Silane coupling agent bearing a photoremovable succinimidyl carbonate for patterning amines on glass and silicon surfaces with controlled surface densities.

PubMed

Nakayama, Hidekazu; Nakanishi, Jun; Shimizu, Takahiro; Yoshino, Yutaro; Iwai, Hideo; Kaneko, Shingo; Horiike, Yasuhiro; Yamaguchi, Kazuo

2010-03-01

Patterned immobilization of synthetic and biological ligands on material surfaces with controlled surface densities is important for various bioanalytical and cell biological purposes. This paper describes the synthesis, characterization, and application of a novel silane coupling agent bearing a photoremovable succinimidyl carbonate, which enables the photopatterning of various primary amines on glass and silicon surfaces. The silane coupling agent is 1-[5-methoxy-2-nitro-4-(3-trimethoxysilylpropyloxy)phenyl]ethyl N-succinimidyl carbonate. The distinct feature of this molecule is that it has a photocleavable 2-nitrobenzyl switch between a trimethoxysilyl group and a succinimidyl carbonate, each reactive to the hydroxy groups of inorganic oxides and primary amines. Based on this molecular design, the compound allows for the one-step introduction of succinimidyl carbonates onto the surface of glass and silicon, immobilization of primary amines, and region-selective and dose-dependent release of the amines by near-UV irradiation. Therefore, we were able to pattern amine ligands on the substrates in given surface densities and arbitrary geometries by controlling the doses and regions of photoirradiation. These features were verified by UV-vis spectroscopy, contact angle measurements, infrared (IR) spectroscopy, X-ray photoelectron spectroscopy (XPS), ellipsometry, and atomic force microscopy (AFM). The compound was applied to form a chemical density gradient of amino-biotin on a silicon substrate in a range of 0.87-0.12 chains/nm(2) by controlling photoirradiation under a standard fluorescence microscope. Furthermore, we also succeeded in forming a chemical density gradient at a lower surface density range (0.15-0.011 chains/nm(2)) on the substrate by diluting the feed amino-biotin with an inert control amine.

Corrosion protection of galvanized steels by silane-based treatments

NASA Astrophysics Data System (ADS)

Yuan, Wei

The possibility of using silane coupling agents as replacements for chromate treatments was investigated on galvanized steel substrates. In order to understand the influence of deposition parameters on silane film formation, pure zinc substrates were first used as a model for galvanized steel to study the interaction between silane coupling agents and zinc surfaces. The silane films formed on pure zinc substrates from aqueous solutions were characterized by ellipsometry, contact angle measurements, reflection absorption infrared spectroscopy, x-ray photoelectron spectroscopy, and atomic force microscopy. The deposition parameters studied include solution concentration, solution dipping time and pH value of the applied solution. It appears that silane film formation involved a true equilibrium of hydrolysis and condensation reactions in aqueous solutions. It has been found that the silane film thickness obtained depends primarily on the solution concentration and is almost independent of the solution dipping time. The molecular orientation of applied silane films is determined by the pH value of applied silane solutions and the isoelectric point of metal substrates. The deposition window in terms of pH value for zinc substrates is between 6.0 and 9.0. The total surface energy of the silane-coated pure zinc substrates decreases with film aging time, the decrease rate, however, is determined by the nature of silane coupling agents. Selected silane coupling agents were applied as prepaint or passivation treatments onto galvanized steel substrates. The corrosion protection provided by these silane-based treatments were evaluated by salt spray test, cyclic corrosion test, electrochemical impedance spectroscopy, and stack test. The results showed that silane coupling agents can possibly be used to replace chromates for corrosion control of galvanized steel substrates. Silane coatings provided by these silane treatments serve mainly as physical barriers. Factors that affect the performance of a silane coupling agent in the application of corrosion control include chemical reactivity, hydrophobic character, siloxane crosslinker network, and film thickness. Good protections afforded by the silane treatments are a synergetic effect of all these factors.

Method for encapsulating and isolating hazardous cations, medium for encapsulating and isolating hazardous cations

DOEpatents

Wasserman, S.R.; Anderson, K.B.; Song, K.; Yuchs, S.E.; Marshall, C.L.

1998-04-28

A method for encapsulating hazardous cations is provided comprising supplying a pretreated substrate containing the cations; contacting the substrate with an organo-silane compound to form a coating on the substrate; and allowing the coating to cure. A medium for containing hazardous cations is also provided, comprising a substrate having ion-exchange capacity and a silane-containing coating on the substrate. 3 figs.

Analysis of Gas Membrane Ultra-High Purification of Small Quantities of Mono-Isotopic Silane

DOE Office of Scientific and Technical Information (OSTI.GOV)

de Almeida, Valmor F.; Hart, Kevin J.

A small quantity of high-value, crude, mono-isotopic silane is a prospective gas for a small-scale, high-recovery, ultra-high membrane purification process. This is an unusual application of gas membrane separation for which we provide a comprehensive analysis of a simple purification model. The goal is to develop direct analytic expressions for estimating the feasibility and efficiency of the method, and guide process design; this is only possible for binary mixtures of silane in the dilute limit which is a somewhat realistic case. Among the common impurities in crude silane, methane poses a special membrane separation challenge since it is chemically similarmore » to silane. Other potential problematic surprises are: ethylene, diborane and ethane (in this order). Nevertheless, we demonstrate, theoretically, that a carefully designed membrane system may be able to purify mono-isotopic, crude silane to electronics-grade level in a reasonable amount of time and expenses. We advocate a combination of membrane materials that preferentially reject heavy impurities based on mobility selectivity, and light impurities based on solubility selectivity. We provide estimates for the purification of significant contaminants of interest. To improve the separation selectivity, it is advantageous to use a permeate chamber under vacuum, however this also requires greater control of in-leakage of impurities in the system. In this study, we suggest cellulose acetate and polydimethylsiloxane as examples of membrane materials on the basis of limited permeability data found in the open literature. We provide estimates on the membrane area needed and priming volume of the cell enclosure for fabrication purposes when using the suggested membrane materials. These estimates are largely theoretical in view of the absence of reliable experimental data for the permeability of silane. Last but not least, future extension of this work to the non-dilute limit may apply to the recovery of silane from rejected streams of natural silicon semi-conductor processes.« less

Modification of the internal surface of photonic crystal fibers with Ag and Au nanoparticles for application as sensor elements

NASA Astrophysics Data System (ADS)

Pidenko, Pavel S.; Borzov, Victor M.; Savenko, Olga A.; Skaptsov, Alexander A.; Skibina, Yulia S.; Goryacheva, Irina Yu.; Rusanova, Tatiana Yu.

2017-03-01

Photonic crystal fibers (PCFs) are one of the most promising materials for biosensors construction due to their unique optical properties. The modification of PCF by noble metal nanoparticles (NPs) provides the SPR and SERS signal detection where as the application amino group-containing compounds allows efficient binding of biomolecules. In this work the internal surface of glass hollow core photonic crystal fibers (HC-PCFs) has been modified Ag and Au nanoparticles using three different approaches. PCFs were treated by: 1) mixture of NPs and precursors for silanization (tetraethoxysilane (TEOS) and (3-aminopropyl)triethoxysilane (APTES)); 2) alternately deposition of polyelectrolytes and NPs, 3) mixture of chitosan with NPs. The shift of local maxima in the HC-PCF transmission spectrum has been selected as a signal for estimating the amount of NPs on the HC-PCF inner surface. The most efficient techniques were the chitosan application for Ag NPs and silanization for Au NPs. The obtaining PCFs could be useful for creating biosensitive elements.

Preparation of optically active bicyclodihydrosiloles by a radical cascade reaction

PubMed Central

Miyazaki, Koichiro; Yamane, Yu; Yo, Ryuichiro; Uno, Hidemitsu

2013-01-01

Summary Bicyclodihydrosiloles were readily prepared from optically active enyne compounds by a radical cascade reaction triggered by tris(trimethylsilyl)silane ((Me3Si)3SiH). The reaction was initiated by the addition of a silyl radical to an α,β-unsaturated ester, forming an α-carbonyl radical that underwent radical cyclization to a terminal alkyne unit. The resulting vinyl radical attacked the silicon atom in an SHi manner to give dihydrosilole. The reaction preferentially formed trans isomers of bicyclosiloles with an approximately 7:3 to 9:1 selectivity. PMID:23946827

Method of high purity silane preparation

DOEpatents

Tsuo, Y. Simon; Belov, Eugene P.; Gerlivanov, Vadim G.; Zadde, Vitali V.; Kleschevnikova, Solomonida I.; Korneev, Nikolai N.; Lebedev, Eugene N.; Pinov, Akhsarbek B.; Ryabenko, Eugene A.; Strebkov, Dmitry S.; Chernyshev, Eugene A.

2000-01-01

A process for the preparation of high purity silane, suitable for forming thin layer silicon structures in various semiconductor devices and high purity poly- and single crystal silicon for a variety of applications, is provided. Synthesis of high-purity silane starts with a temperature assisted reaction of metallurgical silicon with alcohol in the presence of a catalyst. Alcoxysilanes formed in the silicon-alcohol reaction are separated from other products and purified. Simultaneous reduction and oxidation of alcoxysilanes produces gaseous silane and liquid secondary products, including, active part of a catalyst, tetra-alcoxysilanes, and impurity compounds having silicon-hydrogen bonds. Silane is purified by an impurity adsorption technique. Unreacted alcohol is extracted and returned to the reaction with silicon. Concentrated mixture of alcoxysilanes undergoes simultaneous oxidation and reduction in the presence of a catalyst at the temperature -20.degree. C. to +40.degree. C. during 1 to 50 hours. Tetra-alcoxysilane extracted from liquid products of simultaneous oxidation and reduction reaction is directed to a complete hydrolysis. Complete hydrolysis of tetra-alcoxysilane results in formation of industrial silica sol and alcohol. Alcohol is dehydrated by tetra-alcoxysilane and returned to the reaction with silicon.

Lanthanum tricyanide-catalyzed acyl silane-ketone benzoin additions and kinetic resolution of resultant alpha-silyloxyketones.

PubMed

Tarr, James C; Johnson, Jeffrey S

2010-05-21

We report the full account of our efforts on the lanthanum tricyanide-catalyzed acyl silane-ketone benzoin reaction. The reaction exhibits a wide scope in both acyl silane (aryl, alkyl) and ketone (aryl-alkyl, alkyl-alkyl, aryl-aryl, alkenyl-alkyl, alkynyl-alkyl) coupling partners. The diastereoselectivity of the reaction has been examined in both cyclic and acyclic systems. Cyclohexanones give products arising from equatorial attack by the acyl silane. The diastereoselectivity of acyl silane addition to acyclic alpha-hydroxy ketones can be controlled by varying the protecting group to obtain either Felkin-Ahn or chelation control. The resultant alpha-silyloxyketone products can be resolved with selectivity factors from 10 to 15 by subjecting racemic ketone benzoin products to CBS reduction.

Improved antifouling properties and selective biofunctionalization of stainless steel by employing heterobifunctional silane-polyethylene glycol overlayers and avidin-biotin technology

PubMed Central

Hynninen, Ville; Vuori, Leena; Hannula, Markku; Tapio, Kosti; Lahtonen, Kimmo; Isoniemi, Tommi; Lehtonen, Elina; Hirsimäki, Mika; Toppari, J. Jussi; Valden, Mika; Hytönen, Vesa P.

2016-01-01

A straightforward solution-based method to modify the biofunctionality of stainless steel (SS) using heterobifunctional silane-polyethylene glycol (silane-PEG) overlayers is reported. Reduced nonspecific biofouling of both proteins and bacteria onto SS and further selective biofunctionalization of the modified surface were achieved. According to photoelectron spectroscopy analyses, the silane-PEGs formed less than 10 Å thick overlayers with close to 90% surface coverage and reproducible chemical compositions. Consequently, the surfaces also became more hydrophilic, and the observed non-specific biofouling of proteins was reduced by approximately 70%. In addition, the attachment of E. coli was reduced by more than 65%. Moreover, the potential of the overlayer to be further modified was demonstrated by successfully coupling biotinylated alkaline phosphatase (bAP) to a silane-PEG-biotin overlayer via avidin-biotin bridges. The activity of the immobilized enzyme was shown to be well preserved without compromising the achieved antifouling properties. Overall, the simple solution-based approach enables the tailoring of SS to enhance its activity for biomedical and biotechnological applications. PMID:27381834

Improved antifouling properties and selective biofunctionalization of stainless steel by employing heterobifunctional silane-polyethylene glycol overlayers and avidin-biotin technology

NASA Astrophysics Data System (ADS)

Hynninen, Ville; Vuori, Leena; Hannula, Markku; Tapio, Kosti; Lahtonen, Kimmo; Isoniemi, Tommi; Lehtonen, Elina; Hirsimäki, Mika; Toppari, J. Jussi; Valden, Mika; Hytönen, Vesa P.

2016-07-01

A straightforward solution-based method to modify the biofunctionality of stainless steel (SS) using heterobifunctional silane-polyethylene glycol (silane-PEG) overlayers is reported. Reduced nonspecific biofouling of both proteins and bacteria onto SS and further selective biofunctionalization of the modified surface were achieved. According to photoelectron spectroscopy analyses, the silane-PEGs formed less than 10 Å thick overlayers with close to 90% surface coverage and reproducible chemical compositions. Consequently, the surfaces also became more hydrophilic, and the observed non-specific biofouling of proteins was reduced by approximately 70%. In addition, the attachment of E. coli was reduced by more than 65%. Moreover, the potential of the overlayer to be further modified was demonstrated by successfully coupling biotinylated alkaline phosphatase (bAP) to a silane-PEG-biotin overlayer via avidin-biotin bridges. The activity of the immobilized enzyme was shown to be well preserved without compromising the achieved antifouling properties. Overall, the simple solution-based approach enables the tailoring of SS to enhance its activity for biomedical and biotechnological applications.

RAIN REPELLENT

DTIC Science & Technology

COATINGS, *RAINDROPS, *SILANES, *ULTRASONIC RADIATION, ACIDS, AEROSOLS, ALKOXY RADICALS, ALKYL RADICALS, CHLORIDES, FILMS, FLUORIDES, GLASS, LIQUIDS...MATERIALS, METHYL RADICALS, MIXTURES, ORGANIC COMPOUNDS, SALTS, STABILITY, STORAGE, SURFACES

Lanthanum Tricyanide-Catalyzed Acyl Silane-Ketone Benzoin Additions and Kinetic Resolution of Resultant α-Silyloxyketones

PubMed Central

Tarr, James C.

2010-01-01

We report the full account of our efforts on the lanthanum tricyanide-catalyzed acyl silane-ketone benzoin reaction. The reaction exhibits a wide scope in both acyl silane (aryl, alkyl) and ketone (aryl-alkyl, alkyl-alkyl, aryl-aryl, alkenyl-alkyl, alkynyl-alkyl) coupling partners. The diastereoselectivity of the reaction has been examined in both cyclic and acyclic systems. Cyclohexanones give products arising from equatorial attack by the acyl silane. The diastereoselectivity of acyl silane addition to acyclic α-hydroxy ketones can be controlled by varying the protecting group to obtain either Felkin-Ahn or chelation control. The resultant α-silyloxyketone products can be resolved with selectivity factors from 10 to 15 by subjecting racemic ketone benzoin products to CBS reduction. PMID:20392127

Evaluation of experimental installation of silane treatment on bridges : final report.

DOT National Transportation Integrated Search

1988-04-01

In this project the effectiveness of silane-based chemicals as concrete sealants was evaluated for selected bridges throughout the state of Louisiana for a five-year period. The field evaluation was initiated after satisfactory results in the laborat...

Mesoporous Silicate Materials in Sensing

PubMed Central

Melde, Brian J.; Johnson, Brandy J.; Charles, Paul T.

2008-01-01

Mesoporous silicas, especially those exhibiting ordered pore systems and uniform pore diameters, have shown great potential for sensing applications in recent years. Morphological control grants them versatility in the method of deployment whether as bulk powders, monoliths, thin films, or embedded in coatings. High surface areas and pore sizes greater than 2 nm make them effective as adsorbent coatings for humidity sensors. The pore networks also provide the potential for immobilization of enzymes within the materials. Functionalization of materials by silane grafting or through co-condensation of silicate precursors can be used to provide mesoporous materials with a variety of fluorescent probes as well as surface properties that aid in selective detection of specific analytes. This review will illustrate how mesoporous silicas have been applied to sensing changes in relative humidity, changes in pH, metal cations, toxic industrial compounds, volatile organic compounds, small molecules and ions, nitroenergetic compounds, and biologically relevant molecules. PMID:27873810

An investigation of chemically-induced improvement in saturation moisture characteristics of epoxies

NASA Technical Reports Server (NTRS)

Singh, J. J.; St.clair, T. L.; Stoakley, D. M.

1984-01-01

MY-720/DDS epoxy samples were treated with three selected chemical compounds to render the active H-sites inactive for moisture absorption. Treating the epoxy castings with acetyl chloride and dichlorodimethyl silane leads only to surface changes indicating that these molecules are too large to penetrate the epoxy castings. Boron trifluoride, on the other hand, does penetrate the epoxy chain as is indicated by the formation of green domains in the interior of the castings. However, the process of saturating the specimens with moisture appears to leach out the chemical additives--thereby nullifying their possible ameliorative effects.

Photochemical dimerization and functionalization of alkanes, ethers, primary alcohols and silanes

DOEpatents

Crabtree, Robert H.; Brown, Stephen H.

1988-01-01

The space-time yield and/or the selectivity of the photochemical dimerization of alkanes, ethers, primary alcohols and tertiary silanes with Hg and U.V. light is enhanced by refluxing the substrate in the irradiated reaction zone at a temperature at which the dimer product condenses and remains condensed promptly upon its formation. Cross-dimerization of the alkanes, ethers and silanes with primary alcohols is disclosed, as is the functionalization to aldehydes of the alkanes with carbon monoxide.

Photochemical dimerization and functionalization of alkanes, ethers, primary alcohols and silanes

DOEpatents

Crabtree, R.H.; Brown, S.H.

1988-02-16

The space-time yield and/or the selectivity of the photochemical dimerization of alkanes, ethers, primary alcohols and tertiary silanes with Hg and U.V. light is enhanced by refluxing the substrate in the irradiated reaction zone at a temperature at which the dimer product condenses and remains condensed promptly upon its formation. Cross-dimerization of the alkanes, ethers and silanes with primary alcohols is disclosed, as is the functionalization to aldehydes of the alkanes with carbon monoxide.

Resistivity behavior of hydrogen and liquid silane at high shock compression

NASA Astrophysics Data System (ADS)

Wang, Yi-Gao; Liu, Fu-Sheng; Liu, Qi-Jun

2018-07-01

To study the electrical properties of hydrogen rich compounds under extreme conditions, the electrical resistivity of density hydrogen and silane fluid was measured, respectively. The hydrogen sample was prepared by compressing pure hydrogen gas to 10 MPa in a coolant target system at the temperature of 77 K. The silane sample can be obtained with the same method. High-pressure and high-temperature experiments were performed using a two-stage light-gas gun. The electrical resistivity of the sample decreased with increasing pressure and temperature as expected. A minimum electrical resistivity value of 0.3 × 10-3 Ω cm at 138 GPa and 4100 K was obtained for silane. The minimum resistivity of hydrogen in the state of 102 GPa and 4300 K was 0.35 Ω cm. It showed that the measured electrical resistivity of the shock-compressed hydrogen was an order of magnitude higher than fluid silane at 50-90 GPa. However, beyond 100 GPa, the resistivity difference between silane and hydrogen was very minor. The carriers in the sample were hydrogen, and the concentration of hydrogen atoms in these two substances was close to each other. These results supported the theoretical prediction that silane was interpreted simply in terms of chemical decomposition into silicon nanoparticles and fluid hydrogen, and electrical conduction flows predominately dominated by the fluid hydrogen. In addition, the results also supported the theory of "chemical precompression", the existence of Sisbnd H bond helped to reduce the pressure of hydrogen metallization. These findings could lead the way for further metallic phases of hydrogen-rich materials and experimental studies.

Lewis Acidity of Bis(perfluorocatecholato)silane: Aldehyde Hydrosilylation Catalyzed by a Neutral Silicon Compound

DOE PAGES

Liberman-Martin, Allegra L.; Bergman, Robert G.; Tilley, T. Don

2015-04-16

Bis(perfluorocatecholato)silane Si(cat( F) 2 was prepared, and stoichiometric binding to Lewis bases was demonstrated with fluoride, triethylphosphine oxide, and N,N'-diisopropylbenzamide. The potent Lewis acidity of Si(cat( F) 2 was suggested from catalytic hydrosilylation and silylcyanation reactions with aldehydes. Mechanistic studies of hydrosilylation using an optically active silane substrate, R-(+)-methyl-(1-naphthyl)phenylsilane, proceeded with predominant stereochemical retention at silicon, consistent with a carbonyl activation pathway. The enantiospecificity was dependent on solvent and salt effects, with increasing solvent polarity or addition of NBu 4BAr( F) 4 leading to a diminished enantiomeric ratio. The medium effects are consistent with an ionic mechanism, wherein hydride transfermore » occurs prior to silicon-oxygen bond formation.« less

Photochemical dimerization and functionalization of alkanes, ethers, primary and secondary alcohols, phosphine oxides and silanes

DOEpatents

Crabtree, Robert H.; Brown, Stephen H.

1989-01-01

The space-time yield and/or the selectivity of the photochemical dimerization of alkanes, ethers, primary and secondary alcohols, phosphine oxides and primary, secondary and tertiary silanes with Hg and U.V. light is enhanced by refluxing the substrate in the irradiated reaction zone at a temperature at which the dimer product condenses and remains condensed promptly upon its formation. Cross-dimerization of the alkanes, ethers and silanes with primary alcohols is disclosed, as is the functionalization to aldehydes of the alkanes with carbon monoxide.

Photochemical dimerization and functionalization of alkanes, ethers, primary and secondary alcohols, phosphine oxides and silanes

DOEpatents

Crabtree, R.H.; Brown, S.H.

1989-10-17

The space-time yield and/or the selectivity of the photochemical dimerization of alkanes, ethers, primary and secondary alcohols, phosphine oxides and primary, secondary and tertiary silanes with Hg and U.V. light is enhanced by refluxing the substrate in the irradiated reaction zone at a temperature at which the dimer product condenses and remains condensed promptly upon its formation. Cross-dimerization of the alkanes, ethers and silanes with primary alcohols is disclosed, as is the functionalization to aldehydes of the alkanes with carbon monoxide.

Novel SiO2-deposited CaF2 substrate for vibrational sum-frequency generation (SFG) measurements of chemisorbed monolayers in an aqueous environment.

PubMed

Padermshoke, Adchara; Konishi, Shouta; Ara, Masato; Tada, Hirokazu; Ishibashi, Taka-Aki

2012-06-01

A novel SiO(2)-deposited CaF(2) (SiO(2)/CaF(2)) substrate for measuring vibrational sum-frequency generation (SFG) spectra of silane-based chemisorbed monolayers in aqueous media has been developed. The substrate is suitable for silanization and transparent over a broad range of the infrared (IR) probe. The present work demonstrates the practical application of the SiO(2)/CaF(2) substrate and, to our knowledge, the first SFG spectrum at the solid/water interface of a silanized monolayer observed over the IR fingerprint region (1780-1400 cm(-1)) using a back-side probing geometry. This new substrate can be very useful for SFG studies of various chemisorbed organic molecules, particularly biological compounds, in aqueous environments.

Reactivity of sulfide-containing silane toward boehmite and in situ modified rubber/boehmite composites by the silane

NASA Astrophysics Data System (ADS)

Lin, Tengfei; Zhu, Lixin; Chen, Weiwei; Wu, Siwu; Guo, Baochun; Jia, Demin

2013-09-01

The silanization reaction between boehmite (BM) nanoplatelets and bis-[3-(triethoxysilyl)-propyl]-tetrasulfide (TESPT) was characterized in detail. Via such modification process, the grafted sulfide moieties on the BM endow reactivity toward rubber and substantially improved hydrophobicity for BM. Accordingly, TESPT was employed as in situ modifier for the nitrile rubber (NBR)/BM compounds to improve the mechanical properties of the reinforced vulcanizates. The effects of BM content and in situ modification on the mechanical properties, curing characteristics and morphology were investigated. BM was found to be effective in improving the mechanical performance of NBR vulcanizates. The NBR/BM composites could be further strengthened by the incorporation of TESPT. The interfacial adhesion of NBR/BM composites was obviously improved by the addition of TESPT. The substantially improved mechanical performance was correlated to the interfacial reaction and the improved dispersion of BM in rubber matrix.

Free-radical cyclizations onto differently substituted 1,2,3-triazoles installed in sugar templates.

PubMed

Marco-Contelles, J; Rodríguez-Fernández, M

2001-06-01

The synthesis and manipulation of differently substituted 1,2,3-triazoles (7-11 and 12-16) installed in sugar templates gave compounds 29-34 and 44-50, after reaction with tributyltin hydride or tris(trimethylsilyl)silane. Following standard procedures compound 44 was transformed into piperidinose derivative 54. These compounds are chiral, useful building blocks for the synthesis of glycosidase inhibitors of the fused-azole piperidinose type.

Photoluminescent silicon nanocrystals with chlorosilane surfaces - synthesis and reactivity

NASA Astrophysics Data System (ADS)

Höhlein, Ignaz M. D.; Kehrle, Julian; Purkait, Tapas K.; Veinot, Jonathan G. C.; Rieger, Bernhard

2014-12-01

We present a new efficient two-step method to covalently functionalize hydride terminated silicon nanocrystals with nucleophiles. First a reactive chlorosilane layer was formed via diazonium salt initiated hydrosilylation of chlorodimethyl(vinyl)silane which was then reacted with alcohols, silanols and organolithium reagents. With organolithium compounds a side reaction is observed in which a direct functionalization of the silicon surface takes place.We present a new efficient two-step method to covalently functionalize hydride terminated silicon nanocrystals with nucleophiles. First a reactive chlorosilane layer was formed via diazonium salt initiated hydrosilylation of chlorodimethyl(vinyl)silane which was then reacted with alcohols, silanols and organolithium reagents. With organolithium compounds a side reaction is observed in which a direct functionalization of the silicon surface takes place. Electronic supplementary information (ESI) available: Detailed experimental procedures and additional NMR, PL, EDX, DLS and TEM data. See DOI: 10.1039/C4NR05888G

The Effect of Silane Addition on Chitosan-Fly Ash/CTAB as Electrolyte Membrane

NASA Astrophysics Data System (ADS)

Kusumastuti, E.; Isnaeni, D.; Sulistyaningsih, T.; Mahatmanti, F. W.; Jumaeri; Atmaja, L.; Widiastuti, N.

2017-02-01

Electrolyte membrane is an important component in fuel cell system, because it may influence fuel cell performance. Many efforts have been done to produce electrolyte membrane to replace comercial membrane. In this research, electrolyte membrane is composed of chitosan as an organic matrix and fly ash modified with CTAB and silane as inorganic filler. Fly ash is modified using silane as coupling agent to improve interfacial morphology between organic matrix and inorganic filler. This research aims to determine the best membrane performance based on its characteristics such as water uptake, mechanical properties, proton conductivity, and methanol permeability. The steps that have been done include silica preparation from fly ash, modification of silica surface with CTAB, silica coupling process with silane, synthesis of membranes with inversion phase method, and membrane characterization. The result shows that membrane C-FA/CTAB-Silane 10% (w/w) has the best performance with proton conductivity 8.00 x 10-4 S.cm-1, methanol permeability 3.37 x 10-7 cm.s-1, and selectivity 2.12 x 103 S.s.cm-3. The result of FTIR analysis on membrane C-FA/CTAB-Silane 10% shows that there is only physical interaction occured between chitosan, fly ash and silane, because there is no peak differences significantly at wave number 1000-1250 cm-1, while morphology analysis on membrane with Scanning Electron Microscopy (SEM) shows good dispersion and there is no agglomeration on chitosan matrix.

A sensitive and selective chemiluminescence sensor for the determination of dopamine based on silanized magnetic graphene oxide-molecularly imprinted polymer.

PubMed

Duan, Huimin; Li, Leilei; Wang, Xiaojiao; Wang, Yanhui; Li, Jianbo; Luo, Chuannan

2015-03-15

Based on silanized magnetic graphene oxide-molecularly imprinted polymer (Si-MG-MIP), a sensitive and selective chemiluminescence sensor for dopamine measurement was developed. Si-MG-MIP, in which silanes was introduced to improve the mass transfer, graphene oxide was employed to improve absorption capacity, Fe3O4 nanoparticles were applied for separation easily and molecularly imprinted polymer was used to improve selectivity, demonstrated the advantages of the sensor. All the composites were confirmed by SEM, TEM, XRD and FTIR. Under the optimal conditions of chemiluminescence, dopamine could be assayed in the range of 8.0-200.0 ng/mL with a correlation coefficient of linear regression of 0.9970. The detection limit was 1.5 ng/mL (3δ) and the precision for 11 replicate detections of 80.0 ng/mL dopamine was 3.4% (RSD). When the sensor was applied in determining dopamine in actual samples, recovery ranged from 94% to 110%, which revealed that the results were satisfactory. Copyright © 2014 Elsevier B.V. All rights reserved.

A sensitive and selective chemiluminescence sensor for the determination of dopamine based on silanized magnetic graphene oxide-molecularly imprinted polymer

NASA Astrophysics Data System (ADS)

Duan, Huimin; Li, Leilei; Wang, Xiaojiao; Wang, Yanhui; Li, Jianbo; Luo, Chuannan

2015-03-01

Based on silanized magnetic graphene oxide-molecularly imprinted polymer (Si-MG-MIP), a sensitive and selective chemiluminescence sensor for dopamine measurement was developed. Si-MG-MIP, in which silanes was introduced to improve the mass transfer, graphene oxide was employed to improve absorption capacity, Fe3O4 nanoparticles were applied for separation easily and molecularly imprinted polymer was used to improve selectivity, demonstrated the advantages of the sensor. All the composites were confirmed by SEM, TEM, XRD and FTIR. Under the optimal conditions of chemiluminescence, dopamine could be assayed in the range of 8.0-200.0 ng/mL with a correlation coefficient of linear regression of 0.9970. The detection limit was 1.5 ng/mL (3δ) and the precision for 11 replicate detections of 80.0 ng/mL dopamine was 3.4% (RSD). When the sensor was applied in determining dopamine in actual samples, recovery ranged from 94% to 110%, which revealed that the results were satisfactory.

Development of a model and computer code to describe solar grade silicon production processes

NASA Technical Reports Server (NTRS)

Srivastava, R.; Gould, R. K.

1979-01-01

Mathematical models, and computer codes based on these models were developed which allow prediction of the product distribution in chemical reactors in which gaseous silicon compounds are converted to condensed phase silicon. The reactors to be modeled are flow reactors in which silane or one of the halogenated silanes is thermally decomposed or reacted with an alkali metal, H2 or H atoms. Because the product of interest is particulate silicon, processes which must be modeled, in addition to mixing and reaction of gas-phase reactants, include the nucleation and growth of condensed Si via coagulation, condensation, and heterogeneous reaction.

Chemical vapor deposition of silicon, silicon dioxide, titanium and ferroelectric thin films

NASA Astrophysics Data System (ADS)

Chen, Feng

Various silicon-based thin films (such as epitaxial, polycrystalline and amorphous silicon thin films, silicon dioxide thin films and silicon nitride thin films), titanium thin film and various ferroelectric thin films (such as BaTiO3 and PbTiO3 thin films) play critical roles in the manufacture of microelectronics circuits. For the past few years, there have been tremendous interests to search for cheap, safe and easy-to-use methods to develop those thin films with high quality and good step coverage. Silane is a critical chemical reagent widely used to deposit silicon-based thin films. Despite its wide use, silane is a dangerous material. It is pyrophoric, extremely flammable and may explode from heat, shock and/or friction. Because of the nature of silane, serious safety issues have been raised concerning the use, transportation, and storage of compressed gas cylinders of silane. Therefore it is desired to develop safer ways to deposit silicon-based films. In chapter III, I present the results of our research in the following fields: (1) Silane generator, (2) Substitutes of silane for deposition of silicon and silicon dioxide thin films, (3) Substitutes of silane for silicon dioxide thin film deposition. In chapter IV, hydropyridine is introduced as a new ligand for use in constructing precursors for chemical vapor deposition. Detachement of hydropyridine occurs by a low-temperature reaction leaving hydrogen in place of the hydropyridine ligands. Hydropyridine ligands can be attached to a variety of elements, including main group metals, such as aluminum and antimony, transition metals, such as titanium and tantalum, semiconductors such as silicon, and non-metals such as phosphorus and arsenic. In this study, hydropyridine-containing titanium compounds were synthesized and used as chemical vapor deposition precursors for deposition of titanium containing thin films. Some other titanium compounds were also studied for comparison. In chapter V, Chemical Vapor Depositions (CVD) of many oxide thin films including ferroelectric and high dielectric constant BaTiO3, SrTiO 3 and PbTiO3 films had been carried out under reduced pressure (30 torr--80 torr) using liquid precursors containing beta-diketone ligands. The relative reactivities of Ba(beta-diketonate)2, Sr(beta-diketonate) 2, Pb(beta-diketonate)2, Ti(beta-diketonate)3, TiO(beta-diketonate)2 and Ti(OiPr)2(beta-diketonate) 2 had been studied individually prior to the deposition of BaTiO 3, SrTiO3 and PbTiO3 thin films from the mixtures of corresponding precursors. By using multi-step deposition method, carbon free stoichiometric BaTiO3 thin films uniform in large area have been achieved.

Mild partial deoxygenation of esters catalyzed by an oxazolinylborate-coordinated rhodium silylene

DOE PAGES

Xu, Songchen; Boschen, Jeffery S.; Biswas, Abhranil; ...

2015-08-17

An electrophilic, coordinatively unsaturated rhodium complex supported by borate-linked oxazoline, oxazoline-coordinated silylene, and N-heterocyclic carbene donors [{κ³-N,Si,C-PhB(Ox Me²)(Ox Me²SiHPh)Im Mes}Rh(H)CO][HB(C₆F₅)₃] (2, Ox Me² = 4,4-dimethyl-2-oxazoline; Im Mes = 1-mesitylimidazole) is synthesized from the neutral rhodium silyl {PhB(Ox Me²)₂Im Mes}RhH(SiH 2Ph)CO (1) and B(C 6F 5) 3. The unusual oxazoline-coordinated silylene structure in 2 is proposed to form by rearrangement of an unobserved isomeric cationic rhodium silylene species [{PhB(Ox Me²)₂Im Mes}RhH(SiHPh)CO][HB(C₆F₅)₃] generated by H abstraction. Complex 2 catalyzes reductions of organic carbonyl compounds with silanes to give hydrosilylation products or deoxygenation products. The pathway to these reactions is primarily influenced bymore » the degree of substitution of the organosilane. Reactions with primary silanes give deoxygenation of esters to ethers, amides to amines, and ketones and aldehydes to hydrocarbons, whereas tertiary silanes react to give 1,2-hydrosilylation of the carbonyl functionality. In contrast, the strong Lewis acid B(C₆F₅)₃ catalyzes the complete deoxygenation of carbonyl compounds to hydrocarbons with PhSiH₃ as the reducing agent.« less

Mild partial deoxygenation of esters catalyzed by an oxazolinylborate-coordinated rhodium silylene

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Songchen; Boschen, Jeffery S.; Biswas, Abhranil

An electrophilic, coordinatively unsaturated rhodium complex supported by borate-linked oxazoline, oxazoline-coordinated silylene, and N-heterocyclic carbene donors [{κ³-N,Si,C-PhB(Ox Me²)(Ox Me²SiHPh)Im Mes}Rh(H)CO][HB(C₆F₅)₃] (2, Ox Me² = 4,4-dimethyl-2-oxazoline; Im Mes = 1-mesitylimidazole) is synthesized from the neutral rhodium silyl {PhB(Ox Me²)₂Im Mes}RhH(SiH 2Ph)CO (1) and B(C 6F 5) 3. The unusual oxazoline-coordinated silylene structure in 2 is proposed to form by rearrangement of an unobserved isomeric cationic rhodium silylene species [{PhB(Ox Me²)₂Im Mes}RhH(SiHPh)CO][HB(C₆F₅)₃] generated by H abstraction. Complex 2 catalyzes reductions of organic carbonyl compounds with silanes to give hydrosilylation products or deoxygenation products. The pathway to these reactions is primarily influenced bymore » the degree of substitution of the organosilane. Reactions with primary silanes give deoxygenation of esters to ethers, amides to amines, and ketones and aldehydes to hydrocarbons, whereas tertiary silanes react to give 1,2-hydrosilylation of the carbonyl functionality. In contrast, the strong Lewis acid B(C₆F₅)₃ catalyzes the complete deoxygenation of carbonyl compounds to hydrocarbons with PhSiH₃ as the reducing agent.« less

Detection and distribution analysis of organosilicon compounds in wood by means of SEM-EDX and micro-CT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vetter, L. de; Cnudde, V.; Masschaele, B.

This article explores the potential of a scanning electron microscope with an energy dispersive X-ray spectrometer in combination with a new non-destructive 3D visualization technique, X-ray micro-computed tomography, as detection methods for siloxanes/silanes mixtures applied as wood preservatives. In order to have a higher contrast, bromine functional silane was added to the mixture. Scots pine and beech samples were dipped or impregnated with the mixture and subsequently scanned. Both silicon and bromine were easily detectable with both techniques. Dipped siloxanes/silanes covered the cell walls partly in beech and the lumen partly or completely in Scots pine. Impregnated siloxanes/silanes could bemore » found in the cell walls of both wood species. From the results, it can be concluded that, under the circumstances as described in the article, impregnation with a siloxane is necessary to have cell wall penetration. The combination of scanning electron microscopy, energy dispersive X-ray spectroscopy and micro-computed tomography can offer important information concerning the localization of certain products inside wood. While the last of these can monitor changes in 3D, the other two techniques can provide detailed 2D information. Both techniques are complementary and provide important extra information.« less

[Effect of amount of silane coupling agent on flexural strength of dental composite resins reinforced with aluminium borate whisker].

PubMed

Zhu, Ming-yi; Zhang, Xiu-yin

2015-06-01

To evaluate the effect of amount of silane coupling agent on flexural strength of dental composite resins reinforced with aluminium borate whisker (ABW). ABW was surface-treated with 0%, 1%, 2%, 3% and 4% silan coupling agent (γ-MPS), and mixed with resin matrix to synthesize 5 groups of composite resins. After heat-cured at 120 degrees centigrade for 1 h, specimens were tested in three-point flexure to measure strength according to ISO-4049. One specimen was selected randomly from each group and observed under scanning electron microscope (SEM). The data was analyzed with SAS 9.2 software package. The flexural strength (117.93±11.9 Mpa) of the group treated with 2% silane coupling agent was the highest, and significantly different from that of the other 4 groups (α=0.01). The amount of silane coupling agent has impact on the flexural strength of dental composite resins reinforced with whiskers; The flexual strength will be reduced whenever the amount is higher or lower than the threshold. Supported by Research Fund of Science and Technology Committee of Shanghai Municipality (08DZ2271100).

Chemical Selectivity and Sensitivity of a 16-Channel Electronic Nose for Trace Vapour Detection

PubMed Central

Strle, Drago; Trifkovič, Mario; Van Miden, Marion; Kvasić, Ivan; Zupanič, Erik; Muševič, Igor

2017-01-01

Good chemical selectivity of sensors for detecting vapour traces of targeted molecules is vital to reliable detection systems for explosives and other harmful materials. We present the design, construction and measurements of the electronic response of a 16 channel electronic nose based on 16 differential microcapacitors, which were surface-functionalized by different silanes. The e-nose detects less than 1 molecule of TNT out of 10+12 N2 molecules in a carrier gas in 1 s. Differently silanized sensors give different responses to different molecules. Electronic responses are presented for TNT, RDX, DNT, H2S, HCN, FeS, NH3, propane, methanol, acetone, ethanol, methane, toluene and water. We consider the number density of these molecules and find that silane surfaces show extreme affinity for attracting molecules of TNT, DNT and RDX. The probability to bind these molecules and form a surface-adsorbate is typically 10+7 times larger than the probability to bind water molecules, for example. We present a matrix of responses of differently functionalized microcapacitors and we propose that chemical selectivity of multichannel e-nose could be enhanced by using artificial intelligence deep learning methods. PMID:29292764

Surface modification of carbon nanotubes using 3-aminopropyltriethoxysilane to improve mechanical properties of nanocomposite based polymer matrix: Experimental and Density functional theory study

NASA Astrophysics Data System (ADS)

Hamed Mashhadzadeh, A.; Fereidoon, Ab.; Ghorbanzadeh Ahangari, M.

2017-10-01

In current study we combined theoretical and experimental studies to evaluate the effect of functionalization and silanization on mechanical behavior of polymer-based/CNT nanocomposites. Epoxy was selected as thermoset polymer, polypropylene and poly vinyl chloride were selected as thermoplastic polymers. The whole procedure is divided to two sections . At first we applied density functional theory (DFT) to analyze the effect of functionalization on equilibrium distance and adsorption energy of unmodified, functionalized by sbnd OH group and silanized epoxy/CNT, PP/CNT and PVC/CNT nanocomposites and the results showed that functionalization increased adsorption energy and reduced the equilibrium distance in all studied nanocomposites and silanization had higher effect comparing to OH functionalizing. Then we prepared experimental samples of all mentioned nanocomposites and tested their tensile and flexural strength properties. The obtained results showed that functionalization increased the studied mechanical properties in all evaluated nanocomposites. Finally we compared the results of experimental and theoretical sections with each other and estimated a suitable agreement between these parts.

Covalent immobilization of molecularly imprinted polymer nanoparticles using an epoxy silane.

PubMed

Kamra, Tripta; Chaudhary, Shilpi; Xu, Changgang; Johansson, Niclas; Montelius, Lars; Schnadt, Joachim; Ye, Lei

2015-05-01

Molecularly imprinted polymers (MIPs) can be used as antibody mimics to develop robust chemical sensors. One challenging problem in using MIPs for sensor development is the lack of reliable conjugation chemistry that allows MIPs to be fixed on transducer surface. In this work, we study the use of epoxy silane to immobilize MIP nanoparticles on model transducer surfaces without impairing the function of the immobilized nanoparticles. The MIP nanoparticles with a core-shell structure have selective molecular binding sites in the core and multiple amino groups in the shell. The model transducer surface is functionalized with a self-assembled monolayer of epoxy silane, which reacts with the core-shell MIP particles to enable straightforward immobilization. The whole process is characterized by studying the treated surfaces after each preparation step using atomic force microscopy, scanning electron microscopy, fluorescence microscopy, contact angle measurements and X-ray photoelectron spectroscopy. The microscopy results show that the MIP particles are immobilized uniformly on surface. The photoelectron spectroscopy results further confirm the action of each functionalization step. The molecular selectivity of the MIP-functionalized surface is verified by radioligand binding analysis. The particle immobilization approach described here has a general applicability for constructing selective chemical sensors in different formats. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

COMPARISON OF TRICHLOROETHYLENE REDUCTIVE DEHALOGENATION BY MICROBIAL COMMUNITIES STIMULATED ON SILICON-BASED ORGANIC COMPOUNDS AS SLOW-RELEASE ANAEROBIC SUBSTRATES. (R828772C001)

EPA Science Inventory

Microcosm studies were conducted to demonstrate the effectiveness of tetrabutoxysilane (TBOS) as a slow-release anaerobic substrate to promote reductive dehalogenation of trichloroethylene (TCE). The abiotic hydrolysis of TBOS and tetrakis(2-ethylbutoxy)silane (TKEBS), and the...

A STUDY OF HIGH MODULUS, HIGH STRENGTH FILAMENT MATERIALS BY DEPOSITION TECHNIQUES.

DTIC Science & Technology

had an average tensile strength of 240000 psi. The x-ray spectra of silicon carbide filaments made from SiCl4 , trichlorosilane, and...trichloromethylsilane were compared. The filaments produced from the two silane compounds showed strong peaks of SiC whereas the spectra for the SiCl4 produced

Using mechanisms of hydrolysis and sorption to reduce siloxanes occurrence in biogas of anaerobic sludge digesters.

PubMed

Gatidou, Georgia; Arvaniti, Olga S; Stasinakis, Athanasios S; Thomaidis, Nikolaos S; Andersen, Henrik R

2016-12-01

Hydrolysis of hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6) and dodecamethylcyclohexasilane (D6_silane) and their sorption to digested sludge was studied in batch experiments. Hydrolysis was affected by the type of the compound and the applied temperature, while the relevant half-life values ranged between 0.07±0.01d (D3, 55°C) and 48.4±17.1d (D6_silane, 4°C). D5 showed the greatest affinity for sorption to digested sludge (logK d : 3.84±3.42), the lowest LogK d value was found for D3 (1.46±0.95). Prediction of investigated compounds' fate in a single-stage anaerobic digestion system indicated that volatilization seems to be the major fate in both mesophilic and thermophilic conditions. The addition of a pre-digester with 3d retention time would significantly decrease the expected concentrations of all siloxanes in biogas, enhancing their removal through hydrolysis and sorption to sludge. Copyright © 2016 Elsevier Ltd. All rights reserved.

Reactivity of Silanes with ( tBuPONOP)Ruthenium Dichloride: Facile Synthesis of Chloro-Silyl Ruthenium Compounds and Formic Acid Decomposition

DOE PAGES

Anderson, Nickolas H.; Boncella, James M.; Tondreau, Aaron M.

2017-08-15

The coordination of tBuPONOP ( tBuPONOP=2,6-bis(ditert-butylphosphinito)pyridine) to different ruthenium starting materials, to generate ( tBuPONOP)RuCl 2, was investigated in this paper. The resultant ( tBuPONOP)RuCl 2 reactivity with three different silanes was then investigated and contrasted dramatically with the reactivity of ( iPrPONOP)RuCl 2(DMSO) ( iPrPONOP=2,6-bis(diisopropylphosphinito)pyridine) with the same silanes. The 16-electron species ( tBuPONOP)Ru(H)Cl was produced from the reaction of triethylsilane with ( tBuPONOP)RuCl 2. Reactions of ( tBuPONOP)RuCl 2 with both phenylsilane or diphenylsilane afforded the 16-electron hydrido-silyl species ( tBuPONOP)Ru(H)(PhSiCl 2) and ( tBuPONOP)Ru(H)(Ph 2SiCl), respectively. Reactions of all three of these complexes with silver triflate affordedmore » the simple salt metathesis products of ( tBuPONOP)Ru(H)(OTf), ( tBuPONOP)Ru(H)(PhSiCl(OTf)), and ( tBuPONOP)Ru(H)(Ph 2Si(OTf)). Formic acid dehydrogenation was performed in the presence of triethylamine (TEA), and each species proved competent for gas-pressure generation of CO 2 and H 2. Finally, the hydride species ( tBuPONOP)Ru(H)Cl, ( tBuPONOP)Ru(H)(OTf), and ( tBuPONOP)Ru(H)(PhSiCl 2) exhibited faster catalytic activity than the other compounds tested.« less

Design of C18 Organic Phases with Multiple Embedded Polar Groups for Ultraversatile Applications with Ultrahigh Selectivity.

PubMed

Mallik, Abul K; Qiu, Hongdeng; Oishi, Tomohiro; Kuwahara, Yutaka; Takafuji, Makoto; Ihara, Hirotaka

2015-07-07

For the first time, we synthesized multiple embedded polar groups (EPGs) containing linear C18 organic phases. The new materials were characterized by elemental analysis, IR spectroscopy, (1)H NMR, diffuse reflectance infrared Fourier transform (DRIFT), solid-state (13)C cross-polarization magic angle spinning (CP/MAS) NMR, suspended-state (1)H NMR, and differential scanning calorimetry (DSC). (29)Si CP/MAS NMR was carried out to investigate the degree of cross-linking of the silane and silane functionality of the modified silica. Solid-state (13)C CP/MAS NMR and suspended-state (1)H NMR spectroscopy indicated a higher alkyl chain order for the phase containing four EPGs than for the phase with three EPGs. To correlate the NMR results with temperature-dependent chromatographic studies, standard reference materials (SRM 869b and SRM 1647e), a column selectivity test mixture for liquid chromatography was employed. A single EPG containing the C18 phase was also prepared in a similar manner to be used as a reference column especially for the separation of basic and polar compounds in reversed-phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), respectively. Detailed chromatographic characterization of the new phases was performed in terms of their surface coverage, hydrophobic selectivity, shape selectivity, hydrogen bonding capacity, and ion-exchange capacity at pH 2.7 and 7.6 for RPLC as well as their hydrophilicity, the selectivity for hydrophilic-hydrophobic substituents, the selectivity for the region and configurational differences in hydrophilic substituents, the evaluation of electrostatic interactions, and the evaluation of the acidic-basic nature for HILIC-mode separation. Furthermore, peak shapes for the basic analytes propranolol and amitriptyline were studied as a function of the number of EPGs on the C18 phases in the RPLC. The chromatographic performance of multiple EPGs containing C18 HILIC phases is illustrated by the separation of sulfa drugs, β-blockers, xanthines, nucleic acid bases, nucleosides, and water-soluble vitamins. Both of the phases showed the best performance for the separation of shape-constrained isomers, nonpolar, polar, and basic compounds in RPLC- and HILIC-mode separation of sulfa drugs, and other polar and basic analytes compared to the conventional alkyl phases with and without embedded polar groups and HILIC phases. Surprisingly, one phase would be able to serve the performance of three different types of phases with very high selectivity, and we named this phase the "smart phase". Versatile applications with a single column will reduce the column purchasing cost for the analyst as well as achieve high separation, which is challenging with the commercially available columns.

Late-stage chemoselective functional-group manipulation of bioactive natural products with super-electrophilic silylium ions

NASA Astrophysics Data System (ADS)

Bender, Trandon A.; Payne, Philippa R.; Gagné, Michel R.

2018-01-01

The selective (and controllable) modification of complex molecules with disparate functional groups (for example, natural products) is a long-standing challenge that has been addressed using catalysts tuned to perform singular transformations (for example, C-H hydroxylation). A method whereby reactions with diverse functional groups within a single natural product are feasible depending on which catalyst or reagent is chosen would widen the possible structures one could obtain. Fluoroarylborane catalysts can heterolytically split Si-H bonds to yield an oxophilic silylium (R3Si+) equivalent along with a reducing (H-) equivalent. Together, these reactive intermediates enable the reduction of multiple functional groups. Exogenous phosphine Lewis bases further modify the catalyst speciation and attenuate aggressive silylium ions for the selective modification of complex natural products. Manipulation of the catalyst, silane reagent and the reaction conditions provides experimental control over which site is modified (and how). Applying this catalytic method to complex bioactive compounds (natural products or drugs) provides a powerful tool for studying structure-activity relationships.

Mechanical Property and Thermal Endurance of Room Temperature Vulcanizing Silicone Compound with Reduced Environmental Impact

NASA Astrophysics Data System (ADS)

Cho, Hiroaki; Ashida, Yasunori; Nakamura, Shuhei; Shimizu, Wataru; Murakami, Yasushi

Room temperature vulcanizing (RTV) elastic silicone usually employs organic tin compounds as a hardener. It is well known that they are strong biohazardous. Thus, European Union is going to regulate the use of organic tin compounds and to exclude them from industrial products till 2015. Authors have succeeded in making a substitute of organic tin compounds as a hardener for RTV elastic silicone by using titanium alkoxide and a carboxylate ester as a hardener and a promoter, respectively. In this paper, composites of RTV elastic silicone made with silica particles and a silane coupling agent are studied based on the mechanical, heat-resistive and adhesive properties.

Bond strength of selected composite resin-cements to zirconium-oxide ceramic

PubMed Central

Fons-Font, Antonio; Amigó-Borrás, Vicente; Granell-Ruiz, María; Busquets-Mataix, David; Panadero, Rubén A.; Solá-Ruiz, Maria F.

2013-01-01

Objectives: The aim of this study was to evaluate bond strengths of zirconium-oxide (zirconia) ceramic and a selection of different composite resin cements. Study Design: 130 Lava TM cylinders were fabricated. The cylinders were sandblasted with 80 µm aluminium oxide or silica coated with CoJet Sand. Silane, and bonding agent and/or Clearfil Ceramic Primer were applied. One hundred thirty composite cement cylinders, comprising two dual-polymerizing (Variolink II and Panavia F) and two autopolymerizing (Rely X and Multilink) resins were bonded to the ceramic samples. A shear test was conducted, followed by an optical microscopy study to identify the location and type of failure, an electron microscopy study (SEM and TEM) and statistical analysis using the Kruskal-Wallis test for more than two independent samples and Mann-Whitney for two independent samples. Given the large number of combinations, Bonferroni correction was applied (α=0.001). Results: Dual-polymerizing cements provided better adhesion values (11.7 MPa) than the autopolymerizing (7.47 MPa) (p-value M-W<0.001). The worst techniques were Lava TM + sandblasting + Silane + Rely X; Lava TM + sandblasting + Silane + Multilink and Lava TM + CoJet + silane + Multilink. Adhesive failure (separation of cement and ceramic) was produced at a lesser force than cohesive failure (fracture of cement) (p-value M-W<0.001). Electron microscopy confirmed that the surface treatments modified the zirconium-oxide ceramic, creating a more rough and retentive surface, thus providing an improved micromechanical interlocking between the cement and the ceramic. Key words:Shear bond strength, silica coating, surface treatment, zirconia ceramics, phosphate monomer. PMID:22926485

Orthogonal chemical functionalization of patterned gold on silica surfaces

PubMed Central

Léonard, Didier; Le Mogne, Thierry; Zuttion, Francesca; Chevalier, Céline; Phaner-Goutorbe, Magali; Souteyrand, Éliane

2015-01-01

Summary Single-step orthogonal chemical functionalization procedures have been developed with patterned gold on silica surfaces. Different combinations of a silane and a thiol were simultaneously deposited on a gold/silica heterogeneous substrate. The orthogonality of the functionalization (i.e., selective grafting of the thiol on the gold areas and the silane on the silica) was demonstrated by X-ray photoelectron spectroscopy (XPS) as well as time-of-flight secondary ion mass spectrometry (ToF–SIMS) mapping. The orthogonal functionalization was used to immobilize proteins onto gold nanostructures on a silica substrate, as demonstrated by atomic force microscopy (AFM). These results are especially promising in the development of future biosensors where the selective anchoring of target molecules onto nanostructured transducers (e.g., nanoplasmonic biosensors) is a major challenge. PMID:26734519

Surface functionalization of WS2 fullerene-like nanoparticles.

PubMed

Shahar, Chen; Zbaida, David; Rapoport, Lev; Cohen, Hagai; Bendikov, Tatyana; Tannous, Johny; Dassenoy, Fabrice; Tenne, Reshef

2010-03-16

WS(2) belongs to a family of layered metal dichalcogenide compounds that are known to form cylindrical (inorganic nanotubes-INT) and polyhedral nanostructures--onion or nested fullerene-like (IF) particles. The outermost layers of these IF nanoparticles can be peeled under shear stress, thus IF nanoparticles have been studied for their use as solid lubricants. However, the IF nanoparticles tend to agglomerate, presumably because of surface structural defects induced by elastic strain and curvature, a fact that has a deleterious effect on their tribological properties. In the present work, chemical modification of the IF-WS(2) surface with alkyl-silane molecules is reported. The surface-modified IF nanoparticles display improved dispersion in oil-based suspensions. The alkyl-silane coating reduces the IF-WS(2) nanoparticles' tendency to agglomerate and consequently improves the long-term tribological behavior of oil formulated with the IF additive.

New synthesis of fluorine-18-labeled 6-fluoro-L-dopa by cleaving the carbon-silicon bond with fluorine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diksic, M.; Farrokhzad, S.

A new synthesis of 3,4-dihydroxy-6-( YF)fluoro-L-phenylalanine using 6-trimethylsilyl-3,4-dimethoxy-L-dopa-ethylester as a fluorination substrate is described. The silane is prepared from the corresponding bromo compound by reacting the latter with magnesium and trimethylsilyl chloride. Reaction of the silane with ( YF)F2 in a mixture of freon-11/CCl4 (1:1) kept in a dry ice bath, subsequent hydrolysis with concentrated HBr in a bath at 140 degrees C, and simple chromatographic purification yielded YF-labeled 6-fluoro-L-dopa. A radiochemical yield of about 8% was achieved at the end of the 1-hr synthesis. The specific activity at the end of the synthesis was about 680 mCi/mmol after amore » 30-min irradiation.« less

Enhancing the protein resistance of silicone via surface-restructuring PEO-silane amphiphiles with variable PEO length

PubMed Central

Rufin, M. A.; Gruetzner, J. A.; Hurley, M. J.; Hawkins, M. L.; Raymond, E. S.; Raymond, J. E.

2015-01-01

Silicones with superior protein resistance were produced by bulk-modification with poly(ethylene oxide) (PEO)-silane amphiphiles that demonstrated a higher capacity to restructure to the surface-water interface versus conventional non-amphiphilic PEO-silanes. The PEO-silane amphiphiles were prepared with a single siloxane tether length but variable PEO segment lengths: α-(EtO)3Si(CH2)2-oligodimethylsiloxane13-block-poly(ethylene oxide)n-OCH3 (n = 3, 8, and 16). Conventional PEO-silane analogues (n = 3, 8 and 16) as well as a siloxane tether-silane (i.e. no PEO segment) were prepared as controls. When surface-grafted onto silicon wafer, PEO-silane amphiphiles produced surfaces that were more hydrophobic and thus more adherent towards fibrinogen versus the corresponding PEO-silane. However, when blended into a silicone, PEO-silane amphiphiles exhibited rapid restructuring to the surface-water interface and excellent protein resistance whereas the PEO-silanes did not. Silicones modified with PEO-silane amphiphiles of PEO segment lengths n = 8 and 16 achieved the highest protein resistance. PMID:26339488

Silane-modified surfaces in specific antibody-mediated cell recognition.

PubMed

Sterzynska, Karolina; Budna, Joanna; Frydrych-Tomczak, Emilia; Hreczycho, Grzegorz; Malinska, Agnieszka; Maciejewski, Hieronim; Zabel, Maciej

2014-01-01

The immobilization of antibodies on various surfaces has been the subject of advanced research in various immunoassay-based diagnostic devices. The physical and chemical stabilities of the immobilized antibodies on a solid surface still cause many problems because upon immobilizing antibody molecules, the antigen-binding ability usually decreases. The silanization of surfaces with organosilanes carrying chemically active groups such as (3-aminopropyl) triethoxysilane (APTES) can accommodate these antigen-binding molecules in an appropriate orientation so that their functionality and binding activity are essentially retained. In this study, n-butyltrimethoxysilane (BMS) and 3-(octafluoropentyloxy)-propyltriethoxysilane (OFPOS) were used as "blocking silanes". The aims of this study were to compare the effectiveness of specific antibody binding of APTES, APTES + BMS and APTES + OFPOS and to characterize the modified surfaces by contact angle measurements and immunofluorescence measurements prior to and after immobilizing proteins. Additionally, we have evaluated the functionality of the immobilized antibodies by their abilities to bind EpCAM-positive human colon adenocarcinoma cell line (LoVo) and EpCAM-negative mouse embryonic fibroblast cell line (3T3). Cell enumeration was conducted on the basis of DAPI-positive signals and recorded using a confocal laser scanning biological microscope. The results of our study showed that the immobilization capability and reactivity of APTES, APTES + BMS and APTES + OFPOS differ. The modification of APTES with unreactive silanes (BMS,OFPOS) is recommended to improve the antibody binding efficiency. However, using OFPOS resulted in more effective antibody and cell binding, and it appears to be the most useful compound in specific antibody-mediated cell recognition.

Development and design of nanomaterial reagents in conjunction with new methods for their synthetic applications

NASA Astrophysics Data System (ADS)

Kwaramba, Farai Brian

This Ph.D. deals with the integration of nanotechnology with organometallic/ organic synthetic technologies. The first part of this research sought to develop a library of novel molecular gears programmed to exploit photo-switching and electrostatic repulsion to control the molecular rotation of covalently linked triptypyrazines. Incorporation of these two modes allows for control of triptycene based gear systems using unexplored external methods. The triptypyrazine was an attractive scaffold because of its intrinsic pH and electrochemical activity, thus providing a novel construct for controlling molecular motion. This design finds relevance in the fabrication of nano-electromechanical devices and understanding controlled molecular motion. This Ph.D. also sought to address the need to generate and recycle low cost hydrosilylation catalysts. Metal nanoparticle catalysts can potentially meet this need due to their high surface area and reactivity. Their morphology and surface texture provide avenues for selectivity in reactions. Metal-nanoparticles on a silicon matrix can be formed by reducing metal salts with silicon hydrides. Investigations towards iron-nanoparticle catalyzed hydrosilylation of unsaturated bonds were conducted. Furthermore, this research sought to develop highly functionalized silanes, as guiding scaffolds for generating chiral silicon hydrides. Fabrication of metal-nanoparticle catalysts with the same, could install surface definition on these heterogeneous green catalysts, thus allowing selectivity in their catalysis. A bottom up approach to nanofabrication, started with the generation of a library of highly functionalized alkynyl-silane building blocks using the hydrosilylation reaction. Hydrosilylation of carbon-carbon and carbon-heteroatom unsaturated bonds has proven to be an important reaction in organic syntheses. Additionally, silicon tethers have been utilized in complex organic syntheses as a way to increase reaction rates, and selectivity. The most commonly employed silicon tethers have been disiloxanes followed by siloxanes, then silanes. Of these methods the synthesis and utilization of tethered silyl-alkynes was limited. To address this gap, this work developed methodology to prepare tethered silyl alkynes through a hydrosilylation reaction. It was established that [IrCl(COD)]2 in the presence of excess COD can selectively catalyze the hydrosilylation of alkenes with alkynyl-silanes. This approach overrides traditional hydrosilylation catalysts' reactivity trends.

Durable low surface-energy surfaces

NASA Technical Reports Server (NTRS)

Willis, Paul B. (Inventor); McElroy, Paul M. (Inventor); Hickey, Gregory H. (Inventor)

1993-01-01

A formulation for forming a low surface-energy surface on a substrate having (i) a fluoroalkyl silane having a low surface energy part, (ii) a liquid crystal silane operable for enhancing the orientation of the molecules of the fluoroalkyl silane and for crosslinking with the fluoroalkyl silane, and, (iii) a transport medium for applying the fluoroalkyl silane and the liquid crystal silane to the surface of a substrate. In one embodiment the formulation can includes a crosslinking agent for crosslinking the fluoroalkyl silane. In another embodiment the formulation has a condensation catalyst for enhancing chemical bonding of the fluoroalkyl silane to the substrate. The transport medium can be an alcohol such as methanol or ethanol.

Hydrogenation of biomass-derived substrates

DOEpatents

Gordon, John C.; Waidmann, Christopher R.

2016-06-07

The .alpha.,.beta.-unsaturated ketone moiety of a substrate representative of non-food based biomass was hydrogenated to the corresponding saturated alcohol moiety using a composition including (1) a copper salt; (2) a phosphine; (3) a polar aprotic solvent such as acetonitrile, and (4) a compound suitable for providing hydrogen for the hydrogenation, such as a suitable silane material or a suitable siloxane material.

Effects of silane on the properties of wood-plastic composites with polyethylene-polypropylene blends as matrices

Treesearch

Craig M. Clemons; Ronald C. Sabo; Michael L. Kaland; Kolby C. Hirth

2011-01-01

The influence of 3-(trimethoxysilyl)propyl methacrylate and benzoyl peroxide on gel content, crystallinity, and mechanical performance of unfilled PP-PE blends, and their composites with wood was investigated. All materials were compounded in a twin screw extruder and then injection molded. Specimens were then exposed to high-humidity and elevated temperature in a...

Influence of the silane modifiers on the surface thermodynamic characteristics and dispersion of the silica into elastomer compounds.

PubMed

Castellano, Maila; Conzatti, Lucia; Turturro, Antonio; Costa, Giovanna; Busca, Guido

2007-05-03

A good dispersion of silica into elastomers, typically used in tire tread production, is obtained by grafting of the silica with multifunctional organosilanes. In this study, the influence of the chemical structure of a triethoxysilane (TES), octadecyltriethoxysilane (ODTES), and ODTES/bistriethoxysilylpropyltetrasulfane (TESPT) mixture was investigated by inverse gas chromatography (IGC) at infinite dilution. Thermodynamic results indicate a higher polarity of the silica surface modified with TES as compared to that of the unmodified silica due to new OH groups deriving from the hydrolysis of ethoxy groups of the silane; the long hydrocarbon substituent of the ODTES lies on the surface of silica and reduces the dispersive component of the silica surface tension. A comparison with silica modified with TESPT is discussed. An accurate morphological investigation by transmission electron microscopy (TEM) and automated image analysis (AIA) was carried out on aggregates of silica dispersed into a SBR compound loaded with 35 phr (per hundred rubber) of untreated and TESPT-treated silica. Morphological descriptors such as the projected area/perimeter ratio (A/P) and roundness (P2/4piA) provided direct and quantitative indications about the distribution of the filler into the rubber matrix.

Synthesis and Characterization of Potassium Aryl- and Alkyl-Substituted Silylchalcogenolate Salts

DOE PAGES

Brown, Jessica Lynn; Montgomery, Ashley C.; Samaan, Christopher A.; ...

2016-02-23

Treatment of either triphenyl(chloro)silane or tert-butyldiphenyl(chloro)silane with potassium metal in THF, followed by addition of 18-crown-6, affords [K(18-crown-6)][SiPh 3] (1) and [K(18-crown-6)][SiPh 2 tBu] (2), respectively, as the reaction products in high yield. Compounds 1 and 2 were fully characterized including by multi-nuclear NMR and IR spectroscopies. Addition of elemental chalcogen to either 1 or 2, results in facile chalcogen insertion into the potassium-silicon bond to afford the silylchalcogenolates, [K(18-crown-6)][E– SiPh2R] (E = S, R = Ph (3); Se, R = Ph (4); E = Te, R = Ph (5); E = S, R = tBu (6); E = Se,more » R = tBu (7); E = Te, R = tBu (8)), in moderate to good yield. The silylchalcogenolates reported herein were characterized by multi-nuclear NMR and IR spectroscopies, and their solid-state molecular structures were determined by single-crystal X-ray crystallography. Importantly, the reported compounds crystallize as discrete monomers in the solid-state, a structural feature not previously observed in silylchalcogenolates, providing well-defined access routes into systematic metal complexation studies.« less

Influence of surface conditions and silane agent on the bond of resin to IPS Empress 2 ceramic.

PubMed

Spohr, Ana Maria; Sobrinho, Lourenço Correr; Consani, Simonides; Sinhoreti, Mario Alexandre Coelho; Knowles, Jonathan C

2003-01-01

The aim of this study was to evaluate the effect of different ceramic surface treatments on the tensile bond strength between IPS Empress 2 ceramic framework and Rely X adhesive resin cement, with or without the application of a silane coupling agent. One hundred twenty disks were made, embedded in resin, and randomly divided into six groups: group 1 = sandblasting (100 microm), no silanation; group 2 = sandblasting (100 microm), silane treatment; group 3 = sandblasting (50 microm), no silanation; group 4 = sandblasting (50 microm), silane treatment; group 5 = hydrofluoric acid etching, no silanation; and group 6 = hydrofluoric acid etching, silane treatment. The disks were bonded into pairs with adhesive resin cement. All samples were stored in distilled water at 37 degrees C for 24 hours and then thermocycled. The samples were submitted to tensile testing. The use of silane improved the bond strength in relation to the groups in which silane was not applied (P < .05). The most effective surface treatment was etching with 10% hydrofluoric acid, both with (25.6 MPa) and without silane application (16.4 MPa); these values showed a statistically significant difference compared to sandblasting with 50- and 100-microm Al2O3. Sandblasting with 50-microm Al2O3, with (11.8 MPa) and without silane (5.4 MPa), demonstrated significantly higher tensile bond strength than sandblasting with 100-microm Al2O3, with (8.3 MPa) and without silane (3.8 MPa). Combined application of 10% hydrofluoric acid and silane enhanced the bond strength between the IPS Empress 2 ceramic framework and resin agent.

Formation mechanism of a silane-PVA/PVAc complex film on a glass fiber surface.

PubMed

Repovsky, Daniel; Jane, Eduard; Palszegi, Tibor; Slobodnik, Marek; Velic, Dusan

2013-10-21

Mechanical properties of glass fiber reinforced composite materials are affected by fiber sizing. A complex film formation, based on a silane film and PVA/PVAc (polyvinyl alcohol/polyvinyl acetate) microspheres on a glass fiber surface is determined at 1) the nanoscale by using atomic force microscopy (AFM), and 2) the macroscale by using the zeta potential. Silane groups strongly bind through the Si-O-Si bond to the glass surface, which provides the attachment mechanism as a coupling agent. The silane groups form islands, a homogeneous film, as well as empty sites. The average roughness of the silanized surface is 6.5 nm, whereas it is only 0.6 nm for the non-silanized surface. The silane film vertically penetrates in a honeycomb fashion from the glass surface through the deposited PVA/PVAc microspheres to form a hexagonal close pack structure. The silane film not only penetrates, but also deforms the PVA/PVAc microspheres from the spherical shape in a dispersion to a ellipsoidal shape on the surface with average dimensions of 300/600 nm. The surface area value Sa represents an area of PVA/PVAc microspheres that are not affected by the silane penetration. The areas are found to be 0.2, 0.08, and 0.03 μm(2) if the ellipsoid sizes are 320/570, 300/610, and 270/620 nm for silane concentrations of 0, 3.8, and 7.2 μg mL(-1), respectively. The silane film also moves PVA/PVAc microspheres in the process of complex film formation, from the low silane concentration areas to the complex film area providing enough silane groups to stabilize the structure. The values for the residual silane honeycomb structure heights (Ha ) are 6.5, 7, and 12 nm for silane concentrations of 3.8, 7.2, and 14.3 μg mL(-1), respectively. The pH-dependent zeta-potential results suggest a specific role of the silane groups with effects on the glass fiber surface and also on the PVA/PVAc microspheres. The non-silanized glass fiber surface and the silane film have similar zeta potentials ranging from -64 to -12 mV at pH's of 10.5 and 3, respectively. The zeta potentials for the PVA/PVAc microspheres on the glass fiber surface and within the silane film significantly decrease and range from -25 to -5 mV. The shapes of the pH-dependent zeta potentials are different in the cases of silane groups over a pH range from 7 to 4. A triple-layer model is used to fit the non-silanized glass surface and the silane film. The value of the surface-site density for Γ(Xglass) and Γ(Xsilane), in which X denotes the Al-O-Si group, differs by a factor of 10(-4), which suggests an effective coupling of the silane film. A soft-layer model is used to fit the silane-PVA/PVAc complex film, which is approximated as four layers. Such a simplification and compensation of the microsphere shape gives an approximation of the relevant widths of the layers as the follows: 1) the layer of the silane groups makes up 10% of the total length (27 nm), 2) the layer of the first PVA shell contributes 30% to the total length (81 nm), 3) the layer of the PVAc core contributes 30% to the total length (81 nm), and finally 4) the layer of the second PVA shell provides 30% of the total length (81 nm). The coverage simulation resulted in a value of 0.4, which corresponds with the assumption of low-order coverage, and is supported by the AFM scans. Correlating the results of the AFM scans, and the zeta potentials sheds some light on the formation mechanism of the silane-PVA/PVAc complex film. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quaternary ammonium silane-functionalized, methacrylate resin composition with antimicrobial activities and self-repair potential

PubMed Central

Gong, Shi-qiang; Niu, Li-na; Kemp, Lisa K.; Yiu, Cynthia K.Y.; Ryou, Heonjune; Qi, Yi-pin; Blizzard, John D.; Nikonov, Sergey; Brackett, Martha G.; Messer, Regina L.W.; Wu, Christine D.; Mao, Jing; Brister, L. Bryan; Rueggeberg, Frederick A.; Arola, Dwayne D.; Pashley, David H.; Tay, Franklin R.

