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1. Deciphering the Influence of Electrolytes on the Energy Storage Mechanism of Vertically-Oriented Graphene Nanosheet Electrodes by Using Advanced Electrogravimetric Methods

Author

Tao Lé, Gérard Bidan, Florence Billon, Marc Delaunay, Jean-Michel Gérard, Hubert Perrot, Ozlem Sel, and David Aradilla

Subjects
graphene, supercapacitor, electrolyte, ionic liquids, energy storage mechanisms, EQCM, Chemistry, QD1-999
Abstract

Electrolyte composition is a crucial factor determining the capacitive properties of a supercapacitor device. However, its complex influence on the energy storage mechanisms has not yet been fully elucidated. For this purpose, in this study, the role of three different types of electrolytes based on a propylene carbonate (PC) solution containing tetrabutylammonium perchlorate (TBAClO4), lithium perchlorate (LiClO4) and butyltrimethylammonium bis(trifluoromethylsulfonyl)imide (N1114TFSI) ionic liquid on vertically-oriented graphene nanosheet electrodes has been investigated. Herein, in situ electrochemical quartz crystal microbalance (EQCM) and its coupling with electrochemical impedance spectroscopy (EIS), known as ac-electrogravimetry, have allowed the dynamic aspects of the (co)electroadsorption processes at the electrode-electrolyte interface to be examined. A major contribution of ClO4− anions (TBAClO4) was evidenced, whereas in the PC/N1114TFSI mixture (50:50 wt%) both anions (TFSI−) and cations (N1114+) were symmetrically exchanged during cycling. In the particular case of LiClO4, solvation of Li+ cations in PC was involved, affecting the kinetics of electroadsorption. These results demonstrate the suitability of dynamic electrogravimetric methods to unveil the interfacial exchange properties of mobile species for the conception of new high performance energy storage devices.

Published
2020
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2. Charge Storage Properties of Nanostructured Poly (3,4–ethylenedioxythiophene) Electrodes Revealed by Advanced Electrogravimetry

Author

Tao Lé, David Aradilla, Gérard Bidan, Florence Billon, Catherine Debiemme-Chouvy, Hubert Perrot, and Ozlem Sel

Subjects
PEDOT, nanowires, (pseudo)-supercapacitors, charge storage mechanism, interfacial ion transfer, EQCM, AC–EG, Chemistry, QD1-999
Abstract

PEDOT nanowires (NWs) directly grown on the conducting electrode of quartz resonators enable an advanced electrogravimetric analysis of their charge storage behavior. Electrochemical quartz crystal microbalance (EQCM) and its coupling with electrochemical impedance spectroscopy (ac–electrogravimetry or AC–EG) were used complementarily and reveal that TBA+, BF4− and ACN participate in the charge compensation process with different kinetics and quantity. BF4− anions were dominant in terms of concentration over TBA+ cations and the anion transfer results in the exclusion of the solvent molecules. TBA+ concentration variation in the electrode was small compared to that of the BF4− counterpart. However, Mw of TBA+ is much higher than BF4− (242.3 vs. 86.6 g·mol−1). Thus, TBA+ cations’ gravimetric contribution to the EQCM response was more significant than that of BF4−. Additional contribution of ACN with an opposite flux direction compared with BF4−, led to a net mass gain/lost during a negative/positive potential scan, masking partially the anion response. Such subtleties of the interfacial ion transfer processes were disentangled due to the complementarity of the EQCM and AC–EG methodologies, which were applied here for the characterization of electrochemical processes at the PEDOT NW electrode/organic electrolyte interface.

Published
2019
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3. Beyond conventional supercapacitors: Hierarchically conducting polymer-coated 3D nanostructures for integrated on-chip micro-supercapacitors employing ionic liquid electrolytes

Author

Gérard Bidan, Saïd Sadki, and David Aradilla

Subjects
Materials science, Nanowire, Nanotechnology, 02 engineering and technology, 010402 general chemistry, Polypyrrole, 01 natural sciences, Capacitance, law.invention, chemistry.chemical_compound, law, Polyaniline, Materials Chemistry, Supercapacitor, Conductive polymer, Graphene, Mechanical Engineering, Metals and Alloys, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, Electronic, Optical and Magnetic Materials, chemistry, Mechanics of Materials, Ionic liquid, 0210 nano-technology
Abstract

