π-π* C1s satellite peaks characteristic of the surface-tethered aromatic species. Adhesion of aryl layers to the silicas is excellent because they withstand harsh thermal and organic solvent treatments. Phenolic resins (used, for example, as binders in abrasive products) were filled with diazonium-modified silicas at 10-25 wt %. The reactivity of the fillers toward phenolic resins was evaluated by the determination of the flow distance. After annealing at 180 °C, the diazonium-modified silica/phenolic resin composites were mechanically tested using the three-point flexural method. The flexural strength was found to be up to 35% higher than that of the composites prepared without any diazonium salts. Diazonium-modified silica with surface-bound -CH 2 -OH groups is thus ideal reactive filler for phenolic resins. Such filler ensures interfacial chemical reactions with the matrix and imparts robust mechanical properties to the final composites. This specialty diazonium-modified silica will find potential application as fillers in the composites for the abrasive industry. More generally, aryl diazonium salts are a unique new series of compounds for tailoring the surface properties of fillers

Effects of Silica in Rice Husk Ash (RHA) in producing High Strength Concrete

OpenAIRE

Kartini, K; Nurul Nazierah, M.Y; Zaidahtulakmal, M.Z; Siti Aisyah, G

2012-01-01

High strength concrete (HSC) are known to have a higher amount of cement binder in the mix design properties with low w/b ratio. The high mass of cement content produced substantial heat liberation in the concrete due to the reaction between cement and water, which can lead to cracking. Additive likes silica fume is too expensive to use in the HSC in order to overcome the problems, however, the initiative of utilizing the rice husk ash (RHA) which have high silica content are apply for the de...

Sol-Generating Chemical Vapor into Liquid (SG-CViL) deposition – a facile method for encapsulation of diverse cell types in silica matrices

Energy Technology Data Exchange (ETDEWEB)

Johnston, Robert [New Mexico Inst. of Mining and Technology, Socorro, NM (United States). Materials Engineering Dept.; Rogelj, Snezna [New Mexico Inst. of Mining and Technology, Socorro, NM (United States). Biology Dept.; Harper, Jason C. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Bioenergy and Biodefense Technologies Dept.; Tartis, Michaelann [New Mexico Inst. of Mining and Technology, Socorro, NM (United States). Materials and Chemical Engineering Dept.

2014-12-12

In nature, cells perform a variety of complex functions such as sensing, catalysis, and energy conversion which hold great potential for biotechnological device construction. However, cellular sensitivity to ex vivo environments necessitates development of bio–nano interfaces which allow integration of cells into devices and maintain their desired functionality. In order to develop such an interface, the use of a novel Sol-Generating Chemical Vapor into Liquid (SG-CViL) deposition process for whole cell encapsulation in silica was explored. In SG-CViL, the high vapor pressure of tetramethyl orthosilicate (TMOS) is utilized to deliver silica into an aqueous medium, creating a silica sol. Cells are then mixed with the resulting silica sol, facilitating encapsulation of cells in silica while minimizing cell contact with the cytotoxic products of silica generating reactions (i.e. methanol), and reduce exposure of cells to compressive stresses induced from silica condensation reactions. Using SG-CVIL, Saccharomyces cerevisiae (S. cerevisiae) engineered with an inducible beta galactosidase system were encapsulated in silica solids and remained both viable and responsive 29 days post encapsulation. By tuning SG-CViL parameters, thin layer silica deposition on mammalian HeLa and U87 human cancer cells was also achieved. Thus, the ability to encapsulate various cell types in either a multi cell (S. cerevisiae) or a thin layer (HeLa and U87 cells) fashion shows the promise of SG-CViL as an encapsulation strategy for generating cell–silica constructs with diverse functions for incorporation into devices for sensing, bioelectronics, biocatalysis, and biofuel applications.

Silica-supported silicotungstic acid: A study by X-ray photoelectron spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Berry, Frank J.; Derrick, Glyn R. [Department of Chemistry and Analytical Sciences, Robert Hooke Building, Open University, Walton Hall, Milton Keynes, MK7 6AA (United Kingdom); Marco, Jose F. [Instituto de Quimica -Fisica ' Rocasolano' , Consejo Superior de Investigaciones Cientificas, Serrano 119, 28006 Madrid (Spain); Mortimer, Michael [Department of Chemistry and Analytical Sciences, Robert Hooke Building, Open University, Walton Hall, Milton Keynes, MK7 6AA (United Kingdom)], E-mail: m.mortimer@open.ac.uk

2009-04-15

W 4f and O 1s X-ray photoelectron spectra for silicotungstic acid, H{sub 4}SiW{sub 12}O{sub 40}, in pure and silica-supported form are reported. W 4f XP spectra for the supported acid are analysed in terms of contributions from two W(VI) spin-orbit doublets arising from tungsten atoms in terminal W=O bonds some of which directly interact with the silica surface. At low loading (3.2 wt.%) significant changes in the relative contributions and binding energies of the two spin-orbit doublets are taken as evidence of a strong interaction of individual [SiW{sub 12}O{sub 40}]{sup 4-} anions with highly active sites on the silica surface. It is suggested that selective ordering of silanol groups can occur on the silica surface in order to accommodate the adsorption of individual [SiW{sub 12}O{sub 40}]{sup 4-} anions.

Silica nanoparticles for the layer-by-layer assembly of fully electro-active cytochrome c multilayers

Directory of Open Access Journals (Sweden)

Feifel Sven C

2011-12-01

Full Text Available Abstract Background For bioanalytical systems sensitivity and biomolecule activity are critical issues. The immobilization of proteins into multilayer systems by the layer-by-layer deposition has become one of the favorite methods with this respect. Moreover, the combination of nanoparticles with biomolecules on electrodes is a matter of particular interest since several examples with high activities and direct electron transfer have been found. Our study describes the investigation on silica nanoparticles and the redox protein cytochrome c for the construction of electro-active multilayer architectures, and the electron transfer within such systems. The novelty of this work is the construction of such artificial architectures with a non-conducting building block. Furthermore a detailed study of the size influence of silica nanoparticles is performed with regard to formation and electrochemical behavior of these systems. Results We report on interprotein electron transfer (IET reaction cascades of cytochrome c (cyt c immobilized by the use of modified silica nanoparticles (SiNPs to act as an artificial matrix. The layer-by-layer deposition technique has been used for the formation of silica particles/cytochrome c multilayer assemblies on electrodes. The silica particles are characterized by dynamic light scattering (DLS, Fourier transformed infrared spectroscopy (FT-IR, Zeta-potential and transmission electron microscopy (TEM. The modified particles have been studied with respect to act as an artificial network for cytochrome c and to allow efficient interprotein electron transfer reactions. We demonstrate that it is possible to form electro-active assemblies with these non-conducting particles. The electrochemical response is increasing linearly with the number of layers deposited, reaching a cyt c surface concentration of about 80 pmol/cm2 with a 5 layer architecture. The interprotein electron transfer through the layer system and the

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.

A comparative study of three different synthesis routes for hydrophilic fluorophore-doped silica nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Shahabi, Shakiba [University of Bremen, Advanced Ceramics (Germany); Treccani, Laura, E-mail: treccani@petroceramics.com [Petroceramics S.p.A., Kilometro Rosso Science Park (Italy); Rezwan, Kurosch [University of Bremen, Advanced Ceramics (Germany)

2016-01-15

The synthesis of fluorophore-doped silica nanoparticles (FDS NPs) with two conventional approaches, Stöber and microemulsion, as well as a novel amino acid-catalyzed seeds regrowth technique (ACSRT) is presented. The efficiency of each applied synthesis route toward incorporation of selected hydrophilic fluorophores, including rhodamine B isothiocyanate and fluorescein isothiocyanate, without and with an amine-containing crosslinker, into silica matrix was systematically studied. Our results clearly highlight the advantages of ACSRT to obtain FDS NPs with a remarkable encapsulation efficiency, high quantum yield, and enhanced stability against bleaching and dye leaking due to efficient embedding of the dyes inside silica network even without the amine-containing silane reagent. Moreover, evaluation of photostability of FDNPs internalized in human bone cells demonstrates the merits of ACSRT.

Development of fluorocarbon/silica composites via sol/gel process

International Nuclear Information System (INIS)

Ferreira, Max P.; Maria, Daniel A.; Gomes, Luiza M.F.

2009-01-01

Fluorocarbon/silica composites have interesting physical-chemical properties, combining the great resistance to chemical products, the electric insulation, and the thermal stability of fluorine polymers with the optical, magnetic, and dielectric properties of silica. Due to the unique mechanical, thermal, and dielectric properties of fluorocarbon and silica composites, there is interest in their application in the development of fuel cells, the production of integrated circuit boards (ICB), and packages for the transportation of integrated circuits. The sol-gel process is a chemical route to prepare ceramic materials with specific properties that are hard or impossible to obtain by conventional methods. Fluorocarbon/silica composites were obtained by the sol-gel method from tetramethoxysilane - TMOS and fluorinated hydrocarbons with low molecular weight and main chains with 10 - 20 carbon atoms previously obtained from PTFE scraps irradiated with a 60 Co γ source in oxygen atmosphere with a dose of 1 MGy. Syntheses were performed in 125-mL reaction flasks in basic medium at 35 deg C and in acid medium at 60 deg C with N-N dimethylformamide as a chemical additive for drying control. After synthesis, the material was thermally treated in an oven with electronic temperature control. The monoliths obtained were characterized by Fourier transform infrared spectroscopy (FTIR), electron microprobe and by a standard nitrogen adsorption-desorption technique. (author)

Molecular Dynamics Simulations of Water Droplets On Hydrophilic Silica Surfaces

DEFF Research Database (Denmark)

Zambrano, Harvey A; Walther, Jens Honore; Jaffe, Richard L.

2009-01-01

and DNA microarrays technologies.Although extensive experimental, theoretical and computational work has been devoted to study the nature of the interaction between silica and water, at the molecular level a complete understanding of silica-water systems has not been reached. Contact angle computations...... dynamics (MD) simulations of a hydrophilic air-water-silica system using the MD package FASTTUBE. We employ quantum chemistry calculation to obtain air-silica interaction parameters for the simulations. Our simulations are based in the following force fields: i) The silica-silica interaction is based...... of water droplets on silica surfaces offers a useful fundamental and quantitative measurement in order to study chemical and physical properties of water-silica systems. For hydrophobic systems the static and dynamic properties of the fluid-solid interface are influenced by the presence of air. Hence...

Development Of Silica Potassium Fertilizers From Trass Rock With Calcination Process

Science.gov (United States)

Wahyusi, KN; Siswanto

2018-01-01

Rocks and sand mines have important benefits for life. With the many benefits of rocks, it is a pity if Indonesia has a lot of raw material reserves waste it. Examples of the benefits of rocks that can be converted into silica potassium fertilizer by reacting with potassium hydroxide. Examples of rocks that can be taken trass rock. The procedure for making silica potassium is by reacting 100 mesh trass rock with KOH and K2CO3 reagents whose composition is arranged by weight ratio, where the base of the trass rock is 100 gr. The process is carried out at a temperature of 1.250 °C with a reaction time of 1 hour. The results obtained are the best silica potassium fertilizer for K2CO3 reagent which is 500gr: 74gr with SiO2 content: 26.8% and K2O content: 27.3%, with water solubility 24.02%, while for silica potassium fertilizer product from The best trass rock for KOH reagent is with a mol ratio of 400 gr : 60 gr with SiO2 content : 23.6% and K2O content: 22.2%, with 25.65% water solubility. The pore size of silica potassium fertilizer product of this trass rock, the range 350 - 1000 nm.

Silica-Immobilized Enzyme Reactors

Science.gov (United States)

2007-08-01

Silica-IMERs 14 implicated in neurological disorders such as Schizophrenia and Parkinson’s disease.[86] Drug discovery for targets that can alter the...primarily the activation of prodrugs and proantibiotics for cancer treatments or antibiotic therapy , respectively.[87] Nitrobenzene nitroreductase was...BuChE) Monolith disks* Packed Silica Biosilica Epoxide- Silica Silica-gel Enzyme Human AChE Human AChE Human AChE Equine BuChE Human

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.

MASS BALANCE OF SILICA IN STRAW FROM THE PERSPECTIVE OF SILICA REDUCTION IN STRAW PULP

Directory of Open Access Journals (Sweden)

Celil Atik,

2012-06-01

Full Text Available The high silica content of wheat straw is an important limiting factor for straw pulping. High silica content complicates processing and black liquor recovery, wears out factory installations, and lowers paper quality. Each section of wheat straw has different cells and chemical compositions and thus different silica content. In this work, the silica content of balled straw samples were examined according to their physical components, including internodes, nodes, leaves (sheath and blade, rachis, grain, other plant bodies, and other plant spikes. Mass distribution of silica was determined by a dry ashing method. Half (50.90% of the silica comes from leaves, and its mechanical separation will reduce the silica content in wheat straw pulp significantly. Destroying silica bodies by sonication will increase the strength properties of straw pulp.

A Study on Silica Sand Quality in Yazaram and Mugulbu Deposits ...

African Journals Online (AJOL)

The suitability of silica sand deposits of Yazaram and Mugulbu in Mubi South Local Government Area of Adamawa State, Nigeria for commercial glass production were assessed based on the chemical and physical properties of the silica sand samples collected along the river side's. Test was carried out at the National ...

