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.

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.

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.

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.

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

Influence of airborne-particle abrasion on mechanical properties and bond strength of carbon/epoxy and glass/bis-GMA fiber-reinforced resin posts.

PubMed

Soares, Carlos Jose; Santana, Fernanda Ribeiro; Pereira, Janaina Carla; Araujo, Tatiana Santos; Menezes, Murilo Souza

2008-06-01

Controversy exists concerning the use of fiber-reinforced posts to improve bond strength to resin cement because some precementation treatments can compromise the mechanical properties of the posts. The purpose of this study was to analyze the influence of airborne-particle abrasion on the mechanical properties and microtensile bond strength (MTBS) of carbon/epoxy and glass/bis-GMA fiber-reinforced resin posts. Flexural strength (delta(f)), flexural modulus (E(f)), and stiffness (S) were assessed using a 3-point bending test for glass fiber-reinforced and carbon fiber-reinforced resin posts submitted to airborne-particle abrasion (AB) with 50-microm Al(2)O(3), and for posts without any surface treatment (controls) (n=10). Forty glass fiber (GF) and 40 carbon fiber (CF) posts were submitted to 1 of 4 surface treatments (n=10) prior to MTBS testing: silane (S); silane and adhesive (SA); airborne-particle abrasion with 50-microm Al(2)O(3) and silane (ABS); airborne-particle abrasion, silane, and adhesive (ABSA). Two composite resin restorations (Filtek Z250) with rounded depressions in the lateral face were bilaterally fixed to the post with resin cement (RelyX ARC). Next, the specimen was sectioned with a precision saw running perpendicular to the bonded surface to obtain 10 bonded beam specimens with a cross-sectional area of 1 mm(2). Each beam specimen was tested in a mechanical testing machine (EMIC 2,000 DL), under stress, at a crosshead speed of 0.5 mm/min until failure. Data were analyzed by 2-way ANOVA followed by Tukey HSD test (alpha=.05). Failure patterns of tested specimens were analyzed using scanning electron microscopy (SEM). The 3-point bending test demonstrated significant differences among groups only for the post type factor for flexural strength, flexural modulus, and stiffness. The carbon fiber posts exhibited significantly higher mean flexural strength (P=.001), flexural modulus (P=.003), and stiffness (P=.001) values when compared with glass fiber posts, irrespective of surface treatment. An alteration in the superficial structure of the posts could be observed by SEM after airborne-particle abrasion. MTBS testing showed no significant effect for the surface treatment type; however, significant effects for post system factor and for interaction between the 2 factors were observed. For the carbon fiber post, the ABSA surface treatment resulted in values significantly lower than the S surface treatment. SEM analysis of MTBS-tested specimens demonstrated adhesive and cohesive failures. Airborne-particle abrasion did not influence the mechanical properties of the post; however, it produced undesirable surface changes, which could reduce the bond strength to resin cement. For the surface treatments studied, if silane is applied, the adhesive system and airborne-particle abrasion are not necessary.

Method for chemical surface modification of fumed silica particles

DOEpatents

Grabbe, Alexis; Michalske, Terry Arthur; Smith, William Larry

1999-01-01

Dehydroxylated, silica-containing, glass surfaces are known to be at least partially terminated by strained siloxane rings. According to the invention, a surface of this kind is exposed to a selected silane compound or mixture of silane compounds under reaction-promoting conditions. The ensuing reaction results in opening of the strained siloxane rings, and termination of surface atoms by chemical species, such as organic or organosilicon species, having desirable properties. These species can be chosen to provide qualities such as hydrophobicity, or improved coupling to a polymeric coating.

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.

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

PubMed

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

2011-03-01

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

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.

Characterization of Biofouling Marine Caulobacters and Their Adhesive Holdfast

DTIC Science & Technology

1988-06-30

SAD-A 197 211 _, 111 3 CEILL GJU JREPORT DOCUMENTATION PAGE la. REPORT SECURITY CLASSIFiCATION ’b RESTRICTIVE MARKIN6, S U 1 2a. SECURITY...what types of surfaces to which the Caulobacters will attach. This was approached by the preparation of glass surfaces covalently modified with a...finding that dimethyldichlorosilane treated glass (ie classical "silanizing") was reasonably effective in discouraging attachment, a convenience for many

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).

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.

Modifying glass fiber surface with grafting acrylamide by UV-grafting copolymerization for preparation of glass fiber reinforced PVDF composite membrane.

PubMed

Luo, Nan; Zhong, Hui; Yang, Min; Yuan, Xing; Fan, Yaobo

2016-01-01

Experimental design and response surface methodology (RSM) were used to optimize the modification of conditions for glass surface grafting with acrylamide (AM) monomer for preparation of a glass fiber reinforced poly(vinylidene fluoride) (PVDF) composite membrane (GFRP-CM). The factors considered for experimental design were the UV (ultraviolet)-irradiation time, the concentrations of the initiator and solvent, and the kinds and concentrations of the silane coupling agent. The optimum operating conditions determined were UV-irradiation time of 25 min, an initiator concentration of 0-0.25 wt.%, solvent of N-Dimethylacetamide (DMAC), and silane coupling agent KH570 with a concentration of 7 wt.%. The obtained optimal parameters were located in the valid region and the experimental confirmation tests conducted showed good accordance between predicted and experimental values. Under these optimal conditions, the water absorption of the grafted modified glass fiber was improved from 13.6% to 23%; the tensile strength was enhanced and the peeling strength of the glass fiber reinforced PVDF composite membrane was improved by 23.7% and 32.6% with an AM concentration at 1 wt.% and 2 wt.%. The surface composition and microstructure of AM grafted glass fiber were studied via several techniques including Field Emission Scanning Electron Microscopy (FESEM), Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR) and energy dispersive X-ray spectroscopy (EDX). The analysis of the EDX and FTIR-ATR results confirmed that the AM was grafted to the glass fiber successfully by detecting and proving the existence of nitrogen atoms in the GFRP-CM. Copyright © 2015. Published by Elsevier B.V.

Influence of Surface Conditioning Protocols on Reparability of CAD/CAM Zirconia-reinforced Lithium Silicate Ceramic.

PubMed

Al-Thagafi, Rana; Al-Zordk, Walid; Saker, Samah

2016-01-01

To test the effect of surface conditioning protocols on the reparability of CAD/CAM zirconia-reinforced lithium silicate ceramic compared to lithium-disilicate glass ceramic. Zirconia-reinforced lithium silicate ceramic (Vita Suprinity) and lithium disilicate glass-ceramic blocks (IPS e.max CAD) were categorized into four groups based on the surface conditioning protocol used. Group C: no treatment (control); group HF: 5% hydrofluoric acid etching for 60 s, silane (Monobond-S) application for 60 s, air drying; group HF-H: 5% HF acid etching for 60 s, application of silane for 60 s, air drying, application of Heliobond, light curing for 20 s; group CO: sandblasting with CoJet sand followed by silanization. Composite resin (Tetric EvoCeram) was built up into 4 x 6 x 3 mm blocks using teflon molds. All specimens were subjected to thermocycling (5000x, 5°C to 55°C). The microtensile bond strength test was employed at a crosshead speed of 1 mm/min. SEM was employed for evaluation of all the debonded microbars, the failure type was categorized as either adhesive (failure at adhesive layer), cohesive (failure at ceramic or composite resin), or mixed (failure between adhesive layer and substrate). Two-way ANOVA and the Tukey's HSD post-hoc test were applied to test for significant differences in bond strength values in relation to different materials and surface pretreatment (p < 0.05). The highest microtensile repair bond strength for Vita Suprinity was reported in group CO (33.1 ± 2.4 MPa) and the lowest in group HF (27.4 ± 4.4 MPa). Regarding IPS e.max CAD, group CO showed the highest (30.5 ± 4.9 MPa) and HF the lowest microtensile bond strength (22.4 ± 5.7 MPa). Groups HF, HF-H, and CO showed statistically significant differences in terms of all ceramic types used (p < 0.05). The control group showed exclusively adhesive failures, while in HF, HF-H, and CO groups, mixed failures were predominant. Repair bond strength to zirconia-reinforced lithium silicate ceramics and lithium-disilicate glass ceramic could be improved when ceramic surfaces are sandblasted with CoJet sand followed by silanization.

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.

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.

The effect of surface modification of glass fiber on the performance of poly(lactic acid) composites: Graphene oxide vs. silane coupling agents

NASA Astrophysics Data System (ADS)

Jing, Mengfan; Che, Junjin; Xu, Shuman; Liu, Zhenwei; Fu, Qiang

2018-03-01

In this work, a comparison study was carried out to investigate the efficacy of glass fiber (GF) in reinforcing poly(lactic acid) (PLA) by using traditional silane coupling agents (GF-S) and novel graphene oxide (GF-GO) as surface modifiers. The crystallization behavior of the PLA matrix was investigated by differential scanning calorimetry. The mechanical performances and the thermomechanical properties of the composites were evaluated by uniaxial tensile testing and dynamic mechanical analysis, respectively. For neat GF without any treatment, the poor interfacial adhesion and the sharp shortening of the GF length result in the relatively poor mechanical performances of PLA/GF composites. However, the incorporation of GF-S significantly improves the mechanical strength and keeps relatively good toughness of the composites, while GF-GO exhibits excellent nucleation ability for PLA and could moderately increase the modulus of the composites. The thermomechanical properties of the composites are improved markedly resulting from the crystallinity increase. The different surface modification of glass fiber influences the crystallinity of matrix, the interfacial interaction and the length of fiber, which altogether affect the mechanical performances of the prepared PLA/GF composites.

Improvement in the amine glass platform by bubbling method for a DNA microarray

PubMed Central

Jee, Seung Hyun; Kim, Jong Won; Lee, Ji Hyeong; Yoon, Young Soo

2015-01-01

A glass platform with high sensitivity for sexually transmitted diseases microarray is described here. An amino-silane-based self-assembled monolayer was coated on the surface of a glass platform using a novel bubbling method. The optimized surface of the glass platform had highly uniform surface modifications using this method, as well as improved hybridization properties with capture probes in the DNA microarray. On the basis of these results, the improved glass platform serves as a highly reliable and optimal material for the DNA microarray. Moreover, in this study, we demonstrated that our glass platform, manufactured by utilizing the bubbling method, had higher uniformity, shorter processing time, lower background signal, and higher spot signal than the platforms manufactured by the general dipping method. The DNA microarray manufactured with a glass platform prepared using bubbling method can be used as a clinical diagnostic tool. PMID:26468293

Improvement in the amine glass platform by bubbling method for a DNA microarray.

PubMed

Jee, Seung Hyun; Kim, Jong Won; Lee, Ji Hyeong; Yoon, Young Soo

2015-01-01

A glass platform with high sensitivity for sexually transmitted diseases microarray is described here. An amino-silane-based self-assembled monolayer was coated on the surface of a glass platform using a novel bubbling method. The optimized surface of the glass platform had highly uniform surface modifications using this method, as well as improved hybridization properties with capture probes in the DNA microarray. On the basis of these results, the improved glass platform serves as a highly reliable and optimal material for the DNA microarray. Moreover, in this study, we demonstrated that our glass platform, manufactured by utilizing the bubbling method, had higher uniformity, shorter processing time, lower background signal, and higher spot signal than the platforms manufactured by the general dipping method. The DNA microarray manufactured with a glass platform prepared using bubbling method can be used as a clinical diagnostic tool.

Fractography and Mechanical Properties of Urethane Dimethacrylate Dental Composites Reinforced with Glass Nanoparticles.

PubMed

M, Monfared; Me, Bahrololoom

2016-12-01

Dental resin composites are becoming prevalent in restorative dentistry and have almost replaced amalgam nowadays. Consequently, their mechanical properties and durability are critical. The aim of this study was to produce Pyrex glass nano-particles by wet milling process and use them as reinforcement in dental resins for anterior restorations and then examination of fractographic properties of these composites. The glass nano-particles were achieved via wet milling. The surface of the particles was modified with 3-(Trimethoxysilyl) propyl methacrylate (γ-MPTMS) silane in order to improve their surface. Fourier transform infra-red (FTIR) analysis showed that the silane groups provided double bonds to the surface of the particles and prevented agglomeration. Then, the composite resins were made with different weight percentages of Pyrex glass. The mechanical properties of samples flexural test were evaluated. The required energy for fracture of the specimens was achieved via this test. The fracture surfaces of the samples were analyzed using a scanning electron microscope (SEM) in order to explain the mechanisms of fracture. The results and analysis showed that increasing the glass nano-particles mass fraction had a great effect on mechanical properties of the composites due to the mechanisms of crack propagation and crack deflection as well as preventing void formation. The effective energy dissipation mechanisms such as crack pinning and deflection, was observed in SEM micrographs. Void formation in the low filler content composite is one of the mechanisms to decrease the energy required for fracture of these composites and eventually weaken them.

Fractography and Mechanical Properties of Urethane Dimethacrylate Dental Composites Reinforced with Glass Nanoparticles

PubMed Central

M*, Monfared; ME, Bahrololoom

2016-01-01

Statement of Problem: Dental resin composites are becoming prevalent in restorative dentistry and have almost replaced amalgam nowadays. Consequently, their mechanical properties and durability are critical. Objectives: The aim of this study was to produce Pyrex glass nano-particles by wet milling process and use them as reinforcement in dental resins for anterior restorations and then examination of fractographic properties of these composites. Materials and Methods: The glass nano-particles were achieved via wet milling. The surface of the particles was modified with 3-(Trimethoxysilyl) propyl methacrylate (γ-MPTMS) silane in order to improve their surface. Fourier transform infra-red (FTIR) analysis showed that the silane groups provided double bonds to the surface of the particles and prevented agglomeration. Then, the composite resins were made with different weight percentages of Pyrex glass. The mechanical properties of samples flexural test were evaluated. The required energy for fracture of the specimens was achieved via this test. The fracture surfaces of the samples were analyzed using a scanning electron microscope (SEM) in order to explain the mechanisms of fracture. Results: The results and analysis showed that increasing the glass nano-particles mass fraction had a great effect on mechanical properties of the composites due to the mechanisms of crack propagation and crack deflection as well as preventing void formation. The effective energy dissipation mechanisms such as crack pinning and deflection, was observed in SEM micrographs. Conclusions: Void formation in the low filler content composite is one of the mechanisms to decrease the energy required for fracture of these composites and eventually weaken them. PMID:28959761

Self-organization of gold nanoparticles on silanated surfaces.

PubMed

Kyaw, Htet H; Al-Harthi, Salim H; Sellai, Azzouz; Dutta, Joydeep

2015-01-01

The self-organization of monolayer gold nanoparticles (AuNPs) on 3-aminopropyltriethoxysilane (APTES)-functionalized glass substrate is reported. The orientation of APTES molecules on glass substrates plays an important role in the interaction between AuNPs and APTES molecules on the glass substrates. Different orientations of APTES affect the self-organization of AuNps on APTES-functionalized glass substrates. The as grown monolayers and films annealed in ultrahigh vacuum and air (600 °C) were studied by water contact angle measurements, atomic force microscopy, X-ray photoelectron spectroscopy, UV-visible spectroscopy and ultraviolet photoelectron spectroscopy. Results of this study are fundamentally important and also can be applied for designing and modelling of surface plasmon resonance based sensor applications.

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.

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.

Interfacial fracture toughness of different resin cements bonded to a lithium disilicate glass ceramic.

PubMed

Hooshmand, Tabassom; Rostami, Golriz; Behroozibakhsh, Marjan; Fatemi, Mostafa; Keshvad, Alireza; van Noort, Richard

2012-02-01

To evaluate the effect of HF acid etching and silane treatment on the interfacial fracture toughness of a self-adhesive and two conventional resin-based cements bonded to a lithium disilicate glass ceramic. Lithium disilicate glass ceramic discs were prepared with two different surface preparations consisting of gritblasted with aluminium oxide, and gritblasted and etched with hydrofluoric acid. Ceramic surfaces with a chevron shaped circular hole were treated by an optimized silane treatment followed by an unfilled resin and then three different resin cements (Variolink II, Panavia F2, and Multilink Sprint). Specimens were kept in distilled water at 37°C for 24h and then subjected to thermocycling. The interfacial fracture toughness was measured and mode of failures was also examined. Data were analysed using analysis of variance followed by T-test analysis. No statistically significant difference in the mean fracture toughness values between the gritblasted and gritblasted and etched surfaces for Variolink II resin cement was found (P>0.05). For the gritblasted ceramic surfaces, no significant difference in the mean fracture toughness values between Panavia F2 and Variolink II was observed (P>0.05). For the gritblasted and etched ceramic surfaces, a significantly higher fracture toughness for Panavia F2 than the other cements was found (P<0.05). The interfacial fracture toughness for the lithium disilicate glass ceramic system was affected by the surface treatment and the type of luting agent. Dual-cured resin cements demonstrated a better bonding efficacy to the lithium disilicate glass ceramic compared to the self-adhesive resin cement. The lithium disilicate glass ceramic surfaces should be gritblasted and etched to get the best bond when used with Panavia F2 and Multilink Sprint resin cements, whereas for the Variolink II only gritblasting is required. The best bond overall is achieved with Panavia F2. Copyright © 2011 Elsevier Ltd. All rights reserved.

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

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

Mobility restrictions and glass transition behaviour of an epoxy resin under confinement.

PubMed

Djemour, A; Sanctuary, R; Baller, J

2015-04-07

Confinement can have a big influence on the dynamics of glass formers in the vicinity of the glass transition. Already 40 to 50 K above the glass transition temperature, thermal equilibration of glass formers can be strongly influenced by the confining substrate. We investigate the linear thermal expansion and the specific heat capacity cp of an epoxy resin (diglycidyl ether of bisphenol A, DGEBA) in a temperature interval of 120 K around the glass transition temperature. The epoxy resin is filled into controlled pore glasses with pore diameters between 4 and 111 nm. Since DGEBA can form H-bonds with silica surfaces, we also investigate the influence of surface silanization of the porous substrates. In untreated substrates a core/shell structure of the epoxy resin can be identified. The glass transition behaviours of the bulk phase and that of the shell phase are different. In silanized substrates, the shell phase disappears. At a temperature well above the glass transition, a second transition is found for the bulk phase - both in the linear expansion data as well as in the specific heat capacity. The cp data do not allow excluding the glass transition of a third phase as being the cause for this transition, whereas the linear expansion data do so. The additional transition temperature is interpreted as a separation between two regimes: above this temperature, macroscopic flow of the bulk phase inside the porous structure is possible to balance the mismatch of thermal expansion coefficients between DGEBA and the substrate. Below the transition temperature, this degree of freedom is hindered by geometrical constraints of the porous substrates. Moreover, this second transition could also be found in the linear expansion data of the shell phase.

Biofilm formation affects surface properties of novel bioactive glass-containing composites.

PubMed

Hyun, Hong-Keun; Salehi, Satin; Ferracane, Jack L

2015-12-01

This study investigated the effects of bacterial biofilm on the surface properties of novel bioactive glass (BAG)-containing composites of different initial surface roughness. BAG (65 mol% Si; 4% P; 31% Ca) and BAG-F (61% Si; 31% Ca; 4% P; 3% F; 1% B) were synthesized by the sol-gel method and micronized (size ∼0.1-10 μm). Composites with 72wt% total filler load were prepared by replacing 15% of the silanized Sr glass with BAG, BAG-F, or silanized silica. Specimens (n=10/group) were light-cured and divided into 4 subgroups of different surface roughness by wet polishing with 600 and then up to 1200, 2400, or 4000 grit SiC. Surface roughness (SR), gloss, and Knoop microhardness were measured before and after incubating in media with or without a Streptococcus mutans (UA 159) biofilm for 2 weeks. Results were analyzed with ANOVA/Tukey's test (α=0.05). The SR of the BAG-containing composites with the smoothest surfaces (2400/4000 grit) increased in media or bacteria; the SR of the roughest composites (600 grit) decreased. The gloss of the smoothest BAG-containing composites decreased in bacteria and media-only, but more in media-alone. The microhardness of all of the composites decreased with exposure to media or bacteria, with BAG-containing composites affected more than the control. Exposure to bacterial biofilm and its media produced enhanced roughness and reduced gloss and surface microhardness of highly polished dental composites containing a bioactive glass additive, which could affect further biofilm formation, as well as the esthetics, of restorations made from such a material. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

Self-organization of gold nanoparticles on silanated surfaces

PubMed Central

Kyaw, Htet H; Sellai, Azzouz; Dutta, Joydeep

2015-01-01

Summary The self-organization of monolayer gold nanoparticles (AuNPs) on 3-aminopropyltriethoxysilane (APTES)-functionalized glass substrate is reported. The orientation of APTES molecules on glass substrates plays an important role in the interaction between AuNPs and APTES molecules on the glass substrates. Different orientations of APTES affect the self-organization of AuNps on APTES-functionalized glass substrates. The as grown monolayers and films annealed in ultrahigh vacuum and air (600 °C) were studied by water contact angle measurements, atomic force microscopy, X-ray photoelectron spectroscopy, UV–visible spectroscopy and ultraviolet photoelectron spectroscopy. Results of this study are fundamentally important and also can be applied for designing and modelling of surface plasmon resonance based sensor applications. PMID:26734526

Processing and properties of ceramic matrix-polymer composites for dental applications

NASA Astrophysics Data System (ADS)

Huang, Hsuan Yao

The basic composite structure of natural hard tissue was used to guide the design and processing of dental restorative materials. The design incorporates the methodology of using inorganic minerals as the main structural phase reinforced with a more ductile but tougher organic phase. Ceramic-polymer composites were prepared by slip casting a porous ceramic structure, heating and chemical treating the porous preform, infiltrating with monomer and then curing. The three factors that determined the mechanical properties of alumina-polymer composites were the type of polymer used, the method of silane treatments, and the type of bond between particles in the porous preforms. Without the use of silane coupling agents, the composites were measured to have a lower strength. The composite with a more "flexible" porous alumina network had a greater ability to plastically dissipate the energy of propagating cracks. However, the aggressive nature of the alumina particles on opposing enamel requires that these alumina-polymer composites have a wear compatible coating for practical application. A route to dense bioactive apatite wollastonite glass ceramics (AWGC)-polymer composites was developed. The problems associated with glass dissolution into the aqueous medium for slip casting were overcome with the use of silane. The role of heating rate and development of ceramic compact microstructure on composite properties was explored. In general, if isothermal heating was not applied, decreasing heating rate increased glass crystallinity and particle-particle fusion, but decreased pore volume. Also composite strength and fracture toughness decreased while modulus and hardness increased with decreasing heating rate. If isothermal heating was applied, glass crystallinity, pore content, and composite mechanical properties showed relatively little change regardless of the initial heating rate. The potential of AWGC-polymer composites for dental and implant applications was explored. Strengths and toughnesses were not severely degraded by immersion in simulated body fluids up to 30 days. The composite elastic modulus approached that of hard tissues and its wear behavior with opposing tooth was excellent. Growth of apatite over the entire composite surface was achieved in SBF. Growth of apatite in human whole saliva was achieved on the bioactive glass surface, but not on the composite surface.

Ceramic Surface Treatment with a Single-component Primer: Resin Adhesion to Glass Ceramics.

PubMed

Prado, Mayara; Prochnow, Catina; Marchionatti, Ana Maria Estivalete; Baldissara, Paolo; Valandro, Luiz Felipe; Wandscher, Vinicius Felipe

2018-04-19

To evaluate the microshear bond strength (μSBS) of composite cement bonded to two machined glass ceramics and its durability, comparing conventional surface conditioning (hydrofluoric acid + silane) to a one-step primer (Monobond Etch & Prime). Machined slices of lithium disilicate ceramic (LDC) (IPS e.max CAD) and feldspathic ceramic (FC) (VITA Mark II) glass ceramics were divided into two groups (n = 10) according to two factors: 1. surface treatment: HF+S (ca 5% hydrofluoric acid [IPS Ceramic Etching GEL] + silane coupling agent [SIL; Monobond Plus]) or MEP (single-component ceramic conditioner; Monobond Etch & Prime); 2. storage condition: baseline (without aging; tested 24 h after cementing) or aged (70 days of water storage + 12,000 thermal cycles). Composite cement (Multilink Automix, Ivoclar Vivadent) was applied to starch matrices on the treated ceramic surfaces and photoactivated. A μSBS test was performed (0.5 mm/min) and the failure pattern was determined. Contact angle and micromorphological analyses were also performed. Data were analyzed with Student's t-test (α = 5%). For both ceramic materials, HF+S resulted in higher mean μSBS (MPa) at baseline (LDC: HF+S 21.2 ± 2.2 > MEP 10.4 ± 2.4; FC: HF+S 19.6 ± 4.3 > MEP 13.5 ± 5.4) and after aging (LDC: HF+S 14.64 ± 2.31 > MEP 9 ± 3.4; FC HF+S: 14.73 ± 3.33 > MEP 11.1 ± 3.3). HF+S resulted in a statistically significant decrease in mean μSBS after aging (p = 0.0001), while MEP yielded no significant reduction. The main failure type was adhesive between composite cement and ceramic. HF+S resuted in the lowest contact angle. Hydrofluoric acid + silane resulted in higher mean μSBS than Monobond Etch & Prime for both ceramics; however, Monobond Etch & Prime had stable bonding after aging.

An improved method for constructing and selectively silanizing double-barreled, neutral liquid-carrier, ion-selective microelectrodes

PubMed Central

Deveau, Jason S.T.; Grodzinski, Bernard

2005-01-01

We describe an improved, efficient and reliable method for the vapour-phase silanization of multi-barreled, ion-selective microelectrodes of which the silanized barrel(s) are to be filled with neutral liquid ion-exchanger (LIX). The technique employs a metal manifold to exclusively and simultaneously deliver dimethyldichlorosilane to only the ion-selective barrels of several multi-barreled microelectrodes. Compared to previously published methods the technique requires fewer procedural steps, less handling of individual microelectrodes, improved reproducibility of silanization of the selected microelectrode barrels and employs standard borosilicate tubing rather than the less-conventional theta-type glass. The electrodes remain stable for up to 3 weeks after the silanization procedure. The efficacy of a double-barreled electrode containing a proton ionophore in the ion-selective barrel is demonstrated in situ in the leaf apoplasm of pea (Pisum) and sunflower (Helianthus). Individual leaves were penetrated to depth of ~150 μm through the abaxial surface. Microelectrode readings remained stable after multiple impalements without the need for a stabilizing PVC matrix. PMID:16136222

Adhesion mapping of chemically modified and poly(ethylene oxide)-grafted glass surfaces.

PubMed

Jogikalmath, G; Stuart, J K; Pungor, A; Hlady, V

1999-08-01

Two-dimensional mapping of the adhesion pull-off forces was used to study the origin of surface heterogeneity in the grafted poly(ethylene oxide) (PEO) layer. The variance of the pull-off forces measured over the μm-sized regions after each chemical step of modifying glass surfaces was taken to be a measure of the surface chemical heterogeneity. The attachment of γ-glycidoxypropyltrimethoxy silane (GPS) to glass decreased the pull-off forces relative to the clean glass and made the surface more uniform. The subsequent hydrolysis of the terminal epoxide groups resulted in a larger surface heterogeneity which was modeled by two populations of the terminal hydroxyl groups, each with its own distribution of adhesion forces and force variance. The activation of the hydroxyls with carbonyldiimmidazole (CDI) healed the surface and lowered its adhesion, however, the force variance remained rather large. Finally, the grafting of the α,ω-diamino poly(ethyleneoxide) chains to the CDI-activated glass largely eliminated adhesion except at a few discrete regions. The adhesion on the PEO grafted layer followed the Poisson distribution of the pull-off forces. With the exception of the glass surface, a correlation between the water contact angles and the mean pull-off forces measured with the Si(3)N(4) tip surfaces was found for all modified glass surfaces.

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.

Hydraulic transport across hydrophilic and hydrophobic nanopores: Flow experiments with water and n-hexane.

PubMed

Gruener, Simon; Wallacher, Dirk; Greulich, Stefanie; Busch, Mark; Huber, Patrick

2016-01-01

We experimentally explore pressure-driven flow of water and n-hexane across nanoporous silica (Vycor glass monoliths with 7- or 10-nm pore diameters, respectively) as a function of temperature and surface functionalization (native and silanized glass surfaces). Hydraulic flow rates are measured by applying hydrostatic pressures via inert gases (argon and helium, pressurized up to 70 bar) on the upstream side in a capacitor-based membrane permeability setup. For the native, hydrophilic silica walls, the measured hydraulic permeabilities can be quantitatively accounted for by bulk fluidity provided we assume a sticking boundary layer, i.e., a negative velocity slip length of molecular dimensions. The thickness of this boundary layer is discussed with regard to previous capillarity-driven flow experiments (spontaneous imbibition) and with regard to velocity slippage at the pore walls resulting from dissolved gas. Water flow across the silanized, hydrophobic nanopores is blocked up to a hydrostatic pressure of at least 70 bar. The absence of a sticking boundary layer quantitatively accounts for an enhanced n-hexane permeability in the hydrophobic compared to the hydrophilic nanopores.

Role of surface properties in bacterial attachment

NASA Astrophysics Data System (ADS)

Conrad, Jacinta; Sharma, Sumedha

2014-03-01

Bacterial biofilms foul a wide range of engineered surfaces, from pipelines to membranes to biomedical implants, and lead to deleterious costs for industry and for human health. Designing strategies to reduce bacterial fouling requires fundamental understanding of mechanisms by which bacteria attach to surfaces. We investigate the attachment of Escherichia coli on silanized glass surfaces during flow through a linear channel at flow rates of 0.1-1 mL/min using confocal microscopy. We deposit self-assembled monolayers of organosilanes on glass and track the position and orientation of bacteria deposited on these surfaces during flow using high-throughput image processing algorithms. Here, we report differences in deposition rate and surface-tethered motion of cells as a function of surface charge and surface energy, suggesting that attachment of bacteria on these engineered surfaces is dominated by different physical mechanisms.

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

PubMed

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

2009-02-01

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

Chemical Durability Improvement and Static Fatigue of Glasses.

DTIC Science & Technology

1982-05-01

Specifically, the replacement of hydroxyl groups on the glass surface with silane or Grignard reagent nearly completely eliminated stress rate dependence...CK3SiC13 in Heptane solution Cc) 2 vol % (CR3)3SIC1 in Heptane solution (d) 0.1 M CH3MgBr ( Grignard reagent ) in n-Buthyl ether solution • Corning 7900...C113)3- SiCl or C13MgBr ( Grignard reagent ) solution while it remains practi- cally unchanged in CH3SiCI3 solution. In CH3SICI3 , the strength is

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.

Superhydrophobic Surfaces with Very Low Hysteresis Prepared by Aggregation of Silica Nanoparticles During In Situ Urea-Formaldehyde Polymerization.

PubMed

Diwan, Anubhav; Jensen, David S; Gupta, Vipul; Johnson, Brian I; Evans, Delwyn; Telford, Clive; Linford, Matthew R

2015-12-01

We present a new method for the preparation of superhydrophobic materials by in situ aggregation of silica nanoparticles on a surface during a urea-formaldehyde (UF) polymerization. This is a one-step process in which a two-tier topography is obtained. The polymerization is carried out for 30, 60, 120, 180, and 240 min on silicon shards. Silicon surfaces are sintered to remove the polymer. SEM and AFM show both an increase in the area covered by the nanoparticles and their aggregation with increasing polymerization time. Chemical vapor deposition of a fluorinated silane in the presence of a basic catalyst gives these surfaces hydrophobicity. Deposition of this low surface energy silane is confirmed by the F 1s signal in XPS. The surfaces show advancing water contact angles in excess of 160 degrees with very low hysteresis (< 7) after 120 min and 60 min polymerization times for 7 nm and 14 nm silica, respectively. Depositions are successfully demonstrated on glass substrates after they are primed with a UF polymer layer. Superhydrophobic surfaces can also be prepared on unsintered substrates.

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.

Interface effects on mechanical properties of particle-reinforced composites.

PubMed

Debnath, S; Ranade, R; Wunder, S L; McCool, J; Boberick, K; Baran, G

2004-09-01

Effective bonding between the filler and matrix components typically improves the mechanical properties of polymer composites containing inorganic fillers. The aim of this study was to test the hypothesis that composite flexural modulus, flexure strength, and toughness are directly proportional to filler-matrix interfacial shear strength. The resin matrix component of the experimental composite consisted of a 60:40 blend of BisGMA:TEGDMA. Two levels of photoinitiator components were used: 0.15, and 0.5%. Raman spectroscopy was used to determine degree of cure, and thermogravimetry (TGA) was used to quantify the degree of silane, rubber, or polymer attachment to silica and glass particles. Filler-matrix interfacial shear strengths were measured using a microbond test. Composites containing glass particles with various surface treatments were prepared and the modulus, flexure strength, and fracture toughness of these materials obtained using standard methods. Mechanical properties were measured on dry and soaked specimens. The interfacial strength was greatest for the 5% MPS treated silica, and it increased for polymers prepared with 0.5% initiator compared with 0.15% initiator concentrations. For the mechanical properties measured, the authors found that: (1) the flexural modulus was independent of the type of filler surface treatment, though flexural strength and toughness were highest for the silanated glass; (2) rubber at the interface, whether bonded to the filler and matrix or not, did not improve toughness; (3) less grafting of resin to silanated filler particles was observed when the initiator concentration decreased. These findings suggest that increasing the strength of the bond between filler and matrix will not result in improvements in the mechanical properties of particulate-reinforced composites in contrast to fiber-reinforced composites. Also, contraction stresses in the 0.5 vs 0.15% initiator concentration composites may be responsible for increases in interfacial shear strengths, moduli, and flexural strengths.

Surface Modifications in Adhesion and Wetting

NASA Astrophysics Data System (ADS)

Longley, Jonathan

Advances in surface modification are changing the world. Changing surface properties of bulk materials with nanometer scale coatings enables inventions ranging from the familiar non-stick frying pan to advanced composite aircraft. Nanometer or monolayer coatings used to modify a surface affect the macro-scale properties of a system; for example, composite adhesive joints between the fuselage and internal frame of Boeing's 787 Dreamliner play a vital role in the structural stability of the aircraft. This dissertation focuses on a collection of surface modification techniques that are used in the areas of adhesion and wetting. Adhesive joints are rapidly replacing the familiar bolt and rivet assemblies used by the aerospace and automotive industries. This transition is fueled by the incorporation of composite materials into aircraft and high performance road vehicles. Adhesive joints have several advantages over the traditional rivet, including, significant weight reduction and efficient stress transfer between bonded materials. As fuel costs continue to rise, the weight reduction is accelerating this transition. Traditional surface pretreatments designed to improve the adhesion of polymeric materials to metallic surfaces are extremely toxic. Replacement adhesive technologies must be compatible with the environment without sacrificing adhesive performance. Silane-coupling agents have emerged as ideal surface modifications for improving composite joint strength. As these coatings are generally applied as very thin layers (<50 nm), it is challenging to characterize their material properties for correlation to adhesive performance. We circumvent this problem by estimating the elastic modulus of the silane-based coatings using the buckling instability formed between two materials of a large elastic mismatch. The elastic modulus is found to effectively predict the joint strength of an epoxy/aluminum joint that has been reinforced with silane coupling agents. This buckling technique is extended to investigate the effects of chemical composition on the elastic modulus. Finally, the effect of macro-scale roughness on silane-reinforced joints is investigated within the framework of the unresolved problem of how to best characterize rough surfaces. Initially, the fractal dimension is used to characterize grit-blasted and sanded surfaces. It is found that, contrary to what has been suggested in the literature, the fractal dimension is independent of the roughening mechanism. Instead, the use of an anomalous diffusion coefficient is proposed as a more effective way to characterize a rough surface. Surface modification by preparation of surface energy gradients is then investigated. Materials with gradients in surface energy are useful in the areas of microfluidics, heat transfer and protein adsorption, to name a few. Gradients are prepared by vapor deposition of a reactive silane from a filter paper source. The technique gives control over the size and shape of the gradient. This surface modification is then used to induce droplet motion through repeated stretching and compression of a water drop between two gradient surfaces. This inchworm type motion is studied in detail and offers an alternative method to surface vibration for moving drops in microfluidic devices. The final surface modification considered is the application of a thin layer of rubber to a rigid surface. While this technique has many practical uses, such as easy release coatings in marine environments, it is applied herein to enable spontaneous healing between a rubber surface and a glass cover slip. Study of the diffusion controlled healing of a blister can be made by trapping an air filled blister between a glass cover slip and a rubber film. Through this study we find evidence for an interfacial diffusion process. This mechanism of diffusion is likely to be important in many biological systems.

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.

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.

Bioinspired Catecholic Primers for Rigid and Ductile Dental Resin Composites.

PubMed

Shin, Eeseul; Ju, Sung Won; An, Larry; Ahn, Eungjin; Ahn, Jin-Soo; Kim, Byeong-Su; Ahn, B Kollbe

2018-01-17

In the construction of dental restorative polymer composite materials, surface priming on mineral fillers is essential to improve the mechanical performance of the composites. Here we present bioinspired catechol-functionalized primers for a tougher dental resin composite containing glass fillers. The catecholic primers with different polymerizable end groups were designed and then coated on glass surfaces using a simple drop-casting or dip-coating process. The surface binding ability and possible cross-linking (coupling or chemical bridging between the glass substrate and the dental resin) of the catecholic bifunctional primers were evaluated using atomic force microscopy, contact angle measurements, and the knife shear bonding test and compared to a state-of-the-art silane-based coupling agent. Various mechanical tests including shrinkage and compression tests of the dental resin composites were also conducted. Compression tests of the composites containing the catecholic primed fillers exhibited enhanced mechanical properties, owing to the bidentate hydrogen bonding of catechol moieties to the oxide mineral surface. Furthermore, the superior biocompatibility of the primed surface was confirmed via cell attachment assay, thus providing applicability of catecholic primers for practical dental and biomedical applications.

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

Effect of surface condition of dental zirconia ceramic (Denzir) on bonding.

PubMed

Uo, Motohiro; Sjögren, Göran; Sundh, Anders; Goto, Mitsunari; Watari, Fumio; Bergman, Maud

2006-09-01

Yttria partially stabilized zirconia (YPSZ) ceramics are suitable for dental and medical use because of their high fracture toughness and chemical durability. The purpose of this study was to examine the bonding behavior of a dental YPSZ ceramic, Denzir. After being subjected to various surface treatments, Denzir specimens were bonded to each other using an adhesive resin composite, glass ionomer, or zinc phosphate cement. Bonding strength was then determined by the shearing test. No significant differences (p>0.05) were observed between SiC- and Al2O3-blasted specimens. In all surface treatments, the shear bond strength significantly (p<0.05) increased in the order of adhesive resin composite cement > glass ionomer cement > zinc phosphate cement. Moreover, silanization with methacryloxy propyl trimethoxysilane slightly increased the bonding strength of the adhesive resin composite cement.

Influence of biofilm formation on the optical properties of novel bioactive glass-containing composites

PubMed Central

Hyun, Hong-Keun; Ferracane, Jack L.

2016-01-01

Objective Bioactive glass (BAG) has been suggested as a possible additive for dental restorative materials because of its antimicrobial effect and potential for promoting apatite formation in body fluids. The purpose of this study was to investigate the effects of bacterial biofilm on the change of colorimetric value and translucency of novel BAG-containing composites having different initial surface roughness. Methods Composites with 72 wt% total filler load were prepared by replacing 15% of the silanized Sr glass with BAG (65 mole% Si; 4% P; 31% Ca), BAG-F (61% Si; 31% Ca; 4% P; 3% F; 1% B), or silanized silica. Light-cured discs of 2-mm thickness (n=10/group) were divided into 4 different surface roughness subgroups produced by wet polishing with 600 and then up to 1200, 2400, or 4000 grit SiC. CIE L*a*b* were measured and the color difference and translucency parameter (TP) were calculated before and after incubating in media with or without a S. mutans (UA 159) biofilm for 2 wks (no agitation). Results were analyzed using ANOVA/Tukey's test (α = 0.05). Results All the color differences for BAG and BAG-F composite showed significant decreases with bacterial biofilm compared to media-only. The mean TP (SD) of BAG and BAG-F composite before aging [10.0 (2.8) and 8.5 (1.4)] was higher than that of the control composite [4.9 (0.8)], while the change in TP with aging was greater compared to the control with or without bacteria. BAG-F composites with the smoothest surfaces showed a greater decrease in TP under bacterial biofilm compared to the BAG composite. Significance Highly polished dental composites containing bioactive glass additives may become slightly rougher and show reduced translucency when exposed to bacterial biofilms, but do not discolor any more than control composites that do not contain the BAG. PMID:27394086

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.

Surface Nanobubbles Studied by Time-Resolved Fluorescence Microscopy Methods Combined with AFM: The Impact of Surface Treatment on Nanobubble Nucleation.

