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9 results on '"Florence Mercier-Bion"'

1. X‐ray photoelectron spectroscopy characterization of Cu compounds for the development of organic protection treatments dedicated to heritage Cu objects preservation

Author

Muriel Bouttemy, Arnaud Etcheberry, Florence Mercier-Bion, Emilande Apchain, Philippe Dillmann, Maëva L’héronde, Delphine Neff, Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Lavoisier de Versailles (ILV), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut photonique d'analyse non-destructive européen des matériaux anciens (IPANEMA), Muséum national d'Histoire naturelle (MNHN)-Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Centre National de la Recherche Scientifique (CNRS)-Ministère de la Culture (MC), IRAMAT - Laboratoire Métallurgies et Cultures (IRAMAT - LMC), Institut de Recherches sur les Archéomatériaux (IRAMAT), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne-Centre National de la Recherche Scientifique (CNRS), Fondation des Sciences du Patrimoine, Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Rayonnement Matière de Saclay (IRAMIS), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)

Subjects
010302 applied physics, Cuprite, Materials science, [CHIM.MATE]Chemical Sciences/Material chemistry, 02 engineering and technology, Surfaces and Interfaces, General Chemistry, engineering.material, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 01 natural sciences, Surfaces, Coatings and Films, Characterization (materials science), X-ray photoelectron spectroscopy, 13. Climate action, visual_art, 0103 physical sciences, Materials Chemistry, engineering, visual_art.visual_art_medium, Brochantite, 0210 nano-technology, Nuclear chemistry
Abstract

International audience; The preservation of bronze and copper heritage objects is challenging. Exposure to water or pollution in outdoor conditions leads to corrosion phenomena, which can highly degrade the objects or structures. We aim to develop an alternative nontoxic corrosion inhibiting treatment, based on the use of a carboxylate (HC10) treatment. Electron spectroscopies (X‐ray photoelectron spectroscopy and scanning Auger microscopy) are used to determine, from micrometric to nanometric scale, the composition and chemical environments (oxidation degrees) of the copper compounds commonly found in the corrosion product layer. In the present study, we focus on the evaluation of X‐ray beam irradiation damage when performing surface analysis on cuprite, brochantite, and Cu decanoate reference samples. The reduction phenomenon has already been reported, especially for Cu(II) compounds, but not clearly explained. Different behavior has been observed depending on the X‐ray source used, and the nature and hydration level of the compounds. The photoreduction issue is critical, as it guarantees the reliability of the chemical information obtained and sheds light on the best analysis pathway to adopt when multitechnique analyses are implemented. An analytical procedure is employed to track the reduction of Cu(II) reference samples during XPS analysis evidencing practically instantaneous modifications of the spectra and thus, the instability of these phases except for the dehydrated cuprite sample.

Published
2020
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2. Biocorrosion detection by sulphur isotopic fractionation measurements

Author

Laurent Urios, S. Mostefaoui, Florence Mercier-Bion, Delphine Neff, Yannick Linard, Didier Crusset, Philippe Dillmann, Sophie Grousset, Valérie Deydier, Alexandre Dauzères, Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Institut de Recherches sur les Archéomatériaux (IRAMAT), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM), Agence Nationale pour la Gestion des Déchets Radioactifs (ANDRA), PSE-ENV/SEDRE/LETIS, Institut de Radioprotection et de Sûreté Nucléaire (IRSN), Institut des sciences analytiques et de physico-chimie pour l'environnement et les materiaux (IPREM), Université de Pau et des Pays de l'Adour (UPPA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de minéralogie, de physique des matériaux et de cosmochimie (IMPMC), Muséum national d'Histoire naturelle (MNHN)-Institut de recherche pour le développement [IRD] : UR206-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), IRAMAT - Laboratoire Métallurgies et Cultures (IRAMAT - LMC), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM), PLATIN' (PLATeau d'Isotopie de Normandie, France) core facility and MNHN (Museum, National d’Histoire Naturelle, Paris, France) for the sulphur isotopic analysis., Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'étude et de recherche sur les transferts et les interactions dans les sous-sols (IRSN/PSE-ENV/SEDRE/LETIS), Service des déchets radioactifs et des transferts dans la géosphère (IRSN/PSE-ENV/SEDRE), Institut de Radioprotection et de Sûreté Nucléaire (IRSN)-Institut de Radioprotection et de Sûreté Nucléaire (IRSN), and Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Abiotic component, Materials science, Micron size, 020209 energy, General Chemical Engineering, Metallurgy, Radioactive waste, chemistry.chemical_element, 02 engineering and technology, General Chemistry, Fractionation, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Sulfur, Corrosion, chemistry, iron sulphide, microbiological corrosion, 0202 electrical engineering, electronic engineering, information engineering, NanoSIMS, General Materials Science, 0210 nano-technology, sulphur isotopic fractionation
Abstract