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

Uptake of silica covered Quantum Dots into living cells: Long term vitality and morphology study on hyaluronic acid biomaterials

International Nuclear Information System (INIS)

D'Amico, Michele; Fiorica, Calogero; Palumbo, Fabio Salvatore; Militello, Valeria; Leone, Maurizio; Dubertret, Benoit; Pitarresi, Giovanna; Giammona, Gaetano

2016-01-01

Quantum Dots (QDs) are promising very bright and stable fluorescent probes for optical studies in the biological field but water solubility and possible metal bio-contamination need to be addressed. In this work, a simple silica-QD hybrid system is prepared and the uptake in bovine chondrocytes living cells without any functionalization of the external protective silica shield is demonstrated. Moreover, long term treated cells vitality (up to 14 days) and the transfer of silica-QDs to the next cell generations are here reported. Confocal fluorescence microscopy was also used to determine the morphology of the so labelled cells and the relative silica-QDs distribution. Finally, we employ silica-QD stained chondrocytes to characterize, as proof of concept, hydrogels obtained from an amphiphilic derivative of hyaluronic acid (HA-EDA-C _1_8) functionalized with different amounts of the RGD peptide. - Highlights: • Non functionalized silica-quantum dots fluorescent nanoparticles uptake is observed. • Morphology studies of such cells could be done by confocal fluorescence microscopy. • Labelled chondrocytes are viable until at least 14 days. • RGD functionalized Hyaluronic Acid hydrogels are studied as cell scaffolds. • Chondrocyte are promptly attached on RGD-functionalized hydrogels.

Uptake of silica covered Quantum Dots into living cells: Long term vitality and morphology study on hyaluronic acid biomaterials

Energy Technology Data Exchange (ETDEWEB)

D' Amico, Michele [Dip. Biomedico di Medicina Interna e Specialistica, Universitá degli Studi di Palermo, Piazza delle Cliniche, 2, 90127 Palermo (Italy); Dip. di Fisica e Chimica, Universitá degli Studi di Palermo, Viale delle Scienze, Ed. 18, 90128 Palermo (Italy); Fiorica, Calogero, E-mail: calogero.fiorica@unipa.it [Dip. di Scienze e Tecnologie Molecolari e Biomolecolari, Sezione di Chimica e Tecnologie Farmaceutiche, Universitá degli Studi di Palermo, Via Archirafi, 28, 90136 Palermo (Italy); Palumbo, Fabio Salvatore [Dip. di Scienze e Tecnologie Molecolari e Biomolecolari, Sezione di Chimica e Tecnologie Farmaceutiche, Universitá degli Studi di Palermo, Via Archirafi, 28, 90136 Palermo (Italy); Militello, Valeria; Leone, Maurizio [Dip. di Fisica e Chimica, Universitá degli Studi di Palermo, Viale delle Scienze, Ed. 18, 90128 Palermo (Italy); Dubertret, Benoit [Laboratoire de Physique et d’Etude des Matèriaux, ESPCI-ParisTech, PSL Research University, Sorbonne Universitè UPMC Univ. Paris 06, CNRS, 10 rue Vauquelin, 75005 Paris (France); Pitarresi, Giovanna; Giammona, Gaetano [Dip. di Scienze e Tecnologie Molecolari e Biomolecolari, Sezione di Chimica e Tecnologie Farmaceutiche, Universitá degli Studi di Palermo, Via Archirafi, 28, 90136 Palermo (Italy)

2016-10-01

Quantum Dots (QDs) are promising very bright and stable fluorescent probes for optical studies in the biological field but water solubility and possible metal bio-contamination need to be addressed. In this work, a simple silica-QD hybrid system is prepared and the uptake in bovine chondrocytes living cells without any functionalization of the external protective silica shield is demonstrated. Moreover, long term treated cells vitality (up to 14 days) and the transfer of silica-QDs to the next cell generations are here reported. Confocal fluorescence microscopy was also used to determine the morphology of the so labelled cells and the relative silica-QDs distribution. Finally, we employ silica-QD stained chondrocytes to characterize, as proof of concept, hydrogels obtained from an amphiphilic derivative of hyaluronic acid (HA-EDA-C {sub 18}) functionalized with different amounts of the RGD peptide. - Highlights: • Non functionalized silica-quantum dots fluorescent nanoparticles uptake is observed. • Morphology studies of such cells could be done by confocal fluorescence microscopy. • Labelled chondrocytes are viable until at least 14 days. • RGD functionalized Hyaluronic Acid hydrogels are studied as cell scaffolds. • Chondrocyte are promptly attached on RGD-functionalized hydrogels.

The role of residual cracks on alkali silica reactivity of recycled glass aggregates

DEFF Research Database (Denmark)

Maraghechi, Hamed; Shafaatian, Seyed-Mohammad-Hadi; Fischer, Gregor

2012-01-01

Despite its environmental and economical advantages, crushed recycled glass has limited application as concrete aggregates due to its deleterious alkali-silica reaction. To offer feasible mitigation strategies, the mechanism of ASR should be well understood. Recent research showed that unlike some...

Epoxy Crosslinked Silica Aerogels (X-Aerogels)

Science.gov (United States)

fabrizio, Eve; Ilhan, Faysal; Meador, Mary Ann; Johnston, Chris; Leventis, Nicholas

2004-01-01

NASA is interested in the development of strong lightweight materials for the dual role of thermal insulator and structural component for space vehicles; freeing more weight for useful payloads. Aerogels are very-low density materials (0.010 to 0.5 g/cc) that, due to high porosity (meso- and microporosity), can be, depending on the chemical nature of the network, ideal thermal insulators (thermal conductivity approx. 15 mW/mK). However, aerogels are extremely fragile. For practical application of aerogels, one must increase strength without compromising the physical properties attributed to low density. This has been achieved by templated growth of an epoxy polymer layer that crosslinks the "pearl necklace" network of nanoparticles: the framework of a typical silica aerogel. The requirement for conformal accumulation of the epoxy crosslinker is reaction both with the surface of silica and with itself. After cross-linking, the strength of a typical aerogel monolith increases by a factor of 200, in the expense of only a 2-fold increase in density. Strength is increased further by coupling residual unreacted epoxides with diamine.

Anchoring selenido-carbonyl ruthenium clusters to functionalized silica xerogels

International Nuclear Information System (INIS)

Cauzzi, Daniele; Graiff, Claudia; Pattacini, Roberto; Predieri, Giovanni; Tiripicchio, Antonio

2003-01-01

Silica Xerogels containing carbonyl Ru 3 Se 2 nido clusters were prepared in three different ways. The simple dispersion of [Ru 3 (μ 3 -Se) 2 (CO) 7 (PPh 3 ) 2 ] via sol gel process produces an inhomogeneous material; by contrast, homogeneous xerogels were obtained by reaction of [Ru 3 (μ 3 -Se) 2 (CO) 8 (PPh 3 )] with functionalized xerogels containing grafted diphenylphosphine moieties and by reaction of [Ru 3 (CO) 12 ] with a xerogel containing grafted phosphine-selenide groups. The reaction between [Ru 3 (CO) 12 ] and dodecyl diphenylphosphine selenide led to the formation of four selenido carbonyl clusters, which are soluble in hydrocarbon solvents and can be deposited as thin films from their solution by slow evaporation. (author)

Preparation of sponge-reinforced silica aerogels from tetraethoxysilane and methyltrimethoxysilane for oil/water separation

Science.gov (United States)

Li, Ming; Jiang, Hongyi; Xu, Dong

2018-04-01

Polyurethane sponge-reinforced silica aerogels based on tetraethoxysilane (TEOS) and methyltrimethoxysilane (MTMS) were fabricated by a facile method through sol-gel reaction followed by ambient pressure drying. In sponge-reinforced silica aerogels, nanoporous aerogel aggregates fill in the pores of polyurethane sponge. The sponge-reinforced aerogels are hydrophobic and oleophilic and show extremely high absorption for machine oil (10.6 g g‑1 for TEOS-based aerogel and 9.2 g g‑1 for MTMS-based aerogel). In addition, the sponge-reinforced aerogel composites exhibit notable improvements with regards to mechanical properties. The compressive strength was enhanced obviously up to about 349 KPa for TEOS-based aerogel and 60 KPa for MTMS-based aerogel. Specially, sponge-reinforced silica aerogels based on MTMS drastically shrank upon loading and then recovered to the original size when unloaded. The property differences of the sponge-reinforced silica aerogels caused by the two precursors were discussed in terms of morphologies, pore size distributions and chemical structure.

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.

Study of Physical Properties of Nano-Silica Coated Cotton Textiles

OpenAIRE

Sidra Saleemi; Farooq Ahmed; Samandar Malik

2015-01-01

This research was aimed to investigate the effect of silica sol-gel coating on air permeability, stiffness and tensile properties of dyed cotton fabric. Various concentrations of silica nanoparticles were applied on dyed cotton substrate using two different cross-linkers through sol-gel method. The homogenous sol-gel coating dispersions were prepared by using an ultrasonicator. Coated samples were tested for mechanical and comfort properties such as tensile strength, stiffness, crease recover...

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.

Stability studies of colloidal silica dispersions in binary solvent mixtures

International Nuclear Information System (INIS)

Bean, Keith Howard

1997-01-01

A series of monodispersed colloidal silica dispersions, of varying radii, has been prepared. These particles are hydrophilic in nature due to the presence of surface silanol groups. Some of the particles have been rendered hydrophobic by terminally grafting n-alkyl (C 18 ) chains to the surface. The stability of dispersions of these various particles has been studied in binary mixtures of liquids, namely (i) ethanol and cyclohexane, and (ii) benzene and n-heptane. The ethanol - cyclohexane systems have been studied using a variety of techniques. Adsorption excess isotherms have been established and electrophoretic mobility measurements have been made. The predicted stability of the dispersions from D.V.L.O. calculations is compared to the observed stability. The hydrophilic silica particles behave as predicted by the calculations, with the zeta potential decreasing and the van der Waals attraction increasing with increasing cyclohexane concentration. The hydrophobic particles behave differently than expected, and the stability as a function of solvent mixture composition does not show a uniform trend. The effect of varying the coverage of C 18 chains on the surface and the effect of trace water in the systems has also been investigated. Organophilic silica dispersions in benzene - n-heptane solvent mixtures show weak aggregation and phase separation into a diffuse 'gas-like' phase and a more concentrated 'liquid-like' phase, analogous to molecular condensation processes. Calculations of the van der Waals potential as a function of solvent mixture composition show good agreement with the observed stability. Determination of the number of particles in each phase at equilibrium allows the energy of flocculation to be determined using a simple thermodynamic relationship. Finally, the addition of an AB block copolymer to organophilic silica particles in benzene n-heptane solvent mixtures has been shown to have a marked effect on the dispersion stability. This stability

Nanoparticles affect PCR primarily via surface interactions with PCR components: using amino-modified silica-coated magnetic nanoparticles as a main model

Science.gov (United States)

Nanomaterials have been widely reported to affect the polymerase chain reaction (PCR). However, many studies in which these effects were observed were not comprehensive, and many of the proposed mechanisms have been primarily speculative. In this work, we used amino-modified silica-coated magnetic n...

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.

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

Reinforcement of natural rubber hybrid composites based on marble sludge/Silica and marble sludge/rice husk derived silica

Directory of Open Access Journals (Sweden)

Khalil Ahmed

2014-03-01

Full Text Available A research has been carried out to develop natural rubber (NR hybrid composites reinforced with marble sludge (MS/Silica and MS/rice husk derived silica (RHS. The primary aim of this development is to scrutinize the cure characteristics, mechanical and swelling properties of such hybrid composite. The use of both industrial and agricultural waste such as marble sludge and rice husk derived silica has the primary advantage of being eco-friendly, low cost and easily available as compared to other expensive fillers. The results from this study showed that the performance of NR hybrid composites with MS/Silica and MS/RHS as fillers is extremely better in mechanical and swelling properties as compared with the case where MS used as single filler. The study suggests that the use of recently developed silica and marble sludge as industrial and agricultural waste is accomplished to provide a probable cost effective, industrially prospective, and attractive replacement to the in general purpose used fillers like china clay, calcium carbonate, and talc.

Agmatine attenuates silica-induced pulmonary fibrosis.

Science.gov (United States)

El-Agamy, D S; Sharawy, M H; Ammar, E M

2014-06-01

There is a large body of evidence that nitric oxide (NO) formation is implicated in mediating silica-induced pulmonary fibrosis. As a reactive free radical, NO may not only contribute to lung parenchymal tissue injury but also has the ability to combine with superoxide and form a highly reactive toxic species peroxynitrite that can induce extensive cellular toxicity in the lung tissues. This study aimed to explore the effect of agmatine, a known NO synthase inhibitor, on silica-induced pulmonary fibrosis in rats. Male Sprague Dawley rats were treated with agmatine for 60 days following a single intranasal instillation of silica suspension (50 mg in 0.1 ml saline/rat). The results revealed that agmatine attenuated silica-induced lung inflammation as it decreased the lung wet/dry weight ratio, protein concentration, and the accumulation of the inflammatory cells in the bronchoalveolar lavage fluid. Agmatine showed antifibrotic activity as it decreased total hydroxyproline content of the lung and reduced silica-mediated lung inflammation and fibrosis in lung histopathological specimen. In addition, agmatine significantly increased superoxide dismutase (p Agmatine also reduced silica-induced overproduction of pulmonary nitrite/nitrate as well as tumor necrosis factor α. Collectively, these results demonstrate the protective effects of agmatine against the silica-induced lung fibrosis that may be attributed to its ability to counteract the NO production, lipid peroxidation, and regulate cytokine effects. © The Author(s) 2014.

