Standard operating procedure (SOP) for the quantitative determination of organic silicon compounds at the surface of elastomeric sealants

Groß, Th.; Treu, Dieter; Unger, Wolfgang

doi:10.1016/s0169-4332(01)00271-9

Cited by 5 publications

(1 citation statement)

References 4 publications

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“…Figure a shows the fitted high-resolution Si 2p core-level spectrum taken on the aminosilane 1 monolayer in the most surface sensitive mode characterized by an information depth of z 95 = 1.2 nm ( h ν = 210 eV, θ = 60°) . Elemental silicon Si 0 at a binding energy of 99.0 eV represents the bulk region and a second peak originating from the native oxide (SiO 2 ) layer thereon occurs at a binding energy of 103.2 eV. ,− In accordance with the measured peak position of 101.7 eV, the third component is assigned to the silane’s central silicon atom R 3 Si(O) 1 that is bound to the surface by a single siloxane bond (Si silane –O–Si wafer ). − ,− The measured chemical shift of −1.5 eV for R 3 Si(O) 1 in relation to the SiO 2 component is in principal agreement with the shift of −2.0 eV obtained from calculated ionization potentials of a benzamidosilane 2 layer on a quartz surface (for more details, see Table S5 and Figure S7, Supporting Information).…”

Section: Resultsmentioning

confidence: 69%

Quantification of Silane Molecules on Oxidized Silicon: Are there Options for a Traceable and Absolute Determination?

et al. 2015

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Organosilanes are used routinely to functionalize various support materials for further modifications. Nevertheless, reliable quantitative information about surface functional group densities after layer formation is rarely available. Here, we present the analysis of thin organic nanolayers made from nitrogen containing silane molecules on naturally oxidized silicon wafers with reference-free total reflection X-ray fluorescence (TXRF) and X-ray photoelectron spectroscopy (XPS). An areic density of 2-4 silane molecules per nm(2) was calculated from the layer's nitrogen mass deposition per area unit obtained by reference-free TXRF. Complementary energy and angle-resolved XPS (ER/AR-XPS) in the Si 2p core-level region was used to analyze the outermost surface region of the organic (silane layer)-inorganic (silicon wafer) interface. Different coexisting silicon species as silicon, native silicon oxide, and silane were identified and quantified. As a result of the presented proof-of-concept, absolute and traceable values for the areic density of silanes containing nitrogen as intrinsic marker are obtained by calibration of the XPS methods with reference-free TXRF. Furthermore, ER/AR-XPS is shown to facilitate the determination of areic densities in (mono)layers made from silanes having no heteroatomic marker other than silicon. After calibration with reference-free TXRF, these areic densities of silane molecules can be determined when using the XPS component intensity of the silane's silicon atom.

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