2012-01-01

Design of antimicrobial polymers for enhancing healthcare issues and minimizing environmental problems is an important endeavor with both fundamental and practical implications. Quaternary ammonium silane-functionalized methacrylate (QAMS) represents an example of antimicrobial macromonomers synthesized by a sol-gel chemical route; these compounds possess flexible Si-O-Si bonds. In present work, a partially-hydrolyzed QAMS copolymerized with bis-GMA is introduced. This methacrylate resin was shown to possess desirable mechanical properties with both a high degree of conversion and minimal polymerization shrinkage. Kill-on-contact microbiocidal activities of this resin were demonstrated using single-species biofilms of Streptococcus mutans (ATCC 36558), Actinomyces naeslundii (ATCC 12104) and Candida albicans (ATCC 90028). Improved mechanical properties after hydration provided the proof-of-concept that QAMS-incorporated resin exhibits self-repair potential via water-induced condensation of organic modified silicate (ormosil) phases within the polymerized resin matrix. PMID:22659173

[Chemical constituents of Rauvolfia verticillata].

PubMed

Hong, Bo; Li, Wen-Jing; Zhao, Chun-Jie

2012-06-01

The study on the Rauvolfia verticillata (Lour.) Baill., which belongs to Apocynaceae, was carried out to look for its chemical constituents and pharmacological activity. The isolation and purification were performed by chromatography on silica gel, Sephadex LH-20 and ODS (octadecyl silane) open column. The structures of obtained compounds were elucidated on the basis of physicochemical properties and spectral analysis. Three indole alkaloids and one acridone alkaloid were isolated from chloroform layer extract and identified as ajmalicine B (1), sandwicine (2), raunescine (3) and 7-hydroxynoracronycine (4) separately. Ajmalicine B (1) is a new compound belonging to indole alkaloid. Compound 4 as an acridone alkaloid was a new type compound isolated from Rauvolfia genus for the first time. We also did some biological activity research on the new type compound (4) to explore other pharmacological activities in addition to antihypertensive activity.

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

NASA Astrophysics Data System (ADS)

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.

Comparison of detailed and reduced kinetics mechanisms of silane oxidation in the basis of detonation wave structure problem

NASA Astrophysics Data System (ADS)

Fedorov, A. V.; Tropin, D. A.; Fomin, P. A.

2018-03-01

The paper deals with the problem of the structure of detonation waves in the silane-air mixture within the framework of mathematical model of a nonequilibrium gas dynamics. Detailed kinetic scheme of silane oxidation as well as the newly developed reduced kinetic model of detonation combustion of silane are used. On its basis the detonation wave (DW) structure in stoichiometric silane - air mixture and dependences of Chapman-Jouguet parameters of mixture on stoichiometric ratio between the fuel (silane) and an oxidizer (air) were obtained.

Organometallic complexes of bulky, optically active, C 3-symmetric tris(4 S-isopropyl-5,5-dimethyl-2-oxazolinyl)phenylborate (To P*)

DOE PAGES

Xu, Songchen; Magoon, Yitzhak; Reinig, Regina R.; ...

2015-07-16

A bulky, optically active monoanionic scorpionate ligand, tris(4S-isopropyl-5,5-dimethyl-2-oxazolinyl)phenylborate (To P*), is synthesized from the naturally occurring amino acid l-valine as its lithium salt, Li[To P*] (1). That compound is readily converted to the thallium complex Tl[To P*] (2) and to the acid derivative H[To P*] (3). Group 7 tricarbonyl complexes To P*M(CO) 3 (M = Mn (4), Re (5)) are synthesized by the reaction of MBr(CO) 5 and Li[To P*] and are crystallographically characterized. The ν CO bands in their infrared spectra indicate that π back-donation in the rhenium compounds is greater with To P* than with non-methylated tris(4S-isopropyl-2-oxazolinyl)phenylborate (Tomore » P). The reaction of H[To P*] and ZnEt 2 gives To P*ZnEt (6), while To P*ZnCl (7) is synthesized from Li[To P*] and ZnCl 2. The reaction of To P*ZnCl and KOtBu followed by addition of PhSiH 3 provides the zinc hydride complex To P*ZnH (8). In this study, compound 8 is the first example of a crystallographically characterized optically active zinc hydride. We tested its catalytic reactivity in the cross-dehydrocoupling of silanes and alcohols, which provided Si-chiral silanes with moderate enantioselectivity.« less

Organometallic complexes of bulky, optically active, C 3-symmetric tris(4 S-isopropyl-5,5-dimethyl-2-oxazolinyl)phenylborate (To P*)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Songchen; Magoon, Yitzhak; Reinig, Regina R.

A bulky, optically active monoanionic scorpionate ligand, tris(4S-isopropyl-5,5-dimethyl-2-oxazolinyl)phenylborate (To P*), is synthesized from the naturally occurring amino acid l-valine as its lithium salt, Li[To P*] (1). That compound is readily converted to the thallium complex Tl[To P*] (2) and to the acid derivative H[To P*] (3). Group 7 tricarbonyl complexes To P*M(CO) 3 (M = Mn (4), Re (5)) are synthesized by the reaction of MBr(CO) 5 and Li[To P*] and are crystallographically characterized. The ν CO bands in their infrared spectra indicate that π back-donation in the rhenium compounds is greater with To P* than with non-methylated tris(4S-isopropyl-2-oxazolinyl)phenylborate (Tomore » P). The reaction of H[To P*] and ZnEt 2 gives To P*ZnEt (6), while To P*ZnCl (7) is synthesized from Li[To P*] and ZnCl 2. The reaction of To P*ZnCl and KOtBu followed by addition of PhSiH 3 provides the zinc hydride complex To P*ZnH (8). In this study, compound 8 is the first example of a crystallographically characterized optically active zinc hydride. We tested its catalytic reactivity in the cross-dehydrocoupling of silanes and alcohols, which provided Si-chiral silanes with moderate enantioselectivity.« less

Polyfibroblast: A Self-Healing and Galvanic Protection Additive

DTIC Science & Technology

2011-07-25

3 Key Accomplishments 3.1 Silane Formulation Processability Silane coupling agents may be added to the existing microcapsules either in low...constrained by the need to form stable microcapsules . To this end, we explored a number of recipes in which the following silane coupling agents were...Isocyanatopropyltrimethoxy silane (ITS). • Glycidoxypropyltrimethoxy silane (GPS) As expected, the lowest concentrations most readily formed stable microcapsules . The

Safety assessment of nanoparamagnetic contrast agents with different coatings for molecular MRI

NASA Astrophysics Data System (ADS)

Azizian, Gholamreza; Riyahi-Alam, Nader; Haghgoo, Soheila; Saffari, Mojtaba; Zohdiaghdam, Reza; Gorji, Ensieh

2013-04-01

Despite the wide application of gadolinium as a contrast agent for magnetic resonance imaging (MRI), there is a serious lack of information on its toxicity. Gadolinium and gadolinium oxide (Gd-oxide) are used as contrast agents for magnetic resonance imaging (MRI). There are methods for reducing toxicity of these materials, such as core nanoparticles coating or conjugating. Therefore, for toxicity evaluation, we compared the viability of commercial contrast agents in MRI (Gd-DTPA) and three nanoparticles with the same core Gd2O3 and small particulate gadolinium oxide or SPGO (< 40 nm) but different coatings of diethyleneglycol (DEG) as Gd2O3-DEG and methoxy polyethylene glycol-silane (mPEG-silane: 550 and 2000 Dalton) as SPGO-mPEG-silane550 and SPGO-mPEG-silane2000, respectively, in the SK-MEL3 cell line, by light microscopy, MTT assay using 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide, and the LDH assay detecting lactate dehydrogenase activity. The viability values were not statistically different between the three nanoparticles and Gd-DTPA. The MTT and LDH assay results showed that Gd2O3-DEG nanoparticles were more toxic than Gd-DTPA and other nanoparticles. Also, SPGO-mPEG-silane2000 was more biocompatible than other nanoparticles. The obtained results did not show any significant increase in cytotoxicity of the nanoparticles and Gd-DTPA, neither dose-dependent nor time-dependent. Therefore, DEG and PEG, due to their considerable properties and irregular sizes (different molecular weights), were selected as the useful surface covering materials of nanomagnetic particles that could reveal noticeable relaxivity and biocompatibility characteristics.

Characterization of a hybrid-smectite nanomaterial formed by immobilizing of N-pyridin-2-ylmethylsuccinamic acid onto (3-aminopropyl)triethoxysilane modified smectite and its potentiometric sensor application

NASA Astrophysics Data System (ADS)

Topcu, Cihan; Caglar, Sema; Caglar, Bulent; Coldur, Fatih; Cubuk, Osman; Sarp, Gokhan; Gedik, Kubra; Bozkurt Cirak, Burcu; Tabak, Ahmet

2016-09-01

A novel N-pyridin-2-ylmethylsuccinamic acid-functionalized smectite nanomaterial was synthesized by immobilizing of N-pyridin-2-ylmethylsuccinamic acid through chemical bonding onto (3-aminopropyl)triethoxysilane modified smectite. The structural, thermal, morphological and surface properties of raw, silane-grafted and the N-pyridin-2-ylmethylsuccinamic acid-functionalized smectites were investigated by various characterization techniques. The thermal analysis data showed the presence of peaks in the temperature range from 200 °C to 600 °C due to the presence of physically adsorbed silanes, intercalated silanes, surface grafted silanes and chemically grafted silane molecules between the smectite layers. The powder x-ray diffraction patterns clearly indicated that the aminopropyl molecules also intercalated into the smectite interlayers as bilayer arrangement whereas N-pyridin-2-ylmethylsuccinamic acid molecules were only attached to 3-aminopropyltriethoxysilane molecules on the external surface and edges of clay and they did not intercalate. Fourier transform infrared spectroscopy confirms N-pyridin-2-ylmethylsuccinamic acid molecules bonding through the amide bond between the amine group of aminopropyltriethoxysilane molecules and a carboxylic acid functional group of N-pyridin-2-ylmethylsuccinamic acid molecules. The guest molecules functionalized onto the smectite caused significant alterations in the textural and morphological parameters of the raw smectite. The anchoring of N-pyridin-2-ylmethylsuccinamic acid molecules led to positive electrophoretic mobility values when compared to starting materials. N-pyridin-2-ylmethylsuccinamic acid-functionalized smectite was employed as an electroactive ingredient in the structure of potentiometric PVC-membrane sensor. The sensor exhibited more selective potentiometric response towards chlorate ions compared to the other common anionic species.

Fluorination of Boron-Doped Diamond Film Electrodes for Minimization of Perchlorate Formation.

PubMed

Gayen, Pralay; Chaplin, Brian P

2017-08-23

This research investigated the effects of surface fluorination on both rates of organic compound oxidation (phenol and terephthalic acid (TA)) and ClO 4 - formation at boron-doped diamond (BDD) film anodes at 22 °C. Different fluorination methods (i.e., electrochemical oxidation with perfluorooctanoic acid (PFOA), radio frequency plasma, and silanization) were used to incorporate fluorinated moieties on the BDD surface, which was confirmed by X-ray photoelectron spectroscopy (XPS). The silanization method was found to be the most effective fluorination method using a 1H,1H,2H,2H-perfluorodecyltrichlorosilane precursor to form a self-assembled monolayer (SAM) on the oxygenated BDD surface. The ClO 4 - formation decreased from rates of 0.45 ± 0.03 mmol m -2 min -1 during 1 mM NaClO 3 oxidation and 0.28 ± 0.01 mmol m -2 min -1 during 10 mM NaCl oxidation on the BDD electrode to below detectable levels (<0.12 μmoles m -2 min -1 ) for the BDD electrode functionalized by a 1H,1H,2H,2H-perfluorodecyltrichlorosilane SAM. These decreases in rates corresponded to 99.94 and 99.85% decreases in selectivity for ClO 4 - formation during the electrolysis of 10 mM NaCl and 1 mM NaClO 3 electrolytes, respectively. By contrast, the oxidation rates of phenol were reduced by only 16.3% in the NaCl electrolyte and 61% in a nonreactive 0.1 M KH 2 PO 4 electrolyte. Cyclic voltammetry with Fe(CN) 6 3-/4- and Fe 3+/2+ redox couples indicated that the long fluorinated chains created a blocking layer on the BDD surface that inhibited charge transfer via steric hindrance and hydrophobic effects. The surface coverages and thicknesses of the fluorinated films controlled the charge transfer rates, which was confirmed by estimates of film thicknesses using XPS and density functional theory simulations. The aliphatic silanized electrode also showed very high stability during OH • production. Perchlorate formation rates were below the detection limit (<0.12 μmoles m -2 min -1 ) for up to 10 consecutive NaClO 3 oxidation experiments.

Measuring Trace Hydrocarbons in Silanes

NASA Technical Reports Server (NTRS)

Lesser, L. A.

1984-01-01

Technique rapid and uses standard analytical equipment. Silane gas containing traces of hydrocarbons injected into carrier gas of moist nitrogen having about 0.2 percent water vapor. Carrier, water and silane pass through short column packed with powdered sodium hydroxide which combines moisture and silane to form nonvolatile sodium silicate. Carrier gas free of silane but containing nonreactive hydrocarbons, pass to silica-gel column where chromatographic separation takes place. Hydrocarbons measured by FID.

Mechanistic Study of Nickel-Catalyzed Ynal Reductive Cyclizations Through Kinetic Analysis

PubMed Central

Baxter, Ryan D.; Montgomery, John

2011-01-01

The mechanism of nickel-catalyzed, silane-mediated reductive cyclization of ynals has been evaluated. The cyclizations are first-order in [Ni] and [ynal] and zeroth-order in [silane]. These results, in combination with the lack of rapid silane consumption upon reaction initiation are inconsistent with mechanisms involving reaction initiation by oxidative addition of Ni(0) to the silane. Silane consumption occurs only when both the alkyne and aldehyde and are present. Mechanisms involving rate-determining oxidative cyclization to a metallacycle followed by rapid reaction with the silane are consistent with the data obtained. PMID:21438642

Fast and Selective Preconcentration of Europium from Wastewater and Coal Soil by Graphene Oxide/Silane@Fe3O4 Dendritic Nanostructure.

PubMed

Patra, Santanu; Roy, Ekta; Madhuri, Rashmi; Sharma, Prashant K

2015-05-19

In this study, nanocomposite of graphene oxide and silane modified magnetic nanoparticles (silane@Fe3O4) were synthesized in a form of dendritic structure. For this, silane@Fe3O4 nanoparticle gets sandwiched between two layers of graphene oxide by chemical synthesis route. The synthesized dendritic structure was used as a monomer for synthesis of europium ion imprinted polymer. The synthesis of imprinted polymer was contemplated onto the surface of the vinyl group modified silica fiber by activated generated free radical atom-transfer radical polymerization, that is, AGET-ATRP technique. The synthesized dendritic monomer was characterized by XRD, FT-IR, VSM, FE-SEM, and TEM analyses. The imprinted polymer modified silica fiber was first validated in the aqueous and blood samples for successful extraction and detection of europium ion with limit of detection = 0.050 pg mL(-1) (signal/noise = 3). The imprinted polymer modified silica fiber was also used for preconcentration and separation of europium metal ion from various soil samples of coal mine areas. However, the same silica fiber was also used for wastewater treatment and shows 100% performance for europium removal. The findings herein suggested that dendritic nanocomposite could be potentially used as a highly effective material for the enrichment and preconcentration of europium or other trivalent lanthanides/actinides in nuclear waste management.

Effect of silane pretreatment on the immediate bonding of universal adhesives to computer-aided design/computer-aided manufacturing lithium disilicate glass ceramics.

PubMed

Yao, Chenmin; Zhou, Liqun; Yang, Hongye; Wang, Yake; Sun, Hualing; Guo, Jingmei; Huang, Cui

2017-04-01

The aim of this study was to investigate the effect of silane pretreatment on the universal adhesive bonding between lithium disilicate glass ceramic and composite resin. IPS e.max ceramic blocks etched with hydrofluoric acid were randomly assigned to one of eight groups treated with one of four universal adhesives (two silane-free adhesives and two silane-containing adhesives), each with or without silane pretreatment. Bonded specimens were stored in water for 24 h. The shear bond strength (SBS) of the ceramic-resin interface was measured to evaluate bond strength, and the debonded interface after the SBS test was analysed using field-emission scanning electron microscopy to determine failure mode. Light microscopy was performed to analyse microleakage and marginal sealing ability. Silane pretreatment significantly and positively influenced SBS and marginal sealing ability. For all the universal adhesive groups, SBS increased and the percentage of microleakage decreased after the pretreatment. Without the pretreatment, SBS and the percentage of microleakage were not significantly different between the silane-containing universal adhesive groups and the silane-free groups. Cohesive failure was the main fracture pattern. The results suggest that additional silane pretreatment can effectively improve the bonding strength and marginal sealing of adhesives to lithium disilicate glass ceramics. The bonding performance of silane-containing universal adhesives without pretreatment is similar to that of silane-free adhesives. © 2017 Eur J Oral Sci.

Digital One-Disc-One-Compound Method for High-Throughput Discovery of Prostate Cancer - Targeting Ligands

DTIC Science & Technology

2015-10-01

shown in Fig. 1a, the prepolymer mixture was sandwiched between photo mask and glass slide. Microdiscs were fabricated on the glass substrate through...polymerization of the prepolymer mixture and the acrylated silane under UV exposure. To achieve the more stable microdiscs for peptide synthesis, the...composition of prepolymer mixture was changed to PEG (Polyethylene Glycol)-diacrylate, crosslinker, photo initiator, 2-aminoethylmethacrylate, water

Improved method for mutagenicity testing of gaseous compounds by using a gas sampling bag.

PubMed

Araki, A; Noguchi, T; Kato, F; Matsushima, T

1994-05-01

A simple and safety gas exposure method was developed using a gas sampling bag as an exposure vessel and a preparation vessel of diluted gas. The gas exposure conditions such as amount of S9 in the plate, volume of gas for the plate, amount of top agar, exposure period and exposure temperature were examined by mutagenicity testing of 1,3-butadiene using the gas sampling bag. Mutagenicity tests of 14 compounds and 1,3-butadiene on S. typhimurium TA98, TA100, TA1535 and TA1537, and E. coli WP2 uvrA were also examined by the developed gas exposure method. 1,3-Butadiene, propyne (methyl acetylene), monochlorodifluoromethane, ethylchloride, diborane and silane were mutagenic. 1-Butene, 2-butene, 2-methylpropene, methyl vinyl ether, trichlorofluoromethane, dichlorodifluoromethane, 1,2-dichloro-1,1,2,2-tetrafluoroethane, 1,1-difluoroethane and phosphine were not mutagenic on S. typhimurium TA98, TA100, TA1535 and TA1537, and E. coli WP2 uvrA with or without metabolic activation. These results were compatible with a previous report, and this developed method has the advantage that it can be tested easily and safely for combustible and self-combustible substances such as 1,3-butadiene and silane.

Elusive silane-alane complex [Si-H⋅⋅⋅Al]: isolation, characterization, and multifaceted frustrated Lewis pair type catalysis.

PubMed

Chen, Jiawei; Chen, Eugene Y-X

2015-06-01

The super acidity of the unsolvated Al(C6F5)3 enabled isolation of the elusive silane-alane complex [Si-H⋅⋅⋅Al], which was structurally characterized by spectroscopic and X-ray diffraction methods. The Janus-like nature of this adduct, coupled with strong silane activation, effects multifaceted frustrated-Lewis-pair-type catalysis. When compared with the silane-borane system, the silane-alane system offers unique features or clear advantages in the four types of catalytic transformations examined in this study, including: ligand redistribution of tertiary silanes into secondary and quaternary silanes, polymerization of conjugated polar alkenes, hydrosilylation of unactivated alkenes, and hydrodefluorination of fluoroalkanes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Efficient and Selective N-Methylation of Nitroarenes under Mild Reaction Conditions.

PubMed

Pedrajas, Elena; Sorribes, Iván; Guillamón, Eva; Junge, Kathrin; Beller, Matthias; Llusar, Rosa

2017-09-21

Herein, we report a straightforward protocol for the preparation of N,N-dimethylated amines from readily available nitro starting materials using formic acid as a renewable C 1 source and silanes as reducing agents. This tandem process is efficiently accomplished in the presence of a cubane-type Mo 3 PtS 4 catalyst. For the preparation of the novel [Mo 3 Pt(PPh 3 )S 4 Cl 3 (dmen) 3 ] + (3 + ) (dmen: N,N'-dimethylethylenediamine) compound we have followed a [3+1] building block strategy starting from the trinuclear [Mo 3 S 4 Cl 3 (dmen) 3 ] + (1 + ) and Pt(PPh 3 ) 4 (2) complexes. The heterobimetallic 3 + cation preserves the main structural features of its 1 + cluster precursor. Interestingly, this catalytic protocol operates at room temperature with high chemoselectivity when the 3 + catalyst co-exists with its trinuclear 1 + precursor. N-heterocyclic arenes, double bonds, ketones, cyanides and ester functional groups are well retained after N-methylation of the corresponding functionalized nitroarenes. In addition, benzylic-type as well as aliphatic nitro compounds can also be methylated following this protocol. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reactor for fluidized bed silane decomposition

NASA Technical Reports Server (NTRS)

Iya, Sridhar K. (Inventor)

1989-01-01

An improved heated fluidized bed reactor and method for the production of high purity polycrystalline silicon by silane pyrolysis wherein silicon seed particles are heated in an upper heating zone of the reactor and admixed with particles in a lower zone, in which zone a silane-containing gas stream, having passed through a lower cooled gas distribution zone not conducive to silane pyrolysis, contacts the heated seed particles whereon the silane is heterogeneously reduced to silicon.

Corrosion Protection of Nd-Fe Magnets via Phophatization, Silanization and Electrostatic Spraying with Organic Resin Composite Coatings

NASA Astrophysics Data System (ADS)

Ding, Xia; Li, Jingjie; Li, Musen; Ge, Shengsong; Wang, Xiuchun; Ding, Kaihong; Cui, Shengli; Sun, Yongcong

2014-09-01

Nd-Fe-B permanent magnets possess excellent properties. However, they are highly sensitive to the attack of corrosive environment. The aim of this work is to improve the corrosion resistance of the magnets by phosphatization, silanization, and electrostatic spraying with organic resin composite coatings. Field emission scanning electron microscope (FE-SEM) and energy dispersive spectrometer (EDS) tests showed that uniform phosphate conversion coatings and spray layers were formed on the surface of the Nd-Fe-B magnets. Neutral salt spray tests exhibited that, after treated by either phosphating, silanization or electrostatic spraying, the protectiveness of Nd-Fe-B alloys was apparently increased. And corrosion performance of magnets treated with silane only was slightly inferior to those of phosphatized ones. However, significant improvement in corrosion protection was achieved after two-step treatments, i.e. by top-coating spray layer with phosphate or silane films underneath. Grid test indicated that the phosphate and silane coating were strongly attached to the substrate while silane film was slightly weaker than the phosphate-treated ones. Magnetic property analysis revealed phosphatization, silanization, and electrostatic spraying caused decrease in magnetism, but silanization had the relatively smaller effect.

Zone heating for fluidized bed silane pyrolysis

NASA Technical Reports Server (NTRS)

Iya, Sridhar K. (Inventor)

1987-01-01

An improved heated fluidized bed reactor and method for the production of high purity polycrystalline silicon by silane pyrolysis wherein silicon seed particles are heated in an upper heating zone of the reactor and admixed with particles in a lower reaction zone, in which zone a silane-containing gas stream, having passed through a lower cooled gas distribution zone not conducive to silane pyrolysis, contacts the heated seed particles whereon the silane is heterogeneously reduced to silicon.

Surface characterization and cytocompatibility evaluation of silanized magnesium alloy AZ91 for biomedical applications

PubMed Central

Witecka, Agnieszka; Yamamoto, Akiko; Dybiec, Henryk; Swieszkowski, Wojciech

2012-01-01

Mg alloys with high Al contents have superior corrosion resistance in aqueous environments, but poor cytocompatibility compared to that of pure Mg. We have silanized the cast AZ91 alloy to improve its cytocompatibility using five different silanes: ethyltriethoxysilane (S1), 3-aminopropyltriethoxysilane (S2), 3-isocyanatopyltriethoxysilane (S3), phenyltriethoxysilane (S4) and octadecyltriethoxysilane (S5). The surface hydrophilicity/hydrophobicity was evaluated by water contact angle measurements. X-ray photoelectron analysis was performed to investigate the changes in surface states and chemical composition. All silane reagents increased adsorption of the albumin to the modified surface. In vitro cytocompatibility evaluation revealed that silanization improved cell growth on AZ91 modified by silane S1. Measurement of the concentration of Mg2+ ions released during the cell culture indicated that silanization does not affect substrate degradation. PMID:27877541

Resin adhesion strengths to zirconia ceramics after primer treatment with silane coupling monomer or oligomer.

PubMed

Okada, Masahiro; Inoue, Kazusa; Irie, Masao; Taketa, Hiroaki; Torii, Yasuhiro; Matsumoto, Takuya

2017-09-26

Resin bonding to zirconia ceramics is difficult to achieve using the standard methods for conventional silica-based dental ceramics, which employ silane coupling monomers as primers. The hypothesis in this study was that a silane coupling oligomer -a condensed product of silane coupling monomers- would be a more suitable primer for zirconia. To prove this hypothesis, the shear bond strengths between a composite resin and zirconia were compared after applying either a silane coupling monomer or oligomer. The shear bond strength increased after applying a non-activated ethanol solution of the silane coupling oligomer compared with that achieved when applying the monomer. Thermal treatment of the zirconia at 110°C after application of the silane coupling agents was essential to improve the shear bond strength between the composite resin cement and zirconia.

Surface characterization and cytocompatibility evaluation of silanized magnesium alloy AZ91 for biomedical applications

NASA Astrophysics Data System (ADS)

Witecka, Agnieszka; Yamamoto, Akiko; Dybiec, Henryk; Swieszkowski, Wojciech

2012-12-01

Mg alloys with high Al contents have superior corrosion resistance in aqueous environments, but poor cytocompatibility compared to that of pure Mg. We have silanized the cast AZ91 alloy to improve its cytocompatibility using five different silanes: ethyltriethoxysilane (S1), 3-aminopropyltriethoxysilane (S2), 3-isocyanatopyltriethoxysilane (S3), phenyltriethoxysilane (S4) and octadecyltriethoxysilane (S5). The surface hydrophilicity/hydrophobicity was evaluated by water contact angle measurements. X-ray photoelectron analysis was performed to investigate the changes in surface states and chemical composition. All silane reagents increased adsorption of the albumin to the modified surface. In vitro cytocompatibility evaluation revealed that silanization improved cell growth on AZ91 modified by silane S1. Measurement of the concentration of Mg2+ ions released during the cell culture indicated that silanization does not affect substrate degradation.

Medical implants and methods of making medical implants

DOEpatents

Shaw, Wendy J; Yonker, Clement R; Fulton, John L; Tarasevich, Barbara J; McClain, James B; Taylor, Doug

2014-09-16

A medical implant device having a substrate with an oxidized surface and a silane derivative coating covalently bonded to the oxidized surface. A bioactive agent is covalently bonded to the silane derivative coating. An implantable stent device including a stent core having an oxidized surface with a layer of silane derivative covalently bonded thereto. A spacer layer comprising polyethylene glycol (PEG) is covalently bonded to the layer of silane derivative and a protein is covalently bonded to the PEG. A method of making a medical implant device including providing a substrate having a surface, oxidizing the surface and reacting with derivitized silane to form a silane coating covalently bonded to the surface. A bioactive agent is then covalently bonded to the silane coating. In particular instances, an additional coating of bio-absorbable polymer and/or pharmaceutical agent is deposited over the bioactive agent.

Effect of silane concentration on the supersonic combustion of a silane/methane mixture

NASA Technical Reports Server (NTRS)

Northam, G. B.; Mclain, A. G.; Pellett, G. L.; Diskin, G. S.

1986-01-01

A series of direct connect combustor tests was conducted to determine the effect of silane concentration on the supersonic combustion characteristics of silane/methane mixtures. Shock tube ignition delay data indicated more than an order of magnitude reduction in ignition delay times for both 10 and 20 percent silane/methane mixtures as compared to methane. The ignition delay time of the 10 percent mixture was only a factor of 2.3 greater than that of the 20 percent mixture. Supersonic combustion tests were conducted with the fuel injected into a model scramjet combustor. The combustor was mounted at the exit of a Mach 2 nozzle and a hydrogen fired heater was used to provide a variation in test gas total temperature. Tests using the 20 percent silane/methane mixture indicated considerable combustion enhancement when compared to methane alone. This mixture had an autoignition total temperature of 1650 R. This autoignition temperature can be contrasted with 2330 R for hydrogen and 1350 R for a 20 percent silane/hydrogen mixture in similar hardware. Methane without the silane additive did not autoignite in this configuration at total temperatures as high as 3900 R, the maximum temperature at which tests were conducted. Supersonic combustion tests with the silane concentration reduced to 10 percent indicated little improvement in combustion performance over pure methane. The addition of 20 percent silane to methane resulted in a pyrophoric fuel with good supersonic combustion performance. Reducing the silane concentration below this level, however, yielded a less pyrophoric fuel that exhibited poor supersonic combustion performance.

40 CFR 721.9507 - Polyester silane.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Polyester silane. 721.9507 Section 721... Polyester silane. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as a polyester silane (P-95-1022) is subject to reporting under this section for the...

40 CFR 721.9507 - Polyester silane.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Polyester silane. 721.9507 Section 721... Polyester silane. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as a polyester silane (P-95-1022) is subject to reporting under this section for the...

40 CFR 721.10262 - Oxime, Me vinyl silane (generic).

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Oxime, Me vinyl silane (generic). 721... Substances § 721.10262 Oxime, Me vinyl silane (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified generically as oxime, Me vinyl silane (PMN P...

40 CFR 721.10262 - Oxime, Me vinyl silane (generic).

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Oxime, Me vinyl silane (generic). 721... Substances § 721.10262 Oxime, Me vinyl silane (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified generically as oxime, Me vinyl silane (PMN P...

Controlled Interphases in Glass Fiber and Particulate Reinforced Polymers: Structure of Silane Coupling Agents in Solutions and On Substrates

DTIC Science & Technology

1993-01-01

to dissolve into water. Table 3. Typical industrially used silane coupling agents Organofunctional Chemical Formula Group Cationic styryl CH2...can also react with the surface as some unreacted silanol groups remain in the oligomers. The notion of physisorbed and chemisorbed silanes is used ...silanes use many silanol groups for covalent bonding with the substrate surface whereas the loosely chemisorbed silanes use only a few silanols to bond to

Growth kinetics and mass transport mechanisms of GaN columns by selective area metal organic vapor phase epitaxy

NASA Astrophysics Data System (ADS)

Wang, Xue; Hartmann, Jana; Mandl, Martin; Sadat Mohajerani, Matin; Wehmann, Hergo-H.; Strassburg, Martin; Waag, Andreas

2014-04-01

Three-dimensional GaN columns recently have attracted a lot of attention as the potential basis for core-shell light emitting diodes for future solid state lighting. In this study, the fundamental insights into growth kinetics and mass transport mechanisms of N-polar GaN columns during selective area metal organic vapor phase epitaxy on patterned SiOx/sapphire templates are systematically investigated using various pitch of apertures, growth time, and silane flow. Species impingement fluxes on the top surface of columns Jtop and on their sidewall Jsw, as well as, the diffusion flux from the substrate Jsub contribute to the growth of the GaN columns. The vertical and lateral growth rates devoted by Jtop, Jsw and Jsub are estimated quantitatively. The diffusion length of species on the SiOx mask surface λsub as well as on the sidewall surfaces of the 3D columns λsw are determined. The influences of silane on the growth kinetics are discussed. A growth model is developed for this selective area metal organic vapor phase epitaxy processing.

Selective Functionalization of Arbitrary Nanowires

DTIC Science & Technology

2006-11-02

3-mercaptopropyl)- trimethoxysilane (MPTMS). The wires were grown electrochemically in anodic aluminum oxide ( AAO ) templates. Selective deposition...In the past, templates composed of polycarbonate track-etched membranes or anodic aluminum oxide materials have been used for the construction of...modifier MPTMS was used to function- alize the AAO template because it can form covalent bonds with silanes and metal oxide surfaces21 and because of

Investigation of Test Methods, Material Properties, and Processes for Solar Cell Encapsulants

NASA Technical Reports Server (NTRS)

1979-01-01

During this quarter the technical activities were directed toward the reformulation of ethylene/vinyl acetate copolymer for use as a compound in solar cell module fabrication. Successful formulations were devised that lowered the temperature required for cure and raised the gel content. A major volatile component was also eliminated (acrylate crosslinking agent) which should aid in the production of bubble free laminates. Adhesive strengths and primers for the bonding of ethylene/vinyl acetate to supersyrate and substrate materials was assessed with encouraging results. The incorporation of silane compounds gave high bond strengths. A survey of scrim materials was also conducted.

40 CFR 721.10261 - Oxime, di-Me silane (generic).

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Oxime, di-Me silane (generic). 721... Substances § 721.10261 Oxime, di-Me silane (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified generically as oxime, di-Me silane (PMN P-09-589...

40 CFR 721.10261 - Oxime, di-Me silane (generic).

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Oxime, di-Me silane (generic). 721... Substances § 721.10261 Oxime, di-Me silane (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified generically as oxime, di-Me silane (PMN P-09-589...

Demonstrating the feasibility of monitoring the molecular-level structures of moving polymer/silane interfaces during silane diffusion using SFG.

PubMed

Chen, Chunyan; Wang, Jie; Loch, Cheryl L; Ahn, Dongchan; Chen, Zhan

2004-02-04

In this paper, the feasibility of monitoring molecular structures at a moving polymer/liquid interface by sum frequency generation (SFG) vibrational spectroscopy has been demonstrated. N-(2-Aminoethyl)-3-aminopropyltrimethoxysilane (AATM, NH2(CH2)2NH(CH2)3Si(OCH3)3) has been brought into contact with a deuterated poly(methyl methacrylate) (d-PMMA) film, and the interfacial silane structure has been monitored using SFG. Upon initial contact, the SFG spectra can be detected, but as time progresses, the spectral intensity changes and finally disappears. Additional experiments indicate that these silane molecules can diffuse into the polymer film and the detected SFG signals are actually from the moving polymer/silane interface. Our results show that the molecular order of the polymer/silane interface exists during the entire diffusion process and is lost when the silane molecules traverse through the thickness of the d-PMMA film. The loss of the SFG signal is due to the formation of a new disordered substrate/silane interface, which contributes no detectable SFG signal. The kinetics of the diffusion of the silane into the polymer have been deduced from the time-dependent SFG signals detected from the AATM molecules as they diffuse through polymer films of different thickness.

Silane Modification of Glass and Silica Surfaces to Obtain Equally Oil-Wet Surfaces in Glass-Covered Silicon Micromodel Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grate, Jay W.; Warner, Marvin G.; Pittman, Jonathan W.

2013-08-05

The wettability of silicon and glass surfaces can be modified by silanization. However, similar treatments of glass and silica surfaces using the same silane do not necessarily yield the same wettability as determined by the oil-water contact angle. In this technical note, surface cleaning pretreatments were investigated to determine conditions that would yield oil-wet surfaces on glass with similar wettability to silica surfaces treated with the same silane, and both air-water and oil-water contact angles were determined. Air-water contact angles were less sensitive to differences between silanized silica and glass surfaces, often yielding similar values while the oil-water contact anglesmore » were quite different. Borosilicate glass surfaces cleaned with standard cleaning solution 1 (SC1) yield intermediate-wet surfaces when silanized with hexamethyldisilazane, while the same cleaning and silanization yields oil-wet surfaces on silica. However, cleaning glass in boiling concentrated nitric acid creates a surface that can be silanized to obtain oil-wet surfaces using HDMS. Moreover, this method is effective on glass with prior thermal treatment at an elevated temperature of 400oC. In this way, silica and glass can be silanized to obtain equally oil-wet surfaces using HMDS. It is demonstrated that pretreatment and silanization is feasible in silicon-silica/glass micromodels previously assembled by anodic bonding, and that the change in wettability has a significant observable effect on immiscisble fluid displacements in the pore network.« less

Hydrogen-dominated plasma, due to silane depletion, for microcrystalline silicon deposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Howling, A. A.; Sobbia, R.; Hollenstein, Ch.

2010-07-15

Plasma conditions for microcrystalline silicon deposition generally require a high flux of atomic hydrogen, relative to SiH{sub {alpha}=0{yields}3} radicals, on the growing film. The necessary dominant partial pressure of hydrogen in the plasma is conventionally obtained by hydrogen dilution of silane in the inlet flow. However, a hydrogen-dominated plasma environment can also be obtained due to plasma depletion of the silane in the gas mixture, even up to the limit of pure silane inlet flow, provided that the silane depletion is strong enough. At first sight, it may seem surprising that the composition of a strongly depleted pure silane plasmamore » consists principally of molecular hydrogen, without significant contribution from the partial pressure of silane radicals. The aim here is to bring some physical insight by means of a zero-dimensional, analytical plasma chemistry model. The model is appropriate for uniform large-area showerhead reactors, as shown by comparison with a three-dimensional numerical simulations. The SiH{sub {alpha}} densities remain very low because of their rapid diffusion and surface reactivity, contributing to film growth which is the desired scenario for efficient silane utilization. Significant SiH{sub {alpha}} densities due to poor design of reactor and gas flow, on the other hand, would result in powder formation wasting silane. Conversely, hydrogen atoms are not deposited, but recombine on the film surface and reappear as molecular hydrogen in the plasma. Therefore, in the limit of extremely high silane depletion fraction (>99.9%), the silane density falls below the low SiH{sub {alpha}} densities, but only the H radical can eventually reach significant concentrations in the hydrogen-dominated plasma.« less

Morphology and water resistance of mixed silane films of bis[3-(triethoxysilyl) propyl]tetrasulfide and bis-[trimethoxysilylpropyl]amine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan, Guirong; Schaefer, Dale W.; van Ooij, Wim J.

2010-12-03

Functional organosilanes are powerful interface-active agents that find applications as adhesion promoters as well as optical, dielectric and protective coatings. Bis-silanes are of particular interest because they are highly crosslinked leading to very robust films. In almost all applications, the water resistance of the films is a critical performance measure. Here we use neutron reflectivity to address the effect of bridging group on the hydrothermal response of bis-silane films prepared using bis[3-(triethoxysilyl) propyl]tetrasulfide and bis-[trimethoxysilylpropyl]amine. Neat and mixed films are examined as-prepared, after exposure to water vapor and then in the re-dried state. The bridging group is the key factormore » that controls the morphology and water resistance of silane films. Although bis-sulfur silane is not as condensed as bis-amino silane, bis-sulfur swells less in water because of the hydrophobic nature of bridging group. The reflectivity of bis-sulfur silane film is reversible after room-temperature water conditioning but not at 80 C, indicating chemical alternation of the film at 80 C. The water resistance of mixed silane is roughly that of both components weighted by their volume fraction. But based on the enhanced shrinkage that occurs following water-vapor conditioning of the mixed film, condensation is accelerated in the mixed silane. Regarding the precursor solution, bis-amino silane may act as a catalyst in the hydrolysis of bis-sulfur silane leading to more silanols in the solution and further condensation in the film. Variation in the structure normal to the substrate is also examined by swelling the film with d-nitrobenzene, a non-reacting swelling agent.« less

Effect of laser heat treatment on Pull-out bond strength of fiber posts treated with different silanes.

PubMed

Shafiei, Fereshteh; Saadat, Maryam; Jowkar, Zahra

2018-05-01

This study evaluated the effect of three different silanes and post-silanization treatments on the retentive strength of fiber posts luted with an etch-and-rinse resin cement. One hundred intact maxillary central incisors were randomly divided into 10 groups after endodontic treatment and post space preparation (n=10). The fiber posts were etched using 24% hydrogen peroxide. Posts of the control group did not receive silane. In nine experimental groups, each of the three silanes used, Scotchbond Universal adhesive, Bis-Silane and Porcelain Primer, was subjected to three treatments: air-drying at 25°C, warm air-drying and CO2 laser heat treatment. After cementation of the treated posts using One-Step Plus/Duo-Link cement, the specimens were stored for one weak and then subjected to pull-out bond strength (PBS) testing. The data in Newton (N) were analyzed using two-way ANOVA and Tukey tests (α=0.05). PBS was significantly affected by silane type and post-silanization treatment ( p <0.001). The interaction of the two factors was not statistically significant ( p =0.15). The effect of Porcelain Primer on PBS was significantly higher than those of universal adhesive ( p <0.001) and Bis-Silane ( p =0.01), with similar results for the two latter. Warm air-drying and laser treatment significantly increased PBS ( p <0.001). The lowest and highest PBS was obtained in the control (no silane) group (190.9±31) and laser-treated/ Porcelain Primer group (377.1±50), respectively. Warm air-drying and CO2 laser heat treatment had a significantly beneficial effect on retentive strength of fiber posts. Porcelain Primer was significantly more effective than universal adhesive and Bis-Silane. Key words: Laser heat treatment, Pull-out bond strength, fiber post.

Influence of Etching Protocol and Silane Treatment with a Universal Adhesive on Lithium Disilicate Bond Strength.

PubMed

Kalavacharla, V K; Lawson, N C; Ramp, L C; Burgess, J O

2015-01-01

To measure the effects of hydrofluoric acid (HF) etching and silane prior to the application of a universal adhesive on the bond strength between lithium disilicate and a resin. Sixty blocks of lithium disilicate (e.max CAD, Ivoclar Vivadent) were sectioned into coupons and polished. Specimens were divided into six groups (n=10) based on surface pretreatments, as follows: 1) no treatment (control); 2) 5% HF etch for 20 seconds (5HF); 3) 9.5% HF etch for 60 seconds (9.5HF); 4) silane with no HF (S); 5) 5% HF for 20 seconds + silane (5HFS); and 6) 9.5% HF for 60 seconds + silane (9.5HFS). All etching was followed by rinsing, and all silane was applied in one coat for 20 seconds and then dried. The universal adhesive (Scotchbond Universal, 3M ESPE) was applied onto the pretreated ceramic surface, air thinned, and light cured for 10 seconds. A 1.5-mm-diameter plastic tube filled with Z100 composite (3M ESPE) was applied over the bonded ceramic surface and light cured for 20 seconds on all four sides. The specimens were thermocycled for 10,000 cycles (5°C-50°C/15 s dwell time). Specimens were loaded until failure using a universal testing machine at a crosshead speed of 1 mm/min. The peak failure load was used to calculate the shear bond strength. Scanning electron microscopy images were taken of representative e.max specimens from each group. A two-way analysis of variance (ANOVA) determined that there were significant differences between HF etching, silane treatment, and the interaction between HF and silane treatment (p<0.01). Silane treatment provided higher shear bond strength regardless of the use or concentration of the HF etchant. Individual one-way ANOVA and Tukey post hoc analyses were performed for each silane group. Shear bond strength values for each etch time were significantly different (p<0.01) and could be divided into significantly different groups based on silane treatment: no silane treatment: 0 HF < 5% HF < 9.5% HF; and RelyX silane treatment: 0 HF < 5% HF and 9.5% HF. Both HF and silane treatment significantly improved the bond strength between resin and lithium disilicate when used with a universal adhesive.

Development of the silane process for the production of low-cost polysilicon

NASA Technical Reports Server (NTRS)

Iya, S. K.

1986-01-01

It was recognized that the traditional hot rod type deposition process for decomposing silane is energy intensive, and a different approach for converting silane to silicon was chosen. A 1200 metric tons/year capacity commercial plant was constructed in Moses Lake, Washington. A fluidized bed processor was chosen as the most promising technology and several encouraging test runs were conducted. This technology continues to be very promising in producing low cost polysilicon. The Union Carbide silane process and the research development on the fluidized bed silane decomposition are discussed.

Salt exclusion in silane-laced epoxy coatings.

PubMed

Wang, Peng; Schaefer, Dale W

2010-01-05

The corrosion protection mechanism of a one-step silane-laced epoxy coating system was investigated using neutron reflectivity. Pure epoxy and silane-laced epoxy films were examined at equilibrium with saturated NaCl water solution. The results demonstrate that the addition of silane introduces a salt-exclusion effect to epoxy coating. Specifically, the addition of silane densifies the epoxy network, which leads to exclusion of hydrated salt ions by a size effect. The effect is particularly significant at the metal-coating interface. Exclusion of ions improves the corrosion resistance, particularly for metals susceptible to pitting.

Silanes as Fuel for Aerospace Propulsion

NASA Astrophysics Data System (ADS)

Simone, Domenico; Bruno, Claudio; Hidding, Bernhard

In the light of recently revived interest in high energy density fuels for aerospace applications1,2), a new look is being given at unconventional fuels. Among the latter are hydrides, because their hydrogen content and density. Among hydrides silanes are of interest because of their combustion and energetic properties.Silanes are silicon hydrides organized in molecular chains similar to those of hydrocarbons; at STP, lower silanes (SiH4, Si2H6) are gaseous and extremely pyrophoric; with increasing chain length, silanes become liquid from trisilane (Si3H8) on, and therefore easily pumped. Another important feature of silanes is the large amount of hydrogen theoretically available by thermal decomposition: in fact at moderate temperatures (about 500 K) the chains begin to break and at 700 K their decomposition is complete, yielding silicon and gaseous hydrogen, useful for propulsion in combination with air nitrogen and oxygen. This last feature, if confirmed, could identify silanes not only as energy carriers but also components in bi-fuel systems. To assess their theoretical performance, simulations were conducted assuming silanes and/or their thermal decomposition products in combination with various oxidizers and air. Preliminary results are suggestive of their potential for some specialized applications, especially where compactness is at premium.

Degradation of bare and silanized silicon wafer surfaces by constituents of biological fluids.

PubMed

Dekeyser, C M; Buron, C C; Derclaye, S R; Jonas, A M; Marchand-Brynaert, J; Rouxhet, P G

2012-07-15

The 24 h stability of bare silicon wafers as such or silanized with CH(3)O-(CH(2)-CH(2)-O)(n)-C(3)H(6)-trichlorosilane (n=6-9) was investigated in water, NaCl, phosphate and carbonate solutions, and in phosphate buffered saline (PBS) at 37 °C (close to biological conditions regarding temperature, high ionic strength, and pH). The resulting surfaces were analyzed using ellipsometry, X-ray Reflectometry (XRR), X-ray Photoelectron Spectroscopy (XPS), and Atomic Force Microscopy (AFM). Incubation of the silanized wafers in phosphate solution and PBS provokes a detachment of the silane layer. This is due to a hydrolysis of Si-O bonds which is favored by the action of phosphate, also responsible for a corrosion of non-silanized wafers. The surface alteration (detachment of silane layer and corrosion of the non-silanized wafer) is also important with carbonate solution, due to a higher pH (8.3). The protection of the silicon oxide layer brought by silane against the action of the salts is noticeable for phosphate but not for carbonate. Copyright © 2012 Elsevier Inc. All rights reserved.

Method of enhancing the electronic properties of an undoped and/or N-type hydrogenated amorphous silicon film

DOEpatents

Carlson, David E.

1980-01-01

The dark conductivity and photoconductivity of an N-type and/or undoped hydrogenated amorphous silicon layer fabricated by an AC or DC proximity glow discharge in silane can be increased through the incorporation of argon in an amount from 10 to about 90 percent by volume of the glow discharge atmosphere which contains a silicon-hydrogen containing compound in an amount of from about 90 to about 10 volume percent.

Effect of surface treatments on the bond strength between resin cement and differently sintered zirconium-oxide ceramics.

PubMed

Yenisey, Murat; Dede, Doğu Ömür; Rona, Nergiz

2016-01-01

This study investigated the effects of surface treatments on bond strength between resin cement and differently sintered zirconium-oxide ceramics. 220 zirconium-oxide ceramic (Ceramill ZI) specimens were prepared, sintered in two different period (Short=Ss, Long=Ls) and divided into ten treatment groups as: GC, no treatment; GSil, silanized (ESPE-Sil); GSilPen, silane flame treatment (Silano-Pen); GSb, sandblasted; GSbSil, sandblasted+silanized; GSbCoSil, sandblasted+silica coated (CoJet)+silanized; GSbRoSil, sandblasted+silica coated (Rocatech-Plus)+silanized; GSbDSil, sandblasted+diamond particle abraded (Micron MDA)+silanized; GSbSilPen, sandblasted+silane flame treatment+silanized; GSbLSil, sandblasted+Er:Yag (Asclepion-MCL30) laser treated+silanized. The composite resin (Filtek Z-250) cylinders were cemented to the treated ceramic surfaces with a resin cement (Panavia F2.0). Shear bond strength test was performed after specimens were stored in water for 24h and thermo-cycled for 6000 cycles (5-55 °C). Data were statistically analyzed with two-way analysis of variance (ANOVA) and Tamhane's multiple comparison test (α=0.05). According to the ANOVA, sintering time, surface treatments and their interaction were statistically significant (p<0.05). The highest bond strengths were obtained in GSbCoSil (Ss=13.36/Ls=11.19MPa) and lowest values were obtained in GC (Ss=4.70/Ls=4.62 MPa) for both sinter groups. Sintering time may be effective on the bond strength and 30 μm silica coating (Cojet) with silane coupling application technique increased the bond strength between resin cement and differently sintered zirconium-oxide ceramics. Copyright © 2015 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

Chitosan/CNTs green nanocomposite membrane: synthesis, swelling and polyaromatic hydrocarbons removal.

PubMed

Bibi, Saira; Yasin, Tariq; Hassan, Safia; Riaz, Muhammad; Nawaz, Mohsan

2015-01-01

Carbon nanotubes (CNTs) were irradiated in air at 100 kGy under gamma radiations. The Raman spectroscopy of γ-treated CNTs showed distinctive changes in the absorption bands. The CNTs were mixed with blend of chitosan (Cs)/poly (vinyl alcohol) (PVA) and crosslinked with silane. The chemical reactions between the components affected the position and intensities of the infrared bands. Scanning electron micrograph of Cs/CNTs nanocomposite membrane showed the homogeneous dispersion of CNTs in the polymer matrix. The addition of CNTs lowered its swelling in water. Naphthalene (NAPH) was selected as a model compound and its removal was studied using HPLC technique. This membrane showed fast uptake of NAPH and 87% was removed from water within 30 min. The NAPH loaded membrane showed strong chemical interactions and cannot be desorbed. The fast uptake of PAHs and the green nature of this membrane made them suitable candidates for clean-up purposes. Copyright © 2014 Elsevier B.V. All rights reserved.

A New Antiwear Additive/Surface Pretreatment for PFPE Liquid Lubricants

NASA Technical Reports Server (NTRS)

Morales, Wilfredo; Fusaro, Robert L.; Siebert, Mark; Keith, Theo; Jansen, Ralph; Herrera-Fierro, Pilar

1995-01-01

Pin-on-disk tribology experiments were conducted on a perfluoroalkylelher (PFPE) liquid lubricant with and without a new PFPE lubricant antiwear additive material, a silane. It was found that the silane provided moderate improvement in the antiwear performance of the PFPE lubricant when applied to the metallic surface as a surface coating or when added to the PFPE as a dispersion (emulsion). Slightly better results were obtained by using the combination of a surface coating and an emulsion of the silane. The silane emulsions or coatings did not affect the friction properties of the lubricant. Micro-Fourier transformation infrared (muFTIR) spectroscopy analysis was performed to study silane transfer films and the degradation of the PFPE. The silane was found to mitigate degradation of the PFPE which may have been the major reason for the improved antiwear performance observed.

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

PubMed

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

2013-03-01

The preparation of thin films of chitosan-silane hybrid materials by combining sol-gel processing and spin coating is reported. A variety of silanes can be used as starting materials for the preparation of such thin films, namely tetraethoxysilane, tri-tert-butoxysilanol, trimethylethoxysilane, p-trifluoromethyltetra-fluorophenyltriethoxysilane, trivinylmethoxysilane, (methoxymethyl)trimethyl-silane, and hexamethoxydisilane. These silanes are subjected to a sol-gel process before they are added to acidic chitosan solutions. The chitosan:silane ratio is kept constant at 6:1 (w/w) and dilutions with ethanol are prepared and spin coated. Depending on the degree of dilution, film thickness can be controlled in a range between 5 and 70 nm. For the determination of additional surface properties, static water contact angle measurements and atomic force microscopy have been employed. Copyright © 2012 Elsevier Ltd. All rights reserved.

Reinforcement of Dental Methacrylate with Glass Fiber after Heated Silane Application

PubMed Central

Fonseca, Rodrigo Borges; de Paula, Marcella Silva; Favarão, Isabella Negro; Kasuya, Amanda Vessoni Barbosa; de Almeida, Letícia Nunes; Mendes, Gustavo Adolfo Martins; Carlo, Hugo Lemes

2014-01-01

This study evaluated the influence of silane heat treatment and glass fiber fabrication type, industrially treated (I) or pure (P), on flexural and compressive strength of methacrylate resin bars (BISGMA/TEGDMA, 50/50%). Six groups (n = 10) were created: I-sil: I/silanated; P-sil: P-silanated; I-sil/heat: I/silanated heated to 100°; P-sil/heat: P/silanated heated to 100°; (I: I/not silanated; and P: P/not silanated. Specimens were prepared for flexural strength (10 × 2 × 1 mm) and for compressive strength 9.5 × 5.5 × 3 mm) and tested at 0.5 mm/min. Statistical analysis demonstrated the following for flexural strength (P < 0.05): I-sil: 155.89 ± 45.27BC; P-sil: 155.89 ± 45.27BC; I-sil/heat: 130.20 ± 22.11C; P-sil/heat: 169.86 ± 50.29AB; I: 131.87 ± 15.86C. For compressive strength, the following are demonstrated: I-sil: 1367.25 ± 188.77ab; P-sil: 867.61 ± 102.76d; I-sil/heat: 1162.98 ± 222.07c; P-sil/heat: 1499.35 ± 339.06a; and I: 1245.78 ± 211.16bc. Due to the impossibility of incorporating the stipulated amount of fiber, P group was excluded. Glass fiber treatment with heated silane enhanced flexural and compressive strength of a reinforced dental methacrylate. PMID:24967361

Influence of silane coupling agent on microstructure and properties of CCTO-P(VDF-CTFE) composites

NASA Astrophysics Data System (ADS)

Tong, Yang; Zhang, Lin; Bass, Patrick; Rolin, Terry D.; Cheng, Z.-Y.

Influence of the coupling agent on microstructure and dielectric properties of ceramic-polymer composites is systematically studied using CaCu3Ti4O12 (CCTO) as the filler, trichloro-(1H,1H,2H,2H-perfluorooctyl)-silane (Cl3-silane) as coupling agent, and P(VDF-CTFE) 88/12mol.% copolymer as the matrix. It is demonstrated that Cl3-silane molecules can be attached onto CCTO surface using a simple process. The experimental results show that coating CCTO with Cl3-silane can improve the microstructure uniformity of the composites due to the good wettability between Cl3-silane and P(VDF-CTFE), which also significantly improves the electric breakdown field of the composites. It is found that the composites using CCTO coated with 1.0wt.% Cl3-silane exhibit a higher dielectric constant with a higher electric breakdown field. For the composites with 15vol.% CCTO that is coated with 1.0wt.% Cl3-silane, an electric breakdown field of more than 240MV/m is obtained with an energy density of more than 4.5J/cm3. It is also experimentally found that the dielectric constant can be used to easily identify the optimized content of coupling agent.

Mixed matrix membrane incorporated with large pore size halloysite nanotubes (HNT) as filler for gas separation: experimental.

PubMed

Hashemifard, S A; Ismail, A F; Matsuura, T

2011-07-15

This study investigated the gas separation and transport properties of asymmetric mixed matrix membranes (MMM) fabricated from polyetherimide (PEI); Ultem 1000 incorporated with raw and modified halloysite nanotubes (HNT) as filler. The modified HNTs; S-HNTs were prepared by treating HNTs with N-β-(aminoethyl)-γ-aminopropyltrimethoxy silane (AEAPTMS). FESEM, XRD, FTIR, TGA, DSC and pure gas permeation testing were used to characterise the S-HNTs and the fabricated MMMs. In the first part of the experiments, the effect of dope preparation factors such as: ultrasonic sonication period, filler wetting period and priming period were investigated. In the second part, the influence of silane concentration on the fabricated MMMs was studied. Results showed that, increasing the silane concentration, led to higher tendency in HNT agglomeration which resulted in poor separation properties but permeability enhancement. In the last part, the effect of S-HNTs loading was experienced. Our observations showed that the dispersion of nanoparticles decreased with an increase in the S-HNTs loading. Accordingly, 0.5% loading of silylated-HNT yielded the optimum MMMs in terms of permeability (27% increase) and selectivity (8% increase). Copyright © 2011 Elsevier Inc. All rights reserved.

Silicon production in a fluidized bed reactor

NASA Technical Reports Server (NTRS)

Rohatgi, N. K.

1986-01-01

Part of the development effort of the JPL in-house technology involved in the Flat-Plate Solar Array (FSA) Project was the investigation of a low-cost process to produce semiconductor-grade silicon for terrestrial photovoltaic cell applications. The process selected was based on pyrolysis of silane in a fluidized-bed reactor (FBR). Following initial investigations involving 1- and 2-in. diameter reactors, a 6-in. diameter, engineering-scale FBR was constructed to establish reactor performance, mechanism of silicon deposition, product morphology, and product purity. The overall mass balance for all experiments indicates that more than 90% of the total silicon fed into the reactor is deposited on silicon seed particles and the remaining 10% becomes elutriated fines. Silicon production rates were demonstrated of 1.5 kg/h at 30% silane concentration and 3.5 kg/h at 80% silane concentration. The mechanism of silicon deposition is described by a six-path process: heterogeneous deposition, homogeneous decomposition, coalescence, coagulation, scavenging, and heterogeneous growth on fines. The bulk of the growth silicon layer appears to be made up of small diameter particles. This product morphology lends support to the concept of the scavenging of homogeneously nucleated silicon.

Stoichiometry and possible mechanism of SiH/sub 4/-O/sub 2/ explosions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hartman, J.R.; Famil-Ghiriha, J.; Ring, M.A.

1987-04-01

The products of silane-O/sub 2/ mixture explosions vary with mixture composition. For O/sub 2/-rich mixtures (>70% O/sub 2/), the products are H/sub 2/O and SiO/sub 2/. As the mixtures become richer in silane, H/sub 2/ replaces H/sub 2/O as a final product. For very SiH/sub 4/-rich mixtures (>70% SiH/sub 4/), the products are H/sub 2/, SiO/sub x/, and Si. The fact that silane is totally consumed in silane-rich mixtures (70-90% silane) demonstrates that solid particle formation (SiO/sub 2/, SiO, and Si) occurs very rapidly and that the accompanying heat release is essential to drive the reactions to completion. It ismore » also clear that the explosion of a silane-rich mixture is primarily a thermal explosion of silane. Effects due to problems associated with upper pressure limit measurements and mechanistic aspects of the SiH/sub 4/-O/sub 2/ explosion reaction are discussed.« less

Characterization of the reactivity of a silica derived from acid activation of sepiolite with silane by 29Si and 13C solid-state NMR.

PubMed

Valentín, J L; López-Manchado, M A; Posadas, P; Rodríguez, A; Marcos-Fernández, A; Ibarra, L

2006-06-15

The mechanism of the reaction between a silica sample coming from acid treatment of sepiolite (denominated Silsep) and an organosilane, namely bis(triethoxysilylpropyl)tetrasulfane (TESPT), has been evaluated by solid state NMR spectroscopy, being compared with the silanization reaction of a commercial silica. The effect of the silane concentration and temperature on the course of the reaction was considered. Experimental results indicate that the silanization reaction is more effective in the case of Silsep, favoring both the reaction of silane molecules with the filler surface and the reaction between neighboring silane molecules. This different behavior is attributed to structural factors, moisture, and number of acid centers on silica surface. Environmental scanning electron microscopy (ESEM) was used to deposit micrometric water drops on the surface of these samples and to evaluate the proportion and distribution of the organophylization process.

Recent advances in self-assembled monolayers based biomolecular electronic devices.

PubMed

Arya, Sunil K; Solanki, Pratima R; Datta, Monika; Malhotra, Bansi D

2009-05-15

Self-assembled monolayers (SAMs) have aroused much interest due to their potential applications in biosensors, biomolecular electronics and nanotechnology. This has been largely attributed to their inherent ordered arrangement and controllable properties. SAMs can be formed by chemisorption of organic molecules containing groups like thiols, disulphides, amines, acids or silanes, on desired surfaces and can be used to fabricate biomolecular electronic devices. We focus on recent applications of organosulphur compounds (thiols) based SAMs to biomolecular electronic devices in the last about 3 years.

Gas Phase Ion-Molecule Chemistry of Carbon, Nitrogen and Oxygen Compounds.

DTIC Science & Technology

1985-01-29

silyl anions aza allyl anion) phosphide anion sulfides) Reactivity; nitrite estersj electron affinityMechanism’, sulfur dioxidej. (cont’d) M L..J A6*rAcr...use of silane chemistry to attack a problem of fundamental importance to all organic chemistry, the relative acidity of the alkanes.20 While it is well...alkane lost are a measure of the relative acidity of RH. For example, because ethane is lost less easily than methane, we believe that the ethyl anion

Synthesis of tris- and tetrakis(pentafluoroethyl)silanes.

PubMed

Steinhauer, Simon; Bader, Julia; Stammler, Hans-Georg; Ignat'ev, Nikolai; Hoge, Berthold

2014-05-12

The synthesis and complete characterization of functional, highly Lewis acidic tris(pentafluoroethyl)silanes as well as tetrakis(perfluoroalkyl)silanes Si(C2F5)4 and Si(C2F5)3 CF3 by direct fluorination is described. The reaction of SiCl4 with LiC2F5 invariably affords (pentafluoroethyl)fluorosilicates. To avoid silicate formation by fluoride transfer from LiC2F5 the Lewis acidity of the silane has to be decreased by electron-donating substituents, such as dialkylamino groups. The easily accessible Si(C2F5)3 NEt2 is a valuable precursor for a series of tris(pentafluoroethyl)silanes. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Silane-propane ignitor/burner

DOEpatents

Hill, R.W.; Skinner, D.F. Jr.; Thorsness, C.B.

1983-05-26

A silane propane burner for an underground coal gasification process which is used to ignite the coal and to controllably retract the injection point by cutting the injection pipe. A narrow tube with a burner tip is positioned in the injection pipe through which an oxidant (oxygen or air) is flowed. A charge of silane followed by a supply of fuel, such as propane, is flowed through the tube. The silane spontaneously ignites on contact with oxygen and burns the propane fuel.

Silane-propane ignitor/burner

DOEpatents

Hill, Richard W.; Skinner, Dewey F.; Thorsness, Charles B.

1985-01-01

A silane propane burner for an underground coal gasification process which is used to ignite the coal and to controllably retract the injection point by cutting the injection pipe. A narrow tube with a burner tip is positioned in the injection pipe through which an oxidant (oxygen or air) is flowed. A charge of silane followed by a supply of fuel, such as propane, is flowed through the tube. The silane spontaneously ignites on contact with oxygen and burns the propane fuel.

Effects of sandblasting and silica coating on the bond strength of rebonded mechanically retentive ceramic brackets.

PubMed

Toroglu, M Serdar; Yaylali, Sirin

2008-08-01

The aim of this study was to determine the bond strength of rebonded mechanically retentive ceramic brackets after treatment with 2 abrasive techniques. In addition to a group of new brackets, 3 groups were treated according to the following conditions of debonded ceramic bracket bases: sandblasting, sandblasting + silane, and silica coating + silane (15 in each group). Treated ceramic brackets were rebonded on premolars. The samples were stored in distilled deionized water for 24 hours at 37 degrees C in an incubator and then thermocycled for 1000 times between 5 degrees C and 55 degrees C. Shear force was applied to the enamel-adhesive interface until debonding. The highest bond strength values were in the silica coating + silane and the new bracket groups (12.7 and 12.0 MPa, respectively), followed by the sandblasting + silane group (10.5 MPa). The sandblasting group had a significantly lower bond strength value (4.5 MPa). No enamel fracture was noted in any sample tested. In the new bracket and the sandblasting + silane groups, 20% of the samples had adhesive remnant index scores of 2, and 80% had scores of 3. In the sandblasting group, all specimens debonded at the bracket-adhesive interface. The silica coating + silane group showed mixed failures. Sandblasting + silane and silica coating + silane applications on debonded ceramic bracket base can produce bond strengths comparable with new brackets.

Heat treatment of pre-hydrolyzed silane increases adhesion of phosphate monomer-based resin cement to glass ceramic.

PubMed

de Carvalho, Rodrigo Furtado; Cotes, Caroline; Kimpara, Estevão Tomomitsu; Leite, Fabíola Pessoa Pereira; Özcan, Mutlu

2015-01-01

This study evaluated the influence of different forms of heat treatment on a pre-hydrolyzed silane to improve the adhesion of phosphate monomer-based (MDP) resin cement to glass ceramic. Resin and feldspathic ceramic blocks (n=48, n=6 for bond test, n=2 for microscopy) were randomly divided into 6 groups and subject to surface treatments: G1: Hydrofluoric acid (HF) 9.6% for 20 s + Silane + MDP resin cement (Panavia F); G2: HF 9.6% for 20 s + Silane + Heat Treatment (oven) + Panavia F; G3: Silane + Heat Treatment (oven) + Panavia F; G4: HF 9.6% for 20 s + Silane + Heat Treatment (hot air) + Panavia F; G5: Silane + Heat Treatment (hot air) + Panavia F; G6: Silane + Panavia F. Microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using stereomicroscope and scanning electron microscope (SEM) to categorize the failure types. Data were analyzed statistically using two-way test ANOVA and Tukey's test (=0.05). Heat treatment of the silane containing MDP, with prior etching with HF (G2: 13.15 ± 0.89a; G4: 12.58 ± 1.03a) presented significantly higher bond strength values than the control group (G1: 9.16 ± 0.64b). The groups without prior etching (G3: 10.47 ± 0.70b; G5: 9.47 ± 0.32b) showed statistically similar bond strength values between them and the control group (G1). The silane application without prior etching and heat treatment resulted in the lowest mean bond strength (G6: 8.05 ± 0.37c). SEM analysis showed predominantly adhesive failures and EDS analysis showed common elements of spectra (Si, Na, Al, K, O, C) characterizing the microstructure of the glass-ceramic studied. Heat treatment of the pre-hydrolyzed silane containing MDP in an oven at 100 °C for 2 min or with hot air application at 50 ± 5 ºC for 1 min, was effective in increasing the bond strength values between the ceramic and resin cement containing MDP.

Effect of Silanization on Microtensile Bond Strength of Different Resin Cements to a Lithium Disilicate Glass Ceramic.

PubMed

Gré, Cristina Parise; de Ré Silveira, Renan C; Shibata, Shizuma; Lago, Carlo Tr; Vieira, Luiz Cc

2016-02-01

This study evaluated the influence of a silane-coupling agent on the bond strength of a self-adhesive cement and a conventional resin cement to a lithium disilicate glass ceramic. A total of eight ceramic blocks were fabricated and divided into four groups (n = 2). In groups 1 and 3, ceramic surfaces were etched with hydrofluoric acid 10% for 20 seconds, rinsed for 30 seconds, and air-dried. One layer of a silane agent was applied onto all ceramic specimens and air-dried for 30 seconds. In groups 2 and 4, ceramic surfaces were etched with hydrofluoric acid, rinsed, and air-dried without application of the silane-coupling agent. The ceramic blocks were bonded to a block of composite with a self-adhesive resin cement or with a conventional resin cement, according to the manufacturer's instructions. After 24 hours in distilled water at 37°C, the specimens were sectioned perpendicular to the bonding interface area to obtain beams with a bonding area of 0.8 mm(2) and submitted to a microtensile bond strength test at a crosshead speed of 0.5 mm/min. Data were statistically analyzed with one-way analysis of variance and the Games-Howell post hoc test (p = 0.05). Fractured specimens were examined under optical microscopy at 40x magnification. Silanization resulted in higher microtensile bond strength compared to groups without silane. No significant differences were found between the conventional resin cement and the self-adhesive resin cement with silane agent (p = 0.983), and without silane agent (p = 0.877). Silanization appears to be crucial for resin bonding to a lithium disilicate-based ceramic, regardless of the resin cement used. The self-adhesive resin cement performed as well as the conventional resin cement. Applying one layer of a silane-coupling agent after etching the ceramic surface with hydrofluoric acid 10% enhanced the bond strength between resin cements and a glass ceramic.

[Spectroscopic study on film formation mechanism and structure of composite silanes-V-Zr passive film].

PubMed

Wang, Lei; Liu, Chang-sheng; Shi, Lei; An, Cheng-qiang

2015-02-01

A composite silanes-V-Zr passive film was overlayed on hot-dip galvanized steel. Attenuated total reflection Fourier transformed infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectrometer (XPS) and radio frequency glow discharge optical emission spectrometry (rf-GD-OES) were used to characterize the molecular structure of the silanes-V-Zr passive film. The mechanism of film formation was discussed: The results show that the silane molecules are crosslinked as the main film former and inorganic inhibitor is even distributed in the film. The fitting peak of 100.7 eV in XPS single Si2p energy range spectra of the composite silanes-V-Zr passive film and the widening and strengthening of the Si--O infrared absorption peak at 1100 cm(-1) indicate that the silanes were adsorbed on the surface of zinc with chemical bond of Si--O--Zn, and the silane molecules were connected with each other by bond of Si--O--Si. Two characteristic absorption peaks of amide at 1650 and 1560 cm(-1) appear in the infrared spectroscopy of the composite silanes-V-Zr passive film, and a characteristic absorption peak of epoxy groups at 910 cm(-1) disappears in the infrared spectroscopy of the passive film. The results indicate that gamma-APT can be prepared through nucleophilic ring-opening of ethylene oxide in gamma-GPT molecule to form C--N covalent bonds. The rf-GD-OES results indicate that there is a oxygen enriched layer in 0.3 microm depth of the composite silanes-V-Zr passive film. Moreover, ZrF4, ZrO2 and some inorganic matter obtained by the reaction during the forming processof the composite silanes-V-Zr passive film are distributed evenly throughout the film. According to the film composition, the physical processes and chemical reactions during the film forming process were studied by using ATR-FTIR. Based on this, the film forming mechanism was proposed.

Corrosion protection and adhesion properties of the epoxy coating applied on the steel substrate pre-treated by a sol-gel based silane coating filled with amino and isocyanate silane functionalized graphene oxide nanosheets

NASA Astrophysics Data System (ADS)

Parhizkar, Nafise; Ramezanzadeh, Bahram; Shahrabi, Taghi

2018-05-01

This research has focused on the effect of graphene oxide (GO) nano-fillers embedded in the sol-gel based silane coating on the corrosion protection and adhesion properties of the epoxy coating applied on the steel substrate pre-treated by silane coatings. For this purpose, a mixture of Methyltriethoxysilane (MTES) and Tetraethylorthosilicate (TEOS) silane precursors was used for preparation of composite matrix and the GO nanosheets, which are covalently functionalized with 3-(Triethoxysilyl)propyl isocyanate (TEPI, IGO nano-fillers) and 3-aminopropyltriethoxysilane (APTES, AGO nano-fillers), were used as filler. The GO, AGO and IGO nanosheets were characterized by Fourier Transform Infrared Spectroscopy (FT-IR), UV-Visible analysis and field emission-scanning electron microscopy techniques. The performance of the silane/epoxy coatings was investigated by pull-off adhesion, cathodic delamination, salt spray and electrochemical impedance spectroscopy (EIS) tests. Results revealed that AGO and IGO nano-fillers significantly improved the corrosion resistance and adhesion properties of the top epoxy coating due to better compatibility with silane matrix, excellent barrier properties and the formation of covalent bonds with the top epoxy coating.

VAPOR PHASE MERCURY SORPTION BY ORGANIC SULFIDE MODIFIED BIMETALLIC IRON-COPPER NANOPARTICLE AGGREGATES

EPA Science Inventory

Novel organic sulfide modified bimetallic iron-copper nanoparticle aggregate sorbent materials have been synthesized for removing elemental mercury from vapor streams at elevated temperatures (120-140 °C). Silane based (disulfide silane and tetrasulfide silane) and alkyl sulfide ...

40 CFR 721.9501 - Silane, triethoxy[3-oxiranylmethoxy)propyl]-.

Code of Federal Regulations, 2010 CFR

2010-07-01

...) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT NEW USES OF CHEMICAL SUBSTANCES Significant New Uses for Specific Chemical Substances § 721.9501 Silane, triethoxy[3-oxiranylmethoxy)propyl]-. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as silane...

