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1. Towards bottom-up nanopatterning of Prussian blue analogues

Author

Virgile Trannoy, Marco Faustini, David Grosso, Sandra Mazerat, François Brisset, Alexandre Dazzi, and Anne Bleuzen

Subjects
nanopatterning, nanoperforated oxide monolayer, Prussian blue analogues, Technology, Chemical technology, TP1-1185, Science, Physics, QC1-999
Abstract

Ordered nanoperforated TiO2 monolayers fabricated through sol–gel chemistry were used to grow isolated particles of Prussian blue analogues (PBA). The elaboration of the TiO2/CoFe PBA nanocomposites involves five steps. The samples were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), infrared spectroscopy and X-ray photoelectron spectroscopy (XPS) all along the synthesis process. Selected physico-chemical parameters have been varied in order to determine the key steps of the synthesis process and to optimize it. This study is an important step towards the full control of the fabrication process.

Published
2014
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2. A highly efficient solution and solid state ESIPT fluorophore and its OLED application

Author

Pei Yu, Sophie Gadan, Sandra Mazerat, Bernard Geffroy, Gilles Clavier, Anne Léaustic, Clémence Allain, Virgile Trannoy, Régis Guillot, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Institut de Chimie du CNRS (INC)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), Photophysique et Photochimie Supramoléculaires et Macromoléculaires (PPSM), Institut de Chimie du CNRS (INC)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Ecole Normale Supérieure Paris-Saclay (ENS Paris Saclay), Laboratoire Innovation en Chimie des Surfaces et NanoSciences (LICSEN), 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), Laboratoire de physique des interfaces et des couches minces [Palaiseau] (LPICM), École polytechnique (X)-Centre National de la Recherche Scientifique (CNRS), ANR-11-IDEX-0003,IPS,Idex Paris-Saclay(2011), Laboratoire Innovation en Chimie des Surfaces et NanoSciences (LICSEN UMR 3685), 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), 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-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Fluorophore, Proton, 010405 organic chemistry, Chemistry, Hydrogen bond, [CHIM.MATE]Chemical Sciences/Material chemistry, General Chemistry, Electroluminescence, 010402 general chemistry, 01 natural sciences, Fluorescence, Catalysis, 0104 chemical sciences, chemistry.chemical_compound, Crystallography, Intramolecular force, Excited state, Materials Chemistry, OLED
Abstract

We present herein the synthesis and the photophysics of 2,2’-bipyridine-3,3’-diol-5,5’-dicarboxylic acid ethyl ester (BP(OH)$_2$DCEt$_2$), an excited state intramolecular proton tranfer (ESIPT)-based fluorophore featuring two identical intramolecular hydrogen bonds. BP(OH)$_2$DCEt$_2$ emits efficiently not only in solution, including protic solvents ($\lambda _{em}$ = 521 nm, $\Phi$$_f$ = 40 to 75%), but also in crystalline state ($\lambda _{em}$ = 530 nm, $\Phi$$_f$ = 51%). In addition, its saponified form (Na2BP(OH)2DC) is highly fluorescent in water ($\lambda _{em}$ = 490 nm, $\Phi$$_f$ = 51%). Finally, the good electroluminescence performance of BP(OH)$_2$DCEt$_2$ is also demonstrated in an OLED device.

Published
2021
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3. Lanthanide Isophthalate Metal‐Organic Frameworks: Crystal Structure, Thermal Behavior, and White Luminescence

Author

Virgile Trannoy, Isis N’Dala-Louika, Jérôme Lhoste, Thomas Devic, Hélène Serier-Brault, Institut des Matériaux Jean Rouxel (IMN), Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN), Institut des Molécules et Matériaux du Mans (IMMM), and Le Mans Université (UM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Lanthanide, thermodiffraction analyses, TGA, Chemistry, Inorganic chemistry, PL spectra and CIE diagram and some crystal parameters (PDF), 02 engineering and technology, Crystal structure, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, lattice parameters evolution with the temperature, Inorganic Chemistry, FT-IR, PXRD, Thermal, [CHIM.CRIS]Chemical Sciences/Cristallography, Metal-organic framework, [CHIM.COOR]Chemical Sciences/Coordination chemistry, 0210 nano-technology, Luminescence
Abstract