PubMed

Hain, Nicole; Wesner, Daniel; Druzhinin, Sergey I; Schönherr, Holger

2016-11-01

The impact of surface treatment and modification on surface nanobubble nucleation in water has been addressed by a new combination of fluorescence lifetime imaging microscopy (FLIM) and atomic force microscopy (AFM). In this study, rhodamine 6G (Rh6G)-labeled surface nanobubbles nucleated by the ethanol-water exchange were studied on differently cleaned borosilicate glass, silanized glass as well as self-assembled monolayers on transparent gold by combined AFM-FLIM. While the AFM data confirmed earlier reports on surface nanobubble nucleation, size, and apparent contact angles in dependence of the underlying substrate, the colocalization of these elevated features with highly fluorescent features observed in confocal intensity images added new information. By analyzing the characteristic contributions to the excited state lifetime of Rh6G in decay curves obtained from time-correlated single photon counting (TCSPC) experiments, the characteristic short-lived (<600 ps) component of could be associated with an emission at the gas-water interface. Its colocalization with nanobubble-like features in the AFM height images provides evidence for the observation of gas-filled surface nanobubbles. While piranha-cleaned glass supported nanobubbles, milder UV-ozone or oxygen plasma treatment afforded glass-water interfaces, where no nanobubbles were observed by combined AFM-FLIM. Finally, the number density of nanobubbles scaled inversely with increasing surface hydrophobicity.

Fabrication and evaluation of Bis-GMA/TEGDMA dental resins/composites containing halloysite nanotubes

PubMed Central

Chen, Qi; Zhao, Yong; Wu, Weidong; Xu, Tao; Fong, Hao

2012-01-01

Objective To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and the corresponding composites (with conventional glass filler)containing vari ed mass fractions of halloysite nanotubes (HNTs). Methods Three dispersion methods were studied to separate the silanized halloysite as individual HNTs and to uniformly distribute them into dental matrices. Photopolymerization induced volumetric shrinkage was measured by using a mercury dilatometer. Real time near infrared spectroscopy was adopted to study the degree of vinyl double bond conversion and the photopolymerization rate. Mechanical properties of the composites were tested by a universal mechanical testing machine. Analysis of Variance (ANOVA) was used for the statistical analysis of the acquired data. Morphologies of halloysite/HNTs and representative fracture surfaces of the reinforced dental resins/composites were examined by SEM and TEM. Results Impregnation of small mass fractions (e.g., 1% and 2.5%) of the silanized HNTs in Bis-GMA/TEGDMA dental resins/composites improved mechanical properties significantly; however; large mass fractions (e.g., 5%) of impregnation did not further improve the mechanical properties. The impregnation of HNTs into dental resins/composites could result in two opposite effects: the reinforcing effect due to the highly separated and uniformly distributed HNTs, and the weakening effect due to the formation of HNT agglomerates/particles. Significance Uniform distribution of a small amount of well-separated silanized HNTs into Bis-GMA/TEGDMA dental resins/composites could result in substantial improvements on mechanical properties. PMID:22796038

Fabrication and evaluation of Bis-GMA/TEGDMA dental resins/composites containing halloysite nanotubes.

PubMed

Chen, Qi; Zhao, Yong; Wu, Weidong; Xu, Tao; Fong, Hao

2012-10-01

To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and the corresponding composites (with conventional glass filler) containing varied mass fractions of halloysite nanotubes (HNTs). Three dispersion methods were studied to separate the silanized halloysite as individual HNTs and to uniformly distribute them into dental matrices. Photopolymerization induced volumetric shrinkage was measured by using a mercury dilatometer. Real time near infrared spectroscopy was adopted to study the degree of vinyl double bond conversion and the photopolymerization rate. Mechanical properties of the composites were tested by a universal mechanical testing machine. Analysis of variance (ANOVA) was used for the statistical analysis of the acquired data. Morphologies of halloysite/HNTs and representative fracture surfaces of the reinforced dental resins/composites were examined by SEM and TEM. Impregnation of small mass fractions (e.g., 1% and 2.5%) of the silanized HNTs in Bis-GMA/TEGDMA dental resins/composites improved mechanical properties significantly; however; large mass fractions (e.g., 5%) of impregnation did not further improve the mechanical properties. The impregnation of HNTs into dental resins/composites could result in two opposite effects: the reinforcing effect due to the highly separated and uniformly distributed HNTs, and the weakening effect due to the formation of HNT agglomerates/particles. Uniform distribution of a small amount of well-separated silanized HNTs into Bis-GMA/TEGDMA dental resins/composites could result in substantial improvements on mechanical properties. Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Development and Mechanical Behavior of FML/Aluminium Foam Sandwiches

NASA Astrophysics Data System (ADS)

Baştürk, S. B.; Tanoğlu, M.

2013-10-01

In this study, the Fiber-Metal Laminates (FMLs) containing glass fiber reinforced polypropylene (GFPP) and aluminum (Al) sheet were consolidated with Al foam cores for preparing the sandwich panels. The aim of this article is the comparison of the flexural properties of FML/Al foam sandwich panels bonded with various surface modification approaches (silane treatment and combination of silane treatment with polypropylene (PP) based film addition). The FML/foam sandwich systems were fabricated by laminating the components in a mould at 200 °C under 1.5 MPa pressure. The energy absorbtion capacities and flexural mechanical properties of the prepared sandwich systems were evaluated by mechanical tests. Experiments were performed on samples of varying foam thicknesses (8, 20 and 30 mm). The bonding among the sandwich components were achieved by various surface modification techniques. The Al sheet/Al foam sandwiches were also consolidated by bonding the components with an epoxy adhesive to reveal the effect of GFPP on the flexural performance of the sandwich structures.

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

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.

Polysialic acid immobilized on silanized glass surfaces: a test case for its use as a biomaterial for nerve regeneration.

PubMed

Steinhaus, Stephanie; Stark, Yvonne; Bruns, Stephanie; Haile, Yohannes; Scheper, Thomas; Grothe, Claudia; Behrens, Peter

2010-04-01

The immobilization of polysialic acid (polySia) on glass substrates has been investigated with regard to the applicability of this polysaccharide as a novel, biocompatible and bioresorbable material for tissue engineering, especially with regard to its use in nerve regeneration. PolySia, a homopolymer of alpha-2,8-linked sialic acid, is involved in post-translational modification of the neural cell adhesion molecule (NCAM). The degradation of polySia can be controlled which makes it an interesting material for coating and for scaffold construction in tissue engineering. Here, we describe the immobilization of polySia on glass surfaces via an epoxysilane linker. Whereas glass surfaces will not actually be used in nerve regeneration scaffolds, they provide a simple and efficient means for testing various methods for the investigation of immobilized polySia. The modified surfaces were investigated with contact angle measurements and the quantity of immobilized polySia was examined by the thiobarbituric acid assay and a specific polySia-ELISA. The interactions between the polySia-modified surface and immortalized Schwann cells were evaluated via cell adhesion and cell viability assays. The results show that polySia can be immobilized on glass surfaces via the epoxysilane linker and that surface-bound polySia has no toxic effects on Schwann cells. Therefore, as a key substance in the development of vertebrates and as a favourable substrate for the cultivation of Schwann cells, it offers interesting features for the use in nerve guidance tubes for treatment of peripheral nerve injuries.

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.

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.

Surface functionalization of 3D glass-ceramic porous scaffolds for enhanced mineralization in vitro

NASA Astrophysics Data System (ADS)

Ferraris, Sara; Vitale-Brovarone, Chiara; Bretcanu, Oana; Cassinelli, Clara; Vernè, Enrica

2013-04-01

Bone reconstruction after tissue loosening due to traumatic, pathological or surgical causes is in increasing demand. 3D scaffolds are a widely studied solution for supporting new bone growth. Bioactive glass-ceramic porous materials can offer a three-dimensional structure that is able to chemically bond to bone. The ability to surface modify these devices by grafting biologically active molecules represents a challenge, with the aim of stimulating physiological bone regeneration with both inorganic and organic signals. In this research work glass ceramic scaffolds with very high mechanical properties and moderate bioactivity have been functionalized with the enzyme alkaline phosphatase (ALP). The material surface was activated in order to expose hydroxyl groups. The activated surface was further grafted with ALP both via silanization and also via direct grafting to the surface active hydroxyl groups. Enzymatic activity of grafted samples were measured by means of UV-vis spectroscopy before and after ultrasonic washing in TRIS-HCl buffer solution. In vitro inorganic bioactivity was investigated by soaking the scaffolds after the different steps of functionalization in a simulated body fluid (SBF). SEM observations allowed the monitoring of the scaffold morphology and surface chemical composition after soaking in SBF. The presence of ALP enhanced the in vitro inorganic bioactivity of the tested material.

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.

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.

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

Sugar microarray via click chemistry: molecular recognition with lectins and amyloid β (1-42)

NASA Astrophysics Data System (ADS)

Matsumoto, Erino; Yamauchi, Takahiro; Fukuda, Tomohiro; Miura, Yoshiko

2009-06-01

Sugar microarrays were fabricated on various substrates via click chemistry. Acetylene-terminated substrates were prepared by forming self-assembled monolayers (SAMs) on a gold substrate with alkyl-disulfide and on silicon, quartz and glass substrates with a silane-coupling reagent. The gold substrates were subjected to surface plasmon resonance measurements, and the quartz and glass substrates were subjected to spectroscopy measurements and optical microscopy observation. The saccharide-immobilized substrate on the gold substrate showed specific interaction with the corresponding lectin, and the saccharides showed inert surface properties to other proteins with a high signal-to-noise ratio. We also focused on the saccharide-protein interaction on protein amyloidosis of Alzheimer amyloid β. Amyloid β peptide showed conformation transition on the saccharide-immobilization substrate into a β-sheet, and fibril formation and amyloid aggregates were found on the specific saccharides.

Effect of surface preparation with Nd:YAG and Er,Cr:YSGG lasers on the repair bond strength of lithium disilicate glass ceramic to a silorane-based composite resin.

PubMed

Ebrahimi Chaharom, Mohammad Esmaeel; Pournaghi Azar, Fatemeh; Mohammadi, Narmin; Nasiri, Rezvan

2018-01-01

Background. This study was undertaken to evaluate the repair bond strength of lithium disilicate glass ceramic to a silorane-based composite resin after surface preparation with Nd:YAG and Er,Cr:YSGG lasers. Methods. A total of 102 lithium disilicate glass ceramic samples (IPS e.max Press), measuring 5 mm in diameter and 4 mm in thickness, were randomly assigned to 6 groups (n=17): group 1, no surface preparation (control); group 2, acid etching with 9.5% hydrofluoric acid (HF); group 3, surface preparation with 4.5-W Nd:YAG laser; group 4, surface preparation with 6-W Nd:YAG laser; group 5, surface preparation with 1.5-W Er,Cr:YSGG laser; and group 6, surface preparation with 6-W Er,Cr:YSGG laser. After preparation of surfaces and application of silane, all the samples were repaired with the use of a silorane-based composite resin, followed by storage in distilled water at a temperature of 37°C for 24 hours and thermocycling. Finally, the samples were subjected to a shearing bond strength test; the fracture modes were determined under a stereomi-croscope. Results. There were significant differences between the HF group and the other groups (P=0.000). Two-by-two comparisons of the other groups revealed no significant differences (P>0.05). Conclusion. Use of HF proved the most effective surface preparation technique to increase the repair bond strength between lithium disilicate glass ceramic and silorane-based composite resin; compared to the control group.

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.

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.

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.

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

Friction coefficient dependence on electrostatic tribocharging

PubMed Central

Burgo, Thiago A. L.; Silva, Cristiane A.; Balestrin, Lia B. S.; Galembeck, Fernando

2013-01-01

Friction between dielectric surfaces produces patterns of fixed, stable electric charges that in turn contribute electrostatic components to surface interactions between the contacting solids. The literature presents a wealth of information on the electronic contributions to friction in metals and semiconductors but the effect of triboelectricity on friction coefficients of dielectrics is as yet poorly defined and understood. In this work, friction coefficients were measured on tribocharged polytetrafluoroethylene (PTFE), using three different techniques. As a result, friction coefficients at the macro- and nanoscales increase many-fold when PTFE surfaces are tribocharged, but this effect is eliminated by silanization of glass spheres rolling on PTFE. In conclusion, tribocharging may supersede all other contributions to macro- and nanoscale friction coefficients in PTFE and probably in other insulating polymers. PMID:23934227

Durable hydrophobic coating composition for metallic surfaces and method for the preparation of the composition

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

Liu, Jiong

A durable hydrophobic coating composition containing fluorinated silanes for metallic surfaces, such as stainless steel surfaces. The composition includes at least one fluorine-containing silane compound, at least one phosphorus-containing silane compound, and at least one hydrolysable compound. This coating is suitable for condenser tubes, among other applications, to promote dropwise condensation.

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.

The Role of Surface Chemistry in Adhesion and Wetting of Gecko Toe Pads

PubMed Central

Badge, Ila; Stark, Alyssa Y.; Paoloni, Eva L.; Niewiarowski, Peter H.; Dhinojwala, Ali

2014-01-01

An array of micron-sized setal hairs offers geckos a unique ability to walk on vertical surfaces using van der Waals interactions. Although many studies have focused on the role of surface morphology of the hairs, very little is known about the role of surface chemistry on wetting and adhesion. We expect that both surface chemistry and morphology are important, not only to achieve optimum dry adhesion but also for increased efficiency in self-cleaning of water and adhesion under wet conditions. Here, we used a plasma-based vapor deposition process to coat the hairy patterns on gecko toe pad sheds with polar and non-polar coatings without significantly perturbing the setal morphology. By a comparison of wetting across treatments, we show that the intrinsic surface of gecko setae has a water contact angle between 70–90°. As expected, under wet conditions, adhesion on a hydrophilic surface (glass) was lower than that on a hydrophobic surface (alkyl-silane monolayer on glass). Surprisingly under wet and dry conditions the adhesion was comparable on the hydrophobic surface, independent of the surface chemistry of the setal hairs. This work highlights the need to utilize morphology and surface chemistry in developing successful synthetic adhesives with desirable adhesion and self-cleaning properties. PMID:25323067

The Role of Surface Chemistry in Adhesion and Wetting of Gecko Toe Pads

NASA Astrophysics Data System (ADS)

Badge, Ila; Stark, Alyssa Y.; Paoloni, Eva L.; Niewiarowski, Peter H.; Dhinojwala, Ali

2014-10-01

An array of micron-sized setal hairs offers geckos a unique ability to walk on vertical surfaces using van der Waals interactions. Although many studies have focused on the role of surface morphology of the hairs, very little is known about the role of surface chemistry on wetting and adhesion. We expect that both surface chemistry and morphology are important, not only to achieve optimum dry adhesion but also for increased efficiency in self-cleaning of water and adhesion under wet conditions. Here, we used a plasma-based vapor deposition process to coat the hairy patterns on gecko toe pad sheds with polar and non-polar coatings without significantly perturbing the setal morphology. By a comparison of wetting across treatments, we show that the intrinsic surface of gecko setae has a water contact angle between 70-90°. As expected, under wet conditions, adhesion on a hydrophilic surface (glass) was lower than that on a hydrophobic surface (alkyl-silane monolayer on glass). Surprisingly under wet and dry conditions the adhesion was comparable on the hydrophobic surface, independent of the surface chemistry of the setal hairs. This work highlights the need to utilize morphology and surface chemistry in developing successful synthetic adhesives with desirable adhesion and self-cleaning properties.

Chemiluminescence-based pesticide biosensor utilizing the intelligent evolved properties of the enzyme alkaline phosphatase

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

Ayyagari, M.; Kamtekar, S.; Pande, R.

A methodology is described for immobilizing the enzyme alkaline phosphatase onto a glass surface using a novel biotinylated copolymer, poly(3-undecylthiophene-co-3- methanoithiophene). A streptavidin conjugate of alkaline phosphatase is used in this study. The biotinylated polymer is attached to the silanized glass surface via hydrophobic interactions and the enzyme is interfaced with the polymer through the classical biotin- streptavidin interaction. Alkaline phosphatase catalyzes the dephosphorylation of a macrocyclic compound, chloro-3-(4-methoxy spiro) (1,2 dioxetane-3-2`-tricyclo-) (3.3.1.1 )-(decani-4-yl) phenyl phosphate, to a species which emits energy by chemiluminescence. This chemiluminescence signal can be detected with a photomultiplier tube for enzymatic catalysis with the biocatalystmore » both in solution and immobilized on a glass surface. The signal generation is inhibited by the organophosphorus based insecticides such as paraoxon as well as nerve agents. We demonstrate in this study that a number of organophosphorus based insecticides inhibit the enzyme-mediated generation of chemiluminescence signal. This is true for the enzyme conjugate both free in solution and immobilized on a glass surface. In solution, the inhibition resembles the case of a partially uncompetitive system. By this type of inhibition we are able to detect pesticides down to about 50 ppb for the enzyme in solution. The pesticide detection limit of immobilized enzyme is currently being investigated. The enzyme is capable of a number of measurement cycles without significant loss of signal level.« less

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.

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.

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.

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.

Coupling of HDPE/hydroxyapatite composites by silane-based methodologies.

PubMed

Sousa, R A; Reis, R L; Cunha, A M; Bevis, M J

2003-06-01

Several coupling treatments based on silane chemicals were investigated for the development of high density (HDPE)/hydroxyapatite (HA) composites. Two HA powders, sintered HA (HAs) and non sintered HA (HAns), were studied in combination with five silanes, namely y-methacryloxy propyltrimethoxy silane (MEMO), 3-(2-aminoethyl)aminopropyltrimethoxy silane (DAMO), vinyltrimethoxy silane (VTMO), 3-aminopropyltriethoxy silane (AMEO) and trimethoxypropyl silane (PTMO). The HA particles were treated by a dipping in method or by spraying with silane solutions. After drying, the treated powders were compounded with HDPE or HDPE with acrylic acid and/or organic peroxide and subsequently compression molded. The tensile test specimens obtained from the molded plates were tensile tested and their fracture surfaces were observed by scanning electron microscopy (SEM). For the sintered HA (HAs) composites, the most effective coupling treatments concerning stiffness are those based on MEMO and AMEO. The low influence of these coupling procedures on strength is believed to be associated to the low volume fraction and the relatively smooth surface of the used HA particles. For the non-sintered HA (HAns) composites, it was possible to improve significantly both the stiffness and the strength. Amino silanes demonstrated to be highly efficient concerning strength enhancement. The higher effectiveness of the coupling treatments for HAns filled composites is attributed to their higher particle surface area, smaller particle size distribution and expected higher chemical reactivity. For both cases, the improvement in mechanical performance after the coupling treatment is consistent with the enhancement in interfacial adhesion observed by SEM.

A comparison between the shear bond strength of brackets bonded to glazed and deglazed porcelain surfaces with resin-reinforced glass-ionomer cement and a bis-GMA resin adhesive.

PubMed

Lifshitz, Abraham B; Cárdenas, Marianela

2006-01-01

This study compared the shear bond strength of a light-cure resin-reinforced glass-ionomer cement with a bis-GMA light-cure resin system in the bonding of stainless steel brackets to glazed and deglazed porcelain surfaces. Porcelain surfaces were divided into 4 groups: group 1, deglazed porcelain surfaces with Transbond XT, group 2, glazed porcelain surfaces with Transbond XT; group 3, deglazed porcelain surfaces with Fuji Ortho LC; and group 4, porcelain surfaces with Fuji Ortho LC. Microetching with 50-microm aluminum oxide for 2 seconds at a distance of 5 mm deglazed the porcelain surfaces in groups 1 and 3. All brackets were bonded to the porcelain surfaces using the same procedure and light-cured for 40 seconds with a visible light. All samples were thermocycled between 5 degrees C and 55 degrees C for 300 cycles before testing for shear bond strength with a universal testing machine. The analysis of variance showed no significant difference (P < .05) among the 4 groups; ie, group 1, 10.12 MPa; group 2, 7.00 MPa; group 3, 6.78 MPa; and group 4, 11.15 MPa. The F test also failed to demonstrate any statistical difference among the groups. Conditioning the porcelain surfaces with 37% phosphoric acid immediately followed by a nonhydrolyzed silane coupling agent resulted in clinically adequate bond strength when using either a composite resin or a resin-reinforced glass-ionomer cement. Microetching of these porcelain surfaces apparently offers no bonding advantage.

Polydiacetylene nanovesicles as carriers of natural phenylpropanoids for creating antimicrobial food-contact surfaces.

PubMed

Dogra, Navneet; Choudhary, Ruplal; Kohli, Punit; Haddock, John D; Makwana, Sanjaysinh; Horev, Batia; Vinokur, Yakov; Droby, Samir; Rodov, Victor

2015-03-11

The ultimate goal of this study was developing antimicrobial food-contact materials based on natural phenolic compounds using nanotechnological approaches. Among the methyl-β-cyclodextrin-encapsulated phenolics tested, curcumin showed by far the highest activity toward Escherichia coli with a minimum inhibitory concentration of 0.4 mM. Curcumin was enclosed in liposome-type polydiacetylene/phosholipid nanovesicles supplemented with N-hydroxysuccinimide and glucose. The fluorescence spectrum of the nanovesicles suggested that curcumin was located in their bilayer region. Free-suspended nanovesicles tended to bind to the bacterial surface and demonstrated bactericidal activity toward Gram-negative (E. coli) and vegetative cells of Gram-positive (Bacillus cereus) bacteria reducing their counts from 5 log CFU mL(-1) to an undetectable level within 8 h. The nanovesicles were covalently bound to silanized glass. Incubation of E. coli and B. cereus with nanovesicle-coated glass resulted in a 2.5 log reduction in their counts. After optimization this approach can be used for controlling microbial growth, cross-contamination, and biofilm formation on food-contacting surfaces.

Impregnation of glass fibres with polymethylmethacrylate using a powder-coating method

NASA Astrophysics Data System (ADS)

Vallittu, Pekka K.

1995-01-01

The aim of this study was to evaluate the usefulness of a powder-coating method to impregnate glass fibres with polymethylmethacrylate (PMMA) for dental purposes. The continuous unidirectional E-glass fibres, the surface of which had been treated with precured silane, were powder-coated with spherical PMMA particles. Before the powder-coated prepregs were used, the incorporated PMMA powder was dissolved with methylmethacrylate monomer. The degree of impregnation of the polymerized composite was determined with a scanning electron microscope. The results revealed that the mean degree of impregnation varied from 0.87 to 0.92, being lower in the heat-cured PMMA group (which simulated fabrication of a new denture), and higher in the autopolymerizing group (which simulated the repair of a fractured denture). The means between the two groups did not, however, differ significantly ( p=0.249). The results suggest that, even though the method has some shortcomings in terms of dental laboratory technology, the powder-coating method can be used to fabricate or repair acrylic resin-based dentures.

Adhesive restorations: comparative evaluation between the adhesion of the glass-ceramics to the composite cement and the adhesion of the ceromer to the composite cement.

PubMed

Ceruti, P; Erovigni, F; Casella, F; Lombardo, S

2005-10-01

The aim of this work is to compare the adhesion of the glass-ceramic (empress II) to the composite cement and the adhesion of the ceromer to the composite cement. From each of the above materials, 10 little blocks, of 8 x 6 x 2 mm size, have been prepared. All the surface treatments suggested by the manufacturing industry have been performed: sandblasting and acid-etching of the ceramic, ceromer surface roughening with diamond bur and silanization and bonding application on both materials. A homogeneous layer of cement has been placed between couples of blocks of the same material and photopolymerised. Every sample, consisting of 2 bonded blocks, has been submitted to a traction force on a universal test machine connected with a computerized measure system (SINTEC D/10). Samples have been anchored to the machine binding devices by a bicomponent epoxy glue. Data on the breaking charge have been recorded and an analysis of the broken surfaces has been performed in order to classify the breaking modalities. The results ontained showed that the composite-glass-ceramic adhesion force (mean value 64 Mpa) was remarkably higher than the composite-ceromer adhesion (mean value 37.21 Mpa). The analysis of the broken surfaces by SEM showed that a mixed fracture occurred in all samples (both partly adhesive and cohesive).

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.

Preparation and characterization of PVDF-glass fiber composite membrane reinforced by interfacial UV-grafting copolymerization.

PubMed

Luo, Nan; Xu, Rongle; Yang, Min; Yuan, Xing; Zhong, Hui; Fan, Yaobo

2015-12-01

A novel inorganic-organic composite membrane, namely poly(vinylidene fluoride) PVDF-glass fiber (PGF) composite membrane, was prepared and reinforced by interfacial ultraviolet (UV)-grafting copolymerization to improve the interfacial bonding strength between the membrane layer and the glass fiber. The interfacial polymerization between inorganic-organic interfaces is a chemical cross-linking reaction that depends on the functionalized glass fiber with silane coupling (KH570) as the initiator and the polymer solution with acrylamide monomer (AM) as the grafting block. The Fourier transform infrared spectrometer-attenuated total reflectance (FTIR-ATR) spectra and the energy dispersive X-ray (EDX) pictures of the interface between the glass fiber and polymer matrix confirmed that the AM was grafted to the surface of the glass fiber fabric and that the grafting polymer was successfully embedded in the membrane matrix. The formation mechanisms, permeation, and anti-fouling performance of the PGF composite membrane were measured with different amounts of AM in the doping solutions. The results showed that the grafting composite membrane improved the interfacial bonding strength and permeability, and the peeling strength was improved by 32.6% for PGF composite membranes with an AM concentration at 2wt.%. Copyright © 2015. Published by Elsevier B.V.

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.

In Situ Generation of Two-Dimensional Au–Pt Core–Shell Nanoparticle Assemblies

PubMed Central

2010-01-01

Two-dimensional assemblies of Au–Pt bimetallic nanoparticles are generated in situ on polyethyleneimmine (PEI) silane functionalized silicon and indium tin oxide (ITO) coated glass surfaces. Atomic force microscopy (AFM), UV–Visible spectroscopy, and electrochemical measurements reveal the formation of core–shell structure with Au as core and Pt as shell. The core–shell structure is further supported by comparing with the corresponding data of Au nanoparticle assemblies. Static contact angle measurements with water show an increase in hydrophilic character due to bimetallic nanoparticle generation on different surfaces. It is further observed that these Au–Pt core–shell bimetallic nanoparticle assemblies are catalytically active towards methanol electro-oxidation, which is the key reaction for direct methanol fuel cells (DMFCs). PMID:20651923

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.

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.

Bioactive glass fillers reduce bacterial penetration into marginal gaps for composite restorations

PubMed Central

Khvostenko, D.; Hilton, T. J.; Ferracane, J. L.; Mitchell, J. C.; Kruzic, J. J.

2015-01-01

Objectives Bioactive glass (BAG) is known to possess antimicrobial and remineralizing properties; however, the use of BAG as a filler for resin based composite restorations to slow recurrent caries has not been studied. Accordingly, the objective of this study was to investigate the effect of 15 wt% BAG additions to a resin composite on bacterial biofilms penetrating into marginal gaps of simulated tooth fillings in vitro during cyclic mechanical loading. Methods Human molars were machined into approximately 3 mm thick disks of dentin and 1.5–2 mm deep composite restorations were placed. A narrow 15–20 micrometer wide dentin-composite gap was allowed to form along half of the margin by not applying dental adhesive to that region. Two different 72 wt% filled composites were used, one with 15 wt% BAG filler (15BAG) and the balance silanated strontium glass and one filled with OX-50 and silanated strontium glass without BAG (0BAG – control). Samples of both groups had Streptococcus mutans biofilms grown on the surface and were tested inside a bioreactor for two weeks while subjected to periods of cyclic mechanical loading. After post-test biofilm viability was confirmed, each specimen was fixed in glutaraldehyde, gram positive stained, mounted in resin and cross-sectioned to reveal the gap profile. Depth of biofilm penetration for 0BAG and 15BAG was quantified as the fraction of gap depth. The data were compared using a Student’s t-test. Results The average depth of bacterial penetration into the marginal gap for the 15BAG samples was significantly smaller (~61%) in comparison to 0BAG, where 100% penetration was observed for all samples with the biofilm penetrating underneath of the restoration in some cases. Significance BAG containing resin dental composites reduce biofilm penetration into marginal gaps of simulated tooth restorations. This suggests BAG containing composites may have the potential to slow the development and propagation of secondary tooth decay at restoration margins. PMID:26621028

[Effect of hydrofluoric acid concentration on the surface morphology and bonding effectiveness of lithium disilicate glass ceramics to resin composites].

PubMed

Hailan, Qian; Lingyan, Ren; Rongrong, Nie; Xiangfeng, Meng

2017-12-01

This study aimed at determining the influence of hydrofluoric acid (HF) in varied concentrations on the surface morphology of lithium disilicate glass ceramics and bond durability between resin composites and post-treated lithium disilicate glass ceramics. After being sintered, ground, and washed, 72 as-prepared specimens of lithium disilicate glass ceramics with dimensions of 11 mm×13 mm×2 mm were randomly divided into three groups. Each group was treated with acid solution [32% phosphoric acid (PA) or 4% or 9.5% HF] for 20 s. Then, four acidified specimens from each group were randomly selected. One of the specimens was used to observe the surface morphology using scanning electron microscopy, and the others were used to observe the surface roughness using a surface roughness meter (including Ra, Rz, and Rmax). After treatment with different acid solutions in each group, 20 samples were further treated with silane coupling agent/resin adhesive/resin cement (Monobond S/Multilink Primer A&B/Multilink N), followed by bonding to a composite resin column (Filtek™ Z350) with a diameter of 3 mm. A total of 20 specimens in each group were randomly divided into two subgroups, which were used for measuring the microshear bond strength, with one of them subjected to cool-thermal cycle for 20 000 times. The surface roughness (Ra, Rz, and Rmax) of lithium disilicate glass ceramics treated with 4% or 9.5% HF was significantly higher than that of the ceramic treated with PA (P<0.05). The lithium disilicate glass ceramics treated with 9.5% HF also demonstrated better surface roughness (Rz and Rmax) than that of the ceramics treated with 4% HF. Cool-thermal cycle treatment reduced the bond strength of lithium disilicate glass ceramics in all groups (P<0.05). After cool-thermal cycle, the lithium disilicate glass ceramics treated with HF had higher bond strength than that of the ceramics treated with PA. The lithium disilicate glass ceramics treated with 4% HF had higher bond strength than that of the ceramics treated with 9.5% HF (P<0.05). During cool-thermal cycle, the lithium disilicate glass ceramics treated with 4% HF demonstrated higher reduction in bond strength than that of the samples treated with 9.5% HF (P<0.05). The concentration of HF significantly affected the surface morphology of lithium disilicate glass ceramics and the bond durability between resin composites and post-treated lithium disilicate glass ceramics. The bond strength between resin composites and post-treated lithium disilicate glass ceramic was more efficiently maintained by treatment with 9.5% HF.

Effect of two-step and one-step surface conditioning of glass ceramic on adhesion strength of orthodontic bracket and effect of thermo-cycling on adhesion strength.

PubMed

Asiry, Moshabab A; AlShahrani, Ibrahim; Alaqeel, Samer M; Durgesh, Bangalore H; Ramakrishnaiah, Ravikumar

2018-08-01

The adhesion strength of orthodontic brackets bonded to dental glass ceramics was evaluated after ceramic surface was treated with two-step and one-step surface conditioning systems, and subjecting to thermo-cycling. A total of forty specimens were fabricated from silica based glass ceramic (lithium disilicate) by duplicating the buccal surface of maxillary first premolar. The specimens were randomly assigned to two experimental groups (n = 20), group one specimens were treated with two-step surface conditioning system (IPS ceramic etching gel™ and Monobond plus™) and group two specimens were treated with one-step surface conditioning system (Monobond etch and prime™). The surface roughness of the specimens after treatment with two-step and one-step surface conditioning system was measured using non-contact surface profilometer. Ten randomly selected specimens from each group were subjected to thermo-cycling and the remaining ten served as baseline. The shear bond strength of the specimens was measured using universal material testing machine. The adhesive remnant index score was calculated, and the results of surface roughness and bond strength were tabulated and subjected to analysis of variance and post hoc tukey's test at a significance level of p < 0.05. The results of the study showed that the specimens treated with two-step conditioning system had higher surface roughness and bond strength than one-step conditioning system. The majority of the specimens treated with both two-step and one-step conditioned specimens showed adhesive failure after subjecting thermo-cycling. Traditional two-step conditioning provides better bond strength. The clinical importance of the study is that, the silane promoted adhesion significantly reduces on exposure to thermo-cycling. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

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

Properties of discontinuous S2-glass fiber-particulate-reinforced resin composites with two different fiber length distributions.

PubMed

Huang, Qiting; Garoushi, Sufyan; Lin, Zhengmei; He, Jingwei; Qin, Wei; Liu, Fang; Vallittu, Pekka Kalevi; Lassila, Lippo Veli Juhana

2017-10-01

To investigate the reinforcing efficiency and light curing properties of discontinuous S2-glass fiber-particulate reinforced resin composite and to examine length distribution of discontinuous S2-glass fibers after a mixing process into resin composite. Experimental S2-glass fiber-particulate reinforced resin composites were prepared by mixing 10wt% of discontinuous S2-glass fibers, which had been manually cut into two different lengths (1.5 and 3.0mm), with various weight ratios of dimethacrylate based resin matrix and silaned BaAlSiO 2 filler particulates. The resin composite made with 25wt% of UDMA/SR833s resin system and 75wt% of silaned BaAlSiO 2 filler particulates was used as control composite which had similar composition as the commonly used resin composites. Flexural strength (FS), flexural modulus (FM) and work of fracture (WOF) were measured. Fractured specimens were observed by scanning electron microscopy. Double bond conversion (DC) and fiber length distribution were also studied. Reinforcement of resin composites with discontinuous S2-glass fibers can significantly increase the FS, FM and WOF of resin composites over the control. The fibers from the mixed resin composites showed great variation in final fiber length. The mean aspect ratio of experimental composites containing 62.5wt% of particulate fillers and 10wt% of 1.5 or 3.0mm cutting S2-glass fibers was 70 and 132, respectively. No difference was found in DC between resin composites containing S2-glass fibers with two different cutting lengths. Discontinuous S2-glass fibers can effectively reinforce the particulate-filled resin composite and thus may be potential to manufacture resin composites for high-stress bearing application. Copyright © 2017. Published by Elsevier Ltd.

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.

Phospholipid Polymer Biointerfaces for Lab-on-a-Chip Devices.

PubMed

Xu, Yan; Takai, Madoka; Ishihara, Kazuhiko

2010-06-01

This review summarizes recent achievements and progress in the development of various functional 2-methacryloyloxyethyl phosphorylcholine (MPC) polymer biointerfaces for lab-on-a-chip devices and applications. As phospholipid polymers, MPC polymers can form cell-membrane-like surfaces by surface chemistry and physics and thereby provide biointerfaces capable of suppressing protein adsorption and many subsequent biological responses. In order to enable application to microfluidic devices, a number of MPC polymers with diverse functions have been specially designed and synthesized by incorporating functional units such as charge and active ester for generating the microfluidic flow and conjugating biomolecules, respectively. Furthermore, these polymers were incorporated with silane or hydrophobic moiety to construct stable interfaces on various substrate materials such as glass, quartz, poly(methyl methacrylate), and poly(dimethylsiloxane), via a silane-coupling reaction or hydrophobic interactions. The basic interfacial properties of these interfaces have been characterized from multiple aspects of chemistry, physics, and biology, and the suppression of nonspecific bioadsorption and control of microfluidic flow have been successfully achieved using these biointerfaces on a chip. Further, many chip-based biomedical applications such as immunoassays and DNA separation have been accomplished by integrating these biointerfaces on a chip. Therefore, functional phospholipid polymer interfaces are promising and useful for application to lab-on-a-chip devices in biomedicine.

A pH sensor based on electric properties of nanotubes on a glass substrate

PubMed Central

Nakamura, Motonori; Ishii, Atsushi; Subagyo, Agus; Hosoi, Hirotaka; Sueoka, Kazuhisa; Mukasa, Koichi

2007-01-01

We fabricated a pH-sensitive device on a glass substrate based on properties of carbon nanotubes. Nanotubes were immobilized specifically on chemically modified areas on a substrate followed by deposition of metallic source and drain electrodes on the area. Some nanotubes connected the source and drain electrodes. A top gate electrode was fabricated on an insulating layer of silane coupling agent on the nanotube. The device showed properties of ann-type field effect transistor when a potential was applied to the nanotube from the top gate electrode. Before fabrication of the insulating layer, the device showed that thep-type field effect transistor and the current through the source and drain electrodes depend on the buffer pH. The current increases with decreasing pH of the CNT solution. This device, which can detect pH, is applicable for use as a biosensor through modification of the CNT surface. PMID:21806848

The influence of different cementation modes on the fracture resistance of feldspathic ceramic crowns.

PubMed

Groten, M; Pröbster, L

1997-01-01

One hundred twenty pressed feldspathic ceramic crowns were luted to 20 steel dies using six different cementation modes. Fracture resistance was tested under an angle of 45 degrees and was determined as the maximal fracture load. Crowns were tested with luting agent only (groups A and C) and after etching with hydrofluoric acid, silanating, and the application of a bonding agent (groups B, D, E, and F). The resulting means were: phosphate cement 294.3 (A) and 282.2 (B); glass-ionomer cement 217.2 (C) and 255.4 (D); resin composite 382.2 (E) and 687.6 (F). Statistical analysis revealed significantly greater fracture resistance (P < .01) of resin luted crowns. Bonding to the die almost doubled the fracture resistance. Conditioning of the inner surfaces of the crowns did not improve the fracture resistance of crowns luted using zinc phosphate or glass-ionomer cements.

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.

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.

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.

Effect of surface treatments on the flexural properties and adhesion of glass fiber-reinforced composite post to self-adhesive luting agent and radicular dentin.

PubMed

Elnaghy, Amr M; Elsaka, Shaymaa E

2016-01-01

This study evaluated the effect of different surface treatments on the flexural properties and adhesion of glass fiber post to self-adhesive luting agent and radicular dentin. Seventy-five single-rooted human teeth were prepared to receive a glass fiber post (Reblida). The posts were divided into five groups according to the surface treatment: Gr C (control; no treatment), Gr S (silanization for 60 s), Gr AP (airborne-particle abrasion), Gr HF (etching with 9 % hydrofluoric acid for 1 min), and Gr M10 (etching with CH2Cl2 for 10 min). Dual-cure self-adhesive luting agent (Rely X Unicem) was applied to each group for testing the adhesion using micropush-out test. Failure types were examined with stereomicroscope and surface morphology of the posts was characterized using a scanning electron microscopy (SEM). Flexural properties of posts were assessed using a three-point bending test. Data were analyzed using ANOVA and Tukey's HSD test. Statistical significance was set at the 0.05 probability level. Groups treated with M10 showed significantly higher bond strength than those obtained with other surface treatments (P < 0.05). In general, improvements in bond strength (MPa) were found in the following order: M10 > C > S > AP > HF. Most failure modes were adhesive type of failures between dentin and luting agent (48.2%). SEM analysis revealed that the fiber post surfaces were modified after surface treatments. The surface treatments did not compromise the flexural properties of fiber posts. Application of M10 to the fiber post surfaces enhanced the adhesion to self-adhesive luting agent and radicular dentin.

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

Tyagi, Mukta; Agrawal, V. V.; Chandran, Achu

A unique cholesterol oxidase (ChOx) liquid crystal (LC) biosensor, based on the disruption of orientation in LCs, is developed for cholesterol detection. A self-assembled monolayer (SAM) of Dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride (DMOAP) and (3-Aminopropyl)trimethoxy-silane (APTMS) is prepared on a glass plate by adsorption. The enzyme (ChOx) is immobilized on SAM surface for 12 h before utilizing the film for biosensing purpose. LC based biosensing study is conducted on SAM/ChOx/LC (5CB) cells for cholesterol concentrations ranging from 10 mg/dl to 250 mg/dl. The sensing mechanism has been verified through polarizing optical microscopy, scanning electron microscopy, and spectrometric techniques.

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

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

Combining an Optical Resonance Biosensor with Enzyme Activity Kinetics to Understand Protein Adsorption and Denaturation

PubMed Central

Wilson, Kerry A.; Finch, Craig A.; Anderson, Phillip; Vollmer, Frank; Hickman, James J.

2014-01-01

Understanding protein adsorption and resultant conformation changes on modified and unmodified silicon dioxide surfaces is a subject of keen interest in biosensors, microfluidic systems and for medical diagnostics. However, it has been proven difficult to investigate the kinetics of the adsorption process on these surfaces as well as understand the topic of the denaturation of proteins and its effect on enzyme activity. A highly sensitive optical whispering gallery mode (WGM) resonator was used to study a catalytic enzyme’s adsorption processes on different silane modified glass substrates (plain glass control, DETA, 13F, and SiPEG). The WGM sensor was able to obtain high resolution kinetic data of glucose oxidase (GO) adsorption with sensitivity of adsorption better than that possible with SPR. The kinetic data, in combination with a functional assay of the enzyme activity, was used to test hypotheses on adsorption mechanisms. By fitting numerical models to the WGM sensograms for protein adsorption, and by confirming numerical predictions of enzyme activity in a separate assay, we were able to identify mechanisms for GO adsorption on different alkylsilanes and infer information about the adsorption of protein on nanostructured surfaces. PMID:25453976

Combining an optical resonance biosensor with enzyme activity kinetics to understand protein adsorption and denaturation.