International audience; This innovative study presents a local diagnosis approach based on nanoSIMS technique to determine the biotic/abiotic origin of iron sulphides of (sub)micron size heterogeneously located in the corrosion product layers of iron. For iron coupons corroded in controlled conditions, negative δ34Ssulphides-sulphates were obtained in biotic conditions contrary to δ34Ssulphides-sulphates obtained in abiotic ones. These results underline that nanoSIMS is a reliable local technique to detect the formation origin of (sub)micron iron sulphides. This successful methodology was then applied to a complex system representative of an iron corroded in the conditions similar to those of radioactive wastes storage in geological medium.

Published
2020
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3. Electrical properties of iron corrosion layers formed in anoxic environments at the nanometer scale

Author

Delphine Neff, Florence Mercier-Bion, Hélène Lotz, Ludovic Tortech, Jiaying Li, Philippe Dillmann, Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), IRAMAT - Laboratoire Métallurgies et Cultures (IRAMAT - LMC), Institut de Recherches sur les Archéomatériaux (IRAMAT), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM), Laboratoire Innovation en Chimie des Surfaces et NanoSciences (LICSEN), Edifices PolyMétalliques (E-POM), Institut Parisien de Chimie Moléculaire (IPCM), Institut de Chimie du CNRS (INC)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Centre National de la Recherche Scientifique (CNRS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Innovation en Chimie des Surfaces et NanoSciences (LICSEN UMR 3685), and Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, General Chemical Engineering, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Corrosion, Metal, chemistry.chemical_compound, Iron corrosion, General Materials Science, FESEM, Electrical conductor, Magnetite, C-AFM, [CHIM.MATE]Chemical Sciences/Material chemistry, General Chemistry, Conductive atomic force microscopy, 021001 nanoscience & nanotechnology, Anoxic waters, 0104 chemical sciences, chemistry, Chemical engineering, visual_art, Electrical properties, visual_art.visual_art_medium, Archaeological artefact, Carbonate, Nanometre, µRaman, 0210 nano-technology
Abstract

International audience; The electrical properties of the corrosion layers on archaeological iron artefacts were determined by Conductive Atomic Force Microscopy. Different corrosion products were studied: Fe$^{II}$ carbonates, magnetite entrapped in the carbonate, and iron sulfides. The results indicate that the ferrous carbonate matrix is insulating, and that magnetite and iron sulfides have a conductive character, although these phases are not systematically connected to the metal. This suggests that electrons produced by the anodic dissolution of metal would be conducted to the external part of the corrosion product layer through a three-dimensional network of connected magnetite strips passing through the ferrous carbonate matrix.

Published
2018
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4. Multiscale Study of Interactions Between Corrosion Products Layer Formed on Heritage Cu Objects and Organic Protection Treatments