A Demonstration of Concrete Structural Health Monitoring Framework for Degradation due to Alkali-Silica Reaction

Energy Technology Data Exchange (ETDEWEB)

Mahadevan, Sankaran [Idaho National Lab. (INL), Idaho Falls, ID (United States); Agarwal, Vivek [Idaho National Lab. (INL), Idaho Falls, ID (United States); Neal, Kyle [Idaho National Lab. (INL), Idaho Falls, ID (United States); Nath, Paromita [Idaho National Lab. (INL), Idaho Falls, ID (United States); Bao, Yanqing [Idaho National Lab. (INL), Idaho Falls, ID (United States); Cai, Guowei [Idaho National Lab. (INL), Idaho Falls, ID (United States); Orme, Peter [Idaho National Lab. (INL), Idaho Falls, ID (United States); Adams, Douglas [Idaho National Lab. (INL), Idaho Falls, ID (United States); Kosson, David [Idaho National Lab. (INL), Idaho Falls, ID (United States)

2016-04-01

Assessment and management of aging concrete structures in nuclear power plants require a more systematic approach than simple reliance on existing code margins of safety. Structural health monitoring of concrete structures aims to understand the current health condition of a structure based on heterogeneous measurements to produce high-confidence actionable information regarding structural integrity that supports operational and maintenance decisions. This ongoing research project is seeking to develop a probabilistic framework for health diagnosis and prognosis of aging concrete structures in a nuclear power plant that is subjected to physical, chemical, environment, and mechanical degradation. The proposed framework consists of four elements: monitoring, data analytics, uncertainty quantification and prognosis. This report focuses on degradation caused by ASR (alkali-silica reaction). Controlled specimens were prepared to develop accelerated ASR degradation. Different monitoring techniques – thermography, digital image correlation (DIC), mechanical deformation measurements, nonlinear impact resonance acoustic spectroscopy (NIRAS), and vibro-acoustic modulation (VAM) -- were used to detect the damage caused by ASR. Heterogeneous data from the multiple techniques was used for damage diagnosis and prognosis, and quantification of the associated uncertainty using a Bayesian network approach. Additionally, MapReduce technique has been demonstrated with synthetic data. This technique can be used in future to handle large amounts of observation data obtained from the online monitoring of realistic structures.

Modeling Time-Dependent Behavior of Concrete Affected by Alkali Silica Reaction in Variable Environmental Conditions.

Science.gov (United States)

Alnaggar, Mohammed; Di Luzio, Giovanni; Cusatis, Gianluca

2017-04-28

Alkali Silica Reaction (ASR) is known to be a serious problem for concrete worldwide, especially in high humidity and high temperature regions. ASR is a slow process that develops over years to decades and it is influenced by changes in environmental and loading conditions of the structure. The problem becomes even more complicated if one recognizes that other phenomena like creep and shrinkage are coupled with ASR. This results in synergistic mechanisms that can not be easily understood without a comprehensive computational model. In this paper, coupling between creep, shrinkage and ASR is modeled within the Lattice Discrete Particle Model (LDPM) framework. In order to achieve this, a multi-physics formulation is used to compute the evolution of temperature, humidity, cement hydration, and ASR in both space and time, which is then used within physics-based formulations of cracking, creep and shrinkage. The overall model is calibrated and validated on the basis of experimental data available in the literature. Results show that even during free expansions (zero macroscopic stress), a significant degree of coupling exists because ASR induced expansions are relaxed by meso-scale creep driven by self-equilibriated stresses at the meso-scale. This explains and highlights the importance of considering ASR and other time dependent aging and deterioration phenomena at an appropriate length scale in coupled modeling approaches.

Crystallization kinetic study of the lithium-disilicate bioceramic obtained from rice-husk silica starting powder

International Nuclear Information System (INIS)

Santos, F.A.; Santos, C.; Pinatti, D.G.; Davim, E.; Fernandes, M.H.F.V.

2011-01-01

In this work, the study of crystallization of the lithium disilicate glass-ceramic produced for alternative source (rice husk silica), and comparatively by commercial source (commercial silica) it was carried through. The stoichiometry 66%.mol SiO_2: 33%.mol LiO_2 was used. The kinetic studies of crystallization and calculations had been carried through thermal analysis (DTA), and were possible to study the behavior of the curves in accordance with the variation of taxes (5; 10; 15; e 20°C/min), of the granulometries 63 μm, 250μm and 1mm), and for the influence of the substitution commercial SiO_2 by rice husk. The structural characterization was carried through by X-Ray diffractometry (DRX) and scanning electron microscopy (MEV), for chemical characterization used X-Ray fluorescence (FRX). The preliminary results show that the substitution of the silica source is sufficiently promising, since the gotten properties are similar. (author)

High-Yield and Sustainable Production of Phosphatidylserine in Purely Aqueous Solutions via Adsorption of Phosphatidylcholine on Triton-X-100-Modified Silica.

Science.gov (United States)

Zhang, Xiaoli; Li, Binglin; Wang, Jiao; Li, Huanyu; Zhao, Binxia

2017-12-13

Triton X-100 was covalently bound to a surface of silica and acted as an anchor molecule to facilitate the adsorption of phosphatidylcholine (PC) in a purely aqueous solution. The silica-adsorbed PC obtained was successfully used for phospholipase D (PLD)-mediated transphosphatidylation in the production of phosphatidylserine (PS). Organic solvents were completely avoided in the whole production process. The PC loading and PS yield reached 98.9 and 99.0%, respectively. Two adsorption models were studied, and the relevant parameters were calculated to help us understand the adsorption and reaction processes deeply. In addition, the silica-adsorbed PC provides a promising way to continuously biosynthesize PS. A packed-bed reactor was employed to demonstrate the process flow of the continuous production of PS. The recyclability and stability of the Triton-X-100-modified silica were excellent, as demonstrated by its use 30 times during continuous operation without any loss of the productivity.

Functionalization of Silica Nanoparticles for Polypropylene Nanocomposite Applications

Directory of Open Access Journals (Sweden)

Diego Bracho

2012-01-01

Full Text Available Synthetic silica nanospheres of 20 and 100 nm diameter were produced via the sol-gel method to be used as filler in polypropylene (PP composites. Modification of the silica surface was further performed by reaction with organic chlorosilanes in order to improve the particles interaction with the hydrophobic polyolefin matrix. These nanoparticles were characterized using transmission electronic microscopy (TEM, elemental analysis, thermogravimetric analysis (TGA, and solid-state nuclear magnetic resonance (NMR spectroscopy. For unmodified silica, it was found that the 20 nm particles have a greater effect on both mechanical and barrier properties of the polymeric composite. In particular, at 30 wt%, Young's modulus increases by 70%, whereas water vapor permeability (WVP increases by a factor of 6. Surface modification of the 100 nm particles doubles the value of the composite breaking strain compared to unmodified particles without affecting Young's modulus, while 20 nm modified particles presented a slight increase on both Young's modulus and breaking strain. Modified 100 nm particles showed a higher WVP compared to the unmodified particles, probably due to interparticle condensation during the modification step. Our results show that the addition of nanoparticles on the composite properties depends on both particle size and surface modifications.

On the Relation between Natural and Enforced Syneresis of Acidic Precipitated Silica

Directory of Open Access Journals (Sweden)

Sebastian Wilhelm

2014-11-01

Full Text Available Silica in industrial production processes is precipitated by mixing an acid and an inorganic precursor. In this aqueous solution, silica particles form due to a polymerization reaction and agglomeration and, finally, build a gel. Thereafter, the reaction continues, and the gel network shrinks with the expulsion of the enclosed pore liquid. This slow process is known as “natural syneresis” and strongly affects the product properties, such as the agglomerate size, specific surface or porosity of the silica produced. In order to investigate the influence of process parameters, such as temperature, pH or ionic strength, on the shrinkage in shorter time-scales, we propose an acceleration of this process and define it as “enforced syneresis”. The acceleration is performed by applying a mechanical external force to the gel by means of a plunger and measuring the shrinkage behavior under these conditions. Thereby, the conceptual idea is the prediction of the shrinkage due to natural syneresis based on the results of enforced syneresis. We are now able to predict the natural syneresis behavior from enforced syneresis data by the development of a correlative model. Using this prediction model, we can show the influence of temperature on the maximum shrinkage and on its rate in a significantly shorter time of about 12 h instead of several days.

Nitriles at Silica Interfaces Resemble Supported Lipid Bilayers.

Science.gov (United States)

Berne, Bruce J; Fourkas, John T; Walker, Robert A; Weeks, John D

2016-09-20

Nitriles are important solvents not just for bulk reactions but also for interfacial processes such as separations, heterogeneous catalysis, and electrochemistry. Although nitriles have a polar end and a lipophilic end, the cyano group is not hydrophilic enough for these substances to be thought of as prototypical amphiphiles. This picture is now changing, as research is revealing that at a silica surface nitriles can organize into structures that, in many ways, resemble lipid bilayers. This unexpected organization may be a key component of unique interfacial behavior of nitriles that make them the solvents of choice for so many applications. The first hints of this lipid-bilayer-like (LBL) organization of nitriles at silica interfaces came from optical Kerr effect (OKE) experiments on liquid acetonitrile confined in the pores of sol-gel glasses. The orientational dynamics revealed by OKE spectroscopy suggested that the confined liquid is composed of a relatively immobile sublayer of molecules that accept hydrogen bonds from the surface silanol groups and an interdigitated, antiparallel layer that is capable of exchanging into the centers of the pores. This picture of acetonitrile has been borne out by molecular dynamics simulations and vibrational sum-frequency generation (VSFG) experiments. Remarkably, these simulations further indicate that the LBL organization is repeated with increasing disorder at least 20 Å into the liquid from a flat silica surface. Simulations and VSFG and OKE experiments indicate that extending the alkyl chain to an ethyl group leads to the formation of even more tightly packed LBL organization featuring entangled alkyl tails. When the alkyl portion of the molecule is a bulky t-butyl group, packing constraints prevent well-ordered LBL organization of the liquid. In each case, the surface-induced organization of the liquid is reflected in its interfacial dynamics. Acetonitrile/water mixtures are favored solvent systems for separations

Amorphous Silica-Promoted Lysine Dimerization: a Thermodynamic Prediction

Science.gov (United States)

Kitadai, Norio; Nishiuchi, Kumiko; Nishii, Akari; Fukushi, Keisuke

2018-03-01

It has long been suggested that mineral surfaces played a crucial role in the abiotic polymerization of amino acids that preceded the origin of life. Nevertheless, it remains unclear where the prebiotic process took place on the primitive Earth, because the amino acid-mineral interaction and its dependence on environmental conditions have yet to be understood adequately. Here we examined experimentally the adsorption of L-lysine (Lys) and its dimer (LysLys) on amorphous silica over a wide range of pH, ionic strength, adsorbate concentration, and the solid/water ratio, and determined the reaction stoichiometries and the equilibrium constants based on the extended triple-layer model (ETLM). The retrieved ETLM parameters were then used, in combination with the equilibrium constant for the peptide bond formation in bulk water, to calculate the Lys-LysLys equilibrium in the presence of amorphous silica under various aqueous conditions. Results showed that the silica surface favors Lys dimerization, and the influence varies greatly with changing environmental parameters. At slightly alkaline pH (pH 9) in the presence of a dilute NaCl (1 mM), the thermodynamically attainable LysLys from 0.1 mM Lys reached a concentration around 50 times larger than that calculated without silica. Because of the versatility of the ETLM, which has been applied to describe a wide variety of biomolecule-mineral interactions, future experiments with the reported methodology are expected to provide a significant constraint on the plausible geological settings for the condensation of monomers to polymers, and the subsequent chemical evolution of life.

Altering the concentration of silica tunes the functional properties of collagen-silica composite scaffolds to suit various clinical requirements.

Science.gov (United States)

Perumal, Sathiamurthi; Ramadass, Satiesh Kumar; Gopinath, Arun; Madhan, Balaraman; Shanmugam, Ganesh; Rajadas, Jayakumar; Mandal, Asit Baran

2015-12-01

The success of a tissue engineering scaffold depends on a fine balance being achieved between the physicochemical and biological properties. This study attempts to understand the influence of silica concentration on the functional properties of collagen-silica (CS) composite scaffolds for soft tissue engineering applications. Increasing the ratio of silica to collagen (0.25, 0.5, 0.75, 1.0, 1.25, 1.5 and 2.0 w/w) gave a marked advantage in terms of improving the water uptake and compressive modulus of the CS scaffolds, while also enhancing the biological stability and the turnover time. With increase in silica concentration the water uptake and compressive modulus increased concurrently, whereas it was not so for surface porous architecture and biocompatibility which are crucial for cell adhesion and infiltration. Silica:collagen ratio of ≤1 exhibits favourable surface biocompatibility, and any further increase in silica concentration has a detrimental effect. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Metathesis of alkanes and related reactions

KAUST Repository

Basset, Jean-Marie; Copé ret, Christophe; Soulivong, Daravong; Taoufik, Mostafa; Thivolle-Cazat, Jean

2010-01-01

, the process proceeds at relatively low temperature (ambient conditions or higher). It was discovered through the use of a silica-supported tantalum hydride, (=SiO)2TaH, a multifunctional catalyst with a single site of action. This reaction completes the story

H2 uptake in the Li-dispersed silica nano-tubes

International Nuclear Information System (INIS)

Jin Bae Lee; Soon Chang Lee; Sang Moon Lee; Hae Jin Kim

2006-01-01

Highly ordered Li-dispersed silica nano-tubes were prepared by sol-gel template method for hydrogen storage. Isolated Li-dispersed silica nano-tubes can be easily obtained by removing the AAO template with 2M NaOH. From the XRD study, the Li-dispersed silica nano-tubes showed the amorphous phase with silica frameworks. The uniform length and diameter of Li-dispersed silica nano-tubes could be examined with the electron microscopy studies. The wall thickness and diameter of nano-tubes are about 50-60 nm and 200-400 nm, respectively. The obtained Li-dispersed silica nano-tubes have the hydrogen adsorption capacity 2.25 wt% at 77 K under 47 atm. (authors)

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.