The potential of electroactive conducting polymers (ECPs), as innovative pseudocapacitive materials, has recently emerged as a promising strategy to design new and advanced concepts in the field of electrochemical energy storage devices. From this point of view, the synergistic effect produced between high electroactivity ECPs (faradaic behaviour) and large active surface 3D nanostructured materials (electrochemical double layer behaviour) in terms of their high specific capacitance, high energy and power density as well as long lifetime, has awakened an enormous interest in the domain of (micro)-supercapacitors. Accordingly, in this work, we have originally analyzed the conformal electrochemical deposition of three different π-conjugated heterocyclic polymers [poly(3,4-ethylenedioxythiophene, polypyrrole and polyaniline] onto various vertically-oriented 3D nanoarchitectures, as for example silicon nanowires (SiNWs), diamond nanowires (DiNWs) or graphene nanosheets (GNs) among others. Next, the resulting as-grown hybrid materials were evaluated as attractive electrodes in symmetric supercapacitors (sandwich configuration) in presence of organic, aqueous, aprotic and protic ionic liquid (IL) electrolytes respectively. An exhaustive characterization of their corresponding electrochemical performances was investigated according to our previously reported works, confirming the remarkable cycling stability of ECPs in ILs. In addition, a detailed state-of-the-art dealing with other types of (micro)-supercapacitors in the literature was reported to corroborate the great impact of such devices to pave the way towards the elaboration of next generation high performance supercapacitors in the coming years.

Published
2019

4. Plasma Heavily Nitrogen-Doped Vertically Oriented Graphene Nanosheets (N-VOGNs) for High Volumetric Performance On-Chip Supercapacitors in Ionic Liquid

Author

Michael Buhagiar, Hanako Okuno, Dmitry Aldakov, David Aradilla, Jérôme Faure-Vincent, Jean-Michel Gérard, Marc Delaunay, Gérard Bidan, Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Nanophysique et Semiconducteurs (NPSC), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire d'Etude des Matériaux par Microscopie Avancée (LEMMA ), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Aldakov, Dmitry

Subjects
[CHIM.INOR] Chemical Sciences/Inorganic chemistry, Materials science, Nanotechnology, Nitrogen doped, 02 engineering and technology, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, 010402 general chemistry, 7. Clean energy, 01 natural sciences, law.invention, chemistry.chemical_compound, law, ComputingMilieux_MISCELLANEOUS, Supercapacitor, [CHIM.MATE] Chemical Sciences/Material chemistry, Graphene, [CHIM.MATE]Chemical Sciences/Material chemistry, General Medicine, Plasma, 021001 nanoscience & nanotechnology, [PHYS.COND.CM-MS] Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0104 chemical sciences, chemistry, [CHIM.OTHE] Chemical Sciences/Other, Ionic liquid, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [CHIM.OTHE]Chemical Sciences/Other, 0210 nano-technology
Abstract

International audience

Published
2018

5. Understanding the energy storage mechanisms of poly(3,4-ethylenedioxythiophene)-coated silicon nanowires by electrochemical quartz crystal microbalance

Author

Catherine Debiemme-Chouvy, Ozlem Sel, Florence Billon, Gérard Bidan, Pascal Gentile, Tao Lé, Hubert Perrot, David Aradilla, SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Interfaces et Systèmes Electrochimiques (LISE), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Georg-August-University [Göttingen], LABEX MATISSE (ANR-11-IDEX-0004-02), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Georg-August-University = Georg-August-Universität Göttingen

Subjects
Materials science, 02 engineering and technology, Chemical vapor deposition, 010402 general chemistry, Electrochemistry, 01 natural sciences, chemistry.chemical_compound, PEDOT:PSS, [CHIM]Chemical Sciences, General Materials Science, SiNWs, PEDOT, Supercapacitor, Mechanical Engineering, [CHIM.MATE]Chemical Sciences/Material chemistry, Quartz crystal microbalance, 021001 nanoscience & nanotechnology, Condensed Matter Physics, EQCM, 0104 chemical sciences, chemistry, Chemical engineering, Mechanics of Materials, (Pseudo)-supercapacitors, Electrode, Cyclic voltammetry, 0210 nano-technology, Poly(3,4-ethylenedioxythiophene)
Abstract

International audience; The capacitive properties of electrodes elaborated from the electrochemical deposition of poly(3,4-ethylenedioxythiophene) (PEDOT) coatings onto chemical vapor deposition (CVD)-grown silicon nanowires (SiNWs) were investigated for supercapacitor applications. A high areal capacitance value of 17 mF cm−2 (50 F g−1) was obtained at a scan rate of 100 mV s−1 in a 3-electrode cell configuration. Furthermore, this 3D hybrid nanostructure was analyzed by electrochemical quartz crystal microbalance (EQCM) to correlate the interfacial ionic exchange mechanisms to their electrochemical performance. It was demonstrated that both anions (BF4−) and cations (TBA+) were simultaneously involved in the charge compensation during the oxidation-reduction scans of cyclic voltammetry measurements.