Author

Delphine Neff, Arnaud Etcheberry, Maëva L’héronde, Florence Mercier-Bion, Muriel Bouttemy, Philippe Dillmann, Emilande Apchain, Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Recherches sur les Archéomatériaux (IRAMAT), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne-Centre National de la Recherche Scientifique (CNRS), Institut Lavoisier de Versailles (ILV), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IRAMAT - Laboratoire Métallurgies et Cultures (IRAMAT - LMC), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne-Centre National de la Recherche Scientifique (CNRS), Fondation des Sciences du Patrimoine, Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS), and Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Archeology, Cuprite, corrosion inhibitor, Materials science, 020209 energy, Materials Science (miscellaneous), chemistry.chemical_element, 02 engineering and technology, Conservation, engineering.material, Corrosion, Metal, Corrosion inhibitor, chemistry.chemical_compound, 0202 electrical engineering, electronic engineering, information engineering, Brochantite, lcsh:CC1-960, Penetration depth, carboxylate treatment, corrosion, [CHIM.MATE]Chemical Sciences/Material chemistry, cultural heritage, 021001 nanoscience & nanotechnology, Copper, 6. Clean water, Auger spectroscopy, chemistry, Chemical engineering, visual_art, copper, visual_art.visual_art_medium, engineering, lcsh:Archaeology, Nanometre, 0210 nano-technology
Abstract

In the framework of the protection of copper objects exposed to atmospheric corrosion, different solutions are envisaged, among them carboxylate treatments (HC10). In this study, an analytical approach based on complementary techniques from micrometer to nanometer scale (&mu, RS, SEM-EDS, SAM) is used to describe the properties of the corrosion products layer (CPL) and determine the penetration depth of the HC10 protection treatment inside the CPL of copper samples issued from the roof of the Saint Martin church in Metz. The CPL consists in a thick brochantite layer (20 to 50 &mu, m), mainly composed of Cu4SO4(OH)6, on top of a thinner (1 to 5 &mu, m thick) cuprite layer, Cu2O, acting as a natural corrosion barrier on the metal. Application of the organic treatment is implemented by immersing the corroded samples in HC10 solution, consistent with future requirements for large scale applications. Even for short-term duration (one minute), the HC10 treatment penetrates to the cuprite/brochantite interface, but Cu(C10)2 precipitate is only detected locally, whereas for a longer immersion of thirty minutes, it is present in higher proportions in the whole brochantite layer, filling the pores, up to the cuprite/brochantite interface. Cu(C10)2 acts as a second inner barrier and prevents liquid infiltration.

Published
2019
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5. Multitechnique investigation of sulfur phases in the corrosion product layers of iron corroded in long-term anoxic conditions: From micrometer to nanometer scale

Author

Florence Mercier-Bion, Arnaud Etcheberry, Delphine Neff, Sophie Grousset, Philippe Dillmann, Muriel Bouttemy, Institut Lavoisier de Versailles (ILV), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Radioprotection et de Sûreté Nucléaire (IRSN), Agence Nationale pour la Gestion des Déchets Radioactifs (ANDRA), IRAMAT - Laboratoire Métallurgies et Cultures (IRAMAT - LMC), Institut de Recherches sur les Archéomatériaux (IRAMAT), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS), IRSN, ANDRA, Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), and Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM)

Subjects
Greigite, Materials science, Sulfide, chemistry.chemical_element, Iron sulfide, 02 engineering and technology, engineering.material, 010402 general chemistry, 01 natural sciences, Corrosion, Ferrous, chemistry.chemical_compound, Mackinawite, Materials Chemistry, chemistry.chemical_classification, Metallurgy, Surfaces and Interfaces, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Sulfur, 0104 chemical sciences, Surfaces, Coatings and Films, chemistry, 13. Climate action, engineering, Pyrite, 0210 nano-technology
Abstract