Method and apparatus for forming a carbon-silicon bond in a silane

DOEpatents

Schattenmann, Florian Johannes

2002-01-01

A method for forming at least one product silane, comprising reacting a transition metal hydride with a starting silane in a presence of a catalyst and at a temperature that exceeds a threshold temperature associated with said reacting.

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

NASA Technical Reports Server (NTRS)

Mikes, F.

1984-01-01

Silane primers for use as thermal protection on external tanks were subjected to various analytic techniques to determine the most effective testing method for silane lot evaluation. The analytic methods included high performance liquid chromatography, gas chromatography, thermogravimetry (TGA), and fourier transform infrared spectroscopy (FTIR). It is suggested that FTIR be used as the method for silane lot evaluation. Chromatograms, TGA profiles, bar graphs showing IR absorbances, and FTIR spectra are presented.

Fertilization rates and in vitro embryo production using sexed or non-sexed semen selected with a silane-coated silica colloid or Percoll.

PubMed

Rodríguez Villamil, P; Wei, H; Moreira, G; Caccia, M; Fernandez Taranco, M; Bó, G A

2012-07-01

The aim of this study was to evaluate sperm fertilization rates and in vitro embryo development rates for sexed and non-sexed semen selected using a silane-coated silica colloid method (Isolate) or Percoll. Frozen/thawed, sexed and unsexed semen samples from four Holstein bulls were randomly allocated to one of two different density gradient selection methods. Sperm quality (motility, concentration, morphology and membrane integrity) were evaluated and compared before and after sperm selection. Sperm motility and morphology improved (P < 0.005) after the sperm selection process with no differences between the two methods. For non-sexed semen, Percoll gradient increased the mean (± SEM) percentage of sperm recovered (57.3 ± 2.8) compared to Isolate (46.0 ± 1.8; P < 0.01). However, membrane integrity was higher after Isolate than Percoll (sexed semen: 41.0 ± 0.6 vs. 38.8 ± 0.8 and non-sexed semen 60.8 ± 1.6 vs. 58.8 ± 0.5; P < 0.05). The percentage of blastocysts produced was higher when either sexed or non-sexed semen was selected by Isolate (14.0 ± 1.0; 22.0 ± 1.1) than by Percoll (10.5 ± 1.5; 17.0 ± 2.1, respectively; P < 0.05). In summary, Isolate was a more effective method for the recovery of high quality sperm for in vitro fertilization embryo production. Copyright © 2012 Elsevier Inc. All rights reserved.

Synthesis of a novel hydantoin-containing silane and its effect on the tracking and bacteria resistance of addition-cure liquid silicone rubber

NASA Astrophysics Data System (ADS)

Liu, Tian; Zeng, Xingrong; Fang, Weizhen; Lai, Xuejun; Li, Hongqiang

2017-11-01

A novel hydantoin-containing silane, [3-(5,5-dimethylhydantoinurethano) propyl] ethoxyallyloxysilane (DMHURPAS), was synthesized and the structure was characterized by FTIR and 1H NMR. The effect of DMHURPAS was investigated on the anti-tracking and antibacterial properties of addition-cure liquid silicone rubber (ALSR) after surface chlorination. It was found that ALSR containing only 1.5 phr of DMHURPAS passed 1A 4.5 kV level and erosion mass decreased from 0.843 g to 0.037 g. The thermal stability of ALSR was significantly improved and the mechanical properties were also enhanced. From thermogravimetry-Fourier transform infrared spectroscopy (TG-FTIR), ALSR/DMHURPAS showed significant decrease of carbonyl compounds and cyclic oligomers but increase of CH4 and CO2 during thermal degradation, indicating that DMHURPAS could inhibit oxidation of methyl groups and unzipping reaction, and promote the cleavage of methyl groups in ALSR. The antibacterial rates of ALSR containing 2.0 phr of DMHURPAS against Escherichia coli and Staphylococcus aureus were 95.7% and 83.4%, respectively.

Purification of silane via laser-induced chemistry

DOEpatents

Clark, John H.; Anderson, Robert G.

1979-01-01

Impurities such as PH.sub.3, AsH.sub.3, and B.sub.2 H.sub.6 may be removed from SiH.sub.4 by means of selective photolysis with ultraviolet radiation of the appropriate wavelength. An ArF laser operating at 193 nm provides an efficient and effective radiation source for the photolysis.

Potential of Silanes for Chromate Replacement in Metal Finishing Industries

DTIC Science & Technology

2002-09-16

POTENTIAL OF SILANES FOR CHROMATE REPLACEMENT IN METAL FINISHING INDUSTRIES Wim J. van Ooij*, Danqing Zhu, Vignesh Palanivel, J. Anna Lamar...18 2 POTENTIAL OF SILANES FOR CHROMATE REPLACEMENT IN METAL FINISHING INDUSTRIES Wim J. van Ooij, Danqing Zhu, Vignesh Palanivel, J. Anna Lamar

Union Carbide Corp. polysilicon status and plans

NASA Technical Reports Server (NTRS)

Leipold, M. H.

1982-01-01

The status of polysilicon activities is summarized highlighted by moving the silane portion of the experimental process system development unit (EPSDU) to Washougal, Washington. The completion and operation of the silane EPSDU, is discussed along with research on the silane-to-silicon deposition process. Progress on the dichlorosilane process is also reported.

Modification of eucalyptus pulp fiber using silane coupling agents with aliphatic side chains of different length

USDA-ARS?s Scientific Manuscript database

The objective of this work was to evaluate the effect of three silane coupling agents with different aliphatic chain lengths on the hydrophobicity of eucalyptus pulp fiber. The three silanes coupling agents used (isobutyltrimethoxysilane, methyltrimethoxysilane, and n-octyltriethoxysilane [OTES]) we...

Review of the potential of silanes as rocket/scramjet fuels

NASA Astrophysics Data System (ADS)

Hidding, Bernhard; Pfitzner, Michael; Simone, Domenico; Bruno, Claudio

2008-07-01

Experimental use as well as theoretical considerations regarding silanes as fuels for spacecrafts and supersonic flight are reviewed. The historical circumstances leading to the utilization of monosilane as a fuel additive for scramjets are highlighted and milestones in the chemical research on silanes are summarized. Recent developments such as the use of monosilane as an ignition aid in the NASA X-43A scramjet flights as well as general progress in silicon hydride research, including liquid higher silanes and the resulting potential for the propulsion field are discussed.

Enhanced diode characteristics of organic solar cell with silanized fluorine doped tin oxide electrode

NASA Astrophysics Data System (ADS)

Sachdeva, Sheenam; Sharma, Sameeksha; Singh, Devinder; Tripathi, S. K.

2018-05-01

To investigate the diode characteristics of organic solar cell based on the planar heterojunction of 4,4'- cyclohexylidenebis[N,N-bis(4-methylphenyl)benzenamine] (TAPC) and fullerene (C70), we report the use of silanized fluorine-doped tin oxide (FTO) anode with N1-(3-trimethoxysilylpropyl)diethyltriamine (DETA) forming monolayer. The use of silanized FTO results in the decrease of saturation current density and diode ideality factor of the device. Such silanized FTO anode is found to enhance the material quality and improve the device properties.

Impact Strength and Flexural Properties Enhancement of Methacrylate Silane Treated Oil Palm Mesocarp Fiber Reinforced Biodegradable Hybrid Composites

PubMed Central

Ibrahim, Nor Azowa; Ariffin, Hidayah; Yunus, Wan Md. Zin Wan

2014-01-01

Natural fiber as reinforcement filler in polymer composites is an attractive approach due to being fully biodegradable and cheap. However, incompatibility between hydrophilic natural fiber and hydrophobic polymer matrix restricts the application. The current studies focus on the effects of incorporation of silane treated OPMF into polylactic acid (PLA)/polycaprolactone (PCL)/nanoclay/OPMF hybrid composites. The composites were prepared by melt blending technique and characterize the composites with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). FTIR spectra indicated that peak shifting occurs when silane treated OPMF was incorporated into hybrid composites. Based on mechanical properties results, incorporation of silane treated OPMF enhances the mechanical properties of unmodified OPMF hybrid composites with the enhancement of flexural and impact strength being 17.60% and 48.43%, respectively, at 10% fiber loading. TGA thermogram shows that incorporation of silane treated OPMF did not show increment in thermal properties of hybrid composites. SEM micrographs revealed that silane treated OPMF hybrid composites show good fiber/matrix adhesion as fiber is still embedded in the matrix and no cavity is present on the surface. Water absorption test shows that addition of less hydrophilic silane treated OPMF successfully reduces the water uptake of hybrid composites. PMID:25254230

Impact strength and flexural properties enhancement of methacrylate silane treated oil palm mesocarp fiber reinforced biodegradable hybrid composites.

PubMed

Eng, Chern Chiet; Ibrahim, Nor Azowa; Zainuddin, Norhazlin; Ariffin, Hidayah; Yunus, Wan Md Zin Wan

2014-01-01

Natural fiber as reinforcement filler in polymer composites is an attractive approach due to being fully biodegradable and cheap. However, incompatibility between hydrophilic natural fiber and hydrophobic polymer matrix restricts the application. The current studies focus on the effects of incorporation of silane treated OPMF into polylactic acid (PLA)/polycaprolactone (PCL)/nanoclay/OPMF hybrid composites. The composites were prepared by melt blending technique and characterize the composites with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). FTIR spectra indicated that peak shifting occurs when silane treated OPMF was incorporated into hybrid composites. Based on mechanical properties results, incorporation of silane treated OPMF enhances the mechanical properties of unmodified OPMF hybrid composites with the enhancement of flexural and impact strength being 17.60% and 48.43%, respectively, at 10% fiber loading. TGA thermogram shows that incorporation of silane treated OPMF did not show increment in thermal properties of hybrid composites. SEM micrographs revealed that silane treated OPMF hybrid composites show good fiber/matrix adhesion as fiber is still embedded in the matrix and no cavity is present on the surface. Water absorption test shows that addition of less hydrophilic silane treated OPMF successfully reduces the water uptake of hybrid composites.

Nanoscale silicon substrate patterns from self-assembly of cylinder forming poly(styrene)-block-poly(dimethylsiloxane) block copolymer on silane functionalized surfaces.

PubMed

Borah, Dipu; Cummins, Cian; Rasappa, Sozaraj; Watson, Scott M D; Pike, Andrew R; Horrocks, Benjamin R; Fulton, David A; Houlton, Andrew; Liontos, George; Ntetsikas, Konstantinos; Avgeropoulos, Apostolos; Morris, Michael A

2017-01-27

Poly(styrene)-block-poly(dimethylsiloxane) (PS-b-PDMS) is an excellent block copolymer (BCP) system for self-assembly and inorganic template fabrication because of its high Flory-Huggins parameter (χ ∼ 0.26) at room temperature in comparison to other BCPs, and high selective etch contrast between PS and PDMS block for nanopatterning. In this work, self-assembly in PS-b-PDMS BCP is achieved by combining hydroxyl-terminated poly(dimethylsiloxane) (PDMS-OH) brush surfaces with solvent vapor annealing. As an alternative to standard brush chemistry, we report a simple method based on the use of surfaces functionalized with silane-based self-assembled monolayers (SAMs). A solution-based approach to SAM formation was adopted in this investigation. The influence of the SAM-modified surfaces upon BCP films was compared with polymer brush-based surfaces. The cylinder forming PS-b-PDMS BCP and PDMS-OH polymer brush were synthesized by sequential living anionic polymerization. It was observed that silane SAMs provided the appropriate surface chemistry which, when combined with solvent annealing, led to microphase segregation in the BCP. It was also demonstrated that orientation of the PDMS cylinders may be controlled by judicious choice of the appropriate silane. The PDMS patterns were successfully used as an on-chip etch mask to transfer the BCP pattern to underlying silicon substrate with sub-25 nm silicon nanoscale features. This alternative SAM/BCP approach to nanopattern formation shows promising results, pertinent in the field of nanotechnology, and with much potential for application, such as in the fabrication of nanoimprint lithography stamps, nanofluidic devices or in narrow and multilevel interconnected lines.

Nanoscale silicon substrate patterns from self-assembly of cylinder forming poly(styrene)-block-poly(dimethylsiloxane) block copolymer on silane functionalized surfaces

NASA Astrophysics Data System (ADS)

Borah, Dipu; Cummins, Cian; Rasappa, Sozaraj; Watson, Scott M. D.; Pike, Andrew R.; Horrocks, Benjamin R.; Fulton, David A.; Houlton, Andrew; Liontos, George; Ntetsikas, Konstantinos; Avgeropoulos, Apostolos; Morris, Michael A.

2017-01-01

Poly(styrene)-block-poly(dimethylsiloxane) (PS-b-PDMS) is an excellent block copolymer (BCP) system for self-assembly and inorganic template fabrication because of its high Flory-Huggins parameter (χ ˜ 0.26) at room temperature in comparison to other BCPs, and high selective etch contrast between PS and PDMS block for nanopatterning. In this work, self-assembly in PS-b-PDMS BCP is achieved by combining hydroxyl-terminated poly(dimethylsiloxane) (PDMS-OH) brush surfaces with solvent vapor annealing. As an alternative to standard brush chemistry, we report a simple method based on the use of surfaces functionalized with silane-based self-assembled monolayers (SAMs). A solution-based approach to SAM formation was adopted in this investigation. The influence of the SAM-modified surfaces upon BCP films was compared with polymer brush-based surfaces. The cylinder forming PS-b-PDMS BCP and PDMS-OH polymer brush were synthesized by sequential living anionic polymerization. It was observed that silane SAMs provided the appropriate surface chemistry which, when combined with solvent annealing, led to microphase segregation in the BCP. It was also demonstrated that orientation of the PDMS cylinders may be controlled by judicious choice of the appropriate silane. The PDMS patterns were successfully used as an on-chip etch mask to transfer the BCP pattern to underlying silicon substrate with sub-25 nm silicon nanoscale features. This alternative SAM/BCP approach to nanopattern formation shows promising results, pertinent in the field of nanotechnology, and with much potential for application, such as in the fabrication of nanoimprint lithography stamps, nanofluidic devices or in narrow and multilevel interconnected lines.

Bioactive glass/polymer composite materials with mechanical properties matching those of cortical bone.

PubMed

Koleganova, Veronika A; Bernier, Suzanne M; Dixon, S Jeffrey; Rizkalla, Amin S

2006-06-01

Stress shielding resulting from mismatch in dynamic mechanical properties contributes to the reduced stability of osseous implants. Our objective was to develop biocompatible composites having mechanical properties similar to those of cortical bone. Polymers of urethane dimethacrylate (UDMA) and 2-hydroxyethyl methacrylate (HEMA, 0-20%) and composites containing bioactive glass particles (70% SiO(2), 25% CaO, and 5% P(2)O(5)), with or without silane treatment were prepared. Young's moduli of composites containing silane-treated glass (16 GPa) were significantly greater than those of composites containing untreated glass (12-13 GPa) or of unfilled polymers (5-6 GPa). Bioactive glass reduced water sorption by the composites and incorporation of silane-treated glass prevented HEMA-induced increases in water sorption. Osteoblast-like cells attached equally well to UDMA polymer and composite containing silane-treated bioactive glass. Thus, silane treatment improved the mechanical properties of bioactive glass composites without compromising biocompatibility. This material has a Young's modulus comparable to that of cortical bone. Therefore, silane-treated bioactive glass composites, when used as implant or cement materials, would reduce stress shielding and improve implant stability.

Effect of Silane Coupling Agent on Tribological Properties of Hemp Fiber-Reinforced Plant-Derived Polyamide 1010 Biomass Composites

PubMed Central

Kajiyama, Tetsuto; Yamanaka, Toshiyuki

2017-01-01

We have studied the effects of silane coupling agents used for the surface treatment of fiber on the tribological properties of hemp fiber (HF) reinforced plant-derived polyamide 1010 (PA1010) biomass composites. Hemp fibers were surface-treated by two surface treatment methods: (a) alkali treatment by sodium hydroxide solution and (b) surface treatment by silane coupling agents. Three types of silane coupling agents, namely aminosilane, epoxysilane and ureidosilane were used. These HF/PA1010 biomass composites were extruded using a twin extruder, and injection-molded. The mechanical and tribological properties were evaluated by the ring-on-plate type sliding wear test. It was found that tribological properties of HF/PA1010 biomass composites improved with the surface treatment by the silane coupling agent. This may be attributed to the change in the mode of friction and wear mechanism by the interfacial adhesion between fiber and matrix polymer according to the type of silane coupling agent used. In particular, the ureidosilane coupling agent showed the best improvement effect for the tribological properties of these biomass composites in this study. PMID:28872624

Aminosilica materials as adsorbents for the selective removal of aldehydes and ketones from simulated bio-oil.

PubMed

Drese, Jeffrey H; Talley, Anne D; Jones, Christopher W

2011-03-21

The fast pyrolysis of biomass is a potential route to the production of liquid biorenewable fuel sources. However, degradation of the bio-oil mixtures due to reaction of oxygenates, such as aldehydes and ketones, reduces the stability of the liquids and can impact long-term storage and shipping. Herein, solid aminosilica adsorbents are described for the selective adsorptive removal of reactive aldehyde and ketone species. Three aminosilica adsorbents are prepared through the reaction of amine-containing silanes with pore-expanded mesoporous silica. A fourth aminosilica adsorbent is prepared through the ring-opening polymerization of aziridine from pore-expanded mesoporous silica. Adsorption experiments with a representative mixture of bio-oil model compounds are presented using each adsorbent at room temperature and 45 °C. The adsorbent comprising only primary amines adsorbs the largest amount of aldehydes and ketones. The overall reactivity of this adsorbent increases with increasing temperature. Additional aldehyde screening experiments show that the reactivity of aldehydes with aminosilicas varies depending on their chemical functionality. Initial attempts to regenerate an aminosilica adsorbent by acid hydrolysis show that they can be at least partially regenerated for further use. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Silane coupling agent for attaching fusion-bonded epoxy to steel.

PubMed

Tchoquessi Diodjo, Madeleine R; Belec, Lénaïk; Aragon, Emmanuel; Joliff, Yoann; Lanarde, Lise; Perrin, François-Xavier

2013-07-24

We describe the possibility of using γ-aminopropyltriethoxysilane (γ-APS) to increase the durability of epoxy powder coating/steel joints. The curing temperature of epoxy powder coatings is frequently above 200 °C, which is seen so far as a major limitation for the use of the heat-sensitive aminosilane coupling agent. Despite this limitation, we demonstrate that aminosilane is a competitive alternative to traditional chromate conversion to enhance the durability of epoxy powder coatings/steel joints. Fourier-transform reflection-absorption infrared spectroscopy (FT-RAIRS), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM) were used to identify the silane deposition conditions that influence the adhesion of epoxy powder coatings on steel. We show that AFM analysis provides highly sensitive measurements of mechanical property development and, as such, the degree of condensation of the silane. The joint durability in water at 60 °C was lower when the pH of the γ-APS solution was controlled at 4.6 using formic acid, rather than that at natural pH (10.6). At the curing temperature of 220 °C, oxidation of the carbon adjacent to the amine headgroup of γ-APS gives amide species by a pseudofirst-order kinetics. However, a few amino functionalities remain to react with oxirane groups of epoxy resin and, thus, strengthen the epoxy/silane interphase. The formation of ammonium formate in the acidic silane inhibits the reaction between silane and epoxy, which consequently decreases the epoxy/silane interphase cohesion. We find that the nanoroughness of silane deposits increases with the cure temperature which is beneficial to the wet stability of the epoxy/steel joints, due to increased mechanical interlocking.

Thermal properties of Bentonite Modified with 3-aminopropyltrimethoxysilane

NASA Astrophysics Data System (ADS)

Pramono, E.; Pratiwi, W.; Wahyuningrum, D.; Radiman, C. L.

2018-03-01

Chemical modifications of Bentonite (BNT) clay have been carried out by using 3-aminoprophyltrimethoxysilane (APS) in various solvent media. The degradation properties of products (BNTAPS) were characterized by thermogravimetric analysis (TGA). Samples were heated at 30 to 700°C with a heating rate 10 deg/min, and the total silane-grafted amount was determined by calculating the weight loss at 200 – 600°C. The thermogram of TGA showed that there were three main decomposition regions which are attributed to the elimination of physically adsorbed water, decomposition of silane and dehydroxylation of Bentonite. High weight loss attributed to the thermal decomposition of silane was observed between 200 to 550°C. Quantitative analysis of grafted silane results high silane loaded using a solvent with high surface energy, which indicates the type of solvent affected interaction and adsorption of APS in BNT platelets.

Palladium nanoparticles deposited on silanized halloysite nanotubes: synthesis, characterization and enhanced catalytic property

NASA Astrophysics Data System (ADS)

Zhang, Yi; He, Xi; Ouyang, Jing; Yang, Huaming

2013-10-01

Palladium (Pd) nanoparticles were deposited on the surface of halloysite nanotubes (HNTs) modified with γ-aminopropyltriethoxysilane (APTES) to produce Pd/NH2-HNTs nanocomposites. The results indicated that Pd nanoparticles were densely immobilized onto NH2-HNTs with an average diameter of ~ 3 nm. The Pd distribution on the surface of silanized HNTs showed much more uniform, and the Pd nanoparticle size became smaller compared with those directly deposited onto HNTs without silanization. Systematic characterization demonstrated that APTES were chemically bonded onto HNTs, and further confirmed the bond formation between Pd and -NH2 groups, which could ensure the firm deposit of Pd nanoparticles on the surface of silanized HNTs. The as-synthesized Pd/NH2-HNTs exhibited an excellent catalytic activity in the liquid-phase hydrogenation of styrene to ethylbenzene with full conversion within 30 min. The mechanism of the deposit of Pd nanoparticles on silanized HNTs was also investigated.

Enhanced corrosion resistance of magnesium alloy by a silane-based solution treatment after an in-situ formation of the Mg(OH)2 layer

NASA Astrophysics Data System (ADS)

Gong, Fubao; Shen, Jun; Gao, Runhua; Xie, Xiong; Luo, Xiong

2016-03-01

A novel organic-inorganic Mg(OH)2/silane surface layer has been developed for corrosion protection of AZ31 magnesium alloy. The results of electrochemical impedance spectroscopy (EIS), the immersion tests, Fourier-transform infrared spectroscopy (FTIR) and sellotape tests showed that the Mg(OH)2/silane-based composite surface layer possessed excellent corrosion resistance and very good adhesion due to the formation of Si-O-Mg bond between Mg(OH)2 layer and silane layer. Electrochemical impedance spectroscopy tests results indicated that for the long-term corrosion protection of AZ31 the increase of the curing temperature improved the impedance of the composited layer when the curing temperature was lower than 130 °С. However, the impedance of the composited layer deceased when the curing temperature was more than 130 °С due to the carbonization of the silane layer.

Development of a new analytical tool for assessing the mutagen 2-methyl-1,4-dinitro-pyrrole in meat products by LC-ESI-MS/MS.

PubMed

Molognoni, Luciano; Daguer, Heitor; de Sá Ploêncio, Leandro Antunes; Yotsuyanagi, Suzana Eri; da Silva Correa Lemos, Ana Lucia; Joussef, Antonio Carlos; De Dea Lindner, Juliano

2018-08-01

The use of sorbate and nitrite in meat processing may lead to the formation of 2-methyl-1,4-dinitro-pyrrole (DNMP), a mutagenic compound. This work was aimed at developing and validating an analytical method for the quantitation of DNMP by liquid chromatography-tandem mass spectrometry. Full validation was performed in accordance to Commission Decision 2002/657/EC and method applicability was checked in several samples of meat products. A simple procedure, with low temperature partitioning solid-liquid extraction, was developed. The nitrosation during the extraction was monitored by the N-nitroso-DL-pipecolic acid content. Chromatographic separation was achieved in 8 min with di-isopropyl-3-aminopropyl silane bound to hydroxylated silica as stationary phase. Samples of bacon and cooked sausage yielded the highest concentrations of DNMP (68 ± 3 and 50 ± 3 μg kg -1 , respectively). The developed method proved to be a reliable, selective, and sensitive tool for DNMP measurements in meat products. Copyright © 2018 Elsevier B.V. All rights reserved.

Tailoring mechanical properties of aerogels for aerospace applications.

PubMed

Randall, Jason P; Meador, Mary Ann B; Jana, Sadhan C

2011-03-01

Silica aerogels are highly porous solid materials consisting of three-dimensional networks of silica particles and are typically obtained by removing the liquid in silica gels under supercritical conditions. Several unique attributes such as extremely low thermal conductivity and low density make silica aerogels excellent candidates in the quest for thermal insulation materials used in space missions. However, native silica aerogels are fragile at relatively low stresses. More durable aerogels with higher strength and stiffness are obtained by proper selection of silane precursors and by reinforcement with polymers. This paper first presents a brief review of the literature on methods of silica aerogel reinforcement and then discusses our recent activities in improving not only the strength but also the elastic response of polymer-reinforced silica aerogels. Several alkyl-linked bis-silanes were used in promoting flexibility of the silica networks in conjunction with polymer reinforcement by epoxy.

Durability and mechanical properties of silane cross-linked wood thermoplastic composites

Treesearch

Magnus Bengtsson; Nicole M. Stark; Kristiina Oksman

2007-01-01

In this study, silane cross-linked wood–polyethylene composite profiles were manufactured by reactive extrusion. These composites were evaluated regarding their durability and mechanical properties in comparison with two non-cross-linked wood– polyethylene composites. An addition of only 2% w/w of silane solution during manufacturing was enough to achieve almost 60%...

The effects of different silane crosslinking approaches on composites of polyethylene blends and wood flour

Treesearch

Craig M. Clemons; Ronald C. Sabo; Kolby C. Hirth

2011-01-01

Though silane chemistry has been used to crosslink unfilled polyethylene for many years, such crosslinking has only been recently applied to wood plastic composites to improve properties such as creep resistance. However, the presence of wood significantly changes the silane chemistry and a greater understanding is necessary for optimal processing and performance. We...

Assessment of corrosion resistance of Nd-Fe-B magnets by silanization for orthodontic applications

NASA Astrophysics Data System (ADS)

Fabiano, F.; Celegato, F.; Giordano, A.; Borsellino, C.; Bonaccorsi, L.; Calabrese, L.; Tiberto, P.; Cordasco, G.; Matarese, G.; Fabiano, V.; Azzerboni, B.

2014-02-01

Nd-Fe-B permanent magnets are characterised by excellent magnetic properties. However, being extremely vulnerable to the attack of both climate and corrosive environments, their applications are limited. This paper describes how, at different thicknesses of N-propyl-trimetoxy-silane, the coating affects the magnetic force of nickel plated magnets. We also investigate if the corrosion resistance of silanized Nd-Fe-B magnets increases in mildly corrosive environments by immersing them in a synthetic saliva solution. It was found that the silanization treatment does not affect the strength of the magnetic force and provide an enhancement of the corrosion resistance of the substrate.

Functionalisation of Detonation Nanodiamond for Monodispersed, Soluble DNA-Nanodiamond Conjugates Using Mixed Silane Bead-Assisted Sonication Disintegration

DOE PAGES

Edgington, Robert; Spillane, Katelyn M.; Papageorgiou, George; ...

2018-01-15

Here, nanodiamonds have many attractive properties that make them suitable for a range of biological applications, but their practical use has been limited because nanodiamond conjugates tend to aggregate in solution during or after functionalisation. Here we demonstrate the production of DNA-detonation nanodiamond (DNA-DND) conjugates with high dispersion and solubility using an ultrasonic, mixed-silanization chemistry protocol based on the in situ Bead-Assisted Sonication Disintegration (BASD) silanization method. We use two silanes to achieve these properties: (1) 3-(trihydroxysilyl)propyl methylphosphonate (THPMP); a negatively charged silane that imparts high zeta potential and solubility in solution; and (2) (3-aminopropyl)triethoxysilane (APTES); a commonly used functionalmore » silane that contributes an amino group for subsequent bioconjugation. We target these amino groups for covalent conjugation to thiolated, single-stranded DNA oligomers using the heterobifunctional crosslinker sulfosuccinimidyl 4-(N-maleimidomethyl)cyclohexane-1-carboxylate (Sulfo-SMCC). The resulting DNA-DND conjugates are the smallest reported to date, as determined by Dynamic Light Scattering (DLS) and Atomic Force Microscopy (AFM). The functionalisation method we describe is versatile and can be used to produce a wide variety of soluble DND-biomolecule conjugates.« less

Mid-Infrared Interferometry on Spectral Lines. III. Ammonia and Silane around IRC +10216 and VY Canis Majoris

NASA Astrophysics Data System (ADS)

Monnier, J. D.; Danchi, W. C.; Hale, D. S.; Tuthill, P. G.; Townes, C. H.

2000-11-01

Using the University of California Berkeley Infrared Spatial Interferometer with a radio frequency (RF) filter bank, the first interferometric observations of mid-infrared molecular absorption features of ammonia (NH3) and silane (SiH4) with very high spectral resolution (λ/Δλ~105) were made. Under the assumptions of spherical symmetry and uniform outflow, these new data permitted the molecular stratification around carbon star IRC +10216 and red supergiant VY CMa to be investigated. For IRC +10216, both ammonia and silane were found to form in the dusty outflow significantly beyond both the dust formation and gas acceleration zones. Specifically, ammonia was found to form before silane in a region of decaying gas turbulence (>~20R*), while the silane is produced in a region of relatively smooth gas flow much farther from the star (>~80R*). The depletion of gas-phase SiS onto grains soon after dust formation may fuel silane-producing reactions on the grain surfaces. For VY CMa, a combination of interferometric and spectral observations suggest that NH3 is forming near the termination of the gas acceleration phase in a region of high gas turbulence (~40R*).

Functionalisation of Detonation Nanodiamond for Monodispersed, Soluble DNA-Nanodiamond Conjugates Using Mixed Silane Bead-Assisted Sonication Disintegration.

PubMed

Edgington, Robert; Spillane, Katelyn M; Papageorgiou, George; Wray, William; Ishiwata, Hitoshi; Labarca, Mariana; Leal-Ortiz, Sergio; Reid, Gordon; Webb, Martin; Foord, John; Melosh, Nicholas; Schaefer, Andreas T

2018-01-15

Nanodiamonds have many attractive properties that make them suitable for a range of biological applications, but their practical use has been limited because nanodiamond conjugates tend to aggregate in solution during or after functionalisation. Here we demonstrate the production of DNA-detonation nanodiamond (DNA-DND) conjugates with high dispersion and solubility using an ultrasonic, mixed-silanization chemistry protocol based on the in situ Bead-Assisted Sonication Disintegration (BASD) silanization method. We use two silanes to achieve these properties: (1) 3-(trihydroxysilyl)propyl methylphosphonate (THPMP); a negatively charged silane that imparts high zeta potential and solubility in solution; and (2) (3-aminopropyl)triethoxysilane (APTES); a commonly used functional silane that contributes an amino group for subsequent bioconjugation. We target these amino groups for covalent conjugation to thiolated, single-stranded DNA oligomers using the heterobifunctional crosslinker sulfosuccinimidyl 4-(N-maleimidomethyl)cyclohexane-1-carboxylate (Sulfo-SMCC). The resulting DNA-DND conjugates are the smallest reported to date, as determined by Dynamic Light Scattering (DLS) and Atomic Force Microscopy (AFM). The functionalisation method we describe is versatile and can be used to produce a wide variety of soluble DND-biomolecule conjugates.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lutwack, R.

The goal of the Silicon Material Task, a part of the FSA Project, was to develop and demonstrate the technology for the low-cost production of silicon of suitable purity to be used as the basic material for the manufacture of terrestrial photovoltaic solar cells. To be compatible with the price goals of the FSA Project, the price of the produced silicon was to be less than $10/kg (in 1975 dollars). Summarized in this document are 11 different processes for the production of silicon that were investigated and developed to varying extent by industrial, university, and government researchers. The silane-production sectionmore » of the Union Carbide Corp. (UCC) silane process was developed completely in this program. Coupled with Siemens-type chemical vapor deposition reactors, the process was carried through the pilot plant stage. The overall UCC process involves the conversion of metallurgical-grade silicon to silane followed by decomposition of the silane to purified silicon. Production of very high-purity silane and silicon was demonstrated. Although it has as yet not achieved commercial application, the development of fluidized-bed technology for the low-cost, high-throughput conversion of silane-to-silicon has been demonstrated in the research laboratory and now is in engineering development.« less

Simple Heat Treatment of Zirconia Ceramic Pre-Treated with Silane Primer to Improve Resin Bonding.

PubMed

Ha, Jung-Yun; Son, Jun Sik; Kim, Kyo-Han; Kwon, Tae-Yub

2015-01-01

Establishing a strong resin bond to dental zirconia ceramic remains difficult. Previous studies have shown that the conventional application of silane does not work well with zirconia. This paper reports that a silane pre-treatment of dental zirconia ceramic combined with subsequent heat treatment has potential as an adhesive cementation protocol for improving zirconia-resin bonding. Among the various concentrations (0.1 to 16 vol%) of experimental γ-methacryloxypropyltrimethoxysilane (γ-MPTS) primers assessed, the 1% solution was found to be the most effective in terms of the shear bond strength of the resin cement to dental zirconia ceramic. A high shear bond strength (approx. 30 MPa) was obtained when zirconia specimens were pre-treated with this primer and then heat-treated in a furnace for 60 min at 150 degrees C. Heat treatment appeared to remove the hydrophilic constituents from the silane film formed on the zirconia ceramic surface and accelerate the condensation reactions between the silanol groups of the hydrolyzed silane molecules at the zirconia/resin interface, finally making a more desirable surface for bonding with resin. This estimation was supported by Fourier transform infrared spectroscopy of the silanes prepared in this study.

Functionalisation of Detonation Nanodiamond for Monodispersed, Soluble DNA-Nanodiamond Conjugates Using Mixed Silane Bead-Assisted Sonication Disintegration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edgington, Robert; Spillane, Katelyn M.; Papageorgiou, George

Here, nanodiamonds have many attractive properties that make them suitable for a range of biological applications, but their practical use has been limited because nanodiamond conjugates tend to aggregate in solution during or after functionalisation. Here we demonstrate the production of DNA-detonation nanodiamond (DNA-DND) conjugates with high dispersion and solubility using an ultrasonic, mixed-silanization chemistry protocol based on the in situ Bead-Assisted Sonication Disintegration (BASD) silanization method. We use two silanes to achieve these properties: (1) 3-(trihydroxysilyl)propyl methylphosphonate (THPMP); a negatively charged silane that imparts high zeta potential and solubility in solution; and (2) (3-aminopropyl)triethoxysilane (APTES); a commonly used functionalmore » silane that contributes an amino group for subsequent bioconjugation. We target these amino groups for covalent conjugation to thiolated, single-stranded DNA oligomers using the heterobifunctional crosslinker sulfosuccinimidyl 4-(N-maleimidomethyl)cyclohexane-1-carboxylate (Sulfo-SMCC). The resulting DNA-DND conjugates are the smallest reported to date, as determined by Dynamic Light Scattering (DLS) and Atomic Force Microscopy (AFM). The functionalisation method we describe is versatile and can be used to produce a wide variety of soluble DND-biomolecule conjugates.« less

Three-body-wear resistance of the experimental composites containing filler treated with hydrophobic silane coupling agents.

PubMed

Nihei, Tomotaro; Dabanoglu, Alp; Teranaka, Toshio; Kurata, Shigeaki; Ohashi, Katsura; Kondo, Yukishige; Yoshino, Norio; Hickel, Reinhard; Kunzelmann, Karl-Heinz

2008-06-01

This paper evaluated the wear resistance of resin composite materials with fillers which were modified with a novel hydrophobic silane coupling agent. The novel silane coupling agent containing hydrophobic phenyl group 3-(3-methoxy-4-methacryloyloxyphenyl)propyltrimethoxysilane (p-MBS) was synthesized. The experimental light-cure hybrid composites containing 85wt% of filler modified with this silane were formulated. Twelve specimens were prepared for the three-body-wear test with the ACTA machine and the collected data were analyzed statistically using a one-way ANOVA and Tukey's multiple comparison test as the post hoc test. The wear of the composites containing fillers treated with p-MBS was significantly lower compared with the composite materials containing fillers pretreated with 3-methacryloyloxypropyltrimethoxysilane or the commercially composites (AP-X and ELS extra low shrinkage) after a wear test for 200,000 cycles (p<0.05). It is suggested that the resin composites containing fillers modified with the novel hydrophobic silane has high wear resistant, because of the coupling layers treated with this silane had an excellent affinity with the base resin and formed a highly hydrophobic layer on the filler surface.

Surface modification of poly(dimethylsiloxane) for microfluidic assay applications

NASA Astrophysics Data System (ADS)

Séguin, Christine; McLachlan, Jessica M.; Norton, Peter R.; Lagugné-Labarthet, François

2010-02-01

The surface of a poly(dimethylsiloxane) (PDMS) film was imparted with patterned functionalities at the micron-scale level. Arrays of circles with diameters of 180 and 230 μm were functionalized using plasma oxidation coupled with aluminum deposition, followed by silanization with solutions of 3-aminopropyltrimethoxy silane (3-APTMS) and 3-mercaptopropyltrimethoxy silane (3-MPTMS), to obtain patterned amine and thiol functionalities, respectively. The modification of the samples was confirmed using X-ray photoelectron spectroscopy (XPS), gold nanoparticle adhesion coupled with optical microscopy, as well as by derivatization with fluorescent dyes. To further exploit the novel surface chemistry of the modified PDMS, samples with surface amine functionalities were used to develop a protein assay as well as an array capable of cellular capture and patterning. The modified substrate was shown to successfully selectively immobilize fluorescently labeled immunoglobulin G (IgG) by tethering Protein A to the surface, and, for the cellular arrays, C2C12 rat endothelial cells were captured. Finally, this novel method of patterning chemical functionalities onto PDMS has been incorporated into microfluidic channels. Finally, we demonstrate the in situ chemical modification of the protected PDMS oxidized surface within a microfluidic device. This emphasizes the potential of our method for applications involving micron-scale assays since the aluminum protective layer permits to functionalize the oxidized PDMS surface several weeks after plasma treatment simply after etching away the metallic thin film.

The ignition delay times of hydrogen/silan/air mixtures at low temperatures

NASA Astrophysics Data System (ADS)

Tropin, D. A.; Bochenkov, E. S.; Fedorov, A. V.

2018-03-01

In the paper the ignition delay times of hydrogen-silane-air mixtures at low pressures from 0.4 atm to 1 atm and mixture temperatures from 300 K to 900 K using the detailed kinetic mechanisms were calculated. It was shown that dependencies of ignition delay time on temperature are non-monotonic. In these dependences a region of "negative temperature coefficient" is presented. The effect of the mixture pressure and the silane concentration in the mixture on the length of this region was revealed. It was shown that the increasing of the silane concentration in the mixture, as well as the increasing the mixture pressure, leads to increasing of the "negative temperature coefficient" region length.

Low cost silicon solar array project: Feasibility of low-cost, high-volume production of silane and pyrolysis of silane to semiconductor-grade silicon

NASA Technical Reports Server (NTRS)

Breneman, W. C.

1978-01-01

Silicon epitaxy analysis of silane produced in the Process Development Unit operating in a completely integrated mode consuming only hydrogen and metallurgical silicon resulted in film resistivities of up to 120 ohms cm N type. Preliminary kinetic studies of dichlorosilane disproportionation in the liquid phase have shown that 11.59% SiH4 is formed at equilibrium after 12 minutes contact time at 56 C. The fluid-bed reactor was operated continuously for 48 hours with a mixture of one percent silane in helium as the fluidizing gas. A high silane pyrolysis efficiency was obtained without the generation of excessive fines. Gas flow conditions near the base of the reactor were unfavorable for maintaining a bubbling bed with good heat transfer characteristics. Consequently, a porous agglomerate formed in the lower portion of the reactor. Dense coherent plating was obtained on the silicon seed particles which had remained fluidizied throughout the experiment.

Thermal reactor. [liquid silicon production from silane gas

NASA Technical Reports Server (NTRS)

Levin, H.; Ford, L. B. (Inventor)

1982-01-01

A thermal reactor apparatus and method of pyrolyticaly decomposing silane gas into liquid silicon product and hydrogen by-product gas is disclosed. The thermal reactor has a reaction chamber which is heated well above the decomposition temperature of silane. An injector probe introduces the silane gas tangentially into the reaction chamber to form a first, outer, forwardly moving vortex containing the liquid silicon product and a second, inner, rewardly moving vortex containing the by-product hydrogen gas. The liquid silicon in the first outer vortex deposits onto the interior walls of the reaction chamber to form an equilibrium skull layer which flows to the forward or bottom end of the reaction chamber where it is removed. The by-product hydrogen gas in the second inner vortex is removed from the top or rear of the reaction chamber by a vortex finder. The injector probe which introduces the silane gas into the reaction chamber is continually cooled by a cooling jacket.

Palladium nanoparticles deposited on silanized halloysite nanotubes: synthesis, characterization and enhanced catalytic property

PubMed Central

Zhang, Yi; He, Xi; Ouyang, Jing; Yang, Huaming

2013-01-01

Palladium (Pd) nanoparticles were deposited on the surface of halloysite nanotubes (HNTs) modified with γ-aminopropyltriethoxysilane (APTES) to produce Pd/NH2-HNTs nanocomposites. The results indicated that Pd nanoparticles were densely immobilized onto NH2-HNTs with an average diameter of ~ 3 nm. The Pd distribution on the surface of silanized HNTs showed much more uniform, and the Pd nanoparticle size became smaller compared with those directly deposited onto HNTs without silanization. Systematic characterization demonstrated that APTES were chemically bonded onto HNTs, and further confirmed the bond formation between Pd and -NH2 groups, which could ensure the firm deposit of Pd nanoparticles on the surface of silanized HNTs. The as-synthesized Pd/NH2-HNTs exhibited an excellent catalytic activity in the liquid-phase hydrogenation of styrene to ethylbenzene with full conversion within 30 min. The mechanism of the deposit of Pd nanoparticles on silanized HNTs was also investigated. PMID:24126604

Bond strength of self-adhesive resin cements to composite submitted to different surface pretreatments.

PubMed

Dos Santos, Victor Hugo; Griza, Sandro; de Moraes, Rafael Ratto; Faria-E-Silva, André Luis

2014-02-01

Extensively destroyed teeth are commonly restored with composite resin before cavity preparation for indirect restorations. The longevity of the restoration can be related to the proper bonding of the resin cement to the composite. This study aimed to evaluate the microshear bond strength of two self-adhesive resin cements to composite resin. COMPOSITE DISCS WERE SUBJECT TO ONE OF SIX DIFFERENT SURFACE PRETREATMENTS: none (control), 35% phosphoric acid etching for 30 seconds (PA), application of silane (silane), PA + silane, PA + adhesive, or PA + silane + adhesive (n = 6). A silicone mold containing a cylindrical orifice (1 mm(2) diameter) was placed over the composite resin. RelyX Unicem (3M ESPE) or BisCem (Bisco Inc.) self-adhesive resin cement was inserted into the orifices and light-cured. Self-adhesive cement cylinders were submitted to shear loading. Data were analyzed by two-way ANOVA and Tukey's test (p < 0.05). Independent of the cement used, the PA + Silane + Adhesive group showed higher microshear bond strength than those of the PA and PA + Silane groups. There was no difference among the other treatments. Unicem presented higher bond strength than BisCem for all experimental conditions. Pretreatments of the composite resin surface might have an effect on the bond strength of self-adhesive resin cements to this substrate.

Synthesis of waterborne polyurethane containing alkoxysilane side groups and the properties of the hybrid coating films

NASA Astrophysics Data System (ADS)

Li, Qi; Guo, Longhai; Qiu, Teng; Xiao, Weidong; Du, Dianxing; Li, Xiaoyu

2016-07-01

A series of waterborne polyurethane (WPU) containing alkoxysilane side groups were synthesized by using the dihydroxy functionalized alkoxysilane. The diol with trimethoxysilane groups at the side chains was synthesized via Michael addition between 3-(methacryloxypropyl)trimethoxysilane (MAPTS) and diethanolamine (DEA). The silane diol was applied as the chain extender for the NCO-endcapped prepolymer of isophorone diisocyanate, polycarbonate diol, 2,2-bis(hydroxymethyl) butyric acid and 1,4-butanediol. The products with the silane content varied from 1.2 to 16.5 wt% were dispersed in water after neutralization. The effect of the silane diol on the particle size and morphology of the WPU dispersion was studied by dynamic light scattering (DLS) and transmission electron microscopy (TEM), respectively. X-ray photoelectron spectroscopy (XPS) characterization was carried out on the coating film of the WPU, revealing that the long flexible side chain is favorable for the silane components to emigrate toward the film surface and crosslink during the film formation process. As a result, both the surface contact angle to water and water adsorption of the WPU coating films increased with the silane content. Furthermore, the mechanical properties including the modulus and tensile strength of the films were also improved by the incorporation of silane diol.

Organic-Inorganic Hybrids Using Novel Phenylethynyl Imide Silanes

NASA Technical Reports Server (NTRS)

Park, C.; Lowther, S. E.; Smith, J. G., Jr.

2001-01-01

In this presentation, polyimide-silica hybrids using novel phenylethynyl imide silanes are reported. The phenylethynyl group is present in the organic precursor as either a pendent or an end group to bond chemically with the polyimide adhesive containing phenylethynyl groups during processing, while the silane group of the organic precursor would chemically react with the inorganic precursor through oxane bond formation. The chemical compositions of these novel hybrids were examined using X-ray mapping modes of scanning electron microscopy (SEM), which revealed a silicon gradient interphase between the high surface energy substrate and the polyimide adhesive. Novel aromatic phenylethynyl imide silanes (APEISs) and pendent phenylethynyl imide oligomeric disilanes (PPEIDSs) have been synthesized, and sol-gel solutions containing the new silanes, a phenylethynyl terminated imide oligomer (PETI-5), and an inorganic precursor were formulated to develop a gradient hybrid interphase between a titanium alloy and the adhesive. Two different sol-gel systems were investigated to develop organic-inorganic hybrids. Hybrid I was composed of an organic precursor containing both phenylethynyl and silane groups (PPEIDS) and an inorganic precursor. Functional group concentrations were controlled by the variation of the molecular weight of the imide backbone of PPEIDS. Hybrid II was composed of organic and inorganic precursors and a coupling agent containing both phenylethynyl and silane groups. Morphology and chemical composition of the hybrid interphase between the inorganic substrate and the adhesive were investigated, and the bond strength and durability were evaluated using lap shear tests at various conditions. The assessment of how the bonding at an interface is affected by various sol-gel solution compositions and environments is reported.

Synthesis and Characterization of a Novel Reactive Perfluorinated Alkynyl Silane Monomer

DTIC Science & Technology

2010-10-21

8217 For practical purposes, alkoxy- and th loro-silanes arc the most convenient precurwrs to alkynylsilanes because an alkynyl Grignard or lith ium reagent ...of alkoxy silanes has been accomplished by the treatment of Grignard or organa-lithium reagents with eithet" SiC!.. (followed by alcoholysis)," CI_Si...procedure. Grignard reagents nave been rc:poncd to have significantly lowcr re~ctivity than the litbium rcagents, wbicb rapidly decompose at ambient

Polyfibroblast: A Self-Healing and Galvanic Protection Additive

DTIC Science & Technology

2011-06-27

Isocyanatopropyltrimethoxy silane (ITS): This silane forms a covalent bond with both the oxide layer of the underlying steel and the polyurea resin released from the...group that can react with amines in the polyurea to form a covalent bond. The fact that it reacts more slowly than ITS makes it easier to process, but...it may take longer to develop stronger adhesion with the polyurea scar. • Methacryloxypropyltrimethoxy silane (MPTMS): With an exposed vinyl group

Structure and electrochemical behaviour of 4,7-diazaheptyl-trimethoxy-silane and vinyl-trialkoxy-silane adsorbed at silver surface

NASA Astrophysics Data System (ADS)

Łuczak, Teresa; Pankiewicz, Radosław; Łęska, Bogusława; Schroeder, Grzegorz; Bełtowska-Brzezinska, Maria; Brzezinski, Bogumil

2006-12-01

Novel self-assembled monolayers were obtained on silver using 4,7-diazaheptyl-trimethoxy-silane (SiN) and vinyl-trialkoxy-silane (SiVA, where the alkyl group is 3,6,9,12,15,18,21,24,27,30,33,36,39,42,45,48,51,54,57,60-eicozaoxa- hexaheptaconan). It was shown that thus modified metal surface was protected against electrooxidation. A densely packed monolayer remained stable and did not desorb from the Ag electrode on the potential cycling. The structure of SiN and SiVA as well as their complexes with Li + cations were calculated and visualised by the AM1d and PM5 semi-empirical methods.

Chemical modification of TiO2 surfaces with methylsilanes and characterization by infrared absorption spectroscopy

NASA Technical Reports Server (NTRS)

Finklea, H. O.; Vithanage, R.

1982-01-01

Infrared absorption spectra of methylsilanes bonded to a TiO2 powder were obtained. The reacting silanes include Me sub (4-n)SiX sub n (n=1-4; X=Cl, OMe) and hexamethyldisilazane (HMDS). Reactions were performed on hydroxylated-but-anhydrous TiO2 surfaces in the gas phase. IR spectra confirm the presence of a bonded silane layer. Terminal surface OH groups are found to react more readily than bridging OH groups. By-products of the modification adsorp tenaciously to the surface. The various silanes show only small differences in their ability to sequester surface OH groups. Following hydrolysis in moist air, Si-OH groups are observed only for the tetrafunctional silanes.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Addleman, Raymond S; Atkinson, David A; Bays, John T

An enhanced swipe sampler and method of making are described. The swipe sampler is made of a fabric containing selected glass, metal oxide, and/or oxide-coated glass or metal fibers. Fibers are modified with silane ligands that are directly attached to the surface of the fibers to functionalize the sampling surface of the fabric. The swipe sampler collects various target analytes including explosives and other threat agents on the surface of the sampler.

Extraterrestrial materials processing and construction. [space industrialization

NASA Technical Reports Server (NTRS)

Criswell, D. R.; Waldron, R. D.; Mckenzie, J. D.

1980-01-01

Three different chemical processing schemes were identified for separating lunar soils into the major oxides and elements. Feedstock production for space industry; an HF acid leach process; electrorefining processes for lunar free metal and metal derived from chemical processing of lunar soils; production and use of silanes and spectrally selective materials; glass, ceramics, and electrochemistry workshops; and an econometric model of bootstrapping space industry are discussed.

Process for selective monoaddition to silanes containing two silicon-hydrogen bonds and products thereof

NASA Technical Reports Server (NTRS)

Crivello, James V. (Inventor)

1996-01-01

A process for the selective monoadditon of an olefin or acetylene to a siloxane which contains two reactive Si--H bonds to produce a product in which only one of the two Si--H functions has added across the olefin or acetylene is disclosed. A process for making unsymmetrical siloxanes from symmetrical dihydrosiloxanes and products of both of these processes are also disclosed. Products are represented by the formula I in which R.sup.1 and R.sup.4 are different: ##STR1##.

Effect of indirect composite treatment microtensile bond strength of self-adhesive resin cements

PubMed Central

Escribano, Nuria; Baracco, Bruno; Romero, Martin; Ceballos, Laura

2016-01-01

Background No specific indications about the pre-treatment of indirect composite restorations is provided by the manufacturers of most self-adhesive resin cements. The potential effect of silane treatment to the bond strength of the complete tooth/indirect restoration complex is not available.The aim of this study was to determine the contribution of different surface treatments on microtensile bond strength of composite overlays to dentin using several self-adhesive resin cements and a total-etch one. Material and Methods Composite overlays were fabricated and bonding surfaces were airborne-particle abraded and randomly assigned to two different surface treatments: no treatment or silane application (RelyX Ceramic Primer) followed by an adhesive (Adper Scotchbond 1 XT). Composite overlays were luted to flat dentin surfaces using the following self-adhesive resin cements: RelyX Unicem, G-Cem, Speedcem, Maxcem Elite or Smartcem2, and the total-etch resin cement RelyX ARC. After 24 h, bonded specimens were cut into sticks 1 mm thick and stressed in tension until failure. Two-way ANOVA and SNK tests were applied at α=0.05. Results Bond strength values were significantly influenced by the resin cement used (p<0.001). However, composite surface treatment and the interaction between the resin cement applied and surface treatment did not significantly affect dentin bond strength (p>0.05). All self-adhesive resin cements showed lower bond strength values than the total-etch RelyX ARC. Among self-adhesive resin cements, RelyX Unicem and G-Cem attained statistically higher bond strength values. Smartcem2 and Maxcem Elite exhibited 80-90% of pre-test failures. Conclusions The silane and adhesive application after indirect resin composite sandblasting did not improve the bond strength of dentin-composite overlay complex. Selection of the resin cement seems to be a more relevant factor when bonding indirect composites to dentin than its surface treatment. Key words:Bond strength, self-adhesive cement, silane, dentin, indirect composite. PMID:26855700

Propulsion/ASME Rocket-Based Combined Cycle Activities in the Advanced Space Transportation Program Office

NASA Technical Reports Server (NTRS)

Hueter, Uwe; Turner, James

1998-01-01

NASA's Office Of Aeronautics and Space Transportation Technology (OASTT) has establish three major coals. "The Three Pillars for Success". The Advanced Space Transportation Program Office (ASTP) at the NASA's Marshall Space Flight Center in Huntsville,Ala. focuses on future space transportation technologies under the "Access to Space" pillar. The Advanced Reusable Technologies (ART) Project, part of ASTP, focuses on the reusable technologies beyond those being pursued by X-33. The main activity over the past two and a half years has been on advancing the rocket-based combined cycle (RBCC) technologies. In June of last year, activities for reusable launch vehicle (RLV) airframe and propulsion technologies were initiated. These activities focus primarily on those technologies that support the year 2000 decision to determine the path this country will take for Space Shuttle and RLV. In February of this year, additional technology efforts in the reusable technologies were awarded. The RBCC effort that was completed early this year was the initial step leading to flight demonstrations of the technology for space launch vehicle propulsion. Aerojet, Boeing-Rocketdyne and Pratt & Whitney were selected for a two-year period to design, build and ground test their RBCC engine concepts. In addition, ASTROX, Pennsylvania State University (PSU) and University of Alabama in Huntsville also conducted supporting activities. The activity included ground testing of components (e.g., injectors, thrusters, ejectors and inlets) and integrated flowpaths. An area that has caused a large amount of difficulty in the testing efforts is the means of initiating the rocket combustion process. All three of the prime contractors above were using silane (SiH4) for ignition of the thrusters. This follows from the successful use of silane in the NASP program for scramjet ignition. However, difficulties were immediately encountered when silane (an 80/20 mixture of hydrogen/silane) was used for rocket ignition.

Effect of incorporation of silane in the bonding agent on the repair potential of machinable esthetic blocks

PubMed Central

Zaghloul, Hanaa; Elkassas, Dina Wafik; Haridy, Mohamed Fouad

2014-01-01

Objective: To investigate the repair potential of CAD/CAM (computer-aided design/computer-aided manufacturing) ceramic and composite blocks using a silane-containing bonding agent with different repair protocols. Materials and Methods: Twenty-four discs were constructed from CAD/CAM ceramic and composite blocks. The discs were divided into six groups according to surface pre-treatment employed; GI: Diamond stone roughening (SR), GII: SR+ silanization (SR+S), GIII: Hydrofluoric acid etching (HF), GIV: HF+ silanization (HF+S), GV: Silica coating (SC), GVI: SC+ silanization (SC+S). Silane-containing bonding agent (Single Bond Universal adhesive, 3M ESPE) was applied to the pre-treated discs. Prior to light curing, irises were cut from tygon tubes (internal diameter = 0.8 mm and height = 0.5 mm) and mounted on each treated surface. Nanofilled resin composite (Filtek Z350XT, 3M ESPE) was packed into the cylinder lumen and light-cured (n = 10). The specimens were subjected to microshear bond strength testing (μ-SBS) using universal testing machine. Failure modes of the fractured specimens were analyzed using field emission scanning electron microscope (FESEM). Eight representative discs were prepared to analyze the effect of surface treatments on surface topography using FESEM. μ-SBS results were analyzed using ANOVA and Tukeys post-hoc test. Results: Three-way ANOVA results showed that the materials, surface pre-treatment protocols, and silanization step had a statistically significant effect on the mean μ-SBS values at P ≤ 0.001. For ceramic discs, the groups were ranked; GIV (24.45 ± 7.35)> GVI ((20.18 ± 2.84)> GV (7.14 ± 14)= GII (6.72 ± 1.91)=GI (6.34 ± 2.21)=GIII (5.72 ± 2.18). For composite discs, groups were ranked; GI (24.98 ± 7.69)=GVI (24.84 ± 7.00) >GII (15.85 ± 5.29) =GV (14.65 ± 4.5)= GIV (14.24 ± 2.95)≥ GIII ((9.37 ± 2.78). Conclusion: The additional silanization step cannot be omitted if the repair protocol comprises of either hydrofluoric acid etching or silica coating for both CAD/CAM esthetic restorative materials. However, this step can be suppressed by using silane-containing adhesive with diamond stone roughened repair protocol. PMID:24966745

Poly(silyl silane) homo and copolymers

DOEpatents

Zeigler, J.K.

1991-08-13

Poly(silyl silanes) have been prepared. They have high photosensitivity and excellent resistance to oxygen-reactive ion etching processes. They are useful as photodepolymerizable photoresists, barrier layers, etc.

Does 8-methacryloxyoctyl trimethoxy silane (8-MOTS) improve initial bond strength on lithium disilicate glass ceramic?

PubMed

Maruo, Yukinori; Nishigawa, Goro; Yoshihara, Kumiko; Minagi, Shogo; Matsumoto, Takuya; Irie, Masao

2017-03-01

Dental ceramic surfaces are modified with silane coupling agents, such as γ-methacryloxypropyl trimethoxy silane (γ-MPTS), to improve bond strength. For bonding between lithium disilicate glass ceramic and resin cement, the objective was to investigate if 8-methacryloxyoctyl trimethoxy silane (8-MOTS) could yield a similar performance as the widely used γ-MPTS. One hundred and ten lithium disilicate glass ceramic specimens were randomly divided into 11 groups (n=10) according to pretreatment regime. All specimens were pretreated with a different solution composed of one or a combination of these agents: 10 or 20wt% silane coupling agent of γ-MPTS or 8-MOTS, followed by a hydrolysis solution of acetic acid or 10-methacryloyloxydecyl dihydrogen phosphate (10-MDP). Each pretreated surface was luted to a stainless steel rod of 3.6mm diameter and 2.0mm height with resin cement. Shear bond strength between ceramic and cement was measured after 24-h storage in 37°C distilled water. 8-MOTS produced the same bonding performance as γ-MPTS. Both silane coupling agents significantly increased the bond strength of resin cement, depending on their concentration. When activated by 10-MDP hydrolysis solution, 20wt% concentration produced the highest values (γ-MPTS: 24.9±5.1MPa; 8-MOTS: 24.6±7.4MPa). Hydrolysis with acetic acid produced lower bond strengths than with 10-MDP. Silane coupling pretreatment with 8-MOTS increased the initial bond strength between lithium disilicate glass ceramic and resin cement, rendering the same bonding effect as the conventional γ-MPTS. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effectiveness and stability of silane coupling agent incorporated in 'universal' adhesives.

PubMed

Yoshihara, Kumiko; Nagaoka, Noriyuki; Sonoda, Akinari; Maruo, Yukinori; Makita, Yoji; Okihara, Takumi; Irie, Masao; Yoshida, Yasuhiro; Van Meerbeek, Bart

2016-10-01

For bonding indirect restorations, some 'universal' adhesives incorporate a silane coupling agent to chemically bond to glass-rich ceramics so that a separate ceramic primer is claimed to be no longer needed. With this work, we investigated the effectiveness/stability of the silane coupling function of the silanecontaining experimentally prepared adhesives and Scotchbond Universal (3MESPE). Experimental adhesives consisted of Scotchbond Universal and the silane-free Clearfil S3 ND Quick (Kuraray Noritake) mixed with Clearfil Porcelain Bond Activator (Kuraray Noritake) and the two adhesives to which γ-methacryloxypropyltrimethoxysilane (γ-MPTS) was added. Shear bond strength was measured onto silica-glass plates; the adhesive formulations were analyzed using fourier transform infrared spectroscopy (FTIR) and 13C nuclear magnetic resonance (NMR). In addition, shear bond strength onto CAD-CAM composite blocks was measured without and after thermo-cycling ageing. A significantly higher bond strength was recorded when Clearfil Porcelain Bond Activator was freshly mixed with the adhesive. Likewise, the experimental adhesives, to which γ-MPTS was added, revealed a significantly higher bond strength, but only when the adhesive was applied immediately after mixing; delayed application resulted in a significantly lower bond strength. FTIR and (13)C NMR revealed hydrolysis and dehydration condensation to progress with the time after γ-MPTS was mixed with the two adhesives. After thermo-cycling, the bond strength onto CAD-CAM composite blocks remained stable only for the two adhesives with which Clearfil Porcelain Bond Activator was mixed. Only the silane coupling effect of freshly prepared silanecontaining adhesives was effective. Clinically, the use of a separate silane primer or silane freshly mixed with the adhesive remains recommended to bond glass-rich ceramics. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Internal coating of zirconia restoration with silica-based ceramic improves bonding of resin cement to dental zirconia ceramic.

PubMed

Kitayama, Shuzo; Nikaido, Toru; Ikeda, Masaomi; Alireza, Sadr; Miura, Hiroyuki; Tagami, Junji

2010-01-01

Resin bonding to zirconia ceramic cannot be established by standard methods that are utilized for conventional silica-based dental ceramics. This study was aimed to examine the tensile bond strength of resin cement to zirconia ceramic using a new laboratory technique. Sixty-four zirconia ceramic specimens were air-abraded using Al2O3 particles and divided into two groups; the control group with no pretreatment (Control), and the group pretreated using the internal coating technique (INT), in which the surface of the zirconia specimens were thinly coated by fusing silica-based ceramic and air-abraded in the same manner. The specimens in each group were further divided into two subgroups according to the silane coupling agents applied; a mixture of dentin primer/silane coupling agent (Clearfil SE Bond Primer/Porcelain Bond Activator) or a newly developed single-component silane coupling agent (Clearfil Ceramic Primer). After bonding with dual-cured resin cement (Panavia F 2.0), they were stored in water for 24 h and half of them were additionally subjected to thermal cycling. The tensile bond strengths were tested using a universal testing machine. ANOVAs revealed significant influence of ceramic surface pretreatment (p<0.001), silane coupling agent (p<0.001) and thermal cycling (p<0.001); the INT coating technique significantly increased the bond strengths of resin cement to zirconia ceramic, whereas thermal cycling significantly decreased the bond strengths. The use of a single-component silane coupling agent demonstrated significantly higher bond strengths than that of a mixture of dentin primer/silane coupling agent. The internal coating of zirconia dental restorations with silica-based ceramic followed by silanization may be indicated in order to achieve better bonding for the clinical success.

Poly(silyl silane)homo and copolymers

DOEpatents

Zeigler, J.M.

1989-04-11

Poly(silyl silanes) have been prepared. They have high photosensitivity and show excellent resistance to oxygen-reactive ion etching processes. They are useful as photodepolymerizable photoresists, barrier layers, etc.

Structuring unbreakable hydrophobic barriers in paper

NASA Astrophysics Data System (ADS)

Nargang, Tobias M.; Kotz, Frederik; Rapp, Bastian E.

2018-02-01

Hydrophobic barriers are one of the key elements of microfluidic paper based analytical devices (μPADs).μPADs are simple and cost efficient and they can be carried out without the need of high standard laboratories. To carry out such a test a method is needed to create stable hydrophobic barriers. Commonly used methods like printing wax or polystyrene have the major drawback that these barriers are stiff and break if bended which means they will no longer be able to retain a liquid sample. Here we present silanes to structure hydrophobic barriers via polycondensation and show a silanization method which combines the advantages of flexible silane/siloxane layers with the short processing times of UV-light based structuring. The barriers are created by using methoxy silanes which are mixed with a photo acid generator (PAG) as photoinitiator. Also a photosensitizer was given to the mixture to increase the effectiveness of the PAG. After the PAG is activated by UV-light the silane is hydrolyzed and coupled to the cellulose via polycondensation. The created hydrophobic barriers are highly stable and do not break if being bended.

Nano-hybrid carboxymethyl-hexanoyl chitosan modified with (3-aminopropyl)triethoxysilane for camptothecin delivery.

PubMed

Hsiao, Meng-Hsuan; Tung, Tsan-Hua; Hsiao, Chi-Sheng; Liu, Dean-Mo

2012-06-20

Silane-modified amphiphilic chitosan was synthesized by anchoring a silane coupling agent, (3-aminopropyl)triethoxysilane, to a novel amphiphilic carboxymethyl-hexanoyl chitosan (CHC). The chemical structure of this new organic-inorganic hybrid molecule was characterized by FTIR and 13C-, 29Si-nuclear magnetic resonance, while the structural evolution was examined using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and dynamic light scattering (DLS). Experimental results indicated a self-assembly behaviour of molecules into nanoparticles with a stable polygonal geometry, consisting of ordered silane layers of 6 nm in thickness. The self-assembly property was found to be influenced by chemical composition and concentration of silane incorporated, while the size can be varied by the amount of anchored silane. It was also demonstrated that such vesicle exhibited excellent cytocompatibility and cellular internalization capability in ARPE-19 cell line, and presented well-controlled encapsulation and release profiles for (S)-(+)-camptothecin. These unique properties render it as a potential drug delivery nanosystem. Copyright © 2012 Elsevier Ltd. All rights reserved.

Coating extracellular matrix proteins on a (3-aminopropyl)triethoxysilane-treated glass substrate for improved cell culture.

PubMed

Masuda, Hiro-taka; Ishihara, Seiichiro; Harada, Ichiro; Mizutani, Takeomi; Ishikawa, Masayori; Kawabata, Kazushige; Haga, Hisashi

2014-01-01

We demonstrate that a (3-aminopropyl)triethoxysilane-treated glass surface is superior to an untreated glass surface for coating with extracellular matrix (ECM) proteins when used as a cell culture substrate to observe cell physiology and behavior. We found that MDCK cells cultured on untreated glass coated with ECM removed the coated ECM protein and secreted different ECM proteins. In contrast, the cells did not remove the coated ECM protein when seeded on (3-aminopropyl)triethoxysilane-treated (i.e., silanized) glass coated with ECM. Furthermore, the morphology and motility of cells grown on silanized glass differed from those grown on non-treated glass, even when both types of glass were initially coated with laminin. We also found that cells on silanized glass coated with laminin had higher motility than those on silanized glass coated with fibronectin. Based on our results, we suggest that silanized glass is a more suitable cell culture substrate than conventional non-treated glass when coated by ECM for observations of ECM effects on cell physiology.

Simulated molecular-scale interaction of supercritical fluid mobile and stationary phases.

PubMed

Siders, Paul D

2017-12-08

In supercritical fluid chromatography, molecules from the mobile phase adsorb on the stationary phase. Stationary-phase alkylsilane-terminated silica surfaces might adsorb molecules at the silica, among the silanes, on a silane layer, or in pore space between surfaces. Mobile phases of carbon dioxide, pure and modified with methanol, and stationary phases were simulated at the molecular scale. Classical atomistic force fields were used in Gibbs-ensemble hybrid Monte Carlo calculations. Excess adsorption of pure carbon dioxide mobile phase peaked at fluid densities of 0.002-0.003Å -3 . Mobile phase adsorption from 7% methanol in carbon dioxide peaked at lower fluid density. Methanol was preferentially adsorbed from the mixed fluid. Surface silanes prevented direct interaction of fluid-phase molecules with silica. Some adsorbed molecules mixed with tails of bonded silanes; some formed layers above the silanes. Much adsorption occurred by filling the space between surfaces in the stationary-phase model. The distribution in the stationary phase of methanol molecules from a modified fluid phase varied with pressure. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of surface modification on protein retention and cell proliferation under strain.

PubMed

Dunkers, J P; Lee, H-J; Matos, M A; Pakstis, L M; Taboas, J M; Hudson, S D; Cicerone, M T

2011-07-01

When culturing cells on flexible surfaces, it is important to consider extracellular matrix treatments that will remain on the surface under mechanical strain. Here we investigate differences in laminin deposited on oxidized polydimethylsiloxane (PDMS) with plasma treatment (plasma-only) vs. plasma and aminopropyltrimethoxysilane treatment (silane-linked). We use specular X-ray reflectivity (SXR), transmission electron microscopy (TEM), and immunofluorescence to probe the quantity and uniformity of laminin. The surface coverage of laminin is approximately 45% for the plasma-only and 50% for the silane-linked treatment as determined by SXR. TEM and immunofluorescence reveal additional islands of laminin aggregates on the plasma-only PDMS compared with the relatively smooth and uniform silane-linked laminin surface. We also examine laminin retention under strain and vascular smooth muscle cell viability and proliferation under static and strain conditions. Equibiaxial stretching of the PDMS surfaces shows greatly improved retention of the silane-linked laminin over plasma-only. There are significantly more cells on the silane-linked surface after 4 days of equibiaxial strain. Published by Elsevier Ltd.

Kinetics of (3-aminopropyl)triethoxylsilane (APTES) silanization of superparamagnetic iron oxide nanoparticles.

PubMed

Liu, Yue; Li, Yueming; Li, Xue-Mei; He, Tao

2013-12-10

Silanization of magnetic ironoxide nanoparticles with (3-aminopropyl)triethoxylsilane (APTES) is reported. The kinetics of silanization toward saturation was investigated using different solvents including water, water/ethanol (1/1), and toluene/methanol (1/1) at different reaction temperature with different APTES loading. The nanoparticles were characterized by Fourier transform infrared spectroscopy, vibrating sample magnetometry, transmission electron microscopy, and thermal gravimetric analysis (TGA). Grafting density data based on TGA were used for the kinetic modeling. It is shown that initial silanization takes place very fast but the progress toward saturation is very slow, and the mechanism may involve adsorption, chemical sorption, and chemical diffusion processes. The highest equilibrium grafting density of 301 mg/g was yielded when using toluene/methanol mixture as the solvent at a reaction temperature of 70 °C.

KISS: Kinetics and Structure of Superagglomerates Produced by Silane and Acetylene

NASA Technical Reports Server (NTRS)

Mulholland, G. W.; Yang, J. C.; Scott, J. H.; Sivithanu, Y.

2001-01-01

The objective of this study is to understand the process of gas phase agglomeration leading to superagglomerates and a gel-like structure for microgravity (0-g) silane and acetylene flames. Ultimately one would apply this understanding to predicting flame conditions that could lead to the gas phase production of an aero-gel. The approach is to burn acetylene and silane and to analyze the evolution of the soot and silica agglomerates. Acetylene is chosen because it has one of the highest soot volume fractions and there is evidence of super agglomerates being formed in laminar acetylene flames. Silane has the advantage that silica particles are the major combustion product resulting in a particle volume fraction a factor of ten greater than that for a carbonaceous smoke.

A comparative study of in-flow and micro-patterning biofunctionalization protocols for nanophotonic silicon-based biosensors.

PubMed

González-Guerrero, Ana Belén; Alvarez, Mar; García Castaño, Andrés; Domínguez, Carlos; Lechuga, Laura M

2013-03-01

Reliable immobilization of bioreceptors over any sensor surface is the most crucial step for achieving high performance, selective and sensitive biosensor devices able to analyze human samples without the need of previous processing. With this aim, we have implemented an optimized scheme to covalently biofunctionalize the sensor area of a novel nanophotonic interferometric biosensor. The proposed method is based on the ex-situ silanization of the silicon nitride transducer surface by the use of a carboxyl water soluble silane, the carboxyethylsilanetriol sodium salt (CTES). The use of an organosilane stable in water entails advantages in comparison with usual trialkoxysilanes such as avoiding the generation of organic waste and leading to the assembly of compact monolayers due to the high dielectric constant of water. Additionally, cross-linking is prevented when the conditions (e.g. immersion time, concentration of silane) are optimized. This covalent strategy is followed by the bioreceptor linkage on the sensor area surface using two different approaches: an in-flow patterning and a microcontact printing using a biodeposition system. The performance of the different bioreceptor layers assembled is compared by the real-time and label-free immunosensing of the proteins BSA/mAb BSA, employed as a model molecular pair. Although the results demonstrated that both strategies provide the biosensor with a stable biological interface, the performance of the bioreceptor layer assembled by microcontact printing slightly improves the biosensing capabilities of the photonic biosensor. Copyright © 2012 Elsevier Inc. All rights reserved.