Silica-calcium zirconate nanocomposite, studying its thermal

Indian Academy of Sciences (India)

Silica–calcium zirconate nanocomposite was prepared in a two-step procedure. First, nanocalcium zirconate was synthesized by the modified sol–gel method; then, silica was added to the prepared sol and the resulting product was calcined at 700–1000° C. Dilatometric measurements were performed to determine the ...

SANS study of interaction of silica nanoparticles with BSA protein and their resultant structure

International Nuclear Information System (INIS)

Yadav, Indresh; Aswal, V. K.; Kohlbrecher, J.

2014-01-01

Small angle neutron scattering (SANS) has been carried out to study the interaction of anionic silica nanoparticles (88 Å) with globular protein Bovine Serum Albumin (BSA) (M.W. 66.4 kD) in aqueous solution. The measurements have been carried out on fixed concentration (1 wt %) of Ludox silica nanoparticles with varying concentration of BSA (0–5 wt %) at pH7. Results show that silica nanoparticles and BSA coexist as individual entities at low concentration of BSA where electrostatic repulsive interactions between them prevent their aggregation. However, as the concentration of BSA increases (≥ 0.5 wt %), it induces the attractive depletion interaction among nanoparticles leading to finally their aggregation at higher BSA concentration (2 wt %). The aggregates are found to be governed by the diffusion limited aggregation (DLA) morphology of fractal nature having fractal dimension about 2.4

Study of cross-linking reactions induced by gamma rays in hybrid membranes of Bisphenol-A-Polysulfone and precipitated silica; Estudo da formacao de ligacoes cruzadas por irradiacao gama em membranas hibridas de Polissulfona Bisfenol-A e silica precipitada

Energy Technology Data Exchange (ETDEWEB)

Furtado Filho, Acacio Antonio M., E-mail: facacio@ctex.eb.br [Laboratorio de Quimica Militar, CTEx, Rio de Janeiro, RJ (Brazil); Gomes, Ailton de S.; Lopes, Lea; Benzi, Marcia R. [Instituto de Macromoleculas Professora Eloisa Mano, UFRJ, Rio de Janeiro, RJ (Brazil)

2011-07-01

In this work the bisphenol-A-polysulfone (PSF) was sulfonated using trimethyl silyl chlorosulfonate [(CH{sub 3}){sub 3}SiSO{sub 3}Cl] as a mild sulfonating agent in a homogeneous solution of dichloroethane. The sulfonation reaction was confirmed by acid-base titration and FTIR-spectroscopy analysis. The hybrid membranes were obtained by casting the sulfonated bisphenol-A-polysulfone (SPSF) and precipitated silica Tixosil{sup R} 333 solutions in N-N-dimethylacetamide. Cross-linking in the hybrid membranes was obtained by irradiation, with doses ranging from 5 to 30 kGy using gamma ray from a {sup 60}Co source. The water uptake and the swelling of the membranes were estimated by measuring the change in weight between dry and wet conditions. The conductivity of the membranes in acid form was measured with the ac impedance technique using a PGSTAT30 frequency response analyzer. The hybrid cross-linked membranes have conductivity close to 10-1 S.cm{sup -1} at 100% RH and 80 deg C. Electrochemical performances, thermo-mechanical stability and low cost make this cross-linked SPSF hybrid membrane an attractive material for fuel cells using a proton exchange membrane. (author)

Application of a Burkholderia cepacia lipase-immobilized silica monolith to batch and continuous biodiesel production with a stoichiometric mixture of methanol and crude Jatropha oil

Directory of Open Access Journals (Sweden)

Takahashi Ryo

2011-10-01

Full Text Available Abstract Background The enzymatic production of biodiesel through alcoholysis of triglycerides has become more attractive because it shows potential in overcoming the drawbacks of chemical processes. In this study, we investigate the production of biodiesel from crude, non-edible Jatropha oil and methanol to characterize Burkholderia cepacia lipase immobilized in an n-butyl-substituted hydrophobic silica monolith. We also evaluate the performance of a lipase-immobilized silica monolith bioreactor in the continuous production of biodiesel. Results The Jatropha oil used contained 18% free fatty acids, which is problematic in a base-catalyzed process. In the lipase-catalyzed reaction, the presence of free fatty acids made the reaction mixture homogeneous and allowed bioconversion to proceed to 90% biodiesel yield after a 12 hour reaction time. The optimal molar ratio of methanol to oil was 3.3 to 3.5 parts methanol to one part oil, with water content of 0.6% (w/w. Further experiments revealed that B. cepacia lipase immobilized in hydrophobic silicates was sufficiently tolerant to methanol, and glycerol adsorbed on the support disturbed the reaction to some extent in the present reaction system. The continuous production of biodiesel was performed at steady state using a lipase-immobilized silica monolith bioreactor loaded with 1.67 g of lipase. The yield of 95% was reached at a flow rate of 0.6 mL/h, although the performance of the continuous bioreactor was somewhat below that predicted from the batch reactor. The bioreactor was operated successfully for almost 50 days with 80% retention of the initial yield. Conclusions The presence of free fatty acids originally contained in Jatropha oil improved the reaction efficiency of the biodiesel production. A combination of B. cepacia lipase and its immobilization support, n-butyl-substituted silica monolith, was effective in the production of biodiesel. This procedure is easily applicable to the design

Preparation of hierarchical micro-mesoporous aluminosilicate composites by simple Y zeolite/MCM-48 silica assembly

Energy Technology Data Exchange (ETDEWEB)

Enterría, Marina, E-mail: marina@incar.csic.es; Suárez-García, Fabián; Martínez-Alonso, Amelia; Tascón, Juan M.D.

2014-01-15

Highlights: • Hierarchical micro-mesoporous aluminosilicates were synthesized. • Y zeolite core/MCM-48 silica shell structures were obtained. • Y zeolite favors the formation of the mesostructure. • Porosity and structure can be varied by modifying the preparation variables. • Duration of the hydrothermal step has a great effect on the materials properties. -- Abstract: A simple procedure to obtain hierarchical micro-mesoporous aluminosilicate composites was developed by growing MCM-48 silica over commercial Y zeolite. The obtained hierarchical composites have a microporous core and a mesoporous shell. The process consists in assembling dispersed Y zeolite with a mesoporous silica phase that is formed “in situ” by “soft-templating” with cetryltrimethylammonium bromide (CTAB) as surfactant. The Y zeolite/MCM-48 silica ratio and aging time were varied to study their effects on the final porosity and structure of the hierarchical composites. The pore textural and structural characteristics of the composites did not match those of the corresponding Y zeolite/MCM-48 silica physical mixtures. This implies that the synthesized composites integrate micropores and mesopores in the same bulk. The obtained composites exhibited micropore and mesopore volumes ranging between 0.15–0.31 and 0.30–0.51 cm{sup 3}/g, respectively. X-ray diffraction and N{sub 2} adsorption results revealed that the presence of zeolite in the reaction medium favors the formation of mesopores in the obtained materials, especially for short hydrothermal treatments. TEM results showed that the obtained adsorbents are constituted by an integrated micro-mesoporous bimodal system in which Y zeolite is surrounded by a thin cover of MCM-48 silica.

Preparation of hierarchical micro-mesoporous aluminosilicate composites by simple Y zeolite/MCM-48 silica assembly

International Nuclear Information System (INIS)

Enterría, Marina; Suárez-García, Fabián; Martínez-Alonso, Amelia; Tascón, Juan M.D.

2014-01-01

Highlights: • Hierarchical micro-mesoporous aluminosilicates were synthesized. • Y zeolite core/MCM-48 silica shell structures were obtained. • Y zeolite favors the formation of the mesostructure. • Porosity and structure can be varied by modifying the preparation variables. • Duration of the hydrothermal step has a great effect on the materials properties. -- Abstract: A simple procedure to obtain hierarchical micro-mesoporous aluminosilicate composites was developed by growing MCM-48 silica over commercial Y zeolite. The obtained hierarchical composites have a microporous core and a mesoporous shell. The process consists in assembling dispersed Y zeolite with a mesoporous silica phase that is formed “in situ” by “soft-templating” with cetryltrimethylammonium bromide (CTAB) as surfactant. The Y zeolite/MCM-48 silica ratio and aging time were varied to study their effects on the final porosity and structure of the hierarchical composites. The pore textural and structural characteristics of the composites did not match those of the corresponding Y zeolite/MCM-48 silica physical mixtures. This implies that the synthesized composites integrate micropores and mesopores in the same bulk. The obtained composites exhibited micropore and mesopore volumes ranging between 0.15–0.31 and 0.30–0.51 cm 3 /g, respectively. X-ray diffraction and N 2 adsorption results revealed that the presence of zeolite in the reaction medium favors the formation of mesopores in the obtained materials, especially for short hydrothermal treatments. TEM results showed that the obtained adsorbents are constituted by an integrated micro-mesoporous bimodal system in which Y zeolite is surrounded by a thin cover of MCM-48 silica

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

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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.

An ultrasensitive hollow-silica-based biosensor for pathogenic Escherichia coli DNA detection.

Science.gov (United States)

Ariffin, Eda Yuhana; Lee, Yook Heng; Futra, Dedi; Tan, Ling Ling; Karim, Nurul Huda Abd; Ibrahim, Nik Nuraznida Nik; Ahmad, Asmat

2018-03-01

A novel electrochemical DNA biosensor for ultrasensitive and selective quantitation of Escherichia coli DNA based on aminated hollow silica spheres (HSiSs) has been successfully developed. The HSiSs were synthesized with facile sonication and heating techniques. The HSiSs have an inner and an outer surface for DNA immobilization sites after they have been functionalized with 3-aminopropyltriethoxysilane. From field emission scanning electron microscopy images, the presence of pores was confirmed in the functionalized HSiSs. Furthermore, Brunauer-Emmett-Teller (BET) analysis indicated that the HSiSs have four times more surface area than silica spheres that have no pores. These aminated HSiSs were deposited onto a screen-printed carbon paste electrode containing a layer of gold nanoparticles (AuNPs) to form a AuNP/HSiS hybrid sensor membrane matrix. Aminated DNA probes were grafted onto the AuNP/HSiS-modified screen-printed electrode via imine covalent bonds with use of glutaraldehyde cross-linker. The DNA hybridization reaction was studied by differential pulse voltammetry using an anthraquinone redox intercalator as the electroactive DNA hybridization label. The DNA biosensor demonstrated a linear response over a wide target sequence concentration range of 1.0×10 -12 -1.0×10 -2 μM, with a low detection limit of 8.17×10 -14 μM (R 2 = 0.99). The improved performance of the DNA biosensor appeared to be due to the hollow structure and rough surface morphology of the hollow silica particles, which greatly increased the total binding surface area for high DNA loading capacity. The HSiSs also facilitated molecule diffusion through the silica hollow structure, and substantially improved the overall DNA hybridization assay. Graphical abstract Step-by-step DNA biosensor fabrication based on aminated hollow silica spheres.

Feasibility study of silica sol as the carrier of a hydrophobic drug in aqueous solution using enrofloxacin as the model

International Nuclear Information System (INIS)

Song Meirong; Song Junling; Ning Aimin; Cui Baoan; Cui Shumin; Zhou Yaobing; An Wankai; Dong Xuesong; Zhang Gege

2010-01-01

The aim of this study was to determine the feasibility of using silica sol to carry a hydrophobic drug in aqueous solution. Enrofloxacin, which was selected as the model drug because it is a broad-spectrum antibiotic drug with poor solubility in water, was adsorbed onto silica sol in aqueous solution during cooling from 60 deg. C to room temperature. The drug-loaded silica sol was characterized by transmission electron microscopy, Fourier transform infrared spectrum, thermal gravimetric analysis and ultraviolet-visible light spectroscopy. The results showed that enrofloxacin was adsorbed by silica sol without degradation at a loading of 15.23 wt.%. In contrast to the rapid release from pure enrofloxacin, the drug-loaded silica sol showed a slower release over a longer time. Kinetics analysis suggested the drug release from silica sol was mainly a diffusion-controlled process. Therefore, silica sol can be used to carry a hydrophobic drug in aqueous solution for controlled drug delivery.

The effect of impeller type on silica sol formation in laboratory scale agitated tank

Science.gov (United States)

Nurtono, Tantular; Suprana, Yayang Ade; Latif, Abdul; Dewa, Restu Mulya; Machmudah, Siti; Widiyastuti, Winardi, Sugeng

2016-02-01

The multiphase polymerization reaction of the silica sol formation produced from silicic acid and potassium hydroxide solutions in laboratory scale agitated tank was studied. The reactor is equipped with four segmental baffle and top entering impeller. The inside diameter of reactor is 9 cm, the baffle width is 0.9 cm, and the impeller position is 3 cm from tank bottom. The diameter of standard six blades Rushton and three blades marine propeller impellers are 5 cm. The silicic acid solution was made from 0.2 volume fraction of water glass (sodium silicate) solution in which the sodium ion was exchanged by hydrogen ion from cation resin. The reactor initially filled with 286 ml silicic acid solution was operated in semi batch mode and the temperature was kept constant in 60 °C. The 3 ml/minute of 1 M potassium hydroxide solution was added into stirred tank and the solution was stirred. The impeller rotational speed was varied from 100 until 700 rpm. This titration was stopped if the solution in stirred tank had reached the pH of 10-The morphology of the silica particles in the silica sol product was analyzed by Scanning Electron Microscope (SEM). The size of silica particles in silica sol was measured based on the SEM image. The silica particle obtained in this research was amorphous particle and the shape was roughly cylinder. The flow field generated by different impeller gave significant effect on particle size and shape. The smallest geometric mean of length and diameter of particle (4.92 µm and 2.42 µm, respectively) was generated in reactor with marine propeller at 600 rpm. The reactor with Rushton impeller produced particle which the geometric mean of length and diameter of particle was 4.85 µm and 2.36 µm, respectively, at 150 rpm.

