Analytical Methods for the Characterization of Aryl Layers

Hinrichs, Karsten; Roodenko, Katy; Rappich, Jörg; Chehimi, Mohamed M.; Pinson, Jean

doi:10.1002/9783527650446.ch4

Cited by 16 publications

(19 citation statements)

References 89 publications

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“…The fourth component is centred at 406 eV and is assigned to the positively charged nitrogen atom of the diazonium N^N + -. 48 In Fig. 5b, it is interesting to note the drastic change of the N 1s peak shape.…”

Section: Surface Analysis By Means Of Xpsmentioning

confidence: 88%

Exfoliated clay/polyaniline nanocomposites through tandem diazonium cation exchange reactions and in situ oxidative polymerization of aniline

et al. 2014

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Section: Surface Analysis By Means Of Xpsmentioning

confidence: 88%

Exfoliated clay/polyaniline nanocomposites through tandem diazonium cation exchange reactions and in situ oxidative polymerization of aniline

et al. 2014

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“…After attachment of the aryl groups, one can note small S2p and S2s features (at 164 and 229 eV, respectively) which account for the attachment of benzenethiol groups. It is also to note that at 400 eV there is a noisy peak assigned to N1s, which most probably arises from azo (-N=N-) bonds within the aryl layer 38 . This probably accounts for the formation of The S2p peak component at ~168 eV is most probably due to surface oxidation in the form of -SO 3 resulting from air-exposure 39 and/or to irradiation by X-rays during the surface analysis 40 .…”

Section: Microstructural Observations Were Performed By Transmission Electron Microscopymentioning

confidence: 99%

Bimetallic Cu–Rh Nanoparticles on Diazonium-Modified Carbon Powders for the Electrocatalytic Reduction of Nitrates

Mirzaei

Bastide

Aghajani³

et al. 2019

Langmuir

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4-benzenethiol-functionalized High Surface Area Graphite powder was prepared and decorated with bimetallic Cu 100-x Rh x nanoparticles (NPs) to serve as electrocatalysts for the reduction of nitrates. In the first step, the HSAG powder was grafted with in situ generated diazonium compounds from 4-aminothiophenol (ATP), in acidic medium using NaNO 2 for the diazotization process. The surface composition was tuned using different initial quantities of ATP. The surface XPS-determined S/C atomic ratio was found to increase stepwise with the initial amine quantity. In a second step, the grafted and untreated HSAG powders were decorated with Cu 100-x Rh x NPs by a wet chemical method and the elemental composition of the end composites assessed by EDS-SEM and ICP, whereas TEM and EDS-TEM served to characterize the NPs morphology and their composition at the nanometer scale. In all cases, the NP size was invariably found to be ~1.7 nm but with a size distribution becoming narrower under increasing grafting rate and the global composition enriched in copper. Voltammetry was performed with a cavity microelectrode to evaluate the electrocatalytic performances of the composites for nitrate reduction. Increasing diazonium grafting led to a progressive reduction of the peak current intensity and a shift of the peak potentials towards cathodic values. Maximum intensity was obtained for 0.005 µmol of diazonium salt per mg of HSAG, with a gain of 40 % in comparison to the best untreated sample. This improvement and a change of the voltammogram characteristics after grafting seem to result from modifications of the local composition at the level of NPs that differs from the global composition. This work conclusively shows that diazonium surface modification is important not only to attach electrocatalytic NPs to carbon supports but also to provide narrower size distribution of the electrocatalysts together with finely tuned catalytic properties.

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“…The average values are in line with the literature for PMMA grafts but slightly higher for PHEMA probably due to a slight contribution of DMA as gold is detected by XPS through the PHEMA top layer and thus through also DMA. For UV/ozone cleaned Au plate, the water contact angle was reported to be 35.5° while for aryl layer on various substrates the contact angle is in the 55° to 100° range . Interestingly, for each polymer the use of the crosslinker imparts a slight degree of relative hydrophilicity.…”

Section: Xpsmentioning

confidence: 99%

Diazonium salts for surface-confined visible light radical photopolymerization

Bakas

Yılmaz

Ait-Touchente

et al. 2016

J. Polym. Sci. Part A: Polym. Chem.

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The surface chemistry of aryl diazonium salts has progressed at a remarkable pace in the last two decades, and opened many avenues in materials science. These compounds are excellent coupling agents for polymers to surfaces via several surface‐confined polymerization methods. For the first time, we demonstrate that diazonium salts are efficient for surface initiating radical photopolymerization in the visible light of methyl methacrylate (MMA) and 2‐hydroxyethyl methacrylate (HEMA) taken as model monomers. To do so, 4‐(dimethylamino)benzenediazonium salt was electroreduced on gold plates or flexible ITO sheets to provide 4‐(dimethylamino)phenyl (DMA) hydrogen donor layers; while excited state camphorquinone acted as the free hydrogen abstractor. In the same way, we co‐polymerized HEMA and MMA with ethylene glycol dimethacrylate in order to obtain crosslinked polymer grafts. We demonstrate by XPS that gold was efficiently screened by the polymer layers and that the wettability of the surfaces accounts for the hydrophilic or hydrophobic characters of the tethered polymers. Homo‐ and crosslinked PMMA grafts were found to resist removal by the paint stripper methyl ethyl ketone. The grafted DMA/camphorquinone system operating in the visible light holds great promises in terms of adhesion of in situ designed continuous or patterned polymer coatings on various substrates. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016, 54, 3506–3515

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Analytical Methods for the Characterization of Aryl Layers

Cited by 16 publications

References 89 publications

Exfoliated clay/polyaniline nanocomposites through tandem diazonium cation exchange reactions and in situ oxidative polymerization of aniline

Exfoliated clay/polyaniline nanocomposites through tandem diazonium cation exchange reactions and in situ oxidative polymerization of aniline

Bimetallic Cu–Rh Nanoparticles on Diazonium-Modified Carbon Powders for the Electrocatalytic Reduction of Nitrates

Diazonium salts for surface-confined visible light radical photopolymerization

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