Studies on the effects of titanate and silane coupling agents on the performance of poly (methyl methacrylate)/barium titanate denture base nanocomposites.

PubMed

Elshereksi, Nidal W; Ghazali, Mariyam J; Muchtar, Andanastuti; Azhari, Che H

2017-01-01

This study aimed to fabricate and characterise silanated and titanated nanobarium titanate (NBT) filled poly(methyl methacrylate) (PMMA) denture base composites and to evaluate the behaviour of a titanate coupling agent (TCA) as an alternative coupling agent to silane. The effect of filler surface modification on fracture toughness was also studied. Silanated, titanated and pure NBT at 5% were incorporated in PMMA matrix. Neat PMMA matrix served as a control. NBT was sonicated in MMA prior to mixing with the PMMA. Curing was carried out using a water bath at 75°C for 1.5h and then at 100°C for 30min. NBT was characterised via Fourier transform-infrared spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Brunauer-Emmett-Teller (BET) analysis before and after surface modification. The porosity and fracture toughness of the PMMA nanocomposites (n=6, for each formulation and test) were also evaluated. NBT was successfully functionalised by the coupling agents. The TCA exhibited the lowest percentage of porosity (0.09%), whereas silane revealed 0.53% porosity. Statistically significant differences in fracture toughness were observed among the fracture toughness values of the tested samples (p<0.05). While the fracture toughness of untreated samples was reduced by 8%, an enhancement of 25% was achieved after titanation. In addition, the fracture toughness of the titanated samples was higher than the silanated ones by 10%. Formation of a monolayer on the surface of TCA enhanced the NBT dispersion, however agglomeration of silanated NBT was observed due to insufficient coverage of NBT surface. Such behaviour led to reducing the porosity level and improving fracture toughness of titanated NBT/PMMA composites. Thus, TCA seemed to be more effective than silane. Minimising the porosity level could have the potential to reduce fungus growth on denture base resin to be hygienically accepTable Such enhancements obtained with Ti-NBT could lead to promotion of the composites' longevity. Copyright © 2016 Elsevier Ltd. All rights reserved.

Lanthanum tricyanide-catalyzed acyl silane-ketone benzoin additions.

PubMed

Tarr, James C; Johnson, Jeffrey S

2009-09-03

Lanthanum tricyanide efficiently catalyzes a benzoin-type coupling between acyl silanes and ketones. Yields range from moderate to excellent over a broad substrate scope encompassing aryl, alkyl, electron-rich, and sterically hindered ketones.

Effect of Silane Coupling Agent on the Creep Behavior and Mechanical Properties of Carbon Fibers/Acrylonitrile Butadiene Rubber Composites.

PubMed

Choi, Woong-Ki; Park, Gil-Young; Kim, Byoung-Shuk; Seo, Min-Kang

2018-09-01

In this study, we investigated the effect of the silane coupling agent on the relationship between the surface free energy of carbon fibers (CFs) and the mechanical strength of CFs/acrylonitrile butadiene rubber (NBR) composites. Moreover, the creep behavior of the CF/NBR composites at surface energetic point of view were studied. The specific component of the surface free energy of the carbon fibers was found to increase upon grafting of the silane coupling agent, resulting in an increase in the tensile strength of the CF/NBR composites. On the other hand, the compressive creep strength was found to follow a slightly different trend. These results indicate the possible formation of a complex interpenetrating polymer network depending on the molecular size of the organic functional groups of the silane coupling agent.

Stability and activity of lactate dehydrogenase on biofunctional layers deposited by activated vapor silanization (AVS) and immersion silanization (IS)

NASA Astrophysics Data System (ADS)

Calvo, Jorge Nieto-Márquez; Elices, Manuel; Guinea, Gustavo V.; Pérez-Rigueiro, José; Arroyo-Hernández, María

2017-09-01

The interaction between surfaces and biological elements, in particular, proteins is critical for the performance of biomaterials and biosensors. This interaction can be controlled by modifying the surface in a process known as biofunctionalization. In this work, the enzyme lactate dehydrogenase (LDH) is used to study the stability of the interaction between a functional protein and amine-functionalized surfaces. Two different functionalization procedures were compared: Activated Vapor Silanization (AVS) and Immersion Silanization (IS). Adsorption kinetics is shown to follow the Langmuir model for AVS-functionalized samples, while IS-functionalized samples show a certain instability if immersed in an aqueous medium for several hours. In turn, the enzymatic activity of LDH is preserved for longer times by using glutaraldehyde as crosslinker between the AVS biofunctional surface and the enzyme.

Impacts of Different Functional Groups on the Kinetic Rates of α-Amine Ketoximesilanes Hydrolysis in the Preparation of Room Temperature Vulcanized Silicone Rubber

PubMed Central

Xu, Huihui; Liu, Zihou; Liu, Qingyang; Bei, Yiling; Zhu, Qingzeng

2018-01-01

α-Amine ketoximesilanes are proven to be effective crosslinkers in the preparation of ketone-oxime one-component room temperature vulcanized (RTV) silicone rubber without the use of toxic metal catalyst. This work aimed to investigate the hydrolysis kinetic of α-amine ketoximesilanes, which is vitally important for the preparation of RTV silicone rubber. Five kinds of α-amine ketoximesilanes, namely α-(N,N-diethyl)aminomethyltri(methylethylketoxime)silane (DEMOS), α-(N,N-di-n-butyl)aminomethyltri(methylethylketoxime)silane (DBMOS), α-(N-n-butyl)aminomethyltri(methylethylketoxime)silane (n-BMOS), α-(N-cyclohexyl)aminomethyltri(methylethylketoxime)silane (CMOS) and α-(β-aminomethyl)aminomethyltri(methylethylketoxime)silane (AEMOS), were successfully obtained and confirmed using Fourier transform infrared spectrometer (FT-IR) and hydrogen-1 nuclear magnetic resonance ( 1H NMR). Kinetics of hydrolysis reactions were measured by FT-IR and conductivity. Our results illustrated that the kinetic constant rates ranged from 12.2 × 10−4 s−1 to 7.6 × 10−4 s−1, with the decreasing order of DEMOS > n-BMOS > DBMOS > CMOS > AEMOS at the given temperature and humidity. Better performances of thermal stability could be achieved when using the α-amine ketoximesilanes as crosslinkers in the preparation of RTV silicon rubber than that of RTV silicone rubber with the use of methyltri(methylethylketoxime)silane (MOS) as a crosslinker and organic tin as a catalyst. PMID:29757263

Impacts of Different Functional Groups on the Kinetic Rates of α-Amine Ketoximesilanes Hydrolysis in the Preparation of Room Temperature Vulcanized Silicone Rubber.

PubMed

Xu, Huihui; Liu, Zihou; Liu, Qingyang; Bei, Yiling; Zhu, Qingzeng

2018-05-13

α-Amine ketoximesilanes are proven to be effective crosslinkers in the preparation of ketone-oxime one-component room temperature vulcanized (RTV) silicone rubber without the use of toxic metal catalyst. This work aimed to investigate the hydrolysis kinetic of α-amine ketoximesilanes, which is vitally important for the preparation of RTV silicone rubber. Five kinds of α-amine ketoximesilanes, namely α-(N,N-diethyl)aminomethyltri(methylethylketoxime)silane (DEMOS), α-(N,N-di-n-butyl)aminomethyltri(methylethylketoxime)silane (DBMOS), α-(N-n-butyl)aminomethyltri(methylethylketoxime)silane (n-BMOS), α-(N-cyclohexyl)aminomethyltri(methylethylketoxime)silane (CMOS) and α-(β-aminomethyl)aminomethyltri(methylethylketoxime)silane (AEMOS), were successfully obtained and confirmed using Fourier transform infrared spectrometer (FT-IR) and hydrogen-1 nuclear magnetic resonance ( ¹H NMR). Kinetics of hydrolysis reactions were measured by FT-IR and conductivity. Our results illustrated that the kinetic constant rates ranged from 12.2 × 10 −4 s −1 to 7.6 × 10 −4 s −1 , with the decreasing order of DEMOS > n-BMOS > DBMOS > CMOS > AEMOS at the given temperature and humidity. Better performances of thermal stability could be achieved when using the α-amine ketoximesilanes as crosslinkers in the preparation of RTV silicon rubber than that of RTV silicone rubber with the use of methyltri(methylethylketoxime)silane (MOS) as a crosslinker and organic tin as a catalyst.

Exercising Spatiotemporal Control of Cell Attachment with Optically Transparent Microelectrodes

PubMed Central

Shah, Sunny S.; Lee, Ji Youn; Verkhoturov, Stanislav; Tuleuova, Nazgul; Schweikert, Emile A.; Ramanculov, Erlan; Revzin, Alexander

2013-01-01

This paper describes a novel approach of controlling cell-surface interactions through an electrochemical “switching” of biointerfacial properties of optically transparent microelectrodes. The indium tin oxide (ITO) microelectrodes, fabricated on glass substrates, were modified with poly(ethylene glycol) (PEG) silane to make glass and ITO regions resistant to protein and cell adhesion. Cyclic voltammetry, with potassium ferricyanide serving as a redox reporter molecule, was used to monitor electron transfer across the electrolyte–ITO interface. PEG silane modification of ITO correlated with diminished electron transfer, judged by the disappearance of ferricyanide redox activity. Importantly, application of reductive potential (−1.4 V vs Ag/AgCl reference) corresponded with reappearance of typical ferricyanide redox peaks, thus pointing to desorption of an insulating PEG silane layer. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) characterization of the silanized ITO surfaces after electrical stimulation indicated complete removal of the silane layer. Significantly, electrical stimulation allowed to “switch” chosen electrodes from nonfouling to protein-adhesive while leaving other ITO and glass regions protected by a nonfouling PEG silane layer. The spatial and temporal control of biointerfacial properties afforded by our approach was utilized to micropattern proteins and cells and to construct micropatterned co-cultures. In the future, control of the biointerfacial properties afforded by this novel approach may allow the organization of multiple cell types into precise geometric configurations in order to create better in vitro mimics of cellular complexity of the native tissues. PMID:18512875

Influence of the type of solvent on the development of superhydrophobicity from silane-based solution containing nanoparticles

NASA Astrophysics Data System (ADS)

Pantoja, M.; Abenojar, J.; Martinez, M. A.

2017-03-01

Superhydrophobic surfaces are very appealing for numerous industrial applications due to their self-cleaning capacity. Although there are different methods to manufacture superhydrophobic surfaces, some of them do not keep the aesthetic appearance of the neat surface. Sol-gel processes are a valid alternative when transparent coatings are desired. The main goal of this research is to study the viability of this method by making superhydrophobic coatings from silane-based solution containing SiO2 nanoparticles. The effect of using different solvents is investigated, as well as the role played by the different components of the solution (silane, nanoparticles and solvent). Solutions of methyltrimethoxisilane (MTS) and tetraethoxysilane (TEOS) and 1% of SiO2 (%wt) were prepared with different solvents (ethanol, ethanol/water and white spirit). The hydrophobicity of the developed coatings is studied using contact angle measurements, while the aesthetic appearance is evaluated with gloss and color measurements. Also, infrared spectroscopy, dynamic light scattering (DSL), and surface tension measurements are used to study the silane solutions. The results show that the capacity of solvents to promote the dispersion of the nanoparticles is crucial to ensuring superhydrophobicity, since these agglomerates provide the micro- and nano- surface roughness required to get a hierarchical structure. However, the combined use of silanes and nanoparticles is key to make a superhydrophobic surface because physical (the surface roughness provided by nanoparticles) and chemical characteristics (hydrophobicity provided by silanes) are coupled.

N- and O- ligand doped mesoporous silica-chitosan hybrid beads for the efficient, sustainable and selective recovery of rare earth elements (REE) from acid mine drainage (AMD): Understanding the significance of physical modification and conditioning of the polymer.

PubMed

Ramasamy, Deepika Lakshmi; Puhakka, Ville; Iftekhar, Sidra; Wojtuś, Anna; Repo, Eveliina; Ben Hammouda, Samia; Iakovleva, Evgenia; Sillanpää, Mika

2018-04-15

Silica-chitosan hybrid beads were synthesized via three different methods to investigate the selective recovery of REE from AMD. The influence of amino/non-amino silanes, high molecular weight/high viscous chitosan and N-/O- based ligands were studied and their effects on REE removal efficiencies were analyzed. The adsorption efficiencies of three various groups of modified beads were inspected with respect to feed pH, in a single and a multi-component system, and their affinities towards the light and heavy rare earth elements (LREE/ HREEs) were interpreted to understand the intra-series REE separation behavior. The focus of the study was mainly directed towards utilizing these fabricated beads for the recovery of valuable REEs from the real AMD obtained at three different sampling depths which was found rich in iron, sulfur and aluminum. Moreover, the selectivity of the beads towards REEs improved with silanized and ligand immobilized gels and their impacts on REE recovery in the presence of competing ions were successfully presented in this paper. Also, the synthesized beads showed rapid REE adsorption and recovery within a process time of 5 min. Group II adsorbents, synthesized by forming silica-chitosan hybrid beads followed by PAN/acac modifications, showed superiority over the other groups of adsorbents. Copyright © 2018 Elsevier B.V. All rights reserved.

Anti-fouling properties of Fab' fragments immobilized on silane-based adlayers

NASA Astrophysics Data System (ADS)

Crivianu-Gaita, Victor; Romaschin, Alexander; Thompson, Michael

2015-12-01

Biosensors require surfaces that are highly specific towards the target analyte and that are minimally fouling. However, surface tuning to minimize fouling is a difficult task. The last decade has seen an increase in the use of immobilized antigen-binding antibody fragments (Fab') in biosensors. One Fab' linker compound S-(11-trichlorosilyl-undecanyl)-benzothiosulfonate (TUBTS) and three spacers were used to create the silane-based adlayers. The ultra-high frequency electromagnetic piezoelectric acoustic sensor (EMPAS) was used to gauge the fouling properties of the various surfaces using bovine serum albumin (BSA), goat IgG, and mouse serum. X-ray photoelectron spectroscopy (XPS), contact angle, and atomic force microscopy (AFM) were employed to characterize the surfaces. It was discovered that immobilized oriented Fab' fragments reduced the fouling levels of surfaces up to 80% compared to the surfaces without fragments. An explanation for this phenomenon is that the antibody fragments increase the hydration of the surfaces and aid in the formation of an anti-fouling water barrier. The anti-fouling effect of the Fab' fragments is at its maximum when there is an even distribution of fragments across the surfaces. Finally, using Fab'-covered surfaces, a cancer biomarker was detected from serum, showing the applicability of this work to the field of biodetection.

Crystal structures of 3,3'-bis-(hy-droxy-dimethylsilan-yl)azo-benzene and 4,4'-bis-(hy-droxy-dimethyl-silane)azo-benzene.

PubMed

Strüben, Jan; Hoffmann, Jonas; Presa-Soto, David; Näther, Christian; Staubitz, Anne

2016-11-01

The title compounds {systematic names ( E )-[diazene-1,2-diylbis(3,1-phenyl-ene)]bis-(di-methyl-silanol) and ( E )-[diazene-1,2-diylbis(4,1-phenyl-ene)]bis-(di-methyl-silanol)}, both of the sum formula C 16 H 22 N 2 O 2 Si 2 , were obtained by transmetallation of the respective bis-stannylated azo-benzenes with di-chloro-dimethyl-silane and esterification followed by hydrolysis. The asymmetric unit of 3,3'-diazenediylbis[dimeth-yl(phen-yl)silanol] (with the silanol functional group in a meta position) consists of two mol-ecules, of which one occupies a general position, whereas the second is located on a centre of inversion. In 4,4'-diazenediylbis[dimeth-yl(phen-yl)silanol] (with the silanol functional group in a para position) likewise two mol-ecules are present in the asymmetric unit, but in this case both occupy general positions. Differences between all mol-ecules can be found in the torsions about the N=N bond, as well as in the dihedral angles between the benzene rings. In both structures, inter-molecular O-H⋯O hydrogen bonding is observed, leading to the formation of layers parallel to (01-1) for (I) and to chains parallel to the a axis for (II).

Treatment of high-latency microcapsules containing an aluminium complex with an epoxy-functionalised trialkoxysilane.

PubMed

Kamiya, Kazunobu; Suzuki, Noboru

2016-12-01

Some aluminium complexes are excellent catalysts of cationic polymerisation and are used for low-temperature and fast-curing adhesive, used in electronic part mounting. Microencapsulation is a suitable technique for getting high latency of the catalysts and long shelf life of the adhesives. For the higher latency in a cycloaliphatic epoxy compound, the microcapsule surface which retained small amount of aluminium complex was coated with epoxy polymer and the effect was examined. From the X-ray photoelectron spectroscopic results, the surface was recognised to be sufficiently coated and the differential scanning calorimetric analyses showed that the coating did not significantly affect the low-temperature and fast-curing properties of adhesive. After storing the mixture of cycloaliphatic epoxy compound, coated microcapsules, triphenylsilanol and silane coupling agent for 48 h at room temperature, the increase in viscosity was only 0.01 Pa s, resulting in the excellent shelf life.

Microstructure and electrochemical behavior of cerium conversion coating modified with silane agent on magnesium substrates

NASA Astrophysics Data System (ADS)

Lei, Li; Shi, Jing; Wang, Xin; Liu, Dan; Xu, Haigang

2016-07-01

The cerium conversion coating with and without different concentrations of silane agent bis-(γ-triethoxysilylpropyl)-tetrasulfide (BTESPT) modification is obtained on magnesium alloys. Detailed properties of the coatings and the role of BTESPT as an additive are studied and followed with careful discussion. The coating morphology, wettability, chemical composition and corrosion resistance are characterized by scanning electronic microscope (SEM), water contact-angle, X-ray photoelectron spectroscopy (XPS), potentiodynamic measurements and electrochemical impedance spectroscopy (EIS). The electrochemical behavior of the coatings is investigated using EIS. The results indicate that the coating morphology and composition can be controlled by changing silane concentration. The combination of cerium ions and silane molecules could promote the formation of more homogenous and higher hydrophobic coating. The coating turns to be more compact and the adhesive strength between the coating and the magnesium substrate are strongly improved with the formation of Sisbnd Osbnd Si and Sisbnd Osbnd M chemical bonds. The optimum corrosion resistance of the coating in the corrosive media is obtained by 25 ml L-1 BTESPT modification. This whole study implies that the cerium conversion coating modified with certain silane agent deserves cautiousness before its application for corrosion resistance.

Low Cost Solar Array Project. Feasibility of the silane process for producing semiconductor-grade silicon. Final report, October 1975-March 1979

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1979-06-01

The commercial production of low-cost semiconductor-grade silicon is an essential requirement of the JPL/DOE (Department of Energy) Low-Cost Solar Array (LSA) Project. A 1000-metric-ton-per-year commercial facility using the Union Carbide Silane Process will produce molten silicon for an estimated price of $7.56/kg (1975 dollars, private financing), meeting the DOE goal of less than $10/kg. Conclusions and technology status are reported for both contract phases, which had the following objectives: (1) establish the feasibility of Union Carbide's Silane Process for commercial application, and (2) develop an integrated process design for an Experimental Process System Development Unit (EPSDU) and a commercial facility,more » and estimate the corresponding commercial plant economic performance. To assemble the facility design, the following work was performed: (a) collection of Union Carbide's applicable background technology; (b) design, assembly, and operation of a small integrated silane-producing Process Development Unit (PDU); (c) analysis, testing, and comparison of two high-temperature methods for converting pure silane to silicon metal; and (d) determination of chemical reaction equilibria and kinetics, and vapor-liquid equilibria for chlorosilanes.« less

Spatial Resolution of Small Particles in Silane Discharge.

DTIC Science & Technology

1985-02-18

report our results and attempt to qualitatively describe how these zones relate to plasma chemistry and film deposition processes. Originator supplied...keywords include: Rf discharge, Silane, Plasma chemistry , Particles, Clusters, and Laser light scattering.

Lanthanum Tricyanide-Catalyzed Acyl Silane-Ketone Benzoin Additions

PubMed Central

Tarr, James C.; Johnson, Jeffrey S.

2009-01-01

Lanthanum tricyanide efficiently catalyzes a benzoin-type coupling between acyl silanes and ketones. Yields range from moderate to excellent over a broad substrate scope encompassing aryl, alkyl, electron-rich, and sterically hindered ketones. PMID:19655731

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

NASA Technical Reports Server (NTRS)

Mikes, F.

1985-01-01

Fourier transform infrared spectroscopy is currently the best technique for observing hydrolytic changes in DC 1200 silane the primers caused by moisture in the atmosphere. To further prove that FTIR can be used as a criterion test for acceptance of silane primer lots, intensities of the FTIR OH- band are being compared with primer adhesive bond strength using a mechanical test suggested by NASA. Results of tests for shear strength and Oh-absorption are tabulated and compared with FTIR absorption intensities in the OH-region.

Stability and reactivity of dimethylethoxysilane

NASA Technical Reports Server (NTRS)

Johnson, Richard E.; Ford, Douglas I.

1993-01-01

The chemistry of the compound dimethylethoxysilane (DMES) is discussed especially as it relates to waterproofing silica surfaces. Some of the desirable properties of this compound are that it readily reacts with silica in the vapor phase, it is a low boiling point liquid (54 C), and the by-product of its reaction with silica is the rather inert substances ethanol. It is currently used by NASA to re-waterproof the HRSI shuttle tiles before relaunching the vehicle. Very little information is available on this particular compound in the literature or even on related silane compounds that have both a hydride group and an alkoxy group. Since the close proximity of two groups often drastically affects the chemical behavior of each group, chemical reactions were carried out in the laboratory with DMES to verify the expected behavior of these two functional groups located on DMES. Some of the reactions tested would be potentially useful for quantitative or qualitative measurements on DMES. To study the reactions of DMES with silica surfaces, cabosil was used as a silica substrate because of its high surface area and the ease of detection by infrared spectroscopy as well as other techniques.

Silanization of boron nitride nanosheets (BNNSs) through microfluidization and their use for producing thermally conductive and electrically insulating polymer nanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Seyhan, A.Tuğrul, E-mail: atseyhan@anadolu.edu.tr; Composite Materials Manufacturing Science Laboratory; Göncü, Yapıncak

Chemical exfoliation of boron nitride nanosheets (BNNSs) from large flakes of specially synthesized micro-sized hexagonal boron nitride (h-BN) ceramics was carried out through microfluidization. The surface of BNNSs obtained was then functionalized with vinyl-trimethoxy silane (VTS) coupling agent through microfluidization once again in an effort to make them compatible with organic materials, especially those including polymers. The morphology of BNNSs with and without silane treatment was then systematically characterized by conducting various different analytical techniques, including Thermogravimetric analysis (TGA), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Bright field Transmission Electron Microscopy (BF-TEM), Contact angle analyzer (CAA), Particle size analyzer (PSA)more » and Fourier Transmission Infrared (FTIR) spectroscopy attached with attenuated total reflectance (ATR) module. As a result, the silane treatment was determined to be properly and successfully carried out and to give rise to the irregularity of large flakes of the BNNSs by folding back their free edges upon themselves, which in turn assists in inducing further exfoliation of the few-layered nanosheets. To gain more insight into the effectiveness of the surface functionalization, thermal conductivity of polypropylene (PP) nanocomposites containing different amounts (1 wt% and 5 wt%) of BNNSs with and without silane treatment was experimentally investigated. Regardless of the weight content, PP nanocomposites containing silanized BNNSs were found to exhibit high thermal conductivity compared to PP nanocomposites containing BNNSs without silane treatment. It was concluded that microfluidization possesses the robustness to provide a reliable product quality, whether in small or large quantities, in a very time effective manner, when it comes to first exfoliating two-dimensional inorganic materials into few layered sheets, and functionalizing the surface of these sheets afterwards to make it possible to utilize them as promising filler constituent in manufacturing thermally conductive and electrically insulating polymer nanocomposites that could be considered as whole or a part of a heat-releasing device.« less

Silanization of boron nitride nanosheets (BNNSs) through microfluidization and their use for producing thermally conductive and electrically insulating polymer nanocomposites

NASA Astrophysics Data System (ADS)

Seyhan, A. Tuğrul; Göncü, Yapıncak; Durukan, Oya; Akay, Atakan; Ay, Nuran

2017-05-01

Chemical exfoliation of boron nitride nanosheets (BNNSs) from large flakes of specially synthesized micro-sized hexagonal boron nitride (h-BN) ceramics was carried out through microfluidization. The surface of BNNSs obtained was then functionalized with vinyl-trimethoxy silane (VTS) coupling agent through microfluidization once again in an effort to make them compatible with organic materials, especially those including polymers. The morphology of BNNSs with and without silane treatment was then systematically characterized by conducting various different analytical techniques, including Thermogravimetric analysis (TGA), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Bright field Transmission Electron Microscopy (BF-TEM), Contact angle analyzer (CAA), Particle size analyzer (PSA) and Fourier Transmission Infrared (FTIR) spectroscopy attached with attenuated total reflectance (ATR) module. As a result, the silane treatment was determined to be properly and successfully carried out and to give rise to the irregularity of large flakes of the BNNSs by folding back their free edges upon themselves, which in turn assists in inducing further exfoliation of the few-layered nanosheets. To gain more insight into the effectiveness of the surface functionalization, thermal conductivity of polypropylene (PP) nanocomposites containing different amounts (1 wt% and 5 wt%) of BNNSs with and without silane treatment was experimentally investigated. Regardless of the weight content, PP nanocomposites containing silanized BNNSs were found to exhibit high thermal conductivity compared to PP nanocomposites containing BNNSs without silane treatment. It was concluded that microfluidization possesses the robustness to provide a reliable product quality, whether in small or large quantities, in a very time effective manner, when it comes to first exfoliating two-dimensional inorganic materials into few layered sheets, and functionalizing the surface of these sheets afterwards to make it possible to utilize them as promising filler constituent in manufacturing thermally conductive and electrically insulating polymer nanocomposites that could be considered as whole or a part of a heat-releasing device.

Biomarker Sensors and Method for Multi-Color Imaging and Processing of Single-Molecule Life Signatures

NASA Technical Reports Server (NTRS)

Wade, Lawrence A. (Inventor); Collier, Charles Patrick (Inventor)

2013-01-01

The invention is a device including array of active regions for use in reacting one or more species in at least two of the active regions in a sequential process, e.g., sequential reactions. The device has a transparent substrate member, which has a surface region and a silane material overlying the surface region. A first active region overlies a first portion of the silane material. The first region has a first dimension of less than 1 micron in size and has first molecules capable of binding to the first portion of the silane material. A second active region overlies a second portion of the silane material. The second region has a second dimension of less than 1 micron in size, second molecules capable of binding to the second portion of the active region, and a spatial distance separates the first active region and the second active region.

High purity silane and silicon production

NASA Technical Reports Server (NTRS)

Breneman, William C. (Inventor)

1987-01-01

Silicon tetrachloride, hydrogen and metallurgical silicon are reacted at about 400.degree.-600.degree. C. and at pressures in excess of 100 psi, and specifically from about 300 up to about 600 psi to form di- and trichlorosilane that is subjected to disproportionation in the presence of an anion exchange resin to form high purity silane. By-product and unreacted materials are recycled, with metallurgical silicon and hydrogen being essentially the only consumed feed materials. The silane product may be further purified, as by means of activated carbon or cryogenic distillation, and decomposed in a fluid bed or free space reactor to form high purity polycrystalline silicon and by-product hydrogen which can be recycled for further use. The process results in simplified waste disposal operations and enhances the overall conversion of metallurgical grade silicon to silane and high purity silicon for solar cell and semiconductor silicon applications.

Preparation and Characterization of Silanes Films to Protect Electrogalvanized Steel

NASA Astrophysics Data System (ADS)

Seré, Pablo R.; Egli, Walter; Di Sarli, Alejandro R.; Deyá, Cecilia

2018-03-01

Silanes are an interesting alternative to chromate-based surface treatments for temporary protection of electrogalvanized steel. In this work, the protective behavior of 3-mercaptopropyltrimethoxysilane (MTMO), 3-aminopropyltriethoxysilane (AMEO), or 3-glycidoxypropyltrimethoxysilane (GLYMO) films applied on electrogalvanized automotive quality steel sheets has been studied. The silane coating morphology, composition, and porosity were characterized by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDS), x-ray fluorescence, immersion in copper sulfate, and cyclic voltammetry. The corrosion protection was evaluated by polarization curves, electrochemical noise measurements, electrochemical impedance spectrometry, and accelerated humidity chamber tests. The results showed that the silanes protect temporarily electrogalvanized steel from corrosion. MTMO forms a relatively thick and cracked film. AMEO and GLYMO films were so thin that they could not be observed by SEM but silicon was detected by EDS. MTMO provided good temporary protection, being an alternative to replace Cr(VI) as protector of electrogalvanized steel.

Chemical treatment of the intra-canal dentin surface: a new approach to modify dentin hydrophobicity

PubMed Central

GAITAN-FONSECA, Cesar; COLLART-DUTILLEUL, Pierre-Yves; SEMETEY, Vincent; ROMIEU, Olivier; CRUZ, Roel; FLORES, Hector; CUISINIER, Frédéric; PÉREZ, Elías; POZOS-GUILLEN, Amaury

2013-01-01

Objective: This study evaluated the hydrophobicity of dentin surfaces that were modified through chemical silanization with octadecyltrichlorosilane (OTS). Material and Methods: An in vitro experimental study was performed using 40 human permanent incisors that were divided into the following two groups: non-silanized and silanized. The specimens were pretreated and chemically modified with OTS. After the chemical modification, the dentin hydrophobicity was examined using a water contact angle measurement (WCA). The effectiveness of the modification of hydrophobicity was verified by the fluid permeability test (FPT). Results and Conclusions: Statistically significant differences were found in the values of WCA and FPT between the two groups. After silanization, the hydrophobic intraradicular dentin surface exhibited in vitro properties that limit fluid penetration into the sealed root canal. This chemical treatment is a new approach for improving the sealing of the root canal system. PMID:23559114

Light-weight ceramic insulation

NASA Technical Reports Server (NTRS)

Hsu, Ming-Ta S. (Inventor); Chen, Timothy S. (Inventor)

2002-01-01

Ultra-high temperature, light-weight, ceramic insulation such as ceramic tile is obtained by pyrolyzing a siloxane gel derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes may contain also an effective amount of a mono- or trialkoxy silane to obtain the siloxane gel. The siloxane gel is dried at ambient pressures to form a siloxane ceramic precursor without significant shrinkage. The siloxane ceramic precursor is subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation, can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C. and is particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.

Chemical modification of polyvinyl chloride and silicone elastomer in inhibiting adhesion of Aeromonas hydrophila.

PubMed

Kregiel, Dorota; Berlowska, Joanna; Mizerska, Urszula; Fortuniak, Witold; Chojnowski, Julian; Ambroziak, Wojciech

2013-07-01

Disease-causing bacteria of the genus Aeromonas are able to adhere to pipe materials, colonizing the surfaces and forming biofilms in water distribution systems. The aim of our research was to study how the modification of materials used commonly in the water industry can reduce bacterial cell attachment. Polyvinyl chloride and silicone elastomer surfaces were activated and modified with reactive organo-silanes by coupling or co-crosslinking silanes with the native material. Both the native and modified surfaces were tested using the bacterial strain Aeromonas hydrophila, which was isolated from the Polish water distribution system. The surface tension of both the native and modified surfaces was measured. To determine cell viability and bacterial adhesion two methods were used, namely plate count and luminometry. Results were expressed in colony-forming units (c.f.u.) and in relative light units (RLU) per cm(2). Almost all the chemically modified surfaces exhibited higher anti-adhesive and anti-microbial properties in comparison to the native surfaces. Among the modifying agents examined, poly[dimethylsiloxane-co-(N,N-dimethyl-N-n-octylammoniopropyl chloride) methylsiloxane)] terminated with hydroxydimethylsilyl groups (20 %) in silicone elastomer gave the most desirable results. The surface tension of this modifier, was comparable to the non-polar native surface. However, almost half of this value was due to the result of polar forces. In this case, in an adhesion analysis, only 1 RLU cm(-2) and less than 1 c.f.u. cm(-2) were noted. For the native gumosil, the results were 9,375 RLU cm(-2) and 2.5 × 10(8) c.f.u. cm(-2), respectively. The antibacterial activity of active organo-silanes was associated only with the carrier surface because no antibacterial compounds were detected in liquid culture media, in concentrations that were able to inhibit cell growth.

μ3-η(2):η(2):η(2)-Coordination of Primary Silane on a Triruthenium Plane.

PubMed

Nagaoka, Masahiro; Tsuruda, Hiroyuki; Amako, Masa-aki; Suzuki, Hiroharu; Takao, Toshiro

2015-12-01

A μ3-η(2):η(2):η(2)-silane complex, [(Cp*Ru)3(μ3-η(2):η(2):η(2)-H3SitBu)(μ-H)3] (2 a; Cp* = η(5)-C5Me5), was synthesized from the reaction of [{Cp*Ru(μ-H)}3(μ3-H)2] (1) with tBuSiH3. Complex 2 a is the first example of a silane ligand adopting a μ3-η(2):η(2):η(2) coordination mode. This unprecedented coordination mode was established by NMR and IR spectroscopy as well as X-ray diffraction analysis and supported by a density functional study. Variable-temperature NMR analysis implied that 2 a equilibrates with a tautomeric μ3-silyl complex (3 a). Although 3 a was not isolated, the corresponding μ3-silyl complex, [(Cp*Ru)3(μ3-η(2):η(2)-H2SiPh)(H)(μ-H)3] (3 b), was obtained from the reaction of 1 with PhSiH3. Treatment of 2 a with PhSiH3 resulted in a silane exchange reaction, leading to the formation of 3 b accompanied by the elimination of tBuSiH3. This result indicates that the μ3-silane complex can be regarded as an "arrested" intermediate for the oxidative addition/reductive elimination of a primary silane to a trinuclear site. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of prior silane application on the bond strength of a universal adhesive to a lithium disilicate ceramic.

PubMed

Moro, André Fábio Vasconcelos; Ramos, Amanda Barreto; Rocha, Gustavo Miranda; Perez, Cesar Dos Reis

2017-11-01

Universal adhesives combine silane and various monomers in a single bottle to make them more versatile. Their adhesive performance is unclear. The purpose of this in vitro study was to assess the effects of an additional silane application before using a universal adhesive on the adhesion between a disilicate glass ceramic and a composite resin by using a microshear bond strength test (μSBS) and fracture analysis immediately and after thermocycling. One hundred lithium disilicate glass ceramic disks were divided into 10 groups for bond strength testing according to the following 3 surface treatments: silane application (built-in universal adhesive or with additional application), adhesive (Adper Single Bond Plus [SB, 3M ESPE], Scotchbond Universal Adhesive [U, 3M ESPE], and mixed U with Dual Cure Activator [DCA, 3M ESPE]); or thermocycling (half of the specimens were thermocycled 10000 times). After surface treatment, 5 resin cylinders were bonded to each disk and submitted to a μSBS test. The failure mode was analyzed under a stereomicroscope and evaluated by scanning electron microscope and energy-dispersive x-ray spectroscopy. Data from the μSBS test were analyzed by 3-way ANOVA followed by the Tukey HSD post hoc test (α=.05). An additional silane application resulted in a higher μSBS result for all adhesive groups (P<.05). Ceramic surface treatment influenced the performance of adhesives, which may be improved with an additional silane application. Copyright © 2017 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Effect of Surface Treatments on the Bond Strength to Turkom-Cera All-ceramic Material.

PubMed

Razak, Abdul Aa; Abu-Hassan, Mohamed I; Al-Makramani, Bandar Ma; Al-Sanabani, Fuad A; Al-Shami, Ibrahim Z; Almansour, Hosain M

2016-11-01

The aim of this study was to evaluate the effect of surface treatments on shear bond strength (SBS) of Turkom-Cera (Turkom-Ceramic (M) Sdn. Bhd., Puchong, Malaysia) all-ceramic material cemented with resin cement Panavia-F (Kuraray Medical Inc., Okayama, Japan). Forty Turkom-Cera ceramic disks (10 mm × 3 mm) were prepared and randomly divided into four groups. The disks were wet ground to 1000-grit and subjected to four surface treatments: (1) No treatment (Control), (2) sandblasting, (3) silane application, and (4) sandblasting + silane. The four groups of 10 specimens each were bonded with Panavia-F resin cement according to manufacturer's recommendations. The SBS was determined using the universal testing machine (Instron) at 0.5 mm/min crosshead speed. Failure modes were recorded and a qualitative micromorphologic examination of different surface treatments was performed. The data were analyzed using the one-way analysis of variance (ANOVA) and Tukey honestly significant difference (HSD) tests. The SBS of the control, sandblasting, silane, and sandblasting + silane groups were: 10.8 ± 1.5, 16.4 ± 3.4, 16.2 ± 2.5, and 19.1 ± 2.4 MPa respectively. According to the Tukey HSD test, only the mean SBS of the control group was significantly different from the other three groups. There was no significant difference between sandblasting, silane, and sandblasting + silane groups. In this study, the three surface treatments used improved the bond strength of resin cement to Turkom-Cera disks. The surface treatments used in this study appeared to be suitable methods for the cementation of glass infiltrated all-ceramic restorations.

Effects of silica coating and silane surface conditioning on the bond strength of rebonded metal and ceramic brackets.

PubMed

Atsü, Saadet; Çatalbaş, Bülent; Gelgör, İbrahim Erhan

2011-01-01

The aim of this study was to evaluate the effects of tribochemical silica coating and silane surface conditioning on the bond strength of rebonded metal and ceramic brackets. Twenty debonded metal and 20 debonded ceramic brackets were randomly assigned to receive one of the following surface treatments (n=10 for each group): (1) sandblasting (control); (2) tribochemical silica coating combined with silane. Brackets were rebonded to the enamel surface on the labial and lingual sides of premolars with a light-polymerized resin composite. All specimens were stored in distilled water for 1 week and then thermocycled (5,000 cycles) between 5-55ºC. Shear bond strength values were measured using a universal testing machine. Student's t-test was used to compare the data (α=0.05). Failure mode was assessed using a stereomicroscope, and the treated and non-treated bracket surfaces were observed by scanning electron microscopy. Rebonded ceramic brackets treated with silica coating followed by silanization had significantly greater bond strength values (17.7±4.4 MPa) than the sandblasting group (2.4±0.8 MPa, P<0.001). No significant difference was observed between the rebonded metal brackets treated with silica coating with silanization (15±3.9 MPa) and the sandblasted brackets (13.6±3.9 MPa). Treated rebonded ceramic specimens primarily exhibited cohesive failure in resin and adhesive failure at the enamel-adhesive interface. In comparison to sandblasting, silica coating with aluminum trioxide particles followed by silanization resulted in higher bond strengths of rebonded ceramic brackets.

Effect of Surface Treatment, Silane, and Universal Adhesive on Microshear Bond Strength of Nanofilled Composite Repairs.

PubMed

Fornazari, I A; Wille, I; Meda, E M; Brum, R T; Souza, E M

 The aim of this study was to evaluate the effect of surface treatment and universal adhesive on the microshear bond strength of nanoparticle composite repairs.  One hundred and forty-four specimens were built with a nanofilled composite (Filtek Supreme Ultra, 3M ESPE). The surfaces of all the specimens were polished with SiC paper and stored in distilled water at 37°C for 14 days. Half of the specimens were then air abraded with Al 2 O 3 particles and cleaned with phosphoric acid. Polished specimens (P) and polished and air-abraded specimens (A), respectively, were randomly divided into two sets of six groups (n=12) according to the following treatments: hydrophobic adhesive only (PH and AH, respectively), silane and hydrophobic adhesive (PCH, ACH), methacryloyloxydecyl dihydrogen phosphate (MDP)-containing silane and hydrophobic adhesive (PMH, AMH), universal adhesive only (PU, AU), silane and universal adhesive (PCU, ACU), and MDP-containing silane and universal adhesive (PMU, AMU). A cylinder with the same composite resin (1.1-mm diameter) was bonded to the treated surfaces to simulate the repair. After 48 hours, the specimens were subjected to microshear testing in a universal testing machine. The failure area was analyzed under an optical microscope at 50× magnification to identify the failure type, and the data were analyzed by three-way analysis of variance and the Games-Howell test (α=0.05).  The variables "surface treatment" and "adhesive" showed statistically significant differences for p<0.05. The highest mean shear bond strength was found in the ACU group but was not statistically different from the means for the other air-abraded groups except AH. All the polished groups except PU showed statistically significant differences compared with the air-abraded groups. The PU group had the highest mean among the polished groups. Cohesive failure was the most frequent failure mode in the air-abraded specimens, while mixed failure was the most common mode in the polished specimens.  While air abrasion with Al 2 O 3 particles increased the repair bond strength of the nanoparticle composite, the use of MDP-containing silane did not lead to a statistically significant increase in bond strength. Silane-containing universal adhesive on its own was as effective as any combination of silane and adhesive, particularly when applied on air-abraded surfaces.

Studies on silicon NMR characterization and kinetic modeling of the structural evolution of siloxane-based materials and their applications in drug delivery and adsorption

NASA Astrophysics Data System (ADS)

Ambati, Jyothirmai

This dissertation presents studies of the synthetic processes and applications of siloxane-based materials. Kinetic investigations of bridged organoalkoxysilanes that are precursors to organic-inorganic hybrid polysilsesquioxanes are a primary focus. Quick gelation despite extensive cyclization is found during the polymerization of bridged silane precursors except for silanes with certain short bridges. This work is an attempt to characterize and understand some of the distinct features of bridged silanes using experimental characterization, kinetic modeling and simulation. In addition to this, the dissertation shows how the properties of siloxane-materials can be engineered for drug delivery and adsorption. The phase behavior of polymerizing mixtures is first investigated to identify the solutions that favor kinetic characterization. Microphase separation is found to cause gradual loss of NMR signal for certain initial compositions. Distortionless Enhancement by Polarization Transfer 29Si NMR is employed to identify the products of polymerization of some short-bridged silanes under no signal loss conditions. This technique requires knowing indirect 29Si-1H scalar coupling constants which sometimes cannot be measured due to second-order effects. However, the B3LYP density functional method with 6-31G basis set is found to predict accurate 29Si- 1H coupling constants of organoalkoxysilanes and siloxanes. The scalar coupling constants thus estimated are employed to resolve non-trivial coupled NMR spectra and quantitative kinetic modeling is performed using the DEPT Si NMR transients. In order to investigate the role of the organic bridging group, the structural evolution of bridged and non-bridged silanes are compared using Monte Carlo simulations. Kinetic and simulation models suggest that cyclization plays a key role right from the onset of polymerization for bridged silanes even more than in non-bridged silanes. The simulations indicate that the carbosiloxane rings formed from short-bridged precursors slow down but do not prevent gelation. The tuning of siloxane-based materials for adsorption technologies are also discussed here. In the first example, antioxidant enzyme loading is investigated as a means to reduce oxidative stress generated by silica nanoparticle drug carriers. Materials are engineered for promising enzyme loading and protection from proteolysis. Second, the potential of copper sulfate impregnation to enhance adsorption of ammonia by silica is explored by molecular simulation. KEYWORDS: Sol-gel Polymerization, Kinetic Investigation, Si NMR, Bridged Silanes, DFT Calculations.

Silane cross-linkable ethylene-propylene elastomer compositions prepared by reactive processing

NASA Astrophysics Data System (ADS)

Kozawa, Eiji; Nakajima, Yasuo; Kim, Jae Kyung

2015-05-01

Thermoplastic Elastomers (TPEs) have received attention as the alternative materials of EPDM due to an advantage for mass production. In recent years, by the progress of polymerization technology, Ethylene-propylene Elastomer (EP), one of the TPEs, is beginning to be applied to many products because of its good properties as rubber. However, as much as a complete replacement for EPDM, it is not provided with sufficient properties. In such circumstance, we found that EP's performance properties can be further enhanced via chemical modification such as cross-linking. The advent of a newer technique, involving the grafting of organo-functional silane onto the polymer chain in the reaction extrusion process is more attractive due to various industrial advantages. Although the functionalization of the EP by silane grafting through reactive processing is very useful, the silane grafting process of EP has a difficulty. It is most likely a consequence of the nature of the PP chain scission (β-scission), which is the dominant reaction in PP when subjected to free radicals at elevated temperature during processing. Therefore, the objective of our current work is to investigate a reactive extrusion process for the silane cross-linkable EP while minimizing the degradation, as well as evaluate the properties of the modified polymer.

Optimization and characterization of biomolecule immobilization on silicon substrates using (3-aminopropyl)triethoxysilane (APTES) and glutaraldehyde linker

NASA Astrophysics Data System (ADS)

Gunda, Naga Siva Kumar; Singh, Minashree; Norman, Lana; Kaur, Kamaljit; Mitra, Sushanta K.

2014-06-01

In the present work, we developed and optimized a technique to produce a thin, stable silane layer on silicon substrate in a controlled environment using (3-aminopropyl)triethoxysilane (APTES). The effect of APTES concentration and silanization time on the formation of silane layer is studied using spectroscopic ellipsometry and Fourier transform infrared spectroscopy (FTIR). Biomolecules of interest are immobilized on optimized silane layer formed silicon substrates using glutaraldehyde linker. Surface analytical techniques such as ellipsometry, FTIR, contact angle measurement system, and atomic force microscopy are employed to characterize the bio-chemically modified silicon surfaces at each step of the biomolecule immobilization process. It is observed that a uniform, homogenous and highly dense layer of biomolecules are immobilized with optimized silane layer on the silicon substrate. The developed immobilization method is successfully implemented on different silicon substrates (flat and pillar). Also, different types of biomolecules such as anti-human IgG (rabbit monoclonal to human IgG), Listeria monocytogenes, myoglobin and dengue capture antibodies were successfully immobilized. Further, standard sandwich immunoassay (antibody-antigen-antibody) is employed on respective capture antibody coated silicon substrates. Fluorescence microscopy is used to detect the respective FITC tagged detection antibodies bound to the surface after immunoassay.

Effect of tetraethoxysilane coating on the improvement of plasma treated polypropylene adhesion

NASA Astrophysics Data System (ADS)

Pantoja, M.; Encinas, N.; Abenojar, J.; Martínez, M. A.

2013-09-01

Polypropylene is one of the most used polymers due to its lightweight and recyclability properties, among others. However, its poor characteristics regarding surface energy and lack of polar functional groups have to be overcome to perform adhesion processes. The main objective of this work is to improve the adhesion behavior of polypropylene by combining atmospheric pressure plasma surface activation and silane adhesion promoter. Tetraethoxysilane hydrolysis and condensation are followed through infrared spectroscopy by attenuated total reflectance in order to set the coating conditions. Contact angle measurements and surface energy calculations as well as infrared and X-ray photoelectron spectroscopy are used to evaluate polymer chemical modifications. Morphological changes are studied through scanning electron and atomic force microscopy. Results show the ability of plasma treatment to create active oxydised functional groups on the polypropylene surface. These groups lead to a proper wetting of the polymer by the silane. Shear strength of single-lap bonding of polypropylene with a polyurethane adhesive suffers a significant improvement when the silane coating is applied on previously plasma activated samples. It has been also demonstrated that the silane curing conditions play a decisive role on the adhesion response. Finally, the stability of the silane solution is tested up to 30 days, yielding diminished but still acceptable adhesion strength values.

Fiber Surface Modification Technology for Fiber-Optic Localized Surface Plasmon Resonance Biosensors

PubMed Central

Zhang, Qiang; Xue, Chenyang; Yuan, Yanling; Lee, Junyang; Sun, Dong; Xiong, Jijun

2012-01-01

Considerable studies have been performed on the development of optical fiber sensors modified by gold nanoparticles based on the localized surface plasmon resonance (LSPR) technique. The current paper presents a new approach in fiber surface modification technology for biosensors. Star-shaped gold nanoparticles obtained through the seed-mediated solution growth method were found to self-assemble on the surface of tapered optical fibers via amino- and mercapto-silane coupling agents. Transmitted power spectra of 3-aminopropyltrimethoxy silane (APTMS)-modified fiber were obtained, which can verify that the silane coupling agent surface modification method is successful. Transmission spectra are characterized in different concentrations of ethanol and gentian violet solutions to validate the sensitivity of the modified fiber. Assembly using star-shaped gold nanoparticles and amino/mercapto silane coupling agent are analyzed and compared. The transmission spectra of the gold nanoparticles show that the nanoparticles are sensitive to the dielectric properties of the surrounding medium. After the fibers are treated in t-dodecylmercaptan to obtain their transmission spectra, APTMS-modified fiber becomes less sensitive to different media, except that modified by 3-mercaptopropyltrimethoxy silane (MPTMS). Experimental results of the transmission spectra show that the surface modified by the gold nanoparticles using MPTMS is firmer compared to that obtained using APTMS. PMID:22736974

Resistance of poly(ethylene oxide)-silane monolayers to the growth of polyelectrolyte multilayers.

PubMed

Buron, Cédric C; Callegari, Vincent; Nysten, Bernard; Jonas, Alain M

2007-09-11

The ability of poly(ethylene oxide)-silane (PEO-silane) monolayers grafted onto silicon surfaces to resist the growth of polyelectrolyte multilayers under various pH conditions is assessed for different pairs of polyelectrolytes of varying molar mass. For acidic conditions (pH 3), the PEO-silane monolayers exhibit good polyelectrolyte repellency provided the polyelectrolytes bear no moieties that are able to form hydrogen bonds with the ether groups of the PEO chains. At basic pH, PEO-silane monolayers undergo substantial hydrolysis leading to the formation of negatively charged defects in the monolayers, which then play the role of adsorption sites for the polycation. Once the polycation is adsorbed, multilayer growth ensues. Because this is defect-driven growth, the multilayer is not continuous and is made of blobs or an open network of adsorbed strands. For such conditions, the molar mass of the polyelectrolyte plays a key role, with polyelectrolyte chains of larger molar mass adsorbing on a larger number of defects, resulting in stronger anchoring of the polyelectrolyte complex on the surfaces and faster subsequent growth of the multilayer. For polyelectrolytes of sufficiently low molar mass at pH 9, the growth of the multilayer can nevertheless be prevented for as much as five cycles of deposition.

Development of an environmentally benign anticorrosion coating for aluminum alloy using green pigments and organofunctional silanes

NASA Astrophysics Data System (ADS)

Yin, Zhangzhang

Aerospace aluminum alloys such as Al alloy 2024-T3 and 7075-T6 are subject to localized corrosion due the existence of intermetallics containing Cu, Mg or Zn. Current protection measurement employs substantial use of chromate and high VOC organics, both of which are identified as environment and health hazards. The approach of this study is to utilize a combination of organofunctional silanes and a compatible inhibitor integrated into high-performance waterborne resins. First, an extensive pigment screening has been done to find replacements for chromates using the testing methodology for fast corrosion inhibition evaluation and pigment. Zinc phosphate and calcium zinc phosphomolybdate were found to have the best overall performance on Al alloys. Some new corrosion inhibitors were synthesized by chemical methods or modified by plasma polymerization for use in the coatings. Low-VOC, chromate-free primers (superprimer) were developed using these pigments with silane and acrylic-epoxy resins. The developed superprimer demonstrated good corrosion inhibition on aluminum substrates. The functions of inhibitor and silane in the coating were investigated. Both silane and inhibitor are critical for the performance of the superprimer. Silane was found to improve the adhesion of the coating to the substrate and also facilitate corrosion prevention. Addition of zinc phosphate to the coating improved the resistance of a scratched area against corrosion. The microstructure of the acrylic-epoxy superprimer coating was studied. SEM/EDAX revealed that the superprimer has a self-assembled stratified double-layer structure which accounts for the strong anti-corrosion performance of the zinc phosphate pigment. Zinc phosphate leaches out from the coating to actively protect the scratched area. The leaching of pigment was confirmed in the ICP-MS analysis and the leaching rate was measured. Coating-metal interface and the scribe of coated panels subjected to corrosion test was studied. ToF-SIMS studies confirmed the presence of silane at the interface and the hydrolysis of the silane. The abundant presence of silane was believed to improve the adhesion and also facilitate the corrosion prevention. The protection mechanism of the acrylic-epoxy superprimer was proposed. The self-assembled double-layer structure of the acrylic-epoxy superprimer consist of a less-penetrable hydrophobic layer (epoxy-dominated) on the top and a hydrophilic layer (acrylic-dominated) accommodating the inhibitors underneath. This unique structure of the acrylic-epoxy accounts for the good protection of the coating. Furthermore, the inhibition mechanism of zinc phosphate was explored and compared to those which have been reported. Based on the protection mechanism of the superprimer, electrodeposition was explored in order to achieve a more organized coating with a better engineered metal/coating interface. The electrodeposited coatings were found to have higher barrier property and anticorrosion performance.

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

NASA Technical Reports Server (NTRS)

Mikes, F.; Mowrey, C.; Reis, E.

1985-01-01

Results of lap shear tests of various silane primers are presented in graphs and tables. The OH-absorption of these primers (FTIR area values) are correlated with the lap shear tests of coated panels.

Laboratory and field performance of silane anti-strip agent

DOT National Transportation Integrated Search

1986-11-01

A previous ADOT research project resulted in strong evidence that the use of organo-silane as an asphalt additive was very effective in preventing stripping in asphalt concrete pavements. A test section approximately 2800 ft long and 12 ft wide incor...

Viscoelastic Properties of Alkoxy Silane-Epoxy Interpenetrating Networks

DTIC Science & Technology

2003-11-01

Owens Corning Fiberglass for supply of the epoxy film former emulsion used in the model silane formulation. The authors also wish to acknowledge the...inclusion filled composite µm- powderproperties 4 triblock copolymer surfactant. The Owens Corning Company generously provided the film former emulsion

Liquid Chromatographic Analysis of Nitrocellulose-Base Propellants

DTIC Science & Technology

1983-03-28

18 radial PkC column using 10 micron silica coated with octadecyl silane. The detector was a LC 85 variable wavelength UV detector from Perkin-Elmer...Snyder, L. R. J Chrom Scd i6, (1978), 223. i •2 Glatch, J. L., Kirkland, J. J., Squire, K. M., and Miner, J. M.; J. Chromatgography, 199, (1980), 57. 4...assuming non retained peaks elute at 1 minute). This produces 3 solvents of approximately the same strengths bnt greatly differing selectivities. Once

Mechanical properties of dental resin/composite containing urchin-like hydroxyapatite.

PubMed

Liu, Fengwei; Sun, Bin; Jiang, Xiaoze; Aldeyab, Sultan S; Zhang, Qinghong; Zhu, Meifang

2014-12-01

To investigate the reinforcing effect of urchin-like hydroxyapatite (UHA) in bisphenol A glycidyl methacrylate (Bis-GMA)/triethylene glycol dimethacrylate (TEGDMA) dental resin (without silica nanoparticles) and dental composites (with silica nanoparticles), and explore the effect of HA filler morphologies and loadings on the mechanical properties. UHA was synthesized by a facile method of microwave irradiation and studied by X-ray diffraction (XRD), scanning electron microscope (SEM), and thermogravimetric analysis (TGA). Mechanical properties of the dental resin composites containing silanized UHA were tested by a universal mechanical testing machine. Analysis of variance was used for the statistical analysis of the acquired data. The fracture morphologies of tested composites were observed by SEM. Composites with silanized irregular particulate hydroxyapatite (IPHA) and hydroxyapatite whisker (HW) were prepared for comparative studies. Impregnation of lower loadings (5 wt% and 10 wt%) of silanized UHA into dental resin (without silica nanoparticles) substantially improved the mechanical properties; higher UHA loadings (20 wt% and 30 wt%) of impregnation continuously improved the flexural modulus and microhardness, while the strength would no longer be increased. Compared with silanized IPHA and HW, silanized UHA consisting of rods extending radially from center were embedded into the matrix closely and well dispersed in the composite, increasing filler-matrix interfacial contact area and combination. At higher filler loadings, UHA interlaced together tightly without affecting the mobility of monomer inside, which might bear higher loads during fracture of the composite, leading to higher strengths than those of dental resins with IPHA and HW. Besides, impregnation of silanized UHA into dental composites (with silica nanoparticles) significantly improved the strength and modulus. UHA could serve as novel reinforcing HA filler to improve the mechanical properties of dental resin and dental composite.

Polyethylene glycol-covered ultra-small Gd2O3 nanoparticles for positive contrast at 1.5 T magnetic resonance clinical scanning

NASA Astrophysics Data System (ADS)

Fortin, Marc-André; Petoral, Rodrigo M., Jr.; Söderlind, Fredrik; Klasson, A.; Engström, Maria; Veres, Teodor; Käll, Per-Olof; Uvdal, Kajsa

2007-10-01

The size distribution and magnetic properties of ultra-small gadolinium oxide crystals (US-Gd2O3) were studied, and the impact of polyethylene glycol capping on the relaxivity constants (r1, r2) and signal intensity with this contrast agent was investigated. Size distribution and magnetic properties of US-Gd2O3 nanocrystals were measured with a TEM and PPMS magnetometer. For relaxation studies, diethylene glycol (DEG)-capped US-Gd2O3 nanocrystals were reacted with PEG-silane (MW 5000). Suspensions were adequately dialyzed in water to eliminate traces of Gd3+ and surfactants. The particle hydrodynamic radius was measured with dynamic light scattering (DLS) and the proton relaxation times were measured with a 1.5 T MRI scanner. Parallel studies were performed with DEG-Gd2O3 and PEG-silane-SPGO (Gd2O3,< 40 nm diameter). The small and narrow size distribution of US-Gd2O3 was confirmed with TEM (~3 nm) and DLS. PEG-silane-US-Gd2O3 relaxation parameters were twice as high as for Gd-DTPA and the r2/r1 ratio was 1.4. PEG-silane-SPGO gave low r1 relaxivities and high r2/r1 ratios, less compatible with positive contrast agent requirements. Higher r1 were obtained with PEG-silane in comparison to DEG-Gd2O3. Treatment of DEG-US-Gd2O3 with PEG-silane provides enhanced relaxivity while preventing aggregation of the oxide cores. This study confirms that PEG-covered Gd2O3 nanoparticles can be used for positively contrasted MR applications requiring stability, biocompatible coatings and nanocrystal functionalization.

Effect of water storage on the silanization in porcelain repair strength.

PubMed

Berry, T; Barghi, N; Chung, K

1999-06-01

This study examined the long-term water storage affect of silanization on shear bond strength of composite resin to porcelain. One hundred and sixty square-shaped specimens were fabricated and sanded flat sequentially with silicone carbide papers. The specimens were then placed into four groups and 16 subgroups of 10 specimens each randomly. Four commercially available silane systems, two one-mix and two two-mix, were tested in this study. Teflon tubes with an internal diameter of 2.97 mm and 2 mm in height were filled with a dual cure composite resin (Mirage FLC), placed on the silanated surfaces and light-cured for 120 s. Specimens were stored in room temperature water and subjected to shear bond strength testing after 24 h, 1 week, 1 month and 3 month periods of immersion. An Instron Universal testing machine with a crosshead speed of 0.5 mm/min was used for the testing. The mean values of the shear bond strengths ranged from 4.38 MPa (24-h period) to 23.90 MPa (3-month period). ANOVA and Scheffe' tests were used to analyse data with confidence level at 95%. All groups recorded an increase in bond strength after one week as compared with the 24-h period (P<0.05). With the exception of a one-mix system, all systems showed significantly higher bond strength at 3 weeks as compared with the 24-h and 1-week water storage periods. In conclusion, bond strength of composite resin to porcelain resulting from silanization of porcelain increased during the experimental period. The bond strength also varied for different silanes used in this study.

Silanated Surface Treatment: Effects on the Bond Strength to Lithium Disilicate Glass-Ceramic.

PubMed

Baratto, Samantha Schaffer Pugsley; Spina, Denis Roberto Falcão; Gonzaga, Carla Castiglia; Cunha, Leonardo Fernandes da; Furuse, Adilson Yoshio; Baratto Filho, Flares; Correr, Gisele Maria

2015-10-01

The aim of this study was to evaluate the effect of silanization protocols on the bond strength of two resin cements to a lithium disilicate glass-ceramic. Thirty-two ceramic discs were assigned to 2 groups (n=16): G1 - dual-cured resin cement and G2 - light-cured resin cement. Four subgroups were evaluated according to the used silanization protocol. The glass-ceramic was etched with 10% hydrofluoric acid for 20 s and silane was applied for 1 min, as follows: CTL - according to the manufacturer's instructions; HA - dried with hot air; NWA - washed and dried with water and air at room temperature; HWA - washed and dried with hot water and hot air. Thereafter, adhesive was applied and light-cured for 20 s. Silicon molds were used to prepare resin cement cylinders (1x1 mm) on the ceramic surface. The specimens were stored in deionized water at 37 °C for 48 h and subjected to a micro-shear test. The data were submitted to statistical analysis (?#61537;=0.05). Group G1 showed higher bond strengths than G2, except for the CTL and NWA subgroups. Differences as function of the silanization protocol were only observed in G1: HWA (25.13±6.83)≥HA (22.95±7.78)≥CTL(17.44±7.24) ≥NWA(14.63±8.76). For G2 there was no difference among the subgroups. In conclusion, the silanization protocol affected the resin cement/ceramic bond strengths, depending on the material. Washing/drying with hot water and/or hot air increased only the bond strength of the dual-cured resin cement.

Four chemical methods of porcelain conditioning and their influence over bond strength and surface integrity

PubMed Central

Stella, João Paulo Fragomeni; Oliveira, Andrea Becker; Nojima, Lincoln Issamu; Marquezan, Mariana

2015-01-01

OBJECTIVE: To assess four different chemical surface conditioning methods for ceramic material before bracket bonding, and their impact on shear bond strength and surface integrity at debonding. METHODS: Four experimental groups (n = 13) were set up according to the ceramic conditioning method: G1 = 37% phosphoric acid etching followed by silane application; G2 = 37% liquid phosphoric acid etching, no rinsing, followed by silane application; G3 = 10% hydrofluoric acid etching alone; and G4 = 10% hydrofluoric acid etching followed by silane application. After surface conditioning, metal brackets were bonded to porcelain by means of the Transbond XP system (3M Unitek). Samples were submitted to shear bond strength tests in a universal testing machine and the surfaces were later assessed with a microscope under 8 X magnification. ANOVA/Tukey tests were performed to establish the difference between groups (α= 5%). RESULTS: The highest shear bond strength values were found in groups G3 and G4 (22.01 ± 2.15 MPa and 22.83 ± 3.32 Mpa, respectively), followed by G1 (16.42 ± 3.61 MPa) and G2 (9.29 ± 1.95 MPa). As regards surface evaluation after bracket debonding, the use of liquid phosphoric acid followed by silane application (G2) produced the least damage to porcelain. When hydrofluoric acid and silane were applied, the risk of ceramic fracture increased. CONCLUSIONS: Acceptable levels of bond strength for clinical use were reached by all methods tested; however, liquid phosphoric acid etching followed by silane application (G2) resulted in the least damage to the ceramic surface. PMID:26352845

Surface modification for enhanced silanation of zirconia ceramics.

PubMed

Piascik, J R; Swift, E J; Thompson, J Y; Grego, S; Stoner, B R

2009-09-01

The overall goal of this research was to develop a practical method to chemically modify the surface of high strength dental ceramics (i.e. zirconia) to facilitate viable, robust adhesive bonding using commercially available silanes and resin cements. Investigation focused on a novel approach to surface functionalize zirconia with a Si(x)O(y) "seed" layer that would promote chemical bonding with traditional silanes. ProCAD and ZirCAD blocks were bonded to a dimensionally similar composite block using standard techniques designed for silica-containing materials (silane and resin cement). ZirCAD blocks were treated with SiCl4 by vapor deposition under two different conditions prior to bonding. Microtensile bars were prepared and subjected to tensile forces at a crosshead speed of 1 mm/min scanning electron microscopy was used to analyze fracture surfaces and determine failure mode; either composite cohesive failure (partial or complete cohesive failure within composite) or adhesive failure (partial or complete adhesive failure). Peak stress values were analyzed using single-factor ANOVA (p<0.05). Microtensile testing results revealed that zirconia with a surface treatment of 2.6 nm Si(x)O(y) thick "seed" layer was similar in strength to the porcelain group (control). Analysis of failure modes indicated the above groups displayed higher percentages of in-composite failures. Other groups tested had lower strength values and displayed adhesive failure characteristics. Mechanical data support that utilizing a gas-phase chloro-silane pretreatment to deposit ultra-thin silica-like seed layers can improve adhesion to zirconia using traditional silanation and bonding techniques. This technology could have clinical impact on how high strength dental materials are used today.

Plasma processes for producing silanes and derivatives thereof

DOEpatents

Laine, Richard M; Massey, Dean Richard; Peterson, Peter Young

2014-03-25

The invention is generally related to process for generating one or more molecules having the formula Si.sub.xH.sub.y, Si.sub.xD.sub.y, Si.sub.xH.sub.yD.sub.z, and mixtures thereof, where x,y and z are integers .gtoreq.1, H is hydrogen and D is deuterium, such as silane, comprising the steps of: providing a silicon containing material, wherein the silicon containing material includes at least 20 weight percent silicon atoms based on the total weight of the silicon containing material; generating a plasma capable of vaporizing a silicon atom, sputtering a silicon atom, or both using a plasma generating device; and contacting the plasma to the silicon containing material in a chamber having an atmosphere that includes at least about 0.5 mole percent hydrogen atoms and/or deuterium atoms based on the total moles of atoms in the atmosphere; so that a molecule having the formula Si.sub.xH.sub.y; (e.g., silane) is generated. The process preferably includes a step of removing one or more impurities from the Si.sub.xH.sub.y (e.g., the silane) to form a clean Si.sub.xH.sub.y, Si.sub.xD.sub.y, Si.sub.xH.sub.yD.sub.z (e.g., silane). The process may also include a step of reacting the Si.sub.xH.sub.y, Si.sub.xD.sub.y, Si.sub.xH.sub.yD.sub.z (e.g., the silane) to produce a high purity silicon containing material such as electronic grade metallic silicon, photovoltaic grade metallic silicon, or both.

Effect of curing and silanizing on composite repair bond strength using an improved micro-tensile test method

PubMed Central

Eliasson, Sigfus Thor; Dahl, Jon E.

2017-01-01

Abstract Objectives: To evaluate the micro-tensile repair bond strength between aged and new composite, using silane and adhesives that were cured or left uncured when new composite was placed. Methods: Eighty Filtek Supreme XLT composite blocks and four control blocks were stored in water for two weeks and thermo-cycled. Sandpaper ground, etched and rinsed specimens were divided into two experimental groups: A, no further treatment and B, the surface was coated with bis-silane. Each group was divided into subgroups: (1) Adper Scotchbond Multi-Purpose, (2) Adper Scotchbond Multi-Purpose adhesive, (3) Adper Scotchbond Universal, (4) Clearfil SE Bond and (5) One Step Plus. For each adhesive group, the adhesive was (a) cured according to manufacturer’s instructions or (b) not cured before repair. The substrate blocks were repaired with Filtek Supreme XLT. After aging, they were serially sectioned, producing 1.1 × 1.1 mm square test rods. The rods were prepared for tensile testing and tensile strength calculated at fracture. Type of fracture was examined under microscope. Results: Leaving the adhesive uncured prior to composite repair placement increased the mean tensile values statistically significant for all adhesives tested, with or without silane pretreatment. Silane surface treatment improved significantly (p < 0.001) tensile strength values for all adhesives, both for the cured and uncured groups. The mean strength of the control composite was higher than the strongest repair strength (p < 0.001). Conclusions: Application of freshly made silane and a thin bonding layer, rendered higher tensile bond strength. Not curing the adhesive before composite placement increased the tensile bond strength. PMID:28642928

An Ex-vivo Shear and tensile bond strengths of orthodontic molar tubes bonded using different techniques.

PubMed

Abu-Alhaija, Elham; Jaradat, Mohammad; Alwahadni, Ahed

2017-03-01

Molar bonding procedures need continuous improvement to be widely accepted clinically and eventually replace molar bands. The purpose of this study was to determine the effects of enamel micro-abrasion and silane coating of the base of molar tubes on shear and tensile bond strengths of orthodontic molar tubes. A total of 200 third molars were randomly allocated into five groups of 40 teeth as follows: group 1: molar tubes bonded to etched teeth (37% phosphoric acid gel; control group); group 2: molar tubes bonded to etched teeth (37% phosphoric acid) with the addition of silane to the base of molar tubes; group 3: molar tubes bonded to teeth pre-treated with 18% hydrochloric acid and pumice (micro-abrasion); group 4: molar tubes bonded to teeth pre-treated with microabrasion with the addition of silane to the base of molar tubes; group 5: molar tubes bonded to teeth pre-treated with microabrasion before conventional acid etching combined with the addition of silane to the base of molar tubes. The bond strength testing was performed using a computer control electromechanical universal testing machine. The highest mean shear and tensile bond strengths were recorded in group 5 (13.81±2.54MPa and 13.97±2.29 MPa, respectively). Micro-abrasion alone (group 3) and the combination of enamel micro-abrasion and the addition of silane (group 4) produced bond strength values comparable to the control. Enamel surface pre-treatment (micro abrasion) before conventional acid etching combined with the addition of silane to the base of the molar tube produced the highest bond strengths among all tested groups. Key words: Molar, shear strength, tensile strength, orthodontic appliances.

An Ex-vivo Shear and tensile bond strengths of orthodontic molar tubes bonded using different techniques

PubMed Central

Alwahadni, Ahed

2017-01-01

Background Molar bonding procedures need continuous improvement to be widely accepted clinically and eventually replace molar bands. Material and Methods The purpose of this study was to determine the effects of enamel micro-abrasion and silane coating of the base of molar tubes on shear and tensile bond strengths of orthodontic molar tubes. A total of 200 third molars were randomly allocated into five groups of 40 teeth as follows: group 1: molar tubes bonded to etched teeth (37% phosphoric acid gel; control group); group 2: molar tubes bonded to etched teeth (37% phosphoric acid) with the addition of silane to the base of molar tubes; group 3: molar tubes bonded to teeth pre-treated with 18% hydrochloric acid and pumice (micro-abrasion); group 4: molar tubes bonded to teeth pre-treated with microabrasion with the addition of silane to the base of molar tubes; group 5: molar tubes bonded to teeth pre-treated with microabrasion before conventional acid etching combined with the addition of silane to the base of molar tubes. The bond strength testing was performed using a computer control electromechanical universal testing machine. Results The highest mean shear and tensile bond strengths were recorded in group 5 (13.81±2.54MPa and 13.97±2.29 MPa, respectively). Micro-abrasion alone (group 3) and the combination of enamel micro-abrasion and the addition of silane (group 4) produced bond strength values comparable to the control. Conclusions Enamel surface pre-treatment (micro abrasion) before conventional acid etching combined with the addition of silane to the base of the molar tube produced the highest bond strengths among all tested groups. Key words:Molar, shear strength, tensile strength, orthodontic appliances. PMID:28298990

The influence of four dual-cure resin cements and surface treatment selection to bond strength of fiber post

PubMed Central

Liu, Chang; Liu, Hong; Qian, Yue-Tong; Zhu, Song; Zhao, Su-Qian

2014-01-01

In this study, we evaluate the influence of post surface pre-treatments on the bond strength of four different cements to glass fiber posts. Eighty extracted human maxillary central incisors and canines were endodontically treated and standardized post spaces were prepared. Four post pre-treatments were tested: (i) no pre-treatment (NS, control), (ii) sandblasting (SA), (iii) silanization (SI) and (iv) sandblasting followed by silanization (SS). Per pre-treatment, four dual-cure resin cements were used for luting posts: DMG LUXACORE Smartmix Dual, Multilink Automix, RelyX Unicem and Panavia F2.0. All the specimens were subjected to micro push-out test. Two-way analysis of variance and Tukey post hoc tests were performed (α=0.05) to analyze the data. Bond strength was significantly affected by the type of resin cement, and bond strengths of RelyX Unicem and Panavia F2.0 to the fiber posts were significantly higher than the other cement groups. Sandblasting significantly increased the bond strength of DMG group to the fiber posts. PMID:24177170

Integrating Nanostructured Artificial Receptors with Whispering Gallery Mode Optical Microresonators via Inorganic Molecular Imprinting Techniques

PubMed Central

Hammond, G. Denise; Vojta, Adam L.; Grant, Sheila A.; Hunt, Heather K.