PubMed

Wilson, Kerry A; Finch, Craig A; Anderson, Phillip; Vollmer, Frank; Hickman, James J

2015-01-01

Understanding protein adsorption and resultant conformation changes on modified and unmodified silicon dioxide surfaces is a subject of keen interest in biosensors, microfluidic systems and for medical diagnostics. However, it has been proven difficult to investigate the kinetics of the adsorption process on these surfaces as well as understand the topic of the denaturation of proteins and its effect on enzyme activity. A highly sensitive optical whispering gallery mode (WGM) resonator was used to study a catalytic enzyme's adsorption processes on different silane modified glass substrates (plain glass control, DETA, 13 F, and SiPEG). The WGM sensor was able to obtain high resolution kinetic data of glucose oxidase (GO) adsorption with sensitivity of adsorption better than that possible with SPR. The kinetic data, in combination with a functional assay of the enzyme activity, was used to test hypotheses on adsorption mechanisms. By fitting numerical models to the WGM sensograms for protein adsorption, and by confirming numerical predictions of enzyme activity in a separate assay, we were able to identify mechanisms for GO adsorption on different alkylsilanes and infer information about the adsorption of protein on nanostructured surfaces. Copyright © 2014 Elsevier Ltd. All rights reserved.

How do silanes affect the lubricating properties of cationic double chain surfactant on silica surfaces?

PubMed

Beauvais, Muriel; Serreau, Laurence; Heitz, Caroline; Barthel, Etienne

2009-03-01

The effect of an aminosilane on the lubricant properties of a C(18) double-chained cationic surfactant has been investigated in the context of glass fiber forming process. The surfactant adsorption was studied on silica by Fourier transform infrared (FT-IR) spectroscopy in the attenuated total reflexion (ATR) mode as a function of the aminosilane concentration in an organic water based formulation (sizing) used to coat the glass fibers during the process. A reciprocating ball-on-plate tribometer was used to compare friction properties of silica in contact with the aminosilane-surfactant mixture and in presence of each component of the sizing. Surface forces were measured between silica and an atomic force microscope (AFM) silicon nitride tip in the sizing and in the pure cationic surfactant solution. The aminosilane on its own has no lubricant property and reduces or even suppresses the cationic surfactant adsorption on silica. However, the silica-silica contact is lubricated even if the infrared spectroscopy does not detect any surfactant adsorption. The repeated contacts and shear due to the friction experiment itself induce accumulation, organization and compactness of surfactant bilayers.

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.

Acceleration induced water removal from ear canals.

NASA Astrophysics Data System (ADS)

Kang, Hosung; Averett, Katelee; Jung, Sunghwan

2017-11-01

Children and adults commonly experience having water trapped in the ear canals after swimming. To remove the water, individuals will shake their head sideways. Since a child's ear canal has a smaller diameter, it requires more acceleration of the head to remove the trapped water. In this study, we theoretically and experimentally investigated the acceleration required to break the surface meniscus of the water in artificial ear canals and hydrophobic-coated glass tubes. In experiments, ear canal models were 3D-printed from a CT-scanned human head. Also, glass tubes were coated with silane to match the hydrophobicity in ear canals. Then, using a linear stage, we measured the acceleration values required to forcefully eject the water from the artificial ear canals and glass tubes. A theoretical model was developed to predict the critical acceleration at a given tube diameter and water volume by using a modified Rayleigh-Taylor instability. Furthermore, this research can shed light on the potential of long-term brain injury and damage by shaking the head to push the water out of the ear canal. This research was supported by National Science Foundation Grant CBET-1604424.

Thermal expansion of an epoxy-glass microsphere composite

NASA Technical Reports Server (NTRS)

Price, H. L.; Burks, H. D.

1977-01-01

The thermal expansion of a composite of epoxy (diglycidyl ether of bisphenol A) and solid glass microspheres was investigated. The microspheres had surfaces which were either untreated or treated with a silicone release agent, an epoxy coupling agent, or a general purpose silane coupling agent. Both room temperature (about 300 K) and elevated temperature (about 475 K) cures were used for the epoxy. Two microsphere size ranges were used, about 50 microns, which is applicable in filled moldings, and about 125 microns, which is applicable as bond line spacers. The thermal expansion of the composites was measured from 300 to 350 K or from 300 to 500 K, depending on the epoxy cure temperature. Measurements were made on composites containing up to .6 volume fraction microspheres. Two predictive models, which required only the values of thermal expansion of the polymer and glass and their specific gravities, were tested against the experimental data. A finite element analysis was made of the thermal strain of a composite cell containing a single microsphere surrounded by a finite-thickness interface.

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

Thermo-mechanical characterization of siliconized E-glass fiber/hematite particles reinforced epoxy resin hybrid composite

NASA Astrophysics Data System (ADS)

V. R., Arun prakash; Rajadurai, A.

2016-10-01

In this present work hybrid polymer (epoxy) matrix composite has been strengthened with surface modified E-glass fiber and iron(III) oxide particles with varying size. The particle sizes of 200 nm and <100 nm has been prepared by high energy ball milling and sol-gel methods respectively. To enhance better dispersion of particles and improve adhesion of fibers and fillers with epoxy matrix surface modification process has been done on both fiber and filler by an amino functional silane 3-Aminopropyltrimethoxysilane (APTMS). Crystalline and functional groups of siliconized iron(III) oxide particles were characterized by XRD and FTIR spectroscopy analysis. Fixed quantity of surface treated 15 vol% E-glass fiber was laid along with 0.5 and 1.0 vol% of iron(III) oxide particles into the matrix to fabricate hybrid composites. The composites were cured by an aliphatic hardener Triethylenetetramine (TETA). Effectiveness of surface modified particles and fibers addition into the resin matrix were revealed by mechanical testing like tensile testing, flexural testing, impact testing, inter laminar shear strength and hardness. Thermal behavior of composites was evaluated by TGA, DSC and thermal conductivity (Lee's disc). The scanning electron microscopy was employed to found shape and size of iron(III) oxide particles adhesion quality of fiber with epoxy matrix. Good dispersion of fillers in matrix was achieved with surface modifier APTMS. Tensile, flexural, impact and inter laminar shear strength of composites was improved by reinforcing surface modified fiber and filler. Thermal stability of epoxy resin was improved when surface modified fiber was reinforced along with hard hematite particles. Thermal conductivity of epoxy increased with increase of hematite content in epoxy matrix.

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.

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

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.

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.

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.

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.

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.

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.

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

Tough bonding of hydrogels to diverse non-porous surfaces

NASA Astrophysics Data System (ADS)

Yuk, Hyunwoo; Zhang, Teng; Lin, Shaoting; Parada, German Alberto; Zhao, Xuanhe

2016-02-01

In many animals, the bonding of tendon and cartilage to bone is extremely tough (for example, interfacial toughness ~800 J m-2 refs ,), yet such tough interfaces have not been achieved between synthetic hydrogels and non-porous surfaces of engineered solids. Here, we report a strategy to design tough transparent and conductive bonding of synthetic hydrogels containing 90% water to non-porous surfaces of diverse solids, including glass, silicon, ceramics, titanium and aluminium. The design strategy is to anchor the long-chain polymer networks of tough hydrogels covalently to non-porous solid surfaces, which can be achieved by the silanation of such surfaces. Compared with physical interactions, the chemical anchorage results in a higher intrinsic work of adhesion and in significant energy dissipation of bulk hydrogel during detachment, which lead to interfacial toughness values over 1,000 J m-2. We also demonstrate applications of robust hydrogel-solid hybrids, including hydrogel superglues, mechanically protective hydrogel coatings, hydrogel joints for robotic structures and robust hydrogel-metal conductors.

Polymer diffusion in the interphase between surface and solution.

PubMed

Weger, Lukas; Weidmann, Monika; Ali, Wael; Hildebrandt, Marcus; Gutmann, Jochen Stefan; Hoffmann-Jacobsen, Kerstin

2018-05-22

Total internal reflection fluorescence correlation spectroscopy (TIR-FCS) is applied to study the self-diffusion of polyethylene glycol solutions in the presence of weakly attractive interfaces. Glass coverslips modified with aminopropyl- and propyl-terminated silanes are used to study the influence of solid surfaces on polymer diffusion. A model of three phases of polymer diffusion allows to describe the experimental fluorescence autocorrelation functions. Besides the two-dimensional diffusion of adsorbed polymer on the substrate and three-dimensional free diffusion in bulk solution, a third diffusion time scale is observed with intermediate diffusion times. This retarded three-dimensional diffusion in solution is assigned to long range effects of solid surfaces on diffusional dynamics of polymers. The respective diffusion constants show Rouse scaling (D~N -1 ) indicating a screening of hydrodynamic interactions by the presence of the surface. Hence, the presented TIR-FCS method proves to be a valuable tool to investigate the effect of surfaces on polymer diffusion beyond the first adsorbed polymer layer on the 100 nm length scale.

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.

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

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.

[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.

Chemical vapor deposition of aminopropyl silanes in microfluidic channels for highly efficient microchip capillary electrophoresis-electrospray ionization-mass spectrometry.

PubMed

Batz, Nicholas G; Mellors, J Scott; Alarie, Jean Pierre; Ramsey, J Michael

2014-04-01

We describe a chemical vapor deposition (CVD) method for the surface modification of glass microfluidic devices designed to perform electrophoretic separations of cationic species. The microfluidic channel surfaces were modified using aminopropyl silane reagents. Coating homogeneity was inferred by precise measurement of the separation efficiency and electroosmotic mobility for multiple microfluidic devices. Devices coated with (3-aminopropyl)di-isopropylethoxysilane (APDIPES) yielded near diffusion-limited separations and exhibited little change in electroosmotic mobility between pH 2.8 and pH 7.5. We further evaluated the temporal stability of both APDIPES and (3-aminopropyl)triethoxysilane (APTES) coatings when stored for a total of 1 week under vacuum at 4 °C or filled with pH 2.8 background electrolyte at room temperature. Measurements of electroosmotic flow (EOF) and separation efficiency during this time confirmed that both coatings were stable under both conditions. Microfluidic devices with a 23 cm long, serpentine electrophoretic separation channel and integrated nanoelectrospray ionization emitter were CVD coated with APDIPES and used for capillary electrophoresis (CE)-electrospray ionization (ESI)-mass spectrometry (MS) of peptides and proteins. Peptide separations were fast and highly efficient, yielding theoretical plate counts over 600,000 and a peak capacity of 64 in less than 90 s. Intact protein separations using these devices yielded Gaussian peak profiles with separation efficiencies between 100,000 and 400,000 theoretical plates.

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.

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.

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.

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.

Estimation of polymer-surface interfacial interaction strength by a contact AFM technique.

PubMed

Dvir, H; Jopp, J; Gottlieb, M

2006-12-01

Atomic force microscopy (AFM) measurements were employed to assess polymer-surface interfacial interaction strength. The main feature of the measurement is the use of contact-mode AFM as a tool to scratch off the polymer monolayer adsorbed on the solid surface. Tapping-mode AFM was used to determine the depth of the scraped recess. Independent determination of the layer thickness obtained from optical phase interference microscopy (OPIM) confirmed the depth of the AFM scratch. The force required for the complete removal of the polymer layer with no apparent damage to the substrate surface was determined. Polypropylene (PP), low-density polyethylene (PE), and PP-grafted-maleic anhydride (PP-g-ma) were scraped off silane-treated glass slabs, and the strength of surface interaction of the polymer layer was determined. In all cases it was determined that the magnitude of surface interaction force is of the order of van der Waals (VDW) interactions. The interaction strength is influenced either by polymer ability to wet the surface (hydrophobic or hydrophilic interactions) or by hydrogen bonding between the polymer and the surface treatment.

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.

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.

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).

Bioactive composites with designed interfaces

NASA Astrophysics Data System (ADS)

Orefice, Rodrigo Lambert

Bioactive glasses can bond to bone and even soft tissue. However, they are usually weak, brittle and hard to process in specific shapes. The goal of this work is to produce polymer composites having bioactive materials as a reinforcing phase that would display both bioactive behavior and mechanical properties compatible to bone. Polysulfone and bioactive glass particulate were combined in composites with different volume fractions. Composites with 40 vol.% of particulate were submitted to in vitro tests in simulated body fluids. The recorded rates of hydroxy-carbonate-apatite layer deposition were close to the ones observed for pure bioactive glasses. Mechanical properties showed values of elastic modulus, strain at failure and strength within the range of cortical bone for composites with high volume fraction of particles. Fibers can usually favor higher levels of reinforcement in composites than particles. Novel multicomponent fibers were prepared by using the sol-gel method. They were determined to be bioactive in vitro and were successfully used as a reinforcing phase in polysulfone composites. Properties of the bioactive composites were modified by altering the chemistry and structure of the interfaces. Polymers with sulfonic acid and silane groups were specially designed to interact with both the silica surface and the polymer matrix. Nano-composites with a structure and chemistry in between the macrocomponents of the composite were prepared by combining a silanated polymer and silica sol-gel. When applied as interfacial agents, these nano-composites as well as the modified polymers improved the overall properties of the bioactive system. A decay in mechanical properties was observed for composites submitted to an in vitro test. The developed interfacial agents successfully reduced the degree of degradation in properties. Interactions occurring at the interfaces of bioactive composites were studied using Atomic Force Microscopy (AFM). The effect of the structure and chemistry of interfaces was correlated to physical and chemical processes occurring at the interfaces and to the overall properties of composites.

Ensuring repeatability and robustness of poly(glycidyl methacrylate-co-ethylene dimethacrylate) HPLC monolithic columns of 3 mm id through covalent bonding to the column wall.

PubMed

Laaniste, Asko; Kruve, Anneli; Leito, Ivo

2013-08-01

Two different methods to reinforce the poly(glycidyl methacrylate-co-ethylene dimethacrylate) HPLC monolithic columns of 3 mm id in a glass column reservoir were studied: composite columns with polymeric particles in the monolith and surface treatment of the reservoir wall. Of the two methods used to counter the mechanical instability and formation of flow channels (composite columns and column wall surface treatment), we demonstrated that proper column wall surface treatment was sufficient to solve both problems. Our study also indicated that no surface treatment is efficient, and of the methods studied silanization in acidified ethanol solution and constant renewal of the reaction mixture (dynamic mode) proved to be the most effective. As a result of this study, we have been able to prepare repeatable and durable methacrylate HPLC columns with good efficiencies. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sum-frequency generation analyses of the structure of water at amphoteric SAM-liquid water interfaces.

PubMed

Nomura, Kouji; Nakaji-Hirabayashi, Tadashi; Gemmei-Ide, Makoto; Kitano, Hiromi; Noguchi, Hidenori; Uosaki, Kohei

2014-09-01

Surfaces of both a cover glass and the flat plane of a semi-cylindrical quartz prism were modified with a mixture of positively and negatively charged silane coupling reagents (3-aminopropyltriethoxysilane (APTES) and 3-(trihydroxysilyl)propylmethylphosphonate (THPMP), respectively). The glass surface modified with a self-assembled monolayer (SAM) prepared at a mixing ratio of APTES:THPMP=4:6 was electrically almost neutral and was resistant to non-specific adsorption of proteins, whereas fibroblasts gradually adhered to an amphoteric (mixed) SAM surface probably due to its stiffness, though the number of adhered cells was relatively small. Sum frequency generation (SFG) spectra indicated that total intensity of the OH stretching region (3000-3600cm(-1)) for the amphoteric SAM-modified quartz immersed in liquid water was smaller than those for the positively and negatively charged SAM-modified quartz prisms and a bare quartz prism in contact with liquid water. These results suggested that water molecules at the interface of water and an amphoteric SAM-modified quartz prism are not strongly oriented in comparison with those at the interface of a lopsidedly charged SAM-modified quartz prism and bare quartz. The importance of charge neutralization for the anti-biofouling properties of solid materials was strongly suggested. Copyright © 2014 Elsevier B.V. All rights reserved.

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

The impact of hydrofluoric acid etching followed by unfilled resin on the biaxial strength of a glass-ceramic.

PubMed

Posritong, Sumana; Borges, Alexandre Luiz Souto; Chu, Tien-Min Gabriel; Eckert, George J; Bottino, Marco A; Bottino, Marco C

2013-11-01

To evaluate the null hypotheses that hydrofluoric (HF) acid etching time would neither decrease the biaxial flexural strength of a glass-based veneering ceramic nor enhance it after silane and unfilled resin (UR) applications. Disc-shaped IPS e.max ZirPress specimens were allocated into 12 groups: G1-control (no-etching), G2-30 s, G3-60 s, G4-90 s, G5-120 s, G6-60 s+60 s. Groups (G7-G12) were treated in the same fashion as G1-G6, but followed by silane and UR applications. Surface morphology and roughness (Ra and Rq) of the ceramics were assessed by means of scanning electron microscopy (SEM) and profilometry, respectively. Flexural strength was determined by biaxial testing. Data were analyzed by two-way ANOVA and the Sidak test (α=0.05). Weibull statistics were estimated and finite element analysis (FEA) was carried out to verify the stress concentration end areas of fracture. The interaction (etching time vs. surface treatment) was significant for Ra (p=0.008) and Rq (0.0075). Resin-treated groups presented significantly lower Ra and Rq than non-treated groups, except for the 60s group (p<0.005). SEM revealed that etching affected the ceramic microstructure and that the UR was able to penetrate into the irregularities. A significant effect of etching time (p=0.029) on flexural strength was seen. G7-G12 presented higher strength than G1-G6 (p<0.0001). None of experimental groups failed to show 95% confidence intervals of σ0 and m overlapped. FEA showed lower stress concentration after resin treatment. HF acid etching time did not show a damaging effect on the ceramic flexural strength. Moreover, the flexural strength could be enhanced after UR treatment. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

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

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.

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.

Glassy dynamics of polymethylphenylsiloxane in one- and two-dimensional nanometric confinement—A comparison

NASA Astrophysics Data System (ADS)

Kipnusu, Wycliffe K.; Elsayed, Mohamed; Krause-Rehberg, Reinhard; Kremer, Friedrich

2017-05-01

Glassy dynamics of polymethylphenylsiloxane (PMPS) is studied by broadband dielectric spectroscopy in one-dimensional (1D) and two-dimensional (2D) nanometric confinement; the former is realized in thin polymer layers having thicknesses down to 5 nm, and the latter in unidirectional (thickness 50 μm) nanopores with diameters varying between 4 and 8 nm. Based on the dielectric measurements carried out in a broad spectral range at widely varying temperatures, glassy dynamics is analyzed in detail in 1D and in 2D confinements with the following results: (i) the segmental dynamics (dynamic glass transition) of PMPS in 1D confinement down to thicknesses of 5 nm is identical to the bulk in the mean relaxation rate and the width of the relaxation time distribution function; (ii) additionally a well separated surface induced relaxation is observed, being assigned to adsorption and desorption processes of polymer segments with the solid interface; (iii) in 2D confinement with native inner pore walls, the segmental dynamics shows a confinement effect, i.e., the smaller the pores are, the faster the segmental dynamics; on silanization, this dependence on the pore diameter vanishes, but the mean relaxation rate is still faster than in 1D confinement; (iv) in a 2D confinement, a pronounced surface induced relaxation process is found, the strength of which increases with the decreasing pore diameter; it can be fully removed by silanization of the inner pore walls; (v) the surface induced relaxation depends on its spectral position only negligibly on the pore diameter; (vi) comparing 1D and 2D confinements, the segmental dynamics in the latter is by about two orders of magnitude faster. All these findings can be comprehended by considering the density of the polymer; in 1D it is assumed to be the same as in the bulk, hence the dynamic glass transition is not altered; in 2D it is reduced due to a frustration of packaging resulting in a higher free volume, as proven by ortho-positronium annihilation lifetime spectroscopy.

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.

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°.

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.

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.

Energy efficient synthesis of boranes

DOEpatents

Thorn, David L [Los Alamos, NM; Tumas, William [Los Alamos, NM; Schwarz, Daniel E [Los Alamos, NM; Burrell, Anthony K [Los Alamos, NM

2012-01-24

The reaction of halo-boron compounds (B--X compounds, compounds having one or more boron-halogen bonds) with silanes provides boranes (B--H compounds, compounds having one or more B--H bonds) and halosilanes. Inorganic hydrides, such as surface-bound silane hydrides (Si--H) react with B--X compounds to form B--H compounds and surface-bound halosilanes. The surface bound halosilanes are converted back to surface-bound silanes electrochemically. Halo-boron compounds react with stannanes (tin compounds having a Sn--H bond) to form boranes and halostannanes (tin compounds having a Sn--X bond). The halostannanes are converted back to stannanes electrochemically or by the thermolysis of Sn-formate compounds. When the halo-boron compound is BCl.sub.3, the B--H compound is B.sub.2H.sub.6, and where the reducing potential is provided electrochemically or by the thermolysis of formate.

Energy efficient synthesis of boranes

DOEpatents

Thorn, David L.; Tumas, William; Schwarz, Daniel E.; Burrell, Anthony K.

2010-11-23

The reaction of halo-boron compounds (B--X compounds, compounds having one or more boron-halogen bonds) with silanes provides boranes (B--H compounds, compounds having one or more B--H bonds) and halosilanes. Inorganic hydrides, such as surface-bound silane hydrides (Si--H) react with B--X compounds to form B--H compounds and surface-bound halosilanes. The surface bound halosilanes are converted back to surface-bound silanes electrochemically. Halo-boron compounds react with stannanes (tin compounds having a Sn--H bond) to form boranes and halostannanes (tin compounds having a Sn--X bond). The halostannanes are converted back to stannanes electrochemically or by the thermolysis of Sn-formate compounds. When the halo-boron compound is BCl.sub.3, the B--H compound is B.sub.2H.sub.6, and where the reducing potential is provided electrochemically or by the thermolysis of formate.

Performance of universal adhesives on bonding to leucite-reinforced ceramic.

PubMed

Kim, Ryan Jin-Young; Woo, Jung-Soo; Lee, In-Bog; Yi, Young-Ah; Hwang, Ji-Yun; Seo, Deog-Gyu

2015-01-01

This study aimed to investigate the microshear bond strength of universal bonding adhesives to leucite-reinforced glass-ceramic. Leucite-reinforced glass-ceramic blocks were polished and etched with 9.5% hydrofluoric acid for 1 min. The specimens were assigned to one of four groups based on their surface conditioning (n = 16): 1) NC: negative control with no further treatment; 2) SBU: Single Bond Universal (3M ESPE); 3) ABU: ALL-BOND Universal (Bisco); and 4) PC: RelyX Ceramic Primer and Adper Scotchbond Multi-Purpose Adhesive (3M ESPE) as a positive control. RelyX Ultimate resin cement (3M ESPE) was placed on the pretreated ceramic and was light cured. Eight specimens from each group were stored in water for 24 h, and the remaining eight specimens were thermocycled 10,000 times prior to microshear bond strength evaluation. The fractured surfaces were examined by stereomicroscopy and scanning electron microscopy (SEM). After water storage and thermocycling, the microshear bond strength values decreased in the order of PC > SBU and ABU > NC (P < 0.05). Thermocycling significantly reduced the microshear bond strength, regardless of the surface conditioning used (P < 0.05). Cohesive failure in the ceramic and mixed failure in the ceramic and resin cement were observed in the fractured specimens. The percentage of specimens with cohesive failure after 24 h of water storage was: NC (50%), SBU (75%), ABU (75%), and PC (87%). After thermocycling, the percentage of cohesive failure in NC decreased to 25%; however, yet the percentages of the other groups remained the same. Although the bond strength between resin and hydrofluoric acid-etched glass ceramic was improved when universal adhesives were used, conventional surface conditioning using a separate silane and adhesive is preferable to a simplified procedure that uses only a universal adhesive for cementation of leucite-reinforced glass-ceramic.

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.

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.

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.

Characterization and surface treatment effects on topography of a glass-infiltrated alumina/zirconia-reinforced ceramic.

PubMed

Della Bona, Alvaro; Donassollo, Tiago A; Demarco, Flávio F; Barrett, Allyson A; Mecholsky, John J

2007-06-01

Characterize the microstructure, composition and some physical properties of a glass-infiltrated alumina/zirconia-reinforced ceramic (IZ) and the effect of surface treatment on topography. IZ ceramic specimens were fabricated according to ISO6872 instructions and polished through 1 microm alumina abrasive. Quantitative and qualitative analyses were performed using scanning electron microscopy (SEM), backscattered imaging (BSI), electron dispersive spectroscopy (EDS) and stereology. The elastic modulus (E) and Poisson's ratio (nu) were determined using ultrasonic waves, and the density (rho) using a helium pycnometer. The following ceramic surface treatments were used: AP-as-polished; HF-etching with 9.5% hydrofluoric acid for 90 s; SB-sandblasting with 25 microm aluminum oxide particles for 15s and SC-blasting with 30 microm aluminum oxide particles modified by silica (silica coating) for 15s. An optical profilometer was used to examine the surface roughness (Ra) and SEM-EDS were used to measure the amount of silica after all treatments. The IZ mean property values were as follows: rho=4.45+/-0.01 g/cm(3); nu=0.26 and E=245 GPa. Mean Ra values were similar for AP- and HF-treated IZ but significantly increased after either SC or SB treatment (p

Anti-reflective and anti-soiling coatings for self-cleaning properties

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

Brophy, Brenor L.; Nair, Vinod; Dave, Bakul Champaklal

The disclosure discloses abrasion resistant, persistently hydrophobic and oleophobic, anti-reflective and anti-soiling coatings for glass. The coatings described herein have wide application, including for example the front cover glass of solar modules. Methods of applying the coatings using various apparatus are disclosed. Methods for using the coatings in solar energy generation plants to achieve greater energy yield and reduced operations costs are disclosed. Coating materials are formed by combinations of hydrolyzed silane-base precursors through sol-gel processes. Several methods of synthesis and formulation of coating materials are disclosed.

Motion and shape of partially non-wetting drops on inclined surfaces

NASA Astrophysics Data System (ADS)

Puthenveettil, Baburaj A.; Senthilkumar K, Vijaya; Hopfinger, E. J.; IIT Madras-LEGI Collaboration

2011-11-01

We study high Reynolds number (Re) motion of partially non- wetting liquid drops on inclined surfaces using (i) water on Fluoro-Alkyl Silane (FAS) coated glass and (ii) mercury on glass. The high hysteresis (35°) water drop experiments have been conducted for a range of inclination angles 26° < α <62° which give a range of Capillary numbers 0 . 0003 < Ca < 0 . 0075 and 137 < Re < 3142 . For low hysteresis (6°) mercury on glass experiments, 5 .5° < α < 14 .3° so that 0 . 0002 < Ca < 0 . 0023 and 3037 < Re < 20069 . It is shown that when Re >>103 for water and Re >> 19 for mercury, the observed velocities are accounted for by a boundary layer flow model. The dimensionless velocity in the inertial regime, Ca√{ Re } scales as the modified Bond number (Bom), while Ca Bom at low Re . We show that even at high Re , the dynamic contact angles (θd) depend only on Ca , similar to that in low Re drops. Only the model by Shikhmurzaev is consistent with the variation of dynamic contact angles in both mercury and water drops. We show that the corner transition at the rear of the mercury drop occurs at a finite, receding contact angle, which is predicted by a wedge flow model that we propose. For water drops, there is a direct transition to a rivulet from the oval shape at a critical ratio of receding to static contact angles.

Enhancing Adhesion: Relative Merits of Different Approaches

NASA Technical Reports Server (NTRS)

Penn, L. S.; Pater, R.

1996-01-01

Adhesive performance is improved mainly by manipulation of the bimaterials interface zone, which is only a few molecules thick. There are three approaches to enhancement of interfacial adhesion at the molecular level. They are 1) changing the nonchemically bonded interactions across the interface from weak ones to strong ones, 2) making the true interfacial area much larger than the simple geometric area, and 3) inducing chemical bonding between the two materials forming the interface. Our goal this summer was to question some of the built-in assumptions contained within these approaches and to determine the most promising approach, both theoretically and practically, for enhancing adhesion in NASA structures. Our computations revealed that all three of these approaches have, in theory, the potential to enhance molecular adhesion approximately ten-fold. Experiments, however, revealed that this excellent level of enhancement is not likely to be reached in practice. Each approach was found to be severely limited by practical problems. In addition, some of the built-in assumptions associated with these approaches were found to be insufficient or inadequate. The first approach, changing the nonchemically bonded interactions from weak to strong, Is an example of one containing inadequate assumptions. The extensive literature on intermolecular interactions, based on solution studies, shows that certain functional group pairs interact much more strongly than others. It has always been assumed that these data can be reliably extended to systems where only one member of the pair is in solution and the other Is contained in a solid surface. Our experiments this summer demonstrated that solution data do not adequately predict the strength of functional group interaction at the solid-liquid interface. Furthermore, the strong solvents needed to dissolve the monomers or polymers to which the functional groups of interest are attached compete successfully with the solid surface for the functional group. As a result, functional groups in solution cannot pair with the complementary groups in the solid surface, and the expected enhancement of nonchemically bonded interactions is not realized. The second approach, increasing the true interfacial area, is an example of one containing inadequate assumptions and suffering from numerous practical problems. First, practitioners have assumed that material removal, such as bead blasting or etching, increases true surface area (and therefore interfacial area) in a meaningful way. Our geometric analysis demonstrated that removal methods increase area by a factor of two at most. To increase interfacial area by an order of magnitude or more. a thin layer of high porosity must be added to the substrate surface prior to application of the adhesive phase. Consistent with this finding, we attempted to create a thin layer of rigid, highly porous glass on the surface of our smooth glass substrate by means of sol-gel technology. We were unable to surmount a wide variety of practical problems and obtained only collapsed, nonporous layers. Thus this approach, appealing in principle, would require long term development and is not promising in the near term. The third approach, inducing chemical bonding at the interface, is an example of one having neither inadequate assumptions nor insurmountable practical problems. When silicate glass is the substrate, there are only a few chemical reactions that can be successfully conducted to create these chemical bonds, and these reactions usually involve silicon-containing reagents. We compared the silazane reagents to the silane reagents and found through experiment that the silazanes react with the glass surface much more readily, and under milder conditions, than the silanes. The functional groups attached to the glass surface by silazane reactions were not able to be removed by solvent extraction, elevated temperature exposure, or mechanical action. This clearly indicates that the formation of chemical bonds at the interface is the most effective approach for enhancing molecular adhesion.

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.

Stabilization of gold nanoparticle films on glass by thermal embedding.

PubMed

Karakouz, Tanya; Maoz, Ben M; Lando, Gilad; Vaskevich, Alexander; Rubinstein, Israel

2011-04-01

The poor adhesion of gold nanoparticles (NPs) to glass has been a known obstacle to studies and applications of NP-based systems, such as glass/Au-NP optical devices. Here we present a simple scheme for obtaining stable localized surface plasmon resonance (LSPR) transducers based on Au NP films immobilized on silanized glass and annealed. The procedure includes high-temperature annealing of the Au NP film, leading to partial embedding in the glass substrate and stabilization of the morphology and optical properties. The method is demonstrated using citrate-stabilized Au NPs, 20 and 63 nm mean diameter, immobilized electrostatically on glass microscope cover slides precoated with an aminosilane monolayer. Partial thermal embedding of the Au NPs in the glass occurs at temperatures in the vicinity of the glass transition temperature of the substrate. Upon annealing in air the Au NPs gradually settle into the glass and become encircled by a glass rim. In situ transmission UV-vis spectroscopy carried out during the annealing in a specially designed optical oven shows three regions: The most pronounced change of the surface plasmon (SP) band shape occurs in the first ca. 15 min of annealing; this is followed by a blue-shift of the SP band maximum (up to ca. 5 h), after which a steady red-shift of the SP band is observed (up to ca. 70 h, when the experiment was terminated). The development of the SP extinction spectrum was correlated to changes in the system structure, including thermal modification of the NP film morphology and embedding in the glass. The partially embedded Au NP films pass successfully the adhesive-tape test, while their morphology and optical response are stable toward immersion in solvents, drying, and thiol self-assembly. The enhanced adhesion is attributed to the metal NP embedding and rim formation. The stabilized NP films display a refractive index sensitivity (RIS) of 34-48 nm/RIU and 0.1-0.4 abs.u./RIU in SP band shift and extinction change, respectively. The RIS can be improved significantly by electroless deposition of Au on the embedded NPs, while the system stability is maintained. The method presented provides a simple route to obtaining stable Au NP film transducers. © 2011 American Chemical Society

Evaluation of tensile retention of Y-TZP crowns cemented on resin composite cores: effect of the cement and Y-TZP surface conditioning.

PubMed

Rippe, M P; Amaral, R; Oliveira, F S; Cesar, P F; Scotti, R; Valandro, L F; Bottino, M A

2015-01-01

This study evaluated the effect of the cement type (adhesive resin, self-adhesive, glass ionomer, and zinc phosphate) on the retention of crowns made of yttria-stabilized polycrystalline tetragonal zirconia (Y-TZP). Therefore, 108 freshly extracted molars were embedded in acrylic resin, perpendicular to their long axis, and prepared for full crowns: the crown preparations were removed and reconstructed using composite resin plus fiber posts with dimensions identical to the prepared dentin. The preparations were impressed using addition silicone, and Y-TZP copings were produced, which presented a special setup for the tensile testing. Cementation was performed with two adhesive resin cements (Multilink Automix, Ivoclar-Vivadent; RelyX ARC, 3M ESPE, St Paul, MN, USA), one self-adhesive resin cement (RelyX U100, 3M ESPE), one glass ionomer based cement (RelyX Luting, 3M ESPE), and one zinc phosphate cement (Cimento de Zinco, SS White, Rio de Janeiro, Brazil). For the resin cement groups, the inner surfaces of the crowns were subjected to three surface treatments: cleaning with isopropyl alcohol, tribochemical silica coating, or application of a thin low-fusing glass porcelain layer plus silanization. After 24 hours, all groups were subjected to thermocycling (6000 cycles) and included in a special device for tensile testing in a universal testing machine to test the retention of the infrastructure. After testing, the failure modes of all samples were analyzed under a stereomicroscope. The Kruskal-Wallis test showed that the surface treatment and cement type (α=0.05) affected the tensile retention results. The Multilink cement presented the highest tensile retention values, but that result was not statistically different from RelyX ARC. The surface treatment was statistically relevant only for the Multilink cement. The cement choice was shown to be more important than the crown surface treatment for cementation of a Y-TZP crown to a composite resin substrate.

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.

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

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.

Synthesis and Characterization of a New Class of Thermosetting Resins: Allyl and Propargyl Substituted Cyclopentadiene Derivatives

DTIC Science & Technology

1994-07-15

from Fisher or Aldrich. AS-4 unsized carbon fibers were donated by Hercules Chemical Company and vinyl silane treated glass fibers were donated by Owens ... Corning Fiberglass Company. Composites were made using a mold that gave samples 60 mm long and 12.7 mm wide with variable thickness. Cure analysis

Influence of glass particle size of resin cements on bonding to glass ceramic: SEM and bond strength evaluation.

PubMed

Valentini, Fernanda; Moraes, Rafael R; Pereira-Cenci, Tatiana; Boscato, Noéli

2014-05-01

This study investigated the effect of the filler particle size (micron or submicron) of experimental resin cements on the microtensile bond strength to a glass-ceramic pretreated with hydrofluoric acid (HFA) etching or alumina airborne-particle abrasion (AA). Cements were obtained from a Bis-GMA/TEGDMA mixture filled with 60 mass% micron-sized (1 ± 0.2 µm) or submicron-sized (180 ± 30 µm) Ba-Si-Al glass particles. Ceramic blocks (PM9; VITA) were treated with 10% HFA for 60 s or AA for 15 s. Silane and adhesive were applied. Ceramic blocks were bonded to resin composite blocks (Z250; 3M ESPE) using one of the cements. Bonded specimens were sectioned into beams (n = 20/group) and subjected to microtensile bond strength tests. Data were analyzed using ANOVA and Student-Newman-Keuls' tests (5%). Failure modes were classified under magnification. Morphologies of the treated ceramic surfaces and bonded interfaces were evaluated by scanning electron microscopy. The HFA-submicron group had lower bond strengths than the other groups. All AA-submicron specimens debonded prematurely. Mixed failures were predominant for HFA groups, whereas interfacial failures predominated for AA groups. SEM revealed a honeycomb-like aspect in the HFA-treated ceramic, whereas the AA-treated groups showed an irregular retentive pattern. Continuity of cement infiltration along the bonded interface was more uniform for HFA-treated compared to AA-treated specimens. Cracks toward the bulk of the ceramic were observed in AA-treated specimens. Particle size significantly influenced the ceramic bond strength, whereas surface treatment had a minor effect. Copyright © 2014 Wiley Periodicals, Inc.

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.

Nacre-mimetic bulk lamellar composites reinforced with high aspect ratio glass flakes.

PubMed

Guner, Selen N Gurbuz; Dericioglu, Arcan F

2016-12-05

Nacre-mimetic epoxy matrix composites reinforced with readily available micron-sized high aspect ratio C-glass flakes were fabricated by a relatively simple, single-step, scalable, time, cost and man-power effective processing strategy: hot-press assisted slip casting (HASC). HASC enables the fabrication of preferentially oriented two-dimensional inorganic reinforcement-polymer matrix bulk lamellar composites with a micro-scale structure resembling the brick-and-mortar architecture of nacre. By applying the micro-scale design guideline found in nacre and optimizing the relative volume fractions of the reinforcement and the matrix as well as by anchoring the brick-and-mortar architecture, and tailoring the interface between reinforcements and the matrix via silane coupling agents, strong, stiff and tough bio-inspired nacre-mimetic bulk composites were fabricated. As a result of high shear stress transfer lengths and effective stress transfer at the interface achieved through surface functionalization of the reinforcements, fabricated bulk composites exhibited enhanced mechanical performance as compared to neat epoxy. Furthermore, governed flake pull-out mode along with a highly torturous crack path, which resulted from extensive deflection and meandering of the advancing crack around well-aligned high aspect ratio C-glass flakes, have led to high work-of-fracture values similar to nacre.

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.

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.

A study on the preparation of floating photocatalyst supported by hollow TiO2 and its performance

NASA Astrophysics Data System (ADS)

Wang, Jingang; He, Bin; Kong, Xiang Z.

2015-02-01

This research used hollow glass microspheres (HGMS) as carrier and polystyrene (PSt) as template. PSt was loaded on HGMS surface through the modification by silane coupler. Next, amorphous titanium dioxide (TiO2) produced through tetrabutyl titanate (TBT) hydrolysis precipitated on PSt surface, forming HGMS/PSt/TiO2 particles. Lastly, using the calcinations method, this research obtained anatase TiO2, eliminated PSt, and ultimately acquired composite particles with hollow TiO2 loaded on HGMS surface (HGMSHT). SEM results presented that hollow TiO2 was compact on HGMS surface and a multilayer network structure was formed. The specific surface area of HGMSHT particles was 26 m2/g, which was much larger than that of HGMS/TiO2 (HGMST) composite particles (5.6 m2/g) through direct TBT hydrolysis. Results of catalytic degradation experiment with Rhodamine B and phenol under UV light and sunlight demonstrated that due to larger TiO2 load capacity and specific surface area, the catalytic activity of HGMSHT composite particles was significantly more desirable than that of HGMST, and the catalyst presented satisfactory stability.

Surface treatments for repair of feldspathic, leucite - and lithium disilicate-reinforced glass ceramics using composite resin.

PubMed

Neis, Christian Alencar; Albuquerque, Nadine Luísa Guimarães; Albuquerque, Ivo de Souza; Gomes, Erica Alves; Souza-Filho, Celso Bernardo de; Feitosa, Victor Pinheiro; Spazzin, Aloisio Oro; Bacchi, Atais

2015-01-01

The aim of this study was to evaluate the efficacy of different surface conditioning methods on the microtensile bond strength of a restorative composite repair in three types of dental ceramics: lithium disilicate-reinforced, leucite-reinforced and feldspathic. Twelve blocks were sintered for each type of ceramic (n=3) and stored for 3 months in distilled water at 37 °C. The bonding surface of ceramics was abraded with 600-grit SiC paper. Surface treatments for each ceramic were: GC (control) - none; GDB - diamond bur #30 µm; GHF - hydrofluoric acid (10%); GT- tribochemical silica coating (45-μm size particles). Treatments were followed by cleaning with phosphoric acid 37% for 20 s + silane + adhesive. The composite resin was used as restorative material. After repair, samples were subjected to thermocycled ageing (10,000 cycles between 5 °C and 55 °C for 30 s). Thereafter, the samples were sectioned into 1.0 mm2 sticks and tested for microtensile bond strength with 0.5 mm/min crosshead speed. Data were compared by two-way ANOVA and Tukey's test (α=0.05). The superficial wear with diamond bur proved to be suitable for feldspathic porcelain and for leucite-reinforced glass ceramic while hydrofluoric acid-etching is indicated for repairs in lithium disilicate-reinforced ceramic; tribochemical silica coating is applicable to leucite-reinforced ceramic. Predominance of adhesive failures was observed (>85% in all groups). In conclusion, the success of surface treatments depends on the type of ceramic to be repaired.

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.

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.

Selective accumulation of harmful compounds by the DNA-inorganic hybrid-immobilized glass bead.

PubMed

Yamada, Masanori; Hamai, Akari

2009-08-11

Previously, we reported the DNA-inorganic hybrid material including double-stranded DNA by mixing the aqueous DNA solution and silane coupling reagents. Here, we immobilized the DNA-inorganic hybrid material onto the glass bead and prepared the DNA-immobilized glass bead column. The DNA-immobilized glass beads were stable in water and the amount of eluted DNA from the DNA-glass beads did not change for more than 1 week. Additionally, this DNA-immobilized column selectively accumulated the harmful compounds with the planar structure, such as dioxin- and polychlorinated biphenyl (PCB)-derivatives, and these accumulation percentages were 50-70%. Furthermore, the DNA-immobilized glass bead was recycled nine times by the application of ethanol solution and the accumulative ratio was maintained at more than 60% and did not appear to be decreasing. Therefore, these DNA-columns might have a potential for the selective removal and separation of DNA-intercalating molecules and harmful compounds with the planar structure from experimental or industrial drainages.

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.

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.

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.

Self-etching ceramic primer versus hydrofluoric acid etching: Etching efficacy and bonding performance.

PubMed

El-Damanhoury, Hatem M; Gaintantzopoulou, Maria D

2018-01-01

This study assessed the effect of pretreatment of hybrid and glass ceramics using a self-etching primer on the shear bond strength (SBS) and surface topography, in comparison to pretreatment with hydrofluoric acid and silane. 40 rectangular discs from each ceramic material (IPS e.max CAD;EM, Vita Mark II;VM, Vita Enamic;VE), were equally divided (n=10) and assigned to one of four surface pretreatment methods; etching with 4.8% hydrofluoric acid followed by Monobond plus (HFMP), Monobond etch & prime (Ivoclar Vivadent) (MEP), No treatment (NT) as negative control and Monobond plus (Ivoclar Vivadent) with no etching (MP) as positive control. SBS of resin cement (Multilink-N, Ivoclar Vivadent) to ceramic surfaces was tested following a standard protocol. Surface roughness was evaluated using an Atomic force microscope (AFM). Surface topography and elemental analysis were analyzed using SEM/EDX. Data were analyzed with two-way analysis of variance (ANOVA) and post-hoc Bonferroni test at a significance level of α=0.05. Pretreatment with HFMP resulted in higher SBS and increased surface roughness in comparison to MEP and MP. Regardless the method of surface pretreatment, the mean SBS values of EM ceramic was significantly higher (p<0.05) than those recorded for VM and VE, except when VE was treated with MEP, where the difference was statistically insignificant. Traces of fluoride ion were detected when MEP was used with VE and VM. Under limited conditions, using MEP resulted in comparable SBS results to HFMP; meanwhile HFMP remains the gold standard for pretreatment of glass ceramics for resin-luting cementation. Copyright © 2017 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

Effect of silica coating on fracture strength of glass-infiltrated alumina ceramic cemented to dentin.

PubMed

Xie, Haifeng; Zhu, Ye; Chen, Chen; Gu, Ning; Zhang, Feimin

2011-10-01

To examine the availability of sol-gel processed silica coating for alumina-based ceramic bonding, and determine which silica sol concentration was appropriate for silica coating. Sixty disks of In-Ceram alumina ceramic were fabricated and randomly divided into 5 main groups. The disks received 5 different surface conditioning treatments: Group Al, sandblasted; Group AlC, sandblasted + silane coupling agent applied; Groups Al20C, Al30C, and Al40C, sandblasted, silica coating via sol-gel process prepared using 20 wt%, 30 wt%, and 40 wt% silica sols, and then silane coupling agent applied. Before bonding, one-step adhesives were applied on pre-prepared ceramic surfaces of all groups. Then, 60 dentin specimens were prepared and conditioned with phosphoric acid and one-step adhesive. Ceramic disks of all groups were cemented to dentin specimens with dual-curing resin cements. Fracture strength was determined at 24 h and after 20 days of storage in water. Groups Al20C, Al30C, and Al40C revealed significantly higher fracture strength than groups Al and AlC. No statistically significant difference in fracture strength was found between groups Al and AlC, or among groups Al20C, Al30C, and Al40C. Fracture strength values of all the groups did not change after 20 days of water storage. Sol-gel processed silica coating can enhance fracture strength of In-Ceram alumina ceramic after bonding to dentin, and different silica sol concentrations produced the same effects. Twenty days of water storage did not decrease the fracture strength.

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.

Fatigue failure load of two resin-bonded zirconia-reinforced lithium silicate glass-ceramics: Effect of ceramic thickness.

PubMed

Monteiro, Jaiane Bandoli; Riquieri, Hilton; Prochnow, Catina; Guilardi, Luís Felipe; Pereira, Gabriel Kalil Rocha; Borges, Alexandre Luiz Souto; de Melo, Renata Marques; Valandro, Luiz Felipe

2018-06-01

To evaluate the effect of ceramic thickness on the fatigue failure load of two zirconia-reinforced lithium silicate (ZLS) glass-ceramics, adhesively cemented to a dentin analogue material. Disc-shaped specimens were allocated into 8 groups (n=25) considering two study factors: ZLS ceramic type (Vita Suprinity - VS; and Celtra Duo - CD), and ceramic thickness (1.0; 1.5; 2.0; and 2.5mm). A trilayer assembly (ϕ=10mm; thickness=3.5mm) was designed to mimic a bonded monolithic restoration. The ceramic discs were etched, silanized and luted (Variolink N) into a dentin analogue material. Fatigue failure load was determined using the Staircase method (100,000 cycles at 20Hz; initial fatigue load ∼60% of the mean monotonic load-to-failure; step size ∼5% of the initial fatigue load). A stainless-steel piston (ϕ=40mm) applied the load into the center of the specimens submerged in water. Fractographic analysis and Finite Element Analysis (FEA) were also performed. The ceramic thickness influenced the fatigue failure load for both ZLS materials: Suprinity (716N up to 1119N); Celtra (404N up to 1126N). FEA showed that decreasing ceramic thickness led to higher stress concentration on the cementing interface. Different ZLS glass-ceramic thicknesses influenced the fatigue failure load of the bonded system (i.e. the thicker the glass ceramic is, the higher the fatigue failure load will be). Different microstructures of the ZLS glass-ceramics might affect the fatigue behavior. FEA showed that the thicker the glass ceramic is, the lower the stress concentration at the tensile surface will be. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

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.

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

Magnet-induced temporary superhydrophobic coatings from one-pot synthesized hydrophobic magnetic nanoparticles.

PubMed

Fang, Jian; Wang, Hongxia; Xue, Yuhua; Wang, Xungai; Lin, Tong

2010-05-01

In this paper, we report on the production of superhydrophobic coatings on various substrates (e.g., glass slide, silicon wafer, aluminum foil, plastic film, nanofiber mat, textile fabrics) using hydrophobic magnetic nanoparticles and a magnet-assembly technique. Fe(3)O(4) magnetic nanoparticles functionalized with a thin layer of fluoroalkyl silica on the surface were synthesized by one-step coprecipitation of Fe(2+)/Fe(3+) under an alkaline condition in the presence of a fluorinated alkyl silane. Under a magnetic field, the magnetic nanoparticles can be easily deposited on any solid substrate to form a thin superhydrophobic coating with water contact angle as high as 172 degrees , and the surface superhydrophobicity showed very little dependence on the substrate type. The particulate coating showed reasonable durability because of strong aggregation effect of nanoparticles, but the coating layer can be removed (e.g., by ultrasonication) to restore the original surface feature of the substrates. By comparison, the thin particle layer deposited under no magnetic field showed much lower hydrophobicity. The main reason for magnet-induced superhydrophobic surfaces is the formation of nano- and microstructured surface features. Such a magnet-induced temporary superhydrophobic coating may have wide applications in electronic, biomedical, and defense-related areas.

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

[Effect of hydrofluoric acid etching time on the resin bond durability of glass ceramic].

PubMed

Meng, Xiang-feng; Zhou, Xiao-lu; Luo, Xiao-ping

2010-05-01

To analyze the effect of hydrofluoric acid (HFA) etching time on the resin bond durability of glass ceramic. Three groups of samples of machinable glass ceramic (ProCAD) were etched by 4.8% HFA for 0, 30 and 60 s respectively. The roughness parameters (Ra, Sm, S) and surface area of the samples, were measured with a 3D-laser scanning microscope. Then the ceramic surfaces were bonded with four resin cements (silane coupler/resin cement), which were Monobond S/Variolink II, Clearfil Ceramic Primer/Clearfil Esthetic Cement, GC Ceramic Primer/Linkmax HV, and Porcelain Liner M/SuperBond. The micro-bond strengths between the ceramic and the resin were tested at baseline and after the samples had been treated in 30000 thermal cycles. The Ra [(3.89+/-1.94), (12.53+/-0.80), (13.58+/-1.10) microm] and surface area [(7.81+/-2.96), (30.18+/-2.05), (34.16+/-1.97) mm2] of ceramic increased with the increase of HFA etching time. The thermal cycling test reduced the bond strength of all test groups. The bond strength of Monobond S/Variolink II group [(3.59+/-3.51), (16.18+/-2.62), (20.33+/-2.45) MPa] and Clearfil Ceramic Primer/Clearfil Esthetic Cement group [(4.74+/-2.08), (7.77+/-1.55), (13.45+/-3.75) MPa] increased with the increase of HFA etching time; 30 s HFA etching group of Porcelain Liner M/SuperBond had higher bond strength [(22.00+/-1.64) MPa] than its 0 s HFA etching group [(12.96+/-4.17) MPa], and no significant difference was found between the 30 s and 60 s HFA etching groups of Porcelain Liner M/SuperBond [(20.42+/-3.01) MPa]. HFA etching time had no effect on the bond strength of GC Ceramic Primer/Linkmax HV. HFA etching can improve the resin bond durability of glass ceramic, and the etching time is not only related to the change of ceramic surface roughness and area, but also to the characteristics of resins.

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

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.

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

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.

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.

Lubricant-infused nanoparticulate coatings assembled by layer-by-layer deposition

DOE PAGES

Sunny, Steffi; Vogel, Nicolas; Howell, Caitlin; ...

2014-09-01

Omniphobic coatings are designed to repel a wide range of liquids without leaving stains on the surface. A practical coating should exhibit stable repellency, show no interference with color or transparency of the underlying substrate and, ideally, be deposited in a simple process on arbitrarily shaped surfaces. We use layer-by-layer (LbL) deposition of negatively charged silica nanoparticles and positively charged polyelectrolytes to create nanoscale surface structures that are further surface-functionalized with fluorinated silanes and infiltrated with fluorinated oil, forming a smooth, highly repellent coating on surfaces of different materials and shapes. We show that four or more LbL cycles introducemore » sufficient surface roughness to effectively immobilize the lubricant into the nanoporous coating and provide a stable liquid interface that repels water, low-surface-tension liquids and complex fluids. The absence of hierarchical structures and the small size of the silica nanoparticles enables complete transparency of the coating, with light transmittance exceeding that of normal glass. The coating is mechanically robust, maintains its repellency after exposure to continuous flow for several days and prevents adsorption of streptavidin as a model protein. As a result, the LbL process is conceptually simple, of low cost, environmentally benign, scalable, automatable and therefore may present an efficient synthetic route to non-fouling materials.« less

Lubricant-Infused Nanoparticulate Coatings Assembled by Layer-by-Layer Deposition

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

Sunny, S; Vogel, N; Howell, C

2014-09-01

Omniphobic coatings are designed to repel a wide range of liquids without leaving stains on the surface. A practical coating should exhibit stable repellency, show no interference with color or transparency of the underlying substrate and, ideally, be deposited in a simple process on arbitrarily shaped surfaces. We use layer-by-layer (LbL) deposition of negatively charged silica nanoparticles and positively charged polyelectrolytes to create nanoscale surface structures that are further surface-functionalized with fluorinated silanes and infiltrated with fluorinated oil, forming a smooth, highly repellent coating on surfaces of different materials and shapes. We show that four or more LbL cycles introducemore » sufficient surface roughness to effectively immobilize the lubricant into the nanoporous coating and provide a stable liquid interface that repels water, low-surface-tension liquids and complex fluids. The absence of hierarchical structures and the small size of the silica nanoparticles enables complete transparency of the coating, with light transmittance exceeding that of normal glass. The coating is mechanically robust, maintains its repellency after exposure to continuous flow for several days and prevents adsorption of streptavidin as a model protein. The LbL process is conceptually simple, of low cost, environmentally benign, scalable, automatable and therefore may present an efficient synthetic route to non-fouling materials.« less

Scaling of wet granular flows in a rotating drum

NASA Astrophysics Data System (ADS)

Jarray, Ahmed; Magnanimo, Vanessa; Ramaioli, Marco; Luding, Stefan

2017-06-01

In this work, we investigate the effect of capillary forces and particle size on wet granular flows and we propose a scaling methodology that ensures the conservation of the bed flow. We validate the scaling law experimentally by using different size glass beads with tunable capillary forces. The latter is obtained using mixtures of ethanol-water as interstitial liquid and by increasing the hydrophobicity of glass beads with an ad-hoc silanization procedure. The scaling methodology in the flow regimes considered (slipping, slumping and rolling) yields similar bed flow for different particle sizes including the angle of repose that normally increases when decreasing the particle size.

Preparation and characterization of methacrylate hydrogels for zeta potential control

NASA Technical Reports Server (NTRS)

Gregonis, D. E.; Ma, S. M.; Vanwagenen, R.; Andrade, J. D.

1976-01-01

A technique based on the measurement of streaming potentials has been developed to evaluate the effects of hydrophilic coatings on electroosmotic flow. The apparatus and procedure are described as well as some results concerning the electrokinetic potential of glass capillaries as a function of ionic strength, pH, and temperature. The effect that turbulence and entrance flow conditions have on accurate streaming potential measurements is discussed. Various silane adhesion promoters exhibited only a slight decrease in streaming potential. A coating utilizing a glycidoxy silane base upon which methylcellulose is applied affords a six-fold decrease over uncoated tubes. Hydrophilic methacrylate gels show similar streaming potential behavior, independent of the water content of the gel. By introduction of positive or negative groups into the hydrophilic methacrylate gels, a range of streaming potential values are obtained having absolute positive or negative signs.

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.

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*).

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.

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.

Functionalization of poly(methyl methacrylate) (PMMA) as a substrate for DNA microarrays

PubMed Central

Fixe, F.; Dufva, M.; Telleman, P.; Christensen, C. B. V.

2004-01-01

A chemical procedure was developed to functionalize poly(methyl methacrylate) (PMMA) substrates. PMMA is reacted with hexamethylene diamine to yield an aminated surface for immobilizing DNA in microarrays. The density of primary NH2 groups was 0.29 nmol/cm2. The availability of these primary amines was confirmed by the immobilization of DNA probes and hybridization with a complementary DNA strand. The hybridization signal and the hybridization efficiency of the chemically aminated PMMA slides were comparable to the hybridization signal and the hybridization efficiency obtained from differently chemically modified PMMA slides, silanized glass, commercial silylated glass and commercial plastic Euray™ slides. Immobilized and hybridized densities of 10 and 0.75 pmol/cm2, respectively, were observed for microarrays on chemically aminated PMMA. The immobilized probes were heat stable since the hybridization performance of microarrays subjected to 20 PCR heat cycles was only reduced by 4%. In conclusion, this new strategy to modify PMMA provides a robust procedure to immobilize DNA, which is a very useful substrate for fabricating single use diagnostics devices with integrated functions, like sample preparation, treatment and detection using microfabrication and microelectronic techniques. PMID:14718554

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.

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.

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

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.

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.

[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.

Soft liquid phase adsorption for fabrication of organic semiconductor films on wettability patterned surfaces.

PubMed

Watanabe, Satoshi; Akiyoshi, Yuri; Matsumoto, Mutsuyoshi

2014-01-01

We report a soft liquid-phase adsorption (SLPA) technique for the fabrication of organic semiconductor films on wettability-patterned substrates using toluene/water emulsions. Wettability-patterned substrates were obtained by the UV-ozone treatment of self-assembled monolayers of silane coupling agents on glass plates using a metal mask. Organic semiconductor polymer films were formed selectively on the hydrophobic part of the wettability-patterned substrates. The thickness of the films fabricated by the SLPA technique is significantly larger than that of the films fabricated by dip-coating and spin-coating techniques. The film thickness can be controlled by adjusting the volume ratio of toluene to water, immersion angle, immersion temperature, and immersion time. The SLPA technique allows for the direct production of organic semiconductor films on wettability-patterned substrates with minimized material consumption and reduced number of fabrication steps.

Acoustic actuation of in situ fabricated artificial cilia

NASA Astrophysics Data System (ADS)

Orbay, Sinem; Ozcelik, Adem; Bachman, Hunter; Huang, Tony Jun

2018-02-01

We present on-chip acoustic actuation of in situ fabricated artificial cilia. Arrays of cilia structures are UV polymerized inside a microfluidic channel using a photocurable polyethylene glycol (PEG) polymer solution and photomasks. During polymerization, cilia structures are attached to a silane treated glass surface inside the microchannel. Then, the cilia structures are actuated using acoustic vibrations at 4.6 kHz generated by piezo transducers. As a demonstration of a practical application, DI water and fluorescein dye solutions are mixed inside a microfluidic channel. Using pulses of acoustic excitations, and locally fabricated cilia structures within a certain region of the microchannel, a waveform of mixing behavior is obtained. This result illustrates one potential application wherein researchers can achieve spatiotemporal control of biological microenvironments in cell stimulation studies. These acoustically actuated, in situ fabricated, cilia structures can be used in many on-chip applications in biological, chemical and engineering studies.

Biofunctionalized Nanostructured Zirconia for Biomedical Application: A Smart Approach for Oral Cancer Detection

PubMed Central

Kumar, Suveen; Kumar, Saurabh; Tiwari, Sachchidanand; Srivastava, Saurabh; Srivastava, Manish; Yadav, Birendra Kumar; Kumar, Saroj; Tran, Thien Toan; Dewan, Ajay Kumar; Mulchandani, Ashok; Sharma, Jai Gopal; Maji, Sagar

2015-01-01

Results of the studies are reported relating to application of the silanized nanostructured zirconia, electrophoretically deposited onto indium tin oxide (ITO) coated glass for covalent immobilization of the monoclonal antibodies (anti‐CYFRA‐21‐1). This biosensing platform has been utilized for a simple, efficient, noninvasive, and label‐free detection of oral cancer via cyclic voltammetry technique. The results of electrochemical response studies conducted on bovine serum albumin (BSA)/anti‐CYFRA‐21‐1/3‐aminopropyl triethoxy silane (APTES)/ZrO2/ITO immunoelectrode reveal that this immunoelectrode can be used to measure CYFRA‐21‐1 (oral cancer biomarker) concentration in saliva samples, with a high sensitivity of 2.2 mA mL ng−1, a linear detection range of 2–16 ng mL−1, and stability of six weeks. The results of these studies have been validated via enzyme‐linked immunosorbent assay. PMID:27980963

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.

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

Characterization of a novel ultra low refractive index material for biosensor application

PubMed Central

Memisevic, Jasenka; Korampally, Venumadhav; Gangopadhyay, Shubhra; Grant, Sheila A.

2009-01-01

Nanoporous materials can provide significant benefits to the field of biosensors. Their size and porous structure makes them an ideal tool for improving sensor performance. This study characterized a novel ultra low index of refraction nanoporous organosilicate (NPO) material for use as an optical platform for fluorescence-based optical biosensors. While serving as the low index cladding material, the novel coating based on organosilicate nanoparticles also provides an opportunity for a high surface area coating that can be utilized for immobilizing biological probes. Biological molecules were immobilized onto NPO, which was spin-coated on silicon and glass substrates. The biological molecule was composed of Protein A conjugated to AlexaFluor 546 fluorophore and then immobilized onto the NPO substrate via silanization. Sample analysis consisted of spectrofluorometry, FT-IR spectroscopy, scanning electron microscopy, contact angle measurement and ellipsometry. The results showed the presence of emission peaks at 574 nm, indicating that the immobilization of Protein A to the NPO material is possible. When compared to Si and glass substrates not coated with NPO, the results showed a 100X and 10X increase in packing density with the NPO coated films respectively. Ellipsometric analysis, FT-IR, contact angle, and SEM imaging of the surface immobilized NPO films suggested that while the surface modifications did induce some damage, it did not incur significant changes to its unique characteristics, i.e., pore structure, wettability and index of refraction. It was concluded that NPO films would be a viable sensor substrate to enhance sensitivity and improve sensor performance. PMID:20161155

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.

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.

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

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

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 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.

Flash-induced nanowelding of silver nanowire networks for transparent stretchable electrochromic devices.

PubMed

Lee, Chihak; Oh, Youngsu; Yoon, In Seon; Kim, Sun Hong; Ju, Byeong-Kwon; Hong, Jae-Min

2018-02-09

Electrochromic devices (ECDs) are emerging as a novel technology for various applications like commercialized smart window glasses, and auto-dimming rear-view mirrors. Recently, the development of low-power, lightweight, flexible, and stretchable devices has been accelerated to meet the growing demand in the new wearable devices market. Silver nanowires (AgNWs) can become new primary transparent conducting electrode (TCE) materials to replace indium tin oxide (ITO) for ECDs. However, issues such as substrate adhesion, delamination, and higher resistance still exist with AgNWs. Herein, we report a high-performance stretchable flash-induced AgNW-network-based TCE on surface-treated polydimethylsiloxane (PDMS) substrates. A Xe flash light method was used to create nanowelded networks of AgNWs. Surface silane treatments increased the adhesion and durability of the films as well. Finally, ECDs were fabricated under the optimal conditions and examined under strained conditions to demonstrate the resistance and mechanical behaviours of the devices. Results showed a flexible and durable film maintaining a high level of conductivity and reversible resistance behaviour, beyond those currently achievable with standard ITO/PET flexible TCEs.

Reversible superhydrophobic-superhydrophilic transition of ZnO nanorod/epoxy composite films.

PubMed

Liu, Yan; Lin, Ziyin; Lin, Wei; Moon, Kyoung Sik; Wong, C P

2012-08-01

Tuning the surface wettability is of great interest for both scientific research and practical applications. We demonstrated reversible transition between superhydrophobicity and superhydrophilicity on a ZnO nanorod/epoxy composite film. The epoxy resin serves as an adhesion and stress relief layer. The ZnO nanorods were exposed after oxygen reactive ion etching of the epoxy matrix. A subsequent chemcial treatment with fluoroalkyl and alkyl silanes resulted in a superhydrophobic surface with a water contact angle up to 158.4° and a hysteresis as low as 1.3°. Under UV irradiation, the water contact angle decreased gradually, and the surface eventually became superhydrophilic because of UV induced decomposition of alkyl silanes and hydroxyl absorption on ZnO surfaces. A reversible transition of surface wettability was realized by alternation of UV illumination and surface treatment. Such ZnO nanocomposite surface also showed improved mechanical robustness.

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

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

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.

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.

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.

[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).

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.

Modification of silicon nitride surfaces with GOPES and APTES for antibody immobilization: computational and experimental studies

NASA Astrophysics Data System (ADS)

Dien To, Thien; Nguyen, Anh Tuan; Nhat Thanh Phan, Khoa; Thu Thi Truong, An; Doan, Tin Chanh Duc; Mau Dang, Chien

2015-12-01

Chemical modification of silicon nitride (SiN) surfaces by silanization has been widely studied especially with 3-(aminopropyl)triethoxysilane (APTES) and 3-(glycidyloxypropyl) dimethylethoxysilane (GOPES). However few reports performed the experimental and computational studies together. In this study, surface modification of SiN surfaces with GOPES and APTES covalently bound with glutaraldehyde (GTA) was investigated for antibody immobilization. The monoclonal anti-cytokeratin-FITC (MACF) antibody was immobilized on the modified SiN surfaces. The modified surfaces were characterized by water contact angle measurements, atomic force microscopy and fluorescence microscopy. The FITC-fluorescent label indicated the existence of MACF antibody on the SiN surfaces and the efficiency of the silanization reaction. Absorption of APTES and GOPES on the oxidized SiN surfaces was computationally modeled and calculated by Materials Studio software. The computational and experimental results showed that modification of the SiN surfaces with APTES and GTA was more effective than the modification with GOPES.

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.

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.

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

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.

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

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.

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.

Natural Attenuation of Persistent Chemical Warfare Agent VX ...

EPA Pesticide Factsheets

Report Natural attenuation of persistent CWAs such as VX was investigated and occurs, given sufficient time (days to weeks). Natural attenuation was found to be faster at warmer temperatures (i.e., 35 °C and 25 °C) than cooler temperatures (i.e., 10 °C). Attenuation of VX was material dependent with a general trend of faster to slower attenuation in the order ceramic tile - galvanized metal - silanized glass - painted drywall. Trace amounts of VX may still be present weeks to months after a contamination event.

Application of microstructural optical waveguides with hollow core for enzyme immunoassay

NASA Astrophysics Data System (ADS)

Pidenko, Pavel S.; Pidenko, Sergei A.; Burmistrova, Natalia A.; Shuvalov, Andrei A.; Chibrova, Anastasiya A.; Skibina, Yulia S.; Goryacheva, Irina Y.

2018-04-01

Microstructural optical waveguides with the hollow core are actively studied as a promising support for heterogeneous immunoassay in development of new optical biosensor elements for medicine and biology. Overcoming of the limitations associated with the low sorption capacity of glass used for the waveguides production is a crucial step for this assay format. In this work the possibility of silanization of microstructural optical waveguides with the hollow core using (3-glycidyloxypropyl) trimethoxysilane and their further application to enzymatic immunoassay was studied.

Radio frequency shielding behaviour of silane treated Fe2O3/E-glass fibre reinforced epoxy hybrid composite

NASA Astrophysics Data System (ADS)

Arun prakash, V. R.; Rajadurai, A.

2016-10-01

In this work, radio frequency shielding behaviour of polymer (epoxy) matrixes composed of E-glass fibres and Fe2O3 fillers have been studied. The principal aim of this project is to prepare suitable shielding material for RFID application. When RFID unit is pasted on a metal plate without shielding material, the sensing distance is reduced, resulting in a less than useful RFID system. To improve RF shielding of epoxy, fibres and fillers were utilized. Magnetic behaviour of epoxy polymer composites was measured by hysteresis graphs (B-H) followed by radio frequency identifier setup. Fe2O3 particles of sizes 800, 200 and 100 nm and E-glass fibre woven mat of 600 g/m2 were used to make composites. Particle sizes of 800 nm and 200 nm were prepared by high-energy ball milling, whereas particles of 100 nm were prepared by sol-gel method. To enhance better dispersion of particles within the epoxy matrix, a surface modification process was carried out on fillers by an amino functional coupling agent called 3-Aminopropyltrimethoxysilane (APTMS). Crystalline and functional groups of siliconized Fe2O3 particles were characterized by XRD and FTIR spectroscopy analysis. Variable quantity of E-glass fibre (25, 35, and 45 vol%) was laid down along with 0.5 and 1.0 vol% of 800, 200, and 100 nm size Fe2O3 particles into the matrix, to fabricate the hybrid composites. Scanning electron microscopy and transmission electron microscopy images reveal the shape and size of Fe2O3 particles for different milling times and particle dispersion in the epoxy matrix. The maximum improved sensing distance of 45.2, 39.4 and 43.5 % was observed for low-, high-, and ultra-high radio frequency identifier setup along with shielding composite consist of epoxy, 1 vol% 200 nm Fe2O3 particles and 45 vol% of E-glass fibre.

Flexural properties of denture base polymers reinforced with a glass cloth-urethane polymer composite.

PubMed

Kanie, Takahito; Arikawa, Hiroyuki; Fujii, Koichi; Ban, Seiji

2004-10-01

A newly designed light-cured reinforcement made from urethanemethacrylate oligomer and woven glass cloth has orthotropic anisotropy. This is produced for incorporation into the outermost position under the greatest tension in denture base resins. In this study, the flexural properties of self-, heat-, and light-curing reinforced resins were determined. The silanized glass cloth was soaked in urethanemethacrylate oligomer containing camphorquinone and 2-(dimethylamino)ethylmethacrylate. It was sandwiched between two pieces of polyethylene film and pressed to form a reinforcement sheet 0.3 mm in thickness, which was light-cured and prepared using four different surface conditions: with or without the polyethylene film and with or without a bonding agent. The reinforcement sheet was fixed in a fluorocarbon resin mold 3 mm in thickness, which was filled with self-, heat-, or light-curing resin and cured. The cured laminated plate was cut for flexural testing (40 x 7 x 3 mm3). A three-point flexural test was carried out at a crosshead speed of 2 mm/min and a span length of 30 mm. In this study, the glass fiber content was measured at percentages by weight because it was not possible to determine accurately the volume of the various polymers. The baseline flexural strengths of the self-, heat-, and light-curing resins were 76.2, 68.6, and 55.6 MPa, respectively, and these values were increased to 271.7, 216.4, and 266.5 MPa by the reinforcement sheet. The baseline flexural moduli of self-, heat-, and light-curing resins were 2.0, 2.4, and 2.1 GPa, respectively. These values were increased to 7.2, 5.1, and 6.6 GPa by the reinforcement sheet. SEM photographs revealed good impregnation of the glass fiber within the polymer matrix. The differences in the flexural strengths and flexural moduli of the control and reinforced specimens were significant (p < 0.01).

The effects of corn zein protein coupling agent on mechanical properties of flax fiber reinforced composites

NASA Astrophysics Data System (ADS)

Whitacre, Ryan John

In the field of renewable materials, natural fiber composites demonstrate the capacity to be a viable structural material. When normalized by density, flax fiber mechanical properties are competitive with E-glass fibers. However, the hydrophilic nature of flax fibers reduces the interfacial bond strength with polymer thermosets, limiting composite mechanical properties. Corn zein protein was selected as a natural bio-based coupling agent because of its combination of hydrophobic and hydrophilic properties. Zein was deposited on the surface of flax, which was then processed into unidirectional composite. The mechanical properties of zein treated samples where measured and compared against commonly utilized synthetic treatments sodium hydroxide and silane which incorporate harsh chemicals. Fourier transform infrared spectroscopy, chemical analysis, and scanning electron microscopy were also used to determine analyze zein treatments. Results demonstrate the environmentally friendly zein treatment successfully increased tensile strength 8%, flexural strength 17%, and shear strength 30% compared to untreated samples.

Transparent anti-stain coatings with good thermal and mechanical properties based on polyimide-silica nanohybrids.

PubMed

Choi, Myeon-Cheon; Sung, Giju; Nagappan, Saravanan; Han, Mi-Jeong; Ha, Chang-Sik

2012-07-01

In this work, we synthesized polyimide/silica hybrid materials via sol-gel method using a fluorinated poly(amic acid) silane precursor and a variety of perfluorosilane contents. We studied the influence of a hybrid coating film with the following characteristics; hydrophobicity, oleophobicity, optical transparency, and surface hardness of the coating films. The hybrid coatings with the fluorosilane contents up to 10 wt% are optically transparent and present good thermal stability with a degradation temperature of > 500 degrees C as well as a glass transition of > 300 degrees C. Both water contact angle and oil contact angle increase rapidly with introducing small amount of the fluorosilane in the hybrids and reaches the maximum of 115 degrees and 61 degrees, respectively. The hardness of the hybrid coatings increases up to 5H with an increase of the FTES content in the hybrids. These colorless, transparent, and thermally stable hybrid materials could be suitable for applications as anti-stain coatings.

Self-assembling holographic biosensors and biocomputers.

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

Light, Yooli Kim; Bachand, George David; Schoeniger, Joseph S.

2006-05-01

We present concepts for self-assembly of diffractive optics with potential uses in biosensors and biocomputers. The simplest such optics, diffraction gratings, can potentially be made from chemically-stabilized microtubules migrating on nanopatterned tracks of the motor protein kinesin. We discuss the fabrication challenges involved in patterning sub-micron-scale structures with proteins that must be maintained in aqueous buffers to preserve their activity. A novel strategy is presented that employs dry contact printing onto glass-supported amino-silane monolayers of heterobifunctional crosslinkers, followed by solid-state reactions of these cross-linkers, to graft patterns of reactive groups onto the surface. Successive solution-phase addition of cysteine-mutant proteins andmore » amine-reactive polyethylene glycol allows assembly of features onto the printed patterns. We present data from initial experiments showing successful micro- and nanopatterning of lines of single-cysteine mutants of kinesin interleaved with lines of polyethylene, indicating that this strategy can be employed to arrays of features with resolutions suitable for gratings.« less

Investigation of a biofunctional polymeric coating deposited onto silicon microcantilevers

NASA Astrophysics Data System (ADS)

Bergese, P.; Bontempi, E.; Chiari, M.; Colombi, P.; Damin, F.; Depero, L. E.; Oliviero, G.; Pirri, G.; Zucca, M.

2007-02-01

The paper deals with an appealing route to activate silicon microcantilevers (90, 110 and 130 μm long, 35 μm wide and 2 μm thick) for specific binding of biochemical species. The method consists in coating the underivatized microcantilevers with a biofunctional copolymer (based on N, N-dimethylacrylamide bearing silanating moieties) that was developed for low-density microarray assays on microscope glass slides. Coating deposition was obtained by dip-coating and its microstructure investigated by analyzing the resonance frequency values of bare and coated microcantilevers, by SEM and SFM imaging, SFM tip-scratch tests and XRR experiments. Results indicate that the coating is 2.5 nm thick and has a density of 1.22 g/cm 3. The coating surface is nanostructured, displaying nanoblobs, which are from few up to 20 nm wide and, on average, 1.6 nm high. The diameter of the biggest nanoblobs is of the same order of magnitude of the gyration radius of the copolymer chains, suggesting that nanoblobs may identify individual macromolecules.

Dropwise condensation

PubMed Central

Leach, R. N.; Stevens, F.; Langford, S. C.; Dickinson, J. T.

2008-01-01

Dropwise condensation of water vapor from a naturally cooling, hot water reservoir onto a hydrophobic polymer film and a silanized glass slide was studied by direct observation and simulations. The observed drop growth kinetics suggest that smallest drops grow principally by the diffusion of water adsorbed on the substrate to the drop perimeter, while drops larger than 50 μm in diameter grow principally by direct deposition from the vapor onto the drop surface. Drop coalescence plays a critical role in determining the drop size distribution, and stimulates the nucleation of new, small drops on the substrates. Simulations of drop growth incorporating these growth mechanisms provide a good description of the observed drop size distribution. Because of the large role played by coalescence, details of individual drop growth make little difference to the final drop size distribution. The rate of condensation per unit substrate area is especially high for the smallest drops, and may help account for the high heat transfer rates associated with dropwise condensation relative to filmwise condensation in heat exchange applications. PMID:17014129

The Nanoconfined Free Radical Polymerization: Reaction Kinetics and Thermodynamics

NASA Astrophysics Data System (ADS)

Zhao, Haoyu; Simon, Sindee

The reaction kinetics and thermodynamics of nanoconfined free radical polymerizations are investigated for methyl methacrylate (MMA) and ethyl methacrylate (EMA) monomers using differential scanning calorimetry. Controlled pore glass is used as the confinement medium with pore diameters as small as 7.5 nm; the influence of both hydrophobic (silanized such that trimethylsilyl groups cover the surface) and hydrophilic (native silanol) surfaces is investigated. Propagation rates increase when monomers are reacted in the hydrophilic pores presumably due to the specific interactions between the carbonyl and silanol groups; however, the more flexible EMA monomer shows weaker effects. On the other hand, initial rates of polymerization in hydrophobic pores are unchanged from the bulk. In both pores, the onset of autoacceleration occurs earlier due to the reduced diffusivity of confined chains, which may be compensated at high temperatures. In addition to changes in kinetics, the reaction thermodynamics can be affected under nanoconfinement. Specifically, the ceiling temperature (Tc) is shifted to lower temperatures in nanopores, with pore surface chemistry showing no significant effects; the equilibrium conversion is also reduced at high temperatures below Tc. These observations are attributed to a larger negative change in entropy on propagation for the confined system, with the MMA system again showing greater effects. Funding from ACS PRF is gratefully acknowledged.

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

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.

Controlling surface property of K2SiF6:Mn4+ for improvement of lighting-emitting diode reliability

NASA Astrophysics Data System (ADS)

Kim, Juseong; Jang, Inseok; Song, Gwang Yeom; Kim, Wan-Ho; Jeon, Sie-Wook; Kim, Jae-Pil

2018-05-01

The surface property of moisture-sensitive K2SiF6:Mn4+ (KSF) as a red-emitting phosphor was controlled through dry-type surface modification in order to improve the photo-performance and reliability of lighting-emitting diode (LED). The phosphor surface was modified with silane coupling agents having different carbon chain length by plasma-assisted method. Comparing between as-prepared and modified KSF, water-resistance and photo-emission efficiency were enhanced due to the formation of hydrophobic shell and the elimination of surface quenching sites. Moreover, the dispersibility of phosphor was increased as increasing the carbon chain length of silane because the interfacial affinity between phosphor and encapsulant was improved. After fabricating LED device, the enhancement of photo-performance and long-term reliability could be successfully achieved in LED device with modified phosphor. It is attributed to that the degradation of phosphor efficiency by moisture was suppressed and heat dissipation in LED PKG was improved through the surface modification.

Tribochemical Glass Ceramic Coating as a New Approach for Resin Adhesion to Zirconia.

PubMed

Wandscher, Vinícius Felipe; Fraga, Sara; Pozzobon, João Luiz; Soares, Fabio Zovico Maxnuck; Foletto, Edson Luiz; May, Liliana Gressler; Valandro, Luiz Felipe

To investigate the effects of a novel tribochemical silica coating technique with powders made from feldspathic ceramic and leucite-based ceramic on the bond strength of zirconia to resin cement before and after aging. Zirconia blocks were divided into 3 groups according to the material used for airborne-particle abrasion: 1) SP (control): silica-coated alumina particles; 2) FP: feldspathic ceramic powder; 3) LP: leucite glass-ceramic powder. After silanization, composite resin cylinders were cemented on the zirconia surface using a dual-curing resin cement. Prior to the shear bond strength (SBS) test, half of the samples (n = 15) were stored in distilled water for 24 h; the other half (n = 15) were submitted to aging (10,000 thermocycles of 5°C to 55°C; 150 days of water storage). The bond strength data were analyzed using two-way ANOVA and Tukey's test (α = 0.05). Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and x-ray diffraction analysis were performed. The initial bond strengths did not differ significantly between the groups (p = 0.053). However, after aging procedures, airborne-particle abrasion with feldspathic ceramic powder (FP) resulted in higher values of bond strength (p = 0.0001). SEM and EDS indicated that all the treatments promoted silica deposition on the Y-TZP surface ceramic. Airborne-particle abrasion with FP and LP induced a lower percentage of the monoclinic phase. Airborne abrasion with fine feldspathic ceramic particles is a novel tribochemical technique and appears to be suitable for improving the bond strength between zirconia and resin cements.

An insight into current concepts and techniques in resin bonding to high strength ceramics.

PubMed

Luthra, R; Kaur, P

2016-06-01

Reliable bonding between high strength ceramics and resin composite cement is difficult to achieve because of their chemical inertness and lack of silica content. The aim of this review was to assess the current literature describing methods for resin bonding to ceramics with high flexural strength such as glass-infiltrated alumina and zirconia, densely sintered alumina and yttria-partially stabilized tetragonal zirconia polycrystalline ceramic (Y-TZP) with respect to bond strength and bond durability. Suitable peer reviewed publications in the English language were identified through searches performed in PubMed, Google Search and handsearches. The keywords or phrases used were 'resin-ceramic bond', 'silane coupling agents', 'air particle abrasion', 'zirconia ceramic' and 'resin composite cements'. Studies from January 1989 to June 2015 were included. The literature demonstrated that there are multiple techniques available for surface treatments but bond strength testing under different investigations have produced conflicting results. Within the scope of this review, there is no evidence to support a universal technique of ceramic surface treatment for adhesive cementation. A combination of chemical and mechanical treatments might be the recommended solution. The hydrolytic stability of the resin ceramic bond should be enhanced. © 2016 Australian Dental Association.

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.

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.

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

In vitro shear bond strength of cementing agents to fixed prosthodontic restorative materials.

PubMed

Piwowarczyk, Andree; Lauer, Hans-Christoph; Sorensen, John A

2004-09-01

Durable bonding to fixed prosthodontic restorations is desirable; however, little information is available on the strength of the bond between different cements and fixed prosthodontic restorative materials. This study determined the shear-bond strength of cementing agents to high-gold-content alloy castings and different dental ceramics: high-strength aluminum oxide (Procera AllCeram), leucite-reinforced (IPS Empress), and lithium disilicate glass-ceramic (IPS Empress 2). Prepolymerized resin composite cylinders (5.5 mm internal diameter, n=20) were bonded to the pretreated surfaces of prosthodontic materials. High-gold-content alloy and high-strength aluminum oxide surfaces were airborne-particle-abraded, and pressable ceramics were hydrofluoric acid-etched and silanized prior to cementing. The cementing agents tested were a zinc-phosphate cement (Fleck's zinc cement), glass ionomer cements (Fuji I, Ketac-Cem), resin-modified glass ionomer cements (Fuji Plus, Fuji Cem, RelyX Luting), resin cements (RelyX ARC, Panavia F, Variolink II, Compolute), and a self-adhesive universal resin cement (RelyX Unicem). Half the specimens (n=10) were tested after 30 minutes; the other half (n=10) were stored in distilled water at 37 degrees C for 14 days and then thermal cycled 1000 times between 5 degrees C and 55 degrees C prior to testing. Shear-bond strength tests were performed using a universal testing machine at a constant crosshead speed of 0.5 mm/min. Statistical analysis was performed by multifactorial analysis of variance taking interactions between effects into account. For multiple paired comparisons, the Tukey method was used (alpha=.05). In a 3-way ANOVA model, the main factors substrate, cement, time, and all corresponding interactions were statistically significant (all P <.0001). In subsequent separate 1-way or 2-way ANOVA models for each substrate type, significant differences between cement types and polymerizing modes were found (all P <.001). None of the cement types provided the highest bonding values with all substrate types. After 14 days of water storage followed by thermal cycling, only the self-adhesive universal resin cement (RelyX Unicem) and 2 of the resin cements (Panavia F and Compolute) exhibited strong bond strengths to specific prosthodontic materials. In contrast, zinc-phosphate, glass ionomer, and resin-modified glass ionomer cements showed the lowest values of all tested cementing agents after 14 days of water storage followed by thermal cycling.

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.

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.

A novel approach for UV-patterning with binary polymer brushes.

PubMed

Li, Lifu; Nakaji-Hirabayashi, Tadashi; Kitano, Hiromi; Ohno, Kohji; Saruwatari, Yoshiyuki; Matsuoka, Kazuyoshi

2018-01-01

A mixed self-assembled monolayer (SAM) of an initiator (3-(2-bromo-2-isobutyryloxy)propyl triethoxysilane) for atom transfer radical polymerization (ATRP) and an agent (6-(triethoxysilyl)hexyl 2-(((methylthio)carbonothioyl)thio)-2-phenylacetate) for reversible addition-fragmentation chain transfer (RAFT) polymerization was constructed on the surface of a silicon wafer or glass plate by a silane coupling reaction. When a UV light at 254nm was irradiated at the mixed SAM through a photomask, the surface density of the bromine atom at the end of BPE in the irradiated region was drastically reduced by UV-driven scission of the BrC bond, as observed by X-ray photoelectron spectroscopy. Consequently, the surface-initiated (SI)-ATRP of 2-ethylhexyl methacrylate (EHMA) was used to easily construct the poly(EHMA) (PEHMA) brush domain. Subsequently, SI-RAFT polymerization of a zwitterionic vinyl monomer, carboxymethyl betaine (CMB), was performed. Using the sequential polymerization, the PCMB and PEHMA brush domains on the solid substrate could be very easily patterned. Patterning proteins and cells with the binary polymer brush is expected because the PCMB brush indicated strong suppression of protein adsorption and cell adhesion, and the PEHMA brush had non-polar properties. This technique is very simple and useful for regulating the shape and size of bio-fouling and anti-biofouling domains on solid surfaces. Copyright © 2017 Elsevier B.V. All rights reserved.

Fiber post etching with hydrogen peroxide: effect of concentration and application time.

PubMed

de Sousa Menezes, Murilo; Queiroz, Ellyne Cavalcanti; Soares, Paulo Vinícius; Faria-e-Silva, André Luis; Soares, Carlos José; Martins, Luis Roberto Marcondes

2011-03-01

Etching is necessary to expose the fibers and enable both mechanical and chemical bonding of the resin core to the fiber post. This study evaluated the effect of concentration and application time of hydrogen peroxide on the surface topography and bond strength of glass fiber posts to resin cores. Fiber posts were etched with 24% or 50% hydrogen peroxide for 1, 5, or 10 min (n = 10). Posts without any treatment were used as a control. After etching, the posts were silanated and adhesive resin was applied. The posts were positioned into a mold to allow a self-cured resin core to be inserted. The post/resin assembly was serially sectioned into five beams that were subjected to a tensile bond strength test. Data were subjected to two-way ANOVA and Tukey test (α = 0.05). The surface topography was analyzed using scanning electronic microscopy. Non-etched post presents a relatively smooth surface without fiber exposure. Application of hydrogen peroxide increased the surface roughness and exposed the fibers. All experimental conditions yielded similar bond strength values that were higher than those obtained in the control group. Both 24% and 50% hydrogen peroxide exposure increased the bond strength of resin to the posts, irrespective of the application time. Copyright © 2011 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Feasibility Study Exploring the Potential of Novel Battacin Lipopeptides as Antimicrobial Coatings.

PubMed

De Zoysa, Gayan Heruka; Sarojini, Vijayalekshmi

2017-01-18

Colonization of medical implant surfaces by pathogenic microorganisms causes implant failure and undermines their clinical applicability. Alarming increase in multidrug-resistant bacteria poses serious concerns with the use of medical implants. Antimicrobial peptides (AMPs) that form part of the innate immune system in all forms of life are attractive alternatives to conventional antibiotics to treat multidrug-resistant bacterial biofilms. The aim of this study was to assess the in vitro antibacterial potency of our recently discovered lipopeptides from the battacin family upon immobilization to various surfaces. To achieve this, glass, silicon, and titanium surfaces were functionalized through silanization followed by addition of the heterobifunctional cross-linker, succinimidyl-[N-maleimidopropionamido]-poly(ethylene glycol) ester to generate maleimide-functionalized surfaces. The lipopeptide, GZ3.27, with an added N-terminal cysteine was covalently coupled to the surfaces via a thioether bond through a Michael-type addition between the cysteine sulfhydryl group and the maleimide moiety. Success of surface immobilization and antimicrobial activity of the coated surfaces was assessed using water contact angle measurements, X-ray photoelectron spectroscopy, ellipsometry, scanning electron microscopy, colony forming unit assays and biofilm analysis. The lipopeptide-coated surfaces caused significant damage to the cellular envelop of Pseudomonas aeruginosa (P. aeruginosa) and Escherichia coli (E. coli) upon contact and prevented surface colonization by P. aeruginosa and E. coli biofilms. The lipopeptides investigated in this study were not hemolytic to mouse blood cells in solution. Findings from this study indicate that these lipopeptides have the potential to be developed as promising antimicrobial coatings on medical implants.

Tuning the deposition of molecular graphene nanoribbons by surface functionalization.

PubMed

Konnerth, R; Cervetti, C; Narita, A; Feng, X; Müllen, K; Hoyer, A; Burghard, M; Kern, K; Dressel, M; Bogani, L

2015-08-14

We show that individual, isolated graphene nanoribbons, created with a molecular synthetic approach, can be assembled on functionalised wafer surfaces treated with silanes. The use of surface groups with different hydrophobicities allows tuning the density of the ribbons and assessing the products of the polymerisation process.

Tuning the deposition of molecular graphene nanoribbons by surface functionalization

NASA Astrophysics Data System (ADS)

Konnerth, R.; Cervetti, C.; Narita, A.; Feng, X.; Müllen, K.; Hoyer, A.; Burghard, M.; Kern, K.; Dressel, M.; Bogani, L.

2015-07-01

We show that individual, isolated graphene nanoribbons, created with a molecular synthetic approach, can be assembled on functionalised wafer surfaces treated with silanes. The use of surface groups with different hydrophobicities allows tuning the density of the ribbons and assessing the products of the polymerisation process.

Light Trapping in Thin Film Silicon Solar Cells on Plastic Substrates

NASA Astrophysics Data System (ADS)

de Jong, M. M.

2013-01-01

In the search for sustainable energy sources, solar energy can fulfil a large part of the growing demand. The biggest threshold for large-scale solar energy harvesting is the solar panel price. For drastic cost reductions, roll-to-roll fabrication of thin film silicon solar cells using plastic substrates can be a solution. In this thesis, we investigate the possibilities of depositing thin film solar cells directly onto cheap plastic substrates. Micro-textured glass and sheets, which have a wide range of applications, such as in green house, lighting etc, are applied in these solar cells for light trapping. Thin silicon films can be produced by decomposing silane gas, using a plasma process. In these types of processes, the temperature of the growing surface has a large influence on the quality of the grown films. Because plastic substrates limit the maximum tolerable substrate temperature, new methods have to be developed to produce device-grade silicon layers. At low temperature, polysilanes can form in the plasma, eventually forming dust particles, which can deteriorate device performance. By studying the spatially resolved optical emission from the plasma between the electrodes, we can identify whether we have a dusty plasma. Furthermore, we found an explanation for the temperature dependence of dust formation; Monitoring the formation of polysilanes as a function of temperature using a mass-spectrometer, we observed that the polymerization rate is indeed influenced by the substrate temperature. For solar cell substrate material, our choice was polycarbonate (PC), because of its low cost, its excellent transparency and its relatively high glass transition temperature of 130-140°C. At 130°C we searched for deposition recipes for device quality silicon, using a very high frequency plasma enhanced chemical deposition process. By diluting the feedstock silane with hydrogen gas, the silicon quality can be improved for amorphous silicon (a-Si), until we reach the nanocrystalline silicon (nc-Si) regime. In the nc-Si regime, the crystalline fraction can be further controlled by changing the power input into the plasma. With these layers, a-Si thin film solar cells were fabricated, on glass and PC substrates. The adverse effect of the low temperature growth on the photoactive material is further mitigated by using thinner silicon layers, which can deliver a good current only with an adequate light trapping technique. We have simulated and experimentally tested three light trapping techniques, using embossed structures in PC substrates and random structures on glass: regular pyramid structures larger than the wavelength of light (micropyramids), regular pyramid structures comparable to the wavelength of light (nanopyramids) and random nano-textures (Asahi U-type). The use of nanostructured polycarbonate substrates results in initial conversion efficiencies of 7.4%, compared to 7.6% for cells deposited under identical conditions on Asahi U-type glass. The potential of manufacturing thin film solar cells at processing temperatures lower than 130oC is further illustrated by obtained results on texture-etched aluminium doped zinc-oxide (ZnO:Al) on glass: we achieved 6.9% for nc-Si cells using a very thin absorber layer of only 750 nm, and by combining a-Si and nc-Si cells in tandem solar cells we reached an initial conversion efficiency of 9.5%.

Characterization of Airborne Permethrin During the Manufacture of Army Combat Uniforms Using Pre-Treated Fabric

DTIC Science & Technology

2016-08-01

5 Extraction Apparatus. A.5.1 Accelerated Solvent Extractor (ASE) Dionex Corporation or equal A.5.1.1 Liquid Nitrogen Cylinder to Deliver High...Chromatograph equipped with ChemStation software, or equal A.6.1 Carrier Gas Cylinder , Appropriate Regulator Set at 80psi A.6.2 Hewlett-Packard...Capillary Column, 5% Phenyl Methyl Siloxane/30.0m x 250μm 0.25μm nominal, 325oC Max, or equal. A.6.3 Split Inlet Liner , Packed with Silanized Glass

Proceedings of the Critical Review: Techniques for the Characterization of Composite Materials, held Cambridge, Massachusetts, 8-10 June 1981.

DTIC Science & Technology

1982-05-01

systems were used in this study : SP2)J/E-glass and Fiberite 934/ Kevlar 49. The SP250 resin is a diglycidvl ether of bis;,hennl A (DGEBA)/Epoxy...silane coupling agents to the epoxy resin, and the influence of water pH were particularly studied . The theory of generalized fracture mechanics is...the absorbed moisture water molecules are much more restricted in motion than for free water . Although further laboratory studies are needed to better

Effects of different surface treatments and accelerated artificial aging on the bond strength of composite resin repairs.

PubMed

Melo, Marco Aurélio Veiga de; Moysés, Marcos Ribeiro; Santos, Saulo Galvão dos; Alcântara, Carlos Eduardo Pinto; Ribeiro, José Carlos Rabelo

2011-01-01

The purpose of the present study was to assess the bond strength of composite resin repairs subjected to different surface treatments and accelerated artificial aging. 192 cylindrical samples (CSs) were prepared and divided into 24 groups (n = 8). Half of the CSs were stored in water for 24 h, and the other half were subjected to C-UV accelerated aging for non-metallic specimens. The treatments were phosphoric acid + silane + adhesive (PSA); phosphoric acid + adhesive (PA); diamond bur + phosphoric acid + silane + adhesive (DPSA); diamond bur + phosphoric acid + adhesive (DPA); air abrasion + phosphoric acid + silane + adhesive (APSA); and air abrasion + phosphoric acid + adhesive (APA). The repair was performed and the specimens were again aged as described above. A control group (n = 8) was established and did not receive any type of aging or surface treatment. The specimens were loaded to failure in shear mode with a crosshead speed of 0.5 mm/min until fracture. Data were analyzed by one-way ANOVA/Tukey's test (p < 0.05). No statistically significant differences were found among DPSA, DPA, APSA, APA, and the control group. The aged PSA and PA achieved low bonding values and were statistically different from the control group, whereas the non-aged PSA and PA presented no statistically significant difference from the control group. Repairs with the proposed surface treatments were viable on both recent and aged restorations; however, phosphoric acid + adhesive alone were effective only on recent restorations.

Improved LC-MS/MS method for the quantification of hepcidin-25 in clinical samples.

PubMed

Abbas, Ioana M; Hoffmann, Holger; Montes-Bayón, María; Weller, Michael G

2018-06-01

Mass spectrometry-based methods play a crucial role in the quantification of the main iron metabolism regulator hepcidin by singling out the bioactive 25-residue peptide from the other naturally occurring N-truncated isoforms (hepcidin-20, -22, -24), which seem to be inactive in iron homeostasis. However, several difficulties arise in the MS analysis of hepcidin due to the "sticky" character of the peptide and the lack of suitable standards. Here, we propose the use of amino- and fluoro-silanized autosampler vials to reduce hepcidin interaction to laboratory glassware surfaces after testing several types of vials for the preparation of stock solutions and serum samples for isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). Furthermore, we have investigated two sample preparation strategies and two chromatographic separation conditions with the aim of developing a LC-MS/MS method for the sensitive and reliable quantification of hepcidin-25 in serum samples. A chromatographic separation based on usual acidic mobile phases was compared with a novel approach involving the separation of hepcidin-25 with solvents at high pH containing 0.1% of ammonia. Both methods were applied to clinical samples in an intra-laboratory comparison of two LC-MS/MS methods using the same hepcidin-25 calibrators with good correlation of the results. Finally, we recommend a LC-MS/MS-based quantification method with a dynamic range of 0.5-40 μg/L for the assessment of hepcidin-25 in human serum that uses TFA-based mobile phases and silanized glass vials. Graphical abstract Structure of hepcidin-25 (Protein Data Bank, PDB ID 2KEF).

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.

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.

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

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

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.

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.

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.

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

Mercapto-based coupling agent for improved thermophotovoltaic device back surface reflector adhesion and reflectance

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

Wernsman, Bernard; Fiedor, Joseph N.; Irr, Lawrence G.

2016-10-04

A back surface reflector (BSR) is described. The BSR includes a reflecting layer, a substrate and an adhesion layer between the reflecting layer and the substrate. The adhesion layer includes 3-mercaptopropyl (trimethoxy) silane (a.k.a. Merc).

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 modification of aramid fibers by bio-inspired poly(dopamine) and epoxy functionalized silane grafting.

PubMed

Sa, Rina; Yan, Yan; Wei, Zhenhai; Zhang, Liqun; Wang, Wencai; Tian, Ming

2014-12-10

A novel biomimetic surface modification method for meta-aramid (MPIA) fibers and the improvement on adhesion with rubber matrix was demonstrated. Inspired by the composition of adhesive proteins in mussels, we used dopamine (DOPA) self-polymerization to form thin, surface-adherent poly(dopamine) (PDA) films onto the surface of MPIA fibers simply by immersing MPIA fibers in a dopamine solution at room temperature. An epoxy functionalized silane (KH560) grafting was then carried out on the surface of the poly(dopamine)-coated MPIA, either by a "one-step" or "two-step" method, to introduce an epoxy group onto the MPIA fiber surface. The surface composition and microstructure of the modified MPIA was characterized by X-ray photoelectron spectroscopy (XPS), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The results indicated successful grafting of KH560 on the PDA-coated MPIA surface. A single-fiber pull-out test was applied to evaluate the adhesion of MPIA fibers with the rubber matrix. Compared with the untreated MPIA fibers, the adhesion strength between the modified MPIA fibers by "one step" method with rubber matrix has an increase of 62.5%.

Synthesis of controlled polymeric cross-linked coatings via iniferter polymerisation in the presence of tetraethyl thiuram disulphide chain terminator.

PubMed

Bossi, A; Whitcombe, M J; Uludag, Y; Fowler, S; Chianella, I; Subrahmanyam, S; Sanchez, I; Piletsky, S A

2010-05-15

A "grafting from" approach has been used for controlled deposition of cross-linked polymers by living radical polymerisation. Borosilicate glass was modified with N,N-diethylaminodithiocarbamoylpropyl(trimethoxy)silane, in order to confine the iniferter reactive groups solely at its surface, then placed in solution with monomers and cross-linker. The polymerisation was initiated by UV irradiation. Formation of the cross-linked polymers was studied in terms of time course of the reaction, type of monomers incorporated and influence of oxygen. Grafted surfaces were characterised by AFM, FT-IR, ellipsometry and contact angle measurements. The ability to control the grafted layer improved dramatically when the chain terminator agent, N,N-N',N'-tetraethyl thiuram disulphide (TED) was added. Upon irradiation TED increases the concentration of passive capping radicals and decreases the possibility of recombination of active macro-radicals, thus prolonging their lifetime. In the absence of TED the thickness of produced coatings was below 10 nm. TED added at different concentrations assisted in the formation of grafted layers of 10-130 nm thickness. Iniferter chemistry in the presence of TED can be used for growing nanometre-scale polymer layers on solid supports. It constitutes a robust general platform for controlled grafting and offer a general solution to address the needs of surface derivatisation in sensors technology. 2010 Elsevier B.V. All rights reserved.

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.

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.

Preparation of hydrophobic coatings

DOEpatents

Branson, Eric D [Albuquerque, NM; Shah, Pratik B [Albuquerque, NM; Singh, Seema [Rio Rancho, NM; Brinker, C Jeffrey [Albuquerque, NM

2009-02-03

A method for preparing a hydrophobic coating by preparing a precursor sol comprising a metal alkoxide, a solvent, a basic catalyst, a fluoroalkyl compound and water, depositing the precursor sol as a film onto a surface, such as a substrate or a pipe, heating, the film and exposing the film to a hydrophobic silane compound to form a hydrophobic coating with a contact angle greater than approximately 150.degree.. The contact angle of the film can be controlled by exposure to ultraviolet radiation to reduce the contact angle and subsequent exposure to a hydrophobic silane compound to increase the contact angle.

Creep of experimental short fiber-reinforced composite resin.

PubMed

Garoushi, Sufyan; Kaleem, Muhammad; Shinya, Akikazu; Vallittu, Pekka K; Satterthwaite, Julian D; Watts, David C; Lassila, Lippo V J

2012-01-01

The purpose of this study was to investigate the reinforcing effect of short E-glass fiber fillers oriented in different directions on composite resin under static and dynamic loading. Experimental short fiber-reinforced composite resin (FC) was prepared by mixing 22.5 wt% of short E-glass fibers, 22.5 wt% of resin, and 55 wt% of silane-treated silica fillers. Three groups of specimens (n=5) were tested: FC with isotropic fiber orientation, FC with anisotropic fiber orientation, and particulate-filled composite resin (PFC) as a control. Time-dependent creep and recovery were recorded. ANOVA revealed that after secondary curing in a vacuum oven and after storage in dry condition for 30 days, FC with isotropic fiber orientation (1.73%) exhibited significantly lower static creep value (p<0.05) than PFC (2.54%). For the different curing methods and storage conditions evaluated in this study, FC achieved acceptable static and dynamic creep values when compared to PFC.

Thermally Induced Silane Dehydrocoupling on Silicon Nanostructures (International ed.)

DTIC Science & Technology

2016-07-29

grafted. When performed on a mesopo- rous Si wafer, the perfluoro reagent yields a superhydrophobic surface (contact angle 1518). The bromo-derivative... superhydrophobic behavior, with a water contact angle of 1508 (Figure S13 and S14). As with the octadecylsilane derivative, these surface chemistries were not

A Self Consistent RF Discharge, Plasma Chemistry and Surface Model for Plasma Enhanced Chemical Vapor Deposition

DTIC Science & Technology

1988-06-30

consists of three submodels for the electron kinetics, plasma chemistry , and surface deposition kinetics for a-Si:H deposited from radio frequency...properties. Plasma enhanced, Chemical vapor deposition, amorphous silicon, Modeling, Electron kinetics, Plasma chemistry , Deposition kinetics, Rf discharge, Silane, Film properties, Silicon.

Fluorescence sensor for water in organic solvents prepared from covalent immobilization of 4-morpholinyl-1, 8-naphthalimide.

PubMed

Niu, Cheng-Gang; Qin, Pin-Zhu; Zeng, Guang-Ming; Gui, Xiao-Qin; Guan, Ai-Ling

2007-02-01

A new fluorescent dye, N-allyl-4-morpholinyl-1,8-naphthalimide (AMN), was synthesized as a fluorescence indicator in the fabrication of a sensor for determining water content in organic solvents. To prevent leakage of the fluorophore, AMN was photo-copolymerized with acrylamide, (2-hydroxyethyl)methacrylate, and triethylene glycol dimethacrylate on a glass surface treated with a silanizing agent. The sensing mechanism is based on the solvatochromic feature of the covalently immobilized AMN. The fluorescence intensity of AMN decreased with increasing water contents when it was excited at 400 nm. In the range of ca. 0.00-4.40% (v/v), the fluorescence intensity of AMN changed as a linear function of water content. The sensor exhibited satisfactory reproducibility, reversibility, and a response time (t (99)) of the order of 50 s. The detection limit was solvent-dependent, when acetonitrile was used as the solvent, and the detection limit could be as low as 0.006% (v/v) of water. Additionally, the prepared sensor is pH-insensitive and possesses a relatively long lifetime of at least one month.

Effect of various surface treatment methods on the bond strength of the heat-pressed ceramic samples.

PubMed

Saraçoğlu, A; Cura, C; Cötert, H S

2004-08-01

This in vitro study was conducted to evaluate the interaction between the shear bond strength and the surface treatment method for a commercial dental ceramic. Ninety bonded ceramic units were manufactured for this study. Each unit was made by luting two cylinder-shaped ceramic samples to each other with a resin-composite luting agent. The units were then divided into nine groups, containing 10 units in each group. Samples from each group were treated with one of the following: etching with 4.9% hydrofluoric acid for 10, 20 and 40 s, 9.5% hydrofluoric acid for 10, 20 and 40 s, 40% orthophosphoric acid for 40 s, air abrasion with alumina in 50-microm particles, and grinding with a high-speed diamond bur. The treated samples were then silanated and luted with a resin-composite luting agent. The luted units were then loaded to failure. Two samples from each group were neither silanated nor luted after the surface treatment procedure, and morphological changes obtained by various surface treatment regimens were investigated by scanning electron microscopy. A statistically significant difference was observed among the mean shear bond strengths of the groups prepared with different surface treatment techniques (P = 0.00). Hydrofluoric acid appeared to be the most suitable chemical medium to produce a reliable ceramic bond. Etching time and concentration of the acidic medium were also observed as important prognostic variates. Orthophosphoric acid treatment was observed to be the least effective surface treatment method on the heat-pressed ceramic samples. Physical applications such as bur grinding and air blasting maintained stronger bonds than the orthophosphoric acid, while producing weaker bonds than surfaces treated with hydrofluoric acid in all concentrations and etching periods. The effect of the silane priming agent was not considered in this study. Copyright 2004 Blackwell Publishing Ltd.

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.

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.

Development of DNA biosensor based on TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Nadzirah, Sh.; Hashim, U.; Rusop, M.

2018-05-01

A novel technique of DNA hybridization on the TiO2 nanoparticles film was developed by dropping a single droplet of target DNA onto the surface of TiO2 for the study of various concentrations of target DNA. The surface of TiO2 nanoparticle film was functionalized with APTES and covalently immobilized with 1 µM probe DNA on the silanized TiO2 nanoparticles surface. The effect of silanization, immobilization and hybridization were quantitatively measured by the output current signal obtained using a picoammeter. The 1 µM target DNA was found to be the most effective target towards the 1 µM probe DNA as the output current signal was within range; while the output current signal of the 10 µM target DNA was observed to beyond the range of the probe DNA control due to the excessive concentration as compared to the probe DNA. This approach has several advantages such as rapid, simple, low cost, and sensitive current signal during detection of different target DNA concentrations.

Effect of an internal coating technique on tensile bond strengths of resin cements to zirconia ceramics.

PubMed

Kitayama, Shuzo; Nikaido, Toru; Maruoka, Rena; Zhu, Lei; Ikeda, Masaomi; Watanabe, Akihiko; Foxton, Richard M; Miura, Hiroyuki; Tagami, Junji

2009-07-01

This study was conducted to enhance the tensile bond strengths of resin cements to zirconia ceramics. Fifty-six zirconia ceramic specimens (Cercon Base) and twenty-eight silica-based ceramic specimens (GN-1, GN-1 Ceramic Block) were air-abraded using alumina. Thereafter, the zirconia ceramic specimens were divided into two subgroups of 28 each according to the surface pretreatment; no pretreatment (Zr); and the internal coating technique (INT). For INT, the surface of zirconia was coated by fusing silica-based ceramics (Cercon Ceram Kiss). Ceramic surfaces were conditioned with/without a silane coupling agent followed by bonding with one of two resin cements; Panavia F 2.0 (PF) and Superbond C&B (SB). After 24 hours storage in water, the tensile bond strengths were tested (n=7). For both PF and SB, silanization significantly improved the bond strength to GN-1 and INT (p<0.05). The INT coating followed by silanizaton demonstrated enhancement of bonding to zirconia ceramics.

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.

Fracture Strength of Monolithic All-Ceramic Crowns on Titanium Implant Abutments.

PubMed

Weyhrauch, Michael; Igiel, Christopher; Scheller, Herbert; Weibrich, Gernot; Lehmann, Karl Martin

2016-01-01

The fracture strengths of all-ceramic crowns cemented on titanium implant abutments may vary depending on crown materials and luting agents. The purpose of this study was to examine differences in fracture strength among crowns cemented on implant abutments using crowns made of seven different monolithic ceramic materials and five different luting agents. In total, 525 crowns (75 each of Vita Mark II, feldspathic ceramic [FSC]; Ivoclar Empress CAD, leucite-reinforced glass ceramic [LrGC]; Ivoclar e.max CAD, lithium disilicate [LiDS]; Vita Suprinity, presintered zirconia-reinforced lithium silicate ceramic [PSZirLS]; Vita Enamic, polymer-reinforced fine-structure feldspathic ceramic [PolyFSP], Lava Ultimate; resin nanoceramic [ResNC], Celtra Duo; fully crystallized zirconia-reinforced lithium silicate [FcZirLS]) were milled using a CAD/CAM system. The inner surfaces of the crowns were etched and silanized. Titanium implant abutments were fixed on implant analogs, and airborne-particle abrasion was used on their exterior specific adhesion surfaces (Al2O3, 50 μm). Then, the abutments were degreased and silanized. The crowns were cemented on the implant abutments using five luting agents (Multilink Implant, Variolink II, RelyX Unicem, GC FujiCEM, Panavia 2.0). After thermocycling for 5,000 cycles (5 to 55°C, 30 seconds dwell time), the crowns were subjected to fracture strength testing under static load using a universal testing machine. Statistical analyses were performed using analysis of variance (α = .0002) and the Bonferroni correction. No significant difference among the luting agents was found using the different all-ceramic materials. Ceramic materials LiDS, PSZirLS, PolyFSP, and ResNC showed significantly higher fracture strength values compared with FSC, FcZirLS, and LrGC. The PSZirLS especially showed significantly better results. Within the limitations of this study, fracture strength was not differentially affected by the various luting agents. However, the fracture strength was significantly higher for PSZirLS, PolyFSP, ResNC, and LiDS ceramics than for the FSP, LrGC, and the FcZirLS ceramic with all luting agents tested.

Effect of functional end groups of silane self assembled monolayer surfaces on apatite formation, fibronectin adsorption and osteoblast cell function

PubMed Central

Toworfe, G.K.; Bhattacharyya, S.; Composto, R.J.; Adams, C.S.; Shapiro, I.M.; Ducheyne, P.

2008-01-01

Bioactive glass (BG) can directly bond to living bone without fibrous tissue encapsulation. Key mechanistic steps of BG’s activity are attributed to calcium phosphate formation, surface hydroxylation and fibronectin (FN) adsorption. In the present study, self-assembled monolayers (SAMs) of alkanesilanes with different surface chemistry (OH, NH2, and COOH) were used as a model system to mimic BG’s surface activity. Calcium phosphate (Ca-P) was formed on SAMs by immersion in a solution which simulates the electrolyte content of physiological fluids. FN adsorption kinetics and monolayer coverage was determined on SAMs with or without Ca-P coating. The surface roughness was also examined on these substrates before and after FN adsorption. The effects of FN-adsorbed, Ca-P coated SAMs on the function of MC3T3-E1 were evaluated by cell growth, expression of alkaline phosphatase activity, and actin cytoskeleton formation. We demonstrate that, although the FN monolayer coverage and the rms roughness are similar on −OH and −COOH terminated SAMs with or without Ca-P coating, higher levels of ALP activity, more actin cytoskeleton formation and more cell growth are obtained on −OH and −COOH terminated SAMs with Ca-P coating. In addition, although the FN monolayer coverage is higher on Ca-P coated −NH2 terminated SAMs and SiOx surfaces, higher levels of ALP activity and more cell growth are obtained on Ca-P coated −OH and −COOH terminated SAMs. Thus with same Ca-P coatings, different surface functional groups have different effects on the function of osteoblastic cells. These findings represent new insights into the mechanism of bioactivity of BG and, thereby, may lead to designing superior constructs for bone grafting. PMID:19012271

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.

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.

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.

Endothelialization of polyurethanes: Surface silanization and immobilization of REDV peptide.

PubMed

Butruk-Raszeja, Beata A; Dresler, Magdalena S; Kuźmińska, Aleksandra; Ciach, Tomasz

2016-08-01

The paper presents method for chemical immobilization of arginine-glutamic acid-aspartic acid-valine (REDV) peptide on polyurethane surface. The peptide has been covalently bonded using silanes as a spacer molecules. The aim of this work was to investigate the proposed modification process and assess its biological effectiveness, especially in contact with blood and endothelial cells. Physicochemical properties were examined in terms of wettability, atomic composition and density of introduced functional groups and peptide molecules. Experiments with blood showed that material coating reduced number of surface-adhered platelets and fibrinogen molecules. In contrast to polyurethane (PU), there were no blood components deposited on REDV-modified materials (PU-REDV); fibrinogen adsorption on PU-REDV surface has been strongly reduced compared to PU. Analysis of cell adhesion after 1, 2, 3, 4, and 5 days of culture showed a significant increase of the cell-coated area on PU-REDV compared to PU. However, an intense cell growth appeared also on the control surface modified without the addition of REDV. Thus, the positive effect of REDV peptide on the adhesion of HUVEC could not be unequivocally confirmed. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

SPM analysis of fibrinogen adsorption on solid surfaces

NASA Astrophysics Data System (ADS)

Choukourov, A.; Grinevich, A.; Saito, N.; Takai, O.

2007-09-01

The adsorption kinetics, adhesion and orientation of human fibrinogen on solid surfaces have been studied by surface probe microscopy (SPM) and quartz crystal microbalance techniques (QCM). CF 3-, NH 2-terminated organo-silane self-assembled monolayers (SAM) and OH-terminated silicon dioxide have been used as model surfaces. Furthermore, the interaction of fibrinogen with nanocomposite Ti/hydrocarbon plasma polymer films (Ti/ppCH) deposited by dc magnetron sputtering has also been studied.

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

Silicon cantilever functionalization for cellulose-specific chemical force imaging of switchgrass

DOE PAGES

Lee, Ida; Evans, Barbara R.; Foston, Marcus B.; ...

2015-05-08

A method for direct functionalization of silicon and silicon nitride cantilevers with bifunctional silanes was tested with model surfaces to determine adhesive forces for different hydrogen-bonding chemistries. Application for biomass surface characterization was tested by mapping switchgrass and isolated switchgrass cellulose in topographic and force-volume mode using a cellulose-specific cantilever.

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.

Real-time dissolution measurement of sized and unsized calcium phosphate glass fibers.

PubMed

Rinehart, J D; Taylor, T D; Tian, Y; Latour, R A

1999-01-01

The objective of this study was to develop an efficient "real time" measurement system able to directly measure, with microgram resolution, the dissolution rate of absorbable glass fibers, and utilize the system to evaluate the effectiveness of silane-based sizing as a means to delay the fiber dissolution process. The absorbable glass fiber used was calcium phosphate (CaP), with tetramethoxysilane selected as the sizing agent. E-glass fiber was used as a relatively nondegrading control. Both the unsized-CaP and sized-CaP degraded linearly at both the 37 degrees C and 60 degrees C test temperature levels used. No significant decrease in weight-loss rate was recorded when the CaP fiber tows were pretreated, using conventional application methods, with the tetramethoxysilane sizing for either temperature condition. The unsized-CaP and sized-CaP weight loss rates were each significantly higher at 60 than at 37 degrees C (both p < 0.02), as expected from dissolution kinetics. In terms of actual weight loss rate measured using our system for phosphate glass fiber, the unsized-CaP fiber we studied dissolved at a rate of 10.90 x 10(-09) and 41.20 x 10(-09) g/min-cm(2) at 37 degrees C and 60 degrees C, respectively. Considering performance validation of the developed system, the slope of the weight loss vs. time plot for the tested E-glass fiber was not significantly different compared to a slope equal to zero for both test temperatures. Copyright 1999 John Wiley & Sons, Inc.

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

NASA Astrophysics Data System (ADS)

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

2014-10-01

In this paper, we study the two-step dip coating via a sol-gel process to prepare superhydrophobic silica films on the glass substrate. The water repellency of the silica films was controlled by surface silylation method using isooctyltrimethoxysilane (iso-OTMS) as a surface modifying agent. Silica alcosol was synthesized by keeping the molar ratio of ethyltriethoxysilane (ETES) precursor, ethanol (EtOH) solvent, water (H2O) was kept constant at 1:36:6.6 respectively, with 6 M NH4OH throughout the experiment and the percentages of hydrophobic agent in hexane bath was varied from 0 to 15 vol.%. The static water contact angle values of the silica films increased from 108° to 160° with an increase in the vol.% of iso-OTMS. At 15 vol%. of iso-OTMS, the silica film shows static water contact angle as high as 160°. The superhydrophobic silica films are thermally stable up to 440 °C and above this temperature, the silica films lose superhydrophobicity. By controlling the primer particle size of SiO2 about 26 nm, leading to decrease the final size of silica nanoparticles after modification of nanoparticles by isooctyltrimethoxysilane about 42 nm. The films are transparent and have uniform size on the surface. The silica films have been characterized by atomic force microscopy (AFM), fourier transform infrared spectroscopy (FT-IR), transparency, contact angle measurement (CA), Zeta-potential, Thermal stability by TG-DTA analysis.

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.

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.

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

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.

Porcelain surface conditioning protocols and shear bond strength of orthodontic brackets.

PubMed

Lestrade, Ashley M; Ballard, Richard W; Xu, Xiaoming; Yu, Qingzhao; Kee, Edwin L; Armbruster, Paul C

2016-05-01

The objective of the present study was to determine which of six bonding protocols yielded a clinically acceptable shear bond strength (SBS) of metal orthodontic brackets to CAD/CAM lithium disilicate porcelain restorations. A secondary aim was to determine which bonding protocol produced the least surface damage at debond. Sixty lithium disilicate samples were fabricated to replicate the facial surface of a mandibular first molar using a CEREC CAD/CAM machine. The samples were split into six test groups, each of which received different mechanical/chemical pretreatment protocols to roughen the porcelain surface prior to bonding a molar orthodontic attachment. Shear bond strength testing was conducted using an Instron machine. The mean, maximum, minimal, and standard deviation SBS values for each sample group including an enamel control were calculated. A t-test was used to evaluate the statistical significance between the groups. No significant differences were found in SBS values, with the exception of surface roughening with a green stone prior to HFA and silane treatment. This protocol yielded slightly higher bond strength which was statistically significant. Chemical treatment alone with HFA/silane yielded SBS values within an acceptable clinical range to withstand forces applied by orthodontic treatment and potentially eliminates the need to mechanically roughen the ceramic surface.

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.

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.

Evaluation of treatment options for ASR-affected concrete : final report, December 11, 2009.

DOT National Transportation Integrated Search

2009-12-11

This research project was undertaken to evaluate the potential of using surface treatments including lithium nitrate, : sodium tartarate, siloxanes, silane, and boiled linseed oil to mitigate or slow the rate of concrete deterioration : associated wi...

Drop-wise and film-wise water condensation processes occurring on metallic micro-scaled surfaces

NASA Astrophysics Data System (ADS)

Starostin, Anton; Valtsifer, Viktor; Barkay, Zahava; Legchenkova, Irina; Danchuk, Viktor; Bormashenko, Edward

2018-06-01

Water condensation was studied on silanized (superhydrophobic) and fluorinated (superoleophobic) micro-rough aluminum surfaces of the same topography. Condensation on superhydrophobic surfaces occurred via film-wise mechanism, whereas on superoleophobic surfaces it was drop-wise. The difference in the pathways of condensation was attributed to the various energy barriers separating the Cassie and Wenzel wetting states on the investigated surfaces. The higher barriers inherent for superoleophobic surfaces promoted the drop-wise condensation. Triple-stage kinetics of growth of droplets condensed on superoleophobic surfaces is reported and discussed.

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.

Coordination-based gold nanoparticle layers.

PubMed

Wanunu, Meni; Popovitz-Biro, Ronit; Cohen, Hagai; Vaskevich, Alexander; Rubinstein, Israel

2005-06-29

Gold nanoparticle (NP) mono- and multilayers were constructed on gold surfaces using coordination chemistry. Hydrophilic Au NPs (6.4 nm average core diameter), capped with a monolayer of 6-mercaptohexanol, were modified by partial substitution of bishydroxamic acid disulfide ligand molecules into their capping layer. A monolayer of the ligand-modified Au NPs was assembled via coordination with Zr4+ ions onto a semitransparent Au substrate (15 nm Au, evaporated on silanized glass and annealed) precoated with a self-assembled monolayer of the bishydroxamate disulfide ligand. Layer-by-layer construction of NP multilayers was achieved by alternate binding of Zr4+ ions and ligand-modified NPs onto the first NP layer. Characterization by atomic force microscopy (AFM), ellipsometry, wettability, transmission UV-vis spectroscopy, and cross-sectional transmission electron microscopy showed regular growth of NP layers, with a similar NP density in successive layers and gradually increased roughness. The use of coordination chemistry enables convenient step-by-step assembly of different ligand-possessing components to obtain elaborate structures. This is demonstrated by introducing nanometer-scale vertical spacing between a NP layer and the gold surface, using a coordination-based organic multilayer. Electrical characterization of the NP films was carried out using conductive AFM, emphasizing the barrier properties of the organic spacer multilayer. The results exhibit the potential of coordination self-assembly in achieving highly controlled composite nanostructures comprising molecules, NPs, and other ligand-derivatized components.

Preparation of epoxy-based macroporous monolithic columns for the fast and efficient immunofiltration of Staphylococcus aureus.

PubMed

Ott, Sonja; Niessner, Reinhard; Seidel, Michael

2011-08-01

Macroporous epoxy-based monolithic columns were used for immunofiltration of bacteria. The prepared monolithic polymer support is hydrophilic and has large pore sizes of 21 μm without mesopores. A surface chemistry usually applied for immobilization of antibodies on glass slides is successfully transferred to monolithic columns. Step-by-step, the surface of the epoxy-based monolith is hydrolyzed, silanized, coated with poly(ethylene glycol diamine) and activated with the homobifunctional crosslinker di(N-succinimidyl)carbonate for immobilization of antibodies on the monolithic columns. The functionalization steps are characterized to ensure the coating of each monolayer. The prepared antibody-immobilized monolithic column is optimized for immunofiltration to enrich Staphylococcus aureus as an important food contaminant. Different kinds of geometries of monolithic columns, flow rates and elution buffers are tested with the goal to get high recoveries in the shortest enrichment time as possible. An effective capture of S. aureus was achieved at a flow rate of 7.0 mL/min with low backpressures of 20.1±5.4 mbar enabling a volumetric enrichment of 1000 within 145 min. The bacteria were quantified by flow cytometry using a double-labeling approach. After immunofiltration the sensitivity was significantly increased and a detection limit of the total system of 42 S. aureus/mL was reached. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

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.

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.

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.

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.

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.

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.

Thermal cycling effects on adhesion of resin-bovine enamel junction among different composite resins.

PubMed

Chen, Wen-Cheng; Ko, Chia-Ling; Wu, Hui-Yu; Lai, Pei-Ling; Shih, Chi-Jen

2014-10-01

Thermal cycling is used to mimic the changes in oral cavity temperature experienced by composite resins when used clinically. The purpose of this study is to assess the thermal cycling effects of in-house produced composite resin on bonding strength. The dicalcium phosphate anhydrous filler surfaces are modified using nanocrystals and silanization (w/NP/Si). The resin is compared with commercially available composite resins Filtek Z250, Z350, and glass ionomer restorative material GIC Fuji-II LC (control). Different composite resins were filled into the dental enamel of bovine teeth. The bond force and resin-enamel junction graphical structures of the samples were determined after thermal cycling between 5 and 55°C in deionized water for 600 cycles. After thermal cycling, the w/NP/Si 30wt%, 50wt% and Filtek Z250, Z350 groups showed higher shear forces than glass ionomer GIC, and w/NP/Si 50wt% had the highest shear force. Through SEM observations, more of the fillings with w/NP/Si 30wt% and w/NP/Si 50wt% groups flowed into the enamel tubule, forming closed tubules with the composite resins. The push-out force is proportional to the resin flow depth and uniformity. The push-out tubule pore and resin shear pattern is the most uniform and consistent in the w/NP/Si 50wt% group. Accordingly, this developed composite resin maintains great mechanical properties after thermal cycling. Thus, it has the potential to be used in a clinical setting when restoring non-carious cervical lesions. Copyright © 2014 Elsevier Ltd. All rights reserved.

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...

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.

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.

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.

Repair bond strength of nanohybrid composite resins with a universal adhesive

PubMed Central

Altinci, Pinar; Mutluay, Murat; Tezvergil-Mutluay, Arzu

2018-01-01

Abstract Objective: To investigate the repair bond strength of fresh and aged nanohybrid and hybrid composite resins using a universal adhesive (UA). Materials and methods: Fresh and aged substrates were prepared using two nanohybrid (Venus Pearl, Heraus Kulzer; Filtek Supreme XTE, 3 M ESPE) and one hybrid (Z100, 3 M ESPE) composite resin, and randomly assigned to different surface treatments: (1) no treatment (control), (2) surface roughening with 320-grit (SR), (3) SR + UA (iBOND, Heraus Kulzer), (4) SR + Silane (Signum, Ceramic Bond I, Heraeus Kulzer) + UA, (5) SR + Sandblasting (CoJet, 3 M ESPE) + Silane + UA. After surface treatment, fresh composite resin was added to the substrates at 2 mm layer increments to a height of 5 mm, and light cured. Restored specimens were water-stored for 24 h and sectioned to obtain 1.0 × 1.0 mm beams (n = 12), and were either water-stored for 24 h at 37 °C, or water-stored for 24 h, and then thermocycled for 6000 cycles before microtensile bond strength (µTBS) testing. Data were analyzed with ANOVA and Tukey’s HSD tests (p = .05). Results: Combined treatment of SR, sandblasting, silane and UA provided repair bond strength values comparable to the cohesive strength of each tested resin material (p < .05). Thermocycling significantly reduced the cohesive strength of the composite resins upto 65% (p < .05). Repair bond strengths of UA-treated groups were more stable under thermocycling. Conclusions: Universal adhesive application is a reliable method for composite repair. Sandblasting and silane application slightly increases the repair strength for all substrate types. PMID:29250576

Repair bond strength of nanohybrid composite resins with a universal adhesive.

PubMed

Altinci, Pinar; Mutluay, Murat; Tezvergil-Mutluay, Arzu

2018-01-01

Objective: To investigate the repair bond strength of fresh and aged nanohybrid and hybrid composite resins using a universal adhesive (UA). Materials and methods: Fresh and aged substrates were prepared using two nanohybrid (Venus Pearl, Heraus Kulzer; Filtek Supreme XTE, 3 M ESPE) and one hybrid (Z100, 3 M ESPE) composite resin, and randomly assigned to different surface treatments: (1) no treatment (control), (2) surface roughening with 320-grit (SR), (3) SR + UA (iBOND, Heraus Kulzer), (4) SR + Silane (Signum, Ceramic Bond I, Heraeus Kulzer) + UA, (5) SR + Sandblasting (CoJet, 3 M ESPE) + Silane + UA. After surface treatment, fresh composite resin was added to the substrates at 2 mm layer increments to a height of 5 mm, and light cured. Restored specimens were water-stored for 24 h and sectioned to obtain 1.0 × 1.0 mm beams ( n  = 12), and were either water-stored for 24 h at 37 °C, or water-stored for 24 h, and then thermocycled for 6000 cycles before microtensile bond strength (µTBS) testing. Data were analyzed with ANOVA and Tukey's HSD tests ( p  = .05). Results: Combined treatment of SR, sandblasting, silane and UA provided repair bond strength values comparable to the cohesive strength of each tested resin material ( p  < .05). Thermocycling significantly reduced the cohesive strength of the composite resins upto 65% ( p  < .05). Repair bond strengths of UA-treated groups were more stable under thermocycling. Conclusions: Universal adhesive application is a reliable method for composite repair. Sandblasting and silane application slightly increases the repair strength for all substrate types.

Factors affecting the cement-post interface.

PubMed

Zicari, F; De Munck, J; Scotti, R; Naert, I; Van Meerbeek, B

2012-03-01

To evaluate the effect of different factors on the push-out bond strength of glass fiber posts luted in simulated (standard) root canals using different composite cements. Three types of glass-fiber root-canal posts with a different matrix, namely an epoxy resin (RelyX post, 3M ESPE), a proprietary composite resin (FRC-Plus post, Ivoclar-Vivadent), and a methacrylate resin (GC post, GC), and three types of composite cements, namely an etch-and-rinse Bis-GMA-based (Variolink II, Ivoclar-Vivadent), a self-etch 10-MDP-based (Clearfil Esthetic Cement, Kuraray) and a self-adhesive (RelyX Unicem, 3M ESPE) cement, were tested. Posts were either left untreated (control), were treated with silane, or coated with silicated alumina particles (Cojet system, 3M ESPE). Posts were inserted up to 9-mm depth into composite CAD-CAM blocks (Paradigm, 3M ESPE) in order to solely test the strength of the cement-post interface, while excluding interference of the cement-dentin interface. After 1-week storage at 37 °C, three sections (coronal, middle, apical) of 2-mm thickness were subjected to a push-out bond-strength test. All three variables, namely the type of post, the composite cement and the post-surface pre-treatment, were found to significantly affect the push-out bond strength (p<0.001). Regarding the type of post, a significantly lower push-out bond strength was recorded for the FRC-Plus post (Ivoclar-Vivadent); regarding the composite cement, a significantly higher push-out bond strength was recorded for the self-adhesive cement Unicem (3M ESPE); and regarding the post-surface treatment, a significantly higher push-out bond strength was recorded when the post-surface was beforehand subjected to a Cojet (3M ESPE) combined sandblasting/silicatization surface pre-treatment. Many interactions between these three variables were found to be significant as well (p<0.001). Finally, the push-out bond strength was found to significantly reduce with depth from coronal to apical. Laboratory testing revealed that different variables like the type of post, the composite cement and the post-surface pre-treatment may influence the cement-post interface, making clear guidelines for routine clinical practice hard to define. Further long-term durability testing may help to clarify, and should therefore be encouraged. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

Cytotoxicity of silica-glass fiber reinforced composites.

PubMed

Meriç, Gökçe; Dahl, Jon E; Ruyter, I Eystein

2008-09-01

Silica-glass fiber reinforced polymers can be used for many kinds of dental applications. The fiber reinforcement enhances the mechanical properties of the polymers, and they have good esthetic attributes. There is good initial bonding of glass fibers to polymers via an interface made from silane coupling agents. The aim of this in vitro study was to determine the cytotoxicity of two polymers reinforced with two differently sized silica-glass fibers before and after thermal cycling. Cytotoxicity of the polymers without fibers was also evaluated. Two different resin mixtures (A and B) were prepared from poly(vinyl chloridecovinylacetate) powder and poly(methyl methacrylate) (PMMA) dissolved in methyl methacrylate and mixed with different cross-linking agents. The resin A contained the cross-linking agents ethylene glycol dimethacrylate and 1,4-butanediol dimethacrylate, and for resin B diethylene glycol dimethacrylate was used. Woven silica-glass fibers were used for reinforcement. The fibers were sized with either linear poly(butyl methacrylate)-sizing or cross-linking PMMA-sizing. Cytotoxicity was evaluated by filter diffusion test (ISO 7405:1997) of newly made and thermocycled test specimens. Extracts were prepared according to ISO 10993-12 from newly made and from thermocycled specimens and tested by the MTT assay. The results from the experiments were statistically analyzed by one-way ANOVA and Tukey's test (rho<0.05). The filter diffusion test disclosed no change in staining intensity at the cell-test sample contact area indicating non-cytotoxicity in all experimental groups. Cell viability assessed by MTT assay was more than 90% in all experimental groups. All are non-cytotoxic. It can be concluded that correctly processed heat polymerized silica-glass fiber reinforced polymers induced no cytotoxicity and that thermocycling did not alter this property.

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.

Synthesis of amino-silane modified superparamagnetic Fe{sub 3}O{sub 4} nanoparticles and its application in immobilization of lipase from Pseudomonas fluorescens Lp1

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

Kanimozhi, S., E-mail: skanimo@gmail.com; Perinbam, K.

2013-05-15

Highlights: ► Magnetic nanoparticles were synthesized by chemical co-precipitation method. ► Surface was functionalized with amino-silane and used for lipase immobilization. ► Characterized through TEM, SEM, XRD, FT-IR and VSM analysis. ► The functionalization and immobilization did not affect the magnetite properties. ► The immobilized lipase showed greater functional property than free lipase. - Abstract: Superparamagnetic nanoparticles (Fe{sub 3}O{sub 4}–magnetite) were prepared by chemical co-precipitation method and their surface was functionalized with 3-aminopropyltriethoxysilane via silanization reaction to obtain amino functionalized magnetic nanoparticles. The purified lipase from Pseudomonas fluorescens Lp1 was immobilized onto functionalized magnetite using glutaraldehyde as the coupling agent.more » The characterization of the nanoparticles was done by scanning electron microscopy, transmission electron microscopy, powder X-ray diffraction, vibrating sample magnetometry and Fourier transformed infrared spectroscopy. The size of the magnetite was measured about 10–30 nm. The results of characterization study revealed the successful immobilization of lipase on to functionalized magnetite. The saturation magnetization of magnetic nanoparticles was found to be 28.34 emu/g whereas the immobilized magnetic nanoparticle was 17.074 emu/g. The immobilized lipase had greater activity at 50 °C and thermal stability upto 70 °C. It exhibited excellent reusability for 4 cycles and storage stability upto 15 days by retaining 75% of its initial activity.« less

Stability and reactivity of dimethylethoxysilane

NASA Technical Reports Server (NTRS)

Johnson, Richard E.; Ford, Douglas I.

1992-01-01

Dimethylethoxysilane (DMES) is currently used to treat the High-temperature Reusable Surface Insulation (HRSI) shuttle tiles in order to provide a hydrophobic surface on the silica. DMES is a volatile, reactive silane that incorporates two reactive sites, the ethoxy group and the silica-hydride group. The work reported in this paper focused on the reactivity of these two groups with silica, water, quantitative reagents, and within DMES itself.

Evaluation of Contact Friction in Fracture of Rotationally Bent Nitinol Endodontic Files

NASA Astrophysics Data System (ADS)

Haimed, Tariq Abu

2011-12-01

The high flexibility of rotary Nitinol (Ni-Ti) files has helped clinicians perform root canal treatments with fewer technical errors than seen with stainless steel files. However, intracanal file fracture can occur, compromising the outcome of the treatment. Ni-Ti file fracture incidence is roughly around 4% amongst specialists and higher amongst general practitioners. Therefore, eliminating or reducing this problem should improve patient care. The aim of this project was to isolate and examine the role of friction between files and the canal walls of the glass tube model, and bending-related maximum strain amplitudes, on Ni-Ti file lifetimes-tofracture in the presence of different irrigant solutions and file coatings. A specifically designed device was used to test over 300 electropolished EndoSequenceRTM Ni-Ti files for number of cycles to failure (NCF) in smooth, bent glass tube models at 45 and 60 degrees during dry, coated and liquid-lubricated rotation at 600rpm. Fractured files were examined under Scanning Electron Microscopy (SEM) afterwards. Four different file sizes 25.04, 25.06, 35.04, 35.06 (diameter in mm/taper %) and six surface modification conditions were used independently. These conditions included, three solutions; (1) a surfactant-based solution, Surface-Active-Displacement-Solution (SADS), (2) a mouth wash proven to remove biofilms, Delmopinol 1%(DEL), and (3) Bleach 6% (vol.%), the most common antibacterial endodontic irrigant solution. The conditions also included two low-friction silane-based coating groups, 3-Hepta-fluoroisopropyl-propoxymethyl-dichlorosilane (3-HEPT) and Octadecyltrichlorosilane (ODS), in addition to an as-received file control group (Dry). The coefficient of friction (CF) between the file and the canal walls for each condition was measured as well as the surface tension of the irrigant solutions and the critical surface tension of the coated and uncoated files by contact angle measurements. The radius of curvature and maximum strain amplitude (MSA) for each file size were determined based on images of the files inside the glass tubes. The force of insertion for each file type under each condition was also measured inside 45 and 60 degree glass tube paths, static and while dynamic. The results showed that NCF of Ni-Ti files is strongly inversely related to the CF which ranged from 0.15 for ODS and 3-HEPT coated files to 0.43 for irrigant bleach. High CF (in the presence of bleach) significantly reduced the NCF. Conversely, lower CF (in the presence of other solutions and file coatings) resulted in significantly higher NCF. CF was found to be directly related to the surface tension of the media used. Similarly, high MSA typical of low radius of curvature and high bending angle significantly diminished the fatigue life of Ni-Ti files. The integral of the force of insertion versus time curve was the highest for bleach irrigation which also showed the highest CF. Scanning electron microscope inspection of file fracture surfaces illustrated a 2-step progressive failure mode characterized by creation of a smooth initial fatigue area (striation marks) followed by catastrophic ductile fracture (dimple area) when the intact file shaft area was sufficiently reduced. The bleach-lubricated files failed earlier and with a smaller fatigue area (23%) than all other groups (31-35%) indicating premature fracture in the presence of higher frictional forces. The acquired data demonstrate that the combination of low MSA and low CF (by using coatings or solutions with low surface tension), related to the magnitude of the superficial drag force, can lead to statistically longer rotational bending lifetimes for Ni-Ti files. Based on the data of this study, lubricant solutions with low surface tension could significantly improve the fracture life of Ni-Ti files in root canal glass model. Laboratory testing using natural teeth should be performed to evaluate the effect of using such solutions on the fatigue life of Ni-Ti files.

Engineering and characterization of mesoporous silica-coated magnetic particles for mercury removal from industrial effluents

NASA Astrophysics Data System (ADS)

Dong, Jie; Xu, Zhenghe; Wang, Feng

2008-03-01

Mesoporous silica coatings were synthesized on dense liquid silica-coated magnetite particles using cetyl-trimethyl-ammonium chloride (CTAC) as molecular templates, followed by sol-gel process. A specific surface area of the synthesized particles as high as 150 m 2/g was obtained. After functionalization with mercapto-propyl-trimethoxy-silane (MPTS) through silanation reaction, the particles exhibited high affinity of mercury in aqueous solutions. Atomic force microscopy (AFM), zeta potential measurement, thermal gravimetric analysis (TGA), analytical transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and atomic absorption spectroscopy (AAS) were used to characterize the synthesis processes, surface functionalization, and mercury adsorption on the synthesized magnetite particles. The loading capacity of the particles for mercury was determined to be as high as 14 mg/g at pH 2. A unique feature of strong magnetism of the synthesized nanocomposite particles makes the subsequent separation of the magnetic sorbents from complex multiphase suspensions convenient and effective.

Enhancement of anticorrosion property of 304 stainless steel using silane coatings

NASA Astrophysics Data System (ADS)

Akhtar, Sultan; Matin, Asif; Madhan Kumar, A.; Ibrahim, Ahmed; Laoui, Tahar

2018-05-01

In the present work, silane coatings based on glycidoxypropyltrimethoxysilane/methyltrimethoxysilane (GPTMS/MTMS) and silica nanoparticles were prepared by a sol-gel method. A simple dip-coating method was applied for film deposition and the effect of immersion time and number of immersion cycles on corrosion behavior of 304 stainless steel (SS) was investigated. Scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDS) was used to study the surface morphology and elemental composition of the modified surfaces. The corrosion behavior of the coated and uncoated SS substrates was studied by potentiodynamic polarization and electrochemical impedance spectroscopy in 0.6 M sodium chloride solution. Our results showed that the presence of coatings improved the anti-corrosion property of SS substrates. The coating with a dipping time of 10 min and 3 dipping cycles exhibited the best protection efficiency compared to other coatings and the uncoated substrate. SEM/EDS findings and contact angle measurements supported the conclusions drawn from the corrosion study.

Fabrication of surface micro- and nanostructures for superhydrophobic surfaces in electric and electronic applications

NASA Astrophysics Data System (ADS)

Xiu, Yonghao

In our study, the superhydrophobic surface based on biomimetic lotus leave is explored to maintain the desired properties for self-cleaning. Parameters in controlling bead-up and roll-off characteristics of water droplets were investigated on different model surfaces. The governing equations were proposed. Heuristic study is performed. First, the fundamental understanding of the effect of roughness on superhydrophobicity is performed. The effect of hierarchical roughness, i.e., two scale roughness effect on roughness is investigated using systems of (1) monodisperse colloidal silica sphere (submicron) arrays and Au nanoparticle on top and (2) Si micrometer pyramids and Si nanostructures on top from KOH etching and metal assisted etching of Si. The relation between the contact area fraction and water droplet contact angles are derived based on Wenzel and Cassie-Baxter equation for the systems and the two scale effect is explained regarding the synergistic combination of two scales. Previously the microscopic three-phase-contact line is thought to be the key factor in determining contact angles and hystereses. In our study, Laplace pressure was brought up and related to the three-phase-contact line and taken as a key figure of merit in determining superhydrophobicity. In addition, we are one of the first to study the effect of tapered structures (wall inclination). Combining with a second scale roughness on the tapered structures, stable Cassie state for both water and low surface energy oil may be achieved. This is of great significance for designing both superhydrophobicity and superoleophobicity. Regarding the origin of contact angle hysteresis, study of superhydrophobicity on micrometer Si pillars was performed. The relation between the interface work of function and contact angle hysteresis was proposed and derived mathematically based on the Young-Dupre equation. The three-phase-contact line was further related to a secondary scale roughness induced. Based on our understanding of the roughness effect on superhydrophobicity (both contact angle and hysteresis), structured surfaces from polybutadiene, polyurethane, silica, and Si etc. were successfully prepared. For engineering applications of superhydrophobic surfaces, stability issues regarding UV, mechanical robustness and humid environment need to be investigated. Among these factors, UV stability is the first one to be studied. However, most polymer surfaces we prepared failed the purpose. Silica surfaces with excellent UV stability were prepared. This method consists of preparation of rough silica surfaces, thermal treatment and the following surface hydrophobization by fluoroalkyl silane treatment. Fluoroalkyl groups are UV stable and the underlying species are silica which is also UV stable (UV transparent). UV stability on the surface currently is 5,500 h according the standard test method of ASTM D 4329. No degradation on surface superhydrophobicity was observed. New methods for preparing superhydrophobic and transparent silica surfaces were investigated using urea-choline chloride eutectic liquid to generate fine roughness and reduce the cost for preparation of surface structures. Another possible application for self-cleaning in photovoltaic panels was investigated on Si surfaces by construction of the two-scale rough structures followed by fluoroalkyl silane treatment. Metal (Au) assisted etching was employed to fabricate nanostructures on micrometer pyramid surfaces. The light reflection on the prepared surfaces was investigated. After surface texturing using KOH etching for micrometer pyramids and the following nanostructure using metal assisted etching, surface light reflection reduced to a minimum value which shows that this surface texturing technique is highly promising for improving the photovoltaic efficiency while imparting photovoltaics the self-cleaning feature. This surface is also expected to be UV stable due to the same fluoroalkyl silane used. Regarding the mechanical robustness, epoxy-silica superhydrophobic surfaces were prepared by O2 plasma etching to generate enough surface roughness of silica spheres followed by fluoroalkyl silane treatment. A robustness test method was proposed and the test results showed that the surface is among the most robust surfaces for the superhydrophobic surfaces we prepared and currently reported in literature.

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.

Fluorinated silica microchannel surfaces

DOEpatents

Kirby, Brian J.; Shepodd, Timothy Jon

2005-03-15

A method for surface modification of microchannels and capillaries. The method produces a chemically inert surface having a lowered surface free energy and improved frictional properties by attaching a fluorinated alkane group to the surface. The coating is produced by hydrolysis of a silane agent that is functionalized with either alkoxy or chloro ligands and an uncharged C.sub.3 -C.sub.10 fluorinated alkane chain. It has been found that the extent of surface coverage can be controlled by controlling the contact time from a minimum of about 2 minutes to a maximum of 120 minutes for complete surface coverage.

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

Monomolecular Silane Coatings on Magnesium/Aluminium Fuels

DTIC Science & Technology

1991-07-01

iii SUMMARY The aim of this project was to investigate the curing reaction between CTBN and magnesium/aluminium ailoy surfaces. A dispersion of...performing rheoloqacai experiments with these coated magnesium particles and CTBN . Surface analysis ot the alloys show a nigh percentage of magnesium...Rheoloq’cai analysis of these alloys dispersed 40% w/w in CTBN show increasing rates of change in viscosity with time for each alloy with increasing nominal

Functionalization of Titanium with Chitosan via Silanation: Evaluation of Biological and Mechanical Performances

PubMed Central

Renoud, Pauline; Toury, Bérangère; Benayoun, Stéphane; Attik, Ghania; Grosgogeat, Brigitte

2012-01-01

Complications in dentistry and orthopaedic surgery are mainly induced by peri-implant bacterial infections and current implant devices do not prevent such infections. The coating of antibacterial molecules such as chitosan on its surface would give the implant bioactive properties. The major challenge of this type of coating is the attachment of chitosan to a metal substrate. In this study, we propose to investigate the functionalization of titanium with chitosan via a silanation. Firstly, the surface chemistry and mechanical properties of such coating were evaluated. We also verified if the coated chitosan retained its biocompatibility with the peri-implant cells, as well as its antibacterial properties. FTIR and Tof-SIMS analyses confirmed the presence of chitosan on the titanium surface. This coating showed great scratch resistance and was strongly adhesive to the substrate. These mechanical properties were consistent with an implantology application. The Chitosan-coated surfaces showed strong inhibition of Actinomyces naeslundii growth; they nonetheless showed a non significant inhibition against Porphyromonas gingivalis after 32 hours in liquid media. The chitosan-coating also demonstrated good biocompatibility to NIH3T3 fibroblasts. Thus this method of covalent coating provides a biocompatible material with improved bioactive properties. These results proved that covalent coating of chitosan has significant potential in biomedical device implantation. PMID:22859940

Effect of Surface-Modified TiO2 Nanoparticles on the Anti-Ultraviolet Aging Performance of Foamed Wheat Straw Fiber/Polypropylene Composites

PubMed Central

Xuan, Lihui; Han, Guangping; Wang, Dong; Cheng, Wanli; Gao, Xun; Chen, Feng; Li, Qingde

2017-01-01

Surface modification and characterization of titanium dioxide (TiO2) nanoparticles and their roles in thermal, mechanical, and accelerated aging behavior of foamed wheat straw fiber/polypropylene (PP) composites are investigated. To improve the dispersion of nanoparticles and increase the possible interactions between wheat straw fiber and the PP matrix, the surface of the TiO2 nanoparticles was modified with ethenyltrimethoxy silane (A171), a silane coupling agent. The grafting of A171 on the TiO2 nanoparticles’ surface was characterized by Fourier transform infrared spectroscopy (FTIR). The wheat straw fibers treated with A171 and modified TiO2 nanoparticles were characterized by FTIR and thermogravimetric analysis (TGA). FTIR spectra confirmed that the organic functional groups of A171 were successfully grafted onto the TiO2 nanoparticles and wheat straw fibers, and the modified TiO2 nanoparticles were adsorbed onto the wheat straw fibers. Thermogravimetric analysis showed that a higher thermal stability of the wheat straw fiber was obtained with the modified TiO2 nanoparticles. The flexural, tensile, and impact properties were improved. A higher ultraviolet (UV) stability of the samples treated with modified TiO2 nanoparticles was exhibited by the study of the color change and loss in mechanical properties. PMID:28772816

Bone-like apatite coating on functionalized poly(etheretherketone) surface via tailored silanization layers technique.

PubMed

Zheng, Yanyan; Xiong, Chengdong; Zhang, Shenglan; Li, Xiaoyu; Zhang, Lifang

2015-10-01

Poly(etheretherketone) (PEEK) is a rigid semi-crystalline polymer with outstanding mechanical properties, bone-like stiffness and suitable biocompatibility that has attracted much interest as a biomaterial for orthopedic and dental implants. However, the bio-inert surface of PEEK limits its biomedical applications when direct osteointegration between the implants and the host tissue is desired. In this work, -PO4H2, -COOH and -OH groups were introduced on the PEEK surface by further chemical treatments of the vinyl-terminated silanization layers formed on the hydroxylation-pretreated PEEK surface. Both the surface-functionalized and pristine specimens were characterized by X-ray photoelectron spectroscopy (XPS), attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy and water contact angle measurements. When placed in 1.5 strength simulated body fluid (SBF) solution, apatite was observed to form uniformly on the functionalized PEEK surface and firmly attach to the substrate. The characterized results demonstrated that the coating was constituted by poorly crystallized bone-like apatite and the effect of surface functional groups on coating formation was also discussed in detail. In addition, in vitro biocompatibility of PEEK, in terms of pre-osteoblast cell (MC3T3-E1) attachment, spreading and proliferation, was remarkably enhanced by the bone-like apatite coating. Thus, this study provides a method to enhance the bioactivity of PEEK and expand its applications in orthopedic and dental implants. Copyright © 2015 Elsevier B.V. All rights reserved.

Tribology and stability of organic monolayers on CrN: a comparison among silane, phosphonate, alkene, and alkyne chemistries.

PubMed

Pujari, Sidharam P; Li, Yan; Regeling, Remco; Zuilhof, Han

2013-08-20

The fabrication of chemically and mechanically stable monolayers on the surfaces of various inorganic hard materials is crucial to the development of biomedical/electronic devices. In this Article, monolayers based on the reactivity of silane, phosphonate, 1-alkene, and 1-alkyne moieties were obtained on the hydroxyl-terminated chromium nitride surface. Their chemical stability and tribology were systematically investigated. The chemical stability of the modified CrN surfaces was tested in aqueous media at 60 °C at pH 3, 7, and 11 and monitored by static water contact angle measurements, X-ray photoelectron spectroscopy (XPS), ellipsometry, and Fourier transform infrared reflection absorption spectroscopy (FT-IRRAS). The tribological properties of the resulting organic monolayers with different end groups (fluorinated or nonfluorinated) were studied using atomic force microscopy (AFM). It was found that the fluorinated monolayers exhibit a dramatic reduction of adhesion and friction force as well as excellent wear resistance compared to those of nonfluorinated coatings and bare CrN substrates. The combination of remarkable chemical stability and superior tribological properties makes these fluorinated monolayers promising candidates for the development of robust high-performance devices.

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

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

Bowman, Adam J.; Scherrer, Joseph R.; Reiserer, Ronald S., E-mail: ron.reiserer@vanderbilt.edu

We present a simple apparatus for improved surface modification of polydimethylsiloxane (PDMS) microfluidic devices. A single treatment chamber for plasma activation and chemical/physical vapor deposition steps minimizes the time-dependent degradation of surface activation that is inherent in multi-chamber techniques. Contamination and deposition irregularities are also minimized by conducting plasma activation and treatment phases in the same vacuum environment. An inductively coupled plasma driver allows for interchangeable treatment chambers. Atomic force microscopy confirms that silane deposition on PDMS gives much better surface quality than standard deposition methods, which yield a higher local roughness and pronounced irregularities in the surface.

Effect of different adhesion strategies on bond strength of resin composite to composite-dentin complex.

PubMed

Özcan, M; Pekkan, G

2013-01-01

Service life of discolored and abraded resin composite restorations could be prolonged by repair or relayering actions. Composite-composite adhesion can be achieved successfully using some surface conditioning methods, but the most effective adhesion protocol for relayering is not known when the composite restorations are surrounded with dentin. This study evaluated the effect of three adhesion strategies on the bond strength of resin composite to the composite-dentin complex. Intact maxillary central incisors (N=72, n=8 per subgroup) were collected and the coronal parts of the teeth were embedded in autopolymerized poly(methyl tfr54methacrylate) surrounded by a polyvinyl chloride cylinder. Cylindrical cavities (diameter: 2.6 mm; depth: 2 mm) were opened in the middle of the labial surfaces of the teeth using a standard diamond bur, and the specimens were randomly divided into three groups. Two types of resin composite, namely microhybrid (Quadrant Anterior Shine; AS) and nanohybrid (Grandio; G), were photo-polymerized incrementally in the cavities according to each manufacturer's recommendations. The composite-enamel surfaces were ground finished to 1200-grit silicone carbide paper until the dentin was exposed. The surfaces of the substrate composites and the surrounding dentin were conditioned according to one of the following adhesion protocols: protocol 1: acid-etching (dentin) + silica coating (composite) + silanization (composite) + primer (dentin) + bonding agent (dentin + composite); protocol 2: silica coating (composite) + acid-etching (dentin) + silanization (composite) + primer (dentin) + bonding agent (dentin + composite); and protocol 3: acid-etching (dentin) + primer (dentin) + silanization (composite) + bonding agent (dentin + composite). Applied primer and bonding agents were the corresponding materials of the composite manufacturer. Silica coating (CoJet sand, 30 μm) was achieved using a chairside air-abrasion device (distance: 10 mm; duration: four seconds in circular motion). After conditioning protocols, the repair resin was adhered to the substrate surfaces using transparent polyethylene molds (diameter: 3.6 mm) incrementally and photo-polymerized. The substrate-adherend combinations were as follows: AS-AS, G-G, AS-G. Shear force was applied to the adhesive interface in a Universal Testing Machine (crosshead speed: 1 mm/min). The types of failures were further evaluated and categorized as follows: 1) cohesive in the composite substrate and 2) adhesive at the interface. Bond strength values (MPa) were statistically analyzed using two-way analysis of variance and least significant difference post hoc tests (α=0.05). Significant effects of the adhesion strategy (p=0.006) and the composite type (p=0.000) were found. Interaction terms were not significant (p=0.292). Regardless of the substrate-adherend combination, protocol 1 (17-22 MPa) showed significantly higher results than did protocols 2 (15-17 MPa) and 3 (11-17 MPa) (p=0.028, p=0.002, respectively). The highest results were obtained from the G-G combination after all three protocols (17-22 MPa). The incidence of cohesive failures was more common when the substrate and the adherend were the same composite type (AS-AS: 87.5%, 87.5%, 75%; G-G: 100%, 75%, 50% for protocols 1, 2, and 3, respectively). When substrate and adherend were used interchangeably, adhesive failures were more frequent (25%, 50%, and 100% for protocol 1, 2, and 3, respectively). When the substrate and the adherend are of the same type, greater repair strength could be expected. In the repair of composites next to the dentin, depending on the composite type, conditioning the composite with silica coating and silanization after etching the dentin adds to the repair strength compared to the results obtained with silane application only.

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.

Physics and chemistry in the process of hot-wire deposition of thin film silicon

NASA Astrophysics Data System (ADS)

Zheng, Wengang

Hotwire Chemical Vapor Deposition (CVD) has been used in preparing high quality low hydrogen content hydrogenated amorphous or polycrystalline silicon thin film in recent years. Comparing to the most commonly used glow discharge method, Hotwire CVD has the potential of high speed deposition avoiding the damage caused by ion bombardment associated with plasma. Although device quality thin films have been prepared by this method, and some empirical optimized deposition conditions have been established, the mechanisms controlling this technique are not clear. A homebuild threshold ionization mass spectrometer was constructed in this lab, allowing the radicals to be observed with high sensitivity. Hydrogen dissociation on the hot metal surface was studied first both by the direct detection of hydrogen atoms from the hot surface and the temperature change due to the hydrogen dissociation, it was confirmed that the activation energy of this process is around 2.25eV, the same as the dissociation in the gas phase. Further, we observed a first order dependence of hydrogen dissociation probability on the hydrogen pressure. This observation contradicts previously reported models of second order desorption. The monosilicon radicals Si and SiH3 were observed. It was observed that the silane decomposition on the hot surface is mainly a function of filament temperature, but the species released from that surface also depend on the surface condition, and thus on the silane exposure history of that piece of filament. Si is believed to deteriorate the film quality, by comparing the depleted silane and the Si flux, it is observed that Si experienced a lot of gas phase reactions before reaching the substrate, which leads to less reactive precursors. This observation is consistence with Molenbroek's study on the optimization of deposition condition. The dominant disilicon radical is identified as Si2H2, which in the form of lowest energy isomer, is suppose to be much less reactive than Si, and thus contributes to good quality thin film deposition. The corresponding Si insert reaction Si + SiH4 was also studied and an effective reaction coefficient of KSeff = 5 x 10-12( cm3/s was established.

Organofunctional Silane Modification of Aluminum-Doped Zinc Oxide Surfaces as a Route to Stabilization

DOE PAGES

Matthews, Rachael; Glasser, Emily; Sprawls, Samuel C.; ...

2017-05-01

Aluminum-doped zinc oxide (AZO) is a low-temperature processed transparent conductive oxide (TCO) made of earth abundant elements; its applications are currently limited by instability to heat, moisture, and acidic conditions. We demonstrate that the application of an organofunctional silane modifier mitigates AZO degradation, and explore the interplay between performance and material composition and morphology. Specifically, we evaluate degradation of bare AZO and APTES (3-aminopropyltriethoxysilane)-modified AZO in response to damp heat (DH, 85 °C, 85 % relative humidity) exposure over 1000 h, then demonstrate how surface modification impacts changes in electrical and optical properties, and chemical composition in one of themore » most thorough studies to date. Hall measurements show that the resistivity of AZO increases due to a decrease in electron mobility, with no commensurate change in carrier concentration. APTES decelerates this electrical degradation, without affecting AZO optical properties. Percent transmission and yellowness index of an ensemble of bare and modified AZO are stable upon DH exposure, but haze increases slightly for a discrete sample of modified AZO. Atomic force microscopy (AFM) and optical profilometer (OP) measurements do not show evidence of pitting or delamination after 1000 h DH exposure, but indicate a slight increase in surface roughness on both the nanometer and micron length scales. X-ray photoelectron spectroscopy data (XPS) reveal that the surface composition of bare and silanized AZO is stable over this time frame; oxygen vacancies, as measured by XPS, are also stable with DH exposure, which, together with transmission and Hall measurements, indicate stable carrier concentrations. However, after 1500 h of DH exposure, only bare AZO shows signs of catastrophic destruction. Comparison of the data presented herein to previous reports indicates that the initial AZO composition and microstructure dictate the degradation profile. Furthermore, this work demonstrates that surface modification slows the bulk degradation of AZO, and provides insight into how the material can be more widely used as a transparent electrode in the next generation of optoelectronic devices.« less

Organofunctional Silane Modification of Aluminum-Doped Zinc Oxide Surfaces as a Route to Stabilization

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

Matthews, Rachael; Glasser, Emily; Sprawls, Samuel C.

Aluminum-doped zinc oxide (AZO) is a low-temperature processed transparent conductive oxide (TCO) made of earth abundant elements; its applications are currently limited by instability to heat, moisture, and acidic conditions. We demonstrate that the application of an organofunctional silane modifier mitigates AZO degradation, and explore the interplay between performance and material composition and morphology. Specifically, we evaluate degradation of bare AZO and APTES (3-aminopropyltriethoxysilane)-modified AZO in response to damp heat (DH, 85 °C, 85 % relative humidity) exposure over 1000 h, then demonstrate how surface modification impacts changes in electrical and optical properties, and chemical composition in one of themore » most thorough studies to date. Hall measurements show that the resistivity of AZO increases due to a decrease in electron mobility, with no commensurate change in carrier concentration. APTES decelerates this electrical degradation, without affecting AZO optical properties. Percent transmission and yellowness index of an ensemble of bare and modified AZO are stable upon DH exposure, but haze increases slightly for a discrete sample of modified AZO. Atomic force microscopy (AFM) and optical profilometer (OP) measurements do not show evidence of pitting or delamination after 1000 h DH exposure, but indicate a slight increase in surface roughness on both the nanometer and micron length scales. X-ray photoelectron spectroscopy data (XPS) reveal that the surface composition of bare and silanized AZO is stable over this time frame; oxygen vacancies, as measured by XPS, are also stable with DH exposure, which, together with transmission and Hall measurements, indicate stable carrier concentrations. However, after 1500 h of DH exposure, only bare AZO shows signs of catastrophic destruction. Comparison of the data presented herein to previous reports indicates that the initial AZO composition and microstructure dictate the degradation profile. Furthermore, this work demonstrates that surface modification slows the bulk degradation of AZO, and provides insight into how the material can be more widely used as a transparent electrode in the next generation of optoelectronic devices.« less

Morphology of self assembled monolayers using liquid phase reaction on silica and their effect on the morphology of adsorbed insulin

NASA Astrophysics Data System (ADS)

Sharma, Indu; Pattanayek, Sudip K.; Aggarwal, Varsha; Ghosh, Subhasis

2017-05-01

The effect of roughness of two different categories of self-assembled monolayers (SAMs) with propyl amine and propyl groups respectively on the morphology of adsorbed insulin is observed. SAMs are obtained by liquid phase reaction of silica with organo silane coupling agents (SCA). The influence of the morphology and physical characteristics of the SAMs on the reaction time and concentration of the modifiers are explored. We have tested three SCA containing propyl amine with varying groups linked to Si present on it. In addition, we have used a silane coupling agent to prepare SAM of methyl head group. The approach of these molecules towards the surface depends on the head group and the groups linked to Si of the SCA. The morphology of the surfaces is analysed using power spectral density distribution (PSD), skewness, ellipsometry thickness and surface energy. Both chemical nature and physical morphology of the adsorbent influence the morphology of the adsorbed insulin. In general, a low number of aggregates of big size are formed on the surfaces obtained from low concentration of SAMs, while a higher number but of smaller size of aggregates are formed over surfaces obtained from 1% concentration of SAMs modifiers. The peak to valley ratio of the aggregates of insulin is strongly influenced by the size of grains of SCA over the adsorbent.

Effect of surface treatments on shear bond strength of resin composite bonded to CAD/CAM resin-ceramic hybrid materials

PubMed Central

Güngör, Merve Bankoğlu; Bal, Bilge Turhan; Ünver, Senem; Doğan, Aylin

2016-01-01

PURPOSE The purpose of this study was to assess the effect of surface treatments on shear bond strength of resin composite bonded to thermocycled and non-thermocycled CAD/CAM resin-ceramic hybrid materials. MATERIALS AND METHODS 120 specimens (10×10×2 mm) from each material were divided into 12 groups according to different surface treatments in combination with thermal aging procedures. Surface treatment methods were airborne-particle abrasion (abraded with 50 micron alumina particles), dry grinding (grinded with 125 µm grain size bur), and hydrofluoric acid (9%) and silane application. According to the thermocycling procedure, the groups were assigned as non-thermocycled, thermocycled after packing composites, and thermocycled before packing composites. The average surface roughness of the non-thermocycled specimens were measured after surface treatments. After packing composites and thermocycling procedures, shear bond strength (SBS) of the specimens were tested. The results of surface roughness were statistically analyzed by 2-way Analysis of Variance (ANOVA), and SBS results were statistically analyzed by 3-way ANOVA. RESULTS Surface roughness of GC were significantly lower than that of LU and VE (P<.05). The highest surface roughness was observed for dry grinding group, followed by airborne particle abraded group (P<.05). Comparing the materials within the same surface treatment method revealed that untreated surfaces generally showed lower SBS values. The values of untreated LU specimens showed significantly different SBS values compared to those of other surface treatment groups (P<.05). CONCLUSION SBS was affected by surface treatments. Thermocycling did not have any effect on the SBS of the materials except acid and silane applied GC specimens, which were subjected to thermocycling before packing of the composite resin. PMID:27555894

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

Oyola-Reynoso, S.; Tevis, I. D.; Chen, J.