International audience; Two novel lanthanide metal-organic frameworks (LnMOFs), Ln1.14Na0.57(BDC)2(H2O)4H2O (Ln = La 3+ or Ce 3+ , BDC : 1,3-benzenedicarboxylate), have been synthesized under hydrothermal conditions by using a Ln 3+ coordination polymer as precursor. The crystal structure was determined from single crystal X-ray diffraction. Both compounds are isostructural and contain chains of face-sharing [LnO10] polyhedra connected by the linkers to form an anionic three-dimensional network, defining both polar and apolar channels, the latter being occupied by water molecules and Ln 3+ and Na + cations. When doped by optimized content of Eu 3+ and Tb 3+ , the La 3+ counterpart exhibits white luminescence emission with CIE parameters equal to (0.3440, 0.3735) at λexc = 321 nm, which renders the material attractive for white LED application.

Published
2021

4. Fluorescent Zr(IV) Metal–Organic Frameworks Based on an Excited-State Intramolecular Proton Transfer-Type Ligand

Author

Gilles Clavier, Nathalie Guillou, Anne Léaustic, Virgile Trannoy, Carine Livage, Thomas Devic, Clémence Allain, Catherine Roch-Marchal, Mohamed Haouas, Pei Yu, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), 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), Chimie des interactions moléculaires (CIM), Centre National de la Recherche Scientifique (CNRS), Laboratoire de Photophysique et Photochimie Supramoléculaires et Macromoléculaires (PPSM), École normale supérieure - Cachan (ENS Cachan)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie du CNRS (INC)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Centre National de la Recherche Scientifique (CNRS), École normale supérieure - Cachan (ENS Cachan)-Centre National de la Recherche Scientifique (CNRS), Centre d'économie de la Sorbonne (CES), and Université Panthéon-Sorbonne (UP1)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Quantum yield, 010402 general chemistry, 01 natural sciences, Structure analysis, Fluorescence, Inorganic Chemistry, chemistry.chemical_compound, ESIPT, [CHIM]Chemical Sciences, Carboxylate, Physical and Theoretical Chemistry, ComputingMilieux_MISCELLANEOUS, Metal-Organic Frameworks, 010405 organic chemistry, Chemistry, Ligand, Sorption, Nuclear magnetic resonance spectroscopy, 0104 chemical sciences, Intramolecular force, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Physical chemistry, Metal-organic framework, Zirconium, Stability
Abstract

International audience; We report here the preparation of a series of Zr(IV) Metal Organic Frameworks of the MIL-140 structure type incorporating a ligand exhibiting an intense Excited State Intramolecular Proton Transfer (ESIPT) fluorescence. These solids were obtained by systematically varying the substitution rate of 4,4'-biphenyldicarboxylate by 2,2'-bipyridine-3,3'-diol-5,5'-dicarboxylate, and thoroughly characterized by complementary techniques, including high resolution powder X-ray diffraction, solid state NMR spectroscopy, nitrogen sorption experiments and time-resolved fluorescence. We showed that the incorporation of the ESIPT-type ligand induces an increase of the hydrophilicity, leading ultimately to a higher sensitivity toward hydrolysis, a phenomenon rarely observed in this structure type considered as one of the most stable among the Zr carboxylate MOFs. Eventually, the optimization of the amount of fluorescent ligand within the structure allowed combining a decent microposity (SBET > 750 m 2 .g-1) and a high stability even in boiling water, together with a high fluorescence quantum yield (> 30%).

Published
2019

5. Towards the synthesis of mixed oxides with controlled stoichiometry from Prussian blue analogues

Author

Jordan Dezalay, Cédric Baumier, Giulia Fornasieri, Patricia Beaunier, Camille La Fontaine, Anne Bleuzen, Amélie Bordage, Eric Rivière, R. Saint-Martin, Virgile Trannoy, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Réactivité de Surface (LRS), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), Centre de Sciences Nucléaires et de Sciences de la Matière (CSNSM), 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), Synchrotron SOLEIL (SSOLEIL), Centre National de la Recherche Scientifique (CNRS), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), 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
Materials science, Oxide, Nanoparticle, 02 engineering and technology, engineering.material, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, 010402 general chemistry, 01 natural sciences, law.invention, chemistry.chemical_compound, law, Phase (matter), General Materials Science, Calcination, Prussian blue, Spinel, General Chemistry, Mesoporous silica, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, Chemical engineering, chemistry, engineering, 0210 nano-technology, Stoichiometry
Abstract