2016-01-01

The creation of label-free biosensors capable of accurately detecting trace contaminants, particularly small organic molecules, is of significant interest for applications in environmental monitoring. This is achieved by pairing a high-sensitivity signal transducer with a biorecognition element that imparts selectivity towards the compound of interest. However, many environmental pollutants do not have corresponding biorecognition elements. Fortunately, biomimetic chemistries, such as molecular imprinting, allow for the design of artificial receptors with very high selectivity for the target. Here, we perform a proof-of-concept study to show how artificial receptors may be created from inorganic silanes using the molecular imprinting technique and paired with high-sensitivity transducers without loss of device performance. Silica microsphere Whispering Gallery Mode optical microresonators are coated with a silica thin film templated by a small fluorescent dye, fluorescein isothiocyanate, which serves as our model target. Oxygen plasma degradation and solvent extraction of the template are compared. Extracted optical devices are interacted with the template molecule to confirm successful sorption of the template. Surface characterization is accomplished via fluorescence and optical microscopy, ellipsometry, optical profilometry, and contact angle measurements. The quality factors of the devices are measured to evaluate the impact of the coating on device sensitivity. The resulting devices show uniform surface coating with no microstructural damage with Q factors above 106. This is the first report demonstrating the integration of these devices with molecular imprinting techniques, and could lead to new routes to biosensor creation for environmental monitoring. PMID:27314397

Reflectometric measurement of n-hexane adsorption on ZnO2 nanohybrid film modified by hydrophobic gold nanoparticles

NASA Astrophysics Data System (ADS)

Sebők, Dániel; Csapó, Edit; Ábrahám, Nóra; Dékány, Imre

2015-04-01

Zinc-peroxide/poly(styrenesulfonate) nanohybrid thin films (containing 20 bilayers: [ZnO2/PSS]20, d ∼ 500 nm) were prepared using layer-by-layer (LbL) method. The thin film surface was functionalized by different surface modifying agents (silanes, alkylthiols and hydrophobized nanoparticles). Based on the experimental results of quartz crystal microbalance (QCM) and contact angle measurements (as prequalifications) the octanethiol covered gold nanoparticles (OT-AuNPs) were selected for further vapour adsorption studies. Reflectometric interference spectroscopy (RIfS) was used to measure n-hexane vapour adsorption on the original and modified nanohybrid films in a gas flow platform. The thin film provides only the principle of the measurement (by interference phenomenon), the selectivity and hydrophobicity is controlled and enhanced by surface functionalization (by dispersion interaction between the alkyl chains). The interference pattern shift (Δλ) caused by the increase of the optical thickness of the thin film due to vapour adsorption was investigated. It was found that due to the surface functionalization by hydrophobic nanoparticles the effect of water vapour adsorption decreased significantly, while for n-hexane opposite tendency was observed (the effective refractive index and thus the interference pattern shift increased drastically). The correlation between QCM technique and optical method (RIfS) was specified: linear specific adsorbed amount vs. wavelength shift calibration curves were determined in the pr = 0-0.4 relative vapour pressure range. The thin film is suitable for sensorial application (e.g. volatile organic compound/VOC sensor).

Low-cost Solar Array Project. Feasibility of the Silane Process for Producing Semiconductor-grade Silicon

NASA Technical Reports Server (NTRS)

1979-01-01

The feasibility of Union Carbide's silane process for commercial application was established. An integrated process design for an experimental process system development unit and a commercial facility were developed. The corresponding commercial plant economic performance was then estimated.

Characterization of immobilization methods of antiviral antibodies in serum for electrochemical biosensors

NASA Astrophysics Data System (ADS)

Huy, Tran Quang; Hanh, Nguyen Thi Hong; Van Chung, Pham; Anh, Dang Duc; Nga, Phan Thi; Tuan, Mai Anh

2011-06-01

In this paper, we describes different methods to immobilize Japanese encephalitis virus (JEV) antibodies in human serum onto the interdigitated surface of a microelectrode sensor for optimizing electrochemical detection: (1) direct covalent binding to the silanized surface, (2) binding to the silanized surface via a cross-linker of glutaraldehyde (GA), (3) binding to glutaraldehyde/silanized surface via goat anti-human IgG polyclonal antibody and (4) binding to glutaraldehyde/silanized surface via protein A (PrA). Field emission scanning electron microscopy, Fourier transform infrared spectrometry, and fluorescence microscopy are used to verify the characteristics of antibodies on the interdigitated surface after the serum antibodies immobilization. The analyzed results indicate that the use of protein A is an effective choice for immobilization and orientation of antibodies in serum for electrochemical biosensors. This study provides an advantageous immobilization method of serum containing antiviral antibodies to develop electrochemical biosensors for preliminary screening of viruses in clinical samples from outbreaks.

Homoleptic ligands vs heteroleptic ligands on coordination polymerizations: Construction and properties of silver(I) coordination polymers containing dialkylbis(4-pyridy)silanes

NASA Astrophysics Data System (ADS)

Park, Minwoo; Jang, Jaeseong; Moon, So Yun; Jung, Ok-Sang

2014-03-01

Investigations into pure bidentate ligand vs mixed bidentate ligands on self-assembly of AgPF6 with the respective L1, L2, L3, L1/L2, L1/L3, and L2/L3 (L1 = diethylbis(4-pyridyl)silane; L2 = ethylmethylbis(4-pyridyl)silane; L3 = cyclotetramethylenebis(4-pyridyl)silane) were carried out. The self-assembly reactions of AgPF6 with the respective ligand system produce desirable homoleptic or heteroleptic silver(I) coordination polymers. [Ag(L1)2](PF6) gives rise to a tubular loop chain whereas the other five products lead to a twofold interpenetration diamonoid structure. [Ag(L1)2](PF6) shows a strong blue luminescence at 453 nm (λex = 270 nm), which is useful to recognize alcohols. All products were characterized by thermal analyses, and in particular, calcination of [Ag(L3)2](PF6)ṡCH3OH at 600 °C finally produces silver(0) microcrystalline morphology.

Development of processes for the production of solar grade silicon from halides and alkali metals, phase 1 and phase 2

NASA Technical Reports Server (NTRS)

Dickson, C. R.; Gould, R. K.; Felder, W.

1981-01-01

High temperature reactions of silicon halides with alkali metals for the production of solar grade silicon are described. Product separation and collection processes were evaluated, measure heat release parameters for scaling purposes and effects of reactants and/or products on materials of reactor construction were determined, and preliminary engineering and economic analysis of a scaled up process were made. The feasibility of the basic process to make and collect silicon was demonstrated. The jet impaction/separation process was demonstrated to be a purification process. The rate at which gas phase species from silicon particle precursors, the time required for silane decomposition to produce particles, and the competing rate of growth of silicon seed particles injected into a decomposing silane environment were determined. The extent of silane decomposition as a function of residence time, temperature, and pressure was measured by infrared absorption spectroscopy. A simplistic model is presented to explain the growth of silicon in a decomposing silane enviroment.

Adsorption behavior of glycidoxypropyl-trimethoxy-silane on titanium alloy Ti-6.5Al-1Mo-1V-2Zr

NASA Astrophysics Data System (ADS)

Liu, Jian-hua; Zhan, Zhong-wei; Yu, Mei; Li, Song-mei

2013-01-01

The adsorption behavior of glycidoxypropyl-trimethoxy-silane (GTMS) on titanium alloy Ti-6.5Al-1Mo-1V-2Zr was investigated by using X-ray photoelectron spectroscopy (XPS), Tafel polarization test, and electrochemical impedance spectroscopy (EIS). From the XPS results, it was found that the silane coverage on the titanium surface generally increased with GTMS concentration, with a slight decrease at concentration of 0.1%. Based on the relationship between isoelectronic point (IEP) of titanium surface and the pH values of silane solutions, adsorption mechanisms at different concentrations were proposed. The surface coverage data of GTMS on titanium surface was also derived from electrochemical measurements. By linear fitting the coverage data, it revealed that the adsorption of GTMS on the titanium alloy surface at 30 °C was of a physisorption-based mechanism, and obeyed Langmuir adsorption isotherm. The adsorption equilibrium constant (Kads) and free energy of adsorption process (ΔGads) were calculated to elaborate the mechanism of GTMS adsorption.

Silver Makes Better Electrical Contacts to Thiol-Terminated Silanes than Gold.

PubMed

Li, Haixing; Su, Timothy A; Camarasa-Gómez, María; Hernangómez-Pérez, Daniel; Henn, Simon E; Pokorný, Vladislav; Caniglia, Caravaggio D; Inkpen, Michael S; Korytár, Richard; Steigerwald, Michael L; Nuckolls, Colin; Evers, Ferdinand; Venkataraman, Latha

2017-11-06

We report that the single-molecule junction conductance of thiol-terminated silanes with Ag electrodes are higher than the conductance of those formed with Au electrodes. These results are in contrast to the trends in the metal work function Φ(Ag)<Φ(Au). As such, a better alignment of the Au Fermi level to the molecular orbital of silane that mediates charge transport would be expected. This conductance trend is reversed when we replace the thiols with amines, highlighting the impact of metal-S covalent and metal-NH 2 dative bonds in controlling the molecular conductance. Density functional theory calculations elucidate the crucial role of the chemical linkers in determining the level alignment when molecules are attached to different metal contacts. We also demonstrate that conductance of thiol-terminated silanes with Pt electrodes is lower than the ones formed with Au and Ag electrodes, again in contrast to the trends in the metal work-functions. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fluidized-bed reactor modeling for production of silicon by silane pyrolysis

NASA Technical Reports Server (NTRS)

Dudukovic, M. P.; Ramachandran, P. A.; Lai, S.

1986-01-01

An ideal backmixed reactor model (CSTR) and a fluidized bed bubbling reactor model (FBBR) were developed for silane pyrolysis. Silane decomposition is assumed to occur via two pathways: homogeneous decomposition and heterogeneous chemical vapor deposition (CVD). Both models account for homogeneous and heterogeneous silane decomposition, homogeneous nucleation, coagulation and growth by diffusion of fines, scavenging of fines by large particles, elutriation of fines and CVD growth of large seed particles. At present the models do not account for attrition. The preliminary comparison of the model predictions with experimental results shows reasonable agreement. The CSTR model with no adjustable parameter yields a lower bound on fines formed and upper estimate on production rates. The FBBR model overpredicts the formation of fines but could be matched to experimental data by adjusting the unkown jet emulsion exchange efficients. The models clearly indicate that in order to suppress the formation of fines (smoke) good gas-solid contacting in the grid region must be achieved and the formation of the bubbles suppressed.

Enhancing stability and efficiency of perovskite solar cells with crosslinkable silane-functionalized and doped fullerene

DOE PAGES

Bai, Yang; Dong, Qingfeng; Shao, Yuchuan; ...

2016-10-05

The instability of hybrid perovskite materials due to water and moisture arises as one major challenge to be addressed before any practical application of the demonstrated high efficiency perovskite solar cells. Here we report a facile strategy that can simultaneously enhance the stability and efficiency of p-i-n planar heterojunction-structure perovskite devices. Crosslinkable silane molecules with hydrophobic functional groups are bonded onto fullerene to make the fullerene layer highly water-resistant. Methylammonium iodide is introduced in the fullerene layer for n-doping via anion-induced electron transfer, resulting in dramatically increased conductivity over 100-fold. With crosslinkable silane-functionalized and doped fullerene electron transport layer, themore » perovskite devices deliver an efficiency of 19.5% with a high fill factor of 80.6%. Furthermore, a crosslinked silane-modified fullerene layer also enhances the water and moisture stability of the non-sealed perovskite devices by retaining nearly 90% of their original efficiencies after 30 days’ exposure in an ambient environment.« less

Light-weight black ceramic insulation

NASA Technical Reports Server (NTRS)

Hsu, Ming-Ta S. (Inventor); Chen, Timothy S. (Inventor)

2003-01-01

Ultra-high temperature, light-weight, black ceramic insulation having a density ranging from about 0.12 g/cc. to 0.6 g/cc. such as ceramic tile is obtained by pyrolyzing siloxane gels derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes also may contain an effective amount of a mono- or trialkoxy silane to obtain the siloxane gels. The siloxane gels are dried at ambient temperatures and pressures to form siloxane ceramic precursors without significant shrinkage. The siloxane ceramic precursors are subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C., and particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.

Enhancing stability and efficiency of perovskite solar cells with crosslinkable silane-functionalized and doped fullerene

PubMed Central

Bai, Yang; Dong, Qingfeng; Shao, Yuchuan; Deng, Yehao; Wang, Qi; Shen, Liang; Wang, Dong; Wei, Wei; Huang, Jinsong

2016-01-01

The instability of hybrid perovskite materials due to water and moisture arises as one major challenge to be addressed before any practical application of the demonstrated high efficiency perovskite solar cells. Here we report a facile strategy that can simultaneously enhance the stability and efficiency of p–i–n planar heterojunction-structure perovskite devices. Crosslinkable silane molecules with hydrophobic functional groups are bonded onto fullerene to make the fullerene layer highly water-resistant. Methylammonium iodide is introduced in the fullerene layer for n-doping via anion-induced electron transfer, resulting in dramatically increased conductivity over 100-fold. With crosslinkable silane-functionalized and doped fullerene electron transport layer, the perovskite devices deliver an efficiency of 19.5% with a high fill factor of 80.6%. A crosslinked silane-modified fullerene layer also enhances the water and moisture stability of the non-sealed perovskite devices by retaining nearly 90% of their original efficiencies after 30 days' exposure in an ambient environment. PMID:27703136

Facile and high-efficient immobilization of histidine-tagged multimeric protein G on magnetic nanoparticles

NASA Astrophysics Data System (ADS)

Lee, Jiho; Chang, Jeong Ho

2014-12-01

This work reports the high-efficient and one-step immobilization of multimeric protein G on magnetic nanoparticles. The histidine-tagged (His-tag) recombinant multimeric protein G was overexpressed in Escherichia coli BL21 by the repeated linking of protein G monomers with a flexible linker. High-efficient immobilization on magnetic nanoparticles was demonstrated by two different preparation methods through the amino-silane and chloro-silane functionalization on silica-coated magnetic nanoparticles. Three kinds of multimeric protein G such as His-tag monomer, dimer, and trimer were tested for immobilization efficiency. For these tests, bicinchoninic acid (BCA) assay was employed to determine the amount of immobilized His-tag multimeric protein G. The result showed that the immobilization efficiency of the His-tag multimeric protein G of the monomer, dimer, and trimer was increased with the use of chloro-silane-functionalized magnetic nanoparticles in the range of 98% to 99%, rather than the use of amino-silane-functionalized magnetic nanoparticles in the range of 55% to 77%, respectively.

Synthesis route and three different core-shell impacts on magnetic characterization of gadolinium oxide-based nanoparticles as new contrast agents for molecular magnetic resonance imaging

NASA Astrophysics Data System (ADS)

Azizian, Gholamreza; Riyahi-Alam, Nader; Haghgoo, Soheila; Moghimi, Hamid Reza; Zohdiaghdam, Reza; Rafiei, Behrooz; Gorji, Ensieh

2012-10-01

Despite its good resolution, magnetic resonance imaging intrinsically has low sensitivity. Recently, contrast agent nanoparticles have been used as sensitivity and contrast enhancer. The aim of this study was to investigate a new controlled synthesis method for gadolinium oxide-based nanoparticle preparation. For this purpose, diethyleneglycol coating of gadolinium oxide (Gd2O3-DEG) was performed using new supervised polyol route, and small particulate gadolinium oxide (SPGO) PEGylation was obtained with methoxy-polyethylene-glycol-silane (550 and 2,000 Da) coatings as SPGO-mPEG-silane550 and 2,000, respectively. Physicochemical characterization and magnetic properties of these three contrast agents in comparison with conventional Gd-DTPA were verified by dynamic light scattering transmission electron microscopy, Fourier transform infrared spectroscopy, inductively coupled plasma, X-ray diffraction, vibrating sample magnetometer, and the signal intensity and relaxivity measurements were performed using 1.5-T MRI scanner. As a result, the nanoparticle sizes of Gd2O3-DEG, SPGO-mPEG-silane550, and SPGO-mPEG-silane2000 could be reached to 5.9, 51.3, 194.2 nm, respectively. The image signal intensity and longitudinal ( r 1) and transverse relaxivity ( r 2) measurements in different concentrations (0.3 to approximately 2.5 mM), revealed the r 2/ r 1 ratios of 1.13, 0.89, 33.34, and 33.72 for Gd-DTPA, Gd2O3-DEG, SPGO-mPEG-silane550, and SPGO-mPEG-silane2000, respectively. The achievement of new synthesis route of Gd2O3-DEG resulted in lower r 2/ r 1 ratio for Gd2O3-DEG than Gd-DTPA and other previous synthesized methods by this and other groups. The smaller r 2/ r 1 ratios of two PEGylated-SPGO contrast agents in our study in comparison with r 2/ r 1 ratio of previous PEGylation ( r 2/ r 1 = 81.9 for mPEG-silane 6,000 MW) showed that these new three introduced contrast agents could potentially be proper contrast enhancers for cellular and molecular MR imaging.

Tetra­kis(2,3,5,5-tetra­methyl­hexen-2-yl)silane

PubMed Central

Meyer-Wegner, Frank; Bolte, Michael; Lerner, Hans-Wolfram

2014-01-01

In the title compound, C40H76Si, the Si atom is located on a special position of site symmetry -4. Thus, there is just a quarter of a mol­ecule in the asymmetric unit. The C=C double bonds exhibit a trans configuration. The Si atom and the tert-butyl group are located on the same side of the plane formed by the C=C double bond and its four substituents. The crystal packing shows no short contacts between the mol­ecules and despite the low crystal density (0.980 Mg m−3), there are no significant voids in the structure. PMID:24765057

Non-aqueous electrolytes for electrochemical cells

DOEpatents

Dong, Jian; Zhang, Zhengcheng; Amine, Khalil

2016-07-12

A electrolyte for a lithium battery includes a silane/siloxane compound represented by SiR.sub.4-x-yR'.sub.xR''.sub.y, by Formula II, or Formula III: ##STR00001## where each R is individually an alkenyl, alkynyl, alk(poly)enyl, alk(poly)ynyl, aryl; each R' is represented by; ##STR00002## each R'' is represented by Formula I-B; ##STR00003## R.sup.1 is an organic spacer; R.sup.2 is a bond or an organic spacer; R.sup.3 is alkyl or aryl; k is 1-15; m is 1-15; n is 1 or 2; p is 1-3; x' is 1-2; and y' is 0-2.

Methods for attaching polymerizable ceragenins to water treatment membranes using silane linkages

DOEpatents

Hibbs, Michael; Altman, Susan J.; Jones, Howland D. T.; Savage, Paul B.

2013-09-10

This invention relates to methods for chemically grafting and attaching ceragenin molecules to polymer substrates; methods for synthesizing ceragenin-containing copolymers; methods for making ceragenin-modified water treatment membranes and spacers; and methods of treating contaminated water using ceragenin-modified treatment membranes and spacers. Ceragenins are synthetically produced antimicrobial peptide mimics that display broad-spectrum bactericidal activity. Alkene-functionalized ceragenins (e.g., acrylamide-functionalized ceragenins) can be attached to polyamide reverse osmosis membranes using amine-linking, amide-linking, UV-grafting, or silane-coating methods. In addition, silane-functionalized ceragenins can be directly attached to polymer surfaces that have free hydroxyls.

40 CFR 721.6920 - Butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted...

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Butyl acrylate, polymer with... acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane. (a... butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane...

40 CFR 721.6920 - Butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted...

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Butyl acrylate, polymer with... acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane. (a... butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane...

40 CFR 721.6920 - Butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted...

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Butyl acrylate, polymer with... acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane. (a... butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane...

40 CFR 721.6920 - Butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted...

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Butyl acrylate, polymer with... acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane. (a... butyl acrylate, polymer with substituted methyl styrene, methyl methacrylate, and substituted silane...

Production of hybrid lipid-based particles loaded with inorganic nanoparticles and active compounds for prolonged topical release.

PubMed

García-González, C A; Sampaio da Sousa, A R; Argemí, A; López Periago, A; Saurina, J; Duarte, C M M; Domingo, C

2009-12-01

The production of particulate hybrid carriers containing a glyceryl monostearate (Lumulse GMS-K), a waxy triglyceride (Cutina HR), silanized TiO(2) and caffeine were investigated with the aim of producing sunscreens with UV-radiation protection properties. Particles were obtained using the supercritical PGSS (Particles from Gas Saturated Solutions) technique. This method takes advantages of the lower melting temperatures of the lipids obtained from the dissolution of CO(2) in the bulk mixture. Experiments were performed at 13 MPa and 345 K, according to previous melting point measurements. Blends containing Lumulse GMS-K and Cutina HR lipids (50 wt%) were loaded with silanized TiO(2) and caffeine in percentile proportions of 6 and 4 wt%, respectively. The particles produced were characterized using several analytical techniques as follows: system crystallinity was checked by X-ray diffraction and differential scanning calorimetry, thermal stability by thermogravimetric analysis, and morphology by scanning and transmission electron microscopy. Further, the UV-shielding ability of TiO(2) after its dispersion in the lipidic matrix was assessed by solid UV-vis spectroscopy. Preliminary results indicated that caffeine-loaded solid lipid particles presented a two-step dissolution profile, with an initial burst of 60 wt% of the loaded active agent. Lipid blends loaded with TiO(2) and caffeine encompassed the UV-filter behavior of TiO(2) and the photoaging prevention properties of caffeine.

Reduced adherence of Candida to silane-treated silicone rubber.

PubMed

Price, C L; Williams, D W; Waters, M G J; Coulthwaite, L; Verran, J; Taylor, R L; Stickler, D; Lewis, M A O

2005-07-01

Silicone rubber is widely used in the construction of medical devices that can provide an essential role in the treatment of human illness. However, subsequent microbial colonization of silicone rubber can result in clinical infection or device failure. The objective of this study was to determine the effectiveness of a novel silane-treated silicone rubber in inhibiting microbial adherence and material penetration. Test material was prepared by a combination of argon plasma discharge treatment and fluorinated silane coupling. Chemicophysical changes were then confirmed by X-ray photoelectron spectroscopy, contact-angle measurement, and atomic force microscopy. Two separate adherence assays and a material penetration assay assessed the performance of the new material against four strains of Candida species. Results showed a significant reduction (p < 0.01) of Candida albicans GDH 2346 adherence to silane-treated silicone compared with untreated controls. This reduction was still evident after the incorporation of saliva into the assay. Adherence inhibition also occurred with Candida tropicalis MMU and Candida krusei NCYC, although this was assay dependent. Reduced penetration of silane-treated silicone by Candida was evident when compared to untreated controls, plaster-processed silicone, and acrylic-processed silicone. To summarize, a novel silicone rubber material is described that inhibits both candidal adherence and material penetration. The clinical benefit and performance of this material remains to be determined. Copyright 2005 Wiley Periodicals, Inc.

Molecular structures of (3-aminopropyl)trialkoxysilane on hydroxylated barium titanate nanoparticle surfaces induced by different solvents and their effect on electrical properties of barium titanate based polymer nanocomposites

NASA Astrophysics Data System (ADS)

Fan, Yanyan; Wang, Guanyao; Huang, Xingyi; Bu, Jing; Sun, Xiaojin; Jiang, Pingkai

2016-02-01

Surface modification of nanoparticles by grafting silane coupling agents has proven to be a significant approach to improve the interfacial compatibility between inorganic filler and polymer matrix. However, the impact of grafted silane molecular structure after the nanoparticle surface modification, induced by the utilized solvents and the silane alkoxy groups, on the electrical properties of the corresponding nanocomposites, has been seldom investigated. Herein, the silanization on the surface of hydroxylated barium titanate (BT-OH) nanoparticles was introduced by using two kinds of trialkoxysilane, 3-aminopropyltriethoxysilane (AMEO) and 3-aminopropyltrimethoxysilane (AMMO), with different solvents (toluene and ethanol), respectively. Solid-state 13C, 29Si nuclear magnetic resonance (NMR) spectroscopy and high-resolution X-ray photoelectron spectroscopy (XPS) were employed to validate the structure differences of alkoxysilane attachment to the nanoparticles. The effect of alkoxysilane structure attached to the nanoparticle surface on the dielectric properties of the BT based poly(vinylidene fluoride) (PVDF) nanocomposites were investigated. The results reveal that the solvents used for BT nanoparticle surface modification exhibit a significant effect on the breakdown strength of the nanocomposites. Nevertheless, the alkoxy groups of silane show a marginal influence on the dielectric properties of the nanocomposites. These research results provide important insights into the fabrication of advanced polymer nanocomposites for dielectric applications.

Reaction of silanes in supercritical CO2 with TiO2 and Al2O3.

PubMed

Gu, Wei; Tripp, Carl P

2006-06-20

Infrared spectroscopy was used to investigate the reaction of silanes with TiO2 and Al2O3 using supercritical CO2 (Sc-CO2) as a solvent. It was found that contact of Sc-CO2 with TiO2 leads to partial removal of the water layer and to the formation of carbonate, bicarbonate, and carboxylate species on the surface. Although these carbonate species are weakly bound to the TiO2 surface and can be removed by a N2 purge, they poison the surface, resulting in a lower level of reaction of silanes with TiO2. Specifically, the amount of hexamethyldisilazane adsorbed on TiO2 is about 10% of the value obtained when the reaction is performed from the gas phase. This is not unique to TiO2, as the formation of carbonate species also occurs upon contact of Al2O3 with Sc-CO2 and this leads to a lower level of reaction with hexamethyldisilazane. This is in contrast to reactions of silanes on SiO2 where Sc-CO2 has several advantages over conventional gaseous or nonaqueous methods. As a result, caution needs to be applied when using Sc-CO2 as a solvent for silanization reactions on oxides other than SiO2.

Interfacial properties of aluminum/glass-fiberreinforced polypropylene sandwich composites

NASA Astrophysics Data System (ADS)

Baştürk, S. B.; Guruşçu, A.; Tanoğlu, M.

2013-07-01

Aluminum/glass-fiber-reinforced polypropylene (Al/GFPP) laminates were manufactured by using various surface pretreatment techniques. Adhesion at the composite/metal interface was achieved by a surface pretreatment of Al sheets with amino-based silane coupling agents, incorporation of a polyolefin-based adhesive film and modification with a PP-based film containing 20 wt.% of maleic-anhydride-modified polypropylene (PP-g-MA). In order to increase the effect of bonding between components of the laminates, the combination of silane treatment and the addition of the PP-based film was also investigated. The mechanical properties (shear, peel, and bending strengths) of adhesively bonded Al/GFPP laminates were examined to evaluate the effects of the surface treatments mentioned. It was revealed that the adhesion in the laminated Al/GFPP systems could be improved by the treatment of aluminum surface with an amino-based silane coupling agent. Judging from the results of peel and bending strength, with incorporation of polyolefin-based films, adhesion in the Al/GFPP laminates increased significantly. The modification of Al/GFPP interfaces with a PP-g-MA/PP layer led to the highest improvement in their adhesion properties. The combination of surface modification with silane and addition of PP-based films did not yield the high bending strength desired. This may be due to the insufficient bonding between silane groups and PP-based films.

Adhesive strength of total knee endoprostheses to bone cement - analysis of metallic and ceramic femoral components under worst-case conditions.

PubMed

Bergschmidt, Philipp; Dammer, Rebecca; Zietz, Carmen; Finze, Susanne; Mittelmeier, Wolfram; Bader, Rainer

2016-06-01

Evaluation of the adhesive strength of femoral components to the bone cement is a relevant parameter for predicting implant safety. In the present experimental study, three types of cemented femoral components (metallic, ceramic and silica/silane-layered ceramic) of the bicondylar Multigen Plus knee system, implanted on composite femora were analysed. A pull-off test with the femoral components was performed after different load and several cementing conditions (four groups and n=3 components of each metallic, ceramic and silica/silane-layered ceramic in each group). Pull-off forces were comparable for the metallic and the silica/silane-layered ceramic femoral components (mean 4769 N and 4298 N) under standard test condition, whereas uncoated ceramic femoral components showed reduced pull-off forces (mean 2322 N). Loading under worst-case conditions led to decreased adhesive strength by loosening of the interface implant and bone cement using uncoated metallic and ceramic femoral components, respectively. Silica/silane-coated ceramic components were stably fixed even under worst-case conditions. Loading under high flexion angles can induce interfacial tensile stress, which could promote early implant loosening. In conclusion, a silica/silane-coating layer on the femoral component increased their adhesive strength to bone cement. Thicker cement mantles (>2 mm) reduce adhesive strength of the femoral component and can increase the risk of cement break-off.

Hardness of model dental composites - the effect of filler volume fraction and silanation.

PubMed

McCabe, J F; Wassell, R W

1999-05-01

The relationship between structure and mechanical properties for dental composites has often proved difficult to determine due to the use of commercially available materials having a number of differences in composition i.e. different type of resin, different type of filler, etc. This makes a scientific study of any one variable such as filler content difficult if not impossible. In the current study it was the aim to test the hypothesis that hardness measurements of dental composites could be used to monitor the status of the resin-filler interface and to determine the efficacy of any particle silanation process. Ten model composites formulated from a single batch of resin and containing a common type of glass filler were formulated to contain varying amounts of filler. Some materials contained silanated filler, others contained unsilanated filler. Specimens were prepared and stored in water and hardness (Vickers') was determined at 24 h using loads of 50, 100, 200 and 300 g. Composites containing silanated fillers were significantly harder than materials containing unsilanated fillers. For unsilanated products hardness was independent of applied load and in this respect they behaved like homogeneous materials. For composites containing silanated fillers there was a marked increase in measured hardness as applied load was increased. This suggests that the hardness-load profile could be used to monitor the status of the resin-filler interface. Copyright 1999 Kluwer Academic Publishers

Functionalized sorbent for chemical separations and sequential forming process

DOEpatents

Fryxell, Glen E [Kennewick, WA; Zemanian, Thomas S [Richland, WA

2012-03-20

A highly functionalized sorbent and sequential process for making are disclosed. The sorbent includes organic short-length amino silanes and organic oligomeric polyfunctional amino silanes that are dispersed within pores of a porous support that form a 3-dimensional structure containing highly functionalized active binding sites for sorption of analytes.

Spatial Concentrations of Silicon Atoms in RF Discharges of Silane.

DTIC Science & Technology

1985-02-18

regions. These profiles were much more sensitive to plasma chemistry changes than profiles obtained from plasma emission. Experiments with nitrogen...addition demonstrated significant changes in the silicon atom profiles near the sheath boundary. Originator supplied keywords include: rf discharge, silane, plasma chemistry , silicon atom, laser-induced fluorescence.

Heterogeneous decomposition of silane in a fixed bed reactor

NASA Technical Reports Server (NTRS)

Iya, S. K.; Flagella, R. N.; Dipaolo, F. S.

1982-01-01

Heterogeneous decomposition of silane in a fluidized bed offers an attractive route for the low-cost production of silicon for photovoltaic application. To obtain design data for a fluid bed silane pyrolysis reactor, deposition experiments were conducted in a small-scale fixed bed apparatus. Data on the decomposition mode, plating rate, and deposition morphology were obtained in the temperature range 600-900 C. Conditions favorable for heterogeneous decomposition with good deposition morphology were identified. The kinetic rate data showed the reaction to be first order with an activation energy of 38.8 kcal/mol, which agrees well with work done by others. The results are promising for the development of an economically attractive fluid bed process.

Effect of silane/hydrogen ratio on microcrystalline silicon thin films by remote inductively coupled plasma

NASA Astrophysics Data System (ADS)

Guo, Y. N.; Wei, D. Y.; Xiao, S. Q.; Huang, S. Y.; Zhou, H. P.; Xu, S.

2013-05-01

Hydrogenated microcrystalline silicon (μc-Si:H) thin films were prepared by remote low frequency inductively coupled plasma (ICP) chemical vapor deposition system, and the effect of silane/hydrogen ratio on the microstructure and electrical properties of μc-Si:H films was systematically investigated. As silane/hydrogen ratio increases, the crystalline volume fraction Fc decreases and the ratio of the intensity of (220) peak to that of (111) peak drops as silane flow rate is increased. The FTIR result indicates that the μc-Si:H films prepared by remote ICP have a high optical response with a low hydrogen content, which is in favor of reducing light-induced degradation effect. Furthermore, the processing window of the phase transition region for remote ICP is much wider than that for typical ICP. The photosensitivity of μc-Si:H films can exceed 100 at the transition region and this ensures the possibility of the fabrication of microcrystalline silicon thin film solar cells with a open-circuit voltage of about 700 mV.

Protein attachment to silane-functionalized porous silicon: A comparison of electrostatic and covalent attachment.

PubMed

Baranowska, Malgorzata; Slota, Agata J; Eravuchira, Pinkie J; Alba, Maria; Formentin, Pilar; Pallarès, Josep; Ferré-Borrull, Josep; Marsal, Lluís F

2015-08-15

Porous silicon (pSi) is a prosperous biomaterial, biocompatible, and biodegradable. Obtaining regularly functionalized pSi surfaces is required in many biotechnology applications. Silane-PEG-NHS (triethoxysilane-polyethylene-glycol-N-hydroxysuccinimide) is useful for single-molecule studies due to its ability to attach to only one biomolecule. We investigate the functionalization of pSi with silane-PEG-NHS and compare it with two common grafting agents: APTMS (3-aminopropylotrimethoxysilane) as electrostatic linker, and APTMS modified with glutaraldehyde as covalent spacer. We show the arrangement of two proteins (collagen and bovine serum albumin) as a function of the functionalization and of the pore size. FTIR is used to demonstrate correct functionalization while fluorescence confocal microscopy reveals that silane-PEG-NHS results in a more uniform protein distribution. Reflection interference spectroscopy (RIfS) is used to estimate the attachment of linker and proteins. The results open a way to obtain homogenous chemical modified silicon supports with a great value in biosensing, drug delivery and cell biology. Copyright © 2015 Elsevier Inc. All rights reserved.

Flat-plate solar array project. Volume 2: Silicon material

NASA Technical Reports Server (NTRS)

Lutwack, R.

1986-01-01

The goal of the Silicon Material Task, a part of the Flat Plate Solar Array (FSA) Project, was to develop and demonstate the technology for the low cost production of silicon of suitable purity to be used as the basic material for the manufacture of terrestrial photovoltaic solar cells. Summarized are 11 different processes for the production of silicon that were investigated and developed to varying extent by industrial, university, and Government researchers. The silane production section of the Union Carbide Corp. (UCC) silane process was developed completely in this program. Coupled with Siemens-type chemical vapor deposition reactors, the process was carried through the pilot stage. The overall UCC process involves the conversion of metallurgical-grade silicon to silane followed by decomposition of the silane to purified silicon. The other process developments are described to varying extents. Studies are reported on the effects of impurities in silicon on both silicon-material properties and on solar cell performance. These studies on the effects of impurities yielded extensive information and models for relating specific elemental concentrations to levels of deleterious effects.

Studies on silane to 70 GPa

NASA Astrophysics Data System (ADS)

Narayana, C.; Greene, R. G.; Ruoff, A. L.

2008-07-01

Raman and x-ray diffraction studies were made on silane in the diamond anvil cell using three different gaskets, stainless steel, tungsten and rhenium. The structure existing between 10 and 27 GPa is well characterized by the monoclinic space group P21c (#14). While the Gibbs free energy of formation of silane is positive at one atmosphere, it is calculated from the equation of state of silane and its reactants that this becomes negative near 4 GPa and remains negative until 13 GPa and then becomes positive again. At about 27 GPa, where quasi-quantum mechanical calculations suggest there should be a transformation from 4-fold to 6-fold (or even higher), the sample turns black. The Raman modes seize to exist beyond 30 GPa after showing softening above 25 GPa. At higher pressures it turns silvery. The gaskets play a different role as will be discussed. The sample brought back from 70 GPa contains amorphous Si (with attached hydrogen) as well as crystalline silicon. The lowest free energy system at high pressure is the decomposed reactants as observed.

Flat-plate solar array project. Volume 2: Silicon material

NASA Astrophysics Data System (ADS)

Lutwack, R.

1986-10-01

The goal of the Silicon Material Task, a part of the Flat Plate Solar Array (FSA) Project, was to develop and demonstate the technology for the low cost production of silicon of suitable purity to be used as the basic material for the manufacture of terrestrial photovoltaic solar cells. Summarized are 11 different processes for the production of silicon that were investigated and developed to varying extent by industrial, university, and Government researchers. The silane production section of the Union Carbide Corp. (UCC) silane process was developed completely in this program. Coupled with Siemens-type chemical vapor deposition reactors, the process was carried through the pilot stage. The overall UCC process involves the conversion of metallurgical-grade silicon to silane followed by decomposition of the silane to purified silicon. The other process developments are described to varying extents. Studies are reported on the effects of impurities in silicon on both silicon-material properties and on solar cell performance. These studies on the effects of impurities yielded extensive information and models for relating specific elemental concentrations to levels of deleterious effects.

Comparative Study of Solution Phase and Vapor Phase Deposition of Aminosilanes on Silicon Dioxide Surfaces

PubMed Central

Yadav, Amrita R.; Sriram, Rashmi; Carter, Jared A.; Miller, Benjamin L.

2014-01-01

The uniformity of aminosilane layers typically used for the modification of hydroxyl bearing surfaces such as silicon dioxide is critical for a wide variety of applications, including biosensors. However, in spite of many studies that have been undertaken on surface silanization, there remains a paucity of easy-to-implement deposition methods reproducibly yielding smooth aminosilane monolayers. In this study, solution- and vapor-phase deposition methods for three aminoalkoxysilanes differing in the number of reactive groups (3-aminopropyl triethoxysilane (APTES), 3-aminopropyl methyl diethoxysilane (APMDES) and 3-aminopropyl dimethyl ethoxysilane (APDMES)) were assessed with the aim of identifying methods that yield highly uniform and reproducible silane layers that are resistant to minor procedural variations. Silane film quality was characterized based on measured thickness, hydrophilicity and surface roughness. Additionally, hydrolytic stability of the films was assessed via these thickness and contact angle values following desorption in water. We found that two simple solution-phase methods, an aqueous deposition of APTES and a toluene based deposition of APDMES, yielded high quality silane layers that exhibit comparable characteristics to those deposited via vapor-phase methods. PMID:24411379

Characterization of electron-beam-modified surface coated clay fillers and their influence on physical properties of rubbers

NASA Astrophysics Data System (ADS)

Ray, Sudip; Bhowmick, Anil K.; Sarma, K. S. S.; Majali, A. B.; Tikku, V. K.

2002-12-01

A novel process of surface modification of clay filler has been developed by coating this with an acrylate monomer, trimethylol propane triacrylate (TMPTA) or a silane coupling agent, triethoxy vinyl silane (TEVS) followed by electron beam irradiation. Characterization of these surface modified fillers has been carried out by Fourier-transform infrared analysis (FTIR), electron spectroscopy for chemical analysis (ESCA), wettability by dynamic wicking method measuring the rise of a liquid through a filler-packed capillary tube and water flotation test, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). Presence of the acrylate and the silane coupling agent on the modified fillers has been confirmed from FTIR, ESCA, and EDX studies, which has also been supported by TGA studies. The contact angle measurement by dynamic wicking method suggests improvement in hydrophobicity of the treated fillers, which is supported by water flotation test especially in the case of silanized clay. However, XRD studies demonstrate that the entire modification process does not affect the bulk properties of the fillers. Finally, both unmodified and modified clay fillers have been incorporated in styrene butadiene rubber (SBR) and nitrile rubber (NBR). Rheometric and mechanical properties reveal that there is a definite improvement using these modified fillers specially in the case of silanized clay compared to the control sample, probably due to successful enhancement in interaction between the treated clay and the base polymer.

A novel combination of silane-coated silica colloid with hybrid RNA extraction protocol and RNA enrichment for downstream applications of spermatozoal RNA.

PubMed

Vijayalakshmy, K; Kumar, P; Virmani, M; Pawaria, S; Lalaji, N S; Sharma, P; Rajendran, R; Yadav, P S; Kumar, D

2018-05-14

Spermatozoa are specialised cells with low RNA content as compared to somatic cells. The suitable sperm RNA extraction and enrichment protocols for downstream applications are available for human, cattle, stallion and mouse but not for buffalo spermatozoa. Therefore, the present work was conducted to find out suitable colloidal solution for sperm purification and appropriate protocol for sperm RNA extraction and enrichment/amplification of RNA. For purification, we used PVP-coated silica colloidal solution (PVP-Si), silane-coated silica colloidal solution (Silane-Si) and iodixanol. Sperm recovery rate, total sperm motility and progressive sperm motility were significantly improved after separation by Silane-Si and iodixanol compared to PVA-Si method. The combined guanidinium thiocyanate-phenol-chloroform (GTPC) with silica matrix (SM)-based RNA extraction yielded more quantity of RNA in compared to individual method. The hybrid of SM and GTPC into a single protocol yielded 360-450 ng RNA from 30 million buffalo spermatozoa. For the first time, we adopted new way to enrich sperm RNA that increased the RNA concentration 4-5 times that was sufficient for downstream applications. The linear amplification of sperm RNA increased RNA concentration around 27-45 times. In summary, Silane-Si colloid for sperm separation, hybrid SM and GTPC protocol for sperm RNA extraction followed by enrichment or amplification of RNA was found suitable for high-throughput analyses of buffalo sperm RNA. © 2018 Blackwell Verlag GmbH.

Effects of age condition on the distribution and integrity of inorganic fillers in dental resin composites.

PubMed

D'Alpino, Paulo Henrique Perlatti; Svizero, Nádia da Rocha; Bim Júnior, Odair; Valduga, Claudete Justina; Graeff, Carlos Frederico de Oliveira; Sauro, Salvatore

2016-06-01

The aim of this study is to evaluate the distribution of the filler size along with the zeta potential, and the integrity of silane-bonded filler surface in different types of restorative dental composites as a function of the material age condition. Filtek P60 (hybrid composite), Filtek Z250 (small-particle filled composite), Filtek Z350XT (nanofilled composite), and Filtek Silorane (silorane composite) (3M ESPE) were tested at different stage condition (i.e., fresh/new, aged, and expired). Composites were submitted to an accelerated aging protocol (Arrhenius model). Specimens were obtained by first diluting each composite specimen in ethanol and then dispersed in potassium chloride solution (0.001 mol%). Composite fillers were characterized for their zeta potential, mean particle size, size distribution, via poly-dispersion dynamic light scattering. The integrity of the silane-bonded surface of the fillers was characterized by FTIR. The material age influenced significantly the outcomes; Zeta potential, filler characteristics, and silane integrity varied both after aging and expiration. Silorane presented the broadest filler distribution and lowest zeta potential. Nanofilled and silorane composites exhibited decreased peak intensities in the FTIR analysis, indicating a deficiency of the silane integrity after aging or expiry time. Regardless to the material condition, the hybrid and the small-particle-filled composites were more stable overtime as no significant alteration in filler size distribution, diameter, and zeta potential occurred. A deficiency in the silane integrity in the nanofilled and silorane composites seems to be affected by the material stage condition. The materials conditions tested in this study influenced the filler size distribution, the zeta potential, and integrity of the silane adsorbed on fillers in the nanofilled and silorane composites. Thus, this may result in a decrease of the clinical performance of aforementioned composites, in particular, if these are used after inappropriate storage conditions.

Modeling of the silane FBR system

NASA Technical Reports Server (NTRS)

Dudokovic, M. P.; Ramachandran, P. A.; Lai, S.

1984-01-01

Development of a mathematical model for fluidized bed pyrolysis of silane that relates production rate and product properties (size, size distribution, presence or absence of fines) with bed size and operating conditions (temperature, feed concentration, flow rate, seed size, etc.) and development of user oriented algorithm for the model are considered. A parameter sensitivity study of the model was also developed.

Profile extrusion and mechanical properties of crosslinked wood–thermoplastic composites

Treesearch

Magnus Bengtsson; Kristiina Oksman; Stark Nicole M.

2006-01-01

Challenges for wood-thermoplastic composites to be utilized in structural applications are to lower product weight and to improve the long-term load performance. Silane crosslinking of the composites is one way to reduce the creep during long-term loading and to improve the mechanical properties. In this study, silane crosslinked wood-polyethylene composites were...

Fluoroalkyl silane modified silicone rubber/nanoparticle composite: a super durable, robust superhydrophobic fabric coating.

PubMed

Zhou, Hua; Wang, Hongxia; Niu, Haitao; Gestos, Adrian; Wang, Xungai; Lin, Tong

2012-05-08

A superhydrophobic fabric coating made of a crosslinked polydimethylsiloxane elastomer, containing well-dispersed hydrophobic silica nanoparticles and fluorinated alkyl silane, shows remarkable durability against repeated machine washes, severe abrasion, strong acid or base, boiling water or beverages and excellent stain resistance. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improvement of thermal conductivities for silicone nanocomposite via incorporating poly(γ-methacryloxypropyltrimethoxy silane) grafted graphene fillers

NASA Astrophysics Data System (ADS)

Chen, Tian; Liu, Bo

2018-02-01

The proposed grafting polymerization of γ-methacryloxypropyltrimethoxy silane was performed to functionalize graphene, aiming to fabricate functionalized graphene/silicone with excellent thermal conductivities. The surface morphology and element content of poly(γ-methacryloxypropyltrimethoxy silane) grafted reduced graphene oxide (g-RGO) was characterized by Atomic force microscope (AFM) and X-ray photoelectron spectroscopy (XPS). The usage of g-RGO was benefit for improving the thermal conductivity of silicone (SI). The g-RGO/SI (2 wt% filler) had thermal conductivity of 1.31 W·m-1·K-1 and thermal diffusivity of 1.08 mm2·s-1 (increased by 620% compared to that of SI), which held potential for electronic packaging materials and micro-electro-mechanical systems apparatus.

Method of patterning an aerogel

DOEpatents

Reed, Scott T [Edgewood, NM

2012-07-24

A method for producing a pattern in an aerogel disposed as a coating on a substrate comprises exposing the aerogel coating to the vapors of a hydrophobic silane compound, masking the aerogel coating with a shadow photomask and irradiating the aerogel coating with ultraviolet (UV) irradiation. The exposure to UV through the shadow mask creates a pattern of hydrophobic and hydrophilic regions in the aerogel coating. Etching away the hydrophilic regions of the aerogel coating, preferably with a 1 molar solution of sodium hydroxide, leaves the unwetted and unetched hydrophobic regions of the aerogel layer on the substrate, replicating the pattern of the photomask. The hydrophobic aerogel pattern can be further exposed to UV irradiation if desired, to create a hydrophilic aerogel pattern.

Development of amorphous SiC for MEMS-based microbridges

NASA Astrophysics Data System (ADS)

Summers, James B.; Scardelletti, Maximilian; Parro, Rocco; Zorman, Christian A.

2007-02-01

This paper reports our effort to develop amorphous hydrogenated silicon carbide (a-SiC:H) films specifically designed for MEMS-based microbridges using methane and silane as the precursor gases. In our work, the a-SiC:H films were deposited in a simple, commercial PECVD system at a fixed temperature of 300°C. Films with thicknesses from 100 nm to 1000 nm, a typical range for many MEMS applications, were deposited. Deposition parameters such as deposition pressure and methane-to-silane ratio were varied in order to obtain films with suitable residual stresses. Average residual stress in the as-deposited films selected for device fabrication was found by wafer curvature measurements to be -658 +/- 22 MPa, which could be converted to 177 +/- 40 MPa after thermal annealing at 450°C, making them suitable for micromachined bridges, membranes and other anchored structures. Bulk micromachined membranes were constructed to determine the Young's modulus of the annealed films, which was found to be 205 +/- 6 GPa. Chemical inertness was tested in aggressive solutions such as KOH and HF. Prototype microbridge actuators were fabricated using a simple surface micromachining process to assess the potential of the a-SiC:H films as structural layers for MEMS applications.

Production of saturated and unsaturated silahydrocarbon mixtures using rhodium catalyst, and to products produced thereby

DOE Office of Scientific and Technical Information (OSTI.GOV)

Onopchenki, A.; Sabourin, E.T.

1986-02-25

This patent describes a process for the production of a mixture of saturated and unstaurated silahydrocarbons. This process contacts an admixture consisting of (A) at least one alpha-olefin containing from 2 to about 20 carbon atoms per molecule, and (B) at least one alkylsilane selected from the group consisting of (i) a dialkylsilane (ii) a trialkylsilane (iii) mixtures thereof, with a catalyst consisting of a homogeneous monomeric rhodium-containing catalyst having a basicity substantially equal to or less than that provided by a rhodium-containing catalyst having a triphenyl phosphine ligand or a heterogeneous rhodium-containing catalyst in a halogen-free inert solvent. Themore » process conducted at a temperature of from about 30/sup 0/ to about 200/sup 0/C., a weight ratio of olefin to alkylsilane of from about 0.5 to about 20 to one and a catalyst concentration of from about 1 x 10-/sup 5/ to about 1 x 10-/sup 2/ millimoles of catalyst per millimole alkylsilane, to produce a mixture containing saturated silane hydrocarbons and an unsaturated silahydrocarbon. Inclusive with the proviso that the molecular weight of the unsaturated silane hydrocarbon is above 300.« less

[Influence of different porcelain surface treatment method on the bonding of metal brackets to porcelain].

PubMed

Fan, Cun-Hui; Chen, Jie; Liu, Xin-Qiang; Ma, Xin

2005-08-01

To investigate the influence of different porcelain surface treatment methods on the shear bond strength of metal brackets bonded to porcelain. 80 porcelain facets were divided randomly into two groups according to different adhesive material that was used to bond metal brackets. Adhesive material were Jing-Jin enamel adhesive and light-cured composite resin. Each group was further divided into 4 subgroups according to different surface treatment methods, which were acid etching with 37% phosphoric acid (H3PO4), acid etching with 9.6% hydrofluoric acid (HF), deglazing by grinding and silanating the porcelain surface. All specimens were stored in 37 degrees C water for 24 hours and then the shear bond strength and the porcelain fracture after debonding was determined. The porcelain surfaces after HF etching, H3PO4 etching and deglazing by grinding were examined by scanning electron microscopy respectively. The shear bond strengths in the HF etching groups, the deglazing groups and the silanating groups were much greater than that in the phosphoric etching groups (P < 0.01). Adequate orthodontic bonding strength was achieved both when bonded with light-cured composite resin after deglazing by grinding and when bonded with either of these adhesives after HF etching or surface silanating. There were no differences in the rates of porcelain fractures among groups (P > 0.05). HF etching, deglazing by grinding and silanating can all increase the shear bond strength between metal bracket and porcelain. Surface silanating of porcelain is a better surface treatment when metal brackets bonded to porcelain.

Comparison of the Microtensile Bond Strength of a Polyetherketoneketone (PEKK) Tooth Post Cemented with Various Surface Treatments and Various Resin Cements.

PubMed

Song, Chan-Hong; Choi, Jae-Won; Jeon, Young-Chan; Jeong, Chang-Mo; Lee, So-Hyoun; Kang, Eun-Sook; Yun, Mi-Jung; Huh, Jung-Bo

2018-05-29

The aim of this in-vitro research was to evaluate the microtensile bond strength in the newly introduced PEKK tooth post with various surface treatments and resin cements. A fiberglass tooth post was included in order to compare it with PEKK as a possible post material. The microtensile bond strengths of the fiberglass post (FRC Postec Plus) and the PEKK post (Pekkton ® ) were tested using three kinds of self-adhesive resin cements (G-CEM LinkAce, Multilink Speed, and RelyX U200) and one self-etching resin cement (PANAVIA F2.0). The surface treatments of the fiberglass posts were processed according to the manufacturer's recommendations (F1, application of 37% phosphoric acid etching gel and silanization). For the PEKK post groups, various surface treatments were performed like no surface treatment (P1), sandblasting (P2), silica-coating and silanization (P3), and sandblasting with a composite primer (P4). In the surface treatment, PEKK posts with silica coating and silane treatment (P3) showed a significantly higher microtensile bond strength (mean MPa: 18.09, p < 0.05). The highest microtensile bond strength was shown when the PEKK posts were treated with a silica coating and silane treatment and cemented with RelyX U200 (mean MPa: 22.22). The PEKK posts with surface treatments of silica-coating and silanization or sandblasting displayed superior microtensile bond strengths (mean MPa: 18.09 and 16.25, respectively) compared to the conventional fiberglass posts (mean MPa: 14.93, p < 0.05).

Importance of surface modification of γ-alumina in creating its nanostructured composites with zeolitic imidazolate framework ZIF-67.

PubMed

Liu, Yuanyuan; Gonçalves, Alexandre A S; Zhou, Yang; Jaroniec, Mietek

2018-05-07

Application of zeolitic imidazolate framework-67 (ZIF-67) as an adsorbent has been greatly hindered by slow mass transfer of adsorbate molecules due to its inherent microporosity. To address this limitation, we have developed binary nanostructures composed of ZIF-67 and γ-alumina (GA) containing respectively micropores and large mesopores. The nanostructured composites were successfully prepared by coupling ZIF-67 and GA with and without surface modification with imidazole silane that mimics the building blocks of ZIF-67 to obtain GA-Im-ZIF-67 (with imidazole silane) and GA-ZIF-67 (without imidazole silane). The sizes of ZIF-67 crystals in these composites were smaller as compared to those of pure ZIF-67, and the textural properties of these composites with and without surface modification were quite similar. However, the surface grafting of alumina with imidazole silane played an important role in improving interfacial coupling between GA and ZIF-67, which resulted in significant changes in the dispersion of ZIF-67 crystals and better adsorption properties. The presence of large mesopores in the alumina-based composites containing smaller ZIF-67 crystals improved their adsorption properties toward dyes such as Rhodamine B (RhB). The RhB adsorption capacity of GA-Im-ZIF-67 was much higher than that of GA-ZIF-67, suggesting that the imidazole silane modification of GA before its coupling with ZIF-67 and the GA mesoporosity were essential for a substantial increase in the adsorption capacity of RhB. Copyright © 2018 Elsevier Inc. All rights reserved.

Dehydrogenative coupling of silanes with alcohols catalyzed by Cu3(BTC)2.

PubMed

Dhakshinamoorthy, Amarajothi; Concepcion, Patricia; Garcia, Hermenegildo

2016-02-14

Cu3(BTC)2 is an efficient and reusable heterogeneous catalyst for the dehydrogenative coupling of silanes with alcohols. Activity data and CO adsorption suggest that Cu(II) and in situ generated Cu(I) are the active species. Other MOFs such as Fe(BTC), MIL-101(Cr) and UiO-66(Zr) are unable to promote this cross-coupling.

Boron-carbon-silicon polymers and ceramic and a process for the production thereof

NASA Technical Reports Server (NTRS)

Riccitiello, Salvatore (Inventor); Hsu, Ming-Ta (Inventor); Chen, Timothy S. (Inventor)

1992-01-01

The present invention relates to a process for the production of an organoborosilicon preceramic polymer. The polymer is prepared by the reaction of vinylsilane or vinlymethylsilanes (acetylene)silane or acetylene alkyl silanes and borane or borane derivatives. The prepolymer form is pyrolyzed to produce a ceramic article useful in high temperature (e.g., aerospace) or extreme environmental applications.

Effect of Silver or Copper Nanoparticles-Dispersed Silane Coatings on Biofilm Formation in Cooling Water Systems

PubMed Central

Ogawa, Akiko; Kanematsu, Hideyuki; Sano, Katsuhiko; Sakai, Yoshiyuki; Ishida, Kunimitsu; Beech, Iwona B.; Suzuki, Osamu; Tanaka, Toshihiro

2016-01-01

Biofouling often occurs in cooling water systems, resulting in the reduction of heat exchange efficiency and corrosion of the cooling pipes, which raises the running costs. Therefore, controlling biofouling is very important. To regulate biofouling, we focus on the formation of biofilm, which is the early step of biofouling. In this study, we investigated whether silver or copper nanoparticles-dispersed silane coatings inhibited biofilm formation in cooling systems. We developed a closed laboratory biofilm reactor as a model of a cooling pipe and used seawater as a model for cooling water. Silver or copper nanoparticles-dispersed silane coating (Ag coating and Cu coating) coupons were soaked in seawater, and the seawater was circulated in the laboratory biofilm reactor for several days to create biofilms. Three-dimensional images of the surface showed that sea-island-like structures were formed on silane coatings and low concentration Cu coating, whereas nothing was formed on high concentration Cu coatings and low concentration Ag coating. The sea-island-like structures were analyzed by Raman spectroscopy to estimate the components of the biofilm. We found that both the Cu coating and Ag coating were effective methods to inhibit biofilm formation in cooling pipes. PMID:28773758

Surface modification of self-healing poly(urea-formaldehyde) microcapsules using silane-coupling agent

NASA Astrophysics Data System (ADS)

Li, Haiyan; Wang, Rongguo; Hu, Honglin; Liu, Wenbo

2008-12-01

Poly(urea-formaldehyde) (PUF) microcapsules, which are used as self-healing component of fibre reinforced resin matrix composites, were prepared by in situ polymerization method. The surface of PUF microcapsules was modified by using 3-aminopropyltriethoxy silane-coupling agent (KH550), and the interfacial interactions between PUF microcapsules and KH550 was also studied. Fourier transform infrared spectra (FT-IR) and X-ray photoelectron spectra (XPS) analyses showed that the silane-coupling agent molecular binds strongly to PUF microcapsules surface. Chemical bond (Si-O-C) was formed by the reaction between Si-OH and the hydroxyl group of PUF microcapsules, also there have chemical adsorption effect in the interface simultaneously because of the existence of hydrogen bond between Si-OH and the hydroxyl group of PUF microcapsules. Scanning electronic microscopy (SEM) observation showed that a thin layer was formed on the surface of modified PUF microcapsules. Additionally, fractured surface were observed under SEM to investigate the interfacial adhesion effect between PUF microcapsules and epoxy matrix. The result indicted that the silane-coupling agent play an important role in improving the interfacial performance between microcapsules and resin matrix.

Protein immobilization onto various surfaces using a polymer-bound isocyanate

NASA Astrophysics Data System (ADS)

Kang, Hyun-Jin; Cha, Eun Ji; Park, Hee-Deung

2015-01-01

Silane coupling agents have been widely used for immobilizing proteins onto inorganic surfaces. However, the immobilization method using silane coupling agents requires several treatment steps, and its application is limited to only surfaces containing hydroxyl groups. The aim of this study was to develop a novel method to overcome the limitations of the silane-based immobilization method using a polymer-bound isocyanate. Initially, polymer-bound isocyanate was dissolved in organic solvent and then was used to dip-coat inorganic surfaces. Proteins were then immobilized onto the dip-coated surfaces by the formation of urea bonds between the isocyanate groups of the polymer and the amine groups of the protein. The reaction was verified by FT-IR in which NCO stretching peaks disappeared, and CO and NH stretching peaks appeared after immobilization. The immobilization efficiency of the newly developed method was insensitive to reaction temperatures (4-50 °C), but the efficiency increased with reaction time and reached a maximum after 4 h. Furthermore, the method showed comparable immobilization efficiency to the silane-based immobilization method and was applicable to surfaces that cannot form hydroxyl groups. Taken together, the newly developed method provides a simple and efficient platform for immobilizing proteins onto surfaces.

Hybrid electrolytes incorporated with dandelion-like silane-Al2O3 nanoparticles for high-safety high-voltage lithium ion batteries

NASA Astrophysics Data System (ADS)

Xu, Hewei; Shi, Junli; Hu, Guosheng; He, Ying; Xia, Yonggao; Yin, Shanshan; Liu, Zhaoping

2018-07-01

One of the crucial challenge for developing high safety and high voltage lithium ion batteries is to find a reliable electrolyte system. In this work, we report a kind of hybrid electrolytes, which are used for high-voltage lithium ion batteries and are expected to be able to effectively enhance the battery safety. The hybrid electrolytes are obtained by incorporating silane-Al2O3 (Al2O3-ST) into liquid electrolyte, which combines the merits of both solid electrolyte and liquid electrolyte. The Al2O3-ST nanoparticles help to increase lithium-ion transference number and to enhance battery safety, while liquid electrolyte contributes to high ionic conductivity. The cycling stability and rate capacity of LiNi0.5Mn1.5O4/Li batteries are improved by using the hybrid electrolytes. Nail-penetration tests indicate that LiNi0.6Mn0.2Co0.2O2/graphite battery with hybrid electrolyte owns obviously enhanced safety than that using traditional liquid electrolyte. This work provides new insight on electrolyte design for high-safety high-voltage lithium ion batteries.

The influence of silanisation on the mechanical and degradation behaviour of PLGA/HA composites.

PubMed

Naik, Ashutosh; Best, Serena M; Cameron, Ruth E

2015-03-01

This study investigates the influence of silanisation on the mechanical and degradation behaviour of PLGA/HA composites. Three different silanes (mercaptopropyl trimethoxy silane (MPTMS), aminopropyl trimethoxy silane (APTMS) and aminopropyltriethoxy silane (APTES)) were applied to HA substrates in order to study the effect of head group (which binds to the polymer) and tail group (which binds to the surface hydroxyl groups in HA). A composite of hydroxyapatite (HA) and poly(d,l lactide-co-glycolide (50:50)) (PLGA) was investigated. The influence of concentration, the reaction time, drying temperature and substrate surface on silanisation was examined. TGA was used to detect the degree of silanisation. HA with MPTMS (1wt.% MPTMS with reaction time of 1h) was used as filler in PLGA-30wt.% HA composites for an in-vitro degradation study carried out in PBS. In addition, the mechanical properties of the composites were studied. Silanisation affects the properties of the composite by improving the bonding at the interface and hence it was found to influence the plastic mechanical properties rather than the elastic mechanical properties or the degradation profile of the composite. Copyright © 2014. Published by Elsevier B.V.

Effect of moisture on the physical and durability properties of methyl methacrylate polymer concrete

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fontana, J.J.; Reams, W.

1983-01-01

The compressive strength of methyl methacrylate PC composites decays very rapidly as the moisture content of the coarse aggregate is increased from 0 to 1 wt %. The durability of the PC also shows evidence of decay. Addition of silane coupling agent, such as A-1120, to the monomer component of a PC composite increases the compressive strength of such composites made with moist coarse aggregates. The compressive strengths of such PC composites are as high as a normal PCC used in highway applications. The durability of PC composites made with a silane additive seems to increase as the composite undergoesmore » freeze-thaw cycling which reinforces the justification that such materials can be used for PCC repairs without a sacrifice in use lifespans. However, for the convenience of using moist aggregates, one must endure the additional cost of the silane coupling agent. If it costs more than $0.02/lb to dry the aggregate, and one is willing to accept the reduced strengths associated with moist aggregates, then the use of a silane coupling agent can be cost effective. 3 figures, 4 tables.« less

Comparative study of solution-phase and vapor-phase deposition of aminosilanes on silicon dioxide surfaces.

PubMed

Yadav, Amrita R; Sriram, Rashmi; Carter, Jared A; Miller, Benjamin L

2014-02-01

The uniformity of aminosilane layers typically used for the modification of hydroxyl bearing surfaces such as silicon dioxide is critical for a wide variety of applications, including biosensors. However, in spite of many studies that have been undertaken on surface silanization, there remains a paucity of easy-to-implement deposition methods reproducibly yielding smooth aminosilane monolayers. In this study, solution- and vapor-phase deposition methods for three aminoalkoxysilanes differing in the number of reactive groups (3-aminopropyl triethoxysilane (APTES), 3-aminopropyl methyl diethoxysilane (APMDES) and 3-aminopropyl dimethyl ethoxysilane (APDMES)) were assessed with the aim of identifying methods that yield highly uniform and reproducible silane layers that are resistant to minor procedural variations. Silane film quality was characterized based on measured thickness, hydrophilicity and surface roughness. Additionally, hydrolytic stability of the films was assessed via these thickness and contact angle values following desorption in water. We found that two simple solution-phase methods, an aqueous deposition of APTES and a toluene based deposition of APDMES, yielded high quality silane layers that exhibit comparable characteristics to those deposited via vapor-phase methods. Copyright © 2013 Elsevier B.V. All rights reserved.

Reversible cobalt ion binding to imidazole-modified nanopipettes

PubMed Central

Sa, Niya; Fu, Yaqin; Baker, Lane A.

2010-01-01

In this report, we demonstrate that quartz nanopipettes modified with an imidazole-terminated silane respond to metal ions (Co2+) in solution. The response of nanopipettes is evaluated through examination of the ion current rectification response. By cycling nanopipettes between solutions of different pH, adsorbed Co2+ can be released from the nanopipette surface, to regenerate binding sites of the nanopipette. These results demonstrate that rectification-based sensing strategies for nanopore sensors can benefit from selection of recognition elements with intermediate binding affinities, such that reversible responses to be attained. PMID:21090777

Reversible cobalt ion binding to imidazole-modified nanopipettes.

PubMed

Sa, Niya; Fu, Yaqin; Baker, Lane A

2010-12-15

In this report, we demonstrate that quartz nanopipettes modified with an imidazole-terminated silane respond to metal ions (Co(2+)) in solution. The response of nanopipettes is evaluated through examination of the ion current rectification ratio. When nanopipettes are cycled between solutions of different pH, adsorbed Co(2+) can be released from the nanopipette surface, to regenerate binding sites of the nanopipette. These results demonstrate that rectification-based sensing strategies for nanopore sensors can benefit from selection of recognition elements with intermediate binding affinities, such that reversible responses can be attained.

Effect of silane dilution on intrinsic stress in glow discharge hydrogenated amorphous silicon films

NASA Astrophysics Data System (ADS)

Harbison, J. P.; Williams, A. J.; Lang, D. V.

1984-02-01

Measurements of the intrinsic stress in hydrogenated amorphous silicon (a-Si : H) films grown by rf glow discharge decomposition of silane diluted to varying degrees in argon are presented. Films are found to grow under exceedingly high compressive stress. Low values of macroscopic film density and low stress values are found to correlate with high growth rate. An abrupt drop in stress occurs between 2 and 3% silane at precisely the point where columnar growth morphology appears. No corresponding abrupt change is noted in density, growth rate, or plasma species concentrations as determined by optical emissioin spectroscopy. Finally a model of diffusive incorporation of hydrogen or some gaseous impurity during growth into the bulk of the film behind the growing interface is proposed to explain the results.

A comprehensive model to determine the effects of temperature and species fluctuations on reaction rates in turbulent reacting flows

NASA Technical Reports Server (NTRS)

Goldstein, D.; Magnotti, F.; Chinitz, W.

1983-01-01

Reaction rates in turbulent, reacting flows are reviewed. Assumed probability density functions (pdf) modeling of reaction rates is being investigated in relation to a three variable pdf employing a 'most likely pdf' model. Chemical kinetic mechanisms treating hydrogen air combustion is studied. Perfectly stirred reactor modeling of flame stabilizing recirculation regions was used to investigate the stable flame regions for silane, hydrogen, methane, and propane, and for certain mixtures thereof. It is concluded that in general, silane can be counted upon to stabilize flames only when the overall fuel air ratio is close to or greater than unity. For lean flames, silane may tend to destabilize the flame. Other factors favoring stable flames are high initial reactant temperatures and system pressure.

Cellular effect of high doses of silica-coated quantum dot profiled with high throughput gene expression analysis and high content cellomics measurements.

PubMed

Zhang, Tingting; Stilwell, Jackie L; Gerion, Daniele; Ding, Lianghao; Elboudwarej, Omeed; Cooke, Patrick A; Gray, Joe W; Alivisatos, A Paul; Chen, Fanqing Frank

2006-04-01

Quantum dots (Qdots) are now used extensively for labeling in biomedical research, and this use is predicted to grow because of their many advantages over alternative labeling methods. Uncoated Qdots made of core/shell CdSe/ZnS are toxic to cells because of the release of Cd2+ ions into the cellular environment. This problem has been partially overcome by coating Qdots with polymers, poly(ethylene glycol) (PEG), or other inert molecules. The most promising coating to date, for reducing toxicity, appears to be PEG. When PEG-coated silanized Qdots (PEG-silane-Qdots) are used to treat cells, toxicity is not observed, even at dosages above 10-20 nM, a concentration inducing death when cells are treated with polymer or mercaptoacid coated Qdots. Because of the importance of Qdots in current and future biomedical and clinical applications, we believe it is essential to more completely understand and verify this negative global response from cells treated with PEG-silane-Qdots. Consequently, we examined the molecular and cellular response of cells treated with two different dosages of PEG-silane-Qdots. Human fibroblasts were exposed to 8 and 80 nM of these Qdots, and both phenotypic as well as whole genome expression measurements were made. PEG-silane-Qdots did not induce any statistically significant cell cycle changes and minimal apoptosis/necrosis in lung fibroblasts (IMR-90) as measured by high content image analysis, regardless of the treatment dosage. A slight increase in apoptosis/necrosis was observed in treated human skin fibroblasts (HSF-42) at both the low and the high dosages. We performed genome-wide expression array analysis of HSF-42 exposed to doses 8 and 80 nM to link the global cell response to a molecular and genetic phenotype. We used a gene array containing approximately 22,000 total probe sets, containing 18,400 probe sets from known genes. Only approximately 50 genes (approximately 0.2% of all the genes tested) exhibited a statistically significant change in expression level of greater than 2-fold. Genes activated in treated cells included those involved in carbohydrate binding, intracellular vesicle formation, and cellular response to stress. Conversely, PEG-silane-Qdots induce a down-regulation of genes involved in controlling the M-phase progression of mitosis, spindle formation, and cytokinesis. Promoter analysis of these results reveals that expression changes may be attributed to the down-regulation of FOXM and BHLB2 transcription factors. Remarkably, PEG-silane-Qdots, unlike carbon nanotubes, do not activate genes indicative of a strong immune and inflammatory response or heavy-metal-related toxicity. The experimental evidence shows that CdSe/ZnS Qdots, if appropriately protected, induce negligible toxicity to the model cell system studied here, even when exposed to high dosages. This study indicates that PEG-coated silanized Qdots pose minimal impact to cells and are a very promising alternative to uncoated Qdots.

Acute bioassays and hazard evaluation of representative contaminants detected in Great Lakes fish

USGS Publications Warehouse

Passino, Dora R. May; Smith, Stephen B.

1987-01-01

We have provided a hazard ranking for 19 classes of compounds representing many of the nearly 500 organic compounds identified by gas chromatography-mass spectrometry in lake trout (Salvelinus namaycush) and walleye (Stizostedion vitreum vitreum) from the Great Lakes and Lake St. Clair. We initially made a provisional hazard ranking based on available published and unpublished information on aquatic toxicity, bioaccumulation, occurrence and sources. Acute toxicity tests with Daphnia pulex at 17A°C in reconstituted hard water were performed with 30 compounds representative of the 19 classes that were highest in the provisional ranking. The resulting toxicity data, along with information on the compounds' occurrence in Great Lakes fish and their sources, were ranked and weighted and then used in calculating the revised hazard ranking. The 10 most hazardous classes, in descending order, are as follows (values shown are mean 48-h EC50s, in μ/ml): arene halides (e.g., polychlorinated biphenyls, DDT), 0.0011; phthalate esters, 0.133; chlorinated camphenes (toxaphene), 0.0082; polyaromatic hydrocarbons (PAHs; e.g., dimethylnaphthalene) and reduced derivatives, 1.01; chlorinated fused polycyclics (e.g., trans-nonachlor), 0.022; nitrogen-containing compounds (e.g., O-methylhydroxyl-amine), 1.35; alkyl halides (e.g., (bromomethyl)cyclohexene), 10.1; cyclic alkanes (e.g., cyclododecane), 20.9; silicon-containing compounds (e.g., dimethyldiethoxy silane), 1.25; and heterocyclic nitrogen compounds (e.g., nicotine), 2.48. We recommend that chronic bioassays be conducted with fish and invertebrates to determine the sublethal effects of the following classes of compounds, for which few toxicity data are available: PAHs, heterocyclic nitrogen compounds, other nitrogen-containing compounds, alkyl halides, cyclic alkanes and silicon-containing compounds. Information from these types of studies will aid researchers in determining the possible causal role these contaminants play in the decline and reproductive impairment of Great Lakes fish.

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

NASA Technical Reports Server (NTRS)

Mikes, F.

1985-01-01

Concluding tests for the thermogravimetric and FTIR analyses of DC 1200 silane primers are discussed as well as methods for HPLC and GC analyses and for determining titanium and silicon by atomic absorption spectroscopy. Tables summarizes results obtained for residue, ash, titanium, silicone, Si/Ti ratio, OH-absorption, the lap-shear test, and the GC headspace for alcohols.