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

Silica gel matrix immobilized Chlorophyta hydrodictyon africanum ...

African Journals Online (AJOL)

Chlorophyta hydrodictyon africanum was immobilized on a silica gel matrix to improve its mechanical properties. The algae-silica gel adsorbent was used for batch sorption studies of a cationic dye, methylene blue (MB). Optimum adsorption was obtained with a dosage of 0.8 g bio sorbent. Results from sorption studies ...

The macro- and micro properties of cement pastes with silica-rich materials cured by wet-mixed steaming injection

International Nuclear Information System (INIS)

Wu, D.S.; Peng, Y.N.

2003-01-01

This research used cement pastes with a low water/blaine ratio (W/b=0.27). Rice husk ashes (RHA) burned at 700 and 850 deg. C, silica fume, silica sand (Ottawa standard sand), etc., were the added ingredients. Wet-mixed steam injection (WMSI) was at five different temperatures: 65, 80, 120, 150 and 180 deg. C. We investigated cement pastes with added silica-rich materials. For different WMSI temperatures and times, we explored the relations between compressive strength, hydration products, and pozzolanic reaction mechanism. From scanning electron microscopy (SEM) and EDS, we know that hydration products become very complicated, depending on the WMSI temperatures and times. It is difficult to determine the direct effects on the strength based on changes in the products. Experimental results, however, clearly showed that the compressive strength was worst for 80 deg. C and best for 180 deg. C. High-temperature WMSI is best with 4-h presteaming period and 8-h retention time. Curing in saturated limewater for 28 days did not increase the strength. The three types of silica-rich materials used in this research all participated in the reaction during high-temperature WMSI; they helped to increase the strength. Addition of Ottawa standard sand resulted in the best strength, followed by addition of RHA, while addition of silica fume was worse than the others. Specimens treated with high-temperature WMSI would swell slightly if they were placed in air. This was different from normal-temperature curing

Facile preparation of organic-silica hybrid monolith for capillary hydrophilic liquid chromatography based on "thiol-ene" click chemistry.

Science.gov (United States)

Chen, Ming-Luan; Zhang, Jun; Zhang, Zheng; Yuan, Bi-Feng; Yu, Qiong-Wei; Feng, Yu-Qi

2013-04-05

In this work, a one-step approach to facile preparation of organic-inorganic hybrid monoliths was successfully developed. After vinyl-end organic monomers and azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethoxysilane (TMOS) and 3-mercaptopropyltrimethoxysilane (MPTMS), the homogeneous mixture was introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the organic-silica hybrid monoliths. By employing this strategy, two types of organic-silica hybrid monoliths with positively charged quaternary ammonium and amide groups were prepared, respectively. The functional groups were successfully introduced onto the monoliths during the sol-gel process with "thiol-ene" click reaction, which was demonstrated by ζ-potential assessment, energy dispersive X-ray spectroscopy (EDX), and Fourier transform infrared (FT-IR) spectroscopy. The porous structure of the prepared monolithic columns was examined by scanning electron microscopy (SEM), nitrogen adsorption-desorption measurement, and mercury intrusion porosimetry. These results indicate the prepared organic-silica hybrid monoliths possess homogeneous column bed, large specific surface area, good mechanical stability, and excellent permeability. The prepared monolithic columns were then applied for anion-exchange/hydrophilic interaction liquid chromatography. Different types of analytes, including benzoic acids, inorganic ions, nucleosides, and nucleotides, were well separated with high column efficiency around 80,000-130,000 plates/m. Taken together, we present a facile and universal strategy to prepare organic-silica hybrid monoliths with a variety of organic monomers using one-step approach. Copyright © 2013 Elsevier B.V. All rights reserved.

Grassy Silica Nanoribbons and Strong Blue Luminescence

Science.gov (United States)

Wang, Shengping; Xie, Shuang; Huang, Guowei; Guo, Hongxuan; Cho, Yujin; Chen, Jun; Fujita, Daisuke; Xu, Mingsheng

2016-09-01

Silicon dioxide (SiO2) is one of the key materials in many modern technological applications such as in metal oxide semiconductor transistors, photovoltaic solar cells, pollution removal, and biomedicine. We report the accidental discovery of free-standing grassy silica nanoribbons directly grown on SiO2/Si platform which is commonly used for field-effect transistors fabrication without other precursor. We investigate the formation mechanism of this novel silica nanostructure that has not been previously documented. The silica nanoribbons are flexible and can be manipulated by electron-beam. The silica nanoribbons exhibit strong blue emission at about 467 nm, together with UV and red emissions as investigated by cathodoluminescence technique. The origins of the luminescence are attributed to various defects in the silica nanoribbons; and the intensity change of the blue emission and green emission at about 550 nm is discussed in the frame of the defect density. Our study may lead to rational design of the new silica-based materials for a wide range of applications.

Agglomeration mechanism in biomass fluidized bed combustion – Reaction between potassium carbonate and silica sand

DEFF Research Database (Denmark)

Anicic, Bozidar; Lin, Weigang; Dam-Johansen, Kim

2018-01-01

Agglomeration is one of the operational problems in fluidized bed combustion of biomass, which is caused by interaction between bed materials (e.g. silica sand) and the biomass ash with a high content of potassium species. However, the contribution of different potassium species to agglomeration ...

Mechanical and chemical properties of polyvinyl alcohol modified cement mortar with silica fume used as matrix including radioactive waste

International Nuclear Information System (INIS)

Dakroury, A. M.

2007-01-01

This paper discussed the mechanical and chemical properties of polyvinyl alcohol - modified cement mortar with silica fume to assess the safety for disposal of radioactive waste. The modified cement mortars containing polyvinyl alcohol (PVA) in the presence of 10 % silica fume (SF) .The chemical reaction between polymer and cement - hydrated product were investigated by the Infrared Spectral Technology, Differential Thermal Analysis and X-ray diffraction. The leaching of 137Cs from a waste composite into a surrounding fluid has been studied .The results shown that PVA increases the strength and decreases the porosity. The increase in strength duo to the interaction of PVA with cement , may be forming some new compound that fill the pores or improve the bond between the cement . The pozzolanic reaction of the SF increases the calcium silicate hydrates in the hardening matrix composites. There is distinct change in the refinement of the pore structure in cement composites giving fewer capillary pores and more of the finer gel pores

Hydrogen generation systems utilizing sodium silicide and sodium silica gel materials

Science.gov (United States)

Wallace, Andrew P.; Melack, John M.; Lefenfeld, Michael

2015-07-14

Systems, devices, and methods combine reactant materials and aqueous solutions to generate hydrogen. The reactant materials can sodium silicide or sodium silica gel. The hydrogen generation devices are used in fuels cells and other industrial applications. One system combines cooling, pumping, water storage, and other devices to sense and control reactions between reactant materials and aqueous solutions to generate hydrogen. Multiple inlets of varied placement geometries deliver aqueous solution to the reaction. The reactant materials and aqueous solution are churned to control the state of the reaction. The aqueous solution can be recycled and returned to the reaction. One system operates over a range of temperatures and pressures and includes a hydrogen separator, a heat removal mechanism, and state of reaction control devices. The systems, devices, and methods of generating hydrogen provide thermally stable solids, near-instant reaction with the aqueous solutions, and a non-toxic liquid by-product.

A novel method to characterize silica bodies in grasses.

Science.gov (United States)

Dabney, Clemon; Ostergaard, Jason; Watkins, Eric; Chen, Changbin

2016-01-01

The deposition of silicon into epidermal cells of grass species is thought to be an important mechanism that plants use as a defense against pests and environmental stresses. There are a number of techniques available to study the size, density and distribution pattern of silica bodies in grass leaves. However, none of those techniques can provide a high-throughput analysis, especially for a great number of samples. We developed a method utilizing the autofluorescence of silica bodies to investigate their size and distribution, along with the number of carbon inclusions within the silica bodies of perennial grass species Koeleria macrantha. Fluorescence images were analyzed by image software Adobe Photoshop CS5 or ImageJ that remarkably facilitated the quantification of silica bodies in the dry ash. We observed three types of silica bodies or silica body related mineral structures. Silica bodies were detected on both abaxial and adaxial epidermis of K. macrantha leaves, although their sizes, density, and distribution patterns were different. No auto-fluorescence was detected from carbon inclusions. The combination of fluorescence microscopy and image processing software displayed efficient utilization in the identification and quantification of silica bodies in K. macrantha leaf tissues, which should applicable to biological, ecological and geological studies of grasses including forage, turf grasses and cereal crops.

New Silica Magnetite Sorbent: The Influence of Variations of Sodium Silicate Concentrations on Silica Magnetite Character

Science.gov (United States)

Azmiyawati, C.; Pratiwi, P. I.; Darmawan, A.

2018-04-01

The adsorption capacity of an adsorbent is determined by the adsorbent and the adsorbate properties. The character of the adsorbent will play a major role in its ability to adsorb the corresponding adsorbate. Therefore, in this study we looked at the effects of variations of sodium silicate concentrations on the resulting magnetite silica adsorbent properties. The application of silica coating on the magnetite was carried out through a sol-gel process with sodium silicate and HCl precursors. Based on the characterization data obtained, it was found that the silica coating on magnetite can increase the resistance to acid leaching, increase the particle size, but decrease the magnetic properties of the magnetite. Based on Gas Sorption Analyzer (GSA) and X-ray Difraction (XRD) data it can successively be determined that increase in concentration of sodium silicate will increase the surface area and amorphous structure of the Silica Magnetie.

Fluorescent Functionalized Mesoporous Silica for Radioactive Material Extraction

International Nuclear Information System (INIS)

Li, Juan; Zhu, Kake; Shang, Jianying; Wang, Donghai; Nie, Zimin; Guo, Ruisong; Liu, Chongxuan; Wang, Zheming; Li, Xiaolin; Liu, Jun

2012-01-01

Mesoporous silica with covalently bound salicylic acid molecules incorporated in the structure was synthesized with a one-pot, co-condensation reaction at room temperature. The as-synthesized material has a large surface area, uniform particle size, and an ordered pore structure as determined by characterization with transmission electron microscopy, thermal gravimetric analysis, and infrared spectra, etc. Using the strong fluorescence and metal coordination capability of salicylic acid, functionalized mesoporous silica (FMS) was developed to track and extract radionuclide contaminants, such as uranyl (U(VI)) ions encountered in subsurface environments. Adsorption measurements showed a strong affinity of the FMS toward U(VI) with a Kd value of 105 mL/g, which is four orders of magnitude higher than the adsorption of U(VI) onto most of the sediments in natural environments. The new materials have a potential for synergistic environmental monitoring and remediation of the radionuclide U(VI) from contaminated subsurface environments.

Positron annihilation studies of mesoporous silica films using a slow positron beam

International Nuclear Information System (INIS)

He Chunqing; Muramatsu, Makoto; Ohdaira, Toshiyuki; Kinomura, Atsushi; Suzuki, Ryoichi; Ito, Kenji; Kabayashi, Yoshinori

2006-01-01

Positron annihilation lifetime spectra were measured for mesoporous silica films, which were synthesized using triblock copolymer (EO 106 PO 70 EO 106 ) as a structure-directing agent. Different positron lifetime spectra for the deposited and calcined films indicated the formation of meso-structure after calcination, which was confirmed by Fourier transform infrared (FTIR) spectra and field emission-scanning electron microscopy (FE-SEM) observation. Open porosity or pore interconnectivity of a silica film might be evaluated by a two-dimensional positron annihilation lifetime spectrum of an uncapped film. Pore sizes and their distributions in the silica films were found to be affected by thermal treatments

Synthesis of uniform carbon at silica nanocables and luminescent silica nanotubes with well controlled inner diameters

International Nuclear Information System (INIS)

Qian Haisheng; Yu Shuhong; Ren Lei; Yang Yipeng; Zhang Wei

2006-01-01

Uniform carbon at silica nanocables and silica nanotubes with well-controlled inner diameters can be synthesized in an easy way by a sacrificial templating method. This was performed using carbon nanofibres as hard templates that were synthesized previously by a hydrothermal carbonization process. Silica nanotubes with well-controlled inner diameters were synthesized from carbon at silica core-shell nanostructures by removal of the core carbon component. The inner diameters of the as-prepared silica nanotubes can be well controlled from several nanometres to hundreds of nanometres by adjusting the diameters of the carbon nanofibres. The silica nanotubes synthesized by this method display strong photoluminescence in ultraviolet at room temperature. Such uniform silica nanotubes might find potential applications in many fields such as encapsulation, catalysis, chemical/biological separation, and sensing

Molecular Dynamics Simulations of Water Nanodroplets on Silica Surfaces

DEFF Research Database (Denmark)

Zambrano, Harvey A; Walther, Jens Honore; Jaffe, Richard L.

2009-01-01

and DNA microarrays technologies.4,5,6,7,8 Although extensive experimental, theoretical and computational work has been devoted to study the nature of the interaction between silica and water,2,9-16 at the molecular level a complete understanding of silica-water systems has not been reached. Contact angle...... computations of water droplets on silica surfaces offers a useful fundamental and quantitative measurement in order to study chemical and physical properties of water-silica systems.3,16,17,18 For hydrophobic systems the static and dynamic properties of the fluid-solid interface are influenced by the presence...

