Synchrotron-radiation XPS analysis of ultra-thin silane films: Specifying the organic silicon

Dietrich, Paul; Glamsch, Stephan; Ehlert, Christopher; Lippitz, Andreas; Kulak, Nora; Unger, Wolfgang

doi:10.1016/j.apsusc.2015.12.052

Cited by 75 publications

(39 citation statements)

References 28 publications

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“…The core level spectra of C 1 s, 0 1 s, Si 2p and S 2p are reported in Fig. Sa-d These BE values indi cate a main contribution of the Si-0-Si bonds, suggesting a good grade ofreticulation of the coating [9,25,26]. Fig.…”

Section: Zrn (Reference Substrate)mentioning

confidence: 86%

X-ray Photoelectron Spectroscopy as a tool to investigate silane-based coatings for the protection of outdoor bronze: The role of alloying elements

Masi

Balbo

Esvan

et al. 2018

Applied Surface Science

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Application of a protective coating is the most widely used conservation treatment for outdoor\ud bronzes (cast Cu-Sn-Zn-Pb-Sb alloys). However, improving coating protectiveness requires detailed\ud knowledge of the coating/substrate chemical bonding. This is particularly the case for 3-mercapto-propyltrimethoxy-\ud silane (PropS-SH) applied on bronze, exhibiting a good protective behaviour in outdoor\ud simulated conditions. The present work deals with X-Ray Photoelectron Spectroscopy (XPS) and Electron\ud Microscopy (FEG-SEM + FIB (Focused Ion Beam)) characterization of a thin PropS-SH film on bronze.\ud In particular, in order to better understand the influence of alloying elements on coating performance,\ud PropS-SH was studied first on pure Cu and Sn substrates then on bronzes with increasing alloy additions:\ud Cu8Sn as well as a quinary Cu-Sn-Zn-Pb-Sb bronze. Moreover, considering the real application of this\ud coating on historical bronze substrates, previously artificially aged (“patinated”) bronze samples were\ud prepared and a comparison between bare and “patinated” quinary bronzes was performed. In the case\ud of coated quinary bronze, the free surface of samples was analysed by High Resolution Photoelectron\ud Spectroscopy using Synchrotron Radiation (HR-SRPES) at ANTARES (Synchrotron SOLEIL), which offers a\ud higher energy and lateral resolution. By compiling complementary spectroscopic and imaging information,\ud a deeper insight into the interactions between the protective coating and the bronze substrate was\ud achieved

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Section: Zrn (Reference Substrate)mentioning

confidence: 86%

X-ray Photoelectron Spectroscopy as a tool to investigate silane-based coatings for the protection of outdoor bronze: The role of alloying elements

Masi

Balbo

Esvan

et al. 2018

Applied Surface Science

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“…Discrepancies in the binding energies of the same element could be used to distinguish different chemical structures in the compounds. It has been reported that the binding energies of Al–O in boehmite and Al 2 O 3 derived from boehmite, R–Si(O 3 ) in a major Si‐containing compound, –P(O)O–C in epoxy modified by DOPO, and –PO 3 in phosphoric oxyacid created by the decomposition of phosphorus‐containing groups in a polymer were 74.2, 73.8, 102.8, 133.5, and 134.5 eV, respectively . The difference in the binding energies of P2p and Al2p before and after the drop tests shown in Figure (a,b) suggest that the AlOOH−DOPO−GPTS in the epoxy matrix might have decomposed into Al 2 O 3 and phosphoric oxyacid under the impact energy.…”

Section: Resultsmentioning

confidence: 99%

Improvement of the liquid oxygen compatibility of epoxy via the addition of surface‐modified boehmite