The study of anoxic corrosion process of ferrous metals is a matter of concern for industrial sector (pipelines, container for nuclear waste storage….) but also for cultural heritage objects conservation. Indeed, the formation and the presence of sulfide compounds in the corrosion products of buried objects, either in terrestrial or marine environments, can drastically change the corrosion mechanisms and, so, the conservation strategies for these objects. Particularly, in natural environment, the presence of microorganisms such as Sulfate-Reducing Bacteria (SRB) may influence the corrosion rate of ferrous objects by favoring the precipitation of iron sulfide phases and modifying then the initial corrosion process [1]. The determination of the iron sulfides nature and their distribution in the corrosion product layer is a crucial issue to address in order to anticipate the degradation of ferrous object during extraction, storage or conservation operations. In the present work, archeological ferrous samples, representative of long term corrosion systems, with or without bacteria exposition, have been considered. A multi-technique approach was developed to achieve an overall physico-chemical characterization and to cover the dimensions requirement of the corrosion systems. First, FE-SEM imaging coupled with EDS and µ-Raman spectroscopy were performed on the archeological ferrous samples enabling the localization and identification of the natural corrosion products. Mix of phases of greigite (Fe 3 S 4) and mackinawite (FeS) in a corrosion layer mainly constituted of iron carbonates were observed at a sub-micrometric scale, in consistency with the literature [2], showing the precipitation of greigite, mackinawite and/or pyrite (FeS 2) in the presence of bacteria or in sulfur environment. Then, Nano-Auger spectroscopy, owing to its local chemical characterization capability, was investigated to obtain a chemical diagnostic at a nanometric scale. Scanning Auger Microscopy (SAM) was performed to evaluate the ability of this technique to spatially discriminate different phases (iron sulfides, oxides and carbonates) at a local scale and extreme surface sensitivity (5nm escape depth). Then, thanks to µ-Raman mappings, specific areas presenting only one component were selected and identified for the acquisition of reference Auger spectra, and especially high energy resolution spectra of Fe-MVV and S-LVV regions. Finally, the spatial distribution of the different phases obtained with SAM could be compared with nano-SIMS experiments informing about the sulfur isotopic composition variations and the bio-origin of the sulfur phases.

Published
2018
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6. Characterisation and determination of the bio-origin of iron sulphides in anoxic corrosion systems thanks to isotopic analyses by nanoSIMS

Author

Florence Mercier-Bion, Valérie Deydier, Alexandre Dauzères, Didier Crusset, Philippe Dillmann, Yannick Linard, Camille Chautard, Delphine Neff, Sophie Grousset, S. Mostefaoui, Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Agence Nationale pour la Gestion des Déchets Radioactifs (ANDRA), PSE-ENV/SEDRE/LETIS, Institut de Radioprotection et de Sûreté Nucléaire (IRSN), Institut de minéralogie, de physique des matériaux et de cosmochimie (IMPMC), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de recherche pour le développement [IRD] : UR206-Muséum national d'Histoire naturelle (MNHN)-Centre National de la Recherche Scientifique (CNRS), PRP-DGE/SEDRAN/BERIS, IRAMAT - Laboratoire Métallurgies et Cultures (IRAMAT - LMC), Institut de Recherches sur les Archéomatériaux (IRAMAT), and Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne-Centre National de la Recherche Scientifique (CNRS)

Subjects
Anoxic corrosion, Sulphur isotopic fractionation, Bacteria, 020209 energy, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 13. Climate action, Iron sulphide, 0202 electrical engineering, electronic engineering, information engineering, NanoSIMS, [CHIM]Chemical Sciences, General Materials Science, 0210 nano-technology
Abstract