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.

The growth of silica and silica-clad nanowires using a solid-state reaction mechanism on Ti, Ni and SiO2 layers

International Nuclear Information System (INIS)

Sharma, Parul; Anguita, J V; Stolojan, V; Henley, S J; Silva, S R P

2010-01-01

A large area compatible and solid-state process for growing silica nanowires is reported using nickel, titanium and silicon dioxide layers on silicon. The silica nanowires also contain silicon, as indicated by Raman spectroscopy. The phonon confinement model is employed to measure the diameter of the Si rich tail for our samples. The measured Raman peak shift and full width at half-maximum variation with the nanowire diameter qualitatively match with data available in the literature. We have investigated the effect of the seedbed structure on the nanowires, and the effect of using different gas conditions in the growth stages. From this, we have obtained the growth mechanism, and deduced the role of each individual substrate seedbed layer in the growth of the nanowires. We report a combined growth mechanism, where the growth is initiated by a solid-liquid-solid process, which is then followed by a vapour-liquid-solid process. We also report on the formation of two distinct structures of nanowires (type I and type II). The growth of these can be controlled by the use of titanium in the seedbed. We also observe that the diameter of the nanowires exhibits an inverse relation with the catalyst thickness.

Surface modification to produce hydrophobic nano-silica particles using sodium dodecyl sulfate as a modifier

Energy Technology Data Exchange (ETDEWEB)

Qiao, Bing; Liang, Yong; Wang, Ting-Jie, E-mail: wangtj@tsinghua.edu.cn; Jiang, Yanping

2016-02-28

Graphical abstract: Nano silica particle was modified to produce hydrophobic surface with contact angle of 107° using the water soluble SDS as a modifier through a new route. The grafted density reached 1.82–2 nm. Brønsted acid sites supply proton to react with SDS via generating carbocation, forming a Si–O–C structure. - Highlights: • Silica was modified to produce hydrophobic surface using SDS as modifier. • The route is free of organic solvent and gets perfect contact of SDS and silica. • Contact angle of modified silica particles reached 107°. • Grafted density on the silica surface reached 1.82 SDS nm{sup −2}. • Brønsted acid sites supply proton to react with SDS via generating carbocation. - Abstract: Hydrophobic silica particles were prepared using the surfactant sodium dodecyl sulfate (SDS) as a modifier by a new route comprising three processes, namely, aqueous mixing, spray drying and thermal treatment. Since SDS dissolves in water, this route is free of an organic solvent and gave a perfect dispersion of SDS, that is, there was excellent contact between SDS and silica particles in the modification reaction. The hydrophobicity of the modified surface was verified by the contact angle of the nano-sized silica particles, which was 107°. The SDS grafting density reached 1.82 nm{sup −2}, which is near the highest value in the literature. The optimal parameters of the SDS/SiO{sub 2} ratio in the aqueous phase, process temperature and time of thermal treatment were determined to be 20%, 200 °C and 30 min, respectively. The grafting mechanism was studied by comparing the modification with that on same sized TiO{sub 2} particles, which indicated that the protons of the Brønsted acid sites on the surface of SiO{sub 2} reacted with SDS to give a carbocation which then formed a Si–O–C structure. This work showed that the hydrophilic surface of silica can be modified to be a hydrophobic surface by using a water soluble modifier SDS in a

Quantifying Silica Reactivity in Subsurface Environments: Reaction Affinity and Solute Matrix Controls on Quartz and SiO2 Glass Dissolution Kinetics

International Nuclear Information System (INIS)

Dove, Patricia M.

1999-01-01

Our goal is to develop a quantitative and mechanistic understanding of amorphous silica, SiO2(am), dissolution kinetics in aqueous solutions. A knowledge of fundamental controls on the reactivity of simple Si-O bonded phases is the baseline of behavior for understanding highly complex silica phases. In the Earth, silicate minerals comprise >70% of the crust and dominate virtually every subsurface system. More importantly for the objectives of this EMSP project, the silicates are important because compositionally complex glasses will become the front line of defense in containing radioactive wastes in the nation's long term and interim storage strategies. To date, the behavior of SiO2(am) is largely inferred from studies of the better known crystalline polymorphs (e.g. alpha-quartz). In the first step towards constructing a general model for amorphous silica reactivity in the complex fluid compositions of natural waters, we are determining the dissolution behavior as a function of temperature, solution pH and cation concentration. With these data we are determining relationships between SiO2 glass structure and dissolution rates in aqueous solutions, as described below

Thermodynamics of Silica Dissolution From In-situ Raman +Spectroscopy

Science.gov (United States)

Davis, M. K.; Fumagalli, P.; Stixrude, L. P.

2001-12-01

Solubilities of cations, such as silicon, in water strongly effect both the physical and thermodynamical properties of supercritical metamorphic fluids. Modeling the thermodynamics of fluid-rock interactions requires therefore a profound understanding of cation dissolution and aqueous speciation. In-situ Raman experiments of the silica-water system were performed in an externally heated Bassett-type diamond-anvil cell at the Department of Geological Sciences, University of Michigan. Natural quartz samples (from Owl Creek Mountains, Wyoming) were loaded in the sample chamber with de-ionized or spectrographic water. All experiments used doubly polished rhenium gaskets with a thickness of 200 μ m, diameter of 1.0 mm, and a 500 μ m drillhole for the sample chamber. Temperature was measured using K-type thermocouples wrapped around both the upper and lower diamond anvils. Pressures are obtained on the basis of the shift of the 464 cm-1 Raman mode of quartz. In-situ Raman spectra were collected from 250-1200 cm-1, focusing on the vibrational modes of aqueous silica species at temperatures up to 700 ° C and pressures up to 14 kbar. We observed Si-O stretching modes attributable to dimer (H6Si2O7, 965 cm-1) and monomer (H4SiO4, 771 cm-1) aqueous silica species. The relative intensities of these two bands as a function of isochoric heating place constraints on the energetics of the polymerization reaction, if we assume that the intensity ratio is linearly related to concentration ratio. We have been able to perform experiments along two different isochores (0.9 and 0.75 g/cm3, respectively) from which we are able to derive the enthalpy of reaction.

Heterogeneously Catalyzed Oxidation Reactions Using Molecular Oxygen

DEFF Research Database (Denmark)

Beier, Matthias Josef

Heterogeneously catalyzed selective oxidation reactions have attracted a lot of attention in recent time. The first part of the present thesis provides an overview over heterogeneous copper and silver catalysts for selective oxidations in the liquid phase and compared the performance and catalytic...... that both copper and silver can function as complementary catalyst materials to gold showing different catalytic properties and being more suitable for hydrocarbon oxidation reactions. Potential opportunities for future research were outlined. In an experimental study, the potential of silver as a catalyst...... revealed that all catalysts were more active in combination with ceria nanoparticles and that under the tested reaction conditions silver was equally or even more efficient than the gold catalysts. Calcination at 900 °C of silver on silica prepared by impregnation afforded a catalyst which was used...

Sonochemical coating of magnetite nanoparticles with silica.

Science.gov (United States)

Dang, Feng; Enomoto, Naoya; Hojo, Junichi; Enpuku, Keiji

2010-01-01

Magnetite nanoparticles were coated with silica through the hydrolysis and condensation of tetraethyl orthosilicate (TEOS) under ultrasonic irradiation. The ultrasonic irradiation was used to prevent the agglomeration of the magnetite particles and accelerate the hydrolysis and condensation of TEOS. TEM, DLS, XRF, VSM, TG and sedimentation test were used to characterize the silica-coated magnetite particles. The dispersibility of silica-coated magnetite particles in aqueous solution was improved significantly and the agglomerate particle size was decreased to 110 nm. It was found that the agglomerate particle size of silica-coated magnetite particles was mainly decided by the coating temperature and the pH value in the silica-coating process. The weight ratio of silica in silica-coated magnetite particles was mainly decided by the pH value in the silica-coating process. The dispersibility of silica-coated magnetite particles was mainly decided by the agglomerate particle size of the suspension. The oxidation of magnetite particles in air was limited through the coated silica. The magnetism of silica-coated magnetite particles decreased slightly after silica-coating.

IMPROVEMENT OF EXPANSIVE SOIL BY USING SILICA FUME

Directory of Open Access Journals (Sweden)

Kawther Y. AL-Soudany

2018-01-01

Full Text Available Expansive soils are characterized by their considerable volumetric deformations representing a serious challenge for the stability of the engineering structures such as foundations. Consequently, the measurements of swelling properties, involving swelling and swell pressure, become extremely important in spite of their determination needs a lot of time with costly particular equipment. Thus, serious researches attempts have been tried to remedy such soils by means of additives such as cement, lime, steel fibers, stone dust, fly ash and silica fume. In this research the study of silica fume has studied to treatment expansion soil, the clay soil was brought from Al-Nahrawan in Baghdad. The soil selected for the present investigation prepared in laboratory by mixing natural soil with different percentages of bentonite (30, 50 and 70% by soil dry weight. The test program included the effect of bentonite on natural soil then study the effect of silica fume (SF on prepared soil by adding different percentage of silica fume (3, 5, and 7 by weight to the prepared soils and the influence of these admixtures was observed by comparing their results with those of untreated soils (prepared soils. The results show that both liquid limit and plasticity index decreased with the addition of silica fume, while the plastic limit is increase with its addition. As well as, a decrease in the maximum dry unit weight with an increase in the optimum water contents have been obtained with increasing the percentage of addition of the silica fume. It is also observed an improvement in the free swell, swelling pressure by using silica fume. It can be concluded that the silica fume stabilization may be used as a successful way for the treatment of expansive clay.

Quantifying silica reactivity in subsurface environments: Reaction affinity and solute matrix controls on quartz and SiO2 glass. 1997 annual progress report

International Nuclear Information System (INIS)

Dove, P.M.

1997-01-01

'The author reports the preliminary results of the experiments on the dissolution behavior of vitreous silica (v-SiO 2 ) into aqueous solutions of variable pH and ionic strength. The experiments are being conducted in mixed flow reactors with a high circulation rate that simulates constant-stirred conditions, the efficacy of which the authors discuss below. The preliminary results indicate that v-SiO 2 dissolves into aqueous solutions approximately two orders of magnitude more quickly than crystalline silica (e.g., quartz). With additional experiments, they will utilize the dissolution rate data as a framework for understanding the behavior of waste glass compositions in the subsurface. In other work related to the studies of glass reactivity, the author has written one book chapter that will be published as part of a proceedings for the CEA/VALRHO international nuclear waste disposal conference held in Mejannes le Clap, France. In separate work, she is presently writing a second book chapter for the volume entitled Adsorption on Silica Surfaces.'

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

Science.gov (United States)

Faisal, Mahtab

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

Selective oxidation of cyclohexene through gold functionalized silica monolith microreactors

Science.gov (United States)

Alotaibi, Mohammed T.; Taylor, Martin J.; Liu, Dan; Beaumont, Simon K.; Kyriakou, Georgios

2016-04-01

Two simple, reproducible methods of preparing evenly distributed Au nanoparticle containing mesoporous silica monoliths are investigated. These Au nanoparticle containing monoliths are subsequently investigated as flow reactors for the selective oxidation of cyclohexene. In the first strategy, the silica monolith was directly impregnated with Au nanoparticles during the formation of the monolith. The second approach was to pre-functionalize the monolith with thiol groups tethered within the silica mesostructure. These can act as evenly distributed anchors for the Au nanoparticles to be incorporated by flowing a Au nanoparticle solution through the thiol functionalized monolith. Both methods led to successfully achieving even distribution of Au nanoparticles along the length of the monolith as demonstrated by ICP-OES. However, the impregnation method led to strong agglomeration of the Au nanoparticles during subsequent heating steps while the thiol anchoring procedure maintained the nanoparticles in the range of 6.8 ± 1.4 nm. Both Au nanoparticle containing monoliths as well as samples with no Au incorporated were tested for the selective oxidation of cyclohexene under constant flow at 30 °C. The Au free materials were found to be catalytically inactive with Au being the minimum necessary requirement for the reaction to proceed. The impregnated Au-containing monolith was found to be less active than the thiol functionalized Au-containing material, attributable to the low metal surface area of the Au nanoparticles. The reaction on the thiol functionalized Au-containing monolith was found to depend strongly on the type of oxidant used: tert-butyl hydroperoxide (TBHP) was more active than H2O2, likely due to the thiol induced hydrophobicity in the monolith.

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

Science.gov (United States)

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

2018-01-01

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

Surface characterization of polyethylene terephthalate/silica nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Parvinzadeh, Mazeyar, E-mail: mparvinzadeh@gmail.com [Department of Textile, Islamic Azad University, Science and Research Branch, Tehran (Iran, Islamic Republic of); Moradian, Siamak [Department of Polymer and Color Engineering, Amirkabir University of Technology, P.O. Box 15875-4413, Tehran (Iran, Islamic Republic of); Rashidi, Abosaeed [Department of Textile, Islamic Azad University, Science and Research Branch, Tehran (Iran, Islamic Republic of); Yazdanshenas, Mohamad-Esmail [Department of Textile, Islamic Azad University, Yazd Branch, Yazd (Iran, Islamic Republic of)

2010-02-15

Poly(ethylene terephthalate) (PET) based nanocomposites containing hydrophilic (i.e. Aerosil 200 or Aerosil TT 600) or hydrophobic (i.e. Aerosil R 972) nano-silica were prepared by melt compounding. Influence of nano-silica type on surface properties of the resultant nanocomposites was investigated by the use of Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), contact angle measurement (CAM), scanning electron microscopy (SEM) and reflectance spectroscopy (RS). The possible interaction between nano-silica particles and PET functional groups at bulk and surface were elucidated by transmission FTIR and FTIR-ATR spectroscopy, respectively. AFM studies of the resultant nanocomposites showed increased surface roughness compared to pure PET. Contact angle measurements of the resultant PET composites demonstrated that the wettability of such composites depends on surface treatment of the particular nano-silica particles used. SEM images illustrated that hydrophilic nano-silica particles tended to migrate to the surface of the PET matrix.

