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2015

Articles:

Escande, Vincent, Petit, Eddy, Garoux, Laetitia, Boulanger, Clotilde and Grison, Claude
ACS Sustainable Chemistry & Engineering,
2015

Resume: A novel Mn-derived catalyst was prepared starting from biomass of Mn-hyperaccumulating plants growing on metal-rich soils. Recovery of this biomass as value-added ?ecocatalysts? provides incentives for the development of phytoextraction programs on soils degraded by mining activities. Characterization of the resulting plant-based ?Eco-Mn?? catalyst by inductively coupled plasma mass spectrometry (ICP-MS), X-ray diffraction (XRD), X-ray fluorescence spectrometry (XRF) and X-ray photoelectron spectroscopy (XPS) demonstrated the presence of unusual polymetallic complexes of Mn(II) in the catalyst, along with Fe(III). Incorporation of these species into montmorillonite K10 as solid support provided a supported Eco-Mn? catalyst, whose properties were investigated for alkene epoxidation with H2O2 (30 wt%)/NaHCO3 (0.2 M) as a green terminal oxidizing reagent. The supported Eco-Mn? catalyst demonstrated a high efficiency for styrene epoxidation, with only 0.31 mol% of Mn, a much lower content of Mn than in previously described Mn-derived heterogeneous catalysts. Whereas Fe was also present in the supported Eco-Mn? catalyst, comparison experiments showed that Fe had only a limited role in the catalysis. The water content in the reaction medium had a beneficial effect, increasing the reaction efficiency. The supported Eco-Mn? catalyst was recycled four times without any loss of activity. Comparison of its properties to those of heterogeneous catalysts made by incorporation of commercial MnCl2.4H2O and FeCl3.6H2O highlighted the superior catalytic activity of polymetallic species present in the biosourced catalyst. The substrate scope of the method was extended to various alkenes, including bulky natural products, which were epoxidized with high yields (up to 99%), sometimes much higher than those obtained with already described Mn-derived heterogeneous catalysts. Finally, by simple adjustments of reaction conditions, the method allowed controlled access to aldehydes by oxidative cleavage of various styrene-derived substrates (up to 93% yield). The method thus constitutes a valuable alternative not only to classical epoxidation reagents, but also to oxidative cleavage of styrene-derived molecules, which usually involves toxic and hazardous reagents.

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Li, Shen, Chaput, Laurent, Stein, Nicolas, Frantz, Cedric, Lacroix, David and Termentzidis, Konstantinos
Applied Physics Letters, 106(23):233108
2015

Mots clefs: molecular dynamics method phonons thermal conductivity bismuth compounds nanowires

Equipe: Département CP2S : Chimie et électrochimie des matériaux

2014

Articles:

ZHOU, T., COLIN, M., CANDOLFI, C., Boulanger, C., DAUSCHER, A., Santava, E., HEJTMANEK, J., BARANEK, P., AL RAHAL AL ORABI, R., POTEL, M., Fontaine, B., GOUGEON, P., Gautier, R. and LENOIR, B.
Chemistry of Materials, 26(16):4765-4775
2014

Resume: We present a detailed study of the evolution of the electrical, galvanomagnetic, and thermodynamic properties of polycrystalline AgxMo9Se11 compounds for 3.4 ? x ? 3.8 at low temperatures (2?350 K). In agreement with density functional theory calculations, the collected data show an overall gradual variation in the transport properties from metallic to semiconducting behavior on going from x = 3.4 to 3.8. The results evidence subtle variations in the electronic properties with the Ag content, typified by both positive and negative phonon-drag effects together with thermopower and Hall coefficient of opposite signs. Analysis of the data suggests that these features may be due to peculiarities of the dispersion of the valence bands in the vicinity of the chemical potential. A drastic influence of the Ag content on the thermal transport was evidenced by a pronounced change in the temperature dependence of the specific heat below 10 K. Nonlinearities in the Cp(T3) data are correlated to the concentration of Ag atoms, with an increase in x resulting in a more pronounced departure from a Debye law. The observed behavior mirrors that of ionic conductors, suggesting that AgxMo9Se11 for x ? 3.6 might belong to this class of compounds.

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Broch, Laurent, Stein, Nicolas, Zimmer, Alexandre, Battie, Yann and Naciri, Aotmane En
Thin Solid Films, 571, Part 3(0):509-512
2014

Mots clefs: Systematic errors In-situ ellipsometry Electrodeposition Bismuth telluride

Resume: Abstract We describe a spectroscopic ellipsometer in the visible domain (400–800 nm) based on a rotating compensator technology using two detectors. The classical analyzer is replaced by a fixed Rochon birefringent beamsplitter which splits the incidence light wave into two perpendicularly polarized waves, one oriented at + 45° and the other one at ? 45° according to the plane of incidence. Both emergent optical signals are analyzed by two identical CCD detectors which are synchronized by an optical encoder fixed on the shaft of the step-by-step motor of the compensator. The final spectrum is the result of the two averaged ? and ? spectra acquired by both detectors. We show that ? and ? spectra are acquired without systematic errors on a spectral range fixed from 400 to 800 nm. The acquisition time can be adjusted down to 25 ms. The setup was validated by monitoring the first steps of bismuth telluride film electrocrystallization. The results exhibit that induced experimental growth parameters, such as film thickness and volumic fraction of deposited material can be extracted with a better trueness.