The effect of silane applied to glass ceramics on surface structure and bonding strength at different temperatures

PubMed Central

Eraslan, Oguz

2016-01-01

PURPOSE To evaluate the effect of various surface treatments on the surface structure and shear bond strength (SBS) of different ceramics. MATERIALS AND METHODS 288 specimens (lithium-disilicate, leucite-reinforced, and glass infiltrated zirconia) were first divided into two groups according to the resin cement used, and were later divided into four groups according to the given surface treatments: G1 (hydrofluoric acid (HF)+silane), G2 (silane alone-no heat-treatment), G3 (silane alone-then dried with 60℃ heat-treatment), and G4 (silane alone-then dried with 100℃ heat-treatment). Two different adhesive luting systems were applied onto the ceramic discs in all groups. SBS (in MPa) was calculated from the failure load per bonded area (in N/mm2). Subsequently, one specimen from each group was prepared for SEM evaluation of the separated-resin–ceramic interface. RESULTS SBS values of G1 were significantly higher than those of the other groups in the lithium disilicate ceramic and leucite reinforced ceramic, and the SBS values of G4 and G1 were significantly higher than those of G2 and G3 in glass infiltrated zirconia. The three-way ANOVA revealed that the SBS values were significantly affected by the type of resin cement (P<.001). FIN ceramics had the highest rate of cohesive failure on the ceramic surfaces than other ceramic groups. AFM images showed that the surface treatment groups exhibited similar topographies, except the group treated with HF. CONCLUSION The heat treatment was not sufficient to achieve high SBS values as compared with HF acid etching. The surface topography of ceramics was affected by surface treatments. PMID:27141250

New insights into the adsorption of 3-(trimethoxysilyl)propylmethacrylate on hydroxylated ZnO nanopowders.

PubMed

Bressy, Christine; Ngo, Van Giang; Ziarelli, Fabio; Margaillan, André

2012-02-14

Functionalization of zinc oxide (ZnO) nano-objects by silane grafting is an attractive method to provide nanostructured materials with a variety of surface properties. Active hydroxyl groups on the oxide surface are one of the causes governing the interfacial bond strength in nanohybrid particles. Here, "as-prepared" and commercially available zinc oxide nanopowders with a wide range of surface hydroxyl density were functionalized by a well-known polymerizable silane coupling agent, i.e., 3-(trimethoxysilyl)propylmethacrylate (MPS). Fourier transform infrared (FTIR) and solid-state (13)C and (29)Si nuclear magnetic resonance (NMR) spectroscopic investigations demonstrated that the silane coupling agent was fully hydrolyzed and linked to the hydroxyl groups already present on the particle surface through covalent and hydrogen bonds. Due to a basic catalyzed condensation of MPS with water, a siloxane layer was shown to be anchored to the nanoparticles through mono- and tridentate structures. Quantitative investigations were performed by thermogravimetric (TGA) and elemental analyses. The amount of silane linked to ZnO particles was shown to be affected by the amount of isolated hydroxyl groups available to react on the particle surface. For as-prepared ZnO nanoparticles, the number of isolated and available hydroxyl groups per square nanometer was up to 3 times higher than the one found on commercially available ZnO nanoparticles, leading to higher amounts of polymerizable silane agent linked to the surface. The MPS molecules were shown to be mainly oriented perpendicular to the oxide surface for all the as-prepared ZnO nanoparticles, whereas a parallel orientation was found for the preheated commercially ZnO nanopowders. In addition, ZnO nanoparticles were shown to be hydrophobized by the MPS treatment with water contact angles higher than 60°.

Sandblasting may damage the surface of composite CAD-CAM blocks.

PubMed

Yoshihara, Kumiko; Nagaoka, Noriyuki; Maruo, Yukinori; Nishigawa, Goro; Irie, Masao; Yoshida, Yasuhiro; Van Meerbeek, Bart

2017-03-01

CAD-CAM blocks to fabricate semi-direct and indirect restorations are available in different sorts of ceramics as well as composite. In order to bond restorations prepared out of composite blocks into tooth cavities, it is recommended to gently sandblast the surface prior to the application of a primer/adhesive. Today, the effect of sandblasting composite block surfaces has not thoroughly been investigated. In this study, the ultra-structure of composite CAD-CAM blocks was investigated with special attention to the effect of sandblasting on the surface topography and of silanization on the bonding performance. Five different composite CAD-CAM blocks were involved. We correlatively investigated their structural and chemical composition using X-ray diffraction (XRD), energy dispersion spectroscopy (EDS), scanning electron microscopy (SEM) and (scanning) transmission electron microscopy ((S)TEM). The effect of sandblasting was also imaged in cross-section and at the interface with composite cement. Finally, we measured the shear bond strength to the sandblasted block surface with and without silanization. All composite blocks revealed a different ultra-structure. Sandblasting increased surface roughness and resulted in an irregular surface with some filler exposure. Sandblasting also damaged the surface. When the sandblasted composite blocks were silanized, superior bonding receptiveness in terms of higher bond strength was achieved except for Shofu Block HC. Sandblasting followed by silanization improved the bond strength to composite CAD-CAM blocks. However, sandblasting may also damage the composite CAD-CAM block surface. For the composite CAD-CAM block Shofu Block HC, the damage was so severe that silanization did not improve bond strength. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effects of silica coating and silane surface conditioning on the bond strength of metal and ceramic brackets to enamel.

PubMed

Atsü, Saadet Sağlam; Gelgör, Ibrahim Erhan; Sahin, Volkan

2006-09-01

To evaluate the effect of tribochemical silica coating and silane surface conditioning on the bond strength of metal and ceramic brackets bonded to enamel surfaces with light-cured composite resin. Twenty metal and 20 ceramic brackets were divided into four groups (n = 10 for each group). The specimens were randomly assigned to one of the following treatment conditions of the metal and ceramic brackets' surface: (1) tribochemical silica coating combined with silane and (2) no treatment. Brackets were bonded to the enamel surface on the labial and lingual sides of human maxillary premolars (20 total) with a light-polymerized resin composite. All specimens were stored in water for 1 week at 37 degrees C and then thermocycled (5000 cycles, 5 degrees C to 55 degrees C, 30 seconds). The shear bond strength values were measured on a universal testing machine. Student's t-test was used to compare the data (alpha = 0.05). The types of failures were observed using a stereomicroscope. Metal and ceramic brackets treated with silica coating with silanization had significantly greater bond strength values (metal brackets: 14.2 +/- 1.7 MPa, P < .01; ceramic brackets: 25.9 +/- 4.4 MPa, P < .0001) than the control groups (metal brackets: 11.9 +/- 1.3 MPa; ceramic brackets: 15.6 +/- 4.2 MPa). Treated specimens of metal and ceramic exhibited cohesive failures in resin and adhesive failures at the enamel-adhesive interface, whereas control specimens showed mixed types of failures. Silica coating with aluminum trioxide particles coated with silica followed by silanization gave higher bond strengths in both metal and ceramic brackets than in the control group.

Protein resistance efficacy of PEO-silane amphiphiles: Dependence on PEO-segment length and concentration

PubMed Central

Rufin, Marc A.; Barry, Mikayla E.; Adair, Paige A.; Hawkins, Melissa L.; Raymond, Jeffery E.; Grunlan, Melissa A.

2016-01-01

In contrast to modification with conventional PEO-silanes (i.e. no siloxane tether), silicones with dramatically enhanced protein resistance have been previously achieved via bulk-modification with poly (ethylene oxide) (PEO)-silane amphiphiles α-(EtO)3Si(CH2)2-oligodimethylsiloxane13-block-PEOn-OCH3 when n = 8 and 16 but not when n = 3. In this work, their efficacy was evaluated in terms of optimal PEO-segment length and minimum concentration required in silicone. For each PEO-silane amphiphile (n = 3, 8, and 16), five concentrations (5, 10, 25, 50, and 100 μmol per 1 g silicone) were evaluated. Efficacy was quantified in terms of the modified silicones’ abilities to undergo rapid, water-driven surface restructuring to form hydrophilic surfaces as well as resistance to fibrinogen adsorption. Only n = 8 and 16 were effective, with a lower minimum concentration in silicone required for n = 8 (10 μmol per 1 g silicone) versus n = 16 (25 μmol per 1 g silicone). Statement of Significance Silicone is commonly used for implantable medical devices, but its hydrophobic surface promotes protein adsorption which leads to thrombosis and infection. Typical methods to incorporate poly(ethylene oxide) (PEO) into silicones have not been effective due to the poor migration of PEO to the surface-biological interface. In this work, PEO-silane amphiphiles – comprised of a siloxane tether (m = 13) and variable PEO segment lengths (n = 3, 8, 16) – were blended into silicone to improve its protein resistance. The efficacy of the amphiphiles was determined to be dependent on PEO length. With the intermediate PEO length (n = 8), water-driven surface restructuring and resulting protein resistance was achieved with a concentration of only 1.7 wt%. PMID:27090588

Zinc Oxide—From Synthesis to Application: A Review

PubMed Central

Kołodziejczak-Radzimska, Agnieszka; Jesionowski, Teofil

2014-01-01

Zinc oxide can be called a multifunctional material thanks to its unique physical and chemical properties. The first part of this paper presents the most important methods of preparation of ZnO divided into metallurgical and chemical methods. The mechanochemical process, controlled precipitation, sol-gel method, solvothermal and hydrothermal method, method using emulsion and microemulsion enviroment and other methods of obtaining zinc oxide were classified as chemical methods. In the next part of this review, the modification methods of ZnO were characterized. The modification with organic (carboxylic acid, silanes) and inroganic (metal oxides) compounds, and polymer matrices were mainly described. Finally, we present possible applications in various branches of industry: rubber, pharmaceutical, cosmetics, textile, electronic and electrotechnology, photocatalysis were introduced. This review provides useful information for specialist dealings with zinc oxide. PMID:28788596

Effective holographic recordings in the photopolymer nanocomposites with functionalized silica nanoparticle and polyurethane matrix

NASA Astrophysics Data System (ADS)

Han, Samsook; Lee, Muncheul; Kim, Byung Kyu

2011-11-01

Effective holographic nanocomposites were developed by the surface-functionalized silica nanoparticles and two acrylate monomers/polyurethane (PU) matrix polymer. The functionalization was done with silane compounds carrying long alkyl chain or vinyl group. We evaluated the holographic nanocomposite films by the diffraction efficiency, volume shrinkage, optical loss, and the film morphology. It was found that acrylate monomers/PU system gave higher diffraction efficiency than those of two monomers due to the high refractive index mismatch between the acrylate-rich and PU-rich regions. With the modification of silica particle, up to 35% of particle loading was possible to give a maximum diffraction efficiency of 93.6% for a film of 20 μm in thickness, along with improved refractive index modulation and the sensitivity.

Removing Chlorides From Metallurgical-Grade Silicon

NASA Technical Reports Server (NTRS)

Breneman, W. C.; Coleman, L. M.

1982-01-01

Process for making low-cost silicon for solar cells is further improved. Silane product recycled to feed stripper column converts some of heavy impurities to volatile ones that pass off at top of column with light wastes. Impurities--chlorides of arsenic, phosphorus, and boron-would otherwise be carried to subsequent distillations where they would be difficult to remove. Since only a small amount of silane is recycled, silicon production efficiency remains high.

Silane-O/sub 2/ explosions, their characteristics and their control

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ring, M.A.; O'Neil, H.E.; Famil-Ghiriha, J.

1988-07-15

Prior results on the stoichiometry, upper pressure explosion limits and reaction mechanism of SiH/sub 2/-O/sub 2/ explosion reactions are discussed, and new data on the effects of added disilane on the pyrophoric and explosive characters of metastable SiH/sub 4/-O/sub 2/ mixtures are presented. The results have possible application to the prevention of serious explosions due to silane leaks into air.

Synthesis of borasiloxanes by oxidative hydrolysis of silanes and pinacolborane using Cu3(BTC)2 as a solid catalyst.

PubMed

Dhakshinamoorthy, Amarajothi; Asiri, Abdullah M; Concepcion, Patricia; Garcia, Hermenegildo

2017-09-05

A convenient method for the synthesis of borasiloxanes from silanes and pinacolboranes using Cu 3 (BTC) 2 as a heterogeneous catalyst in acetonitrile at 70 °C is reported. This procedure is more convenient than Ru and Pd based homogeneous catalysts because it avoids the use of noble metals, easy handling of starting materials and the catalyst can be reused.

Thermal decomposition of silane to form hydrogenated amorphous Si

DOEpatents

Strongin, M.; Ghosh, A.K.; Wiesmann, H.J.; Rock, E.B.; Lutz, H.A. III

Hydrogenated amorphous silicon is produced by thermally decomposing silane (SiH/sub 4/) or other gases comprising H and Si, at elevated temperatures of about 1700 to 2300/sup 0/C, in a vacuum of about 10/sup -8/ to 10/sup -4/ torr. A gaseous mixture is formed of atomic hydrogen and atomic silicon. The gaseous mixture is deposited onto a substrate to form hydrogenated amorphous silicon.

1-butanethiol vapor sensing based on gold nanoparticle immobilized on glass slide by digital color analysis

NASA Astrophysics Data System (ADS)

Shokoufi, Nader; Adeleh, Sara

2017-12-01

We demonstrate that gold nanoparticles (GNPs) immobilized on silanized glass act as an optical sensor that is able to quantify 1-butanethiol vapor. GNPs optical properties in the visible region are dominated by the surface plasmon resonance (SPR). The high affinity between 1-butanethiol and GNPs through Au-s bond leads to change in plasmon feature of GNPs that immobilized on silanized glass and causes absorption decrease at 542 nm in SPR spectrum of GNPs. It can be used as an optical sensor for quantitative detection. In this research, the glass slide surface activated by aminopropyltriethoxysilane (APTES). Spherical GNPs immobilized on silanized glass by silanization agent. The sensor is based on the spectrophotometry and digital color analysis (DCA) through RGB. We monitored R value and linear range 50-700 µM (R 2  =  0.97) with 2.05% relative standard deviation and 26.5 µM value was achieved, for the limit of detection. This method represents advantages of metal gold nanoparticles and solid substrate stability in one package, being inexpensive and low time consuming is another advantage of our method that can be conducted in petrochemical, pharmaceutical industries, and for detection of rotten food in food industries.

The influence of silanized nano-SiO{sub 2} on the hydration of cement paste: NMR investigations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bede, A., E-mail: Andrea.Bede@phys.utcluj.ro; Pop, A.; Ardelean, I.

2015-12-23

It is known that by adding a small amount of nanoparticles to the cement-based materials a strong influence on the workability, strength and durability is obtained. These characteristics of the material are fundamentally determined by the hydration process taking place after mixing the cement grains with water. In the present study the influence introduced by the addition of nano-silica with silanized surfaces on the hydration process was investigated using low-field nuclear magnetic resonance (NMR) relaxometry. The cement samples were prepared using gray cement at a water-to-cement ratio of 0.4 and a 5% addition of nanosilica. The surface of the nanoparticlesmore » was modified using a coating of Silane A174. The cement pastes were monitored during their standard curing time of 28 days. It was established that, by using unmodified nanosilica particles, an acceleration of the hydration process takes place as compared with the pure cement paste. On the other side, by adding silanized nanoparticles, the dormancy stage significantly extends and the hydration process is slower. This slowing down process could enhance the mechanical strength of cement based materials as a result of a better compaction of the hydrated samples.« less

Rational interface design of epoxy-organoclay nanocomposites: role of structure-property relationship for silane modifiers.

PubMed

Bruce, Alex N; Lieber, Danielle; Hua, Inez; Howarter, John A

2014-04-01

Montmorillonite was modified by three silane surfactants with different functionalities to investigate the role of surfactant structure on the properties of a final epoxy-organoclay nanocomposite. N-aminopropyldimethylethoxysilane (APDMES), an aminated monofunctional silane, was chosen as a promising surfactant for several reasons: (1) it will bond to silica in montmorillonite, (2) it will bond to epoxide groups, and (3) to overcome difficulties found with trifunctional aminosilane bonding clay layers together and preventing exfoliation. A trifunctional and non-aminated version of APDMES, 3-aminopropyltriethoxysilane (APTES) and n-propyldimethylmethoxysilane (PDMMS), respectively, was also studied to provide comparison to this rationally chosen surfactant. APDMES and APTES were grafted onto montmorillonite in the same amount, while PDMMS was barely grafted (<1 wt%). The gallery spacing of APDMES organoclay was greater than APTES or PDMMS, but the final nanocomposite gallery spacing was not dependent on the surfactant used. Different concentrations of APDMES modified montmorillonite yielded different properties, as concentration decreased glass transition temperature increased, thermal stability increased, and the storage modulus decreased. Storage modulus, glass transition temperature, and thermal stability were more similar for epoxy-organoclay composites modified with the same concentration of silane surfactant, neat epoxy, and epoxy-montmorillonite nanocomposite. Copyright © 2013 Elsevier Inc. All rights reserved.

Mechanical behavior of bioactive composite cements consisting of resin and glass-ceramic powder in a simulated body fluid: effect of silane coupling agent.

PubMed

Miyata, N; Matsuura, W; Kokubo, T; Nakamura, T

2004-09-01

Time-dependent strength behavior was investigated for bisphenol-a-glycidyl methacrylate/triethylene glycol dimethacrylate (Bis-GMA/TEGDMA) resin cements combined with glass-ceramic A-W filler treated with various kinds of silane coupling agents. The fracture strength of the composite resin cements was measured by three-point bending as a function of stressing rate in a simulated body fluid (SBF), and thereby the stress-corrosion susceptibility constant was evaluated. The fracture strength was found to depend on the kind of coupling agent used. For the present Bis-GMA/TEGDMA resin, the silane coupling agents without hydrophilic amine groups can be used to obtain good adhesion between resin and A-W filler owing to their nature of co-polymerizing with the resin. On the other hand, all the composite resin cements showed nearly the same degree of stress-corrosion susceptibility whether the A-W fillers were treated or untreated with silane coupling agents. This means that the stress-corrosion susceptibility of the present composite cements is predominantly affected by that of the matrix resin. Thus, the microcrack formation and growth at the resin matrix near particle - resin interface were thought to determine overall time-dependent strength behavior of the composite cements.

Superhydrophobic, Hybrid, Electrospun Cellulose Acetate Nanofibrous Mats for Oil/Water Separation by Tailored Surface Modification.

PubMed

Arslan, Osman; Aytac, Zeynep; Uyar, Tamer

2016-08-03

Electrospun cellulose acetate nanofibers (CA-NF) have been modified with perfluoro alkoxysilanes (FS/CA-NF) for tailoring their chemical and physical features aiming oil-water separation purposes. Strikingly, hybrid FS/CA-NF showed that perfluoro groups are rigidly positioned on the outer surface of the nanofibers providing superhydrophobic characteristic with a water contact angle of ∼155°. Detailed analysis showed that hydrolysis/condensation reactions led to the modification of the acetylated β(1 → 4) linked d-glucose chains of CA transforming it into a superhydrophobic nanofibrous mat. Analytical data have revealed that CA-NF surfaces can be selectively controlled for fabricating the durable, robust and water resistant hybrid electrospun nanofibrous mat. The -OH groups available on the CA structure allowed the basic sol-gel reactions started by the reactive FS hybrid precursor system which can be monitored by spectroscopic analysis. Since alkoxysilane groups on the perfluoro silane compound are capable of reacting for condensation together with the CA, superhydrophobic nanofibrous mat is obtained via electrospinning. This structural modification led to the facile fabrication of the novel oil/water nanofibrous separator which functions effectively demonstrated by hexane/oil and water separation experiments. Perfluoro groups consequently modified the hydrophilic CA nanofibers into superhydrophobic character and therefore FS/CA-NF could be quite practical for future applications like water/oil separators, as well as self-cleaning or water resistant nanofibrous structures.

Chip PCR. I. Surface passivation of microfabricated silicon-glass chips for PCR.

PubMed Central

Shoffner, M A; Cheng, J; Hvichia, G E; Kricka, L J; Wilding, P

1996-01-01

The microreaction volumes of PCR chips (a microfabricated silicon chip bonded to a piece of flat glass to form a PCR reaction chamber) create a relatively high surface to volume ratio that increases the significance of the surface chemistry in the polymerase chain reaction (PCR). We investigated several surface passivations in an attempt to identify 'PCR friendly' surfaces and used those surfaces to obtain amplifications comparable with those obtained in conventional PCR amplification systems using polyethylene tubes. Surface passivations by a silanization procedure followed by a coating of a selected protein or polynucleotide and the deposition of a nitride or oxide layer onto the silicon surface were investigated. Native silicon was found to be an inhibitor of PCR and amplification in an untreated PCR chip (i.e. native slicon) had a high failure rate. A silicon nitride (Si(3)N(4) reaction surface also resulted in consistent inhibition of PCR. Passivating the PCR chip using a silanizing agent followed by a polymer treatment resulted in good amplification. However, amplification yields were inconsistent and were not always comparable with PCR in a conventional tube. An oxidized silicon (SiO(2) surface gave consistent amplifications comparable with reactions performed in a conventional PCR tube. PMID:8628665

Tailored interphase structure for improved strength and energy absorption of composites

NASA Astrophysics Data System (ADS)

Gao, Xiao

Fiber reinforced polymeric composites are lightweight, high-strength and high impact-resistant materials used widely for various applications. It has been shown that the mechanical performance of composites are dependent on the interphase, a three-dimensional region of nanometer size in the vicinity of the fiber-matrix boundary that possesses properties different from those of either the fiber reinforcement or the matrix resin and governs the load transfer from matrix to fiber. This research conducts a systematic study on glass fiber-epoxy interphase structure by tailoring adhesion between constituents and the creation of textures to control strength and energy absorption through mechanical interlocking between glass fiber and epoxy matrix. Our objective is to establish the foundation for microstructural design and optimization of the composite's structural and impact performance. Two ways of roughening the glass fiber surface have been studied to create the mechanical interlocking between fiber and resin; the first technique involves forming in-situ islands on the glass fiber surface by using silane blends of Glycidoxypropyltrimethoxy silane (GPS) and Tetraethoxy silane (TEOS); the second technique applies a silane coupling agents based sizing with the incorporation of silica nanoparticles (Ludox TMA, 22 nm) onto the fiber surface. The microdroplet test was selected to characterize the influence of adhesion and mechanical interlocking effects on interphase properties of different sizing sized glass fiber reinforced epoxy systems. A suitable data reduction scheme enables the strength and specified energy absorbed due to debonding, dynamic sliding, and quasi-static sliding to be quantified. In order to validate the effect of tailored interphase structure, which is induced by creating mechanical interlocking between fiber and resin, on macroscopic composite properties, composite panels were made from these four different sizing sized glass fibers and tested using the punch shear test. The composite panel made from the hybrid sizing sized glass fiber exhibited improved strength and energy absorption consistent with the trends in micromechanical measurements. Through all failure stages under macromechanical testing, hybrid sizing sized glass fiber/epoxyamine composite panel shows an increase in the strength and total energy absorption by 13% and 26%, respectively, compared to the compatible sizing sized baseline. Both micromechanical and macromechanical tests demonstrate the significant influence of tailoring the interphase structure on improving the impact performance of the composites. The hybrid sizing with the incorporation of nanoparticles, in particular, can greatly improve the impact resistance (i.e. energy absorption) of composites without sacrificing its structural performance (i.e. strength).

Aircraft Fuel Tank Inerting System

DTIC Science & Technology

1983-07-01

The 4950th T~st Wing was to determine If any compass/navigation problems were encoun- tered. Boeing reported that the " Winglet Program" Is encountering... blending TPX, silane, and a peroxide catalyst and reacting the grafted material with water. 2. Extrusioa of the grafted TPX was not successful under a...experiments, particularly in order to evaluate how much of a problem a loss of silane by evaporation would be at the high blending temperatures that had

Silane-Pyrolysis Reactor With Nonuniform Heating

NASA Technical Reports Server (NTRS)

Iya, Sridhar K.

1991-01-01

Improved reactor serves as last stage in system processing metallurgical-grade silicon feedstock into silicon powder of ultrahigh purity. Silane pyrolized to silicon powder and hydrogen gas via homogeneous decomposition reaction in free space. Features set of individually adjustable electrical heaters and purge flow of hydrogen to improve control of pyrolysis conditions. Power supplied to each heater set in conjunction with flow in reactor to obtain desired distribution of temperature as function of position along reactor.

The Effect of Silane on the Microstructure, Corrosion, and Abrasion Resistances of the Anodic Films on Ti Alloy

NASA Astrophysics Data System (ADS)

Wang, Jinwei; Chen, Jiali

2016-04-01

Anodic oxide films on Ti-6Al-4V alloy are prepared using sodium hydroxide as the base electrolyte containing aminopropyl trimethoxysilane (APS) as an additive. Some APS undergo hydrolysis, adsorption, and chemical reaction with the TiO x to form Ti-O-Si bond as confirmed by ATR-FTIR and XPS spectra, and in turn their surface appearance and roughness are greatly changed with the addition of APS as observed by their SEM images. These amino anodic films possess much higher corrosive resistances since the formation of Ti-O-Si complex enhances the compactness of the anodic films and the existence of aminopropyl groups inside the pores provides additional blocking effects. Besides, their improvement in anti-abrasive capability is attributed to the toughening effect of the chemically bonded silanes and the lubrication functions from both the chemically bonded and physically absorbed silanes between the touched interfaces.

Low cost silicon solar array project silicon materials task: Establishment of the feasibility of a process capable of low-cost, high volume production of silane (step 1) and the pyrolysis of silane to semiconductor-grade silicon (step 2)

NASA Technical Reports Server (NTRS)

Breneman, W. C.; Cheung, H.; Farrier, E. G.; Morihara, H.

1977-01-01

A quartz fluid bed reactor capable of operating at temperatures of up to 1000 C was designed, constructed, and successfully operated. During a 30 minute experiment, silane was decomposed within the reactor with no pyrolysis occurring on the reactor wall or on the gas injection system. A hammer mill/roller-crusher system appeared to be the most practical method for producing seed material from bulk silicon. No measurable impurities were detected in the silicon powder produced by the free space reactor, using the cathode layer emission spectroscopic technique. Impurity concentration followed by emission spectroscopic examination of the residue indicated a total impurity level of 2 micrograms/gram. A pellet cast from this powder had an electrical resistivity of 35 to 45 ohm-cm and P-type conductivity.

A durable PtRu/C catalyst with a thin protective layer for direct methanol fuel cells.

PubMed

Shimazaki, Yuzuru; Hayasaka, Sho; Koyama, Tsubasa; Nagao, Daisuke; Kobayashi, Yoshio; Konno, Mikio

2010-11-15

A methanol oxidation catalyst with improved durability in acidic environments is reported. The catalyst consists of PtRu alloy nanoparticles on a carbon support that were stabilized with a silane-coupling agent. The catalyst was prepared by reducing ions of Pt and Ru in the presence of a carbon support and the silane-coupling agent. The careful choice of preparatory conditions such as the concentration of the silane-coupling agent and solution pH resulted in the preparation of catalyst in which the PtRu nanoparticles were dispersively adsorbed onto the carbon support. The catalytic activity was similar to that of a commercial catalyst and was unchanged after immersion in sulfuric acid solution for 1000 h, suggesting the high durability of the PtRu catalyst for the anode of direct methanol fuel cells. Copyright © 2010 Elsevier Inc. All rights reserved.

Low cost silicon solar array project silicon materials task: Establishment of the feasibility of a process capable of low-cost, high volume production of silane (step 1) and the pyrolysis of silane to semiconductor-grade silicon (step 2)

NASA Technical Reports Server (NTRS)

Breneman, W. C.; Farrier, E. G.; Rexer, J.

1977-01-01

Extended operation of a small process-development unit routinely produced high quality silane in 97+% yield from dichlorosilane. The production rate was consistent with design loadings for the fractionating column and for the redistribution reactor. A glass fluid-bed reactor was constructed for room temperature operation. The behavior of a bed of silcon particles was observed as a function of various feedstocks, component configurations, and operating conditions. For operating modes other than spouting, the bed behaved in an erratic and unstable manner. A method was developed for casting molten silicon powder into crack-free solid pellets for process evaluation. The silicon powder was melted and cast into thin walled quartz tubes that sacrificially broke on cooling.

Adhesive bonding to polymer infiltrated ceramic.

PubMed

Schwenter, Judith; Schmidli, Fredy; Weiger, Roland; Fischer, Jens

2016-01-01

Aim of this study was to investigate the mechanism of adhesive bonding to the polymer-infiltrated ceramic VITA Enamic [VE]. Shear bond strength was measured with three resin composite cements: RelyX Unicem 2 Automix, Clearfil SA and Variolink II on polished surfaces of VE and its components silicate ceramic [SC] and polymer [PM] (n=12). Further, the effect of etching VE with 5% HF for 15-240 s and the application of silane coupling agents was analyzed in a screening test (n=6). Shear bond strength measurements were performed after 24 h of water storage at 37°C. Significant bonding to polished substrates could only be achieved on VE and SC when silane coupling agents were used. Etching of VE with 5% HF increased shear bond strength. Following silanization of etched VE, a further increase in shear bond strength could be established. Etching for more than 30 s did not improve shear bond strength.

Two dimensional fluid simulation in capacitively coupled silane discharges

NASA Astrophysics Data System (ADS)

Song, Yuan-Hong; Liu, Xiang-Mei; Wang, Yan; Wang, You-Nian

2011-10-01

A two-dimensional (2D) self-consistent fluid model is developed to describe the formation, subsequent growth, transport and charging mechanisms of nanoparticles in a capacitively coupled silane plasma. In this discharge process, large anions are produced by a series of chemical reactions of anions with silane molecules, while the lower limit of the initial nanoparticles are taken as large anions to directly link the coagulation module with the nucleation module. The influences of source parameters on the electron density, electron temperature, nanoparticle uniformity, and deposition rate, are carefully studied. Moreover, the behavior of silicon plasma mixed with SiH4, N2 and O2 in a pulse modulated capacitively coupled plasma has been also investigated. Results showed a strong dependence of the electron density and electron temperature on the duty cycle and the modulated frequency. Supported by NSFC (No.10775025 and No. 10805008), INSTSP (Grant No: 2011ZX02403-001), and PNCETU (NCET-08-0073).

Ultrahigh molecular weight aromatic siloxane polymers

NASA Technical Reports Server (NTRS)

Ludwick, L. M.

1982-01-01

The condensation of a diol with a silane in toluene yields a silphenylene-siloxane polymer. The reaction of stiochiometric amounts of the diol and silane produced products with molecular weights in the range 2.0 - 6.0 x 10 to the 5th power. The molecular weight of the product was greatly increased by a multistep technique. The methodology for synthesis of high molecular weight polymers using a two step procedure was refined. Polymers with weight average molecular weights in excess of 1.0 x 10 to the 6th power produced by this method. Two more reactive silanes, bis(pyrrolidinyl)dimethylsilane and bis(gamma butyrolactam)dimethylsilane, are compared with the dimethyleminodimethylsilane in ability to advance the molecular weight of the prepolymer. The polymers produced are characterized by intrinsic viscosity in tetrahydrofuran. Weight and number average molecular weights and polydispersity are determined by gel permeation chromatography.

Process feasibility study in support of silicon material task 1

NASA Technical Reports Server (NTRS)

Fang, C. S.; Hansen, K. C.; Miller, J. W., Jr.; Yaws, C. L.

1978-01-01

Initial results for gas thermal conductivity of silicon tetrafluoride and trichlorosilane are reported in respective temperature ranges of 25 to 400 C and 50 to 400 C. For chemical engineering analyses, the preliminary process design for the original silane process of Union Carbide was completed for Cases A and B, Regular and Minimum Process Storage. Included are raw material usage, utility requirements, major process equipment lists, and production labor requirements. Because of the large differences in surge tankage between major unit operations the fixed capital investment varied from $19,094,000 to $11,138,000 for Cases A and B, respectively. For the silane process the original flowsheet was revised for a more optimum arrangement of major equipment, raw materials and operating conditions. The initial issue of the revised flowsheet (Case C) for the silane process indicated favorable cost benefits over the original scheme.

Silane–Acrylate Chemistry for Regulating Network Formation in Radical Photopolymerization

PubMed Central

2017-01-01

Photoinitiated silane–ene chemistry has the potential to pave the way toward spatially resolved organosilicon compounds, which might find application in biomedicine, microelectronics, and other advanced fields. Moreover, this approach could serve as a viable alternative to the popular photoinitiated thiol–ene chemistry, which gives access to defined and functional photopolymer networks. A difunctional bis(trimethylsilyl)silane with abstractable hydrogens (DSiH) was successfully synthesized in a simple one-pot procedure. The radical reactivity of DSiH with various homopolymerizable monomers (i.e., (meth)acrylate, vinyl ester, acrylamide) was assessed via 1H NMR spectroscopic studies. DSiH shows good reactivity with acrylates and vinyl esters. The most promising silane–acrylate system was further investigated in cross-linking formulations toward its reactivity (e.g., heat of polymerization, curing time, occurrence of gelation, double-bond conversion) and compared to state-of-the-art thiol–acrylate resins. The storage stability of prepared resin formulations is greatly improved for silane–acrylate systems vs thiol–ene resins. Double-bond conversion at the gel point (DBCgel) and overall DBC were increased, and polymerization-induced shrinkage stress has been significantly reduced with the introduction of silane–acrylate chemistry. Resulting photopolymer networks exhibit a homogeneous network architecture (indicated by a narrow glass transition) that can be tuned by varying silane concentration, and this confirms the postulated regulation of radical network formation. Similar to thiol–acrylate networks, this leads to more flexible photopolymer networks with increased elongation at break and improved impact resistance. Additionally, swelling tests indicate a high gel fraction for silane–acrylate photopolymers. PMID:29033466

Selective hydrophobic derivatization on the surface of helical silica nanotubes

NASA Astrophysics Data System (ADS)

Jin, Sun-Mi; Sung, Ji Yeong; Sim, Eun-Kyung; Jo, Nam-Ju; Kim, Jong Wook; Lee, Sumin; Jin, Jong Sung

2018-02-01

The chiral 1,2-diphenylethylenediamine derivative that is capable of spontaneous self-assembly was employed as an organogel template to produce a helical mesoporous silica nanotube containing gelators therein by following sol-gel polycondensation of TEOS. The synthesis enabled the successful introduction of the hydrocarbon of octyl silane (hydrophobic functional group) onto the outer surface of the silica nanotube while preserving the hydrophilic silanol (Sisbnd OH) group on internal surface of silica nanotube free from the gelators. This synthetic condition consists of a pre-stage of the introduction of a hydrophobic hydrocarbon functional group onto the outer surface of the silica nanotube selectively, and the post-stage washing of the gelators was presented together with a method analyzing the actions of organogels in the respective experimental processes.

Selective rhodium-catalyzed reduction of tertiary amides in amino acid esters and peptides.

PubMed

Das, Shoubhik; Li, Yuehui; Bornschein, Christoph; Pisiewicz, Sabine; Kiersch, Konstanze; Michalik, Dirk; Gallou, Fabrice; Junge, Kathrin; Beller, Matthias

2015-10-12

Efficient reduction of the tertiary amide bond in amino acid derivatives and peptides is described. Functional group selectivity has been achieved by applying a commercially available rhodium precursor and bis(diphenylphosphino)propane (dppp) ligand together with phenyl silane as a reductant. This methodology allows for specific reductive derivatization of biologically interesting peptides and offers straightforward access to a variety of novel peptide derivatives for chemical biology studies and potential pharmaceutical applications. The catalytic system tolerates a variety of functional groups including secondary amides, ester, nitrile, thiomethyl, and hydroxy groups. This convenient hydrosilylation reaction proceeds at ambient conditions and is operationally safe because no air-sensitive reagents or highly reactive metal hydrides are needed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bonding to new CAD/CAM resin composites: influence of air abrasion and conditioning agents as pretreatment strategy.

PubMed

Reymus, Marcel; Roos, Malgorzata; Eichberger, Marlis; Edelhoff, Daniel; Hickel, Reinhard; Stawarczyk, Bogna

2018-04-27

Because of their industrially standardized process of manufacturing, CAD/CAM resin composites show a high degree of conversion, making a reliable bond difficult to achieve. The purpose of this experiment was to investigate the tensile bond strength (TBS) of luting composite to CAD/CAM resin composite materials as influenced by air abrasion and pretreatment strategies. The treatment factors of the present study were (1) brand of the CAD/CAM resin composite (Brilliant Crios [Coltene/Whaledent], Cerasmart [GC Europe], Shofu Block HC [Shofu], and Lava Ultimate [3M]); (2) air abrasion vs. no air abrasion; and (3) pretreatment using a silane primer (Clearfil Ceramic Primer, Kuraray) vs. a resin primer (One Coat 7 Universal, Coltene/Whaledent). Subsequently, luting composite (DuoCem, Coltene/Whaledent) was polymerized onto the substrate surface using a mold. For each combination of the levels of the three treatment factors (4 (materials) × 2 (air abrasion vs. no air abrasion; resin) × 2 (primer vs. silane primer)), n = 15, specimens were prepared. After 24 h of water storage at 37 °C and 5000 thermo-cycles (5/55 °C), TBS was measured and failure types were examined. The resulting data was analyzed using Kaplan-Meier estimates of the cumulative failure distribution function with Breslow-Gehan tests and non-parametric ANOVA (Kruskal-Wallis test) followed by the multiple pairwise Mann-Whitney U test with α-error adjustment using the Benjamini-Hochberg procedure and chi-square test (p < 0.05). The additional air abrasion step increased TBS values and lowered failure rates. Specimens pretreated using a resin primer showed significantly higher TBS and lower failure rates than those pretreated using a silane primer. The highest failure rates were observed for groups pretreated with a silane primer. Within the Shofu Block HC group, all specimens without air abrasion and pretreatment with a silane primer debonded during the aging procedure. Before fixation of CAD/CAM resin composites, the restorations should be air abraded and pretreated using a resin primer containing methyl-methacrylate to successfully bond to the luting composite. The pretreatment of the CAD/CAM resin composite using merely a silane primer results in deficient adhesion. For a reliable bond of CAD/CAM resin composites to the luting composite, air abrasion and a special pretreatment strategy are necessary in order to achieve promising long-term results.

One Step Synthesis of a PerchlorinatedCyclohexasilane from Trichlorosilane: A Route to New Materials for Flexible Electronics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Philip Boudjouk

2010-03-27

The serendipitous discovery of tetradecachlorocyclohexasilane dianion 1 was recently reported by our group at NDSU. The dianion is isolated from a mixture of an amine template (pentaethyldiethylenetriamine, pedeta) and HSiCl{sub 3} as insoluble colorless crystals that are easily reduced to give cyclohexasilane (Si{sub 6}H{sub 12}) in high yields and purity. While the product Si{sub 6}H{sub 12} has been shown to be useful as a liquid silane precursor to a-Si:H rectifying diodes and field effect transistors, these initial studies show a non-uniform dopant distributions. The need for a homogeneous dopant has led our group to further develop the chemistry of cyclohexasilane.more » Toward that end, we have focused on the design of molecules that contain a single dopant moiety bound to one or more Si{sub 6} ring(s). New Si{sub 6}H{sub 11}E compounds (where E is an n-type or p-type dopant) are being investigated (eqs. 2, 3) and initial results will be reported including the isolation of chlorocyclohexasilane, Si{sub 6}H{sub 11}Cl. In addition, several different triamine ligand templates to for Si{sub 6}Cl{sub 14}{sup 2-} salts were investigated toward optimizing the yield and ease of isolation for both the salt and the product liquid silane. Cyclohexasilane (Si{sub 6}H{sub 12})-based inks have been used as liquid precursor to silicon-containing electronic materials. Spin-coating of Si{sub 6}H{sub 12}-based inks with subsequent UV light and/or thermal treatment yielded amorphous silicon (a-Si:H) films. Initial results demonstrated the formation of n-type and p-type a-Si that were used in heterojunction structures (i.e., thin a-Si films on heavily-doped Si wafer substrates). While present ink chemistries produce a-Si:H with a high resistivity (i.e., > 10{sup 6} {Omega}.cm), efforts are under development to address this limitation. Additionally, a new printing approach (i.e., collimated aerosol beam direct write, CAB-DW) was developed that allows the deposition of silane-based features with linewidths <10 {micro}m. Assuming silicon-based materials with good electrical properties will be developed, there may be significant cost advantages associated with the ability to controllably deposit the semiconductor in a metered fashion.« less

Area-Selective Atomic Layer Deposition of SiO2 Using Acetylacetone as a Chemoselective Inhibitor in an ABC-Type Cycle

PubMed Central

2017-01-01

Area-selective atomic layer deposition (ALD) is rapidly gaining interest because of its potential application in self-aligned fabrication schemes for next-generation nanoelectronics. Here, we introduce an approach for area-selective ALD that relies on the use of chemoselective inhibitor molecules in a three-step (ABC-type) ALD cycle. A process for area-selective ALD of SiO2 was developed comprising acetylacetone inhibitor (step A), bis(diethylamino)silane precursor (step B), and O2 plasma reactant (step C) pulses. Our results show that this process allows for selective deposition of SiO2 on GeO2, SiNx, SiO2, and WO3, in the presence of Al2O3, TiO2, and HfO2 surfaces. In situ Fourier transform infrared spectroscopy experiments and density functional theory calculations underline that the selectivity of the approach stems from the chemoselective adsorption of the inhibitor. The selectivity between different oxide starting surfaces and the compatibility with plasma-assisted or ozone-based ALD are distinct features of this approach. Furthermore, the approach offers the opportunity of tuning the substrate-selectivity by proper selection of inhibitor molecules. PMID:28850774

Synthesis of Silane and Silicon in a Non-equilibrium Plasma Jet

NASA Technical Reports Server (NTRS)

Calcote, H. F.

1978-01-01

The original objective of this program was to determine the feasibility of high volume, low-cost production of high purity silane or solar cell grade silicon using a non equilibrium plasma jet. The emphasis was changed near the end of the program to determine the feasibility of preparing photovoltaic amorphous silicon films directly using this method. The non equilibrium plasma jet should be further evaluated as a technique for producing high efficiency photovoltaic amorphous silicon films.

Shear Bond Strength of Resin Buttons to Lithium Disilicate and Leucite Reinforced Feldspathic Restorations

DTIC Science & Technology

2016-05-01

Hydrofluoric acid, silane coupling agent, light cured composite and ceramic restoration specimens (10 of each IPS e.max and Empress). The surface treatment...cured composite and ceramic restoration specimens (10 of each IPS e.max and Empress). The surface treatment in group C was applied to all specimens...and light cured for 20 seconds. 4) Group D: 5% Hydrofluoric acid, silane coupling agent, light cured composite and ceramic restoration (10 of

Ion Kinetics in Silane Plasmas

DTIC Science & Technology

1988-02-01

stimulated emission. Rg2 + is then a classical excimer laser scheme which ought to apply generally to the homonuclear and heteronuclear rare- gas dimer...kinetics of ion formation by electron impact and subsequent reaction in silane:noble- gas mixtures have been examined using pulsed ion cyclotron reso...charge transfer reactions such as X + + SiH4 -- SiH + + X + (4 - n)(H, H2) where X+ is a rare- gas or s:licon-hydride ion. Room-temperature rate constants

Influence of surface treatments on the shear bond strength of orthodontic brackets to porcelain

NASA Astrophysics Data System (ADS)

Wang, Cong; Zeng, Jishan; Wang, Shaoan; Yang, Zheng; Huang, Qian; Chen, Pixiu; Zhou, Shujuan; Liu, Xiaoqing

2008-11-01

The purpose of this study was to investigate the effect of various surface treatments after different storage time and thermocycling on the shear bond strength of orthodontic brackets to the feldspathic porcelain surfaces. 128 disc-shaped porcelain specimens were randomly assigned to the following surface treatments: 9.6% HFA, 9.6% HFA combined with silane, 50 μ aluminum trioxide sandblasting followed by silane and application of silane after 37% phosphoric acid. Metal or ceramic brackets were bonded onto each treated porcelain facet with light cured resin. The samples were stored in 37 °C water 1 day or 7 days, thermocycled 500 times from 5 to 55 °C. The shear bond strengths were measured (1 mm/min), and statistically analyzed. The bond failure sites were classified according to ARI system. The surface of the glazed, sandblasted, hydrofluoric and phosphoric acid etched porcelain were examined with SEM. All groups achieved reasonable bond strengths to withstand the application of orthodontic forces. Water storage for 7 days caused lower shear bond strength than that of 1 day. But there is no statistically significant difference between the two groups. The mean shear bond strength provided by ceramic bracket with mechanical retention had no statistical difference with that of metal bracket. Therefore, the optimal treatment for orthodontic brackets bonding to feldspathic porcelain was to apply phosphoric acid combined with silane.

Modification of silicone elastomer with zwitterionic silane for durable antifouling properties.

PubMed

Yeh, Shiou-Bang; Chen, Chien-Sheng; Chen, Wen-Yih; Huang, Chun-Jen

2014-09-30

Biofouling on medical devices generally causes adverse complications, such as thrombosis, infection, and pathogenic calcification. Silicone is a widely used material for medical applications. Its surface modification typically encounters undesirable "hydrophobic recovery", leading to deterioration of surface engineering. In this study, we developed a stable superhydrophilic zwitterionic interface on polydimethylsiloxane (PDMS) elastomer by covalent silanization of sulfobetaine silane (SBSi) to resist nonspecific adsorption of bacteria, proteins, and lipids. SBSi is a zwitterionic organosilane assembly, enabling resisting surface reconstruction by forming a cross-linked network and polar segregation. Surface elemental composition was confirmed by X-ray photoelectron spectroscopy (XPS), and the long-term stability of modification was accessed using a contact angle goniometer. The biofouling tests were carried out by exposing substrates to bacterial, protein, and lipid solutions, revealing the excellent bioinertness of SBSi-tailored PDMS, even after 30 day storage in ambient. For the real-world application, we modified commercially available silicone hydrogel contact lenses with developed zwitterionic silane, presenting its antibacterial adhesion property. Moreover, the cytotoxicity of SBSi was accessed with NIH-3T3 fibroblast by the MTT assay, showing negligible cytotoxicity up to a concentration of 5 mM. Consequently, the strategy of surface engineering in this work can effectively retard the "hydrophobic recovery" occurrence and can be applied to other silicone-based medical devices in a facile way.

In vitro investigation of biodegradable polymeric coating for corrosion resistance of Mg-6Zn-Ca alloy in simulated body fluid.

PubMed

Gaur, Swati; Singh Raman, R K; Khanna, A S

2014-09-01

A silane-based biodegradable coating was developed and investigated to improve corrosion resistance of an Mg-6Zn-Ca magnesium alloy to delay the biodegradation of the alloy in the physiological environment. Conditions were optimized to develop a stable and uniform hydroxide layer on the alloys surface-known to facilitate silane-substrate adhesion. A composite coating of two silanes, namely, diethylphosphatoethyltriethoxysilane (DEPETES) and bis-[3-(triethoxysilyl) propyl] tetrasulfide (BTESPT), was developed, by the sol-gel route. Corrosion resistance of the coated alloy was characterized in a modified-simulated body fluid (m-SBF), using potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The silane coating provided significant and durable corrosion resistance. During the course of this, hydrogen evolution and pH variation, if any, were monitored for both bare and coated alloys. The coating morphology was characterized using scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX) and the cross-linking in the coating was studied using Fourier transform infrared spectroscopy (FTIR). As indicated by X-ray diffraction (XRD) results, an important finding was the presence of hydrated magnesium phosphate on the sample that was subjected to immersion in m-SBF for 216h. Magnesium phosphate is reported to support osteoblast formation and tissue healing. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of Er,Cr:YSGG laser, air abrasion, and silane application on repaired shear bond strength of composites.

PubMed

Cho, S D; Rajitrangson, P; Matis, B A; Platt, J A

2013-01-01

Aged resin composites have a limited number of carbon-carbon double bonds to adhere to a new layer of resin. Study objectives were to 1) evaluate various surface treatments on repaired shear bond strength between aged and new resin composites and 2) to assess the influence of a silane coupling agent after surface treatments. Eighty disk-shape resin composite specimens were fabricated and thermocycled 5000 times prior to surface treatment. Specimens were randomly assigned to one of the three surface treatment groups (n=20): 1) air abrasion with 50-μm aluminum oxide, 2) tribochemical silica coating (CoJet), or 3) Er,Cr:YSGG (erbium, chromium: yttrium-scandium-gallium-garnet) laser or to a no-treatment control group (n=20). Specimens were etched with 35% phosphoric acid, rinsed, and dried. Each group was divided into two subgroups (n=10): A) no silanization and B) with silanization. The adhesive agent was applied and new resin composite was bonded to each conditioned surface. Shear bond strength was evaluated and data analyzed using two-way analysis of variance (ANOVA). Air abrasion with 50-μm aluminum oxide showed significantly higher repair bond strength than the Er,Cr:YSGG laser and control groups. Air abrasion with 50-μm aluminum oxide was not significantly different from tribochemical silica coating. Tribochemical silica coating had significantly higher repair bond strength than Er,Cr:YSGG laser and the control. Er,Cr:YSGG laser and the control did not have significantly different repair bond strengths. Silanization had no influence on repair bond strength for any of the surface treatment methods. Air abrasion with 50-μm aluminum oxide and tribochemical silica followed by the application of bonding agent provided the highest repair shear bond strength values, suggesting that they might be adequate methods to improve the quality of repairs of resin composites.

Effects of three silane primers and five adhesive agents on the bond strength of composite material for a computer-aided design and manufacturing system.

PubMed

Shinohara, Ayano; Taira, Yohsuke; Sakihara, Michino; Sawase, Takashi

2018-01-01

Objective The objective of this study was to evaluate the effects of combinations of silane primers and adhesive agents on the bond strength of a composite block for a computer-aided design and manufacturing system. Material and Methods Three silane primers [Clearfil Ceramic Primer (CP), Super-Bond PZ Primer (PZ), and GC Ceramic Primer II (GP)] were used in conjunction with five adhesive agents [G-Premio Bond (P-Bond), Repair Adhe Adhesive (R-Adhesive), Super-Bond D-Liner Dual (SB-Dual), Super-Bond C&B (SB-Self), and SB-Dual without tributylborane derivative (SB-Light)]. The surface of a composite block (Gradia Block) was ground with silicon carbide paper. After treatment with a silane primer, a adhesive agent was applied to each testing specimen. The specimens were then bonded with a light-curing resin composite. After 24 h, the shear bond strength values were determined and compared using a post hoc test (α=0.05, n=8/group). We also prepared control specimens without primer (No primer) and/or without adhesive agent (No adhesive). Results PZ/SB-Dual and GP/SB-Dual presented the highest bond strength, followed by GP/P-Bond, CP/SB-Dual, CP/R-Adhesive, No primer/SB-Dual, GP/R-Adhesive, CP/P-Bond, No primer/R-Adhesive, PZ/R-Adhesive, CP/SB-Self, PZ/P-Bond, PZ/SB-Self, and GP/SB-Self in descending order of bond strength. No primer/P-Bond, No primer/SB-Self, and all specimens in the SB-Light and No adhesive groups presented the lowest bond strengths. Conclusion A dual-curing adhesive agent (SB-Dual) containing a tributylborane derivative in combination with a silane primer (GP or PZ) presents a greater bond strength between the composite block and the repairing resin composite than the comparators used in the study.

Effects of three silane primers and five adhesive agents on the bond strength of composite material for a computer-aided design and manufacturing system

PubMed Central

2018-01-01

Abstract Objective The objective of this study was to evaluate the effects of combinations of silane primers and adhesive agents on the bond strength of a composite block for a computer-aided design and manufacturing system. Material and Methods Three silane primers [Clearfil Ceramic Primer (CP), Super-Bond PZ Primer (PZ), and GC Ceramic Primer II (GP)] were used in conjunction with five adhesive agents [G-Premio Bond (P-Bond), Repair Adhe Adhesive (R-Adhesive), Super-Bond D-Liner Dual (SB-Dual), Super-Bond C&B (SB-Self), and SB-Dual without tributylborane derivative (SB-Light)]. The surface of a composite block (Gradia Block) was ground with silicon carbide paper. After treatment with a silane primer, a adhesive agent was applied to each testing specimen. The specimens were then bonded with a light-curing resin composite. After 24 h, the shear bond strength values were determined and compared using a post hoc test (α=0.05, n=8/group). We also prepared control specimens without primer (No primer) and/or without adhesive agent (No adhesive). Results PZ/SB-Dual and GP/SB-Dual presented the highest bond strength, followed by GP/P-Bond, CP/SB-Dual, CP/R-Adhesive, No primer/SB-Dual, GP/R-Adhesive, CP/P-Bond, No primer/R-Adhesive, PZ/R-Adhesive, CP/SB-Self, PZ/P-Bond, PZ/SB-Self, and GP/SB-Self in descending order of bond strength. No primer/P-Bond, No primer/SB-Self, and all specimens in the SB-Light and No adhesive groups presented the lowest bond strengths. Conclusion A dual-curing adhesive agent (SB-Dual) containing a tributylborane derivative in combination with a silane primer (GP or PZ) presents a greater bond strength between the composite block and the repairing resin composite than the comparators used in the study. PMID:29742254

Low cost solar array project. Experimental process system development unit for producing semiconductor-grade silicon using the silane-to-silicon process

NASA Technical Reports Server (NTRS)

1980-01-01

Technical activities are reported in the design of process, facilities, and equipment for producing silicon at a rate and price comensurate with production goals for low cost solar cell modules. The silane-silicone process has potential for providing high purity poly-silicon on a commercial scale at a price of fourteen dollars per kilogram by 1986, (1980 dollars). Commercial process, economic analysis, process support research and development, and quality control are discussed.

Method for Waterproofing Ceramic Materials

NASA Technical Reports Server (NTRS)

Cagliostro, Domenick E. (Inventor); Hsu, Ming-Ta S. (Inventor)

1998-01-01

Hygroscopic ceramic materials which are difficult to waterproof with a silane, substituted silane or silazane waterproofing agent, such as an alumina containing fibrous, flexible and porous, fibrous ceramic insulation used on a reentry space vehicle, are rendered easy to waterproof if the interior porous surface of the ceramic is first coated with a thin coating of silica. The silica coating is achieved by coating the interior surface of the ceramic with a silica precursor converting the precursor to silica either in-situ or by oxidative pyrolysis and then applying the waterproofing agent to the silica coated ceramic. The silica precursor comprises almost any suitable silicon containing material such as a silane, silicone, siloxane, silazane and the like applied by solution, vapor deposition and the like. If the waterproofing is removed by e.g., burning, the silica remains and the ceramic is easily rewaterproofed. An alumina containing TABI insulation which absorbs more that five times its weight of water, absorbs less than 10 wt. % water after being waterproofed according to the method of the invention.

Surface modification and characterization of basalt fibers as potential reinforcement of concretes

NASA Astrophysics Data System (ADS)

Iorio, M.; Santarelli, M. L.; González-Gaitano, G.; González-Benito, J.

2018-01-01

Basalt fibers were surface treated with silane coupling agents as a method to enhance the adhesion and durability of fiber-matrix interfaces in concrete based composite materials. In particular, this work has been focused on the study of basalt fibers chemical coatings with aminosilanes and their subsequent characterization. Surface treatments were carried out after removing the original sizing applied by manufacturer and pretreating them with an activation process of surface silanol regeneration. Different samples were considered to make convenient comparisons: as received fibers (commercial), calcinated fibers (without commercial sizing), activated samples (calcinated fibers subjected to an acid process for hydroxyl regeneration), and silanized fibers with γ-aminopropiltriethoxysilane, γ-aminopropilmethyldiethoxysilane and a mixture of 50% by weight of both silanes. A deep characterization was carried out in terms of structure using X-ray diffraction, XRD, and Fourier transform infrared spectroscopy, FTIR, thermal properties by thermogravimetric analysis, TGA, coupled with single differential thermal analysis, SDTA, and morphology by scanning electron microscopy, SEM, and atomic force microscopy, AFM.

Versatile bio-ink for covalent immobilization of chimeric avidin on sol-gel substrates.

PubMed

Heikkinen, Jarkko J; Kivimäki, Liisa; Määttä, Juha A E; Mäkelä, Inka; Hakalahti, Leena; Takkinen, Kristiina; Kulomaa, Markku S; Hytönen, Vesa P; Hormi, Osmo E O

2011-10-15

A bio-ink for covalent deposition of thermostable, high affinity biotin-binding chimeric avidin onto sol-gel substrates was developed. The bio-ink was prepared from heterobifunctional crosslinker 6-maleimidohexanoic acid N-hydroxysuccinimide which was first reacted either with 3-aminopropyltriethoxysilane or 3-aminopropyldimethylethoxysilane to form silane linkers 6-maleimide-N-(3-(triethoxysilyl)propyl)hexanamide or -(ethoxydimethylsilyl)propyl)-hexanamide. C-terminal cysteine genetically engineered to chimeric avidin was reacted with the maleimide group of silane linker in methanol/PBS solution to form a suspension, which was printed on sol-gel modified PMMA film. Different concentrations of chimeric avidin and ratios between silane linkers were tested to find the best properties for the bio-ink to enable gravure or inkjet printing. Bio-ink prepared from 3-aminopropyltriethoxysilane was found to provide the highest amount of active immobilized chimeric avidin. The developed bio-ink was shown to be valuable for automated fabrication of avidin-functionalized polymer films. Copyright © 2011 Elsevier B.V. All rights reserved.

Evaluation of the effects of aging in synthetic saliva solution of both commercial and silanized Nd-Fe-B magnets for dental application

NASA Astrophysics Data System (ADS)

Fabiano, F.; Puliafito, V.; Calabrese, L.; Borsellino, C.; Bonaccorsi, L. M.; Giordano, A.; Fabiano, V.; Cordasco, G.

2016-04-01

Neodymium-iron-boron magnets are able to ensure a magnetic flux with high maximum energy product also at miniaturized size. In the past, due to their marked corrosion in saliva they were unsuccessfully implemented in orthodontic systems. Thereby, we propose a multi-layered organic-inorganic coating able to supply anticorrosion resistance, wear resistance and durability to the whole assembly. We evaluated the influence on the magnetic force of commercial nickel plated and silanized Nd-Fe-B during aging time in synthetic Fusayama saliva. Two magnets based-micromagnetic simulations were performed in order to analyze the magnetic field generated which is linked to the magnetic force. Our key results underline that the proposed hybrid coating does not affect the magnetic force of Nd-Fe-B magnets, moreover, preventing corrosion degradation in aggressive solution. Thus the limiting aspects avoiding the use of Nd-Fe-B magnets for orthodontic and prosthodontic applications can be overcome by using silane agents as surface coating.

Silane surface modification for improved bioadhesion of esophageal stents

NASA Astrophysics Data System (ADS)

Karakoy, Mert; Gultepe, Evin; Pandey, Shivendra; Khashab, Mouen A.; Gracias, David H.

2014-08-01

Stent migration occurs in 10-40% of patients who undergo placement of esophageal stents, with higher migration rates seen in those treated for benign esophageal disorders. This remains a major drawback of esophageal stent therapy. In this paper, we propose a new surface modification method to increase the adhesion between self-expandable metallic stents (SEMS) and tissue while preserving their removability. Taking advantage of the well-known affinity between epoxide and amine terminated silane coupling agents with amine and carboxyl groups that are abundant in proteins and related molecules in the human body; we modified the surfaces of silicone coated esophageal SEMS with these adhesive self-assembled monolayers (SAMs). We utilized vapor phase silanization to modify the surfaces of different substrates including PDMS strips and SEMS, and measured the force required to slide these substrates on a tissue piece. Our results suggest that surface modification of esophageal SEMS via covalent attachment of protein-binding coupling agents improves adhesion to tissue and could offer a solution to reduce SEMS migration while preserving their removability.

Control of electroosmosis in coated quartz capillaries

NASA Technical Reports Server (NTRS)

Herren, Blair J.; Van Alstine, James; Snyder, Robert S.; Shafer, Steven G.; Harris, J. Milton

1987-01-01

The effectiveness of various coatings for controlling the electroosmotic fluid flow that hinders electrophoretic processes is studied using analytical particle microelectrophoresis. The mobilities of 2-micron diameter glass and polystyrene latex spheres (exhibiting both negative and zero effective surface charge) were measured in 2-mm diameter quartz capillaries filled with NaCl solutions within the 3.5-7.8 pH range. It is found that capillary inner surface coatings using 5000 molecular weight (or higher) poly(ethylene glycol): significantly reduced electroosmosis within the selected pH range, were stable for long time periods, and appeared to be more effective than dextran, methylcellulose, or silane coatings.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wilde, E.W.; Radway, J.C.; Hazen, T.C.

The immobilization of TCE-degrading bacterium Burkholderia cepacia was evaluated using hydrophilic polyurethane foam. The influence of several foam formulation parameters upon cell retention was examined. Surfactant type was a major determinant of retention, with a lecithin- based compound retaining more cells than pluronic or silicone based surfactants. Excessive amounts of surfactant led to increased washout of bacteria. Increasing the biomass concentration from 4.8% to 10.5% caused fewer cells to be washed out. Embedding at reduced temperature did not significantly affect retention, while the use of a silane binding agent gave inconsistent results. The optimal formulation retained all but 0.2% ofmore » total embedded cells during passage of 2 liters of water through columns containing 2 g of foam. All foam formulations tested reduced the culturability of embedded cells by several orders of magnitude. However, O{sub 2} and CO{sub 2} evolution rates of embedded cells were never less than 50% of unembedded cells. Nutrient amendments stimulated an increase in cell volume and ribosomal activity as indicated by hybridization studies using fluorescently labeled ribosomal probes. these results indicated that, although immobilized cells were nonculturable, they were metabolically active and thus could be used for biodegradation of toxic compounds.« less

Cyclodextrin-based microsensor for volatile organic compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Swanson, B.I.; Li, D.Q.

1996-12-31

The direct covalent attachment of modified {alpha}- and {beta}-cyclodextrin on oxide surfaces has been studied for application in chemical sensors. First, oxide surfaces were treated with a silane coupling layer followed by the addition of cyclodextrin to form a self-assembled monolayer (SAM) of host receptors. Second, the oxide surfaces were reacted with a sol-gel (SG) precursor based on cyclodextrin structure to form a thick film with defined hydrophobic cyclodextrin cavities. The sensing properties of both films (SAM and SG) were examined with surface acoustic wave (SAW) measurement platform. Molecular interactions between an organic guest and a host thin-film on amore » 200 MHZ SAW resonator are being studied as a method of tracking and recognizing the presence of volatile organics. Surface acoustic wave sensors based on the inclusion chemistry of the bucket-type (cyclodextrin) molecules, were capable of detecting volatile organic compounds (VOCs) down to ppb levels. Because the nature of the interactions is moderate but noncovalent, detection of these VOCs was possible using a reversible real-time mode. Pattern recognition with an array of complementary microsensors appears to be a viable approach for identifying and quantifying VOCs. Recent results using optical waveguides for sensor transduction will also be discussed.« less

Identification of Hydrogen Disulfanes and Hydrogen Trisulfanes in H2S Bottle, in Flint, and in Dry Mineral White Wine.

PubMed

Starkenmann, Christian; Chappuis, Charles Jean-Francois; Niclass, Yvan; Deneulin, Pascale

2016-11-30

Through the accidental contamination of a gas cylinder of H 2 S, the importance of polysulfanes for flint, gun powder, and match odors was discovered. The hydrogen disulfane was prepared from disulfanediylbis[methyl(diphenyl)silane], and its odor descriptor was evaluated in the gas phase from a gas chromatograph coupled to an olfaction port. The occurrence of this compound in flint and pebbles was confirmed by analyses after derivatization with pentafluorobromobenzene. The occurrence of this sulfane was also confirmed in two dry white Swiss Chasselas wines, sorted by a large-scale sensory analysis from 80 bottles and evaluated by 62 wine professionals. The occurrence of disulfane was confirmed for the two wines described as the most mineral. Polysulfane comprises a class of compounds contributing to the flint odor and that may contribute to the wine mineral odor descriptor. Due to the high volatility and instability pure HSSH was not isolated but kept in solution and its odor profile was described by gas chromatography coupled to an olfaction port as flint, matches, and fireworks with a higher odor intensity compared to H 2 S.

A simple and sensitive methodology for voltammetric determination of valproic acid in human blood plasma samples using 3-aminopropyletriethoxy silane coated magnetic nanoparticles modified pencil graphite electrode.

PubMed

Zabardasti, Abedin; Afrouzi, Hossein; Talemi, Rasoul Pourtaghavi

2017-07-01

In this work, we have prepared a nano-material modified pencil graphite electrode for the sensing of valproic acid (VA) by immobilization 3-aminopropyletriethoxy silane coated magnetic nanoparticles (APTES-MNPs) on the pencil graphite surface (PGE). Electrochemical studies indicated that the APTES-MNPs efficiently increased the electron transfer kinetics between VA and the electrode and the free NH 2 groups of the APTES on the outer surface of magnetic nanoparticles can interact with carboxyl groups of VA. Based on this, we have proposed a sensitive, rapid and convenient electrochemical method for VA determination. Under the optimized conditions, the reduction peak current of VA is found to be proportional to its concentration in the range of 1.0 (±0.2) to 100.0 (±0.3) ppm with a detection limit of 0.4 (±0.1) ppm. The whole sensor fabrication process was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) methods with using [Fe(CN) 6 ] 3-/4- as an electrochemical redox indicator. The prepared modified electrode showed several advantages such as high sensitivity, selectivity, ease of preparation and good repeatability, reproducibility and stability. The proposed method was applied to determination of valproic acid in blood plasma samples and the obtained results were satisfactory accurate. Copyright © 2017. Published by Elsevier B.V.

Organosilane self-assembled layers (SAMs) and hybrid silicate magnesium-rich primers for the corrosion protection of aluminum alloy 2024 T3

NASA Astrophysics Data System (ADS)

Wang, Duhua

Although current chromate coatings function very well in corrosion protection for aircraft alloys, such as aluminum alloy 2024 T3, the U.S. Environmental Protection Agency is planning to totally ban the use of chromates as coating materials in the next decade or so because of their extremely toxic effect. For this purpose, both self-assembled layers and silicate magnesium-rich primers were tested to provide the corrosion protection for aluminum alloy. The long-term goal of this research is to develop a coating system to replace the current chromate coating for aircraft corrosion protection. Aluminum alloy 2024 T3 substrates were modified with self-assembled monolayer or multilayer thin films from different alkylsilane compounds. Mono-functional silanes, such as octadecyltrichlorosilane (C18SiCl3), can form a mixed hydrophobic monolayer or multilayer thin film on the aluminum oxide surface to provide a barrier to water and other electrolytes, so the corrosion resistance of the SAMs modified surface was increased significantly. On the other hand, the bi-functional silane self-assembly could attach the aluminum surface through the silicon headgroup while using its functional tailgroup to chemically bond the polymer coating, thus improving the adhesion between the aluminum substrate and coating substantially, and seems to contribute more to corrosion protection of aluminum substrate. Organosilanes were also combined with tetraethyl orthosilicate (TEOS) in propel ratios to form a sol-gel binder to make silicate magnesium-rich primers. Analogue to the inorganic zinc-rich coatings, the silicate magnesium-rich primers also showed excellent adhesion and solvent resistance. The sacrificial magnesium pigments and the chemically inert silicate binder both contribute to the anti-corrosion properties. Future studies will be focused on the formula optimization for better toughness, chemical resistance and anticorrosion performance.

Investigation of quaternary ammonium silane-coated sand filter for the removal of bacteria and viruses from drinking water.

PubMed

Torkelson, A A; da Silva, A K; Love, D C; Kim, J Y; Alper, J P; Coox, B; Dahm, J; Kozodoy, P; Maboudian, R; Nelson, K L

2012-11-01

To develop an anti-microbial filter media using an attached quaternary ammonium compound (QAC) and evaluate its performance under conditions relevant to household drinking water treatment in developing countries. Silica sand was coated with dimethyloctadecyl [3-(trimethoxysilyl) propyl] ammonium chloride via covalent silane chemistry. Filter columns packed with coated media were challenged with micro-organisms under different water quality conditions. The anti-bacterial properties were investigated by visualizing Escherichia coli (E. coli) attachment to coated media under fluorescence microscopy combined with a live/dead stain. A 9-cm columns with a filtration velocity of 18 m h(-1) achieved log(10) removals of 1·7 for E. coli, 1·8 for MS2 coliphage, 1·9 for Poliovirus type 3 and 0·36 for Adenovirus type 2, compared to 0·1-0·3 log(10) removals of E. coli and MS2 by uncoated sand. Removal scaled linearly with column length and decreased with increasing ionic strength, flow velocity, filtration time and humic acid presence. Escherichia coli attached to QAC-coated sand were observed to be membrane-permeable, providing evidence of inactivation. Filtration with QAC-coated sand provided higher removal of bacteria and viruses than filtration with uncoated sand. However, major limitations included rapid fouling by micro-organisms and natural organic matter and low removal of viruses PRD1 and Adenovirus 2. QAC-coated media may be promising for household water treatment. However, more research is needed on long-term performance, options to reduce fouling and inactivation mechanisms. © 2012 The Authors Journal of Applied Microbiology © 2012 The Society for Applied Microbiology.

Low Cost Silicon Solar Array Project. Feasibility of Low-cost, High-volume Production of Silane and Pyrolysis of Silane to Semiconductor-grade Silicon

NASA Technical Reports Server (NTRS)

Breneman, W. C.; Farrier, E. G.; Morihara, H.

1978-01-01

The presence of copper promotes a more rapid approach to the steady stete operating condition and results in a more consistent reactor effluent composition. The average kinetic and equilibrium yield are unchanged. Incoloy has been identified as the preferred choice of material of construction for the hydrogenation reactor although certain metallurgical changes were noted in samples exposed to the H2/HCl atmosphere at 500 C which indicate the need for more testing.

Catalytic enantioselective silylation of N-sulfonylimines: asymmetric synthesis of α-amino acids from CO2 via stereospecific carboxylation of α-amino silanes.

PubMed

Mita, Tsuyoshi; Sugawara, Masumi; Saito, Keisuke; Sato, Yoshihiro

2014-06-06

A catalytic enantioselective silylation of N-tert-butylsulfonylimines using a Cu-secondary diamine complex was demonstrated. The resulting optically active α-amino silanes could be carboxylated under a CO2 atmosphere (1 atm) to afford the corresponding α-amino acids in a stereoretentive manner. This two-step sequence provides a new synthetic protocol for optically active α-amino acids from gaseous CO2 and imines in the presence of a catalytic amount of a chiral source.

Homogeneous reactions of hydrocarbons, silane, and chlorosilanes in radiofrequency plasmas at low pressures

NASA Technical Reports Server (NTRS)

Avni, R.; Carmi, U.; Inspektor, A.; Rosenthal, I.

1984-01-01

The ion-molecule and radical-molecule mechanisms are responsible for the dissociation of hydrocarbon, silane, and chlorosilane monomers and the formation of polymerized species, respectively, in an RF plasma discharge. In a plasma containing a mixture of monomer and argon the rate-determining step for both dissociation and polymerization is governed by an ion-molecule type of interaction. Adding hydrogen or ammonia to the monomer-argon mixture transforms the rate-determining step from an ion-molecule interaction to a radical-molecule interaction for both monomer dissociation and polymerization.

Mechanical and thermal properties of short-coirfiber-reinforced natural rubber/polyethylene composites

NASA Astrophysics Data System (ADS)

Xu, Zh. H.; Kong, Zh. N.

2014-07-01

Natural rubber (NR) and polyethylene (PE) composites were compounded with chemically treated coir fibers by using a heated two-roll mill. Two chemical treatments of the fibers — by silane and sodium hydroxide — were carried out to improve the interfacial adhesion between them and the polyethylene matrix. The mechanical properties of the composites obtained were evaluated and compared with those made from a neat polymer and untreated fibers. The mechanical properties of the composites, such as the tensile strength, Young's modulus, and the elongation at break, were examined, and their shrinkage and flame retardant characteristics were measured. From these experiments, the effect of plasma treatment on the mechanical-physical behavior of coconut-fiberreinforced NR/PE composites was identified. In addition, their thermal characteristics were evaluated, and the results showed a slight decrease in them with increasing content of coir fibers.