International audience; Controlling the synthesis of mixed oxides is of great interest since their stoichiometry influences the properties. We present here the transformation of the Co4[Fe(CN)6]2.7 Prussian blue analogue (PBA) into the mixed Co1.8Fe1.2O4 spinel oxide, with a detailed characterization of the final phase (obtained by calcination in air at 900 °C for 2 hours) and an emphasis on the calcination process by TDA/TGA, X-ray diffraction, (high-resolution) TEM and energy-filtered TEM. Single-crystalline particles with a homogeneous distribution of Fe and Co ions within each particle are observed, with the same Co : Fe ratio as in the PBA. The calcination mechanism is a 2-step transformation, with first the elimination of water molecules and then the cyanide decomposition. XRD and TEM at intermediate temperatures additionally show the occurrence of a phase separation between 500 °C and 850 °C before the formation of the single final phase. We demonstrate also through the calcination of intermediate PBAs between Co4[Fe(CN)6]2.7 and Co4[Co(CN)6]2.7 that this synthesis route leads to the perfect control of the oxide stoichiometry through control of the PBA. The versatility of this synthesis route is finally illustrated through the successful synthesis of Co1.8Fe1.2O4 nanoparticles (diameter ∼5 nm) from PBA nanoparticles confined within the pores of a mesoporous silica monolith.

Published
2019

6. Transforming a Diamagnetic Ordered Mesoporous Silica Monolith into a Room Temperature Permanent Magnet through Multiscale Control of the Magnetic Properties

Author

Giulia Fornasieri, Virgile Trannoy, Patricia Beaunier, Amélie Bordage, Eric Rivière, Anne Bleuzen, Laura Altenschmidt, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Laboratoire de Réactivité de Surface (LRS), and Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS]Physics [physics], geography, Materials science, geography.geographical_feature_category, Renewable Energy, Sustainability and the Environment, Energy Engineering and Power Technology, 02 engineering and technology, Mesoporous silica, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Biomaterials, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, Chemical engineering, Magnet, Materials Chemistry, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Diamagnetism, Magnetic nanoparticles, Monolith, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018

7. Engineering of Mixed Eu 3+ /Tb 3+ Metal‐Organic Frameworks Luminescent Thermometers with Tunable Sensitivity

Author

Albano N. Carneiro Neto, Carlos D. S. Brites, Virgile Trannoy, Luís D. Carlos, Hélène Serier-Brault, Institut des Matériaux Jean Rouxel (IMN), Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN), and Universidade de Aveiro

Subjects
Tb-to-Eu energy transfer, Materials science, terbium, chemistry.chemical_element, Terbium, Nanotechnology, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Atomic and Molecular Physics, and Optics, 0104 chemical sciences, Electronic, Optical and Magnetic Materials, chemistry, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Metal-organic framework, Sensitivity (control systems), 0210 nano-technology, Europium, Luminescence, metal-organic frameworks, europium, ComputingMilieux_MISCELLANEOUS, luminescent thermometers
Abstract

International audience

Published
2021

8. Spatially controlled positioning of coordination polymer nanoparticles onto heterogeneous nanostructured surfaces

Author

Patricia Beaunier, Magali Putero, David Grosso, Virgile Trannoy, Marco Faustini, Anne Bleuzen, François Brisset, Eric Rivière, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS), Matériaux Hybrides et Nanomatériaux (MHN), Laboratoire de Chimie de la Matière Condensée de Paris (LCMCP), Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF)-Centre National de la Recherche Scientifique (CNRS)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF)-Centre National de la Recherche Scientifique (CNRS), Centre d'Études en Civilisations Langues et Lettres Étrangères (CECILLE) - EA 4074 (CECILLE), Université de Lille, Laboratoire de Réactivité de Surface (LRS), Centre National de la Recherche Scientifique (CNRS)-Université Pierre et Marie Curie - Paris 6 (UPMC), Institut des Matériaux, de Microélectronique et des Nanosciences de Provence (IM2NP), Aix Marseille Université (AMU)-Université de Toulon (UTLN)-Centre National de la Recherche Scientifique (CNRS), Université Paris-Sud - Paris 11 (UP11)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), Matériaux Hybrides et Procédés (LCMCP-MHP ), Matériaux Hybrides et Nanomatériaux (LCMCP-MHN), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Laboratoire de Chimie de la Matière Condensée de Paris (LCMCP), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-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), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), and Université de Toulon (UTLN)-Centre National de la Recherche Scientifique (CNRS)-Aix Marseille Université (AMU)