Published
2019

6. Powering electrodes for high performance aqueous micro-supercapacitors: Diamond-coated silicon nanowires operating at a wide cell voltage of 3 V

Author

Georgia Lewes-Malandrakis, Gérard Bidan, Christoph E. Nebel, Pascal Gentile, Fang Gao, Stéphanie Pouget, David Aradilla, and W. Müller-Sebert

Subjects
Supercapacitor, Materials science, Silicon, business.industry, General Chemical Engineering, Diamond, chemistry.chemical_element, 02 engineering and technology, engineering.material, 010402 general chemistry, 021001 nanoscience & nanotechnology, 7. Clean energy, 01 natural sciences, 0104 chemical sciences, Coating, chemistry, Electrode, Electrochemistry, engineering, Optoelectronics, 0210 nano-technology, business, Current density, Electrochemical window, Power density
Abstract

In this study, we report originally the excellent electrochemical performance of a micro-supercapacitor based on diamond-coated silicon nanowire (SiNW) electrodes using an aqueous electrolyte (0.1 M LiClO4). The deposition of a nanometric boron-doped diamond coating on SiNWs allowed the enlargement of the electrochemical window up to 3 V maintaining an extraordinary capacitive electrochemical response due to its high overvoltage. Thereby, the device exhibited an areal capacitance of 0.4 mF cm-2, a high power density of 50 mW cm-2 as well as an outstanding cycling stability after 2·106 galvanostatic charge-discharge cycles at a high current density of 10 mA cm-2. In addition, an ultra-fast charge-discharge rate was determined to be 1.5 ms, demonstrating the supercapacitor's enormous ability to deliver high power values at very rapid pulse times (Pmax: 321 mW cm-2). These results also evidence the potential of diamond coating to overcome the main drawbacks of silicon (e.g. rapid silicon oxidation due to presence of water) to be employed in aqueous electrolyte supercapacitors. Consequently, the role of diamond paves the way to high performance SiNW-based micro-supercapacitor development at large electrochemical windows in aqueous electrolytes, which are at present limited to 1 V.

Published
2017

7. Charge Storage Properties of Nanostructured Poly (3,4–ethylenedioxythiophene) Electrodes Revealed by Advanced Electrogravimetry

Author

Gérard Bidan, Tao Lé, David Aradilla, Ozlem Sel, Florence Billon, Catherine Debiemme-Chouvy, Hubert Perrot, SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Interfaces et Systèmes Electrochimiques (LISE), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), University Medical Center Göttingen (UMG), Labex MATISSE ANR-11-IDEX-0004-02, Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)

Subjects
Materials science, General Chemical Engineering, Analytical chemistry, 02 engineering and technology, Electrolyte, 010402 general chemistry, Electrochemistry, 01 natural sciences, lcsh:Chemistry, chemistry.chemical_compound, PEDOT:PSS, Electrogravimetry, TheoryofComputation_ANALYSISOFALGORITHMSANDPROBLEMCOMPLEXITY, [CHIM]Chemical Sciences, General Materials Science, (pseudo)-supercapacitors, AC–EG, EQCM, PEDOT, charge storage mechanism, interfacial ion transfer, nanowires, Communication, AC-EG, Quartz crystal microbalance, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Dielectric spectroscopy, chemistry, lcsh:QD1-999, Electrode, 0210 nano-technology, Poly(3,4-ethylenedioxythiophene)
Abstract

PEDOT nanowires (NWs) directly grown on the conducting electrode of quartz resonators enable an advanced electrogravimetric analysis of their charge storage behavior. Electrochemical quartz crystal microbalance (EQCM) and its coupling with electrochemical impedance spectroscopy (ac–electrogravimetry or AC–EG) were used complementarily and reveal that TBA+, BF4− and ACN participate in the charge compensation process with different kinetics and quantity. BF4− anions were dominant in terms of concentration over TBA+ cations and the anion transfer results in the exclusion of the solvent molecules. TBA+ concentration variation in the electrode was small compared to that of the BF4− counterpart. However, Mw of TBA+ is much higher than BF4− (242.3 vs. 86.6 g·mol−1). Thus, TBA+ cations’ gravimetric contribution to the EQCM response was more significant than that of BF4−. Additional contribution of ACN with an opposite flux direction compared with BF4−, led to a net mass gain/lost during a negative/positive potential scan, masking partially the anion response. Such subtleties of the interfacial ion transfer processes were disentangled due to the complementarity of the EQCM and AC–EG methodologies, which were applied here for the characterization of electrochemical processes at the PEDOT NW electrode/organic electrolyte interface.