Effects of Mechanical and Chemical Pretreatments of Zirconia or Fiber Posts on Resin Cement Bonding

PubMed Central

Li, Rui; Zhou, Hui; Wei, Wei; Wang, Chen; Sun, Ying Chun; Gao, Ping

2015-01-01

The bonding strength between resin cement and posts is important for post and core restorations. An important method of improving the bonding strength is the use of various surface pretreatments of the post. In this study, the surfaces of zirconia (fiber) posts were treated by mechanical and/or chemical methods such as sandblasting and silanization. The bonding strength between the zirconia (fiber) post and the resin cement was measured by a push-out method after thermocycling based on the adhesion to Panavia F 2.0 resin cement. The zirconia and fiber posts exhibited different bonding strengths after sandblasting and/or silanization because of the different strengths and chemical structures. The zirconia post showed a high bonding strength of up to 17.1 MPa after a combined treatment of sandblasting and silanization because of the rough surface and covalent bonds at the interface. This effect was also enhanced by using 1,2-bis(trimethoxysilyl)ethane for the formation of a flexible layer at the interface. In contrast, a high bonding strength of 13.9 MPa was obtained for the fiber post treated by silane agents because the sandblasting treatment resulted in damage to the fiber post, as observed by scanning electron microscopy. The results indicated that the improvement in the bonding strength between the post and the resin cement could be controlled by different chemical and/or mechanical treatments. Enhanced bonding strength depended on covalent bonding and the surface roughness. A zirconia post with high bonding strength could potentially be used for the restoration of teeth in the future. PMID:26066349

Nanoscopic insights into the effect of silicon on core-shell InGaN/GaN nanorods: Luminescence, composition, and structure

NASA Astrophysics Data System (ADS)

Ren, Christopher X.; Tang, Fengzai; Oliver, Rachel A.; Zhu, Tongtong

2018-01-01

GaN-based nanorods and nanowires have recently shown great potential as a platform for future energy-efficient photonic and optoelectronic applications, such as light emitting diodes and nanolasers. Currently, the most industrially scalable method of growing III-nitride nanorods remains metal-organic vapour phase epitaxy: whilst this growth method is often used in conjunction with extrinsic metallic catalyst particles, these particles can introduce unwanted artifacts in the nanorods such as stacking faults. In this paper, we examine the catalyst-free growth of GaN/InGaN core-shell nanorods by metal-organic vapor phase epitaxy for optoelectronic applications using silane to enhance the vertical growth of the nanorods. We find that both the silane concentration and exposure time can greatly affect the nanorod properties, and that larger concentrations and longer exposure times can severely degrade the nanorod structure and thus result in reduced emission from the InGaN QW shell. Finally, we report that the mechanism behind the effect of silane on the nanorod structure is the unintentional formation of an SiNx interlayer following completion of the growth of the nanorod core. This interlayer induces the growth of GaN islands on the nanorod sidewalls, the spatial distribution of which can affect their subsequent coalescence during the lateral growth stages and result in non-uniformity in the nanorod structure. This suggests that careful control of the silane flow must be exerted during growth to achieve both high aspect ratio nanorods and uniform emission along the length of the nanorod.

Development of high-viscosity, two-paste bioactive bone cements.

PubMed

Deb, S; Aiyathurai, L; Roether, J A; Luklinska, Z B

2005-06-01

Self-curing two-paste bone cements have been developed using methacrylate monomers with a view to formulate cements with low polymerization exotherm, low shrinkage, better mechanical properties, and improved adhesion to bone and implant surfaces. The monomers include bis-phenol A glycidyl dimethacrylate (bis-GMA), urethane dimethacrylate (UDMA) and triethylene glycol dimethacrylate (TEGDMA) as a viscosity modifier. Two-paste systems were formulated containing 60% by weight of a bioactive ceramic, hydroxyapatite. A methacroyloxy silane (A174) was used as a coupling agent due to its higher water stability in comparison to other aminosilanes to silanate the hydroxyapatite particles prior to composite formulation. A comparison of the FT-infrared spectrum of hydroxyapatite and silanated hydroxyapatite showed the presence of the carbonyl groups ( approximately 1720 cm(-1)), -C=C-( approximately 1630 cm(-1)) and Si-O- (1300-1250 cm(-1)) which indicated the availability of silane groups on the filler surface. Two methods of mixing were effected to form the bone cement: firstly by mixing in an open bowl and secondly by extruding the two pastes by an auto-mixing tip using a gun to dispense the pastes. Both types of cements yielded low polymerization exotherms with good mechanical properties; however, the lower viscosity of UDMA allowed better extrusion and handling properties. A biologically active apatite layer formed on the bone cement surface within a short period after its immersion in simulated body fluid, demonstrating in vitro bioactivity of the composite. This preliminary data thus suggests that UDMA is a viable alternative to bis-GMA as a polymerizable matrix in the formation of bone cements.

Ultrathin Polymer Films, Patterned Arrays, and Microwells

NASA Astrophysics Data System (ADS)

Yan, Mingdi

2002-05-01

The ability to control and tailor the surface and interface properties of materials is important in microelectronics, cell growth control, and lab-on-a-chip devices. Modification of material surfaces with ultrathin polymer films is attractive due to the availability of a variety of polymers either commercially or by synthesis. We have developed two approaches to the attachment of ultrathin polymer films on solid substrates. In the first method, a silane-functionalized perfluorophenyl azide (PFPA-silane) was synthesized and used to covalently immobilize polymer thin films on silicon wafers. Silanization of the wafer surface with the PFPA-silane introduced a monolayer of azido groups which in turn covalently attached the polymer film by way of photochemically initiated insertion reactions. The thickness of the film could be adjusted by the type and the molecular weight of the polymer. The method is versatile due to the general C-H and/or N-H insertion reactions of crosslinker; and therefore, no specific reactive functional groups on the polymers are required. Using this method, a new type of microwell array was fabricated from covalently immobilized polymer thin films on flat substrates. The arrays were characterized with AFM, XPS, and TOF-SIMS. The second method describes the attachment of polymer thin films on solid substrates via UV irradiation. The procedure consisted of spin-coating a polymer film and irradiating the film with UV light. Following solvent extraction, a thin film remained. The thickness of the film, from a few to over a hundred nanometers, was controlled by varying solution concentration and the molecular weight of the polymer.

Effects of tributylborane-activated adhesive and two silane agents on bonding computer-aided design and manufacturing (CAD/CAM) resin composite.

PubMed

Shinohara, Ayano; Taira, Yohsuke; Sawase, Takashi

2017-10-01

The present study was conducted to evaluate the effects of an experimental adhesive agent [methyl methacrylate-tributylborane liquid (MT)] and two adhesive agents containing silane on the bonding between a resin composite block of a computer-aided design and manufacturing (CAD/CAM) system and a light-curing resin composite veneering material. The surfaces of CAD/CAM resin composite specimens were ground with silicon-carbide paper, treated with phosphoric acid, and then primed with either one of the two silane agents [Scotchbond Universal Adhesive (SC) and GC Ceramic Primer II (GC)], no adhesive control (Cont), or one of three combinations (MT/SC, MT/GC, and MT/Cont). A light-curing resin composite was veneered on the primed CAD/CAM resin composite surface. The veneered specimens were subjected to thermocycling between 4 and 60 °C for 10,000 cycles, and the shear bond strengths were determined. All data were analyzed using analysis of variance and a post hoc Tukey-Kramer HSD test (α = 0.05, n = 8). MT/SC (38.7 MPa) exhibited the highest mean bond strengths, followed by MT/GC (30.4 MPa), SC (27.9 MPa), and MT/Cont (25.7 MPa), while Cont (12.9 MPa) and GC (12.3 MPa) resulted in the lowest bond strengths. The use of MT in conjunction with a silane agent significantly improved the bond strength. Surface treatment with appropriate adhesive agents was confirmed as a prerequisite for veneering CAD/CAM resin composite restorations.

High-Q whispering-gallery mode sensor in liquids

NASA Astrophysics Data System (ADS)

Nadeau, Jay L.; Ilchenko, Vladimir S.; Kossakovski, Dmitri; Bearman, Gregory H.; Maleki, Lute

2002-06-01

Optical sensing of biomolecules on microfabricated glass surfaces requires surface coatings that minimize nonspecific binding while preserving the optical properties of the sensor. Microspheres with whispering-gallery (WG) modes can achieve quality factor (Q) levels many orders of magnitude greater than those of other WG-based microsensors: greater than 1010 in air, and greater than 109 in a variety of solvents, including methanol, H2O and phosphate buffered saline (PBS). The presence of dyes that absorb in the wavelength of the WG excitation in the evanescent zone can cause this Q value to drop by almost 3 orders of magnitude. Silanization of the surface with mercapto-terminal silanes is compatible with high Q (>109), but chemical cross-linking of streptavidin reduces the Q to 105-106 due to build-up of a thick, irregular layer of protein. However, linkage of biotin to the silane terminus preserves the Q at a ~2x107 and yields a reactive surface sensitive to avidin-containing ligands in a concentration-dependent manner. Improvements in the reliability of the surface chemistry show promise for construction of an ultrasensitive biosensor.

Synthesis and characterizations of melamine-based epoxy resins.

PubMed

Ricciotti, Laura; Roviello, Giuseppina; Tarallo, Oreste; Borbone, Fabio; Ferone, Claudio; Colangelo, Francesco; Catauro, Michelina; Cioffi, Raffaele

2013-09-05

A new, easy and cost-effective synthetic procedure for the preparation of thermosetting melamine-based epoxy resins is reported. By this innovative synthetic method, different kinds of resins can be obtained just by mixing the reagents in the presence of a catalyst without solvent and with mild curing conditions. Two types of resins were synthesized using melamine and a glycidyl derivative (resins I) or by adding a silane derivative (resin II). The resins were characterized by means of chemical-physical and thermal techniques. Experimental results show that all the prepared resins have a good thermal stability, but differ for their mechanical properties: resin I exhibits remarkable stiffness with a storage modulus value up to 830 MPa at room temperature, while lower storage moduli were found for resin II, indicating that the presence of silane groups could enhance the flexibility of these materials. The resins show a pot life higher than 30 min, which makes these resins good candidates for practical applications. The functionalization with silane terminations can be exploited in the formulation of hybrid organic-inorganic composite materials.

Mechanical properties of functionalised CNT filled kenaf reinforced epoxy composites

NASA Astrophysics Data System (ADS)

Sapiai, Napisah; Jumahat, Aidah; Mahmud, Jamaluddin

2018-04-01

This paper aims to study the effect of functionalised carbon nanotubes (CNT) on mechanical properties of kenaf fibre reinforced polymer composites. The CNT was functionalised using acid mixtures of H2SO4:HNO3 and 3-Aminopropyl Triethoxysilane before it was incorporated into epoxy resin. Three different types of CNT were used, i.e. pristine (PCNT), acid-treated (ACNT) and acid-silane treated (SCNT), to fabricate kenaf composite. Three different filler contents were mixed in each composite system, i.e. 0.5, 0.75 and 1.0 wt%. The functionalised CNT was characterized using x-ray Diffraction (XRD), Fourier Transform Infrared (FTIR) and Transmission Electron Microscopy (TEM). Tensile, flexural and Izod impact tests were conducted in order to evaluate the effect of CNT contents and surface treatment of mechanical properties of kenaf composites. It was observed that the inclusion of 1 wt% acid-silane treated CNT improved the tensile, flexural and impact strengths of kenaf/epoxy composite by 43.30%, 21.10%, and 130%, respectively. Silane modification had been proven to be beneficial in enhancing the dispersibility and reducing agglomeration of CNT in the epoxy matrix.

Synthesis and Characterizations of Melamine-Based Epoxy Resins

PubMed Central

Ricciotti, Laura; Roviello, Giuseppina; Tarallo, Oreste; Borbone, Fabio; Ferone, Claudio; Colangelo, Francesco; Catauro, Michelina; Cioffi, Raffaele

2013-01-01

A new, easy and cost-effective synthetic procedure for the preparation of thermosetting melamine-based epoxy resins is reported. By this innovative synthetic method, different kinds of resins can be obtained just by mixing the reagents in the presence of a catalyst without solvent and with mild curing conditions. Two types of resins were synthesized using melamine and a glycidyl derivative (resins I) or by adding a silane derivative (resin II). The resins were characterized by means of chemical-physical and thermal techniques. Experimental results show that all the prepared resins have a good thermal stability, but differ for their mechanical properties: resin I exhibits remarkable stiffness with a storage modulus value up to 830 MPa at room temperature, while lower storage moduli were found for resin II, indicating that the presence of silane groups could enhance the flexibility of these materials. The resins show a pot life higher than 30 min, which makes these resins good candidates for practical applications. The functionalization with silane terminations can be exploited in the formulation of hybrid organic-inorganic composite materials. PMID:24013372

Quantum molecular dynamics study on the structures and dc conductivity of warm dense silane

NASA Astrophysics Data System (ADS)

Sun, Huayang; Kang, Dongdong; Dai, Jiayu; Zeng, Jiaolong; Yuan, Jianmin

2014-02-01

The ionic and electronic structures of warm dense silane at the densities of 1.795, 2.260, 3.382, and 3.844 g/cm3 have been studied with temperatures from 1000 K to 3 eV using quantum molecular dynamics simulations. At all densities, the structures are melted above 1000 K. The matter states are characterized as polymeric from 1000 to 4000 K and become dense plasma states with further increasing temperature to 1 eV. At two lower densities of 1.795 and 2.260 g/cm3, silane first dissociates and then becomes the polymeric state via a chain state from the initial crystalline structure. At higher densities, however, no dissociation stage was found. These findings can help us understand how the warm dense matter forms. A rise is found for the direct current electric conductivity at T ˜1000 K, indicating the nonmetal-to-metal transition. The conductivity decreases slightly with the increase of temperature, which is due to the more disordered structures at higher temperatures.

Discovery of methyl silane and confirmation of silyl cyanide in IRC +10216.

PubMed

Cernicharo, J; Agúndez, M; Velilla Prieto, L; Guélin, M; Pardo, J R; Kahane, C; Marka, C; Kramer, C; Navarro, S; Quintana-Lacaci, G; Fonfría, J P; Marcelino, N; Tercero, B; Moreno, E; Massalkhi, S; Santander-García, M; McCarthy, M C; Gottlieb, C A; Alonso, J L

2017-10-01

We report the discovery in space of methyl silane, CH 3 SiH 3 , from observations of ten rotational transitions between 80 and 350 GHz ( J u from 4 to 16) with the IRAM 30 m radio telescope. The molecule was observed in the envelope of the C-star IRC +10216. The observed profiles and our models for the expected emission of methyl silane suggest that the it is formed in the inner zones of the circumstellar envelope, 1-40 R * , with an abundance of (0.5-1) × 10 -8 relative to H 2 . We also observed several rotational transitions of silyl cyanide (SiH 3 CN), confirming its presence in IRC +10216 in particular, and in space in general. Our models indicate that silyl cyanide is also formed in the inner regions of the envelope, around 20 R * , with an abundance relative to H 2 of 6×10 -10 . The possible formation mechanisms of both species are discussed. We also searched for related chemical species but only upper limits could be obtained.

Ordering of lamellar block copolymers on oxidized silane coatings

DOE PAGES

Mahadevapuram, Nikhila; Mitra, Indranil; Sridhar, Shyam; ...

2016-01-02

Thin films of lamellar poly(styrene-b-methyl methacrylate) (PS-PMMA) block copolymers are widely investigated for surface patterning. These materials can generate dense arrays of nanoscale lines when the lamellar domains are oriented perpendicular to the substrate. To stabilize this preferred domain orientation, we tuned the substrate surface energy using oxidation of hydrophobic silane coatings. This simple approach is effective for a broad range of PS-PMMA film thicknesses when the oxidation time is optimized, which demonstrates that the substrate coating is energetically neutral with respect to PS and PMMA segments. The lamellar films are characterized by high densities of defects that exhibit amore » strong dependence on film thickness: in-plane topological defects disrupt the lateral order in ultrathin films, while lamellar domains in thick films can bend and tilt to large misorientation angles. As a result, the types and densities of these defects are similar to those observed with other classes of neutral substrate coatings, such as random copolymer brushes, which demonstrates that oxidized silanes can be used to control PS-PMMA self assembly in thin films.« less

A Study on the Rheological and Mechanical Properties of Photo-Curable Ceramic/Polymer Composites with Different Silane Coupling Agents for SLA 3D Printing Technology.

PubMed

Song, Se Yeon; Park, Min Soo; Lee, Jung Woo; Yun, Ji Sun

2018-02-07

Silane coupling agents (SCAs) with different organofunctional groups were coated on the surfaces of Al₂O₃ ceramic particles through hydrolysis and condensation reactions, and the SCA-coated Al₂O₃ ceramic particles were dispersed in a commercial photopolymer based on interpenetrating networks (IPNs). The organofunctional groups that have high radical reactivity and are more effective in UV curing systems are usually functional groups based on acryl, such as acryloxy groups, methacrloxy groups, and acrylamide groups, and these silane coupling agents seem to improve interfacial adhesion and dispersion stability. The coating morphology and the coating thickness distribution of SCA-coated Al₂O₃ ceramic particles according to the different organofunctional groups were observed by FE-TEM. The initial dispersibility and dispersion stability of the SCA-coated Al₂O₃/High-temp composite solutions were investigated by relaxation NMR and Turbiscan. The rheological properties of the composite solutions were investigated by viscoelastic analysis and the mechanical properties of 3D-printed objects were observed with a nanoindenter.

Initial and long-term bond strengths of one-step self-etch adhesives with silane coupling agent to enamel-dentin-composite in combined situation.

PubMed

Mamanee, Teerapong; Takahashi, Masahiro; Nakajima, Masatoshi; Foxton, Richard M; Tagami, Junji

2015-01-01

This study evaluated the effect of adding silane coupling agent on initial and long-term bond strengths of one-step self-etch adhesives to enamel-dentin-composite in combined situation. Cervical cavities were prepared on extracted molars and filled with Clearfil AP-X. After water-storage for one-week, the filled teeth were sectioned in halves to expose enamel, dentin and composite surfaces and then enamel-dentin-composite surface was totally applied with one of adhesive treatments (Clearfil SE One, Clearfil SE One with Clearfil Porcelain Bond Activator, Beautibond Multi, Beautibond Multi with Beautibond Multi PR Plus and Scotchbond Universal). After designed period, micro-shear bond strengths (µSBSs) to each substrate were determined. For each period of water-storage, additive silane treatments significantly increased µSBS to composite (p<0.001). On the other hand, they significantly decreased µSBS to dentin (p<0.001), although did not have adverse effect on µSBS to enamel (p>0.05). Moreover, the stability of µSBS was depended on materials and substrates used.

Update on dental nanocomposites.

PubMed

Chen, M-H

2010-06-01

Dental resin-composites are comprised of a photo-polymerizable organic resin matrix and mixed with silane-treated reinforcing inorganic fillers. In the development of the composites, the three main components can be modified: the inorganic fillers, the organic resin matrix, and the silane coupling agents. The aim of this article is to review recent studies of the development of dental nanocomposites and their clinical applications. In nanocomposites, nanofillers are added and distributed in a dispersed form or as clusters. For increasing the mineral content of the tooth, calcium and phosphate ion-releasing composites and fluoride-releasing nanocomposites were developed by the addition of DCPA-whiskers or TTCP-whiskers or by the use of calcium fluoride or kaolinite. For enhancing mechanical properties, nanocomposites reinforced with nanofibers or nanoparticles were investigated. For reducing polymerization shrinkage, investigators modified the resin matrix by using methacrylate and epoxy functionalized nanocomposites based on silsesquioxane cores or epoxy-resin-based nanocomposites. The effects of silanization were also studied. Clinical consideration of light-curing modes and mechanical properties of nanocomposites, especially strength durability after immersion, was also addressed.

Silane surface modification for improved bioadhesion of esophageal stents

PubMed Central

Karakoy, Mert; Gultepe, Evin; Pandey, Shivendra; Khashab, Mouen A.; Gracias, David H.

2014-01-01

Stent migration occurs in 10-40% of patients who undergo placement of esophageal stents, with higher migration rates seen in those treated for benign esophageal disorders. This remains a major drawback of esophageal stent therapy. In this paper, we propose a new surface modification method to increase the adhesion between self-expandable metallic stents (SEMS) and tissue while preserving their removability. Taking advantage of the well-known affinity between epoxide and amine terminated silane coupling agents with amine and carboxyl groups that are abundant in proteins and related molecules in the human body; we modified the surfaces of silicone coated esophageal SEMS with these adhesive self-assembled monolayers (SAMs). We utilized vapor phase silanization to modify the surfaces of different substrates including PDMS strips and SEMS, and measured the force required to slide these substrates on a tissue piece. Our results suggest that surface modification of esophageal SEMS via covalent attachment of protein-binding coupling agents improves adhesion to tissue and could offer a solution to reduce SEMS migration while preserving their removability. PMID:25663731

Influence of additional coupling agent on the mechanical properties of polyester–agave cantala roxb based composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ubaidillah, E-mail: ubaidillah@uns.ac.id; Malaysia-Japan International Institute of Technology, Universiti Teknologi Malaysia, Jalan Sultan Yahya Petra, Kuala Lumpur; Raharjo, Wijang W.

The mechanical and morphological properties of the unsaturated polyester resins (UPRs)-agave cantala roxb based composite are investigated in this paper. The cantala fiber woven in 3D angle interlock was utilized as the composite reinforcement. Surface grafting of the cantala fiber through chemical treatment was performed by introducing silane coupling agent to improving the compatibility with the polymer matrix. The fabrication of the composite specimens was conducted using vacuum bagging technique. The effect of additional coupling agent to the morphological appearance of surface fracture was observed using scanning electron microscopy. Meanwhile, the influence of additional silane to the mechanical properties wasmore » examined using tensile, bending and impact test. The photograph of surface fracture on the treated specimens showed the residual matrix left on the fibers in which the phenomenon was not found in the untreated specimens. Based on mechanical tests, the treated specimens were successfully increased their mechanical properties by 55%, 9.67%, and 92.4% for tensile strength, flexural strength, and impact strength, respectively, at 1.5% silane coupling agent.« less

A Study on the Rheological and Mechanical Properties of Photo-Curable Ceramic/Polymer Composites with Different Silane Coupling Agents for SLA 3D Printing Technology

PubMed Central

Song, Se Yeon; Park, Min Soo; Lee, Jung Woo; Yun, Ji Sun

2018-01-01

Silane coupling agents (SCAs) with different organofunctional groups were coated on the surfaces of Al2O3 ceramic particles through hydrolysis and condensation reactions, and the SCA-coated Al2O3 ceramic particles were dispersed in a commercial photopolymer based on interpenetrating networks (IPNs). The organofunctional groups that have high radical reactivity and are more effective in UV curing systems are usually functional groups based on acryl, such as acryloxy groups, methacrloxy groups, and acrylamide groups, and these silane coupling agents seem to improve interfacial adhesion and dispersion stability. The coating morphology and the coating thickness distribution of SCA-coated Al2O3 ceramic particles according to the different organofunctional groups were observed by FE-TEM. The initial dispersibility and dispersion stability of the SCA-coated Al2O3/High-temp composite solutions were investigated by relaxation NMR and Turbiscan. The rheological properties of the composite solutions were investigated by viscoelastic analysis and the mechanical properties of 3D-printed objects were observed with a nanoindenter. PMID:29414912

Synthesis of liquid crystal silane-functionalized gold nanoparticles and their effects on the optical and electro-optic properties of a structurally related nematic liquid crystal.

PubMed

Mirzaei, Javad; Urbanski, Martin; Kitzerow, Heinz-S; Hegmann, Torsten

2014-05-19

Chemically and thermally robust liquid crystal silane-functionalized gold nanoparticles (i.e. AuNP1-AuNP3) were synthesized through silane conjugation. Colloidal dispersions of these particles with mesogenic ligands that are structurally identical (as in AuNP1, AuNP2) or compatible (as in AuNP3) with molecules of the nematic liquid crystal (N-LC) host showed superior colloidal stability and dispersibility. The thermal, optical, and electro-optic behaviors of the N-LC composites at different concentrations of each gold nanoparticle were investigated. All dispersions showed lower values for the rotational viscosity and elastic constant, but only AuNP3 with a dissimilar structure between the nanoparticle ligand and the host displayed the most drastic thermal effects and overall strongest impact on the electro-optic properties of the host. The observed results were explained considering both the structure and the density of the surface ligands of each gold nanoparticle. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A General One-Pot Synthesis of 2H-Indazoles Using an Organophosphorus-Silane System.

PubMed

Schoene, Jens; Bel Abed, Hassane; Schmieder, Peter; Christmann, Mathias; Nazaré, Marc

2018-04-12

A simple and direct approach for the regioselective construction of the privileged 2H-indazole scaffold is described. The developed one-pot strategy employs a phospholene mediated N-N bond formation to access 2H-indazoles. The amount of organophosphorus reagent was minimized by recycling the phospholene oxide with organosilanes as reductant. Starting from functionalized 2-nitrobenzaldehydes and primary amines a mild reductive cyclisation, using commercially available phospholene oxide and silanes, delivered a wide variety of substituted 2H-indazoles in good to excellent yields. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The silane depletion fraction as an indicator for the amorphous/crystalline silicon interface passivation quality

NASA Astrophysics Data System (ADS)

Descoeudres, A.; Barraud, L.; Bartlome, R.; Choong, G.; De Wolf, Stefaan; Zicarelli, F.; Ballif, C.

2010-11-01

In silicon heterojunction solar cells, thin amorphous silicon layers passivate the crystalline silicon wafer surfaces. By using in situ diagnostics during plasma-enhanced chemical vapor deposition (PECVD), the authors report how the passivation quality of such layers directly relate to the plasma conditions. Good interface passivation is obtained from highly depleted silane plasmas. Based upon this finding, layers deposited in a large-area very high frequency (40.68 MHz) PECVD reactor were optimized for heterojunction solar cells, yielding aperture efficiencies up to 20.3% on 4 cm2 cells.

Plasma Enabled Fabrication of Silicon Carbide Nanostructures

NASA Astrophysics Data System (ADS)

Fang, Jinghua; Levchenko, Igor; Aramesh, Morteza; Rider, Amanda E.; Prawer, Steven; Ostrikov, Kostya (Ken)

Silicon carbide is one of the promising materials for the fabrication of various one- and two-dimensional nanostructures. In this chapter, we discuss experimental and theoretical studies of the plasma-enabled fabrication of silicon carbide quantum dots, nanowires, and nanorods. The discussed fabrication methods include plasma-assisted growth with and without anodic aluminium oxide membranes and with or without silane as a source of silicon. In the silane-free experiments, quartz was used as a source of silicon to synthesize the silicon carbide nanostructures in an environmentally friendly process. The mechanism of the formation of nanowires and nanorods is also discussed.

Ultrasonic activated efficient synthesis of chromenes using amino-silane modified Fe3O4 nanoparticles: A versatile integration of high catalytic activity and facile recovery

NASA Astrophysics Data System (ADS)

Safari, Javad; Zarnegar, Zohre

2014-08-01

An efficient synthesis of 2-amino-4H-chromenes is achieved by one pot three component coupling reaction of aldehyde, malononitrile, and resorcinol using amino-silane modified Fe3O4 nanoparticles (MNPs-NH2) heterogeneous nanocatalyst under sonic condition. The attractive advantages of the present process are mild reaction conditions, short reaction times, easy isolation of products, good yields and simple operational procedures. Combination of the advantages of ultrasonic irradiation and magnetic nanoparticles provides important methodology to carry out catalytic transformations.

Process for the production of ultrahigh purity silane with recycle from separation columns

NASA Technical Reports Server (NTRS)

Coleman, Larry M. (Inventor)

1982-01-01

Tri- and dichlorosilanes formed by hydrogenation in the course of the reaction of metallurgical silicon, hydrogen and recycle silicon tetrachloride are employed as feed into a separation column arrangement of sequential separation columns and redistribution reactors which processes the feed into ultrahigh purity silane and recycle silicon tetrachloride. A slip stream is removed from the bottom of two sequential columns and added to the recycle silicon tetrachloride process stream causing impurities in the slip streams to be subjected to reactions in the hydrogenation step whereby waste materials can be formed and readily separated.

Process for the production of ultrahigh purity silane with recycle from separation columns

DOEpatents

Coleman, Larry M.

1982-07-20

Tri- and dichlorosilanes formed by hydrogenation in the course of the reaction of metallurgical silicon, hydrogen and recycle silicon tetrachloride are employed as feed into a separation column arrangement of sequential separation columns and redistribution reactors which processes the feed into ultrahigh purity silane and recycle silicon tetrachloride. A slip stream is removed from the bottom of two sequential columns and added to the recycle silicon tetrachloride process stream causing impurities in the slip streams to be subjected to reactions in the hydrogenation step whereby waste materials can be formed and readily separated.

Biofouling-resistant ceragenin-modified materials and structures for water treatment

DOEpatents

Hibbs, Michael; Altman, Susan J.; Jones, Howland D. T.; Savage, Paul B.

2013-09-10

This invention relates to methods for chemically grafting and attaching ceragenin molecules to polymer substrates; methods for synthesizing ceragenin-containing copolymers; methods for making ceragenin-modified water treatment membranes and spacers; and methods of treating contaminated water using ceragenin-modified treatment membranes and spacers. Ceragenins are synthetically produced antimicrobial peptide mimics that display broad-spectrum bactericidal activity. Alkene-functionalized ceragenins (e.g., acrylamide-functionalized ceragenins) can be attached to polyamide reverse osmosis membranes using amine-linking, amide-linking, UV-grafting, or silane-coating methods. In addition, silane-functionalized ceragenins can be directly attached to polymer surfaces that have free hydroxyls.

Refractory Oxidative-Resistant Ceramic Carbon Insulation

NASA Technical Reports Server (NTRS)

Leiser, Daniel B. (Inventor); Hsu, Ming-Ta S. (Inventor); Chen, Timothy S. (Inventor)

2001-01-01

High-temperature, lightweight, ceramic carbon insulation is prepared by coating or impregnating a porous carbon substrate with a siloxane gel derived from the reaction of an organodialkoxy silane and an organotrialkoxy silane in an acid or base medium in the presence of the carbon substrate. The siloxane gel is subsequently dried on the carbon substrate to form a ceramic carbon precursor. The carbon precursor is pyrolyzed, in an inert atmosphere, to form the ceramic insulation containing carbon, silicon, and oxygen. The carbon insulation is characterized as a porous, fibrous, carbon ceramic tile which is particularly useful as lightweight tiles for spacecraft.

Optimization of functionalization conditions for protein analysis by AFM

NASA Astrophysics Data System (ADS)

Arroyo-Hernández, María; Daza, Rafael; Pérez-Rigueiro, Jose; Elices, Manuel; Nieto-Márquez, Jorge; Guinea, Gustavo V.

2014-10-01

Activated vapor silanization (AVS) is used to functionalize silicon surfaces through deposition of amine-containing thin films. AVS combines vapor silanization and chemical vapor deposition techniques and allows the properties of the functionalized layers (thickness, amine concentration and topography) to be controlled by tuning the deposition conditions. An accurate characterization is performed to correlate the deposition conditions and functional-film properties. In particular, it is shown that smooth surfaces with a sufficient surface density of amine groups may be obtained with this technique. These surfaces are suitable for the study of proteins with atomic force microscopy.

The effect of different surface treatments on the shear bond strength of luting cements to titanium.

PubMed

Abi-Rached, Filipe de Oliveira; Fonseca, Renata Garcia; Haneda, Isabella Gagliardi; de Almeida-Júnior, Antonio Alves; Adabo, Gelson Luis

2012-12-01

Although titanium presents attractive physical and mechanical properties, there is a need for improving the bond at the titanium/luting cement interface for the longevity of metal ceramic restorations. The purpose of this study was to evaluate the effect of surface treatments on the shear bond strength (SBS) of resin-modified glass ionomer and resin cements to commercially pure titanium (CP Ti). Two hundred and forty CP Ti cast disks (9.0 × 3.0 mm) were divided into 8 surface treatment groups (n=30): 1) 50 µm Al(2)O(3) particles; 2) 120 µm Al(2)O(3) particles; 3) 250 µm Al(2)O(3) particles; 4) 50 µm Al(2)O(3) particles + silane (RelyX Ceramic Primer); 5) 120 µm Al(2)O(3) particles + silane; 6) 250 µm Al(2)O(3) particles + silane; 7) 30 µm silica-modified Al(2)O(3) particles (Cojet Sand) + silane; and 8) 120 µm Al(2)O(3) particles, followed by 110 µm silica-modified Al(2)O(3) particles (Rocatec). The luting cements 1) RelyX Luting 2; 2) RelyX ARC; or 3) RelyX U100 were applied to the treated CP Ti surfaces (n=10). Shear bond strength (SBS) was tested after thermal cycling (5000 cycles, 5°C to 55°C). Data were analyzed by 2-way analysis of variance (ANOVA) and the Tukey HSD post hoc test (α=.05). Failure mode was determined with a stereomicroscope (×20). The surface treatments, cements, and their interaction significantly affected the SBS (P<.001). RelyX Luting 2 and RelyX U100 exhibited similar behavior for all surface treatments. For both cements, only the group abraded with 50 μm Al(2)O(3) particles had lower SBS than the other groups (P<.05). For RelyX ARC, regardless of silane application, abrasion with 50 μm Al(2)O(3) particles resulted in significantly lower SBS than abrasion with 120 μm and 250 μm particles, which exhibited statistically similar SBS values to each other. Rocatec + silane promoted the highest SBS for RelyX ARC. RelyX U100 presented the highest SBS mean values (P<.001). All groups showed a predominance of adhesive failure mode. The adhesive capability of RelyX Luting 2 and RelyX U100 on the SBS was decisive, while for RelyX ARC, mechanical and chemical factors were more influential. Copyright © 2012 The Editorial Council of the Journal of Prosthetic Dentistry. Published by Mosby, Inc. All rights reserved.

Evaluation of Effect of Zirconia Surface Treatment, Using Plasma of Argon and Silane, on the Shear Bond Strength of Two Composite Resin Cements

PubMed Central

Ramdev, Poojya; Shruthi, C S

2017-01-01

Introduction Yttria stabilised tetragonal zirconia opens new vistas for all ceramic restoration by the mechanism of transformation toughening, making it much stronger compared to all other ceramic materials. Currently, it is the most recent core material for all ceramic fixed partial dentures due to its ability to withstand high simulated masticatory loads. Problems which have been reported with zirconia restorations involve the core cement interface leading to loss of retention of the prosthesis. Different reasons which have been reported for the same include the lack of adhesion between zirconia and commonly used cements due to absence of silica phase which makes zirconia not etchable. In addition, the hydrophobic nature of zirconia causes low wettability of zirconia surface by the adhesive cements which are commonly used. Aim The purpose of this in vitro study was to compare and evaluate the effect of two pre-treatments of zirconia, using plasma of argon and silane, on the shear bond strength values of two composite resin cements to zirconia and to evaluate the failure pattern of the debonded areas using stereomicroscopic analysis. Materials and Methods Sixty zirconia discs (10 mm×2 mm) were randomly divided into three groups (n=20), following surface treatment, with airborne particle abrasion, using 110 µm Al2O3: Group I (control), Group II (plasma of argon cleaning), and Group III (application of silane primer). Each group had two subgroups based on the type of resin cement used for bonding: subgroup A; Rely X Ultimate (3M ESPE) and subgroup B; Panavia F (Kuraray). In subgroup A, Rely X universal silane primer and in subgroup B Clearfil ceramic primer was used. Shear bond strengths were determined after water storage for one day and thermocycling for 5000 cycles. Data (megapascal) were analyzed using ANOVA and Bonferroni test. Specimens were subjected to stereomicroscopic analysis, for evaluation of failure pattern. Results Group III produced the highest shear bond strength followed by Group II and Group I. Subgroup A showed higher shear bond strength than Subgroup B. Stereomicroscopic analysis showed cohesive failure in Group III, while in Group I adhesive failure was seen. Conclusion Silane primer application caused maximum increase in shear bond strength due to increased wettability. Argon plasma treatment was less effective in comparison to silane treatment. Air abrasion when used alone resulted in lower bond strength values, thereby making it necessary to use a combination of surface treatments. Rely X Ultimate cement was superior to Panavia F in terms of adhesive bonding to zirconia. PMID:28969271

Polymer precursors for ceramic matrix composites

NASA Technical Reports Server (NTRS)

Litt, M. H.; Kumar, K.

1986-01-01

The synthesis and characterization of a polycyclohexasilane is reported. Because of its cyclic structure, it is anticipated that this polymer might serve as a precursor to SIC having a high char yield with little rearrangement to form small, volatile cyclic silanes, and, as such, would be of interest as a precursor to SiC composite matrices and fibers, or as a binder in ceramic processing. Several approaches to the synthesis of a bifunctional cyclic monomer were attempted; the most successful of these was metal coupling of PhMeSiCl2 and Me2SiCl2. The procedure gives six-membered ring compounds with all degrees of phenyl substitution, from none to hexaphenyl. The compounds with from 0-2 groups were isolated and characterized. The fraction with degree of phenyl substitution equal to 2, a mixture of cis and trans 1,2-; 1,3-; and 1,4 isomers, was isolated in 32 percent yield. Pure 1,4 diphenyldecamethylcyclohexasilane was isolated from the mixed diphenyl compounds and characterized. Diphenyldecamethylcyclohexasilanes were dephenylated to dichlorodecamethylcyclohexasilanes by treating with H2SO4.NH4Cl in benzene. The latter were purified and polymerized by reacting with sodium in toluene. The polymers were characterized by HPGPC, elemental analysis, proton NMR, and IR. Thermogravimetric analyses were carried out on the polymers. As the yield of residual SiC was low, polymers were heat treated to increase the residual char yield. As high as 51.52 percent residual char yield was obtained in one case.

Comparative evaluation of antimicrobials for textile applications.

PubMed

Windler, Lena; Height, Murray; Nowack, Bernd

2013-03-01

Many antimicrobial technologies are available for textiles. They may be used in many different textile applications to prevent the growth of microorganisms. Due to the biological activity of the antimicrobial compounds, the assessment of the safety of these substances is an ongoing subject of research and regulatory scrutiny. This review aims to give an overview on the main compounds used today for antimicrobial textile functionalization. Based on an evaluation of scientific publications, market data as well as regulatory documents, the potential effects of antimicrobials on the environment and on human health were considered and also life cycle perspectives were taken into account. The characteristics of each compound were summarized according to technical, environmental and human health criteria. Triclosan, silane quaternary ammonium compounds, zinc pyrithione and silver-based compounds are the main antimicrobials used in textiles. The synthetic organic compounds dominate the antimicrobials market on a weight basis. On the technical side the application rates of the antimicrobials used to functionalize a textile product are an important parameter with treatments requiring lower dosage rates offering clear benefits in terms of less active substance required to achieve the functionality. The durability of the antimicrobial treatment has a strong influence on the potential for release and subsequent environmental effects. In terms of environmental criteria, all compounds were rated similarly in effective removal in wastewater treatment processes. The extent of published information about environmental behavior for each compound varies, limiting the possibility for an in-depth comparison of all textile-relevant parameters across the antimicrobials. Nevertheless the comparative evaluation showed that each antimicrobial technology has specific risks and benefits that should be taken into account in evaluating the suitability of different antimicrobial products. The results also indicated that nanoscale silver and silver salts that achieve functionality with very low application rates offer clear potential benefits for textile use. The regular care of textiles consumes lots of resources (e.g. water, energy, chemicals) and antimicrobial treatments can play a role in reducing the frequency and/or intensity of laundering which can give potential for significant resource savings and associated impact on the environment. Copyright © 2013 Elsevier Ltd. All rights reserved.

Palladium pincer complex catalyzed stannyl and silyl transfer to propargylic substrates: synthetic scope and mechanism.

PubMed

Kjellgren, Johan; Sundén, Henrik; Szabó, Kálmán J

2005-02-16

Pincer complex catalyzed substitution of various propargylic substrates could be achieved using tin- and silicon-based dimetallic reagents to obtain propargyl- and allenylstannanes and silanes. These reactions involving chloride, mesylate, and epoxide substrates could be carried out under mild conditions, and therefore many functionalities (such as COOEt, OR, OH, NR, and NAc) are tolerated. It was shown that pincer catalysts with electron-supplying ligands, such as NCN, SCS, and SeCSe complexes, display the highest catalytic activity. The catalytic substitution of secondary propargyl chlorides and primary propargyl chlorides with electron-withdrawing substituents proceeds with high regioselectivity providing the allenyl product. Opening of the propargyl epoxides takes place with an excellent stereo- and regioselectivity to give stereodefined allenylstannanes. Silylstannanes as dimetallic reagents undergo an exclusive silyl transfer to the propargylic substrate affording allenylsilanes with high regioselectivity. According to our mechanistic studies, the key intermediate of the reaction is an organostannane (or silane)-coordinated pincer complex, which is formed from the dimetallic reagent and the corresponding pincer complex catalyst. DFT modeling studies have shown that the trimethylstannyl functionality is transferred to the propargylic substrate in a single reaction step with high allenyl selectivity. Inspection of the TS structures reveals that the trimethylstannyl group transfer is initiated by the attack of the palladium-tin sigma-bond electrons on the propargylic substrate. This is a novel mechanism in palladium chemistry, which is based on the unique topology of the pincer complex catalysts.

Effect of surface treatments on the bond strength of CAD/CAM fiberglass posts.

PubMed

Garcia, Paula-Pontes; da Costa, Rogério-Goulart; Garcia, André-Vivan; Gonzaga, Carla-Castiglia; da Cunha, Leonardo-Fernandes; Rezende, Carlos-Eduardo-Edwards; Correr, Gisele-Maria

2018-06-01

There is no ideal protocol for the surface treatment of fiber posts, especially when using a computer-aided design/computer-aided manufacturing (CAD/CAM) experimental fiberglass block. The purpose of this study was to evaluate the bond strength of a CAD/CAM customized glass fiber post and core after applying different surface treatment techniques. Forty premolars were prepared to receive a customized CAD/CAM glass-fiber post and core obtained from an experimental block of glass fiber and epoxy resin. The specimens were randomly distributed in 4 groups (n=10) according to the post and core surface treatment: ETH - 70% ethanol; HP - 24% hydrogen peroxide for 1 minute; ETH/S - 70% ethanol + silane; HP/S - 24% hydrogen peroxide + silane. The universal adhesive containing silane was applied on the posts and prepared post spaces in all groups. The posts were cemented using dual cure resin cement. The specimens were stored in distilled water at 37°C for 24 h, cut (two slices of 1 mm for each root third - coronal, middle, and apical) and subjected to push-out test (0.5 mm/min). Data was subjected to two-way ANOVA (surface treatment and root third) and Tukey's test (α=0,05). There was no significant difference of bond strength values among groups, regardless the surface treatment ( p >0.05). There was significant difference on bond strength values for the different root thirds ( p <0.05) (coronal>middle=apical). The different surface treatment and application of additional silane in the CAD/CAM customized glass-fiber post and core does not interfere on bond strength values. The root dentin third interfered on the bond strength, with higher values for the coronal third. Key words: Post and core technique, cad/cam, shear strength, hydrogen peroxide.

Shear Bond Strength of Al2O3 Sandblasted Y-TZP Ceramic to the Orthodontic Metal Bracket

PubMed Central

Byeon, Seon Mi; Lee, Min Ho; Bae, Tae Sung

2017-01-01

As the proportion of adult orthodontic treatment increases, mainly for aesthetic reasons, orthodontic brackets are directly attached to yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) restorations. This, study analyzed the shear bond strength (SBS) between various surface treated Y-TZP and orthodontic metal brackets. The Y-TZP specimens were conditioned by 110 μm Al2O3 sandblasting, or sandblasting followed by coating with one of the primers (silane, MDP, or an MDP-containing silane primer). After surface treatment, the orthodontic metal bracket was bonded to the specimen using a resin cement, and then 24 h storage in water and thermal cycling (5000 cycles, 5–55 °C), SBS was measured. Surface roughness was analyzed for surface morphology, and X-ray photoelectron spectroscopy (XPS) was employed for characterization of the chemical bond between the Y-TZP and the MDP-based primers (MDP, MDP containing silane primer). It was found that after surface treatment, the surface roughness of all groups increased. The groups treated with 110 μm Al2O3 sandblasting and MDP, or MDP-containing silane primer showed the highest SBS values, at 11.92 ± 1.51 MPa and 13.36 ± 2.31 MPa, respectively. The SBS values significantly decreased in all the groups after thermal cycling. Results from XPS analysis demonstrated the presence of chemical bonds between Y-TZP and MDP. Thus, the application of MDP-based primers after Al2O3 sandblasting enhances the resin bond strength between Y-TZP and the orthodontic metal bracket. However, bonding durability of all the surface-treated groups decreased after thermal cycling. PMID:28772508

Experimental Design on Laminated Veneer Lumber Fiber Composite: Surface Enhancement

NASA Astrophysics Data System (ADS)

Meekum, U.; Mingmongkol, Y.

2010-06-01

Thick laminate veneer lumber(LVL) fibre reinforced composites were constructed from the alternated perpendicularly arrayed of peeled rubber woods. Glass woven was laid in between the layers. Native golden teak veneers were used as faces. In house formulae epoxy was employed as wood adhesive. The hand lay-up laminate was cured at 150° C for 45 mins. The cut specimen was post cured at 80° C for at least 5 hours. The 2k factorial design of experimental(DOE) was used to verify the parameters. Three parameters by mean of silane content in epoxy formulation(A), smoke treatment of rubber wood surface(B) and anti-termite application(C) on the wood surface were analysed. Both low and high levels were further subcategorised into 2 sub-levels. Flexural properties were the main respond obtained. ANOVA analysis of the Pareto chart was engaged. The main effect plot was also testified. The results showed that the interaction between silane quantity and termite treatment is negative effect at high level(AC+). Vice versa, the interaction between silane and smoke treatment was positive significant effect at high level(AB+). According to this research work, the optimal setting to improve the surface adhesion and hence flexural properties enhancement were high level of silane quantity, 15% by weight, high level of smoked wood layers, 8 out of 14 layers, and low anti termite applied wood. The further testes also revealed that the LVL composite had superior properties that the solid woods but slightly inferior in flexibility. The screw withdrawn strength of LVL showed the higher figure than solid wood. It is also better resistance to moisture and termite attack than the rubber wood.

To evaluate and compare the effect of different Post Surface treatments on the Tensile Bond Strength between Fiber Posts and Composite Resin.

PubMed

Shori, Deepa; Pandey, Swapnil; Kubde, Rajesh; Rathod, Yogesh; Atara, Rahul; Rathi, Shravan

2013-10-01

Fiber posts are widely used for restoration of mutilated teeth that lack adequate coronal tooth structure to retain a core for definitive restoration, bond between the fiber post and composite material depends upon the chemical reaction between the post surface and the resin material used for building up the core. In attempt to maximize the resin bonding with fiber post, different post surface conditioning is advocated. Therefore the purpose of the study is to examine the interfacial strength between fiber post and composite, as core build-up material after different surface treatments of fiber posts. Twenty fiber posts were split into four groups off five each according to different surface treatments viz. Group I-(Negative Control), Group II-Silanization (Positive control), Group III-(37% Phosphoric Acid & Silanization) ,Group IV- (10% Hydrogen Peroxide and Silanization). With the preformed plastic mould, a core of dual cure composite resin around the fiber post having the uniform thickness was created. Tensile bond strength of each specimen was measured under Universal Testing Machine (UTM) at the cross head speed of 3mm/min. The results achieved with 10% Hydrogen peroxide had a marked effect on micro tensile bond strength values between the tested materials. Immense enhancement in the silanization efficiency of quartz fiber phase was observed with different surface chemical treatment of the resin phase of fiber posts with the marked increase in the micro-tensile bond strength between fiber post and composite core. Shori D, Pandey S, Kubde R, Rathod Y, Atara R, Rathi S. To evaluate and compare the effect of different Post Surface treatments on the Tensile Bond Strength between Fiber Posts and Composite Resin. J Int Oral Health 2013; 5(5):27-32.

Synthesis of wrinkled mesoporous silica and its reinforcing effect for dental resin composites.

PubMed

Wang, Ruili; Habib, Eric; Zhu, X X

2017-10-01

The aim of this work is to explore the reinforcing effect of wrinkled mesoporous silica (WMS), which should allow micromechanical resin matrix/filler interlocking in dental resin composites, and to investigate the effect of silica morphology, loading, and compositions on their mechanical properties. WMS (average diameter of 496nm) was prepared through the self-assembly method and characterized by the use of the electron microscopy, dynamic light scattering, and the N 2 adsorption-desorption measurements. The mechanical properties of resin composites containing silanized WMS and nonporous smaller silica were evaluated with a universal mechanical testing machine. Field-emission scanning electron microscopy was used to study the fracture morphology of dental composites. Resin composites including silanized silica particles (average diameter of 507nm) served as the control group. Higher filler loading of silanized WMS substantially improved the mechanical properties of the neat resin matrix, over the composites loaded with regular silanized silica particles similar in size. The impregnation of smaller secondary silica particles with diameters of 90 and 190nm, denoted respectively as Si90 and Si190, increased the filler loading of the bimodal WMS filler (WMS-Si90 or WMS-Si190) to 60wt%, and the corresponding composites exhibited better mechanical properties than the control fillers made with regular silica particles. Among all composites, the optimal WMS-Si190- filled composite (mass ratio WMS:Si190=10:90, total filler loading 60wt%) exhibited the best mechanical performance including flexural strength, flexural modulus, compressive strength and Vickers microhardness. The incorporation of WMS and its mixed bimodal fillers with smaller silica particles led to the design and formulation of dental resin composites with superior mechanical properties. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Use of silane-functionalized graphene oxide in organic photovoltaic cells and organic light-emitting diodes.

PubMed

Lee, Chang Yeong; Le, Quyet Van; Kim, Cheolmin; Kim, Soo Young

2015-04-14

Graphene oxide (GO) and silane-functionalized GO (sGO) sheets obtained through a simple sonication exfoliation method are employed as hole transport layers to improve the efficiency of organic photovoltaic (OPV) cells and organic light-emitting diodes (OLED). GO was functionalized using (3-glycidyl oxypropyl)trimethoxysilane (GPTMS) and triethoxymethylsilane (MTES). The appearance of new peaks in the Fourier-transform infrared spectra of the sGOs indicates the formation of Si-O-C, Si-O-Si, Si-H, and Si-O-C moieties, which provide evidence of the addition of silane to the GO surface. Furthermore, the appearance of Si-O-Si bonds in the synchrotron radiation photoelectron spectra (SRPES) of the MTES-sGO and GPTMS-sGO samples suggests that silane groups were effectively functionalized onto the GO sheets. An OPV cell with GO layers showed a lower performance with a power conversion efficiency (PCE) of 2.06%; in contrast, OPV cells based on GPTMS-sGO and MTES-sGO have PCE values of 3.00 and 3.08%, respectively. The OLED devices based on GPTMS-sGO and MTES-sGO showed a higher maximum luminance efficiency of 13.91 and 12.77 cd A(-1), respectively, than PEDOT:PSS-based devices (12.34 cd A(-1)). The SRPES results revealed that the work functions of GO, GPTMS-sGO, and MTES-sGO were 4.8, 4.9, and 5.0 eV, respectively. Therefore, the increase in the PCE value is attributed to improved band-gap alignment. It is thought that sGO could be used as an interfacial layer in OPV and OLED devices.

Virtual Screening as a Strategy for the Identification of Xenobiotics Disrupting Corticosteroid Action

PubMed Central

Praxmarer, Lukas; Chantong, Boonrat; Cereghetti, Diego; Winiger, Rahel; Schuster, Daniela; Odermatt, Alex

2012-01-01

Background Impaired corticosteroid action caused by genetic and environmental influence, including exposure to hazardous xenobiotics, contributes to the development and progression of metabolic diseases, cardiovascular complications and immune disorders. Novel strategies are thus needed for identifying xenobiotics that interfere with corticosteroid homeostasis. 11β-hydroxysteroid dehydrogenase 2 (11β-HSD2) and mineralocorticoid receptors (MR) are major regulators of corticosteroid action. 11β-HSD2 converts the active glucocorticoid cortisol to the inactive cortisone and protects MR from activation by glucocorticoids. 11β-HSD2 has also an essential role in the placenta to protect the fetus from high maternal cortisol concentrations. Methods and Principal Findings We employed a previously constructed 3D-structural library of chemicals with proven and suspected endocrine disrupting effects for virtual screening using a chemical feature-based 11β-HSD pharmacophore. We tested several in silico predicted chemicals in a 11β-HSD2 bioassay. The identified antibiotic lasalocid and the silane-coupling agent AB110873 were found to concentration-dependently inhibit 11β-HSD2. Moreover, the silane AB110873 was shown to activate MR and stimulate mitochondrial ROS generation and the production of the proinflammatory cytokine interleukin-6 (IL-6). Finally, we constructed a MR pharmacophore, which successfully identified the silane AB110873. Conclusions Screening of virtual chemical structure libraries can facilitate the identification of xenobiotics inhibiting 11β-HSD2 and/or activating MR. Lasalocid and AB110873 belong to new classes of 11β-HSD2 inhibitors. The silane AB110873 represents to the best of our knowledge the first industrial chemical shown to activate MR. Furthermore, the MR pharmacophore can now be used for future screening purposes. PMID:23056542

Silica Coating of Nonsilicate Nanoparticles for Resin-Based Composite Materials

PubMed Central

Kaizer, M.R.; Almeida, J.R.; Gonçalves, A.P.R.; Zhang, Y.; Cava, S.S.; Moraes, R.R.

2016-01-01

This study was designed to develop and characterize a silica-coating method for crystalline nonsilicate ceramic nanoparticles (Al2O3, TiO2, and ZrO2). The hypothesis was that the coated nonsilicate nanoparticles would stably reinforce a polymeric matrix due to effective silanation. Silica coating was applied via a sol-gel method, with tetraethyl orthosilicate as a silica precursor, followed by heat treatment. The chemical and microstructural characteristics of the nanopowders were evaluated before and after silica coating through x-ray diffraction, BET (Brunauer-Emmett-Teller), energy-dispersive x-ray spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy analyses. Coated and noncoated nanoparticles were silanated before preparation of hybrid composites, which contained glass microparticles in addition to the nanoparticles. The composites were mechanically tested in 4-point bending mode after aging (10,000 thermal cycles). Results of all chemical and microstructural analyses confirmed the successful obtaining of silica-coated nanoparticles. Two distinct aspects were observed depending on the type of nanoparticle tested: 1) formation of a silica shell on the surface of the particles and 2) nanoparticle clusters embedded into a silica matrix. The aged hybrid composites formulated with the coated nanoparticles showed improved flexural strength (10% to 30% higher) and work of fracture (35% to 40% higher) as compared with composites formulated with noncoated nanoparticles. The tested hypothesis was confirmed: silanated silica-coated nonsilicate nanoparticles yielded stable reinforcement of dimethacrylate polymeric matrix due to effective silanation. The silica-coating method presented here is a versatile and promising novel strategy for the use of crystalline nonsilicate ceramics as a reinforcing phase of polymeric composite biomaterials. PMID:27470069

Area Reports. Advanced materials and devices research area. Silicon materials research task, and advanced silicon sheet task

NASA Technical Reports Server (NTRS)

1986-01-01

The objectives of the Silicon Materials Task and the Advanced Silicon Sheet Task are to identify the critical technical barriers to low-cost silicon purification and sheet growth that must be overcome to produce a PV cell substrate material at a price consistent with Flat-plate Solar Array (FSA) Project objectives and to overcome these barriers by performing and supporting appropriate R&D. Progress reports are given on silicon refinement using silane, a chemical vapor transport process for purifying metallurgical grade silicon, silicon particle growth research, and modeling of silane pyrolysis in fluidized-bed reactors.

Methods for attaching polymerizable ceragenins to water treatment membranes using amine and amide linkages

DOEpatents

Hibbs, Michael; Altman, Susan J.; Jones, Howland D.T.; Savage, Paul B.

2013-10-15

This invention relates to methods for chemically grafting and attaching ceragenin molecules to polymer substrates; methods for synthesizing ceragenin-containing copolymers; methods for making ceragenin-modified water treatment membranes and spacers; and methods of treating contaminated water using ceragenin-modified treatment membranes and spacers. Ceragenins are synthetically produced antimicrobial peptide mimics that display broad-spectrum bactericidal activity. Alkene-functionalized ceragenins (e.g., acrylamide-functionalized ceragenins) can be attached to polyamide reverse osmosis membranes using amine-linking, amide-linking, UV-grafting, or silane-coating methods. In addition, silane-functionalized ceragenins can be directly attached to polymer surfaces that have free hydroxyls.

Reversible Silylene Insertion Reactions into Si-H and P-H σ-Bonds at Room Temperature.

PubMed

Rodriguez, Ricardo; Contie, Yohan; Nougué, Raphael; Baceiredo, Antoine; Saffon-Merceron, Nathalie; Sotiropoulos, Jean-Marc; Kato, Tsuyoshi

2016-11-07

Phosphine-stabilized silylenes react with silanes and a phosphine by silylene insertion into E-H σ-bonds (E=Si,P) at room temperature to give the corresponding silanes. Of special interest, the process occurs reversibly at room temperature. These results demonstrate that both the oxidative addition (typical reaction for transient silylenes) and the reductive elimination processes can proceed at the silicon center under mild reaction conditions. DFT calculations provide insight into the importance of the coordination of the silicon center to achieve the reductive elimination step. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

A sonochemical approach to the direct surface functionalization of superparamagnetic iron oxide nanoparticles with (3-aminopropyl)triethoxysilane.

PubMed

Sodipo, Bashiru Kayode; Aziz, Azlan Abdul

2014-01-01

We report a sonochemical method of functionalizing superparamagnetic iron oxide nanoparticles (SPION) with (3-aminopropyl)triethoxysilane (APTES). Mechanical stirring, localized hot spots and other unique conditions generated by an acoustic cavitation (sonochemical) process were found to induce a rapid silanization reaction between SPION and APTES. FTIR, XPS and XRD measurements were used to demonstrate the grafting of APTES on SPION. Compared to what was reported in literature, the results showed that the silanization reaction time was greatly minimized. More importantly, the product displayed superparamagnetic behaviour at room temperature with a more than 20% higher saturation magnetization.

Low-pressure chemical vapor deposition of low in situ phosphorus doped silicon thin films

NASA Astrophysics Data System (ADS)

Sarret, M.; Liba, A.; Bonnaud, O.

1991-09-01

In situ low phosphorus doped silicon films are deposited onto glass substrates by low-pressure chemical vapor deposition method. The deposition parameters, temperature, total pressure, and pure silane gas flow are, respectively, fixed at 550 °C, 0.08 Torr, and 50 sccm. The varying deposition parameter is phosphine/silane mole ratio; when this ratio varies from 2×10-6 to 4×10-4, the phosphorus concentration and the resistivity after annealing, respectively, vary from 2×1018 to 3×1020 atoms cm-3 and from 1.5 Ω cm to 2.5×10-3 Ω cm.

Decomposition of silane on tungsten or other materials

DOEpatents

Wiesmann, H.J.

This invention relates to hydrogenated amorphous silicon produced by thermally decomposing silane (SiH/sub 4/) or other gases comprising H and Si, from a W or foil heated to a temperature of about 1400 to 1600/sup 0/C, in a vacuum of about 10-/sup 6/ to 10-/sup 4/ torr. A gaseous mixture is formed of atomic hydrogen and atomic silicon. The gaseous mixture is deposited onto a substrate independent of and outside the source of thermal decomposition. Hydrogenated amorphous silicon is formed. The presence of an ammonia atmosphere in the vacuum chamber enhances the photoconductivity of the hydrogenated amorphous silicon film.

Oxygen-Permeable, Hydrophobic Membranes of Silanized alpha-Al2O3

NASA Technical Reports Server (NTRS)

Atwater, James E.; Akse, James R.

2006-01-01

Membranes made of silanized alumina have been prepared and tested as prototypes of derivatized ceramic membranes that are both highly permeable to oxygen and hydrophobic. Improved oxygen-permeable, hydrophobic membranes would be attractive for use in several technological disciplines, including supporting high-temperature aqueousphase oxidation in industrial production of chemicals, oxygenation of aqueous streams for bioreactors, and oxygenation of blood during open-heart surgery and in cases of extreme pulmonary dysfunction. In comparison with organic polymeric oxygen-permeable membranes now commercially available, the derivatized ceramic membranes are more chemically robust, are capable of withstanding higher temperatures, and exhibit higher oxygen-diffusion coefficients.

Enhanced wear performance of ultra high molecular weight polyethylene crosslinked by organosilane.

PubMed

Tang, C Y; Xie, X L; Wu, X C; Li, R K Y; Mai, Y W

2002-11-01

Ultra high molecular weight polyethylene (UHMWPE) crosslinked by organosilane was thermal compression molded. The organosilane used was the tri-ethyloxyl vinyl silane. Its gelation, melting behavior, crystallinity, mechanical and wear-resisting properties were systematically investigated. The results showed that the gel ratio of UHMWPE increases with the incorporation of organosilane. At a low content of organosilane, the melting point and crystallinity of the crosslinked UHMWPE increase, and hence the mechanical and wear-resisting properties are improved. However, at a high content of organosilane, these performances of the crosslinked UHMWPE become worse. At 0.4 phr silane, the wear resistance of crosslinked UHMWPE reaches its optimum value.

Glycol-modified silanes: novel possibilities for the synthesis of hierarchically organized (hybrid) porous materials.

PubMed

Hartmann, Sarah; Brandhuber, Doris; Hüsing, Nicola

2007-09-01

The preparation of porous hierarchical architectures that have structural features spanning from the nanometer to micrometer and even larger dimensions and that exhibit certain functionalities is one of the new challenging frontiers in materials chemistry. The sol-gel process is one of the most promising synthesis routes toward such materials because it not only offers the possibility to incorporate organic functions into the porous host but also offers the possibility to deliberately tailor the pore structure. In this Account, the opportunities given by the application of novel diol-modified silanes are discussed for the synthesis of hierarchically organized inorganic and also inorganic-organic porous monoliths.

Preparation of durable hydrophobic cellulose fabric from water glass and mixed organosilanes

NASA Astrophysics Data System (ADS)

Shang, Song-Min; Li, Zhengxiong; Xing, Yanjun; Xin, John H.; Tao, Xiao-Ming

2010-12-01

Durable superhydrophobic cellulose fabric was prepared from water glass and n-octadecyltriethoxysilane (ODTES) with 3-glycidyloxypropyltrimethoxysilane (GPTMS) as crosslinker by sol-gel method. The result showed that the addition of GPTMS could result in a better fixation of silica coating from water glass on cellulose fabric. The silanization of hydrolyzed ODTES at different temperatures and times was studied and optimized. The results showed that silanization time was more important than temperature in forming durable hydrophobic surface. The durability of superhydrophobicity treatment was analyzed by XPS. As a result, the superhydrophobic cotton treated under the optimal condition still remained hydrophobic properties after 50 washing cycles.

Surface modification of cellulose using silane coupling agent.

PubMed

Thakur, Manju Kumari; Gupta, Raju Kumar; Thakur, Vijay Kumar

2014-10-13

Recently there has been a growing interest in substituting traditional synthetic polymers with natural polymers for different applications. However, natural polymers such as cellulose suffer from few drawbacks. To become viable potential alternatives of synthetic polymers, cellulosic polymers must have comparable physico-chemical properties to that of synthetic polymers. So in the present work, cellulose polymer has been modified by a series of mercerization and silane functionalization to optimize the reaction conditions. Structural, thermal and morphological characterization of the cellulose has been done using FTIR, TGA and SEM, techniques. Surface modified cellulose polymers were further subjected to evaluation of their properties like swelling and chemical resistance behavior. Published by Elsevier Ltd.

Forced-flow bioreactor for sucrose inversion using ceramic membrane activated by silanization.

PubMed

Nakajima, M; Watanabe, A; Jimbo, N; Nishizawa, K; Nakao, S

1989-02-20

A forced-flow enzyme membrane reactor system for sucrose inversion was investigated using three ceramic membranes having different pore sizes. Invertase was immobilized chemically to the inner surface of a ceramic membrane activated by a silane-glutaraldehyde technique. With the cross-flow filtration of sucrose solution, the reaction rate was a function of the permeate flux, easily controlled by pressure. Using 0.5 microm support pore size of membrane, the volumetric productivity obtained was 10 times higher than that in a reported immobilized enzyme column reactor, with a short residence time of 5 s and 100% conversion of the sucrose inversion.

Effect of glass fiber surface treatments on mechanical strength of epoxy based composite materials.

PubMed

Iglesias, J G; González-Benito, J; Aznar, A J; Bravo, J; Baselga, J

2002-06-01

Sizing glass fibers with silane coupling agents enhances the adhesion and the durability of the fiber/polymer matrix interface in composite materials. There are several tests to determine the interfacial strength between a fiber and resin, but all of them present difficulties in interpreting the results and/or sample preparation. In this study, we observed the influence of different aminosilanes fiber coatings on the resistance of epoxy-based composite materials using a very easy fractographic test. In addition, we tried a new fluorescence method to get information on a molecular level precisely at the interface. Strength was taken into account from two standpoints: (i) mechanical strength and (ii) the resistance to hydrolysis of the interface in oriented glass-reinforced epoxy-based composites. Three silanes: gamma-aminopropyltriethoxysilane, gamma-Aminopropylmethyldiethoxysilane, and gamma-Aminopropyldimethylethoxysilane were used to obtain different molecular structures at the interface. It was concluded that: (i) the more accessible amine groups are, the higher the interface rigidity is; (ii) an interpenetrating network mechanism seems to be the most important for adhesion and therefore to the interfacial strength; and (iii) the higher the degree of crosslinking in the silane coupling layer is, the higher the hydrolytic damage rate is.

Crystallization and textural porosity of synthetic clay minerals.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carrado, K. A.; Csencsits, R.; Thiyagarajan, P.

2002-12-01

The crystallization of synthetic layered magnesium silicate hectorite clays from both silica sol and organosilane sources is compared. For the silica sol-derived clays, a templating method is employed wherein organic or polymeric molecules are included during clay crystallization that are then removed from the composites via calcination. The mechanism of silane-derived hectorite formation is followed by XRD, TGA, 29Si MAS NMR, and small angle X-ray scattering (SAXS), and results are compared to those obtained for the sol-derived hectorite. The mechanism appears to be similar but the rate is approximately doubled when the silane is used rather than silica sol. Analyticalmore » transmission electron microscopy (TEM) is exploited to glean structural morphology information towards resolving the nature of the resulting pore network structures. Results are compared with nitrogen adsorption-desorption isotherm behavior; dominant hysteresis loops are present in the type IV isotherms. Pore size distributions based on both the adsorption and desorption isotherms are compared. Small angle neutron scattering (SANS) experiments reveal that the average particle size increases as synthetic laponite < sol-derived hectorite < silane-derived hectorite < natural hectorite. Contrast matching SANS studies in aqueous and organic solvents are carried out to extract information about pore accessibility.« less

The influence of polymer architectures on the dewetting behavior of thin polymer films: from linear chains to ring chains.

PubMed

Wang, Lina; Xu, Lin; Liu, Binyuan; Shi, Tongfei; Jiang, Shichun; An, Lijia

2017-05-03

The dewetting behavior of ring polystyrene (RPS) film and linear polystyrene (LPS) film on silanized Si substrates with different grafting densities and PDMS substrate was investigated. Results showed that polymer architectures greatly influenced the dewetting behavior of the thin polymer film. On the silanized Si substrate with 69% grafting density, RPS chains exhibited stronger adsorption compared with LPS chains, and as a result the wetting layer formed more easily. For LPS films, with a decreased annealing temperature, the stability of the polymer film changed from non-slip dewetting via apparent slip dewetting to apparently stable. However, for RPS films, the polymer film stability switched from apparent slip dewetting to apparently stable. On the silanized Si substrate with 94% grafting density, the chain adsorption became weaker and the dewetting processes were faster than that on the substrate with 69% grafting density at the same experimental temperature for both the LPS and RPS films. Moreover, on the PDMS substrate, LPS films always showed non-slip dewetting, while the dewetting kinetics of RPS films switched from non-slip dewetting to slip dewetting behaviour. Forming the wetting layer strongly influenced the stability and dewetting behavior of the thin polymer films.

Hybrid joining of polyamide and hydrogenated acrylonitrile butadiene rubber through heat-resistant functional layer of silane coupling agent

NASA Astrophysics Data System (ADS)

Sang, Jing; Sato, Riku; Aisawa, Sumio; Hirahara, Hidetoshi; Mori, Kunio

2017-08-01

A simple, direct adhesion method was developed to join polyamide (PA6) to hydrogenated acrylonitrile butadiene rubber (HNBR) by grafting a functional layer of a silane coupling agent on plasma functionalized PA6 surfaces. The functional layer of the silane coupling agent was prepared using a self-assembly method, which greatly improved the heat resistance of PA6 from 153 °C up to 325 °C and the resulting PA6/HNBR joints showed excellent adhesion properties with cohesive failure between PA6 and HNBR. X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and nanoscale infrared microscopy and chemical imaging (Nano-IR, AFM-IR) were employed to characterize the surfaces and interfaces. The Nano-IR analysis method was employed for the first time to analyze the chemical structures of the adhesion interfaces between different materials and to establish the interface formation mechanism. This study is of significant value for interface research and the study of adhesion between resins and rubbers. There is a promising future for heat-resistant functional layers on resin surfaces, with potential application in fuel hose composite materials for the automotive and aeronautical industries.

Altered Calcium Dynamics in Cardiac Cells Grown on Silane-Modified Surfaces

PubMed Central

Ravenscroft-Chang, Melissa S.; Stohlman, Jayna; Molnar, Peter; Natarajan, Anupama; Canavan, Heather E.; Teliska, Maggie; Stancescu, Maria; Krauthamer, Victor; Hickman, J.J.

2013-01-01

Chemically defined surfaces were created using self-assembled monolayers (SAMs) of hydrophobic and hydrophilic silanes as models for implant coatings, and the morphology and physiology of cardiac myocytes plated on these surfaces were studied in vitro. We focused on changes in intracellular Ca2+ because of its essential role in regulating heart cell function. The SAM-modified coverslips were analyzed using X-ray Photoelectron Spectroscopy to verify composition. The morphology and physiology of the cardiac cells were examined using fluorescence microscopy and intracellular Ca2+ imaging. The imaging experiments used the fluorescent ratiometric dye fura-2, AM to establish both the resting Ca2+ concentration and the dynamic responses to electrical stimulation. A significant difference in excitation-induced Ca2+ changes on the different silanated surfaces was observed. However, no significant change was noted based on the morphological analysis. This result implies a difference in internal Ca2+ dynamics, and thus cardiac function, occurs when the composition of the surface is different, and this effect is independent of cellular morphology. This finding has implications for histological examination of tissues surrounding implants, the choice of materials that could be beneficial as implant coatings and understanding of cell-surface interactions in cardiac systems. PMID:19828193

Enhanced lithium battery with polyethylene oxide-based electrolyte containing silane-Al2 O3 ceramic filler.

PubMed

Zewde, Berhanu W; Admassie, Shimelis; Zimmermann, Jutta; Isfort, Christian Schulze; Scrosati, Bruno; Hassoun, Jusef

2013-08-01

A solid polymer electrolyte prepared by using a solvent-free, scalable technique is reported. The membrane is formed by low-energy ball milling followed by hot-pressing of dry powdered polyethylene oxide polymer, LiCF3 SO3 salt, and silane-treated Al2 O3 (Al2 O3 -ST) ceramic filler. The effects of the ceramic fillers on the properties of the ionically conducting solid electrolyte membrane are characterized by using electrochemical impedance spectroscopy, XRD, differential scanning calorimeter, SEM, and galvanostatic cycling in lithium cells with a LiFePO4 cathode. We demonstrate that the membrane containing Al2 O3 -ST ceramic filler performs well in terms of ionic conductivity, thermal properties, and lithium transference number. Furthermore, we show that the lithium cells, which use the new electrolyte together with the LiFePO4 electrode, operate within 65 and 90 °C with high efficiency and long cycle life. Hence, the Al2 O3 -ST ceramic can be efficiently used as a ceramic filler to enhance the performance of solid polymer electrolytes in lithium batteries. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Discovery of methyl silane and confirmation of silyl cyanide in IRC +10216

NASA Astrophysics Data System (ADS)

Cernicharo, J.; Agúndez, M.; Velilla Prieto, L.; Guélin, M.; Pardo, J. R.; Kahane, C.; Marka, C.; Kramer, C.; Navarro, S.; Quintana-Lacaci, G.; Fonfría, J. P.; Marcelino, N.; Tercero, B.; Moreno, E.; Massalkhi, S.; Santander-García, M.; McCarthy, M. C.; Gottlieb, C. A.; Alonso, J. L.

