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References

2016

Articles:

Turgis, R., Arrachart, G., Dubois, V., Dourdain, S., Virieux, D., Michel, S., Legeai, S., Lejeune, M., Draye, M. and Pellet-Rostaing, S.
Dalton Transactions, 45(Copyright (C) 2016 American Chemical Society (ACS). All Rights Reserved.):1259-1268
2016

Resume: The extn. of rare earth elements (REEs) from nitric acid soln. with a triphosphine trioxide (TPO) is presented. Performances of such a ligand in ionic liqs. vs. a classical solvent (benzyl ether) are compared. TPO seems to be 10 to 100 times more efficient when it is dissolved in ionic media whatever the concn. of nitric acid involved. Mechanistic investigations reveal that cation exchange classically obsd. in ionic liqs. is not consistent with the exptl. data. Moreover, clear differences in the TPO/Ln complexes between classical and ionic media are highlighted. A stable complex of 1 lanthanide for 3 TPO is formed in an ionic liq. whereas a complex of 1 lanthanide for 6 to 9 TPO is formed in benzyl ether. Back extn. is also studied and good recovery of REEs could be obtained. The TPO/ionic liq. system shows remarkable performances i.e. efficiency and selectivity towards lanthanides in a simulated leaching soln. of a Nd/Fe/B/Dy magnet. [on SciFinder(R)]

Equipe: Département CP2S : Chimie et électrochimie des matériaux

2015

Articles:

Hazotte, Claire, Meux, Eric, Leclerc, Nathalie and Lapicque, Francois
Chemical Engineering and Processing: Process Intensification, 96:83-93
2015

Mots clefs: Electroassisted leaching Electrodeposition Ni–Cd batteries Solid waste Transport rates

Resume: Abstract Combined leaching of solid wastes to electrodeposition can be an attractive technique for their optimal beneficiation. In most investigations in the area, results are given in terms of energy consumption and selectivity, without thorough analysis of the rates of the various processes involved. The present investigation deals with the significance of transport and transfer phenomena involved in relation to reaction processes, in a cell combining electroassisted leaching to electrodeposition in view to designing treatment processes of manufactured wares after their end of life. The case of the so-called black mass of used Ni–Cd batteries has been considered here, for the separate productions of nickel salts and metal cadmium. First, leaching of the various hydroxides contained in the black mass has been studied either upon addition of acid or by electrochemical generation of H+ at the anode. Moreover, transport of the metal cations produced from the anode compartment to the cathode through the cloth acting as the separator has been investigated through a simple description of transport phenomena. Comparison and discussion of the various transport or reaction rates could show that ion transport through the porous separator could represent the rate-determining step.

Equipe: Département CP2S : Chimie et électrochimie des matériaux

Hazotte, Claire, Leclerc, Nathalie, Diliberto, Sébastien, Meux, Eric and Lapicque, Francois
Environmental Technology, 36(6):796-805
2015

Resume: The aim of this paper is the characterization of spent NiCd batteries and the characterization of an industrial Black Mass obtained after crushing spent NiCd batteries and physical separation in a treatment plant. The characterization was first performed with five cylindrical NiCd batteries which were manually dismantled. Their characterization includes mass balance of the components, active powders elemental analysis and phase identification by X-ray powder diffraction. Chemical speciation of the two metals was also investigated. For cadmium, speciation was previously developed on solid synthetic samples. In a spent battery, the active powders correspond to about 43% of the battery weight. The other components are the separator and polymeric pieces (5%), the support plates (25%) and the carbon steel external case (27%). The sequential procedure shows that the nickel in the positive powders from the dismantled Ni?Cd batteries is distributed between Ni0 (39.7%), Ni(OH)2 (58.5%) and NiOOH (1.8%). Cadmium in the negative powder is about 99.9% as the Cd(OH)2 form with 0.1% of metal cadmium. In the industrial Black Mass, the distribution of cadmium is the same, whereas the distribution of nickel is Ni0 (46.9%), Ni(OH)2 (43.2%) and NiOOH (9.9%). This material contains also 1.8% cobalt and approx. 1% iron.