Subjects
Nanocomposite, Materials science, Scanning electron microscope, Coordination polymer, Nucleation, Oxide, Nanoparticle, Nanotechnology, [CHIM.MATE]Chemical Sciences/Material chemistry, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Titanium oxide, chemistry.chemical_compound, chemistry, [CHIM]Chemical Sciences, General Materials Science, Thin film, 0210 nano-technology
Abstract

International audience; Prussian Blue Analog (PBA) nanoparticles were formed on a heterogeneous nanostructured surface made of an ordered nanoperforated titanium oxide thin film deposited on a gold layer. The study of the nanocomposite film by grazing-incidence wide angle X-ray scattering, infrared spectroscopy, scanning electron microscopy and atomic force microscopy shows that the PBA particles are precisely positioned within all the perforations of the oxide film over very large surface areas. Further investigation on the formation of the PBA particles demonstrates a decisive role of a heterogeneous nucleation of the coordination polymer driven by well-adjusted surfaces energies and reactant concentrations in the spatial positioning of the PBA particles. Thanks to the well-controlled positioning of the particles within the ordered nanoperforations, the latter were successfully used as nano crucibles for the local transformation of PBA into the corresponding metal alloy by heat treatment. The thin film heterostructure thus obtained, made of ferromagnetic islands isolated by diamagnetic walls, opens interesting perspectives for the design of magnetic storage devices.

Published
2017

9. Towards bottom-up nanopatterning of Prussian blue analogues

Author

Anne Bleuzen, Alexandre Dazzi, Virgile Trannoy, David Grosso, François Brisset, Marco Faustini, Sandra Mazerat, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Matériaux Hybrides et Nanomatériaux (MHN), Laboratoire de Chimie de la Matière Condensée de Paris (LCMCP), Université Pierre et Marie Curie - Paris 6 (UPMC)-Centre National de la Recherche Scientifique (CNRS)-Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Centre National de la Recherche Scientifique (CNRS)-Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC), Université Pierre et Marie Curie - Paris 6 (UPMC)-Centre National de la Recherche Scientifique (CNRS)-Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC), CNRS / Université Paris-Sud, Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie Physique D'Orsay (LCPO), Université Paris-Sud - Paris 11 (UP11)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), C'Nano IdF, University Paris-Sud, University Paris 6, Region Ile-de-France C'Nano program, Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Fabrication, Scanning electron microscope, nanoperforated oxide monolayer, General Physics and Astronomy, Infrared spectroscopy, Nanotechnology, 02 engineering and technology, 010402 general chemistry, lcsh:Chemical technology, 01 natural sciences, lcsh:Technology, Full Research Paper, nanopatterning, chemistry.chemical_compound, X-ray photoelectron spectroscopy, Monolayer, General Materials Science, lcsh:TP1-1185, Electrical and Electronic Engineering, lcsh:Science, Prussian blue, Nanocomposite, Atomic force microscopy, lcsh:T, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, lcsh:QC1-999, 0104 chemical sciences, Nanoscience, Prussian blue analogues, chemistry, lcsh:Q, 0210 nano-technology, lcsh:Physics
Abstract

Ordered nanoperforated TiO2 monolayers fabricated through sol–gel chemistry were used to grow isolated particles of Prussian blue analogues (PBA). The elaboration of the TiO2/CoFe PBA nanocomposites involves five steps. The samples were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), infrared spectroscopy and X-ray photoelectron spectroscopy (XPS) all along the synthesis process. Selected physico-chemical parameters have been varied in order to determine the key steps of the synthesis process and to optimize it. This study is an important step towards the full control of the fabrication process.

