Observation of silane coupling agents adsorbed on silica by solid state 1H NMR under fast magic angle spinning

Han, Jianglong; Zuo, Chuanwei; Gu, Qiang; Li, Dawei; Wang, Xiaoliang; Xue, Gi

doi:10.1016/j.apsusc.2008.07.086

Cited by 8 publications

(8 citation statements)

References 22 publications

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“…The NMR signals for protons of adsorbed water on the suspended NPs were completely suppressed, as shown in the spectra of Figure . We recorded 1 H SSNMR spectra from the TiO 2 NPs adsorbed with water, by using fast MAS ( v R = 25 kHz) to suppress line broadening caused by strong 1 H– 1 H couplings and chemical shift anisotropy. , Figures and show 1 H SSNMR spectra for water molecules replaced by OLA on TiO 2 NPs with two different diameters. The 1 H SSNMR spectra were normalized to the quantity of samples.…”

Section: Resultsmentioning

confidence: 99%

“…In our previous studies, we demonstrated that by using fast magic angle spinning (MAS, spinning speed v R of >20 kHz) high-resolution 1 H SSNMR spectra of adsorbed species on nanoparticles could be obtained. ,− Moreover, we demonstrated that the 12-pulse dipolar filter experiment developed by Schmidt-Rohr et al , can be utilized to investigate the mobility of adsorbed ligands on the surface of nanoparticles. ,− This method has been applied to distinguish a “mobile” component that has a dipolar interaction weaker than that of the rigid ones. , …”

Section: Introductionmentioning

confidence: 99%

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Characterization of the Mobility and Reactivity of Water Molecules on TiO₂ Nanoparticles by ¹H Solid-State Nuclear Magnetic Resonance

Zhu

Sun

et al. 2013

ACS Appl. Mater. Interfaces

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Understanding interfacial water behavior is essential to improving our understanding of the surface chemistry and interfacial properties of nanomaterials. Here using 1H solid-state nuclear magnetic resonance (1H SSNMR), we successfully monitored ligand exchange reaction between oleylamine (OLA) and adsorbed water on titanium dioxide nanoparticles (TiO2 NPs). Three different types of interfacial waters with different reactivities were distinguished. The mobility of the adsorbed water molecules was characterized by dipolar filtered 1H SSNMR. Our experimental results demonstrate that the adsorbed water can be categorized into three different layers: (i) rigid water species with restricted mobility closest to the surface of TiO2 NPs, (ii) less mobile water species weakly confined on TiO2 NPs, and (iii) water molecules with high mobility. Water in the third layer could be replaced by OLA, while water in the first and second layers remained intact. The finding that the interfacial water with the highest mobility has the strongest reactivity has guiding significance for tailoring the hydrophilic and hydrophobic properties of TiO2 NPs.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Characterization of the Mobility and Reactivity of Water Molecules on TiO₂ Nanoparticles by ¹H Solid-State Nuclear Magnetic Resonance

Zhu

Sun

et al. 2013

ACS Appl. Mater. Interfaces

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“…Much research has been conducted on the reactivity of silane coupling agents and characterization of the resulting silane layers formed on inorganic surfaces. [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17] We have also characterized the silane layer on inorganic particle surfaces and studied the effect of interfacial adhesion between fillers and a matrix polymer on the mechanical properties of a composite of the treated inorganic particles with various silane coupling agents. [18][19][20][21][22][23][24][25][26][27] In our previous study, [25] spherical silica particles were treated with a silane coupling agent having a mercapto group.…”

Section: Introductionmentioning

confidence: 99%

Tensile properties of styrene-butadiene rubber/silica composites with mercapto functional silane coupling agents: influences of loading method and alkoxy group number