Silica Sol-Gel Entrapment of the Enzyme Chloro peroxidase

International Nuclear Information System (INIS)

Le, T.; Chan, S.; Ebaid, B.; Sommerhalter, M.

2015-01-01

The enzyme chloro peroxidase (CPO) was immobilized in silica sol-gel beads prepared from tetramethoxysilane. The average pore diameter of the silica host structure (∼3 nm) was smaller than the globular CPO diameter (∼6 nm) and the enzyme remained entrapped after sol-gel maturation. The catalytic performance of the entrapped enzyme was assessed via the pyrogallol peroxidation reaction. Sol-gel beads loaded with 4 μg CPO per mL sol solution reached 9-12% relative activity compared to free CPO in solution. Enzyme kinetic analysis revealed a decrease in K_cat but no changes in K_M or K_I . Product release or enzyme damage might thus limit catalytic performance. Yet circular dichroism and visible absorption spectra of transparent CPO sol-gel sheets did not indicate enzyme damage. Activity decline due to methanol exposure was shown to be reversible in solution. To improve catalytic performance the sol-gel protocol was modified. The incorporation of 5, 20, or 40% methyltrimethoxysilane resulted in more brittle sol-gel beads but the catalytic performance increased to 14% relative to free CPO in solution. The use of more acidic casting buffers (ph 4.5 or 5.5 instead of 6.5) resulted in a more porous silica host reaching up to 18% relative activity

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...

Pattern transfer on fused silica samples using sub-aperture reactive ion beam etching

Energy Technology Data Exchange (ETDEWEB)

Miessler, Andre; Arnold, Thomas [Leibniz-Institut fuer Oberflaechenmodifizierung (IOM), Permoserstrasse 15, D-04318 Leipzig (Germany)

2012-07-01

In comparison to sole Ar ion beam sputtering Reactive Ion Beam Etching (RIBE) reveals the main advantage of increasing the selectivity for different kind of materials due to chemical contributions during the material removal. Therefore RIBE is qualified to be an excellent candidate for pattern transfer applications. The goal of the present study is to apply a sub-aperture reactive ion beam for pattern transfer on large fused silica samples. Concerning this matter, the etching behavior in the ion beam periphery plays a decisive role. Using a Kaufman-typed ion source with NF{sub 3} as reactive gas, XPS measurements of the modified surface exposes impurities like Ni, Fe and Cr, which belongs to chemically eroded material of the plasma pot and a layer formation of silicon nitride, handicaps the etching process mainly in the beam periphery where the sputtering contribution decrease. These side effects influence the pattern transfer of trench structures, produced in AZ MIR 701 photoresist by lithography on a 2'' fused silica plate, by changing the selectivity due to modified chemical reactions of the resist layer. Concerning this we investigate a RF-Ion source for sub aperture reactive ion beam applications and finally we examine the pattern transfer on large fused silica plates using NF{sub 3}-sub-aperture RIBE.

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

Impregnation of mesoporous silica for catalyst preparation studied with differential scanning calorimetry

NARCIS (Netherlands)

Eggenhuisen, T.M.; van Steenbergen, M.J.; Talsma, H.; de Jongh, P.E.; de Jong, K.P.

2009-01-01

Aqueous impregnation of mesoporous silica as a first step in catalyst preparation was studied to investigate the distribution of the metal-precursor solution over the support. The degree of pore-filling after impregnation was determined using the freezing point depression of confined liquids. A

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...

Effect of silica concentration on electrical conductivity of epoxy resin-carbon black-silica nanocomposites

International Nuclear Information System (INIS)

Zhang Wei; Blackburn, Richard S.; Dehghani-Sanij, Abbas A.

2007-01-01

Electrical properties of nanocomposites are determined by the conductive paths of carbon black and influenced by a 'network' of silica. With increasing content of silica, carbon black (CB) particles are optimally dispersed, contributing to the generation of a conductive network between CB particles via direct particle contact and a tunneling effect; maximum conductivity for the epoxy resin-CB-silica nanocomposite described herein occurs at a ratio of 0.6:1.0 (SiO 2 :CB). As a non-conductive component, excessive silica will prevent electron flow, giving rise to low conductivity

Acceleration of Intended Pozzolanic Reaction under Initial Thermal Treatment for Developing Cementless Fly Ash Based Mortar

Directory of Open Access Journals (Sweden)

Yang-Hee Kwon

2017-02-01

Full Text Available Without using strong alkaline solution or ordinary Portland cement, a new structural binder consisting of fly ash and hydrated lime was hardened through an intensified pozzolanic reaction. The main experimental variables are the addition of silica fume and initial thermal treatment (60 °C for 3 days. A series of experiments consisting of mechanical testing (compressive and flexural strength, modulus of elasticity, X-ray diffraction, and measurements of the heat of hydration, pore structure, and shrinkage were conducted. These tests show that this new fly ash-based mortar has a compressive strength of 15 MPa at 91 days without any silica fume addition or initial thermal treatment. The strength increased to over 50 MPa based on the acceleration of the intensified pozzolanic reaction from the silica fume addition and initial thermal treatment. This is explained by a significant synergistic effect induced by the silica fume. It intensifies the pozzolanic reaction under thermal treatment and provides a space filling effect. This improved material performance can open a new pathway to utilize the industrial by-product of fly ash in cementless construction materials.

Effect of silica particle size on macrophage inflammatory responses.

Directory of Open Access Journals (Sweden)

Toshimasa Kusaka

Full Text Available Amorphous silica particles, such as nanoparticles (<100 nm diameter particles, are used in a wide variety of products, including pharmaceuticals, paints, cosmetics, and food. Nevertheless, the immunotoxicity of these particles and the relationship between silica particle size and pro-inflammatory activity are not fully understood. In this study, we addressed the relationship between the size of amorphous silica (particle dose, diameter, number, and surface area and the inflammatory activity (macrophage phagocytosis, inflammasome activation, IL-1β secretion, cell death and lung inflammation. Irrespective of diameter size, silica particles were efficiently internalized by mouse bone marrow-derived macrophages via an actin cytoskeleton-dependent pathway, and induced caspase-1, but not caspase-11, activation. Of note, 30 nm-1000 nm diameter silica particles induced lysosomal destabilization, cell death, and IL-1β secretion at markedly higher levels than did 3000 nm-10000 nm silica particles. Consistent with in vitro results, intra-tracheal administration of 30 nm silica particles into mice caused more severe lung inflammation than that of 3000 nm silica particles, as assessed by measurement of pro-inflammatory cytokines and neutrophil infiltration in bronchoalveolar lavage fluid of mice, and by the micro-computed tomography analysis. Taken together, these results suggest that silica particle size impacts immune responses, with submicron amorphous silica particles inducing higher inflammatory responses than silica particles over 1000 nm in size, which is ascribed not only to their ability to induce caspase-1 activation but also to their cytotoxicity.

Modified silica sol coatings for surface enhancement of leather.

Science.gov (United States)

Mahltig, Boris; Vossebein, Lutz; Ehrmann, Andrea; Cheval, Nicolas; Fahmi, Amir

2012-06-01

The presented study reports on differently modified silica sols for coating applications on leather. Silica sols are prepared by acidic hydrolysis of tetraethoxysilane and modified by silane compounds with fluorinated and non-fluorinated alkylgroups. In contrast to many earlier investigations regarding sol-gel applications on leather, no acrylic resin is used together with the silica sols when applying on leather. The modified silica particles are supposed to aggregate after application, forming thus a modified silica coating on the leather substrate. Scanning electron microscopy investigation shows that the applied silica coatings do not fill up or close the pores of the leather substrate. However, even if the pores of the leather are not sealed by this sol-gel coating, an improvement of the water repellent and oil repellent properties of the leather substrates are observed. These improved properties of leather by application of modified silica sols can provide the opportunity to develop sol-gel products for leather materials present in daily life.

Enhancement of Degradation and Dechlorination of Trichloroethylene via Supporting Palladium/Iron Bimetallic Nanoparticles onto Mesoporous Silica

Directory of Open Access Journals (Sweden)

Jianjun Wei

2016-07-01

Full Text Available This study is aimed to prevent the agglomeration of Pd/Fe bimetallic nanoparticles and thus improve the efficiency toward degradation and dechlorination of chlorinated organic contaminants. A mesoporous silica with a primary pore diameter of 8.3 nm and a specific surface area of 688 m2/g was prepared and used as the host of Pd/Fe nanoparticles. The Pd/Fe nanoparticles were deposited onto or into the mesoporous silica by reduction of ferrous ion and hexachloropalladate ion in aqueous phase. Batch degradation and dechlorination reactions of trichloroethylene were conducted with initial trichloroethylene concentration of 23.7 mg/L, iron loading of 203 or 1.91 × 103 mg/L and silica loading of 8.10 g/L at 25 °C. Concentration of trichloroethylene occurs on the supported Pd/Fe nanoparticles, with trichloroethylene degrading to 56% and 59% in 30 min on the supported Pd/Fe nanoparticles with weight percentage of palladium to iron at 0.075% and 0.10% respectively. The supported Pd/Fe nanoparticles exhibit better dechlorination activity. When the supported Pd/Fe nanoparticles with a weight percentage of palladium to iron of 0.10% were loaded much less than the bare counterpart, the yield of ethylene plus ethane in 10 h on them was comparable, i.e., 19% vs. 21%. This study offers a future approach to efficiently combine the reactivity of supported Pd/Fe nanoparticles and the adsorption ability of mesoporous silica.

Characterization for Post-treatment Effect of Bagasse Ash for Silica Extraction

OpenAIRE

Patcharin Worathanakul; Wisaroot Payubnop; Akhapon Muangpet

2009-01-01

Utilization of bagasse ash for silica sources is one of the most common application for agricultural wastes and valuable biomass byproducts in sugar milling. The high percentage silica content from bagasse ash was used as silica source for sodium silicate solution. Different heating temperature, time and acid treatment were studies for silica extraction. The silica was characterized using various techniques including X-ray fluorescence, X-ray diffraction, Scanning electro...

The development of flow-through bio-catalyst microreactors from silica micro structured fibers for lipid transformations.

Science.gov (United States)

Anuar, Sabiqah Tuan; Villegas, Carla; Mugo, Samuel M; Curtis, Jonathan M

2011-06-01

This study demonstrates the utility of a flow-through enzyme immobilized silica microreactor for lipid transformations. A silica micro structured fiber (MSF) consisting of 168 channels of internal diameter 4-5 μm provided a large surface area for the covalent immobilization of Candida antartica lipase. The specific activity of the immobilized lipase was determined by hydrolysis of p-nitrophenyl butyrate and calculated to be 0.81 U/mg. The catalytic performance of the lipase microreactor was demonstrated by the efficient ethanolysis of canola oil. The parameters affecting the performance of the MSF microreactor, including temperature and reaction flow rate, were investigated. Characterization of the lipid products exiting the microreactor was performed by non-aqueous reversed-phased liquid chromatography (NARP-LC) with evaporative light scattering detector (ELSD) and by comprehensive two-dimensional gas chromatography (GC x GC). Under optimized conditions of 1 μL/min flow rate of 5 mg/mL trioleoylglycerol (TO) in ethanol and 50 °C reaction temperature, 2-monooleoylglycerol was the main product at > 90% reaction yield. The regioselectivity of the Candida antartica lipase immobilized MSF microreactor in the presence of ethanol was found to be comparable to that obtained under conventional conditions. The ability of these reusable flow-through microreactors to regioselectively form monoacylglycerides in high yield from triacylglycerides demonstrate their potential use in small-scale lipid transformations or analytical lipids profiling.

Integrating reaction and analysis: investigation of higher-order reactions by cryogenic trapping

Directory of Open Access Journals (Sweden)

Skrollan Stockinger

2013-09-01

Full Text Available A new approach for the investigation of a higher-order reaction by on-column reaction gas chromatography is presented. The reaction and the analytical separation are combined in a single experiment to investigate the Diels–Alder reaction of benzenediazonium-2-carboxylate as a benzyne precursor with various anthracene derivatives, i.e. anthracene, 9-bromoanthracene, 9-anthracenecarboxaldehyde and 9-anthracenemethanol. To overcome limitations of short reaction contact times at elevated temperatures a novel experimental setup was developed involving a cooling trap to achieve focusing and mixing of the reactants at a defined spot in a fused-silica capillary. This trap functions as a reactor within the separation column in the oven of a gas chromatograph. The reactants are sequentially injected to avoid undefined mixing in the injection port. An experimental protocol was developed with optimized injection intervals and cooling times to achieve sufficient conversions at short reaction times. Reaction products were rapidly identified by mass spectrometric detection. This new approach represents a practical procedure to investigate higher-order reactions at an analytical level and it simultaneously provides valuable information for the optimization of the reaction conditions.