Equipe: Département CP2S : Chimie et électrochimie des matériaux

2014

Articles:

Turgut, C., Sinha, G., Mether, L., Lahtinen, J., Nordlund, K., Belmahi, M. and Philipp, P.
Analytical Chemistry, 86:11217-11225
2014

Equipe: Département CP2S : Expériences et Simulations des Plasmas Réactifs - Interaction plasma-surface et Traitement des Surfaces ESPRITS

Meglali, O., Attaf, N., Bouraiou, A., Bougdira, J. and Aida, M.S.
Journal of Alloys and Compounds, 587:303-307
2014

Equipe: Département CP2S : Expériences et Simulations des Plasmas Réactifs - Interaction plasma-surface et Traitement des Surfaces ESPRITS

Messaoudi, M., S. Aida, M., Attaf, N., Bezzi, T., Bougdira, J. and Medjahdi, G.
Materials Science in Semiconductor Processing, 17:38-42
2014

Equipe: Département CP2S : Expériences et Simulations des Plasmas Réactifs - Interaction plasma-surface et Traitement des Surfaces ESPRITS

Margueron, S., Ropers, S., Genty, F., Bartasyte, A. and Belmonte, T.
Materials Chemistry and Physics, 147:623-628
2014

Equipe: Département CP2S : Expériences et Simulations des Plasmas Réactifs - Interaction plasma-surface et Traitement des Surfaces ESPRITS

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

Martin, J., Leone, P., Nominé, A., Veys-Renaux, D., Henrion, G. and Belmonte, T.
Surface and Coatings Technology, In Press - available on line
2014

Resume: The chemical stability of the electrolyte in Plasma Electrolytic Oxidation (PEO) has been the subject of much systematic investigation. The present study reports on experimental results on the ageing of a usual PEO electrolyte and its effect on the oxidation of the Al2214 aluminium alloy. A solution of potassium hydroxide ([KOH] = 1 g/L) and sodium silicate ([Na2SiO3] = 1.65 g/L) diluted in deionized water was either aged by running a process during 8 h at most or not. Comparison between materials treated in either solution was made next. Cross-checked experimental results from analytical chemistry, plasma diagnostics and materials science clearly evidence the effect of ageing of the electrolyte on the PEO process behaviour. The transition from arc to "soft" regime occurs earlier (from 18 min to 13 min processing time) as the electrolyte gets older. The concomitant decrease in the electrolyte electrical conductivity (from 7.5 mS.cm-1 to 6.8 mS.cm-1) is correlated with changes in the ionic species content in the electrolyte. Fast video-imaging (125 kfr./s) reveals that the micro-discharge characteristics are also sensitive since they become less numerous per area and unit time (from 220.103 cm-2s-1 to 120.103 cm-2s-1), exhibit shorter lifetime and have smaller sizes as the electrolyte ages. SEM observations of the as-grown coatings combined with roughness measures indicate a decrease in coating thickness ( ~ 20 %) and roughness ( ~ 30 %) while species from the electrolyte accumulate in the outer porous layer simultaneously with a gradual enrichment in a-Al2O3 phase in the inner compact layer (from 36 % to 43 %). Finally, within the PEO conditions that were used, it is shown that the ageing phenomenon of the PEO electrolyte starts to influence the process after 2 hours aged.

Equipe: Département CP2S : Expériences et Simulations des Plasmas Réactifs - Interaction plasma-surface et Traitement des Surfaces ESPRITS

Veys-Renaux, D., ROCCA, E., Martin, J. and Henrion, G.
Electrochimica Acta, 124:30-45
2014

Resume: In the framework of the new ecological regulations, micro-arc oxidation (MAO) appears as an alternativeto usual processes in the field of corrosion protection of Mg alloys. In this work, the initial stagesof anodic layer growth in KOH-based electrolytes are studied up to and beyond the initiation of themicro-arc regime.The properties of the first anodized film preceding the occurrence of the dielectric breakdown (corre-sponding to the start of the micro-arc regime) are mainly determined by the incorporation of additives(fluorides or silicates) in the film, as shown by in situ electrochemical measurements. Scanning electronmicroscopy (SEM), X-ray photoelectron spectroscopy (XPS) and micro-Raman spectroscopy reveal boththe change of morphology and chemical state of silicate and fluoride in the anodized layer before andafter the micro-arc regime. In terms of electrochemical behaviour, investigated by stationary methodsand electrochemical impedance spectroscopy (EIS) in reference corrosive water, the anodic film grownin the silicate medium provides the best corrosion resistance thanks to a thick layer containing Mg2SiO4,whose degradation products seal the porosities of the coating.

Equipe: Département CP2S : Expériences et Simulations des Plasmas Réactifs - Interaction plasma-surface et Traitement des Surfaces ESPRITS

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