Effect of Surface Water and Base Catalysis on the Silanization of Silica by (Aminopropyl)alkoxysilanes Studied by X-ray Photoelectron Spectroscopy and 13C Cross-Polarization/Magic Angle Spinning Nuclear Magnetic Resonance

Kallury, Krishna M. R.; Macdonald, Peter M.; Thompson, Michael C.

doi:10.1021/la00014a025

Cited by 216 publications

(183 citation statements)

References 8 publications

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“…The peak consists of two components centered at 399.5 eV and 402.0 eV. In agreement with the literature, the former is attributed to the free amine group (R-NH 2 ) and the latter is attributed to a protonated amino group (R-NH 3 + ) [41,43]. Quantitative analysis of the N1s peak yields that 85.7% of the amine is present in its protonated form and 14.3% as free amine (see Table 3).…”

Section: Aptms-sba-15supporting

confidence: 89%

The mechanism for the controlled synthesis of highly dispersed vanadia supported on silica SBA-15

Heß

Wild

Schlögl

2006

Microporous and Mesoporous Materials

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The mechanism for the controlled synthesis of highly dispersed vanadia supported on mesoporous silica SBA-15 (VO x /SBA-15) is elucidated using X-ray photoelectron spectroscopy (XPS), Raman and diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS). The synthesis consists of functionalization of SBA-15 using 3-aminopropyltrimethoxysilane (APTMS) followed by HCl treatment, anion exchange of decavanadate (V 10 O 28 6-) and calcination to yield the final material. Spectroscopic analysis yields that APTMS is grafted onto the surface via hydroxyl groups. Under ambient conditions, protonated APTMS on SBA-15 is largely hydrolyzed and present in its bidentate and tridentate form. Detailed XPS analysis reveals a strong influence of surface water on the resulting structure of APTMS on SBA-15. Under dry conditions, the protonated APTMS molecules on SBA-15 adopt the monodentate and bidentate form. During the anion exchange reaction, decavanadate is incorporated intactly into the pores, without any changes in the structure of the organic framework. In the calcination step, decavanadate is decomposed and vanadia is anchored onto the surface of SBA-15 via silanol groups resulting in highly dispersed surface vanadia species, while the organic resiues are fully removed from the pores of the silica matrix. d

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Section: Aptms-sba-15supporting

confidence: 89%

The mechanism for the controlled synthesis of highly dispersed vanadia supported on silica SBA-15

Heß

Wild

Schlögl

2006

Microporous and Mesoporous Materials

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“…Improved deposition protocols allow thinner, more regular, APTES interfaces to be made (Moon et al 1996;Han et al 2006), but multilayer formation remains an intrinsic potential of the reagent (Kallury et al 1994). APTES monomers can form infinite, cross-linked siloxane polymer lattices because APTES is a multi(tri)-valent silane.…”

Section: Introductionmentioning

confidence: 99%

Nanoscale adhesion, friction and wear studies of biomolecules on silane polymer-coated silica and alumina-based surfaces

Bhushan

Kwak

Gupta

et al. 2008

J. R. Soc. Interface.

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Proteins on biomicroelectromechanical systems (BioMEMS) confer specific molecular functionalities. In planar FET sensors (field-effect transistors, a class of devices whose protein-sensing capabilities we demonstrated in physiological buffers), interfacial proteins are analyte receptors, determining sensor molecular recognition specificity. Receptors are bound to the FET through a polymeric interface, and gross disruption of interfaces that removes a large percentage of receptors or inactivates large fractions of them diminishes sensor sensitivity. Sensitivity is also determined by the distance between the bound analyte and the semiconductor. Consequently, differential properties of surface polymers are design parameters for FET sensors. We compare thickness, surface roughness, adhesion, friction and wear properties of silane polymer layers bound to oxides (SiO 2 and Al 2 O 3 , as on AlGaN HFETs). We compare those properties of the film-substrate pairs after an additional deposition of biotin and streptavidin. Adhesion between protein and device and interfacial friction properties affect FET reliability because these parameters affect wear resistance of interfaces to abrasive insult in vivo. Adhesion/friction determines the extent of stickage between the interface and tissue and interfacial resistance to mechanical damage. We document systematic, consistent differences in thickness and wear resistance of silane films that can be correlated with film chemistry and deposition procedures, providing guidance for rational interfacial design for planar AlGaN HFET sensors.

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“…Segundo Kallury 26 este sinal é atribuído a um grupo metil (-CH 3 ) ligado ao silício. Para as amostras S5, S6, S7 e S8 observou-se três distintos sinais em 12,1; 23,4 e 43,9 ppm, atribuídos aos três carbonos do grupo propil com origem nos precursores cloropropil e aminopropil.…”

Section: Amostrasunclassified

Influência da catálise ácida e básica na preparação da sílica funcionalizada pelo método sol-gel

Nassar¹,

Messaddeq²,

Ribeiro³

2002

Quím. Nova

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Effect of Surface Water and Base Catalysis on the Silanization of Silica by (Aminopropyl)alkoxysilanes Studied by X-ray Photoelectron Spectroscopy and 13C Cross-Polarization/Magic Angle Spinning Nuclear Magnetic Resonance

Cited by 216 publications

References 8 publications

The mechanism for the controlled synthesis of highly dispersed vanadia supported on silica SBA-15

The mechanism for the controlled synthesis of highly dispersed vanadia supported on silica SBA-15

Nanoscale adhesion, friction and wear studies of biomolecules on silane polymer-coated silica and alumina-based surfaces

Influência da catálise ácida e básica na preparação da sílica funcionalizada pelo método sol-gel

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