Published
2019

8. A step forward into hierarchically nanostructured materials for high performance micro-supercapacitors: Diamond-coated SiNW electrodes in protic ionic liquid electrolyte

Author

Pascal Gentile, W. Müller-Sebert, Gérard Bidan, Christoph E. Nebel, Fang Gao, Dorian Gaboriau, David Aradilla, Georgia Lewes-Malandrakis, Thomas J. S. Schubert, Saïd Sadki, Boyan Iliev, Polymères Conducteurs Ioniques (PCI), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Fraunhofer Institute for Applied Solid State Physics (Fraunhofer IAF), Fraunhofer (Fraunhofer-Gesellschaft), Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Ionic Liquids Technologies GmbH (IOLITECH), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), gentile, pascal, Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, [SPI.NANO] Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, Inorganic chemistry, Nanowire, 02 engineering and technology, Electrolyte, Chemical vapor deposition, engineering.material, [SPI.MAT] Engineering Sciences [physics]/Materials, 010402 general chemistry, 01 natural sciences, 7. Clean energy, Capacitance, [SPI.MAT]Engineering Sciences [physics]/Materials, lcsh:Chemistry, chemistry.chemical_compound, Electrochemistry, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS, Supercapacitor, [SPI.NRJ]Engineering Sciences [physics]/Electric power, Diamond, 021001 nanoscience & nanotechnology, [PHYS.COND.CM-MS] Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0104 chemical sciences, chemistry, Chemical engineering, lcsh:Industrial electrochemistry, lcsh:QD1-999, Electrode, Ionic liquid, engineering, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology, [SPI.NRJ] Engineering Sciences [physics]/Electric power, lcsh:TP250-261
Abstract

Silicon nanowires (SiNWs) were successfully coated by uniform, adherent and homogenous ultra-thin crystalline diamond films through microwave enhanced chemical vapor deposition (MWCVD). The as-grown functionalized nanowires were employed as electrodes in a symmetric micro-supercapacitor (MSC) using a protic ionic liquid electrolyte [triethylammonium bis(trifluoromethylsulfonyl)imide; Et3NH TFSI]. The electrochemical performance of the device delivered a specific capacitance of 1.5 mF cm−2 and a power density of 25 mW cm−2 using an enlarged cell voltage of 4 V. Furthermore, a remarkable cycling stability was evaluated after 1 · 106 galvanostatic cycles at a high current density of 10 mA cm−2 with an excellent capacitive behavior. These results confirm that diamond-coated SiNW micro-supercapacitors exhibit very promising performances dealing with MSCs based on CVD-grown SiNWs. Keywords: Supercapacitors, Ionic liquid, Diamond, Silicon nanowires

Published
2016

9. Unveiling the ionic exchange mechanisms in vertically-oriented graphene nanosheet supercapacitor electrodes with electrochemical quartz crystal microbalance and ac -electrogravimetry

Author

Tao Lé, Marc Delaunay, Gérard Bidan, Jean-Michel Gérard, Florence Billon, Ozlem Sel, Hubert Perrot, David Aradilla, Laboratoire Interfaces et Systèmes Electrochimiques (LISE), Université Pierre et Marie Curie - Paris 6 (UPMC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Nanophysique et Semiconducteurs (NPSC), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), ANR-11-IDEX-0004,SUPER,Sorbonne Universités à Paris pour l'Enseignement et la Recherche(2011), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG)

Subjects
Materials science, Ionic bonding, 02 engineering and technology, Electrolyte, 010402 general chemistry, Electrochemistry, 01 natural sciences, law.invention, lcsh:Chemistry, law, Electrogravimetry, Supercapacitors, Microbalance, Ac-electrogravimetry, Nanosheet, Supercapacitor, Graphene, Quartz crystal microbalance, 021001 nanoscience & nanotechnology, 0104 chemical sciences, lcsh:Industrial electrochemistry, lcsh:QD1-999, Chemical engineering, 0210 nano-technology, [CHIM.OTHE]Chemical Sciences/Other, lcsh:TP250-261
Abstract

This work presents the first electrochemical quartz crystal microbalance (EQCM) results for vertically-oriented graphene nanosheets (VOGNs) as supercapacitor electrodes. Conventional EQCM technique delivered primary insights on the ionic exchange mechanisms between VOGNs and organic electrolytes, showing a major contribution of anions. A more advanced electrogravimetric methodology, ac-electrogravimetry, was then used to access specific dynamic attributes for each species exchanged at the VOGN electrode surface. Accordingly, under the conditions of this study, anions were confirmed to be the major energy storage vector with high kinetic values and low transfer resistance while cations and free solvent molecules are given non-negligible supporting roles. Keywords: Supercapacitors, Microbalance, ac-electrogravimetry, Graphene

Published
2018

10. Etude électrogravimétrique d'électrodes à base de nanofils de silicium pour le stockage électrochimique de l'énergie

Author

Tao Lé, Gentile, P., David Aradilla, Gérard Bidan, Hubert Perrot, Ozlem Sel, Laboratoire Interfaces et Systèmes Electrochimiques (LISE), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), