Surface Analysis of Silane Nanolayer on Silica Particles Using 1H Pulse NMR

Nakamura, Yoshinobu; Nishida, Yuji; Honda, Hiroaki; Fujii, Syuji; Sasaki, Mariko

doi:10.1163/016942411x556079

Cited by 30 publications

(32 citation statements)

References 34 publications

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“…The glycidoxy functional silane is widely utilized for reinforcement of the interface for silica particle-filled epoxy resin, such as the encapsulating resin for a semiconductor chip. The surface treatment of silica particles with glycidoxy functional silanes was performed under the same conditions as that for the previously reported mercapto functional silanes [5,7,8]. The influence of the organic functional group of the silane on the molecular mobility of the silane layer on the silica particle surface is discussed with comparison of the previous [5,7,8] and present results.…”

Section: Introductionmentioning

confidence: 67%

“…Surface treatment was conducted in the same way as previously described [5,7,8]. The amount of silane required for monolayer coverage of the silica particles was calculated as previously described [5,7,8], using the area occupied by a single silane molecule and the specific surface area values of the silica particles.…”

Section: Surface Treatmentmentioning

confidence: 99%

“…We have investigated the effect of interfacial adhesion between inorganic fillers surface-treated with various silane coupling agents and a matrix polymer on the mechanical properties of these composites [1][2][3][4][5][6][7][8]. Surface treatment of spherical silica particles using a silane coupling agent with a mercapto group was previously [7] conducted and the structure of the silanelayer formed on the silica surface was analyzed by 1 H pulse nuclear magnetic resonance (NMR).…”

Section: Introductionmentioning

confidence: 99%

“…Surface treatment of spherical silica particles using a silane coupling agent with a mercapto group was previously [7] conducted and the structure of the silanelayer formed on the silica surface was analyzed by 1 H pulse nuclear magnetic resonance (NMR). Silanes with di-alkoxy and tri-alkoxy structures were used as silane coupling agents and the amount of silane loading on the silica surface was varied from one to nine times the amount required for monolayer coverage.…”

Section: Introductionmentioning

confidence: 99%

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Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by¹H pulse NMR

Fukuda

Yamazaki

Fujii

et al. 2013

Journal of Adhesion Science and Technology

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The surface treatment of spherical silica particles using a silane coupling agent with a glycidoxy group was conducted and the effect of the alkoxy group number on the molecular mobility of the silane chain was investigated by 1 H pulse nuclear magnetic resonance (NMR). Silanes with di-alkoxy and tri-alkoxy structures were used, and the silica particles were treated with 2-propanol solution and heated at 120°C for 24 h after solvent evaporation. The surface coverage of the silica surface was in the range from two to three layers. For multilayer coverage, linear chain and network structures were expected to form on the surface by polycondensation reaction using the di-and tri-alkoxy structures, respectively. However, the relaxation times for silane chains with both di-and tri-alkoxy structures measured by pulse NMR were short, which indicates that both silane chains formed rigid network structures. Fourier transform infrared spectroscopic analysis revealed that ring opening of the epoxy group occurred, followed by reaction to form the network structure, even with the di-alkoxy structure. Ring opening of the epoxy group could be reduced by setting the heating temperature at 80°C. There was a significant difference in flexibility between the silane-layers with di-and tri-alkoxy structures after heating at 80°C, as reflected by the relaxation time.