2017-10-01

We report the discovery in space of methyl silane, CH3SiH3, from observations of ten rotational transitions between 80 and 350 GHz (Ju from 4 to 16) with the IRAM 30 m radio telescope. The molecule was observed in the envelope of the C-star IRC +10216. The observed profiles and our models for the expected emission of methyl silane suggest that the it is formed in the inner zones of the circumstellar envelope, 1-40 R∗, with an abundance of (0.5-1) × 10-8 relative to H2. We also observed several rotational transitions of silyl cyanide (SiH3CN), confirming its presence in IRC +10216 in particular, and in space in general. Our models indicate that silyl cyanide is also formed in the inner regions of the envelope, around 20 R∗, with an abundance relative to H2 of 6 × 10-10. The possible formation mechanisms of both species are discussed. We also searched for related chemical species but only upper limits could be obtained. This work was based on observations carried out with the IRAM 30-m telescope. IRAM is supported by INSU/CNRS (France), MPG (Germany), and IGN (Spain).

Biofunctionalized anti-corrosive silane coatings for magnesium alloys.

PubMed

Liu, Xiao; Yue, Zhilian; Romeo, Tony; Weber, Jan; Scheuermann, Torsten; Moulton, Simon; Wallace, Gordon

2013-11-01

Biodegradable magnesium alloys are advantageous in various implant applications, as they reduce the risks associated with permanent metallic implants. However, a rapid corrosion rate is usually a hindrance in biomedical applications. Here we report a facile two step procedure to introduce multifunctional, anti-corrosive coatings on Mg alloys, such as AZ31. The first step involves treating the NaOH-activated Mg with bistriethoxysilylethane to immobilize a layer of densely crosslinked silane coating with good corrosion resistance; the second step is to impart amine functionality to the surface by treating the modified Mg with 3-amino-propyltrimethoxysilane. We characterized the two-layer anticorrosive coating of Mg alloy AZ31 by Fourier transform infrared spectroscopy, static contact angle measurement and optical profilometry, potentiodynamic polarization and AC impedance measurements. Furthermore, heparin was covalently conjugated onto the silane-treated AZ31 to render the coating haemocompatible, as demonstrated by reduced platelet adhesion on the heparinized surface. The method reported here is also applicable to the preparation of other types of biofunctional, anti-corrosive coatings and thus of significant interest in biodegradable implant applications. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Rigidity and retention of ceramic root canal posts.

PubMed

Purton, D G; Love, R M; Chandler, N P

2000-01-01

Ceramic root-canal posts offer potential advantages over other types with respect to aesthetics and biocompatibility. Any post must be sufficiently rigid and retentive to withstand functional forces. Ceraposts (1.2 mm coronal diameter, ceramic, tapering, smooth posts) and Paraposts (1.25 mm, stainless-steel, parallel, serrated posts) were tested for rigidity by means of a three-point bending test. To test retention in roots, ceramic posts were cemented using one of three protocols: (1) glass-ionomer cement, (2) silane coupling agent and resin cement, or (3) sandblasted post surface, silane coupling agent, and resin cement. Stainless-steel posts were cemented with resin. The tensile force required to dislodge the posts, following four weeks of storage in water, was recorded. Data were compared using Student's t-test and Mann-Whitney U analysis. Ceraposts were significantly more rigid than Paraposts (p < 0.001). Paraposts cemented with resin were significantly more strongly retained than Ceraposts following any cementation protocol (p < 0.001). Retention of the ceramic posts was significantly greater with a silane coupling agent and resin cement than with glass-ionomer cement (p < 0.001). Sandblasting the ceramic posts produced variable results and needs further investigation before it could be recommended.

Can a novel silver nano coating reduce infections and maintain cell viability in vitro?

PubMed

Qureshi, Ammar T; Landry, Jace P; Dasa, Vinod; Janes, Marlene; Hayes, Daniel J

2014-03-01

Herein we report a facile layer-by-layer method for creating an antimicrobial coating composed of silver nanoparticles on medical grade titanium test discs. Nanoscale silver nanoparticle layers are attached to the titanium orthopedic implant material via aminopropyltriethoxy silane crosslinker that reacts with neighboring silane moieties to create an interconnected network. A monolayer of silane, followed by a monolayer of silver nanoparticles would form one self-assembled layer and this process can be repeated serially, resulting in increased silver nanoparticles deposition. The release rate of silver ion increases predictably with increasing numbers of layers and at appropriate thicknesses these coatings demonstrate 3-4 log reduction of viable Escherichia coli and Staphylococcus aureus bacteria. Increasing the thickness of the coatings resulted in reduced bacterial colonization as determined by fluorescent staining and image analysis. Interestingly, the cytotoxicity of murine 3T3 cells as quantified by fluorescent staining and flow cytometry, was minimal and did not vary significantly with the coating thickness. Additionally, these coatings are mechanically stable and resist delamination by orthogonal stress test. This simple layer-by-layer coating technique may provide a cost-effective and biocompatible method for reducing microbial colonization of implantable orthopedic devices.

Effect of conditioning methods on the microtensile bond strength of phosphate monomer-based cement on zirconia ceramic in dry and aged conditions.

PubMed

Amaral, Regina; Ozcan, Mutlu; Valandro, Luiz Felipe; Balducci, Ivan; Bottino, Marco Antonio

2008-04-01

The objective of this study was to evaluate the durability of bond strength between a resin cement and aluminous ceramic submitted to various surface conditioning methods. Twenty-four blocks (5 x 5 x 4 mm(3)) of a glass-infiltrated zirconia-alumina ceramic (In-Ceram Zirconia Classic) were randomly divided into three surface treatment groups: ST1-Air-abrasion with 110-mum Al2O3 particles + silanization; ST2-Laboratory tribochemical silica coating method (110-microm Al2O3, 110-microm silica) (Rocatec) + silanization; ST3-Chairside tribochemical silica coating method (30-microm SiO(x)) (CoJet) + silanization. Each treated ceramic block was placed in its silicone mold with the treated surface exposed. The resin cement (Panavia F) was prepared and injected into the mold over the treated surface. Specimens were sectioned to achieve nontrimmed bar specimens (14 sp/block) that were randomly divided into two conditions: (a) Dry-microtensile test after sectioning; (b) Thermocycling (TC)-(6,000x, 5-55 degrees C) and water storage (150 days). Thus, six experimental groups were obtained (n = 50): Gr1-ST1 + dry; Gr2-ST1 + TC(;) Gr3-ST2 + dry; Gr4-ST2 + TC; Gr5-ST3 + dry; Gr6-ST3 + TC. After microtensile testing, the failure types were noted. ST2 (25.1 +/- 11) and ST3 (24.1 +/- 7.4) presented statistically higher bond strength (MPa) than that of ST1 (17.5 +/- 8) regardless of aging conditions (p < 0.0001). While Gr2 revealed the lowest results (13.3 +/- 6.4), the other groups (21.7 +/- 7.4-25. 9 +/- 9.1) showed statistically no significant differences (two-way ANOVA and Tukey's test, alpha = 0.05). The majority of the failures were mixed (82%) followed by adhesive failures (18%). Gr2 presented significantly higher incidence of ADHESIVE failures (54%) than those of other groups (p = 0.0001). Both laboratory and chairside silica coating plus silanization showed durable bond strength. After aging, air-abrasion with 110-microm Al(2)O(3) + silanization showed the largest decrease indicating that aging is fundamental for bond strength testing for acid-resistant zirconia ceramics in order to estimate their long-term performance in the mouth.

The Emergence of Manganese-Based Carbonyl Hydrosilylation Catalysts.

PubMed

Trovitch, Ryan J

2017-11-21

In recent years, interest in homogeneous manganese catalyst development has intensified because of the earth-abundant and nontoxic nature of this metal. Although compounds of Mn have largely been utilized for epoxidation reactions, recent efforts have revealed that Mn catalysts can mediate a broad range of reductive transformations. Low-valent Mn compounds have proven to be particularly effective for the hydrosilylation of carbonyl- and carboxylate-containing substrates, and this Account aims to highlight my research group's contributions to this field. In our initial 2014 communication, we reported that the bis(imino)pyridine-supported compound ( Ph2PPr PDI)Mn mediates ketone hydrosilylation with exceptional activity under solvent-free conditions. Silanes including Ph 2 SiH 2 , (EtO) 3 SiH, (EtO) 2 MeSiH, and (EtO)Me 2 SiH were found to partially reduce cyclohexanone in the presence of ( Ph2PPr PDI)Mn, while turnover frequencies of up to 1280 min -1 were observed using PhSiH 3 . This led us to evaluate the hydrosilylation of 11 additional ketones and allowed for the atom-efficient preparation of tertiary and quaternary silanes. At that time, it was also discovered that ( Ph2PPr PDI)Mn catalyzes the dihydrosilylation of esters (by way of acyl C-O bond hydrosilylation) to yield a mixture of silyl ethers with modest activity. Earlier this year, the scope of these transformations was extended to aldehydes and formates, and the observed hydrosilylation activities are among the highest obtained for any transition-metal catalyst. The effectiveness of three related catalysts has also been evaluated: ( Ph2PPr PDI)MnH, ( PyEt PDEA)Mn, and [( Ph2PEt PDI)Mn] 2 . To our surprise, ( Ph2PPr PDI)MnH was found to exhibit higher carboxylate dihydrosilylation activity than ( Ph2PPr PDI)Mn, while ( PyEt PDEA)Mn demonstrated remarkable carbonyl hydrosilylation activity considering that it lacks a redox-active supporting ligand. The evaluation of [( Ph2PEt PDI)Mn] 2 revealed competitive aldehyde hydrosilylation and formate dihydrosilylation turnover frequencies; however, this catalyst is significantly inhibited by pyridine and alkene donor groups. In our efforts to fully understand how ( Ph2PPr PDI)Mn operates, a thorough electronic structure evaluation was conducted, and the ground-state doublet calculated for this compound was found to exhibit nonclassical features consistent with a low-spin Mn(II) center supported by a singlet PDI dianion and an intermediate-spin Mn(II) configuration featuring antiferromagnetic coupling to PDI diradical dianion. A comprehensive mechanistic investigation of ( Ph2PPr PDI)Mn- and ( Ph2PPr PDI)MnH-mediated hydrosilylation has revealed two operable pathways, a modified Ojima pathway that is more active for carbonyl hydrosilylation and an insertion pathway that is more effective for carboxylate reduction. Although these efforts represent a small fraction of the recent advances made in Mn catalysis, this work has proven to be influential for the development of Mn-based reduction catalysts and is likely to inform future efforts to develop Mn catalysts that can be used to prepare silicones.

Titanium-silicon oxide film structures for polarization-modulated infrared reflection absorption spectroscopy

PubMed Central

Dunlop, Iain E.; Zorn, Stefan; Richter, Gunther; Srot, Vesna; Kelsch, Marion; van Aken, Peter A.; Skoda, Maximilian; Gerlach, Alexander; Spatz, Joachim P.; Schreiber, Frank

2010-01-01

We present a titanium-silicon oxide film structure that permits polarization modulated infrared reflection absorption spectroscopy on silicon oxide surfaces. The structure consists of a ~6 nm sputtered silicon oxide film on a ~200 nm sputtered titanium film. Characterization using conventional and scanning transmission electron microscopy, electron energy loss spectroscopy, X-ray photoelectron spectroscopy and X-ray reflectometry is presented. We demonstrate the use of this structure to investigate a selectively protein-resistant self-assembled monolayer (SAM) consisting of silane-anchored, biotin-terminated poly(ethylene glycol) (PEG). PEG-associated IR bands were observed. Measurements of protein-characteristic band intensities showed that this SAM adsorbed streptavidin whereas it repelled bovine serum albumin, as had been expected from its structure. PMID:20418963

Mechanical properties of HDPE/UHMWPE blends: effect of filler loading and filler treatment.

PubMed

Lai, K L K; Roziyanna, A; Ogunniyi, D S; Zainal, Arifin M I; Azlan, Ariffin A

2004-05-01

Various blend ratios of high-density polyethylene (HDPE) and ultra high molecular weight polyethylene (UHMWPE) were prepared with the objective of determining their suitability as biomaterials. In the unfilled state, a blend of 50/50 (HDPE/UHMWPE) ratio by weight was found to yield optimum properties in terms of processability and mechanical properties. Hydroxyapatite (HA) was compounded with the optimum blend ratio. The effects of HA loading, varied from 0 to 50wt% for both filled and unfilled blends were tested for mechanical properties. It was found that the inclusion of HA in the blend led to a remarkable improvement of mechanical properties compared to the unfilled blend. In order to improve the bonding between the polymer blend and the filler, the HA used was chemically treated with a coupling agent known as 3-(trimethoxysiyl) propyl methacrylate and the treated HA was mixed into the blend. The effect of mixing the blend with silane-treated HA also led to an overall improvement of mechanical properties.

Evaluation of mosquito larvicidal activity of fruit extracts of Acacia auriculiformis against the Japanese encephalitis vector Culex vishnui.

PubMed

Barik, Mousumi; Rawani, Anjali; Laskar, Subrata; Chandra, Goutam

2018-02-19

The larvicidal potentiality of crude and ethyl acetate extracts of fruits of Acacia auriculiformis was investigated against all the larval instars of JE vector Culex vishnui. The crude extracts showed good results against all the larval instars with highest mortality at 0.09%. Highest mortality was found at 300 ppm of ethyl acetate extract. Lowest LC 50 value was obtained at 72 h for third instar larvae. Non target organisms tested, showed no to very less mortality to ethyl acetate solvent extract. Presence of N-H stretching, a C=O stretching, C=C and C-N stretching vibrations of secondary amide or amine group were confirmed from IR analysis. GC-MS analysis revealed the presence of three compounds namely Ethane 2-chloro-1,1-dimethoxy, Acetic acid, 1-methyl ether ester and [4-[1-[3,5-Dimethyl-4[(trimethylsilyl)oxy)phenyl]-1,3-dimethylbutyl)-2,6dimethylphenoxy)(trimethyl) silane, responsible for mosquito larval death.

Modified silica sol coatings for surface enhancement of leather.

PubMed

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.

Volatile metabolites of higher plant crops as a photosynthesizing life support system component under temperature stress at different light intensities

NASA Astrophysics Data System (ADS)

Gitelson, I. I.; Tikhomirov, A. A.; Parshina, O. V.; Ushakova, S. A.; Kalacheva, G. S.

The effect of elevated temperatures of 35 and 45°C (at the intensities of photosynthetically active radiation 322, 690 and 1104 μmol·m -2·s -1) on the photosynthesis, respiration, and qualitative and quantitative composition of the volatiles emitted by wheat ( Triticum aestuvi L., cultivar 232) crops was investigated in growth chambers. Identification and quantification of more than 20 volatile compounds (terpenoids-α-pinene, Δ3 carene, limonene, benzene, α-and trans-caryophyllene, α- and γ-terpinene, their derivatives, aromatic hydrocarbons, etc.) were conducted by gas chromatograph/mass spectrometry. Under light intensity of 1104 μmol·m -2·s -1 heat resistance of photosynthesis and respiration increased at 35°C and decreased at 45°C. The action of elevated temperatures brought about variations in the rate and direction of the synthesis of volatile metabolites. The emission of volatile compounds was the greatest under a reduced irradiation of 322 μmol·m -2·s -1 and the smallest under 1104 μmol·m -2·s -1, at 35°C. During the repair period, the contents and proportions of volatile compounds were different from their initial values, too. The degree of disruption and the following recovery of the functional state depended on the light intensity during the exposure to elevated temperatures. The investigation of the atmosphere of the growth chamber without plants has revaled the substances that were definitely technogenic in origin: tetramethylurea, dimethylsulfide, dibutylsulfide, dibutylphthalate, and a number of components of furan and silane nature.

1,3,4-Oxadiazole containing silanes as novel hosts for blue phosphorescent organic light emitting diodes.

PubMed

Leung, Man-kit; Yang, Wan-Hsi; Chuang, Ching-Nan; Lee, Jiun-Haw; Lin, Chi-Feng; Wei, Mao-Kuo; Liu, Yu-Hao

2012-10-05

Five rigid oxadiazole (OXD) containing silanes, denoted 1-5, have been developed with high morphological stability. Disruption of the π-aromatic conjugation by introduction of Si atoms leads to a large band gap and high triplet energy. Among the OXDs we studied, 2,5-bis(triphenylsilylphenyl)-1,3,4-oxadiazole 5 is the best host for FIrpic, with a phosphorescent organic light emitting diode (PHOLED) turn-on voltage of 6.9 V, maximum luminance of 5124 cd/m(2), current efficiency of 39.9 cd/A, and external quantum efficiency of 13.1%. Special molecular stacking in the single crystal of 5 was discussed.

Fabrication of pH sensitive nanovalves using smart surface coated nanopores

NASA Astrophysics Data System (ADS)

Nieto-Soto, A. M.; Diaz-Maldonado, D. K.; Rios Angarita, F. A.

2017-01-01

A pH sensitive nanovalve was fabricated using different smart surfaces covalently attached to an anodized aluminium oxide membrane (AAO). The smart surfaces were synthesized using a mixture of aliphatic and aminated silanes. Effect on the contact angle of the aliphatic silane chain length was evaluated. The smart surface, in conjunction with a nanoporous membrane, allowed the formation of a hydrophobic plug which controlled the transport of the molecule safranine depending on the pH of the solution. It was demonstrated that mixtures of butyl and methyl-trimethoxysilane with aminopropyl-trimethoxysilane were able to perform as effective nanovalves creating a plug that remained closed at pH>7 and opened up at pH<5.

N,N-difluorotris(tert-butyl)silylamine-the first organosilyl difluoroamine. Synthesis and computational studies.

PubMed

Majumder, Utpal; Armantrout, John R; Williams, Richard Vaughan; Shreeve, Jean'ne M

2002-11-29

The synthesis and characterization of the first stable trialkyl(difluoroamino)silane, R3SiNF2, as well as of R3SiNHF and R3SiN(CH3)F in moderate yields are reported. The (difluoroamino)silane has promise as a new synthon for the introduction of the -NF2 group into a variety of electrophilic inorganic and organic substrates. Activation barriers and relative energies were calculated for the unimolecular decompositions of Me3SiCF3 and t-Bu3SiNF2 using density functional theory (B3LYP/6-31G). The calculated activation energies confirm the long-assumed kinetic stability of Me3SiCF3.

Preparation and wettability examinations of transparent SiO2 binder-added MgF2 nanoparticle coatings covered with fluoro-alkyl silane self-assembled monolayer.

PubMed

Murata, Tsuyoshi; Hieda, Junko; Saito, Nagahiro; Takai, Osamu

2012-05-01

SiO2-added MgF2 nanoparticle coatings with various surface roughness properties were formed on fused silica-glass substrates from autoclaved sols prepared at 100-180 °C. To give it hydrophobicity, we treated the samples with fluoro-alkyl silane (FAS) vapor to form self-assembled monolayers on the nanoparticle coating and we examined the wettability of the samples. The samples preserved good transparency even after the FAS treatment. The wettability examination revealed that higher autoclave temperatures produced a larger average MgF2 nanoparticle particle size, a larger surface roughness, and a higher contact angle and the roll-off angle.

Deposition of device quality low H content, amorphous silicon films

DOEpatents

Mahan, A.H.; Carapella, J.C.; Gallagher, A.C.

1995-03-14

A high quality, low hydrogen content, hydrogenated amorphous silicon (a-Si:H) film is deposited by passing a stream of silane gas (SiH{sub 4}) over a high temperature, 2,000 C, tungsten (W) filament in the proximity of a high temperature, 400 C, substrate within a low pressure, 8 mTorr, deposition chamber. The silane gas is decomposed into atomic hydrogen and silicon, which in turn collides preferably not more than 20--30 times before being deposited on the hot substrate. The hydrogenated amorphous silicon films thus produced have only about one atomic percent hydrogen, yet have device quality electrical, chemical, and structural properties, despite this lowered hydrogen content. 7 figs.

Deposition of device quality low H content, amorphous silicon films

DOEpatents

Mahan, Archie H.; Carapella, Jeffrey C.; Gallagher, Alan C.

1995-01-01

A high quality, low hydrogen content, hydrogenated amorphous silicon (a-Si:H) film is deposited by passing a stream of silane gas (SiH.sub.4) over a high temperature, 2000.degree. C., tungsten (W) filament in the proximity of a high temperature, 400.degree. C., substrate within a low pressure, 8 mTorr, deposition chamber. The silane gas is decomposed into atomic hydrogen and silicon, which in turn collides preferably not more than 20-30 times before being deposited on the hot substrate. The hydrogenated amorphous silicon films thus produced have only about one atomic percent hydrogen, yet have device quality electrical, chemical, and structural properties, despite this lowered hydrogen content.

Measurement of cyclic volatile methylsiloxanes in the aquatic environment using low-density polyethylene passive sampling devices using an in-field calibration study--challenges and guidance.

PubMed

Bruemmer, Janine; Falcon, Raquel; Greenwood, Richard; Mills, Graham A; Hastie, Colin; Sparham, Chris; van Egmond, Roger

2015-03-01

Cyclic volatile methylsiloxanes (cVMS) are used in personal care products and are hydrophobic, volatile and persistent. Their environmental water concentrations are low and are difficult to detect using conventional sampling methods. This study shows the potential of passive sampling for cVMS. We used low-density polyethylene (LDPE) samplers and in-field calibration methods for octamethylcyclotetrasiloxane (D4) and decamethylcyclopentasiloxane (D5). (13)C-D4 and (13)C-D5, methyltris(trimethylsiloxy)silane (MT), tetrakis(trimethylsiloxy)silane (TK), and five deuterated polycyclic aromatic hydrocarbons (PAHs) were used as performance reference compounds (PRCs). Samplers were calibrated (7-d) using effluent at a treatment plant, with uptake of cVMS and losses of the PRCs measured at 12 time-points. Concentrations of D4 (53ngL(-1)) and D5 (1838ngL(-1)) were stable in the effluent. Uptake of D4 and loss of (13)C-D4 were isotropic and equilibrium was approached by 7-d. Two estimates of sampler uptake rate (Rs) were 2.1Ld(-1) and 2.5Ld(-1). The estimated log LDPE/water partition coefficient was 4.4. The uptake of D5 was slower (Rs=0.32Ld(-1)) and equilibrium was not reached. Offloading of (13)C-D5, MT and TK were slow, and isotropic behaviour was not demonstrated for D5. Offloading of PAHs followed the predicted pattern for LDPE. Uptake of cVMS appeared to be under membrane control, due to low diffusion coefficients in LDPE. Samplers can monitor time-weighted average concentrations of D4 for less than a week, and D5 for longer periods. LDPE samplers allow cVMS to be determined at lower concentrations than by spot sampling methods. Copyright © 2014 Elsevier Ltd. All rights reserved.

Mesoporous silica fillers and resin composition effect on dental composites cytocompatibility.

PubMed

Attik, Nina; Hallay, Franck; Bois, Laurence; Brioude, Arnaud; Grosgogeat, Brigitte; Colon, Pierre

2017-02-01

Many new dental composites containing mesoporous silica fillers have been developed to improve rheological properties and enhance the resin-filler interface. To investigate the correlation between the cytocompatibility of several dental composites and their composition; two aspects have been considered: presence of bisphenol A (BPA)-glycidyl methacrylate (Bis-GMA) or triethyleneglycol-dimethacrylate (TEGDMA) among the resin monomers and presence of porous particles among the filler blends. Five commercial composites with different resin matrices and mineral fillers were compared to four experimental composites designed without any BPA-based monomers or TEGDMA. Porous fillers, with or without silanation, were added in some of the experimental composites. Two reference resin matrices were also selected. Cytocompatibility with cultured primary human gingival fibroblasts was assessed by confocal laser scanning microscopy with time-lapse imaging. Fourier transform infrared spectroscopy was used to control monomer conversion rate. Conversion rates of the experimental composites ranged from 57% to 71%, a comparable ratio for dental composites. Experimental samples were better tolerated than tested commercial samples not containing TEGDMA and significantly better than those containing TEGDMA. Experimental composites with porous fillers exhibited good cytocompatibility, especially when surfaces were silanated. Cytotoxicity was associated with resin amount and especially resin nature. Composites containing porous fillers might behave as if the resin trapped into pores has no effect on toxicity. The cytotoxicity of composites with and without BPA derivatives was mainly attributed to the release of residual TEGDMA rather than the BPA derivatives. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Tris(trimethylsilyl)silane as a co-initiator for dental adhesive: Photo-polymerization kinetics and dynamic mechanical property

PubMed Central

Song, Linyong; Ye, Qiang; Ge, Xueping; Misra, Anil; Spencer, Paulette

2017-01-01

Objectives The purpose of this study was to evaluate the polymerization behavior of a model dentin adhesive with tris(trimethylsilyl)silane (TTMSS) as a co-initiator, and to investigate the polymerization kinetics and mechanical properties of copolymers in dry and wet conditions. Methods A co-monomer mixture based on HEMA/BisGMA (45/55, w/w) was used as a model dentin adhesive. The photoinitiator system included camphorquinone (CQ) as the photosensitizer and the co-initiator was ethyl-4-(dimethylamino) benzoate (EDMAB) or TTMSS. Iodonium salt, diphenyliodonium hexafluorophosphate (DPIHP) serving as a catalyst, was selectively added into the adhesive formulations. The control and the experimental formulations were characterized with regard to the degree of conversion (DC) and dynamic mechanical properties under dry and wet conditions. Results In two-component photoinitiator system (CQ/TTMSS), with an increase of TTMSS concentration, the polymerization rate and DC of C═C double bond increased, and showed a dependence on the irradiation time and curing light intensity. The copolymers that contained the three-component photoinitiator system (CQ/TTMSS/DPIHP) showed similar dynamic mechanical properties, under both dry and wet conditions, to the EDMAB-containing system. Significance The DC of formulations using TTMSS as co-initiator showed a strong dependence on irradiation time. With the addition of TTMSS, the maximum polymerization rate can be adjusted and the network structure became more homogenous. The results indicated that the TTMSS could be used as a substitute for amine-type co-initiator in visible-light induced free radical polymerization of methacrylate-based dentin adhesives. PMID:26616688

A new organofunctional ethoxysilane self-assembly monolayer for promoting adhesion of rubber to aluminum.

PubMed

Wang, Fang; Xu, Juan; Luo, Heyi; Wang, Jinggang; Wang, Qian

2009-10-12

Practical adhesion of rubber to aluminum is measured for various aluminum silanization treatments. In this study, 6-(3-triethoxysilylpropylamino)-1,3,5-triazine-2,4-dithiol (TES) was used as the coupling agent for preparing self-assembly monolayers (SAMs) on an aluminum surface. The structure and chemical composition of the SAMs were analyzed using Fourier transform infra-red spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The changes in the surface features of the aluminum surface due to TES treatment were investigated by atomic force microscopy (AFM). The adhesive properties of the silanized aluminum surface and EPDM rubber have been evaluated by a T-peel strength test. The results suggested that the Si-O-Al bonding at aluminum TES interface existed and a TES self-assembly monolayer was formed on the aluminum surface. More than 6.0 KN/m adhesion strength is obtained when the aluminum is silanized with 2.5 mmol/dm(3) TES, cured at 160 degrees C and vulcanized with EPDM rubber at 160 degrees C for 30 min. It is suggested that the TES self-assembly monolayer is bound to aluminum through its ethoxysilyl functional group, and the thiol function group is strongly crosslinked to EPDM rubber, respectively.

Inhibition of Photocatalytic Activity of Basic Blue-41 by ZnO Modified Surface with Amino Silane

NASA Astrophysics Data System (ADS)

Limsapapkasiphon, S.; Sirisaksoontorn, W.; Songsasen, A.

2018-03-01

The reduction of the photo catalytic efficiency of ZnO can be achieved by modifying its surface with amino silane, which synthesized through condensation reaction under basic condition. The pH of solution was varied from 8 to 14 during the synthesis and was found that pH 12 was the most suitable pH for the preparation. All of ZMAS were characterized by Elemental Analysis which showed the highest percentage of nitrogen at 3.1064% and IR technique which indicated the Si-O-Zn bond at about 1000 cm-1. The photodegradation property of ZMAS prepared at pH 8-12 toward basic blue 41 was retarded when compared with the unmodified ZnO. Effect of mole ratio of ZnO:APTES (1:0.1, 1:0.5, 1:1, and 1:2) in the preparation of ZMAS was investigated. The photodegration activity of ZMAS prepared at mole ratio of ZnO:APTES as 1:0.5 to 1:2 toward basic blue 41 was retarded when compared with the unmodified ZnO. The coating of amino silane on ZnO surface did not have much effect on the band gap energy of modified ZnO. The absorption edge of ZMAS was only slightly shifted from 392 to 397 nm.

Fabrication of bio-inspired nitinol alloy surface with tunable anisotropic wetting and high adhesive ability.

PubMed

Tian, Yan L; Zhao, Yue C; Yang, Cheng J; Wang, Fu J; Liu, Xian P; Jing, Xiu B

2018-10-01

In this paper, micro/nano-scale structures were fabricated on nitinol alloy (NiTi) to realize tunable anisotropic wetting and high adhesive capability. Laser texturing and silanization process are utilized to change the morphological and chemical properties of substrates. It is noted that these treated substrates exhibit the joint characteristics of anisotropic wetting and high adhesive capability. In order to investigate the influences of laser-texturing and silanization processes on NiTi, these surfaces were evaluated using scanning electron microscope (SEM), a white light confocal microscope, X-ray photoelectron spectroscopy (XPS) and goniometer. The relationship between water volume and anisotropic wetting was also established. From the experimental testing, we can obtain the following conclusions: (1) the anisotropic wetting characterized by the difference between the water contact angles (WCAs) in the vertical and parallel directions ranges from 0° to 20.3°, which is far more than the value of natural rice leaves. (2) the water sliding angles (WSAs) kept stable at 180°, successfully mimicking the adhesive ability of rose petals. (3) the silanization process could strengthen the hydrophobicity but weaken anisotropic wetting. These bio-inspired NiTi surfaces have a tremendous potential applications such as microfluidic devices, bio-mimetic materials fabrication and lab on chip. Copyright © 2018 Elsevier Inc. All rights reserved.

Nanodusty plasma chemistry: a mechanistic and variational transition state theory study of the initial steps of silyl anion-silane and silylene anion-silane polymerization reactions.

PubMed

Bao, Junwei Lucas; Seal, Prasenjit; Truhlar, Donald G

2015-06-28

The growth of nanodusty particles, which is critical in plasma chemistry, physics, and engineering. The aim of the present work is to understand the detailed reaction mechanisms of early steps in this growth. The polymerization of neutral silane with the silylene or silyl anion, which eliminates molecular hydrogen with the formation of their higher homologues, governs the silicon hydride clustering in nanodusty plasma chemistry. The detailed mechanisms of these important polymerization reactions in terms of elementary reactions have not been proposed yet. In the present work, we investigated the initial steps of these polymerization reactions, i.e., the SiH4 + Si2H4(-)/Si2H5(-) reactions, and we propose a three-step mechanism, which is also applicable to the following polymerization steps. CM5 charges of all the silicon-containing species were computed in order to analyze the character of the species in the proposed reaction mechanisms. We also calculated thermal rate constant of each step using multi-structural canonical variational transition state theory (MS-CVT) with the small-curvature tunneling (SCT) approximation, based on the minimum energy path computed using M08-HX/MG3S electronic structure method.

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

PubMed Central

Liu, Peng; Chen, Ying; Yu, Zhiwu

2016-01-01

A method to prepare novel organic-inorganic hydrophobic nanocomposite films was proposed by a site-specific polymerization process. The inorganic part, the core of the nanocomposite, is a ternary SiO2–Al2O3–TiO2 nanoparticles, which is grafted with methacryloxy propyl trimethoxyl silane (KH570), and wrapped by fluoride and siloxane polymers. The synthesized samples are characterized by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectrscopy, X-ray diffractometry (XRD), contact angle meter (CA), and scanning electron microscope (SEM). The results indicate that the novel organic-inorganic hydrophobic nanocomposite with a core-shell structure was synthesized successfully. XRD analysis reveals the nanocomposite film has an amorphous structure, and FTIR analysis indicates the nanoparticles react with a silane coupling agent (methacryloxy propyl trimethoxyl silane KH570). Interestingly, the morphology of the nanoparticle film is influenced by the composition of the core. Further, comparing with the film synthesized by silica nanoparticles, the film formed from SiO2–Al2O3–TiO2 nanoparticles has higher hydrophobic performance, i.e., the contact angle is greater than 101.7°. In addition, the TEM analysis reveals that the crystal structure of the particles can be changed at high temperatures. PMID:28774141

Method of bonding functional surface materials to substrates and applications in microtechnology and anti-fouling

DOEpatents

Feng, Xiangdong; Liu, Jun; Liang, Liang

2001-01-01

A simple and effective method to bond a thin coating of poly(N-isopropylacylamide) (NIPAAm) on a glass surface by UV photopolymerization, and the use of such a coated surface in nano and micro technology applications. A silane coupling agent with a dithiocarbamate group is provided as a photosensitizer preferably, (N,N'-diethylamine) dithiocarbamoylpropyl-(trimethoxy) silane (DATMS). The thiocarbamate group of the sensitizer is then bonded to the glass surface by coupling the silane agent with the hydroxyl groups on the glass surface. The modified surface is then exposed to a solution of NIPAAm and a crosslinking agent which may be any organic molecule having an acrylamide group and at least two double bonds in its structure, such as N, N'-methylenebisacrylamide, and a polar solvent which may be any polar liquid which will dissolve the monomer and the crosslinking agent such as acetone, water, ethanol, or combinations thereof. By exposing the glass surface to a UV light, free radicals are generated in the thiocarbamate group which then bonds to the crosslinking agent and the NIPAAm. Upon bonding, the crosslinking agent and the NIPAAm polymerize to form a thin coating of PNIPAAm bonded to the glass. Depending upon the particular configuration of the glass, the properties of the PNIPAAm allow applications in micro and nano technology.

Method of bonding functional surface materials to substrates and applications in microtechnology and antifouling

DOEpatents

Feng, Xiangdong; Liu, Jun; Liang, Liang

1999-01-01

A simple and effective method to bond a thin coating of poly(N-isopropylacylamide) (NIPAAm) on a glass surface by UV photopolymerization, and the use of such a coated surface in nano and micro technology applications. A silane coupling agent with a dithiocarbamate group is provided as a photosensitizer, preferably, (N,N'-diethylamine)dithiocarbamoylpropyl-(trimethoxy)silane (DATMS). The thiocarbamate group of the sensitizer is then bonded to the glass surface by coupling the silane agent with the hydroxyl groups on the glass surface. The modified surface is then exposed to a solution of NIPAAm and a crosslinking agent which may be any organic molecule having an acrylamide group and at least two double bonds in its structure, such as N,N'-methylenebisacrylamide, and a polar solvent which may be any polar liquid which will dissolve the monomer and the crosslinking agent such as acetone, water, ethanol, or combinations thereof. By exposing the glass surface to a UV light, free radicals are generated in the thiocarbamate group which then bonds to the crosslinking agent and the NIPAAm. Upon bonding, the crosslinking agent and the NIPAAm polymerize to form a thin coating of PNIPAAm bonded to the glass. Depending upon the particular configuration of the glass, the properties of the PNIPAAm allow applications in micro and nano technology.

Inorganic/Organic Hybrid Silica Nanoparticles as a Nitric Oxide Delivery Scaffold.

PubMed

Shin, Jae Ho; Schoenfisch, Mark H

2008-01-01

The preparation and characterization of nitric oxide (NO)-releasing silica particles formed following the synthesis of N -diazeniumdiolate-modified aminoalkoxysilanes are reported. Briefly, an aminoalkoxysilane solution was prepared by dissolving an appropriate amount of aminoalkoxysilane in a mixture of ethanol, methanol, and sodium methoxide (NaOMe) base. The silane solution was reacted with NO (5 atm) to form N -diazeniumdiolate NO donor moieties on the amino-alkoxysilanes. Tetraethoxy- or tetramethoxysilane (TEOS or TMOS) was then mixed with different ratios of N -diazeniumdiolate-modified aminoalkoxysilane (10 - 75 mol%, balance TEOS or TMOS). Finally, the silane mixture was added into ethanol in the presence of an ammonia catalyst to form NO donor silica nanoparticles via a sol-gel process. This synthetic approach allows for the preparation of NO delivery silica scaffolds with remarkably improved NO storage and release properties, surpassing all macromolecular NO donor systems reported to date with respect to NO payload (11.26μmol·mg -1 ), maximum NO release amount (357000 ppb·mg -1 ), NO release half-life (253 min), and NO release duration (101 h). The N -diazeniumdiolate-modified silane monomers and the resulting silica nanoparticles were characterized by 29 Si nuclear magnetic resonance (NMR) spectroscopy, UV-visible spectroscopy, chemiluminescence, atomic force microscopy (AFM), gas adsorption-desorption isotherms, and elemental analysis.

Using Deep Learning for Compound Selectivity Prediction.

PubMed

Zhang, Ruisheng; Li, Juan; Lu, Jingjing; Hu, Rongjing; Yuan, Yongna; Zhao, Zhili

2016-01-01

Compound selectivity prediction plays an important role in identifying potential compounds that bind to the target of interest with high affinity. However, there is still short of efficient and accurate computational approaches to analyze and predict compound selectivity. In this paper, we propose two methods to improve the compound selectivity prediction. We employ an improved multitask learning method in Neural Networks (NNs), which not only incorporates both activity and selectivity for other targets, but also uses a probabilistic classifier with a logistic regression. We further improve the compound selectivity prediction by using the multitask learning method in Deep Belief Networks (DBNs) which can build a distributed representation model and improve the generalization of the shared tasks. In addition, we assign different weights to the auxiliary tasks that are related to the primary selectivity prediction task. In contrast to other related work, our methods greatly improve the accuracy of the compound selectivity prediction, in particular, using the multitask learning in DBNs with modified weights obtains the best performance.

Internal energy deposition with silicon nanoparticle-assisted laser desorption/ionization (SPALDI) mass spectrometry

NASA Astrophysics Data System (ADS)

Dagan, Shai; Hua, Yimin; Boday, Dylan J.; Somogyi, Arpad; Wysocki, Ronald J.; Wysocki, Vicki H.

2009-06-01

The use of silicon nanoparticles for laser desorption/ionization (LDI) is a new appealing matrix-less approach for the selective and sensitive mass spectrometry of small molecules in MALDI instruments. Chemically modified silicon nanoparticles (30 nm) were previously found to require very low laser fluence in order to induce efficient LDI, which raised the question of internal energy deposition processes in that system. Here we report a comparative study of internal energy deposition from silicon nanoparticles to previously explored benzylpyridinium (BP) model compounds during LDI experiments. The internal energy deposition in silicon nanoparticle-assisted laser desorption/ionization (SPALDI) with different fluorinated linear chain modifiers (decyl, hexyl and propyl) was compared to LDI from untreated silicon nanoparticles and from the organic matrix, [alpha]-cyano-4-hydroxycinnamic acid (CHCA). The energy deposition to internal vibrational modes was evaluated by molecular ion survival curves and indicated that the ions produced by SPALDI have an internal energy threshold of 2.8-3.7 eV. This is slightly lower than the internal energy induced using the organic CHCA matrix, with similar molecular survival curves as previously reported for LDI off silicon nanowires. However, the internal energy associated with desorption/ionization from the silicon nanoparticles is significantly lower than that reported for desorption/ionization on silicon (DIOS). The measured survival yields in SPALDI gradually decrease with increasing laser fluence, contrary to reported results for silicon nanowires. The effect of modification of the silicon particle surface with semifluorinated linear chain silanes, including fluorinated decyl (C10), fluorinated hexyl (C6) and fluorinated propyl (C3) was explored too. The internal energy deposited increased with a decrease in the length of the modifier alkyl chain. Unmodified silicon particles exhibited the highest analyte internal energy deposition. These findings may suggest a role of the modifier as a moderator in the energy dissipation and relaxation process. The relatively low internal energy content of SPALDI-produced ions indicates that this is a "soft" desorption technique, with potential advantages in the analysis of labile compounds.

Two-year interfacial bond durability and nanoleakage of repaired silorane-based resin composite.

PubMed

Mobarak, E; El-Deeb, H

2013-01-01

To investigate the effect of silane primer application, intermediate adhesive agent/repair composite, and storage period on the interfacial microtensile bond strength (μTBS) of repaired silorane-based resin composite compared with unrepaired composites and on the nanoleakage. Forty-eight 1-month-old substrate specimens from Filtek P90 were roughened, etched, and distributed over two groups (n=24) based on receiving silane (Clearfil Ceramic Primer) or not. Then, half of the specimens (n=12) were repaired with P90 System Adhesive/Filtek P90 and the other half with Adper Scotchbond Multipurpose adhesive/Filtek Z250 resin composite. Within each repair category, repaired specimens were stored in artificial saliva at 37°C for either 24 hours (n=6) or two years before being serially sectioned into sticks (0.6 ± 0.01 mm(2)). From each specimen, two sticks were prepared for nanoleakage determination and four sticks were used for μTBS testing. Additional unrepaired specimens from each composite (n=12) were made to determine the cohesive strength at 24 hours and two years. Mean μTBS were calculated and statistically analyzed. Modes of failure were also determined. General linear model analysis revealed no significant effect for the silane priming, intermediate adhesive agent/repair composite, and storage period or for their interactions on the μTBS values of the repaired specimens. There was no significant difference between the cohesive strength of Filtek P90 and Filtek Z250; both were significantly higher than all repaired categories. At 24 hours, nanoleakage was not detected when silorane-based composite was repaired with the same material. However, after two years, all repair categories showed nanoleakage. Silane application has no effect on μTBS and nanoleakage. Durability of the interfacial bond of repaired silorane-based resin composite appeared successful regardless of the chemistry of the intermediate adhesive agent/composite used for repair. However, nanoleakage was detected early when a different repair intermediate adhesive agent/composite was used.

A preliminary report on short-term clinical outcomes of three-unit resin-bonded fixed prostheses using two adhesive cements and surface conditioning combinations.

PubMed

Dündar, Mine; Ozcan, Mutlu; Cömlekoğlu, M Erhan; Güngör, Mehmet Ali

2010-01-01

The aim of this study was to evaluate the survival rate of three-unit surface-retained, resin-bonded, metal-ceramic fixed dental prostheses (RBFDP) using two adhesive cements and two surface conditioning methods. Between 2005 and 2009, a total of 58 patients (34 women, 24 men; mean age: 42.1 years) received 58 three-unit RBFDPs made of a nonprecious alloy (Wirocast Co-Cr). Restorations were cemented employing the following combinations: (1) alumina air abrasion-silane + Panavia F 2.0 (group A1), (2) tribochemical silica coating (CoJet)-silane + Panavia F 2.0 (group A2), (3) alumina air abrasion-silane + Super-Bond C and B (group B1), and (4) CoJet-silane + Super-Bond C and B (group B2). Teeth were conditioned using the adhesives of the cements accordingly. Adaptation, debonding, fracture, and crack and caries formation were considered for clinical evaluation. Data were collected at baseline, 6 months, and annually thereafter. Forty-eight RBFDPs were available for follow-up (mean: 20.3 months, minimum: 6 months, maximum: 42 months). The effect of cement type on the survival rate of RBFDPs was not significant (P > .05). The survival rate was also not significantly affected by the location (maxilla: 93.2%, mandible: 92.9%; P = .928). All experienced failures were observed within the first year after cementation. In total, four complete debondings were encountered (two in group A1, one in group A2, and one in group B1 at months 1, 3, 7, and 3, respectively). Group B2 did not result in any failures during the observation period. The failures were adhesive debondings between the metal surface and the cement. Early findings did not show significant differences between the cement and conditioning type combinations, with group B2 presenting no failures.

The effect of two fibre impregnation methods on the cytotoxicity of a glass and carbon fibre-reinforced acrylic resin denture base material on oral epithelial cells and fibroblasts.

PubMed

Sipahi, Cumhur; Ozen, Julide; Ural, A Ugur; Dalkiz, Mehmet; Beydemir, Bedri

2006-09-01

Acrylic resin dentures may have cytotoxic effects on oral soft tissues. However, there is sparse data about the cytotoxic effect of fibre-reinforced acrylic resin denture base materials. The purpose of this in vitro study was to determine the effect of two fibre impregnation methods on the cytotoxicity of a glass and carbon fibre-reinforced heat-polymerized acrylic resin denture base material on oral epithelial cells and fibroblasts. One hundred acrylic resin discs were assigned to five experimental groups (n = 20). One of the groups did not include any fibre. Two groups consisted of silane and monomer treated glass fibres (Vetrolex) impregnated into acrylic resin (QC-20) discs. The other two groups consisted of silane and monomer treated carbon fibres (Type Tenox J, HTA). Untreated cell culture was used as positive control. The human oral epithelial cell line and buccal fibroblast cultures were exposed to test specimens. The cytotoxicity of the test materials was determined by succinic dehydrogenase activity (MTT method) after 24 and 72 h exposures. Data were analysed with a statistical software program (SPSSFW, 9.0). A one-way analysis of variance (anova) test and Bonferroni test were used for the comparisons between the groups. All statistical tests were performed at the 0.95 confidence level (P < 0.05). After 24 and 72 h incubation, cell viability percentages of all experimental groups showed significant decrease according to the positive control cell culture. Fibroblastic cell viability percentages of silane and monomer treated fibre-reinforced groups were lower than the unreinforced group. Cell viability of monomer-treated groups displayed the lowest percentages. Elapsed incubation time decreased epithelial cell viability in silane-treated groups. Fibroblastic cell viability was not influenced by elapsed time except the unreinforced group.

Composite cements benefit from light-curing.

PubMed

Lührs, Anne-Katrin; De Munck, Jan; Geurtsen, Werner; Van Meerbeek, Bart

2014-03-01

To investigate the effect of curing of composite cements and a new ceramic silanization pre-treatment on the micro-tensile bond strength (μTBS). Feldspathic ceramic blocks were luted onto dentin using either Optibond XTR/Nexus 3 (XTR/NX3; Kerr), the silane-incorporated 'universal' adhesive Scotchbond Universal/RelyX Ultimate (SBU/RXU; 3M ESPE), or ED Primer II/Panavia F2.0 (ED/PAF; Kuraray Noritake). Besides 'composite cement', experimental variables were 'curing mode' ('AA': complete auto-cure at 21°C; 'AA*': complete auto-cure at 37°C; 'LA': light-curing of adhesive and auto-cure of cement; 'LL': complete light-curing) and 'ceramic surface pre-treatment' ('HF/S/HB': hydrofluoric acid ('HF': IPS Ceramic Etching Gel, Ivoclar-Vivadent), silanization ('S': Monobond Plus, Ivoclar-Vivadent) and application of an adhesive resin ('HB': Heliobond, Ivoclar-Vivadent); 'HF/SBU': 'HF' and application of the 'universal' adhesive Scotchbond Universal ('SBU'; 3M ESPE, only for SBU/RXU)). After water storage (7 days at 37°C), ceramic-dentin sticks were subjected to μTBS testing. Regarding the 'composite cement', the significantly lowest μTBSs were measured for ED/PAF. Regarding 'curing mode', the significantly highest μTBS was recorded when at least the adhesive was light-cured ('LA' and 'LL'). Complete auto-cure ('AA') revealed the significantly lowest μTBS. The higher auto-curing temperature ('AA*') increased the μTBS only for ED/PAF. Regarding 'ceramic surface pre-treatment', only for 'LA' the μTBS was significantly higher for 'HF/S/HB' than for 'HF/SBU'. Complete auto-cure led to inferior μTBS than when either the adhesive (on dentin) or both adhesive and composite cement were light-cured. The use of a silane-incorporated adhesive did not decrease luting effectiveness when also the composite cement was light-cured. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

a 480 MHz Chirped-Pulse Fourier-Transform Microwave Spectrometer: Construction and Measurement of the Rotational Spectra of Divinyl Silane and 3,3-DIFLUOROPENTANE

NASA Astrophysics Data System (ADS)

Obenchain, Daniel A.; Steber, Amanda L.; Elliott, Ashley A.; Peebles, Rebecca A.; Peebles, Sean A.; Wurrey, Charles J.; Guirgis, Gamil A.

2010-06-01

A chirped-pulse Fourier-transform microwave (CP-FTMW) spectrometer based on the original Pate design has been constructed to allow analysis of any 480 MHz region in the 7 - 18 GHz range. A 1 μs chirped-pulse (0 - 240 MHz) from an arbitrary function generator is mixed with output from a microwave synthesizer and used to polarize a supersonic gas expansion; the resulting free induction decay is collected over 20 μs and Fourier-transformed on a 500 MHz oscilloscope to produce a rotational spectrum. A variety of molecules have now been studied with this instrument and results will be presented for numerous conformers of divinyl silane (predicted μtotal = 0.6 - 0.7 D) and the more polar 3,3-difluoropentane (predicted μtotal = 2.5 - 2.8 D). Two of the three possible conformers of divinyl silane were assigned (both having a C_1=C_2-Si-C_3 dihedral angle of -120° and a {C_2-Si-C_3=C_4} dihedral of either 0° (C_1 symmetry) or -120° (C_2 symmetry)). For 3,3-difluoropentane, three of the four possible {conformers} were identified: anti-gauche (C_1), gauche-gauche (C_2) and anti-anti (C2v). While rotational spectra for only the silicon isotopologues were observed for divinyl silane, measurement of the 13C spectra of 3,3-difluoropentane allowed heavy atom structure determinations for the anti-gauche and gauche-gauche conformers. Initial assignments of all spectra were made on the CP-FTMW {spectrometer}, and a Balle-Flygare FTMW spectrometer was used to compare frequencies of measured transitions and also to provide Stark effect data. Substitution (r_s) and inertial fit (r_0) structures will be compared with computational data and instrumental details will be presented. G.G. Brown, B.C. Dian, K.O. Douglass, S.M. Geyer, S.T. Shipman, B.H. Pate, Rev. Sci. Instrum., 79, (2008), 053103.

Bond strength of metal brackets bonded to a silica-based ceramic with light-cured adhesive : Influence of various surface treatment methods.

PubMed

Zhang, Zhe-Chen; Qian, Yu-Fen; Yang, Yi-Ming; Feng, Qi-Ping; Shen, Gang

2016-09-01

The purpose of this work was to evaluate the effects of several surface treatment methods on the shear bond strengths of metal brackets bonded to a silica-based ceramic with a light-cured adhesive. Silica-based ceramic (IPS Classic(®)) with glazed surfaces was cut into discs that were used as substrates. A total of 80 specimens were randomly divided into four groups according to the method used: 9.6 % hydrofluoric acid (group 1), 9.6 % hydrofluoric acid (HF) + silane coupling agent (group 2), sandblasting (aluminum trioxide, 50 μm) + silane (group 3), and tribochemical silica coating (CoJet™ sand, 30 μm) + silane (group 4). Brackets were bonded to the treated specimens with a light-cure adhesive (Transbond XT, 3 M Unitek). Shear bond strength was tested after bracket bonding, and the Adhesive Remnant Index (ARI) scores were quantified after debonding. Group 4 showed the highest bond strength (12.3 ± 1.0 MPa), which was not significantly different from that of group 3 (11.6 ± 1.2 MPa, P > 0.05); however, the bond strength of group 4 was substantially higher than that of group 2 (9.4 ± 1.1 MPa, P < 0.05). The shear bond strength of group 1 (3.1 ± 0.6 MPa, P< 0.05) was significantly lower than that of the other groups. Shear bond strengths exceeded the optimal range of ideal bond strength for clinical practice, except for the isolated HF group. HF acid etching followed by silane was the best suited method for bonding on IPS Classic(®). Failure modes in the sandblasting and silica-coating groups revealed signs of damaged ceramic surfaces.

Effect of surface treatments on the bond strength of CAD/CAM fiberglass posts

PubMed Central

Garcia, Paula-Pontes; da Costa, Rogério-Goulart; Garcia, André-Vivan; Gonzaga, Carla-Castiglia; da Cunha, Leonardo-Fernandes; Rezende, Carlos-Eduardo-Edwards

2018-01-01

Background There is no ideal protocol for the surface treatment of fiber posts, especially when using a computer-aided design/computer-aided manufacturing (CAD/CAM) experimental fiberglass block. The purpose of this study was to evaluate the bond strength of a CAD/CAM customized glass fiber post and core after applying different surface treatment techniques. Material and Methods Forty premolars were prepared to receive a customized CAD/CAM glass-fiber post and core obtained from an experimental block of glass fiber and epoxy resin. The specimens were randomly distributed in 4 groups (n=10) according to the post and core surface treatment: ETH - 70% ethanol; HP - 24% hydrogen peroxide for 1 minute; ETH/S - 70% ethanol + silane; HP/S - 24% hydrogen peroxide + silane. The universal adhesive containing silane was applied on the posts and prepared post spaces in all groups. The posts were cemented using dual cure resin cement. The specimens were stored in distilled water at 37°C for 24 h, cut (two slices of 1 mm for each root third - coronal, middle, and apical) and subjected to push-out test (0.5 mm/min). Data was subjected to two-way ANOVA (surface treatment and root third) and Tukey’s test (α=0,05). Results There was no significant difference of bond strength values among groups, regardless the surface treatment (p >0.05). There was significant difference on bond strength values for the different root thirds (p<0.05) (coronal>middle=apical). Conclusions The different surface treatment and application of additional silane in the CAD/CAM customized glass-fiber post and core does not interfere on bond strength values. The root dentin third interfered on the bond strength, with higher values for the coronal third. Key words:Post and core technique, cad/cam, shear strength, hydrogen peroxide. PMID:29930778

Postassembly chemical modification of a highly ordered organosilane multilayer: new insights into the structure, bonding, and dynamics of self-assembling silane monolayers.

PubMed

Wen, Ke; Maoz, Rivka; Cohen, Hagai; Sagiv, Jacob; Gibaud, Alain; Desert, Anne; Ocko, Benjamin M

2008-03-01

Experimental evidence derived from a comprehensive study of a self-assembled organosilane multilayer film system undergoing a process of postassembly chemical modification that affects interlayer-located polar groups of the constituent molecules while preserving its overall molecular architecture allows a quantitative evaluation of both the degree of intralayer polymerization and that of interlayer covalent bonding of the silane headgroups in a highly ordered layer assembly of this type. The investigated system consists of a layer-by-layer assembled multilayer of a bifunctional n-alkyl silane with terminal alcohol group that is in situ converted, via a wet chemical oxidation process conducted on the entire multilayer, to the corresponding carboxylic acid function. A combined chemical-structural analysis of data furnished by four different techniques, Fourier transform infrared spectroscopy (FTIR), synchrotron X-ray scattering, X-ray photoelectron spectroscopy (XPS), and contact angle measurements, demonstrates that the highly ordered 3D molecular arrangement of the initial alcohol-silane multilayer stack is well preserved upon virtually quantitative conversion of the alcohol to carboxylic acid and the concomitant irreversible cleavage of interlayer covalent bonds. Thus, the correlation of quantitative chemical and structural data obtained from such unreacted and fully reacted film samples offers an unprecedented experimental framework within which it becomes possible to differentiate between intralayer and interlayer covalent bonding. In addition, the use of a sufficiently thick multilayer effectively eliminates the interfering contributions of the underlying silicon oxide substrate to both the X-ray scattering and XPS data. The present findings contribute a firm experimental basis to the elucidation of the self-assembly mechanism, the molecular organization, and the modes and dynamics of intra- and interlayer bonding prevailing in highly ordered organosilane films; with further implications for the rational exploitation of some of the unique options such supramolecular surface entities can offer in the advancement of a chemical nanofabrication methodology.

Electrochemical characterization of organosilane-functionalized nanostructured ITO surfaces

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pruna, R., E-mail: rpruna@el.ub.edu; Palacio, F.; López, M.

2016-08-08

The electroactivity of nanostructured indium tin oxide (ITO) has been investigated for its further use in applications such as sensing biological compounds by the analysis of redox active molecules. ITO films were fabricated by using electron beam evaporation at different substrate temperatures and subsequently annealed for promoting their crystallization. The morphology of the deposited material was monitored by scanning electron microscopy, confirming the deposition of either thin films or nanowires, depending on the substrate temperature. Electrochemical surface characterization revealed a 45 % increase in the electroactive surface area of nanostructured ITO with respect to thin films, one third lower than themore » geometrical surface area variation determined by atomic force microscopy. ITO surfaces were functionalized with a model organic molecule known as 6-(ferrocenyl)hexanethiol. The chemical attachment was done by means of a glycidoxy compound containing a reactive epoxy group, the so-called 3-glycidoxypropyltrimethoxy-silane. ITO functionalization was useful for determining the benefits of nanostructuration on the surface coverage of active molecules. Compared to ITO thin films, an increase in the total peak height of 140 % was observed for as-deposited nanostructured electrodes, whereas the same measurement for annealed electrodes resulted in an increase of more than 400 %. These preliminary results demonstrate the ability of nanostructured ITO to increase the surface-to-volume ratio, conductivity and surface area functionalization, features that highly benefit the performance of biosensors.« less

Improving the bioactivity of bioglass/ (PMMA-co-MPMA) organic/inorganic hybrid.

PubMed

Ravarian, R; Wei, H; Dehghani, F

2011-01-01

Binary system of CaO-SiO(2) glasses enables the apatite formation in simulated body fluid (SBF). However, the presence of phosphate content in SiO(2)-CaO-P(2)O(5) glasses leads to the formation of orthophosphate nanocrystalline nuclei, which facilitates the generation of carbonate hydroxyapatite; this compound is more compatible with natural bone. The brittle and less flexible properties of bioactive glasses are the major obstacle for their application as bone implant. The hybridization of essential constituents of bioactive glasses and glass-ceramics with polymers such as PMMA can improve their poor mechanical properties. The aim of this study was to improve the bioactivity of nanocomposites fabricated from poly(methyl metacrylate) (PMMA) and bioglass for bone implant applications. Bioglass compounds with various phosphate contents were used for the preparation of PMMA/bioglass hybrid matrices. Since the lack of adhesion between the two phases impedes the homogenous composite formation, a silane coupling agent such as 3-(trimethoxysilyl)propyl methacrylates (MPMA) was incorporated into the polymer structure. The effect of addition of MPMA on the molecular structure of composite was investigated. Furthermore, the presence of MPMA in the system improved the homogeneity of sample. Increasing phosphate content in the inorganic segment of hybrid up to 10 mol% resulted in the formation of apatite layer on the surface; hence the hybrid was bioactive and suitable candidate for bone tissue engineering.

Cooperative growth phenomena in silicon/germanium low-temperature epitaxy

NASA Astrophysics Data System (ADS)

Meyerson, Bernard S.; Uram, Kevin J.; LeGoues, Francoise K.

1988-12-01

A series of Si:Ge alloys and structures has been prepared by ultrahigh-vacuum chemical vapor deposition. Alloys of composition 0≤Ge/Si≤0.20 are readily deposited at T=550 °C. Commensurate, defect-free strained layers are deposited up to a critical thickness, whereupon the accumulated stress in the films is accommodated by the formation of dislocation networks in the substrate wafers. A cooperative growth phenomenon is observed where the addition of 10% germane to the gaseous deposition source accelerates silane's heterogeneous reaction rate by a factor of 25. A model is proposed where Ge acts as a desorption center for mobile hydrogen adatoms on the Si[100] surface, accelerating heterogeneous silane pyrolysis by the enhanced availability of chemisorption sites.

Solution-Based Synthesis of Crystalline Silicon from Liquid Silane through Laser and Chemical Annealing

DOE PAGES

Iyer, Ganjigunte R. S.; Hobbie, Erik K.; Guruvenket, Srinivasan; ...

2012-05-23

We report a solution process for the synthesis of crystalline silicon from the liquid silane precursor cyclohexasilane (Si 6H 12). Polysilane films were crystallized through thermal and laser annealing, with plasma hydrogenation at atmospheric pressure generating further structural changes in the films. The evolution from amorphous to microcrystalline is characterized using scanning electron microscopy (SEM), atomic force microscopy (AFM), Raman spectroscopy and impedance spectroscopy. A four-decade enhancement in the electrical conductivity is attributed to a disorder-order transition in a bonded Si network. Lastly, our results demonstrate a potentially attractive approach that employs a solution process coupled with ambient post-processing tomore » produce crystalline silicon thin films.« less

Characterization of the modified nickel-zinc ferrite nanoparticles coated with APTES by salinization reaction

NASA Astrophysics Data System (ADS)

Zainal, Israa G.; Al-Shammari, Ahmed Majeed; Kachi, Wjeah

2018-05-01

Surface functionalization of magnetic iron oxide nanoparticles (NPs) is a kind of functional materials, which have been widely used in the biotechnology and catalysis. In this study, Nickel-Zinc ferrite nanoparticles was functionalized with amino propyl triethoxy silane (APTES) by silanization reaction and both non coated and organosilane-coated magnetite characterized by energy-dispersive X-ray spectroscopy (EDX), X-ray diffractometry, Fourier transformed infrared spectroscopy (FTIR) and atomic force microscopy. Basic groups of amino anchored on the external surface of the coated magnetite were observed. Our study procedure nanoparticles which have surface with free - NH2 groups which can carry out ionic interaction with carboxylic groups and act as a carrier of biological molecules, drugs and metals.

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

NASA Astrophysics Data System (ADS)

Shahabi, Shakiba; Treccani, Laura; Rezwan, Kurosch

2016-01-01

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.

Magnetite nanoparticles functionalized with α-tocopheryl succinate (α-TOS) promote selective cervical cancer cell death

NASA Astrophysics Data System (ADS)

Angulo-Molina, Aracely; Méndez-Rojas, Miguel Ángel; Palacios-Hernández, Teresa; Contreras-López, Oscar Edel; Hirata-Flores, Gustavo Alonso; Flores-Alonso, Juan Carlos; Merino-Contreras, Saul; Valenzuela, Olivia; Hernández, Jesús; Reyes-Leyva, Julio

2014-08-01

The vitamin E analog α-tocopheryl succinate (α-TOS) selectively induces apoptosis in several cancer cells, but it is sensitive to esterases present in cervical cancer cells. Magnetite nanoparticles (Nps) were prepared by a reduction-coprecipitation method; their surface was silanized and conjugated to α-TOS to enhance its resistance. Morphology, size, and crystal structure were analyzed by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. Chemical composition was analyzed by energy-dispersive X-ray spectroscopy; functional groups were determined by Fourier transform infrared spectroscopy; and α-TOS content was estimated by thermogravimetric analysis. The cytotoxic activity of α-TOS-Nps was evaluated in non-malignant fibroblasts and cervical cancer cells by means of the colorimetric MTT viability test. Intracellular localization was identified by confocal laser scanning microscopy. Characterization of α-TOS-Nps revealed sphere-like Nps with 15 nm average size, formed by mineral and organic constituents with high stability. α-TOS-Nps were internalized in the nucleus and selectively affected the viability of cervical cancer cells in a dose- and time-dependent manner but were biocompatible with non-malignant fibroblasts. In conclusion, functionalization of magnetite Nps protected the cytotoxic activity of α-TOS in non-sensitive cervical cancer cells.

Effect of γ-aminopropyltriethoxy silane (γ-APS) coupling agent on mechanical and morphological properties of high density polyethylene (HDPE)/acrylonitrile butadiene rubber (NBR)/palm pressed fibre (PPF) composites

NASA Astrophysics Data System (ADS)

Norizan, Nabila Najwa; Santiagoo, Ragunathan; Ismail, Hanafi

2017-07-01

The fabrication of High Density Polyethylene (HDPE)/ Acrylonitrile-butadiene rubber (NBR)/ Palm Pressed Fibre (PPF) composite were investigated. The effect of γ-Aminopropyltriethoxy Silane (APS) as coupling agent on the properties of HDPE/ NBR/ PPF composite were studied. The composites were melt mixed using heated two roll mill at 180°C and speed of 15rpm with six different loading (100/0/10, 80/20/10, 70/30/10, 60/40/10, 50/50/10, and 40/60/10). The effects of γ-APS silane on mechanical, and morphological properties were examined using universal tensile machine (UTM) and scanning electron microscopy (SEM), respectively. Tensile strength and Young's modulus of HDPE/ NBR/ PPF composites decrease with increasing of NBR loading, whilst increasing the elongation at break. However, treated composites have resulted 3% to 29%, and 9% to 19%, higher in tensile strength and young's modulus compared to untreated composites. This was due to the better adhesion between HDPE/ NBR matrices and PPF filler with the presence of silanol moieties. From the morphological study, the micrograph of treated composites has proved the well bonded and good attachment of PPF filler with HDPE/ NBR matrices which resulted to better tensile strength to the HDPE/ NBR/ PPF composites.

Influence of Embedding SMA Fibres and SMA Fibre Surface Modification on the Mechanical Performance of BFRP Composite Laminates

PubMed Central

Liu, Yanfei; Wang, Zhenqing; Li, Hao; Sun, Min; Wang, Fangxin; Chen, Bingjie

2018-01-01

In this paper, a new shape memory alloy (SMA) hybrid basalt fibre reinforced polymer (BFRP) composite laminate was fabricated and a new surface modification method with both silane coupling agent KH550 and Al2O3 nanoparticles was conducted to enhance the interface performance. The mechanical performance of BFRP composite laminates with and without SMA fibres and the influence of SMA surface modification were studied in this paper. Different SMA fibre surface treatment methods, including etching with both H2SO4 and NaOH, modification with the silane coupling agent KH550 and new modification method with both KH550 and Al2O3 nanoparticles, were conducted to enhance the bonding between the SMA fibres and polymer matrix. Scanning electron microscopy (SEM) was used to observe the micromorphology of the SMA fibre surfaces exposed to different treatments and the damage morphology of composite laminates. The mechanical performance of the composites was investigated with tensile, three-point bending and low-velocity impact tests to study the influence of embedded SMA fibres and the different surface modifications of the SMA fibres. The results demonstrated that the embedded Ni-Ti SMA fibres can significantly enhance the mechanical performance of BFRP composite laminates. SMA fibres modified with both the silane coupling agent KH550 and Al2O3 nanoparticles illustrate the best mechanical performance among all samples. PMID:29300321

Study of thermal stability of (3-aminopropyl)trimethoxy silane-grafted titanate nanotubes for application as nanofillers in polymers.

PubMed

Plodinec, Milivoj; Gajović, Andreja; Iveković, Damir; Tomašić, Nenad; Zimmermann, Boris; Macan, Jelena; Haramina, Tatjana; Su, D S; Willinger, Marc

2014-10-31

Protonated titanate nanotubes (TiNT-H) were surface-modified with (3-aminopropyl)trimethoxy silane (APTMS) by a novel method suitable for the syntheses of large amounts of materials at a low cost. The usage of prepared nanotubes for polymer reinforcement was studied. Since the thermal stability of the nanofiller was important to preserve its functional properties, its stability was studied by in situ high-temperature measurements. The most thermally stable nanotubes were silanized for 20 min and used for the preparation of epoxy-based nanocomposites. The nanofiller formed smaller (a few hundred nm) and larger (a few μm) aggregates in the polymer matrix, and the amount of aggregates increased as the nanofiller content increased. The APTMS-modified titanate nanotubes bonded well with the epoxy matrix since amine groups on the TiNT's surface can react with an epoxy group to form covalent bonds between the matrix and the nanofiller. A very small addition (0.19-1.52 wt%) of the nanotubes significantly increased the glass transition temperature and the modulus in the rubbery state of the epoxy-based polymer. Smaller nanofiller content leads to a larger increase in these parameters and therefore better dynamic mechanical properties due to the smaller amount of large aggregates. APTMS-modified titanate nanotubes have proven to be a promising nanofiller in epoxy-based nanocomposites.

The Effect of Different Coupling Agents on Nano-ZnO Materials Obtained via the Sol-Gel Process.

PubMed

Purcar, Violeta; Şomoghi, Raluca; Niţu, Sabina Georgiana; Nicolae, Cristian-Andi; Alexandrescu, Elvira; Gîfu, Ioana Cătălina; Gabor, Augusta Raluca; Stroescu, Hermine; Ianchiş, Raluca; Căprărescu, Simona; Cinteză, Ludmila Otilia

2017-12-12

Hybrid nanomaterials based on zinc oxide were synthesized via the sol-gel method, using different silane coupling agents: (3-glycidyloxypropyl)trimethoxysilane (GPTMS), phenyltriethoxysilane (PhTES), octyltriethoxysilane (OTES), and octadecyltriethoxysilane (ODTES). Morphological properties and the silane precursor type effect on the particle size were investigated using dynamic light scattering (DLS), environmental scanning electron microscopy (ESEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). The bonding characteristics of modified ZnO materials were investigated using Fourier transform infrared spectroscopy (FTIR). The final solutions were deposited on metallic substrate (aluminum) in order to realize coatings with various wettability and roughness. The morphological studies, obtained by ESEM and TEM analysis, showed that the sizes of the ZnO nanoparticles are changed as function of silane precursor used in synthesis. The thermal stability of modified ZnO materials showed that the degradation of the alkyl groups takes place in the 300-500 °C range. Water wettability study revealed a contact angle of 142 ± 5° for the surface covered with ZnO material modified with ODTES and showed that the water contact angle increases as the alkyl chain from the silica precursor increases. These modified ZnO materials, therefore, can be easily incorporated in coatings for various applications such as anti-corrosion and anti-icing.

Tensile strength of glass fiber posts submitted to different surface treatments.

PubMed

Faria, Maria Isabel A; Gomes, Érica Alves; Messias, Danielle Cristine; Silva Filho, João Manoel; Souza Filho, Celso Bernardo; Paulino, Silvana Maria

2013-01-01

The aim of this in vitro study was to evaluate the tensile strength of glass fiber posts submitted to different surface treatments. Forty-eight maxillary canines had their crowns sectioned and root canals endodontically treated. The roots were embedded in acrylic resin and distributed into 3 groups according to the surface treatment: Group I: the posts were treated with silane agent for 30 s and adhesive; Group II: the posts were cleaned with alcohol before treatment with silane agent and adhesive; Group III: the posts were submitted to conditioning with 37% phosphoric acid for 30 s before treatment with silane agent and adhesive. Each group was divided into 2 subgroups for adhesive polymerization or not before insertion into the canal: A - adhesive was not light cured and B - adhesive was light cured. All posts were cemented with Panavia F and the samples were subjected to tensile strength test in a universal testing machine at crosshead speed of 1 mm/min. Data were submitted to one-way ANOVA and Tukey's test at 5% significance level. There was statistically significant difference (p<0.01) only between group GIII-B and groups GI-A and GI-B. No significant difference was found among the other groups (p>0.05). It was concluded that the products used for cleaning the posts influenced the retention regardless of adhesive light curing.

Rapid bonding of polydimethylsiloxane (PDMS) to various stereolithographically (STL) structurable epoxy resins using photochemically cross-linked intermediary siloxane layers

NASA Astrophysics Data System (ADS)

Wilhelm, Elisabeth; Neumann, Christiane; Sachsenheimer, Kai; Länge, Kerstin; Rapp, Bastian E.

2014-03-01

In this paper we present a fast, low cost bonding technology for combining rigid epoxy components with soft membranes made out of polydimethylsiloxane (PDMS). Both materials are commonly used for microfluidic prototyping. Epoxy resins are often applied when rigid channels are required, that will not deform if exposed to high pressure. PDMS, on the other hand, is a flexible material, which allows integration of membrane valves on the chip. However, the integration of pressure driven components, such as membrane valves and pumps, into a completely flexible device leads to pressure losses. In order to build up pressure driven components with maximum energy efficiency a combination of rigid guiding channels and flexible membranes would be advisable. Stereolithographic (STL) structuring would be an ideal fabrication technique for this purpose, because complex 3D-channels structures can easily be fabricated using this technology. Unfortunately, the STL epoxies cannot be bonded using common bonding techniques. For this reason we propose two UV-light based silanization techniques that enable plasma induced bonding of epoxy components. The entire process including silanization and corona discharge bonding can be carried out within half an hour. Average bond strengths up to 350 kPa (depending on the silane) were determined in ISO-conform tensile testing. The applicability of both techniques for microfluidic applications was proven by hydrolytic stability testing lasting more than 40 hours.