Published
2014

10. Co(2+)@Mesoporous Silica Monoliths: Tailor-Made Nanoreactors for Confined Soft Chemistry

Author

Emilie Delahaye, Robinson Moulin, Virgile Trannoy, Giulia Fornasieri, Merwen Aouadi, Anne Bleuzen, and Patricia Beaunier

Subjects
Prussian blue, Organic Chemistry, Nanoparticle, General Chemistry, Nanoreactor, Mesoporous silica, Catalysis, Soft chemistry, chemistry.chemical_compound, Transition metal, chemistry, Tetramethyl orthosilicate, Chemical engineering, Organic chemistry, Mesoporous material
Abstract

Mesoporous silica monoliths with various ordered nanostructures containing transition metal M(2+) cations in variable amounts were elaborated and studied. A phase diagram depicting the different phases as a function of the M(2+) salt/tetramethyl orthosilicate (TMOS) and surfactant P123/TMOS ratios was established. Thermal treatment resulted in mesoporous monoliths containing isolated, accessible M(2+) species or condensed metal oxides, hydroxides, and salts, depending on the strength of the interactions between the metal species and the ethylene oxide units of P123. The ordered mesoporosity of the monoliths containing accessible M(2+) ions was used as a nanoreactor for the elaboration of various transition metal compounds (Prussian blue analogues, Hofmann compounds, metal-organic frameworks), and this opens the way to the elaboration of a large range of nanoparticles of multifunctional materials.

Published
2015

11. In situ site-selective transition metal K-edge XAS: a powerful probe of the transformation of mixed-valence compounds

Author

Olivier Proux, Robinson Moulin, Anne Bleuzen, Hugo Vitoux, Amélie Bordage, Virgile Trannoy, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), and European Synchrotron Radiation Facility (ESRF)

Subjects
Prussian blue, X-ray absorption spectroscopy, Valence (chemistry), Absorption spectroscopy, Oxide, Analytical chemistry, General Physics and Astronomy, chemistry.chemical_compound, chemistry, K-edge, Transition metal, Physical chemistry, [CHIM]Chemical Sciences, Emission spectrum, Physical and Theoretical Chemistry
Abstract

International audience; We present herein the first in situ site-selective XAS experiment performed on a proof-of-principle transformation of a mixed-valence compound: the calcination of the K0.1Co4II[Co-III(CN)(6)](2.7)center dot 20H(2)O Prussian Blue analogue (containing Co2+ and Co3+ ions in two different O-h sites) into Co3O4 (containing Co2+ ions in a T-d site and Co3+ in an O-h site). By recording the Co K-edge X-ray absorption spectra using a spectrometer aligned at the Co K beta(1,3) emission line, the evolution of each species was singly monitored from 20 degrees C up to the oxide formation. The experimental spectrum of the Co2+(T-d) and Co3+ (O-h) species in Co3O4 is reported for the first time. Our results demonstrate the possibilities offered by site-selective XAS for the investigation of chemical transformations and the study of materials under working conditions whenever the chemical element of interest is present in several states and/or sites

Published
2015

12. Using Prussian blue analogue nanoparticles confined into ordered mesoporous silica monoliths as precursors of oxides

Author

Emilie Delahaye, Giulia Fornasieri, Virgile Trannoy, Patricia Beaunier, Anne Bleuzen, Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Réactivité de Surface (LRS), and Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Silice mésoporeuse, General Chemical Engineering, Oxide, Nanoparticle, Nanotechnology, 02 engineering and technology, Thermal treatment, engineering.material, 010402 general chemistry, 01 natural sciences, Analogues du bleu de Prusse, chemistry.chemical_compound, Co3O4, [CHIM]Chemical Sciences, High-resolution transmission electron microscopy, Prussian blue, Small-angle X-ray scattering, Spinel, Nanoparticules, General Chemistry, Mesoporous silica, 021001 nanoscience & nanotechnology, 0104 chemical sciences, chemistry, Chemical engineering, engineering, 0210 nano-technology
Abstract

International audience; Powdered Prussian blue analogues (PBAs) and PBAs confined in ordered mesoporous silica monoliths were used as oxide precursors through thermal treatment under an oxidizing atmosphere. The study focuses on the transformation of the alkali cation-free CoCo PBA of chemical formula K0.1CoII4[CoIII(CN)6]2.7·20 H2O. The compounds were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), IR spectroscopy and small-angle X-ray scattering (SAXS), and the magnetic properties of the calcined samples were investigated. In both cases, powdered and confined PBAs, the coordination polymers are transformed into well-crystallized Co3O4 spinel oxide. In the case of the confined PBA, isolated Co3O4 single crystals confined within the ordered mesoporosity of the monoliths were evidenced by HRTEM. A preliminary study shows an effect of particle size and confinement on the magnetic properties of the confined oxide particles.

Published
2014

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