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Section: Introductionmentioning

confidence: 67%

Section: Surface Treatmentmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by¹H pulse NMR

Fukuda

Yamazaki

Fujii

et al. 2013

Journal of Adhesion Science and Technology

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“…Water emulsions of silanes form suspensions composed of two insoluble liquids. Silane is mixed with water and an emulsifier [24].…”

Section: Introductionmentioning

confidence: 99%

Free of Volatile Organic Compounds Protection against Moisture in Building Materials/Zabezpieczenia Przegród Budowlanych Przed Wilgocią Wolne Od Lotnych Związków Organicznych

Suchorab

Barnat-Hunek

Smarzewski

et al. 2014

Ecological Chemistry and Engineering S

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Abstract:The article presents information about moisture protection of building materials. The discussed parameters determining the efficiency of the water protection are material porosity, water absorptivity and surface condition of building materials. Moreover the ecological aspect of hydrophobic VOC-free preparations available on the market has been underlined. The first part of the article is a description of moisture problem in the building envelopes and the possibilities of its prevention. The special attention is put on the electric methods of moisture estimation with a special emphasis on the Time Domain Reflectometry (TDR) method. The second part of the article is devoted an experiment of model red-brick walls exhibited on capillary uptake process. For the experiment three model red-brick walls were built and prepared for water uptake process. The experiment was monitored by the capacitive and surface TDR probes thanks to which the necessity of sampling and material destruction could be avoided. Conducted experiments show the progress of water uptake phenomenon in the model walls which differ in type of protection against moisture and prove the potential of the non-invasive measurements using the surface TDR probes. Basic physical parameters of the applied bricks were determined together with the reflectometric measurements. Furthermore, Scanning Electron Microscopy (SEM) was used to analyze the hydrophobic layer continuity.

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Mechanical properties of silane‐treated silica particle‐filled polyisoprene composites: Influence of the alkoxy group mixing ratio in silane coupling agent containing mercapto group

Nakamura¹,

Nishida²,

Fukuda³

et al. 2012

J of Applied Polymer Sci

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Spherical silica particles were treated with a mixture of silane coupling agents with mercapto functional groups and dialkoxy or trialkoxy groups. The surface coverage, which indicates the number of layers covering the silica surface, was in the range from 1.6 to 6.0. The molecular mobility of the treated layer was analyzed with 1H‐NMR spectroscopy. The silane chain became more flexible with increasing dialkoxy structures in the mixture and with increasing surface coverage. The stress–strain behavior was measured for a composite consisting of the treated silica and vulcanized polyisoprene rubber (PIR). There was no influence of the dialkoxy and trialkoxy mixing ratio for near monolayer coverage. In the case of the pure dialkoxy and low trialkoxy contents, a higher stress was observed at the same strain for surface coverages of 2.4–3.8. However, a longer length flexible silane chain, that is, with a surface coverage of 6.0, was disadvantageous for the reinforcement effect. The results of pulse NMR analysis of the unextracted PIR on the particle surface and swelling test indicate that the reinforcement effect was strongly affected both by entanglement and the crosslinking reaction between the silane chain and PIR at the interfacial region. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013

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Surface Analysis of Silane Nanolayer on Silica Particles Using 1H Pulse NMR

Cited by 30 publications

References 34 publications

Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by¹H pulse NMR

Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by¹H pulse NMR

Free of Volatile Organic Compounds Protection against Moisture in Building Materials/Zabezpieczenia Przegród Budowlanych Przed Wilgocią Wolne Od Lotnych Związków Organicznych

Mechanical properties of silane‐treated silica particle‐filled polyisoprene composites: Influence of the alkoxy group mixing ratio in silane coupling agent containing mercapto group

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Surface Analysis of Silane Nanolayer on Silica Particles Using 1H Pulse NMR

Cited by 30 publications

References 34 publications

Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by1H pulse NMR

Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by1H pulse NMR

Free of Volatile Organic Compounds Protection against Moisture in Building Materials/Zabezpieczenia Przegród Budowlanych Przed Wilgocią Wolne Od Lotnych Związków Organicznych

Mechanical properties of silane‐treated silica particle‐filled polyisoprene composites: Influence of the alkoxy group mixing ratio in silane coupling agent containing mercapto group

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Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by¹H pulse NMR

Influences of the alkoxy group number and treatment condition on the structure of glycidoxy functional silane-treated layer on silica particles analyzed by¹H pulse NMR