International audience; Characterisation and determination of the bio-origin of iron sulphides in anoxiccorrosion systems thanks to isotopic analyses by nanoSIMS. This study is devoted to the determinationof the bacterial or inorganic origin of iron sulphides formed during anoxic corrosion processesby sulfur isotopic composition analyses. Broadly, these analyses are realized by IRMS on dissolved sulphidesand sulphates. Yet in this study, surface local isotopic analyses are realized by nanoSIMS in orderto preserve the information about the corrosion products’ localization. Two kinds of samples are studied:a sample (CBCC) corroded during 13 months in controlled laboratory conditions; and one archeologicalsample corroded during about 2000 years in not very well known conditions. When the corrosion system isperfectly well known, as for the CBCC sample, the local isotopic analyses by nanoSIMS actually enable toconclude on the (bio-)origin of the iron sulphides observed. However, when the isotopic composition of thesulphate’s source is unknown, as for the archeological sample, the origin of iron sulphides cannot alwaysbe determined.; Cette étude est consacrée à la détermination de l'origine biotique ou abiotique de sulfures de fer formés au cours de processus de corrosion anoxiques par l'analyse de la composition isotopique du soufre. Usuellement ces analyses sont réalisées par IRMS (Isotopic Ratio Mass Spectrometry) sur des sulfures et des sulfates préalablement dissous. Dans cette étude, en revanche, une nouvelle approche est utilisée, basée sur des analyses isotopiques locales de surface réalisées en nanoSIMS afin de conserver l'information sur la localisation des produits de corrosion. Deux types d'échantillons ont été étudiés : un échantillon (CBCC) corrodé pendant 13 mois en conditions contrôlées, et un échantillon archéologique corrodé pendant environ 2000 ans dans des conditions mal connues. Lorsque le système de corrosion est parfaitement connu, tel que le cas de l'échantillon CBCC, l'analyse isotopique locale par nanoSIMS permet effectivement de conclure sur la (bio-)origine des liserés de sulfures de fer formés. En revanche, lorsque la composition isotopique de la source de sulfates est inconnue, comme dans le cas de l'échantillon archéologique, il n'est pas toujours possible de conclure sur l'origine des sulfures de fer observés.

Published
2017
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7. Capillary zone electrophoresis for U(VI) and short chain carboxylic acid sorption studies on silica and rutile

Author

Yujia Zhao, Vladimir Sladkov, Florence Mercier-Bion, Institut de Physique Nucléaire d'Orsay (IPNO), and Université Paris-Sud - Paris 11 (UP11)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Carboxylic acid, Inorganic chemistry, Carboxylic Acids, 02 engineering and technology, 01 natural sciences, Oxalate, Absorption, Analytical Chemistry, chemistry.chemical_compound, Capillary electrophoresis, Formate, Titanium, chemistry.chemical_classification, Aqueous solution, 010401 analytical chemistry, Electrophoresis, Capillary, Sorption, Silicon Dioxide, 021001 nanoscience & nanotechnology, Uranyl, 6. Clean water, 0104 chemical sciences, chemistry, Ionic strength, Uranium, [PHYS.PHYS.PHYS-CHEM-PH]Physics [physics]/Physics [physics]/Chemical Physics [physics.chem-ph], 0210 nano-technology
Abstract

Capillary zone electrophoresis was used to study the uranyl and short chain carboxylic acid sorption on silica and rutile. The separation and the simultaneous determination (in a single run) of a number of short chain carboxylic acids (oxalic, formic, acetic and propionic) and U(VI) with direct UV detection is developed for the analysis of solutions after the sorption experiments. The reverse polarity mode is used (the injection is performed at the negative end). The matrix effect of Si(IV) (possible silica dissolution product) and perchlorate (added for constant ionic strength in sorption experiments) on the separation of U(VI) and organic acids is investigated. The influence of methanol addition in carrier electrolyte on the separation selectivity of given analytes is also studied. Under the chosen conditions (carbonate buffer (ionic strength of 0.1 M), pH 9.8, 0.15 mM of tetradecyltrimethylammonium bromide, 25% (v/v) of methanol) the calibration curves are plotted. They are linear in two ranges of concentration from not, vert, similar1 × 10−5 to not, vert, similar1 × 10−3 M for oxalate, acetate, propionate, U(VI) and not, vert, similar1 × 10−4 to not, vert, similar1 × 10−3 for formate. The accuracy of the procedure is checked by the “added-found” method in simulation solutions. The relative standard deviations of the concentrations found are within the range of 1–10% and the recovery is in the range of 90–115%. This method is applied for the analysis of aqueous samples issued from sorption experiments on silica and rutile. The obtained results indicate that the given organic acids decrease uranium sorption both on silica and rutile. These experiments demonstrate that short chain carboxylic acids can influence the mobility and the chemistry of U(VI) in the environment.