Wang

Peng

et al. 2018

J of Applied Polymer Sci

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To improve the liquid oxygen compatibility and cryogenic mechanical properties of epoxy resin, we synthesized and characterized a hybrid compound (functionalized boehmite) containing boehmite, phosphorus, and silicon element. The thermal properties and liquid oxygen compatibility of the composites were investigated in detail. The results show that the addition of functionalized boehmite increased the char residue obviously but had little effect on the thermal decomposition temperature and glass-transition temperature of the composites. The liquid oxygen compatibility of the composites was significantly improved. Composites with 4 wt % boehmite, 0.99 wt % Si, and 1.1 wt % P passed the impact test. Surface element analyses before and after the drop tests suggested that the functionalized boehmite in epoxy might have prevented the impact reaction in liquid oxygen through two steps. First, the compound decomposed into phosphoric oxyacid and Al 2 O 3 under the impact energy and captured the H• and •OH radicals produced from the decomposition of the resin. Then, the decomposition covered the surface, forming a protective layer to isolate the oxygen. The mechanism of the liquid oxygen compatibility of the epoxy composites was subsequently analyzed. In addition, the cryogenic tensile properties of the epoxy composites containing functionalized boehmite showed that the composites had potential applications under cryogenic liquid oxygen environments.

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“…To further probe the nature of fundamental interactions involved in the oscillatory adsorption behaviour observed for PTMS, the number of methoxy groups present on the central silicon atom was reduced from the 3 present in PTMS to 2 in propylmethyldimethoxysilane (PMDMS) and 1 in propyldimethylmethoxysilane (PDMMS). The exploitation of monofunctional silanes to produce a monolayer along with trifunctional silanes to produce multilayer films has been well established in the literature and studied with techniques such as angle‐resolved XPS, ToFSIMS, AFM, and contact angle, and even with angle‐resolved XPS and NEXAFS with a synchrotron radiation source . However, the influence of the number of hydrolysable groups on the self‐assembly mechanism has not been investigated.…”

Section: Introductionmentioning

confidence: 99%

“…The exploitation of monofunctional silanes to produce a monolayer along with trifunctional silanes to produce multilayer films has been well established in the literature and studied with techniques such as angle-resolved XPS, 7 ToFSIMS, AFM, and contact angle, 17 and even with angle-resolved XPS and NEXAFS with a synchrotron radiation source. 18 However, the influence of the number of hydrolysable groups on the self-assembly mechanism has not been investigated. Here, we show the effect of limiting interactions between molecules and thus a reduction in the number of condensation products available.…”

Section: Introductionmentioning

confidence: 99%

The oscillatory adsorption of self‐assembled organosilane films on aluminium oxide surfaces

Sims

Harmer

Quinton

2018

Surface & Interface Analysis

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The time‐dependent oscillatory growth mechanism of organosilane film self‐assembly on aluminium oxide has been investigated using X‐ray photoelectron spectroscopy. While this unusual oscillatory process has been reported for the trifunctional silane, propyltrimethoxysilane, we report here, for the first time, that this oscillatory behaviour is also present during the self‐assembly of the difunctional silane propylmethyldimethoxysilane. The presence of multiple oscillations in this growth mechanism is also first reported for propyltrimethoxysilane and propylmethyldimethoxysilane as a function of exposure time. Multiple oscillations indicate that the 3‐component model that is used to describe and fit a single coverage oscillation must be reconsidered and contain additional components to account for the multiple oscillations seen experimentally. The absence of such oscillatory behaviour in the growth of the monofunctional organosilane propyldimethylmethoxysilane, which in fact follows a Langmuir‐type growth mechanism, indicates that this measurable oscillatory behaviour is because of the ability of multifunctional silanes to oligomerise both on the substrate and in solution.

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Synchrotron-radiation XPS analysis of ultra-thin silane films: Specifying the organic silicon

Cited by 75 publications

References 28 publications

X-ray Photoelectron Spectroscopy as a tool to investigate silane-based coatings for the protection of outdoor bronze: The role of alloying elements

X-ray Photoelectron Spectroscopy as a tool to investigate silane-based coatings for the protection of outdoor bronze: The role of alloying elements

Improvement of the liquid oxygen compatibility of epoxy via the addition of surface‐modified boehmite

The oscillatory adsorption of self‐assembled organosilane films on aluminium oxide surfaces

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