Here, chemical grafting has been widely used to modify the surface properties of materials, especially surface energy for controlled wetting, because of the resilience of such coatings/modifications. Reagents with multiple reactive sites have been used with the expectation that a monolayer will form. The step-growth polymerization mechanism, however, suggests the possibility of gel formation for hydrolyzable moieties in the presence of physisorbed water. In this report, we demonstrated that using alkyltrichlorosilanes (trivalent [i.e., 3 reactive sites]) in the surface modification of a cellulosic material (paper) does not yield a monolayer but rather gives surface-bound particles. We infer that the presencemore » of physisorbed (surface-bound) water allows for polymerization (or oligomerization) of the silane prior to its attachment on the surface. Surface energy mismatch between the hydrophobic tails of the growing polymer and any unreacted bound water leads to the assembly of the polymerizing material into spherical particles to minimize surface tension. By varying paper grammage (16.2–201.4 g m –2), we varied the accessible surface area and thus the amount of surface-adsorbed water, allowing us to control the ratio of the silane to the bound water. Using this approach, polymeric particles were formed on the surface of cellulose fibers ranging from ~70 nm to a film. The hydrophobicity of the surface, as determined by water contact angles, correlates with particle sizes (p < 0.001, Student's t-test), and, hence, the hydrophobicity can be tuned (contact angle between 94° and 149°). Using a model structure of a house, we demonstrated that as a result of this modification, paper-based houses can be rendered self-cleaning or tolerant to surface running water. In another application, we demonstrated that the felicitous choice of architectural design allows for the hydrophobic paper to be used for water harvesting.« less

Engineering tunable bio-inspired polymeric coatings for amphiphobic fibrous materials

NASA Astrophysics Data System (ADS)

Oyola-Reynoso, Stephanie

Chemical grafting has been widely used to modify the surface properties of materials, especially surface energy for controlled wetting, because of the resilience of such coatings/modifications. Reagents with multiple reactive sites have been used with the expectation that a monolayer will form. The step-growth polymerization mechanism, however, suggests the possibility of gel formation for hydrolysable moieties in the presence of physisorbed water. In the following chapters, we demonstrate that using alkyltrichlorosilanes (trivalent [3 reactive sites]) in the surface modification of a cellulosic material (paper) does not yield a monolayer but rather gives surface-bound polymeric particles. We infer that the presence of physisorbed (surface-bound) water allows for polymerization (or oligomerization) of the silane, prior to its attachment on the surface. Surface energy mismatch between the hydrophobic tails of the growing polymer and any unreacted bound water leads to the assembly of the polymerizing material into spherical particles to minimize surface tension. By varying paper grammage (16.2-201.4 g/m2), we varied the accessible surface area and thus the amount of surface-adsorbed water, allowing us to control the ratio of the silane to the bound water. Using this approach, polymeric particles were formed on the surface of cellulose fibers ranging from 70 nm to a film. The hydrophobicity of the surface, as determined by water contact angles, correlates with particle sizes (p < 0.001, Student t-test), and, hence, the hydrophobicity can be tuned (contact angle between 94° and 149°). Using a model structure of a house, we demonstrated that as a result of this modification, cardboard houses can be rendered self-cleaning or tolerant to surface running water. Each of the chapters below supports the mechanism via a series of applications, material characterization, and/or, smart engineering.

Porcelain surface alterations and refinishing after use of two orthodontic bonding methods.

PubMed

Herion, Drew T; Ferracane, Jack L; Covell, David A

2010-01-01

To compare porcelain surfaces at debonding after use of two surface preparation methods and to evaluate a method for restoring the surface. Lava Ceram feldspathic porcelain discs (n = 40) underwent one of two surface treatments prior to bonding orthodontic brackets. Half the discs had sandblasting, hydrofluoric acid, and silane (SB + HF + S), and the other half, phosphoric acid and silane (PA + S). Brackets were debonded using bracket removing pliers, and resin was removed with a 12-fluted carbide bur. The surface was refinished using a porcelain polishing kit, followed by diamond polishing paste. Measurements for surface roughness (Ra), gloss, and color were made before bonding (baseline), after debonding, and after each step of refinishing. Surfaces were also examined by scanning electron microscopy (SEM). Data was analyzed with 2-way ANOVA followed by Tukey HSD tests (alpha = 0.05). The SB + HF + S bonding method increased Ra (0.160 to 1.121 microm), decreased gloss (41.3 to 3.7) and altered color (DeltaE = 4.37; P < .001). The PA + S method increased Ra (0.173 to 0.341 microm; P < .001), but the increase in Ra was significantly less than that caused by the SB + HF + S bonding method (P < . 001). The PA + S method caused insignificant changes in gloss (41.7 to 38.0) and color (DeltaE = 0.50). The measurements and SEM observations showed that changes were fully restored to baseline with refinishing. The PA + S method caused significantly less damage to porcelain than the SB + HF + S method. The refinishing protocol fully restored the porcelain surfaces.

Replacement of glass particles by multidirectional short glass fibers in experimental composites: Effects on degree of conversion, mechanical properties and polymerization shrinkage.

PubMed

Bocalon, Anne C E; Mita, Daniela; Narumyia, Isabela; Shouha, Paul; Xavier, Tathy A; Braga, Roberto Ruggiero

2016-09-01

To test the null hypothesis that the replacement of a small fraction of glass particles with random short glass fibers does not affect degree of conversion (DC), flexural strength (FS), fracture toughness (FT) and post-gel polymerization shrinkage (PS) of experimental composites. Four experimental photocurable composites containing 1 BisGMA:1 TEGDMA (by weight) and 60vol% of fillers were prepared. The reinforcing phase was constituted by barium glass particles (2μm) and 0%, 2.5%, 5.0% or 7.5% of silanated glass fibers (1.4mm in length, 7-13μm in diameter). DC (n=4) was obtained using near-FTIR. FS (n=10) was calculated via biaxial flexural test and FT (n=10) used the "single edge notched beam" method. PS at 5min (n=8) was determined using the strain gage method. Data were analyzed by ANOVA/Tukey test (DC, FS, PS) or Kruskal-Wallis/Dunn's test (FT, alpha: 5% for both tests). DC was similar among groups (p>0.05). Only the composite containing 5.0% of fibers presented lower FS than the control (p<0.001). FT increased significantly between the control (1.3±0.17MPam(0.5)) and the composites containing either 5.0% (2.7±0.6MPam(0.5)) or 7.5% of fibers (2.8±0.6MPam(0.5), p<0.001). PS in relation to control was significantly reduced at 2.5% fibers (from 0.81±0.13% to 0.57±0.13%) and further reduced between 5.0% and 7.5% (from 0.42±0.12% to 0.23±0.07%, p<0.001). The replacement of a small fraction of filler particles with glass fibers significantly increased fracture toughness and reduced post-gel shrinkage of experimental composites. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

Fabrication and Evaluation of Bis-GMA/TEGDMA Dental Resins/Composites Containing Nano Fibrillar Silicate

PubMed Central

Tian, Ming; Gao, Yi; Liu, Yi; Liao, Yiliang; Hedin, Nyle E.; Fong, Hao

2008-01-01

Objective To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and composites (with conventional glass filler) with various mass fractions of nano fibrillar silicate (FS). Methods Three dispersion methods were studied to separate the silanized FS as nano-scaled single crystals and uniformly distribute them into dental matrices. The photo-curing behaviors of the Bis-GMA/TEGDMA/FS resins were monitored in situ by RT-NIR to study the photopolymerization rate and the vinyl double bond conversion. Mechanical properties (flexural strength, elastic modulus and work of fracture) of the nano FS reinforced resins/composites were tested, and Analysis of Variance (ANOVA) was used for the statistical analysis of the acquired data. The morphology of nano FS and the representative fracture surfaces of its reinforced resins/composites were examined by SEM/TEM. Results Impregnation of small mass fractions (1 % and 2.5 %) of nano FS into Bis-GMA/TEGDMA (50/50 mass ratio) dental resins/composites improved the mechanical properties substantially. Larger mass fraction of impregnation (7.5 %), however, did not further improve the mechanical properties (one way ANOVA, P > 0.05) and may even reduce the mechanical properties. The high degree of separation and uniform distribution of nano FS into dental resins/composites was a challenge. Impregnation of nano FS into dental resins/composites could result in two opposite effects: a reinforcing effect due to the highly separated and uniformly distributed nano FS single crystals, or a weakening effect due to the formation of FS agglomerates/particles. Significance Uniform distribution of highly separated nano FS single crystals into dental resins/composites could significantly improve the mechanical properties of the resins/composites. PMID:17572485

Fabrication and evaluation of Bis-GMA/TEGDMA dental resins/composites containing nano fibrillar silicate.

PubMed

Tian, Ming; Gao, Yi; Liu, Yi; Liao, Yiliang; Hedin, Nyle E; Fong, Hao

2008-02-01

To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and composites (with conventional glass filler) with various mass fractions of nano fibrillar silicate (FS). Three dispersion methods were studied to separate the silanized FS as nano-scaled single crystals and uniformly distribute them into dental matrices. The photo-curing behaviors of the Bis-GMA/TEGDMA/FS resins were monitored in situ by RT-NIR to study the photopolymerization rate and the vinyl double bond conversion. Mechanical properties (flexural strength, elastic modulus and work-of-fracture) of the nano FS reinforced resins/composites were tested, and analysis of variance (ANOVA) was used for the statistical analysis of the acquired data. The morphology of nano FS and the representative fracture surfaces of its reinforced resins/composites were examined by SEM/TEM. Impregnation of small mass fractions (1% and 2.5%) of nano FS into Bis-GMA/TEGDMA (50/50 mass ratio) dental resins/composites improved the mechanical properties substantially. Larger mass fraction of impregnation (7.5%), however, did not further improve the mechanical properties (one way ANOVA, P>0.05) and may even reduce the mechanical properties. The high degree of separation and uniform distribution of nano FS into dental resins/composites was a challenge. Impregnation of nano FS into dental resins/composites could result in two opposite effects: a reinforcing effect due to the highly separated and uniformly distributed nano FS single crystals, or a weakening effect due to the formation of FS agglomerates/particles. Uniform distribution of highly separated nano FS single crystals into dental resins/composites could significantly improve the mechanical properties of the resins/composites.

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.

A Close Look at the Structure of the TiO2-APTES Interface in Hybrid Nanomaterials and Its Degradation Pathway: An Experimental and Theoretical Study

PubMed Central

2016-01-01

The surface functionalization of TiO2-based materials with alkylsilanes is attractive in several cutting-edge applications, such as photovoltaics, sensors, and nanocarriers for the controlled release of bioactive molecules. (3-Aminopropyl)triethoxysilane (APTES) is able to self-assemble to form monolayers on TiO2 surfaces, but its adsorption geometry and solar-induced photodegradation pathways are not well understood. We here employ advanced experimental (XPS, NEXAFS, AFM, HR-TEM, and FT-IR) and theoretical (plane-wave DFT) tools to investigate the preferential interaction mode of APTES on anatase TiO2. We demonstrate that monomeric APTES chemisorption should proceed through covalent Si–O–Ti bonds. Although dimerization of the silane through Si–O–Si bonds is possible, further polymerization on the surface is scarcely probable. Terminal amino groups are expected to be partially involved in strong charge-assisted hydrogen bonds with surface hydroxyl groups of TiO2, resulting in a reduced propensity to react with other species. Solar-induced mineralization proceeds through preferential cleavage of the alkyl groups, leading to the rapid loss of the terminal NH2 moieties, whereas the Si-bearing head of APTES undergoes slower oxidation and remains bound to the surface. The suitability of employing the silane as a linker with other chemical species is discussed in the context of controlled degradation of APTES monolayers for drug release and surface patterning. PMID:28191270

Bond strength between a polymer-infiltrated ceramic network and a composite for repair: effect of several ceramic surface treatments.

PubMed

Silva, Pollyanna Nogueira Ferreira da; Martinelli-Lobo, Carolina Machado; Bottino, Marco Antonio; Melo, Renata Marques de; Valandro, Luiz Felipe

2018-01-01

The effects of several ceramic surface treatments on bond strength of a polymer-infiltrated ceramic network and resin composite as repair material were evaluated. CAD-CAM blocks of a polymer-infiltrated ceramic network (Vita Enamic) were sliced and subjected to aging process, followed by embedding in acrylic resin. The bonding/repair area was treated as follows (n = 30): C- without treatment; UA- universal adhesive application; FM- 10% hydrofluoric acid and silane application; OM-airborne-particle abrasion with aluminum oxide and silane application; RP- tribochemical silica coating; and CA- surface grinding and application of universal adhesive. Composite resin cylinders were made on the treated surface. Specimens from each group were assigned randomly to two subgroups (n = 15) considering storage condition: Baseline (shear tests after 48 hours) or Storage (tests after 6 months under distilled water). The treated surfaces were analyzed by goniometry, roughness, and SEM. Two-way ANOVA and 1-way ANOVA were applied to analyze the bond data and roughness / contact angle data, respectively, followed by Tukey's test (α = 5%). Surface treatments and storage conditions affected bond strengths (p < 0.01). Surface grinding (CA) followed by universal adhesive promoted the highest value of bond strength (14.5 ± 4.8 MPa for baseline, 8.5 ± 3.4 MPa for storage) and the roughest ceramic surface. Grinding with silicon carbide paper (simulating diamond bur) followed by the application of a universal adhesive system is the best option for repairing fractures of the polymer-infiltrated ceramic network.

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.

Molecular dynamics simulation of sodium aluminosilicate glass structures and glass surface-water reactions using the reactive force field (ReaxFF)

NASA Astrophysics Data System (ADS)

Dongol, R.; Wang, L.; Cormack, A. N.; Sundaram, S. K.

2018-05-01

Reactive potentials are increasingly used to study the properties of glasses and glass water reactions in a reactive molecular dynamics (MD) framework. In this study, we have simulated a ternary sodium aluminosilicate glass and investigated the initial stages of the glass surface-water reactions at 300 K using reactive force field (ReaxFF). On comparison of the simulated glass structures generated using ReaxFF and classical Buckingham potentials, our results show that the atomic density profiles calculated for the surface glass structures indicate a bond-angle distribution dependency. The atomic density profiles also show higher concentrations of non-bridging oxygens (NBOs) and sodium ions at the glass surface. Additionally, we present our results of formation of silanol species and the diffusion of water molecules at the glass surface using ReaxFF.

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.

Advanced, Non-Toxic, Anti-Corrosion, Anti-Fouling and Foul-Release Coatings Based on Covalently Attached Monolayers, Multilayers and Polymers

DTIC Science & Technology

2007-08-08

McCarthy Polymer Science and Engineering Department, University of Massachusetts, Amherst, Massachusetts 01003 Electrophilic aromatic substitution reactions...with a fluorinated silane reagent. Reduction of the amide groups with borane-THF (BH 3-THF) complex leads to a 69% conversion of surface amides to the

ExoMol line lists - XXII. The rotation-vibration spectrum of silane up to 1200 K

NASA Astrophysics Data System (ADS)

Owens, A.; Yachmenev, A.; Thiel, W.; Tennyson, J.; Yurchenko, S. N.

2017-11-01

A variationally computed 28SiH4 rotation-vibration line list applicable for temperatures up to T = 1200 K is presented. The line list, called OY2T, considers transitions with rotational excitation up to J = 42 in the wavenumber range 0-5000 cm-1 (wavelengths λ > 2 μm). Just under 62.7 billion transitions have been calculated between 6.1 million energy levels. Rovibrational calculations have utilized a new `spectroscopic' potential energy surface determined by empirical refinement to 1452 experimentally derived energy levels up to J = 6, and a previously reported ab initio dipole moment surface. The temperature-dependent partition function of silane, the OY2T line list format, and the temperature dependence of the OY2T line list are discussed. Comparisons with the PNNL spectral library and other experimental sources indicate that the OY2T line list is robust and able to accurately reproduce weaker intensity features. The full line list is available from the ExoMol data base and the CDS data base.

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

Mahadevapuram, Nikhila; Mitra, Indranil; Sridhar, Shyam

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

Effect of plasma treatment (He/CH4) on glass surface for the reduction of powder flux adhesion in the spray drying process

NASA Astrophysics Data System (ADS)

Ramlan, Nadiah; Zamri, Nazirah Wahidah Mohd; Maskat, Mohd Yusof; Hoong, Chin Oi; Theng, Lau Yen; Zubairi, Saiful Irwan

2018-04-01

A 50Hz glow discharge He/CH4 plasma was generated and applied for the modification of glass surface to reduce powder adhesion on the wall of spray dryer. The hydrophobicity of the glass samples determined by the water droplet contact angle and adhesion weight on glass, dependent on the CH4 flow rate and plasma exposure time. There was a peak that appeared at 1470 cm-1 on the surface of treated glass indicating the presence of CH3 groups from ATR-FTIR data. Surface morphology analysis using scanning electron microscopy (SEM) showed changes of roughness in the surface-treated glass. The presence of alkyl group (CH3) that deposited on the glass surface is one of the factors that contribute to the increase in the surface roughness. The surface roughness will reflect the value of contact angle where hydrophobic surface are rougher compared to hydrophilic surface. The plasma treatment could enhance the value of the contact angle and thus reduced the adhesion on the spray dryer glass surface.

Multifunctional silicon surfaces: reaction of dichlorocarbene generated from Seyferth reagent with hydrogen-terminated silicon (111) surfaces.

PubMed

Liu, Wenjun; Sharp, Ian D; Tilley, T Don

2014-01-14

Insertion of dichlorocarbene (:CCl2), generated by decomposition of the Seyferth reagent PhHgCCl2Br, into the Si-H bond of a tertiary silane to form a Si-CCl2H group is an efficient homogeneous, molecular transformation. A heterogeneous version of this reaction, between PhHgCCl2Br and a silicon (111) surface terminated by tertiary Si-H bonds, was studied using a combination of surface-sensitive infrared and X-ray photoelectron spectroscopies. The insertion of dichlorocarbene into surface Si-H bonds parallels the corresponding reaction of silanes in solution, to produce surface-bound dichloromethyl groups (Si-CCl2H) covering ∼25% of the silicon surface sites. A significant fraction of the remaining Si-H bonds on the surface was converted to Si-Cl/Br groups during the same reaction, with PhHgCCl2Br serving as a halogen atom source. The presence of two distinct environments for the chlorine atoms (Si-CCl2H and Si-Cl) and one type of bromine atom (Si-Br) was confirmed by Cl 2p, Br 3d, and C 1s X-ray photoelectron spectroscopy. The formation of reactive, halogen-terminated atop silicon sites was also verified by reaction with sodium azide or the Grignard reagent (CH3MgBr), to produce Si-N3 or Si-Me functionalities, respectively. Thus, reaction of a hydrogen-terminated silicon (111) surface with PhHgCCl2Br provides a facile route to multifunctional surfaces possessing both stable silicon-carbon and labile silicon-halogen sites, in a single pot synthesis. The reactive silicon-halogen groups can be utilized for subsequent transformations and, potentially, the construction of more complex organic-silicon hybrid systems.

[Study of Interaction between Fluorinated Coating Glass and the Medicines].

PubMed

Kawano, Yayoi; Otsu, Saki; Bamba, Takao; Hanawa, Takehisa

2017-11-01

 The adsorption of active pharmaceutical ingredients on the surface of medical devices such as polyvinl chloride, ethylene-vinyl acetate copolymer and glass often prevent the acuurate dose of drug. At dispensing of pharmaceuticals, mètre glass (MG) has been widely used for dispensing syrup. When measuring the viscous syrup, it often takes long time to dispense the accurate volume due to their adhesiveness on the glass surface. In this study, we investigate the adhesion of various syrups to MG made with uncoated glass or glass with a strongly hydrophobic silicone or fluorinated coating in terms of the following formulation parameters: viscosity, surface tension, contact angle, and surface free energy. The contact angles for syrups on the coated glass surfaces were significantly higher than those on the uncoated glass surface. In addition, the relationship between surface tension and contact angle was examined. We found that the contact angle was independent of surface tension for the uncoated glass, while it increased with increasing surface tension for the coated glasses. These results can be explained as follows: the silicone or fluorinated coatings inhibit the hydrogen bonding that usually takes place between water and silanol and siloxane groups at glass surfaces. The coatings reduced the surface free energy and increased the hydrophobicity of the glass, reduced its wettability by the syrups, and thus reduced the adhesion loss for the syrups. It was considered that as for the hydrophobic action, properties of matter of sample influence the coated device by coating in order that it is reinforced.

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

Facile Preparation of Nanostructured, Superhydrophobic Filter Paper for Efficient Water/Oil Separation

PubMed Central

Wang, Jianhua; Wong, Jessica X. H.; Kwok, Honoria; Li, Xiaochun; Yu, Hua-Zhong

2016-01-01

In this paper, we present a facile and cost-effective method to obtain superhydrophobic filter paper and demonstrate its application for efficient water/oil separation. By coupling structurally distinct organosilane precursors (e.g., octadecyltrichlorosilane and methyltrichlorosilane) to paper fibers under controlled reaction conditions, we have formulated a simple, inexpensive, and efficient protocol to achieve a desirable superhydrophobic and superoleophilic surface on conventional filter paper. The silanized superhydrophobic filter paper showed nanostructured morphology and demonstrated great separation efficiency (up to 99.4%) for water/oil mixtures. The modified filter paper is stable in both aqueous solutions and organic solvents, and can be reused multiple times. The present study shows that our newly developed binary silanization is a promising method of modifying cellulose-based materials for practical applications, in particular the treatment of industrial waste water and ecosystem recovery. PMID:26982055

Investigation of γ-(2,3-Epoxypropoxy)propyltrimethoxy Silane Surface Modified Layered Double Hydroxides Improving UV Ageing Resistance of Asphalt.

PubMed

Zhang, Canlin; Yu, Jianying; Xue, Lihui; Sun, Yubin

2017-01-19

γ-(2,3-Epoxypropoxy)propyltrimethoxy silane surface modified layered double hydroxides (KH560-LDHs) were prepared and used to improve the ultraviolet ageing resistance of asphalt. The results of X-ray photoelectron spectrometry (XPS) indicated that KH560 has been successfully grafted onto the surface of LDHs. The agglomeration of LDHs particles notably reduced after KH560 surface modification according to scanning electron microscopy (SEM), which implied that the KH560 surface modification was helpful to promote the dispersibility of LDHs in asphalt. Then, the influence of KH560-LDHs and LDHs on the physical and rheological properties of asphalt before and after UV ageing was thoroughly investigated. The storage stability test showed that the difference in softening point (Δ S ) of LDHs modified asphalt decreased from 0.6 °C to 0.2 °C at an LDHs content of 1% after KH560 surface modification, and the tendency became more pronounced with the increase of LDH content, indicating that KH560 surface modification could improve the stability of LDHs in asphalt. After UV ageing, the viscous modulus ( G'' ) of asphalt significantly reduced, and correspondingly, the elastic modulus ( G' ) and rutting factor ( G */sin δ) rapidly increased. Moreover, the asphaltene increased and the amount of "bee-like" structures of the asphalt decreased. Compared with LDHs, KH560-LDHs obviously restrained performance deterioration of the asphalt, and helped to relieve the variation of the chemical compositions and morphology of asphalt, which suggested that the improvement of KH560-LDHs on UV ageing resistance of asphalt was superior to LDHs.

Preparation and single molecule structure of electroactive polysilane end-grafted on a crystalline silicon surface

NASA Astrophysics Data System (ADS)

Furukawa, Kazuaki; Ebata, Keisuke

2000-12-01

Electrically active polysilanes of poly(methylphenylsilane) (PMPS) and poly[bis(p-n-butylphenyl)silane] (PBPS), which are, respectively, known as a good hole transporting material and a near-ultraviolet electroluminescent material, are end-grafted directly on a crystalline silicon surface. The single polysilane molecules are clearly distinguished one from the other on the surface by means of atomic force microscopy observations. End-grafted single molecules of PMPS are observed as dots while end-grafted PBPS appear as worms extending for more than 100 nm on the crystalline silicon surface.

Superhydrophobic diatomaceous earth

DOEpatents

Simpson, John T [Clinton, TN; D& #x27; Urso, Brian R [Clinton, TN

2012-07-10

A superhydrophobic powder is prepared by coating diatomaceous earth (DE) with a hydrophobic coating on the particle surface such that the coating conforms to the topography of the DE particles. The hydrophobic coating can be a self assembly monolayer of a perfluorinated silane coupling agent. The DE is preferably natural-grade DE where organic impurities have been removed. The superhydrophobic powder can be applied as a suspension in a binder solution to a substrate to produce a superhydrophobic surface on the substrate.

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.

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.

Fabrication of ultrathin multilayered superomniphobic nanocoatings by liquid flame spray, atomic layer deposition, and silanization.

PubMed

Sorvali, Miika; Vuori, Leena; Pudas, Marko; Haapanen, Janne; Mahlberg, Riitta; Ronkainen, Helena; Honkanen, Mari; Valden, Mika; Mäkelä, Jyrki M

2018-05-04

Superomniphobic, i.e. liquid-repellent, surfaces have been an interesting area of research during recent years due to their various potential applications. However, producing such surfaces, especially on hard and resilient substrates like stainless steel, still remains challenging. We present a stepwise fabrication process of a multilayered nanocoating on a stainless steel substrate, consisting of a nanoparticle layer, a nanofilm, and a layer of silane molecules. Liquid flame spray was used to deposit a TiO 2 nanoparticle layer as the bottom layer for producing a suitable surface structure. The interstitial Al 2 O 3 nanofilm, fabricated by atomic layer deposition (ALD), stabilized the nanoparticle layer, and the topmost fluorosilane layer lowered the surface energy of the coating for enhanced omniphobicity. The coating was characterized with field emission scanning electron microscopy, focused ion beam scanning electron microscopy, x-ray photoelectron spectroscopy, contact angle (CA) and sliding angle (SA) measurements, and microscratch testing. The widely recognized requirements for superrepellency, i.e. CA > 150° and SA < 10°, were achieved for deioinized water, diiodomethane, and ethylene glycol. The mechanical stability of the coating could be varied by tuning the thickness of the ALD layer at the expense of repellency. To our knowledge, this is the thinnest superomniphobic coating reported so far, with the average thickness of about 70 nm.

Fabrication of ultrathin multilayered superomniphobic nanocoatings by liquid flame spray, atomic layer deposition, and silanization

NASA Astrophysics Data System (ADS)

Sorvali, Miika; Vuori, Leena; Pudas, Marko; Haapanen, Janne; Mahlberg, Riitta; Ronkainen, Helena; Honkanen, Mari; Valden, Mika; Mäkelä, Jyrki M.

2018-05-01

Superomniphobic, i.e. liquid-repellent, surfaces have been an interesting area of research during recent years due to their various potential applications. However, producing such surfaces, especially on hard and resilient substrates like stainless steel, still remains challenging. We present a stepwise fabrication process of a multilayered nanocoating on a stainless steel substrate, consisting of a nanoparticle layer, a nanofilm, and a layer of silane molecules. Liquid flame spray was used to deposit a TiO2 nanoparticle layer as the bottom layer for producing a suitable surface structure. The interstitial Al2O3 nanofilm, fabricated by atomic layer deposition (ALD), stabilized the nanoparticle layer, and the topmost fluorosilane layer lowered the surface energy of the coating for enhanced omniphobicity. The coating was characterized with field emission scanning electron microscopy, focused ion beam scanning electron microscopy, x-ray photoelectron spectroscopy, contact angle (CA) and sliding angle (SA) measurements, and microscratch testing. The widely recognized requirements for superrepellency, i.e. CA > 150° and SA < 10°, were achieved for deioinized water, diiodomethane, and ethylene glycol. The mechanical stability of the coating could be varied by tuning the thickness of the ALD layer at the expense of repellency. To our knowledge, this is the thinnest superomniphobic coating reported so far, with the average thickness of about 70 nm.

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.

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

Effect of different surface treatments on adhesion of In-Ceram Zirconia to enamel and dentin substrates.

PubMed

Saker, Samah; Ibrahim, Fatma; Ozcan, Mutlu

2013-08-01

Resin bonding of In-Ceram Zirconia (ICZ) ceramics is still a challenge, especially for minimally invasive applications. This study evaluated the adhesion of ICZ to enamel and dentin after different surface treatments of the ceramic. ICZ ceramic specimens (diameter: 6 mm; thickness: 2 mm) (N = 100) were fabricated following the manufacturer's instructions and randomly assigned to 5 groups (n = 20), according to the surface treatment methods applied. The groups were as follows: group C: no treatment; group SB: sandblasting; group SCS-S: CoJet+silane; group SCS-P: CoJet+Alloy Primer; group GE-S: glaze+ hydrofluoric acid etching (9.6%) for 60 s+silane. Each group was randomly divided into two subgroups to be bonded to either enamel or dentin (n = 10 per group) using MDP-based resin cement (Panavia F2.0). All the specimens were subjected to thermocycling (5000x, 5°C-55°C). The specimens were mounted in a universal testing machine and tensile force was applied to the ceramic/cement interface until failure occurred (1 mm/min). After evaluating all the debonded specimens under SEM, the failure types were defined as either "adhesive" with no cement left on the ceramic surface (score 0) or "mixed" with less than 1/2 of the cement left adhered to the surface with no cohesive failure of the substrate (score 1). The data were statistically evaluated using 2-way ANOVA and Tukey's tests (α = 0.05). The highest tensile bond strength for the enamel surfaces was obtained in group GE-S (18.1 ± 2 MPa) and the lowest in group SB (7.1 ± 1.4 MPa). Regarding dentin, group CSC-P showed the highest (12 ± 1.3 MPa) and SB the lowest tensile bond strength (5.7 ± 0.4 MPa). Groups SB, CSC-S, CSC-P, and GE-S did not show significant differences between the different surface treatments on either enamel or dentin surfaces (p < 0.05, p < 0.001, respectively). Groups CSC-P and GE-S presented similar bond strength for both the enamel and dentin substrates (p < 0.8 and p < 0.9), respectively. While on enamel substrates, exclusively adhesive failures from ICZ (score 0) were found, on dentin exclusively mixed failures were observed (score 1). Adhesion of ICZ to both enamel and dentin can be improved when ceramics are glazed, etched, and silanized, or sandblasted, primed, and cemented with an MDP-based cement.

Superhydrophobic aluminum alloy surfaces by a novel one-step process.

PubMed

Saleema, N; Sarkar, D K; Paynter, R W; Chen, X-G

2010-09-01

A simple one-step process has been developed to render aluminum alloy surfaces superhydrophobic by immersing the aluminum alloy substrates in a solution containing NaOH and fluoroalkyl-silane (FAS-17) molecules. Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and water contact angle measurements have been performed to characterize the morphological features, chemical composition and superhydrophobicity of the surfaces. The resulting surfaces provided a water contact angle as high as ∼162° and a contact angle hysteresis as low as ∼4°. The study indicates that it is possible to fabricate superhydrophobic aluminum surfaces easily and effectively without involving the traditional two-step processes.

Effect of different surface treatments and adhesives on repair bond strength of resin composites after one and 12 months of storage using an improved microtensile test method.

PubMed

Eliasson, S T; Tibballs, J; Dahl, J E

2014-01-01

To evaluate the effect of surface treatments and bonding systems on the repair bond strength between composite materials after one and 12 months of storage, using an improved microtensile test method. A total of 72 composite cylinders (Tetric Evo Ceram, Ivoclar) were fabricated, stored in distilled water for two weeks followed by thermal cycling (5000 times between 5°C and 55°C), and served as substrate. The cylinders were mechanically roughened using 320-grit silicon carbide sandpaper, etched with 37% phosphoric acid gel, rinsed with water, and divided equally into three experimental groups: group 1, unchanged surface; group 2, sandblasting of the surface (CoJet tribochemical silica sand, 3M ESPE; Microetcher II, Danville Engineering Inc); and group 3, surface silane coating (Bis-Silane, BISCO Inc). Eight control cylinders were prepared and underwent similar aging as the substrate. Each experimental group was divided into subgroups that received the following bonding systems: one-step self-etching adhesive (AdheSE One, Ivoclar Vivadent), two-step self-etching adhesive (Clearfil SE, Kuraray America), and three-step etch-and-rinse adhesive (Adper Scotchbond Multi-Purpose, 3M ESPE). Fresh composite (Tetric Evo Ceram, Ivoclar) was placed and cured on top of the prepared substrate cylinders. The specimens were placed in distilled water for a week and thermocycled the same way as before. Eight composite control cylinders were also stored and thermocycled for the same period of time. Half of the cylinders in each test group were tested at one month and the second half at 12 months. The cylinders were serially sectioned in an automatic cutting machine, producing 10 to 20 1.1 × 1.1-mm test specimen beam from each cylinder. Specimens were prepared for microtensile testing and the tensile strength calculated based on the force at fracture and specimen dimension. The fracture surfaces were examined under a stereomicroscope and the type of fracture noted. The mean tensile strength of composite control was 54.5 ± 6.0 MPa at one month and 49.6 ± 5.1 MPa at 12 months. The mean tensile strength for the repaired groups ranged from 26.4 ± 6.8 MPa to 49.9 ± 10.4 MPa at one month and 21.2 ± 9.9 to 41.3 ± 7.5 at 12 months. There was a statistical difference between all groups (p<0.05) at one month. This difference was less pronounced at 12 months. The highest repair strength was obtained in the group having a silane-coated surface and Clearfil, the two-step self-etching adhesive. Clearfil also had the highest repair strength within each surface treatment group. There was a tendency for lower tensile strength at 12 months compared with one month. Most fractures were of the adhesive type; the highest number of cohesive fractures, 16% at one month and 12% at 12 months, were in groups with the highest tensile strength. The best repair bond strength was achieved by using freshly mixed silane solution on the substrate in addition to an adhesive, rendering a thin bonding layer.

Plasma Diagnostics For The Investigation of Silane Based Glow Discharge Deposition Processes

NASA Astrophysics Data System (ADS)

Mataras, Dimitrios

2001-10-01

In this work is presented the study of microcrystalline silicon PECVD process through highly diluted silane in hydrogen discharges. The investigation is performed by applying different non intrusive plasma diagnostics (electrical, optical, mass spectrometric and laser interferometric measurements). Each of these measurements is related to different plasma sub-processes (gas physics, plasma chemistry and plasma surface interaction) and compose a complete set, proper for the investigation of the effect of external discharge parameters on the deposition processes. In the specific case these plasma diagnostics are applied for prospecting the optimal experimental conditions from the ic-Si:H deposition rate point of view. Namely, the main characteristics of the effect of frequency, discharge geometry, power consumption and total gas pressure on the deposition process are presented successively. Special attention is given to the study of the frequency effect (13.56 MHz 50 MHz) indicating that the correct way to compare results of different driving frequency discharges is by maintaining constant the total power dissipation in the discharge. The important role of frequency in the achievement of high deposition rates and on the optimization of all other parameters is underlined. Finally, the proper combination of experimental conditions that result from the optimal choice of each of the above-mentioned discharge parameters and lead to high microcrystalline silicon deposition rates (7.5 Å/sec) is presented. The increase of silane dissociation rate towards neutral radicals (frequency effect), the contribution of highly sticking to the surface radicals (discharge geometry optimum) and the controlled production of higher radicals through secondary gas phase reactions (total gas pressure), are presented as prerequisites for the achievement of high deposition rates.

Preparation and antifouling properties of 2-(meth-acryloyloxy)ethyl cholinephosphate based polymers modified surface with different molecular architectures by ATRP.

PubMed

Jiang, Yuchen; Su, Yuling; Zhao, Lili; Meng, Fancui; Wang, Quanxin; Ding, Chunmei; Luo, Jianbin; Li, Jianshu

2017-08-01

Choline phosphate (CP) containing polymers modified surfaces have been shown good resist to the adhesion of proteins while prompt the attaching of mammalian cells due to the dipole pairing between the CP groups of the polymer and the phosphorylcholine (PC) groups on the cell membrane. However, the antifouling activities of CP modified surface against microbes have not been investigated at present. In addition, CP containing polymers modified surface with different molecular architectures has not been prepared and studied. To this end, glass slides surface modified with two different 2-(meth-acryloyloxy)ethyl cholinephosphate (MCP) containing polymer (PMCP) structures, i.e. brush-like (Glass-PMCP) and bottle brush-like (Glass-PHEMA-g-PMCP) architectures, were prepared in this work by surface-initiated atom transfer radical polymerization (SI-ATRP). The surface physichemical and antifouling properties of the prepared surfaces were characterized and studied. The Glass-PMCP shows improved antifouling properties against proteins and bacteria as compared to pristine glass slides (Glass-OH) and glass slides grafted with poly(2-hydroxyethyl methacrylate) (Glass-PHEMA). Notably, a synergetic fouling resistant properties of PHEMA and PMCP is presented for Glass-PHEMA-g-PMCP, which shows superior antifouling activities over Glass-PHEMA and Glass-PMCP. Furthermore, glass slides containing PMCP, i.e. Glass-PMCP and Glas-PHEMA-g-PMCP, decrease platelet adhesion and prevent their activation significantly. Therefore, the combination of antifouling PHEMA and PMCP into one system holds potential for prevention of bacterial fouling and biomaterial-centered infections. Copyright © 2017 Elsevier B.V. All rights reserved.

Fluoride glass: Crystallization, surface tension

NASA Technical Reports Server (NTRS)

Doremus, R. H.

1988-01-01

Fluoride glass was levitated acoustically in the ACES apparatus on STS-11, and the recovered sample had a different microstructure from samples cooled in a container. Further experiments on levitated samples of fluoride glass are proposed. These include nucleation, crystallization, melting observations, measurement of surface tension of molten glass, and observation of bubbles in the glass. Ground experiments are required on sample preparation, outgassing, and surface reactions. The results should help in the development and evaluation of containerless processing, especially of glass, in the development of a contaminent-free method of measuring surface tensions of melts, in extending knowledge of gas and bubble behavior in fluoride glasses, and in increasing insight into the processing and properties of fluoride glasses.

Repair bond strength in aged methacrylate- and silorane-based composites.

PubMed

Bacchi, Atais; Consani, Rafael Leonardo; Sinhoreti, Mario Alexandre; Feitosa, Victor Pinheiro; Cavalcante, Larissa Maria; Pfeifer, Carmem Silva; Schneider, Luis Felipe

2013-10-01

To evaluate the tensile bond strength at repaired interfaces of aged dental composites, either dimethacrylate- or silorane-based, when subjected to different surface treatments. The composites used were Filtek P60 (methacrylate-based, 3M ESPE) and Filtek P90 (silorane-based, 3M ESPE), of which 50 slabs were stored for 6 months at 37°C. The surface of adhesion was abraded with a 600-grit silicone paper and the slabs repaired with the respective composite, according to the following surface treatment protocols: G1: no treatment; G2: adhesive application; G3: silane + adhesive; G4: sandblasting (Al2O3) + adhesive; G5: sandblasting (Al2O3) + silane + adhesive. After 24-h storage in distilled water at 37°C, tensile bond strength (TBS) was determined in a universal testing machine (Instron 4411) at a crosshead speed of 0.5 mm/min. The original data were submitted to two-way ANOVA and Tukey's test (α = 5%). The methacrylate-based composite presented a statistically significantly higher repair potential than did the silorane-based resin (p = 0.0002). Of the surface treatments for the silorane-based composite, aluminum-oxide air abrasion and adhesive (18.5 ± 3.3MPa) provided higher bond strength than only adhesive application or the control group without surface treatment. For Filtek P60, the control without treatment presented lower repair strength than all other groups with surface treatments, which were statistically similar to each other. The interaction between the factors resin composite and surface treatment was significant (p = 0.002). For aged silorane-based materials, repairs were considered successful after sandblasting (Al2O3) and adhesive application. For methacrylate resin, repair was successful with all surface treatments tested.

Fabrication of glass microspheres with conducting surfaces

DOEpatents

Elsholz, William E.

1984-01-01

A method for making hollow glass microspheres with conducting surfaces by adding a conducting vapor to a region of the glass fabrication furnace. As droplets or particles of glass forming material pass through multiple zones of different temperature in a glass fabrication furnace, and are transformed into hollow glass microspheres, the microspheres pass through a region of conducting vapor, forming a conducting coating on the surface of the microspheres.

Fabrication of glass microspheres with conducting surfaces

DOEpatents

Elsholz, W.E.

1982-09-30

A method for making hollow glass microspheres with conducting surfaces by adding a conducting vapor to a region of the glass fabrication furnace. As droplets or particles of glass forming material pass through multiple zones of different temperature in a glass fabrication furnace, and are transformed into hollow glass microspheres, the microspheres pass through a region of conducting vapor, forming a conducting coating on the surface of the microspheres.

Synthesis, properties and applications of bio-based materials

NASA Astrophysics Data System (ADS)

Srinivasan, Madhusudhan

Bio-based feedstock have become very significant as they offer a value proposition in terms of carbon balance and also in terms of endowing biodegradability where needed. Thus a lot of attention is being given to the modification such feedstock for different applications. Soybean oil is one such feedstock. The oil is a triglyceride ester composed of different fatty acids, which are common to other plant oils. Thus soybean oil serves as a platform for plant oils, as modifications of this oil, can in theory be extended to cover other plant oils. Methyl oleate was used as a model fatty acid ester, to synthesize hydroxyesters with ethylene glycol via a two stage oxidative cleavage of the double bonds. Ozone was chosen as the oxidant due to its many advantages. The first stage involved oxidation of the double bond to aldehydes, ozonides and acetals, which were subsequently converted to hydroxyesters (hydroxy values of 220 - 270) in near quantitative yield by treatment with Oxone. This method could be extended to soybean oil to make "polyols" which could find applications in resin syntheses. Silylation was employed as another platform to functionalize soybean oil and fatty acid methyl esters with a reactive silane (vinyltrimethoxy silane). This simple modification produced materials that are cured by atmospheric moisture and are useful as coatings. The silylation was controlled by varying the grafting time, cure temperature and the concentration of the silane. Products with gel content as high as 90% could be achieved. The coating exhibited good adhesion to metal, glass, concrete and paper. Steel panels coated with these coatings exhibited good stability against corrosion in high humidity conditions and moderate stability against a salt spray. The silylation was also successfully utilized to improve the tensile strength of the blend of biodegradable polyester, poly (butylene adipate-co-terephthalate) with talc. A reactive extrusion process was employed to graft vinyl silanes on the polyester in short reaction times of 5 minutes. This improved the compatibility with the talc filler. This biodegradable polyester product was characterized by high tensile strength and moderate elongation. The modification method is simple is applicable to a variety of aliphatic biodegradable polyesters. Finally a rapid polymerization of 1, 4-dioxan-2-one in very short times was accomplished with titanium alkoxides as initiators. At low [monomer]/ [initiator] ratios (100:1), nearly all the alkoxide groups initiated polymerization. High conversions up to 90% were achieved even at high ratios (2400:1). The activation energy for polymerization for titanium tetraisopropoxide is the lowest reported (33.5 kJ/mol) for this monomer system.