Silica particles and method of preparation thereof

NARCIS (Netherlands)

2015-01-01

The invention is in the field of silica products. More in particular, the invention is in the field of amorphous silica particles. The invention is directed to amorphous silica particles and related products including clusters of said silica particles, a suspension of said silica particles, and an

In situ-growth of silica nanowires in ceramic carbon composites

Directory of Open Access Journals (Sweden)

Rahul Kumar

2017-09-01

Full Text Available An understanding of the processing and microstructure of ceramic–carbon composites is critical to development of these composites for applications needing electrically conducting, thermal shock resistant ceramic materials. In the present study green compacts of carbon ceramic composites were prepared either by slurry processing or dry powder blending of one or more of the three — clay, glass, alumina and carbon black or graphite. The dried green compacts were sintered at 1400 °C in flowing argon. The ceramic carbon composites except the ones without clay addition showed formation of silica nanowires. The silica nanowire formation was observed in both samples prepared by slip casting and dry powder compaction containing either carbon black or graphite. TEM micrographs showed presence of carbon at the core of the silica nanowires indicating that carbon served the role of a catalyst. Selected area electron diffraction (SAED suggested that the silica nanowires are amorphous. Prior studies have reported formation of silica nanowires from silicon, silica, silicon carbide but this is the first report ever on formation of silica nanowires from clay.

Gas-Solid Displacement Reactions for Converting Silica Diatom Frustules into MgO and TiO₂

Energy Technology Data Exchange (ETDEWEB)

Kalem, Tugba [Iowa State Univ., Ames, IA (United States)

2004-01-01

Technology for the microfabrication of freely moving parts began with a Bell Labs microgear spun by an air jet, and electrostatic silicon micro motors in the mid-1980s. It continued with development work on micropositioning of optics, miniature heat exchangers, small fluidic devices, and chemical reaction chambers. Recently, there has been a great deal of interest centered on the design and manufacture of devices of nanometer proportions and this speculation has spawned a new industry named, nanotechnology. Despite the technological and economic promise of this technology, current commercial micro/mesofabrication methods have largely been based upon two-dimensional processing principles which is not well suited to the low-cost mass production of three-dimensional micro devices with complex geometries and meso/nanoscale features. Diatoms are three dimensional (3D) microstructures from nature that provide a practical alternative for nanotechnology and microfabrication. Diatoms (Figure 1) are single-celled micro algae that form rigid cell walls (frustules) composed of amorphous silica. Their dimensions can range from less than 1 micron to several hundreds of microns. They are distributed throughout the world in aquatic, semi-aquatic and moist habitats, and extremely abundant in freshwater and marine ecosystems. Diatoms are thought to be responsible for up to 25% of the world's net primary production of organic carbon (by transforming of carbon dioxide and water into sugars by photosynthesis). Approximately 10⁵ unique diatom frustule shapes have been claimed to exist in nature. The frustules are composed of two valves that fit together like a petri-dish, connected to each other by one or more girdle bands. The frustule wall consists of a nanoporous assembly of silica nanoparticles. They absorb soluble silica from water even at extremely low concentrations and metabolize and deposit it as an external skeleton. Continued reproduction of a single parent

Interactions of silica with iron oxides: Effects on oxide transformations and sorption properties

Energy Technology Data Exchange (ETDEWEB)

Taylor, P

1995-08-01

This report is a review of the literature on the adsorption of silica species on iron oxides and oxyhydroxides, and its effects on the adsorption of other species and on oxide interconversion reactions. The information is discussed briefly in the contexts of nuclear waste disposal and boiler-water chemistry. (author). 76 refs.

Interactions of silica with iron oxides: Effects on oxide transformations and sorption properties

International Nuclear Information System (INIS)

Taylor, P.

1995-08-01

This report is a review of the literature on the adsorption of silica species on iron oxides and oxyhydroxides, and its effects on the adsorption of other species and on oxide interconversion reactions. The information is discussed briefly in the contexts of nuclear waste disposal and boiler-water chemistry. (author). 76 refs

Granulation study of porous silica particles for MA recovery process

International Nuclear Information System (INIS)

Goto, Ichiro; Kofuji, Hirohide; Oriuchi, Akio; Watanabe, Sou; Takeuchi, Masayuki

2017-01-01

JAEA has been working on partition of MA from HLLW generated in the reprocessing by extraction chromatography technology. This technology utilizes 50 μm porous silica particles coated by styrene-divinylbenzene copolymer in which an extractant for MA recovery is impregnated as adsorbent. In this study, spray drying granulating experiments with various operating conditions and with different experimental apparatuses were carried out to find an appropriate condition to control the size of the particle and the pore. The target average sizes of the particle and pore are more than 50 μm and 600 nm respectively. Suspension containing fine silica particles were supplied to the spray drying devices, and small droplets generated through the spray nozzle were dried inside the drying chamber. In this study, viscosity of the feed solution and some granulation conditions were parametrically changed, and two different types of the spray nozzles were used. An air atomizing nozzle and a rotary disk nozzle were equipped at different chambers respectively. Then, performance of the product particle was evaluated by particle and pore size distributions and adsorption experiment after the polymer coating and an extractant impregnation. The particle size of the product depended on the atomizing pressure and viscosity of the feed solution, and the size increased with decrease in the pressure and in the viscosity. The maximum size obtained in this study was about 40 μm. Large viscosity of the feed solution lead poor recovery ratio and uniformity in the size distribution of the product powder. The pore size of the resultant particle was 550-800 nm as expected. As the type of the nozzle changed from the air atomizing nozzle to the rotary disk nozzle and size of the drying chamber became large, the average particle size and the particle size distribution became large and sharp, respectively. Rotation speed of the nozzle also influenced on the particle size, and targeted average size of the

Pre-concentration of pesticide residues in environmental water samples using Silica nanoparticles and identification of residues By GC-MS method

OpenAIRE

Tentu. Nageswara Rao; A. Muralidhar Reddy; SNVS. Murthy; Prathipati Revathi; K. Suneel Kumar

2016-01-01

The silica nanoparticles prepared by stober’s mechanism by reaction of tetraethylorthosilicate (TEOS) with ammonia was tested for their adsorption capacity in the pre-concentration of residues of pesticides in water. The synthesized nanoparticles were characterized by Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The size of the silica nanoparticles were 50 to 250 nm. The solid phase extraction (SPE) cartridges were prepared by filling...

Synchrotron WAXS and XANES studies of silica (SiO2) powders synthesized from Indonesian natural sands

International Nuclear Information System (INIS)

Muchlis, Khairanissa; Fauziyah, Nur Aini; Pratapa, Suminar; Soontaranon, Siriwat; Limpirat, Wanwisa

2017-01-01

In this study, we have investigated polymorphic silica (SiO 2 ) powders using, Wide Angle X-ray Scattering (WAXS) and X-Ray Absorption Near Edge Spectroscopy (XANES), laboratory X-Ray Diffraction (XRD) instruments. The WAXS and XANES spectra were collected using synchrotron radiation at Synchrotron Light Research Institute (SLRI), Nakhon Ratchasima, Thailand. The silica powders were obtained by processing silica sand from Tanah Laut, South Kalimantan, Indonesia. Purification process of silica sand was done by magnetic separation and immersion with HCl. The purification step was needed to reduce impurity or undesirable non Si elements. Three polymorphs of silica were produced, i.e. amorphous phase (A), quartz (B), and cristobalite (C). WAXS profile for each phase was presented in terms of intensity vs. 2θ prior to analyses. Both XRD (λ CuKα =1.54056 Å) and WAXS (λ=1.09 Å) patttern show that (1) A sample contains no crystallites, (2) B sample is monophasic, contains only quartz, and (3) C sample contains cristobalite and trydimite. XRD quantitative analysis using Rietica gave 98,8 wt% cristobalite, while the associated WAXS data provided 98.7 wt% cristobalite. Si K-edge XANES spectra were measured at energy range 1840 to 1920 eV. Qualitatively, the pre-edge and edge features for all phases are similar, but their main peaks in the post-edge region are different. (paper)

The central tower of the cathedral of Schleswig - New investigations to understand the alcali-silica reaction of historical mortars

Science.gov (United States)

Wedekind, Wanja; Protz, Andreas

2016-04-01

The damaging alcali-silica reaction leads to crack-formation and structural destruction at noumerous, constructed with cement mortar, buildings worldwide. The ASR-reaction causes the expansion of altered aggregates by the formation of a swelling gel. This gel consists of calcium silicate hydrate (C-S-H) that increases in volume with water, which exerts an expansive pressure inside the material. The cathedral of Schleswig is one of the oldest in northern Germany. The first church was built in 985-965. The Romanesque building part was erected around 1180 and the Gothic nave at the end of the 13th century. The central tower was constructed between 1888 and 1894 with brick and cement mortar. With 112 meters, the tower is the second-largest church spire of the country of Schleswig-Holstein in northern Germany. Due to the formation of cracks and damages from 1953 to 1956 first restoration works took place. Further developments of cracks are making restoration necessary again today. For developing a suitable conservation strategy, different investigations were done. The investigation included the determination of the pore space properties, the hygric and thermal dilatation and mercury porosimetry measurements. Furthermore, the application of cathodoluminescence microscopy may give information about the alteration process and microstructures present and reveal the differences between unaltered and altered mortars. An obvious relation between the porosity and the swelling intensity could be detected. Furthermore it becomes apparent, that a clear zonation of the mortar took place. The mortar near the surface is denser with a lower porosity and has a significantly lower swelling or dilatation.

Nano-porosity in silica reinforced methyltrimethoxysilane coatings studied by positron beam analysis

NARCIS (Netherlands)

Escobar Galindo, R.; Veen, A. van; Schut, H.; Falub, C.V.; Balkenende, A.R.; With, G. de; Hosson, J.Th.M. De

The porosity in particle reinforced sol-gel coatings has been studied. Silica particles (Ludox-TM40) are introduced into methyl silicate coatings to increase the hardness, the elastic modulus and the fracture toughness. The methyl silicate has a relatively low density (about 1.2 g/cm(2)), while the

Measurement and modelization of silica opal reflection properties: Optical determination of the silica index

Science.gov (United States)

Avoine, Amaury; Hong, Phan Ngoc; Frederich, Hugo; Frigerio, Jean-Marc; Coolen, Laurent; Schwob, Catherine; Nga, Pham Thu; Gallas, Bruno; Maître, Agnès

2012-10-01

Self-assembled artificial opals (in particular silica opals) constitute a model system to study the optical properties of three-dimensional photonic crystals. The silica optical index is a key parameter to correctly describe an opal but is difficult to measure at the submicrometer scale and usually treated as a free parameter. Here, we propose a method to extract the silica index from the opal reflection spectra and we validate it by comparison with two independent methods based on infrared measurements. We show that this index gives a correct description of the opal reflection spectra, either by a band structure or by a Bragg approximation. In particular, we are able to provide explanations in quantitative agreement with the measurements for two features : the observation of a second reflection peak in specular direction, and the quasicollapse of the p-polarized main reflection peak at a typical angle of 54∘.

Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bis-(L-tyrosinatocopper(II, Immersed in a Magnetite-Infused Silica Matrix

Directory of Open Access Journals (Sweden)

Massomeh Ghorbanloo

2016-01-01

Full Text Available Bis-(L-tyrosinatocopper(II was reacted with 3-(chloropropyl-trimethoxysilane functionalized silica that has infused magnetite to yield a magnetically separable catalyst in which the copper carboxylate is covalently linked to the silica matrix through the silane linkage. The immobilized catalyst has been characterized by spectroscopic studies (such as FT-IR, EPR, Magnetic Measurement, SEM and chemical analyses. The immobilized catalytic system functions as an efficient heterogeneous catalyst for oxidation of cyclohexene, toluene and ethyl benzene in the presence of hydrogen peroxide (as an oxidant and sodium bicarbonate (a co-catalyst. The reaction conditions have been optimized for solvent, temperature and amount of oxidant and catalyst. Comparison of the encapsulated catalyst with the corresponding homogeneous catalyst showed that the heterogeneous catalyst had higher activity and selectivity than the homogeneous catalyst. The immobilized catalyst could be readily recovered from the reaction mixture by using a simple magnet, and  reused up to five times without any loss of activity.

Application of a Microfluidic Reactor for Screening Cancer Prodrug Activation Using Silica-Immobilized Nitrobenzene Nitroreductase

Science.gov (United States)

2006-01-01

molecules18 can mediate an analogous reaction15 that combines the advantages of silica encapsulation with a signifi- cant reduction in cost... Alltech , Deerfield, IL) with a mobile phase of acetonitrile and water (containing 0.05% and 0.1% trifluoroacetic acid, respectively). The concentration

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 180silicas 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.

Respiratory health effects of exposure to crystalline silica epidemiology.

CSIR Research Space (South Africa)

Hnzido, E

1999-01-01

Full Text Available The present report describes two additional studies of exposure-response relationship between respiratory disease and silica dust in gold mines. Section 3 describes a study of pulmonary tuberculosis in relation to silica dust, and section 4...

Selective epoxidation of allylic alcohols with a titania-silica aerogel

Energy Technology Data Exchange (ETDEWEB)

Dusi, M.; Mallat, T.; Baiker, A. [Lab. of Technical Chemistry, Swiss Federal Inst. of Technology, ETH-Zentrum, Zuerich (Switzerland)

1998-12-31

An amorphous mesoporous titania-silica aerogel (20 wt%TiO{sub 2} - 80 wt% SiO{sub 2}) and tert.-butylhydroperoxide (TBHP) have been used for the epoxidation of various allylic alcohols. Allylic alcohols possessing an internal double bond were more reactive than those with a terminal C=C bond. Epoxide selectivities could be improved by addition of (basic) zeolite 4 A and NaHCO{sub 3} to the reaction mixture. (orig.)