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Escande, Vincent, Garoux, Laetitia, Grison, Claire, Thillier, Yann, Debart, Francoise, Vasseur, Jean-Jacques, Boulanger, Clothilde and Grison, Claude
Applied Catalysis., B, 146:279-288
2014

Resume: Metallophyte plants derived from phytoextn. are used as starting materials to prep. novel polymetallic catalysts. Polymetallic catalyst activity is used in many Lewis acid catalyzed reactions according to the polymetallic catalyst prepn. The synergetic catalysis of these systems leads to efficient syntheses of complex biomols. such as dihydropyrimidinone, 5'-capped DNA and RNA, and glycosyl aminoacid. These new polymetallic catalysts also bring new possibilities in Green Catalysis, that we named "Ecol. Catalysis". [on SciFinder(R)]

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Szymczak, Jonathan, Legeai, Sophie, Michel, Stéphanie, Diliberto, Sébastien, Stein, Nicolas and Boulanger, Clotilde
Electrochimica Acta, 137(0):586-594
2014

Mots clefs: Bismuth telluride Ionic liquid Electrodeposition Thermoelectricity

Resume: Abstract In this paper, we report the electrodeposition of stoichiometric Bi2Te3 compound using an ionic liquid binary mixture: 1-ethyl-1-octyl-piperidinium bis(trifluoromethylsulfonyl)imide: 1-ethyl-1-octyl-piperidinium bromide (EOPipTFSI:EOPipBr 95:5 (mol%)). The use of this mixture allows to reach a higher solubility of Bi(III) and Te(IV) precursors compared to pure EOPipTFSI ionic liquid in which Te(IV) salts are not soluble. Moreover, this electrolyte presents an extended cathodic stability, allowing the study of electrochemical processes that occur at high cathodic potential values. A detailed voltammetric study of electrochemical systems was performed for electrolytes containing different [Bi(III)]/[Te(IV)] ratio, allowing the attribution of cathodic signals to electrochemical processes. Experimental conditions leading to the deposition of stoichiometric Bi2Te3 were then determined by varying deposition potential and electrolyte composition, using potentiostatic experiments followed by XRD and SEM-EDX analysis. By varying the concentration of precursors in the electrolyte, mirror-like coatings, adherent and homogeneous, were obtained. Electroplated Bi2Te3 presents n-type conductivity with a Seebeck coefficient equal to ?70 ?V K?1 and an electrical resistivity of 133 ?? m.

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Schoenleber, J., Stein, N. and Boulanger, C.
Journal of Electroanalytical Chemistry, 724(0):111-117
2014

Mots clefs: Coefficient Diffusion Electrodeposition Films Sand Thermoelectric

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Guyot, E., Boulanger, C. and Lecuire, J.M.
Chemical Engineering Transactions, vol 41:67-71
2014

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Samih, Y., Marcos, G., Stein, N., Allain, N., Fleury, E., Dong, C. and Grosdidier, T.
Surface and Coatings Technology,
2014

Mots clefs: High Current Pulsed Electron Beam Treatment (HCPEB) Surface hardening Corrosion Phase selection Phase transformation Martensitic steel

Resume: Abstract The surface of the AISI 420 martensitic stainless steel was subjected to High Current Pulsed Electron Beam (HCPEB) treatment. The microstructure in the melted layer consisted of a three phase mixture: (i) fine ?-Fe grains formed via epitaxial growth from the substrate, (ii) larger ?–grains nucleated from the top surface of the melt and (iii) some needles-like variants issued from the solid state martenitic transformation. Despite this complex multi-phase microstructure, the corrosion performance, tested in a sulfuric acid solution, was significantly enhanced by the HCPEB treatment. The increase in corrosion potential and delayed pitting are essentially attributed to an increase in Cr content, rising from 13.3 wt. % in the bulk to about 14 wt. % at the surface, together with a very limited amount of surface craters. This low density of craters did not give rise to significant deep hardening in the sub-surface but the top surface melted layer hardness was increased by more than 50% because of the triggering of the martensitic transformation.

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Maas, M., Diliberto, S., de Vaulx, C., Azzouz, K. and Boulanger, C.
Journal Electronic Materials, 43(10):3857-3862
2014

Mots clefs: Bismuth telluride thick films soluble anode thermoelectric

Equipe: Département CP2S : Chimie et électrochimie des matériaux

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