High-pressure synthesis, amorphization, and decomposition of silane.

PubMed

Hanfland, Michael; Proctor, John E; Guillaume, Christophe L; Degtyareva, Olga; Gregoryanz, Eugene

2011-03-04

By compressing elemental silicon and hydrogen in a diamond anvil cell, we have synthesized polymeric silicon tetrahydride (SiH(4)) at 124 GPa and 300 K. In situ synchrotron x-ray diffraction reveals that the compound forms the insulating I4(1)/a structure previously proposed from ab initio calculations for the high-pressure phase of silane. From a series of high-pressure experiments at room and low temperature on silane itself, we find that its tetrahedral molecules break up, while silane undergoes pressure-induced amorphization at pressures above 60 GPa, recrystallizing at 90 GPa into the polymeric crystal structures.

Improved laser damage threshold for chalcogenide glasses through surface microstructuring

NASA Astrophysics Data System (ADS)

Florea, Catalin; Sanghera, Jasbinder; Busse, Lynda; Shaw, Brandon; Aggarwal, Ishwar

2011-03-01

We demonstrate improved laser damage threshold of chalcogenide glasses with microstructured surfaces as compared to chalcogenide glasses provided with traditional antireflection coatings. The surface microstructuring is used to reduce Fresnel losses over large bandwidths in As2S3 glasses and fibers. The treated surfaces show almost a factor of two of improvement in the laser damage threshold when compared with untreated surfaces.

Composition-dependent metallic glass alloys correlate atomic mobility with collective glass surface dynamics.

PubMed

Nguyen, Duc; Zhu, Zhi-Guang; Pringle, Brian; Lyding, Joseph; Wang, Wei-Hua; Gruebele, Martin

2016-06-22

Glassy metallic alloys are richly tunable model systems for surface glassy dynamics. Here we study the correlation between atomic mobility, and the hopping rate of surface regions (clusters) that rearrange collectively on a minute to hour time scale. Increasing the proportion of low-mobility copper atoms in La-Ni-Al-Cu alloys reduces the cluster hopping rate, thus establishing a microscopic connection between atomic mobility and dynamics of collective rearrangements at a glass surface made from freshly exposed bulk glass. One composition, La60Ni15Al15Cu10, has a surface resistant to re-crystallization after three heating cycles. When thermally cycled, surface clusters grow in size from about 5 glass-forming units to about 8 glass-forming units, evidence of surface aging without crystal formation, although its bulk clearly forms larger crystalline domains. Such kinetically stable glass surfaces may be of use in applications where glassy coatings stable against heating are needed.

Recruiting physisorbed water in surface polymerization for bio-inspired materials of tunable hydrophobicity

DOE PAGES

Oyola-Reynoso, S.; Tevis, I. D.; Chen, J.; ...

2016-08-18

Here, chemical grafting has been widely used to modify the surface properties of materials, especially surface energy for controlled wetting, because of the resilience of such coatings/modifications. Reagents with multiple reactive sites have been used with the expectation that a monolayer will form. The step-growth polymerization mechanism, however, suggests the possibility of gel formation for hydrolyzable moieties in the presence of physisorbed water. In this report, we demonstrated that using alkyltrichlorosilanes (trivalent [i.e., 3 reactive sites]) in the surface modification of a cellulosic material (paper) does not yield a monolayer but rather gives surface-bound particles. We infer that the presencemore » of physisorbed (surface-bound) water allows for polymerization (or oligomerization) of the silane prior to its attachment on the surface. Surface energy mismatch between the hydrophobic tails of the growing polymer and any unreacted bound water leads to the assembly of the polymerizing material into spherical particles to minimize surface tension. By varying paper grammage (16.2–201.4 g m –2), we varied the accessible surface area and thus the amount of surface-adsorbed water, allowing us to control the ratio of the silane to the bound water. Using this approach, polymeric particles were formed on the surface of cellulose fibers ranging from ~70 nm to a film. The hydrophobicity of the surface, as determined by water contact angles, correlates with particle sizes (p < 0.001, Student's t-test), and, hence, the hydrophobicity can be tuned (contact angle between 94° and 149°). Using a model structure of a house, we demonstrated that as a result of this modification, paper-based houses can be rendered self-cleaning or tolerant to surface running water. In another application, we demonstrated that the felicitous choice of architectural design allows for the hydrophobic paper to be used for water harvesting.« less

Extreme wettability of nanostructured glass fabricated by non-lithographic, anisotropic etching

PubMed Central

Yu, Eusun; Kim, Seul-Cham; Lee, Heon Ju; Oh, Kyu Hwan; Moon, Myoung-Woon

2015-01-01

Functional glass surfaces with the properties of superhydrophobicity/or superhydrohydrophilicity, anti-condensation or low reflectance require nano- or micro-scale roughness, which is difficult to fabricate directly on glass surfaces. Here, we report a novel non-lithographic method for the fabrication of nanostructures on glass; this method introduces a sacrificial SiO2 layer for anisotropic plasma etching. The first step was to form nanopillars on SiO2 layer-coated glass by using preferential CF4 plasma etching. With continuous plasma etching, the SiO2 pillars become etch-resistant masks on the glass; thus, the glass regions covered by the SiO2 pillars are etched slowly, and the regions with no SiO2 pillars are etched rapidly, resulting in nanopatterned glass. The glass surface that is etched with CF4 plasma becomes superhydrophilic because of its high surface energy, as well as its nano-scale roughness and high aspect ratio. Upon applying a subsequent hydrophobic coating to the nanostructured glass, a superhydrophobic surface was achieved. The light transmission of the glass was relatively unaffected by the nanostructures, whereas the reflectance was significantly reduced by the increase in nanopattern roughness on the glass. PMID:25791414

Au nanoparticles films used in biological sensing

NASA Astrophysics Data System (ADS)

Rosales Pérez, M.; Delgado Macuil, R.; Rojas López, M.; Gayou, V. L.; Sánchez Ramírez, J. F.

2009-05-01

Lactobacillus para paracasei are used commonly as functional food and probiotic substances. In this work Au nanoparticles self-assembled films were used for Lactobacillus para paracasei determination at five different concentrations. Functionalized substrates were immersed in a colloidal solution for one and a half hour at room temperature and dried at room temperature during four hours. After that, drops of Lactobacillus para paracasei in aqueous solution were put into the Au nanoparticles film and let dry at room temperature for another two hours. Infrared spectroscopy in attenuated total reflectance sampling mode was used to observe generation peaks due to substrate silanization, enhancement of Si-O band intensity due to the Au colloids added to silanized substrate and also to observe the enhancement of Lactobacillus para paracasei infrared intensity of the characteristic frequencies at 1650, 1534 and 1450 cm-1 due to surface enhancement infrared absorption.

Effect of Filler Content and Chemical Modification on Mechanical Properties of Polylactic Acid/Polymethyl Methacrylate/Nypa Fruticans Husk Biocomposites

NASA Astrophysics Data System (ADS)

Mohamad Syahmie, MR; Pei Leng, T.; Nurul Najwa, Zabidi

2018-03-01

The main purpose of incorporating Nypa fruticans husks (NFH) into Polylactic acid (PLA)/Polymethylmethacrylate (PMMA) is to decrease the costs and enhanced the properties of the biocomposites. 3-Aminopropyl Triethoxysilane (3-APE) was used as coupling agent. The effect of NFH content and 3-APE on the mechanical properties and morphology of the biocomposites were investigated. Results show that the effect of NFH content increased Young’s modulus but decreased the tensile strength and elongation at break of PLA/PMMA/NFH biocomposites. However, silanized biocomposites using 3-APE) was found to enhanced the tensile strength and Young’s modulus but decreased the elongation at break of the silanized biocomposites. Scanning electron microscopy (SEM) study of the tensile fracture surface of the biocomposites indicated that the used of 3-APE as couling agent improved the interfacial interaction netween NFH and PLA/PMMA blends.

Locating a silane coupling agent in silica-filled rubber composites by EFTEM.

PubMed

Dohi, Hidehiko; Horiuchi, Shin

2007-11-20

A silane coupling agent (SA) was added to silica/rubber composites at different mixing temperatures and the formation of a coupling layer at the silica/rubber interface was investigated by energy-filtering transmission electron microscopy. Bis(triethoxysilypropyl)tetrasulfane (TESPT), which was used as the SA, reacted with the silanol groups on the silica surface and with styrene-butadiene rubber to form an interfacial coupling layer. The silicon and sulfur elemental distributions were analyzed by electron energy loss spectroscopy (EELS) and elemental mapping. The amount of TESPT trapped in the rubber matrix could be qualitatively estimated by EELS, and the in situ formed coupling layer could be characterized by elemental mapping. The result indicated that the formation of the coupling layer was affected by the mixing temperature. The technique described here will contribute to the study of interface-property relationships and the evaluation of the role of SAs in polymeric composites.

Fabrication of nanocomposites by collagen templated synthesis of layered double hydroxides assisted by an acrylic silane coupling agent

NASA Astrophysics Data System (ADS)

Sun, Yanqing; Zhou, Yuming; Wang, Zhiqiang; Ye, Xiaoyun

2009-02-01

The purpose of this study was to control the fabrication of nanocomposites at the nanoscale interface by collagen templated synthesis of Zn-Al layered double hydroxides (LDHs) assisted by γ-methacryloxypropyl trimethoxy silane (KH570) with further treatment of graft polymerization. The results show that collagen directs the growth of LDHs into curved nanorods by length of 300 nm in perfect consistency with collagen chain in both the size and flexility under the essential hydrophobic environment on the solid surface provided by KH570. The nanorods are aggregated into thin curved platelets due to strong interaction between collagen molecules themselves and strong interaction between collagen and LDH sheets. By further treatment of graft polymerization, the adjacent curved platelets encircle into numerous hollows via chemical linkage, achieving polyporous nanocomposites. Nanohybrid materials with this structure are especially interesting for applications as biosensors or supported catalysis.

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.

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

Catalytic Dehydrogenative Coupling of Hydrosilanes with Alcohols for the Production of Hydrogen On-demand: Application of a Silane/Alcohol Pair as a Liquid Organic Hydrogen Carrier.

PubMed

Ventura-Espinosa, David; Carretero-Cerdán, Alba; Baya, Miguel; García, Hermenegildo; Mata, Jose A

2017-08-10

The compound [Ru(p-cym)(Cl) 2 (NHC)] is an effective catalyst for the room-temperature coupling of silanes and alcohols with the concomitant formation of molecular hydrogen. High catalyst activity is observed for a variety of substrates affording quantitative yields in minutes at room temperature and with a catalyst loading as low as 0.1 mol %. The coupling reaction is thermodynamically and, in the presence of a Ru complex, kinetically favourable and allows rapid molecular hydrogen generation on-demand at room temperature, under air, and without any additive. The pair silane/alcohol is a potential liquid organic hydrogen carrier (LOHC) for energy storage over long periods in a safe and secure way. Silanes and alcohols are non-toxic compounds and do not require special handling precautions such as high pressure or an inert atmosphere. These properties enhance the practical applications of the pair silane/alcohol as a good LOHC in the automotive industry. The variety and availability of silanes and alcohols permits a pair combination that fulfils the requirements for developing an efficient LOHC. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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

A novel technique for producing antibody-coated microprobes using a thiol-terminal silane and a heterobifunctional crosslinker.

PubMed

Routh, V H; Helke, C J

1997-02-01

Antibody-coated microprobes are used to measure neuropeptide release in the central nervous system. Although they are not quantitative, they provide the most precise spatial resolution of the location of in vivo release of any currently available method. Previous methods of coating antibody microprobes are difficult and time-consuming. Moreover, using these methods we were unable to produce evenly coated antibody microprobes. This paper describes a novel method for the production of antibody microprobes using thiol-terminal silanes and the heterobifunctional crosslinker, 4-(4-N-maleimidophenyl)butyric acid hydrazide HCl 1/2 dioxane (MPBH). Following silation, glass micropipettes are incubated with antibody to substance P (SP) that has been conjugated to MPBH. This method results in a dense, even coating of antibody without decreasing the biological activity of the antibody. Additionally, this method takes considerably less time than previously described methods without sacrificing the use of antibody microprobes as micropipettes. The sensitivity of the microprobes for SP is in the picomolar range, and there is a linear correlation between the log of SP concentration (M) and B/B0 (r2 = 0.98). The microprobes are stable for up to 3 weeks when stored in 0.1 M sodium phosphate buffer with 50 mM NaCl (pH 7.4) at 5 degrees C. Finally, insertion into the exposed spinal cord of an anesthetized rat for 15 min produces no damage to the antibody coating.

Chemical modifications of Au/SiO2 template substrates for patterned biofunctional surfaces.

PubMed

Briand, Elisabeth; Humblot, Vincent; Landoulsi, Jessem; Petronis, Sarunas; Pradier, Claire-Marie; Kasemo, Bengt; Svedhem, Sofia

2011-01-18

The aim of this work was to create patterned surfaces for localized and specific biochemical recognition. For this purpose, we have developed a protocol for orthogonal and material-selective surface modifications of microfabricated patterned surfaces composed of SiO(2) areas (100 μm diameter) surrounded by Au. The SiO(2) spots were chemically modified by a sequence of reactions (silanization using an amine-terminated silane (APTES), followed by amine coupling of a biotin analogue and biospecific recognition) to achieve efficient immobilization of streptavidin in a functional form. The surrounding Au was rendered inert to protein adsorption by modification by HS(CH(2))(10)CONH(CH(2))(2)(OCH(2)CH(2))(7)OH (thiol-OEG). The surface modification protocol was developed by testing separately homogeneous SiO(2) and Au surfaces, to obtain the two following results: (i) SiO(2) surfaces which allowed the grafting of streptavidin, and subsequent immobilization of biotinylated antibodies, and (ii) Au surfaces showing almost no affinity for the same streptavidin and antibody solutions. The surface interactions were monitored by quartz crystal microbalance with dissipation monitoring (QCM-D), and chemical analyses were performed by polarization modulation-reflexion absorption infrared spectroscopy (PM-RAIRS) and X-ray photoelectron spectroscopy (XPS) to assess the validity of the initial orthogonal assembly of APTES and thiol-OEG. Eventually, microscopy imaging of the modified Au/SiO(2) patterned substrates validated the specific binding of streptavidin on the SiO(2)/APTES areas, as well as the subsequent binding of biotinylated anti-rIgG and further detection of fluorescent rIgG on the functionalized SiO(2) areas. These results demonstrate a successful protocol for the preparation of patterned biofunctional surfaces, based on microfabricated Au/SiO(2) templates and supported by careful surface analysis. The strong immobilization of the biomolecules resulting from the described protocol is advantageous in particular for micropatterned substrates for cell-surface interactions.

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

Investigating buried polymer interfaces using sum frequency generation vibrational spectroscopy

PubMed Central

Chen, Zhan

2010-01-01

This paper reviews recent progress in the studies of buried polymer interfaces using sum frequency generation (SFG) vibrational spectroscopy. Both buried solid/liquid and solid/solid interfaces involving polymeric materials are discussed. SFG studies of polymer/water interfaces show that different polymers exhibit varied surface restructuring behavior in water, indicating the importance of probing polymer/water interfaces in situ. SFG has also been applied to the investigation of interfaces between polymers and other liquids. It has been found that molecular interactions at such polymer/liquid interfaces dictate interfacial polymer structures. The molecular structures of silane molecules, which are widely used as adhesion promoters, have been investigated using SFG at buried polymer/silane and polymer/polymer interfaces, providing molecular-level understanding of polymer adhesion promotion. The molecular structures of polymer/solid interfaces have been examined using SFG with several different experimental geometries. These results have provided molecular-level information about polymer friction, adhesion, interfacial chemical reactions, interfacial electronic properties, and the structure of layer-by-layer deposited polymers. Such research has demonstrated that SFG is a powerful tool to probe buried interfaces involving polymeric materials, which are difficult to study by conventional surface sensitive analytical techniques. PMID:21113334

Effect of different surface treatments and retainer designs on the retention of posterior Pd-Ag porcelain-fused-to-metal resin-bonded fixed partial dentures

PubMed Central

Chen, Xiwen; Zhang, Yixin; Zhou, Jinru; Chen, Chenfeng; Zhu, Zhimin; Li, Lei

2018-01-01

The aim of this study was to investigate the adhesive property of palladium-silver alloy (Pd-Ag) and the simulated clinical performance of Pd-Ag porcelain-fused-to-metal (PFM), resin-bonded, fixed partial dentures (RBFPDs). A total of 40 Pd-Ag discs (diameter=5 mm) were prepared and divided into the following four groups (n=10): a) No sandblasting, used as a control; and b, 50 µm; c, 110 µm; and d, 250 µm aluminum oxide (Al2O3) particles, respectively. Another 50 discs were pre-sandblasted and divided into five groups (n=10) subjected to different treatments: e) Sandblasting, used as a control; f) silane; g) alloy primer; h) silica coating + silane and i) silica coating + alloy primer. All 90 discs were bonded to enamel with Panavia F 2.0 and then subjected to shear bond strength (SBS) testing. The fracture surfaces were examined by scanning electron microscopy. Next, 40 missing maxillary second premolar models were restored with one of the four following RBFPD designs (n=10): I) A premolar occlusal bar combined with molar double rests (MDR); II) both occlusal bars with a wing (OBB); III) a premolar occlusal bar combined with a molar dental band (MDB); and IV) two single rests adjacent to the edentulous space with a wing (SRB) used as a control. All specimens were aged with thermal cycling and mechanical loading. Subsequently, they were loaded until broken. The data were analyzed by one-way analysis of variance. Al2O3 (250 µm) abrasion provided the highest SBS (P<0.05). The alloy primer and silica + silane exhibited increased SBS. Furthermore, fracture analysis revealed that the failure mode varied among the different treatments. Whereas MDB exhibited the highest retention (P<0.05), that of OBB was greater than that of MDR (P<0.05), and the control exhibited the lowest retention. Abrasion with Al2O3 (250 µm) effectively increased the adhesive property of Pd-Ag. Additionally, treatment with the alloy primer and silica coating + silane was able to increase the adhesive property of abraded Pd-Ag. Under the present conditions, all three modified retainer types provided improved outcomes for Pd-Ag PFM RBFPDs compared with the control. PMID:29434797

Surface Conductive Glass.

ERIC Educational Resources Information Center

Tanaka, John; Suib, Steven L.

1984-01-01

Discusses the properties of surface-conducting glass and the chemical nature of surface-conducting stannic (tin) oxide. Also provides the procedures necessary for the preparation of surface-conducting stannic oxide films on glass substrates. The experiment is suitable for the advanced inorganic chemistry laboratory. (JN)

Molecularly imprinted nanopatterns for the recognition of biological warfare agent ricin.

PubMed

Pradhan, Santwana; Boopathi, M; Kumar, Om; Baghel, Anuradha; Pandey, Pratibha; Mahato, T H; Singh, Beer; Vijayaraghavan, R

2009-11-15

Molecularly imprinted polymer (MIP) for biological warfare agent (BWA) ricin was synthesized using silanes in order to avoid harsh environments during the synthesis of MIP. The synthesized MIP was utilized for the recognition of ricin. The complete removal of ricin from polymer was confirmed by fluorescence spectrometer and SEM-EDAX. SEM and EDAX studies confirmed the attachment of silane polymer on the surface of silica gel matrix. SEM image of Ricin-MIP exhibited nanopatterns and it was found to be entirely different from the SEM image of non-imprinted polymer (NIP). BET surface area analysis revealed more surface area (227 m(2)/g) for Ricin-MIP than that of NIP (143 m(2)/g). In addition, surface area study also showed more pore volume (0.5010 cm(3)/g) for Ricin-MIP than that of NIP (0.2828 cm(3)/g) at 12 nm pore diameter confirming the presence of imprinted sites for ricin as the reported diameter of ricin is 12 nm. The recognition and rebinding ability of the Ricin-MIP was tested in aqueous solution. Ricin-MIP rebound more ricin when compared to the NIP. Chromatogram obtained with Ricin-MIP exhibited two peaks due to imprinting, however, chromatogram of NIP exhibited only one peak for free ricin. SDS-PAGE result confirmed the second peak observed in chromatogram of Ricin-MIP as ricin peak. Ricin-MIP exhibited an imprinting efficiency of 1.76 and it also showed 10% interference from the structurally similar protein abrin.

Femtosecond transient absorption spectroscopy of silanized silicon quantum dots

NASA Astrophysics Data System (ADS)

Kuntermann, Volker; Cimpean, Carla; Brehm, Georg; Sauer, Guido; Kryschi, Carola; Wiggers, Hartmut

2008-03-01

Excitonic properties of colloidal silicon quantum dots (Si qdots) with mean sizes of 4nm were examined using stationary and time-resolved optical spectroscopy. Chemically stable silicon oxide shells were prepared by controlled surface oxidation and silanization of HF-etched Si qdots. The ultrafast relaxation dynamics of photogenerated excitons in Si qdot colloids were studied on the picosecond time scale from 0.3psto2.3ns using femtosecond-resolved transient absorption spectroscopy. The time evolution of the transient absorption spectra of the Si qdots excited with a 150fs pump pulse at 390nm was observed to consist of decays of various absorption transitions of photoexcited electrons in the conduction band which overlap with both the photoluminescence and the photobleaching of the valence band population density. Gaussian deconvolution of the spectroscopic data allowed for disentangling various carrier relaxation processes involving electron-phonon and phonon-phonon scatterings or arising from surface-state trapping. The initial energy and momentum relaxation of hot carriers was observed to take place via scattering by optical phonons within 0.6ps . Exciton capturing by surface states forming shallow traps in the amorphous SiOx shell was found to occur with a time constant of 4ps , whereas deeper traps presumably localized in the Si-SiOx interface gave rise to exciton trapping processes with time constants of 110 and 180ps . Electron transfer from initially populated, higher-lying surface states to the conduction band of Si qdots (>2nm) was observed to take place within 400 or 700fs .

Surface Coatings on Lunar Volcanic Glasses

NASA Technical Reports Server (NTRS)

Wentworth, Susan J.; McKay, D. S.; Thomas,-Keprta, K. L.; Clemett, S. J.

2007-01-01

We are undertaking a detailed study of surface deposits on lunar volcanic glass beads. These tiny deposits formed by vapor condensation during cooling of the gases that drove the fire fountain eruptions responsible for the formation of the beads. Volcanic glass beads are present in most lunar soil samples in the returned lunar collection. The mare-composition beads formed as a result of fire-fountaining approx.3.4-3.7 Ga ago, within the age range of large-scale mare volcanism. Some samples from the Apollo 15 and Apollo 17 landing sites are enriched in volcanic spherules. Three major types of volcanic glass bead have been identified: Apollo 15 green glass, Apollo 17 orange glass, and Apollo 17 "black" glass. The Apollo 15 green glass has a primitive composition with low Ti. The high-Ti compositions of the orange and black glasses are essentially identical to each other but the black glasses are opaque because of quench crystallization. A poorly understood feature common to the Apollo 15 and 17 volcanic glasses is the presence of small deposits of unusual materials on their exterior surfaces. For example, early studies indicated that the Apollo 17 orange glasses had surface enrichments of In, Cd, Zn, Ga, Ge, Au, and Na, and possible Pb- and Zn-sulfides, but it was not possible to characterize the surface features in detail. Technological advances now permit us to examine such features in detail. Preliminary FE-TEM/X-ray studies of ultramicrotome sections of Apollo 15 green glass indicate that the surface deposits are heterogeneous and layered, with an inner layer consisting of Fe with minor S and an outer layer of Fe and no S, and scattered Zn enrichments. Layering in surface deposits has not been identified previously; it will be key to defining the history of lunar fire fountaining.

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.

Evaluation of tensile retention of Y-TZP crowns after long-term aging: effect of the core substrate and crown surface conditioning.

PubMed

Amaral, R; Rippe, M; Oliveira, B G; Cesar, P F; Bottino, M A; Valandro, L F

2014-01-01

This study evaluated the effect of the core substrate type (dentin and composite resin) on the retention of crowns made of yttrium oxide stabilized tetragonal zirconia polycrystal (Y-TZP), submitted to three inner surface conditionings. For this purpose, 72 freshly extracted molars were embedded in acrylic resin, perpendicular to the long axis, and prepared for full crowns: 36 specimens had crown preparations in dentin; the remaining 36 teeth had the crowns removed, and crown preparations were reconstructed with composite resin plus fiber posts with dimensions identical to the prepared dentin. The preparations were impressed using addition silicone, and 72 Y-TZP copings for the tensile test were produced. Cementation was performed with a dual-cured cement containing phosphate monomers. For cementation, the crown preparation (dentin or resin) was conditioned with the adhesive system, and the ceramic was subjected to one of three surface treatments: isopropyl alcohol, tribochemical silica coating, or thin low-fusing glassy porcelain layer application plus silanization. After 24 hours, all specimens were submitted to thermocycling (6000 cycles) and placed in a special tensile testing device in a universal testing machine to determine failure loads. The failure modes of all samples were analyzed under a stereomicroscope. Two-way analysis of variance showed that the surface treatment and substrate type (α=0.05) affected the tensile retention results. The dentin substrate presented the highest tensile retention values, regardless of the surface treatment. When the substrate was resin, the tribochemical silica coating and low-fusing glaze application plus silanization groups showed the higher retention values.

Comparison of shear bond strength of orthodontic brackets using various zirconia primers.

PubMed

Lee, Ji-Yeon; Kim, Jin-Seok; Hwang, Chung-Ju

2015-07-01

The aim of this study was to compare the shear bond strength (SBS) of orthodontic brackets bonded to zirconia surfaces using three different zirconia primers and one silane primer, and subjected to thermocycling. We designed 10 experimental groups following the surface treatment and thermocycling. The surface was treated with one of the following method: no-primer (NP), Porcelain Conditioner (PC), Z-PRIME Plus (ZP), Monobond Plus (MP) and Zirconia Liner Premium (ZL) (n=20). Then each group was subdivided to non-thermocycled and thermocycled groups (NPT, PC, ZPT, MPT, ZLT) (n=10). Orthodontic brackets were bonded to the specimens using Transbond™ XT Paste and light cured for 15 s at 1,100 mW/cm(2). The SBS was measured at a 1 mm/min crosshead speed. The failure mode was assessed by examination with a stereomicroscope and the amount of bonding resin remaining on the zirconia surface was scored using the modified adhesive remnant index (ARI). The SBS of all experimental groups decreased after thermocycling. Before thermocycling, the SBS was ZL, ZP ≥ MP ≥ PC > NP but after thermocycling, the SBS was ZLT ≥ MPT ≥ ZPT > PCT = NPT (p > 0.05). For the ARI score, both of the groups lacking primer (NP and NPT) displayed adhesive failure modes, but the groups with zirconia primers (ZP, ZPT, MP, MPT, ZL, and ZLT) were associated with mixed failure modes. Surface treatment with a zirconia primer increases the SBS relative to no-primer or silane primer application between orthodontic brackets and zirconia prostheses.

Effect of sandblasting, silica coating, and laser treatment on the microtensile bond strength of a dental zirconia ceramic to resin cements.

PubMed

Mahmoodi, Nasrin; Hooshmand, Tabassom; Heidari, Solmaz; Khoshro, Kimia

2016-02-01

The purpose of this in vitro study was to evaluate the effect of laser irradiation as well as other surface treatment methods on the microtensile bond strength of a dental zirconia ceramic to the two types of resin cements. Zirconia ceramic blocks (ICE Zirkon) were sintered according to the manufacturer's instructions and duplicated in resin composites. The ceramic specimens were divided into four groups according to the following surface treatments: no surface treatment (control), sandblasting with alumina, silica coating plus silanization, and Nd:YAG laser irradiation. The specimens were divided equally and then bonded with Panavia F2.0 (self-etching resin cement) and Clearfil SA Luting (self-adhesive resin cement) to the composite blocks. The bonded ceramic-composite blocks were stored in distilled water at 37 °C for 72 h, cut to prepare bar-shaped specimens with a bonding area of approximately 1 mm(2), and thermocycled for 3000 cycles between 5 and 55 °C, and the microtensile bond strengths were measured using a universal testing machine. The data were analyzed by ANOVA and Tukey post hoc test. The results showed that the self-adhesive resin cement used in this study did not improve the microtensile bond strength when the zirconia surface was sandblasted by alumina. The use of the Nd:YAG laser did not enhance the bond strength between the zirconia and both types of resin cements. In addition, silica coating of the zirconia surfaces plus silane application significantly improved the bond strength regardless of the type of resin cement utilized.

Influence of surface treatment on shear bond strength of orthodontic brackets.

PubMed

Brunharo, Ione Helena Vieira Portella; Fernandes, Daniel Jogaib; de Miranda, Mauro Sayão; Artese, Flavia

2013-01-01

The shear bond strength of orthodontic brackets bonded to micro-hybrid and micro-particulate resins under different surface treatment methods was assessed. Two hundred and eighty test samples were divided into 28 groups (n = 10), where 140 specimens were filled with Durafill micro-particulate resin and 140 with Charisma composite. In 140 samples, a coupling agent (silane) was applied. The surface treatment methods were: Phosphoric and hydrofluoric acid etching, sodium bicarbonate and aluminum oxide blasting, stone and burs. A Universal Instron Machine was used to apply an occlusal shear force directly to the resin composite bracket surface at a speed of 0.5 mm/min. The means were compared using analysis of variance and multivariate regression to assess the interaction between composites and surface treatment methods. Means and standard deviations for the groups were: Sodium bicarbonate jet 11.27 ± 2.78; burs 9.26 ± 3.01; stone 7.95 ± 3.67; aluminum oxide blasting 7.04 ± 3.21; phosphoric acid 5.82 ± 1.90; hydrofluoric acid 4.54 ± 2.87, and without treatment 2.75 ± 1.49. An increase of 1.94 MPa in shear bond strength was seen in Charisma groups. Silane agent application reduced the Charisma shear bond strength by 0.68 Mpa, but increased Durafill means for bicarbonate blasting (0.83), burs (0.98) and stone drilling (0.46). The sodium bicarbonate blasting, burs and stone drilling methods produced adequate shear bond strength and may be suitable for clinical use. The Charisma micro hybrid resin composite showed higher shear bond means than Durafill micro particle composite.

Effect of surface mobility on the particle sliding along a bubble or a solid sphere.

PubMed

Wang, Weixing; Zhou, Zhiang; Nandakumar, K; Xu, Zhenghe; Masliyah, Jacob H

2003-03-01

The sliding velocity of glass beads on a spherical surface, made either of an air bubble or of a glass sphere held stationary, is measured to investigate the effect of surface mobility on the particle sliding velocity. The sliding process is recorded with a digital camera and analyzed frame by frame. The sliding glass bead was found to accelerate with increasing angular position on the collector's surface. It reaches a maximum velocity at an angular position of about 100 degrees and then, under certain conditions, the glass bead leaves the surface of the collector. The sliding velocity of the glass bead depends strongly on the surface mobility of a bubble, decreasing with decreasing surface mobility. By a mobile surface we mean one which cannot set up resistive forces to an applied stress on the surface. The sliding velocity on a rigid surface, such as a glass sphere, is much lower than that on a mobile bubble surface. The sliding velocity can be described through a modified Stokes equation. A numerical factor in the modified Stokes equation is determined by fitting the experimental data and is found to increase with decreasing surface mobility. Hydrophobic glass beads sliding on a hydrophobic glass sphere were found to stick at the point of impact without sliding if the initial angular position of the impact is less than some specific angle, which is defined as the critical sticking angle. The sticking of the glass beads can be attributed to the capillary contracting force created by the formation of a cavity due to spontaneous receding of the nonwetting liquid from the contact zone. The relationship between the critical sticking angle and the particle size is established based on the Yushchenko [J. Colloid Interface Sci. 96 (1983) 307] analysis.

Effect of thermal cycling on composites reinforced with two differently sized silica-glass fibers.

PubMed

Meriç, Gökçe; Ruyter, I Eystein

2007-09-01

To evaluate the effects of thermal cycling on the flexural properties of composites reinforced with two differently sized fibers. Acid-washed, woven, fused silica-glass fibers, were heat-treated at 500 degrees C, silanized and sized with one of two sizing resins (linear poly(butyl methacrylate)) (PBMA), cross-linked poly(methyl methacrylate) (PMMA). Subsequently the fibers were incorporated into a polymer matrix. Two test groups with fibers and one control group without fibers were prepared. The flexural properties of the composite reinforced with linear PBMA-sized fibers were evaluated by 3-point bend testing before thermal cycling. The specimens from all three groups were thermally cycled in water (12,000 cycles, 5/55 degrees C, dwell time 30 s), and afterwards tested by 3-point bending. SEM micrographs were taken of the fibers and of the fractured fiber reinforced composites (FRC). The reduction of ultimate flexural strength after thermal cycling was less than 20% of that prior to thermal cycling for composites reinforced with linear PBMA-sized silica-glass fibers. The flexural strength of the composite reinforced with cross-linked PMMA-sized fibers was reduced to less than half of the initial value. This study demonstrated that thermal cycling differently influences the flexural properties of composites reinforced with different sized silica-glass fibers. The interfacial linear PBMA-sizing polymer acts as a stress-bearing component for the high interfacial stresses during thermal cycling due to the flexible structure of the linear PBMA above Tg. The cross-linked PMMA-sizing, however, acts as a rigid component and therefore causes adhesive fracture between the fibers and matrix after the fatigue process of thermal cycling and flexural fracture.

The effect of high fiber fraction on some mechanical properties of unidirectional glass fiber-reinforced composite.

PubMed

Abdulmajeed, Aous A; Närhi, Timo O; Vallittu, Pekka K; Lassila, Lippo V

2011-04-01

This study was designed to evaluate the effect of an increase of fiber-density on some mechanical properties of higher volume fiber-reinforced composite (FRC). Five groups of FRC with increased fiber-density were fabricated and two additional groups were prepared by adding silanated barium-silicate glass fillers (0.7 μm) to the FRC. The unidirectional E-glass fiber rovings were impregnated with light-polymerizable bisGMA-TEGDMA (50-50%) resin. The fibers were pulled through a cylindrical mold with an opening diameter of 4.2mm, light cured for 40s and post-cured at elevated temperature. The cylindrical specimens (n=12) were conditioned at room temperature for 2 days before testing with the three-point bending test (Lloyd Instruments Ltd.) adapted to ISO 10477. Fiber-density was analyzed by combustion and gravimetric analyzes. ANOVA analysis revealed that by increasing the vol.% fraction of E-glass fibers from 51.7% to 61.7% there was a change of 27% (p<0.05) in the modulus of elasticity, 34% (p<0.05) in the toughness, and 15% (p<0.05) in the load bearing capacity, while there was only 8% (p<0.05) increase in the flexural strength although it was statistically insignificant. The addition of particulate fillers did not improve the mechanical properties. This study showed that the properties of FRC could be improved by increasing fibervolume fraction. Modulus of elasticity, toughness, and load bearing capacity seem to follow the law of ratio of quantity of fibers and volume of the polymer matrix more precisely than flexural strength when high fiber-density is used. Copyright © 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

Surface modification of silicon carbide with silane coupling agent and hexadecyl iodiele

NASA Astrophysics Data System (ADS)

Shang, Xujing; Zhu, Yumei; Li, Zhihong

2017-02-01

In this paper, two kinds of silane coupling agents, namely 3-aminopropyl triethoxysilane (KH550) and 3-mercaptopropyl trimethoxysilane (KH590), were adopted as preliminary modifiers to improve the hydrophobic surface properties of silicon carbide (SiC) powder for the first step. The factors that influence the modification effects were investigated by measuring the contact angle. The results showed that KH590 has a better effect than KH550 for the hydrophobic modification of SiC, and the contact angle improved most after SiC powder was reacted with 0.3 g KH590 at 75 °C in aqueous/alcohol solution for 4 h. On account of further enhancement of hydrophobicity, the study was focused on utilizing nucleophilic substitution between KH590 and hexadecyl iodiele to extend the length of alkyl chain. Compared with using KH590 alone, SiC powder modified by KH590 and hexadecyl iodiele showed better water resistance with an increase of contact angle from 106.8° to 127.5°. The Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectra (XPS) as well as X-ray diffraction (XRD) analysis results showed that KH550/KH590 and hexadecyl iodiele can be covalently bonded to the surface of SiC powder without altering its crystal configuration. This methodology may provide a new way of the modification of inorganic materials in further.

Fatigue resistance of bovine teeth restored with resin-bonded fiber posts: effect of post surface conditioning.

PubMed

Zamboni, Sandra C; Baldissara, Paolo; Pelogia, Fernanda; Bottino, Marco Antonio; Scotti, Roberto; Valandro, Luiz Felipe

2008-01-01

This study evaluated the effect of post surface conditioning on the fatigue resistance of bovine teeth restored with resin-bonded fiber-reinforced composite (FRC). Root canals of 20 single-rooted bovine teeth (16 mm long) were prepared to 12 mm using a preparation drill of a double-tapered fiber post system. Using acrylic resin, each specimen was embedded (up to 3.0 mm from the cervical part of the specimen) in a PVC cylinder and allocated into one of two groups (n = 10) based on the post surface conditioning method: acid etching plus silanization or tribochemical silica coating (30 pm SiO(x) + silanization). The root canal dentin was etched (H2PO3 for 30 seconds), rinsed, and dried. A multi-step adhesive system was applied to the root dentin and the fiber posts were cemented with resin cement. The specimens were submitted to one million fatigue cycles. After fatigue testing, a score was given based on the number of fatigue cycles until fracture. All of the specimens were resistant to fatigue. No fracture of the root or the post and no loss of retention of the post were observed. The methodology and the results of this study indicate that tribochemical silica coating and acid etching performed equally well when dynamic mechanical loading was used.

Hydroxyapatite and bioactive glass surfaces for fiber reinforced composite implants via surface ablation by Excimer laser.

PubMed

Kulkova, Julia; Moritz, Niko; Huhtinen, Hannu; Mattila, Riina; Donati, Ivan; Marsich, Eleonora; Paoletti, Sergio; Vallittu, Pekka K

2017-11-01

In skeletal reconstructions, composites, such as bisphenol-A-glycidyldimethacrylate resin reinforced with glass fibers, are potentially useful alternatives to metallic implants. Recently, we reported a novel method to prepare bioactive surfaces for these composites. Surface etching by Excimer laser was used to expose bioactive glass granules embedded in the resin. The purpose of this study was to analyze two types of bioactive surfaces created by this technique. The surfaces contained bioactive glass and hydroxyapatite granules. The selected processing parameters were adequate for the creation of the surfaces. However, the use of porous hydroxyapatite prevented the complete exposure the granules. In cell culture, for bioactive glass coatings, the pattern of proliferation of MG63 cells was comparable to that in the positive control group (Ti6Al4V) while inferior cell proliferation was observed on the surfaces containing hydroxyapatite granules. Scanning electron microscopy revealed osteointegration of implants with both types of surfaces. The technique is suitable for the exposure of solid bioactive glass granules. However, the long-term performance of the surfaces needs further assessment. Copyright © 2017 Elsevier Ltd. All rights reserved.

Interfacial adhesion of dental ceramic-resin systems

NASA Astrophysics Data System (ADS)

Della Bona, Alvaro

The clinical success of resin bonding procedures for indirect ceramic restorations and ceramic repairs depends on the quality and durability of the bond between the ceramic and the resin. The quality of this bond will depend upon the bonding mechanisms that are controlled in part by the surface treatment that promotes micromechanical and/or chemical bonding to the substrate. The objective of this study is to correlate interfacial toughness (K A) with fracture surface morphological parameters of the dental ceramic-resin systems as a function of ceramic surface treatment. The analytical procedures focused on characterizing the microstructure and fracture properties of EmpressRTM ceramics (a leucite-based core ceramic, two lithia disilicate-based core ceramics, and a glass veneer) and determining the ceramic-resin adhesion zone bond strength characteristics. Microstructure and composition are controlling factors in the development of micromechanical retention produced by etching. Silane treated ceramics negated the effect of surface roughening produced by etching, inducing lower surface energy of the ceramic and, reduced bonding effectiveness. There was a positive correlation between WA, tensile bond strength (a), and KA, i.e., higher mean WA value, and higher mean sigma and KA values. This study suggests that (1) the sigma and KA values for ceramic bonded to resin are affected by the ceramic microstructure and the ceramic surface treatments; (2) the definition of the adhesion zone is essential to classify the modes of failure, which should be an integral component of all failure analyses; (3) the microtensile test may be preferable to conventional shear or flexural tests as an indicator of composite-ceramic bond quality; and (4) careful microscopic analysis of fracture surfaces and an x-ray dot map can produce a more consistent and complete description of the fracture process and interpretation of the modes of failure. The mode of failure and fractographic analyses provide important a more comprehensive assessment of mechanisms that control the survival times of dental adhesive systems. Thus, the quality of the bond should not be assessed based on bond strength data alone.

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.