Published
2011
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8. Temperature effects on the interaction mechanisms between U(VI) and Eu(III) and ZrP2O7: experiment and modelling

Author

Florence Mercier-Bion, H. Catalette, G. Lagarde, Romuald Drot, N. Finck, Eric Simoni, Institut de Physique Nucléaire d'Orsay (IPNO), and Centre National de la Recherche Scientifique (CNRS)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université Paris-Sud - Paris 11 (UP11)

Subjects
Zirconium diphosphate, Speciation, Inorganic chemistry, TRLFS, chemistry.chemical_element, 02 engineering and technology, 010501 environmental sciences, 01 natural sciences, Modelling, Ion, Chemical kinetics, chemistry.chemical_compound, Europium, Surface complexation, Mass transfer, Physical and Theoretical Chemistry, 0105 earth and related environmental sciences, Zirconium, Temperature, Substrate (chemistry), Sorption, 021001 nanoscience & nanotechnology, Uranyl, chemistry, Uranium, [PHYS.PHYS.PHYS-CHEM-PH]Physics [physics]/Physics [physics]/Chemical Physics [physics.chem-ph], 0210 nano-technology
Abstract

In the field of nuclear waste management, prediction of the radionuclides migration through the geosphere has to take into account the effects of temperature. The chosen substrate, zirconium diphosphate, was previously described concerning its surface acidity properties for several temperatures (25 °C, 50 °C, 75 °C, 90 °C). Edges for uranyl sorption were obtained in NaClO4medium, and the europium(III) sorption edges were realized in KNO3medium to evaluate the influence of the complexing nitrate ions. Influence of the temperature, the nature of the cation and the nature of the substrate were pointed out by comparing the edges for the different systems. A structural investigation (TRLFS) was carried out to define experimentally, at the microscopic level, the sorption equilibria. Only UO22+and Eu3+were sorbed on both ZrP2O7surface sites (≡Zr–O and ≡P–O), the nitrate medium having no influence on the sorbed species. Furthermore, temperature did not change the sorption mechanisms. The surface complexation modelling of both investigated systems was realized using i) the constant capacitance model ii) the results of the substrate characterizations iii) uranyl sorbed complex determinations. The formation of bidentate surface complexes onto the ≡Zr–O site is not accompanied by a proton release, whereas the formation of bidentate surface complexes onto the ≡P–O site is followed by a release of 2 protons, for both cations and at all temperatures studied. The determined sorption constants increase with temperature, as was expected from the analysis of the sorption edge positions.

Published
2008
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9. Comparison between batch and column experiments to determine the surface charge properties of rutile TiO2 powder

Author

Catherine Sirguey, Michel Sardin, Lenka Svecova, Marie-Odile Simonnot, Manuel Dossot, Sébastien Cremel, Florence Mercier-Bion, Institut de Physique Nucléaire d'Orsay (IPNO), and Centre National de la Recherche Scientifique (CNRS)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université Paris-Sud - Paris 11 (UP11)

Subjects
Analytical chemistry, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Biomaterials, Colloid and Surface Chemistry, Specific surface area, Electrophoretic mobility, Zeta potential, TiO2, Surface charge, Nonlinear chromatography, Aqueous solution, Chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, Electrophoresis, Rutile, Ionic strength, Particle, 0210 nano-technology, [CHIM.RADIO]Chemical Sciences/Radiochemistry
Abstract

This paper reports a comparative study of three methods for determining the surface charge and acid–base behavior of a TiO2 rutile material. Electrophoretic mobility measurements were performed using two different batch protocols: (i) a “static” mode that consisted of immersing the rutile powder in aqueous solutions of given pH's and ionic strengths for 10 h, and (ii) a “dynamic” mode that consisted of using an automatic titrator to continuously adjust the solution pH with a contact time of 15 min. The same apparatus (a Nanosizer from Malvern) was used to measure the zeta potential of the particles in both methods. These batch experiments were next compared to the determination of the surface charge of rutile using nonlinear chromatography in column experiments. In that case, the rutile powder was compacted to enable the formation of a proper column bed. Therefore, Raman scattering and X-ray photoelectron spectra were used, as well as other physical information such as specific surface area and morphology of the particles, to verify that the rutile powder and compacted form were identical. The three approaches were then compared and discussed in relation to the acid–base behavior of the rutile material.

Published
2008
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