Fukuda

Fujii

Nakamura

et al. 2013

Composite Interfaces

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The influences of alkoxy group number and loading method of silane coupling agents on the mechanical properties of a styrene-butadiene rubber/silica composite were investigated. Mercapto functional silane coupling agents with dialkoxy and trialkoxy structures were used. The pre-treatment method and the integral blend method were compared. Both the fracture stress and modulus at 200% strain were higher in the pre-treatment than in the integral blend for dialkoxy type composites. However, they were higher in the integral blend than in the pre-treatment for trialkoxy-type composites. The interaction between the silane chains on the silica surface and the rubber molecular chains at the interfacial region was estimated by 1 H pulse nuclear magnetic resonance spectroscopy using an unvulcanized silica/ rubber mixture. It was found that the binding of rubber molecular chains by the silane chains was higher in the pre-treatment system for dialkoxy-type composites, whereas it was higher in the integral blend for trialkoxy-type composites. The reason is proposed as follows: in the pre-treatment for dialkoxy type, a linear silane chain formed in the case of multi-layer coverage. The silane chain entangled with the rubber chain in the interfacial region and improved the reinforcement effect. For the trialkoxy type, a network structure formed using the pre-treatment method, lowering the amount of entanglement. However, in the integral blend for trialkoxy type, the formation of the silane network and the entanglement progressed simultaneously during the preparation process. A well-entangled interfacial region was formed.

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“…They are also sometimes directly added to a polymer during processing . Many researchers and our group 37–43 have conducted investigations on the reactivity of silane coupling agents, the characterization of a silane layer formed on an inorganic surface, and the reinforcement effect in composites. Silane coupling agents react with inorganic surfaces as follows .…”

Section: Introductionmentioning

confidence: 99%

Quantitative measurement of physisorbed silane on a silica particle surface treated with silane coupling agents by thermogravimetric analysis

Yamazaki

Karyu

Noda

et al. 2015

J of Applied Polymer Sci

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We investigated a new method for estimating the amount of silanes physisorbed on a silica particle surface treated with silane coupling agents from a weight loss curve measured by thermogravimetric (TG) analysis. The silica particles were treated with 3-glycidoxypropyl trimethoxysilane (GPTMS) or 3-mercaptopropyl trimethoxysilane (MrPTMS) with both dry and wet treatment methods. In the TG curve for silica particles treated with GPTMS, the weight decreased in three steps: 100-1708C (first step), 170-2508C (second step), and 250-4008C (third step). The weight loss in the first step decreased with heating or acetone washing to remove the physisorbed molecules as the posttreatment. The three weight losses were found to be based on physisorbed monomeric silanes (first step), physisorbed polycondensed silanes (second step), and chemisorbed silanes (third step), respectively. The amount of physisorbed silanes on the silane-treated layer could be estimated from the TG curve without solvent washing to remove the physisorbed molecules. The amounts obtained were almost equal to those measured from a comparison of the weight losses for the treated particles before and after acetone washing. A similar tendency was observed for MrPTMS-treated silica. Thus, the amount of physisorbed silanes in silane-coupling-agent-treated silica particles was successfully estimated from the TG measurements. V C 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43256.

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Observation of silane coupling agents adsorbed on silica by solid state 1H NMR under fast magic angle spinning

Cited by 8 publications

References 22 publications

Characterization of the Mobility and Reactivity of Water Molecules on TiO₂ Nanoparticles by ¹H Solid-State Nuclear Magnetic Resonance

Characterization of the Mobility and Reactivity of Water Molecules on TiO₂ Nanoparticles by ¹H Solid-State Nuclear Magnetic Resonance

Tensile properties of styrene-butadiene rubber/silica composites with mercapto functional silane coupling agents: influences of loading method and alkoxy group number

Quantitative measurement of physisorbed silane on a silica particle surface treated with silane coupling agents by thermogravimetric analysis

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Observation of silane coupling agents adsorbed on silica by solid state 1H NMR under fast magic angle spinning

Cited by 8 publications

References 22 publications

Characterization of the Mobility and Reactivity of Water Molecules on TiO2 Nanoparticles by 1H Solid-State Nuclear Magnetic Resonance

Characterization of the Mobility and Reactivity of Water Molecules on TiO2 Nanoparticles by 1H Solid-State Nuclear Magnetic Resonance

Tensile properties of styrene-butadiene rubber/silica composites with mercapto functional silane coupling agents: influences of loading method and alkoxy group number

Quantitative measurement of physisorbed silane on a silica particle surface treated with silane coupling agents by thermogravimetric analysis

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Characterization of the Mobility and Reactivity of Water Molecules on TiO₂ Nanoparticles by ¹H Solid-State Nuclear Magnetic Resonance

Characterization of the Mobility and Reactivity of Water Molecules on TiO₂ Nanoparticles by ¹H Solid-State Nuclear Magnetic Resonance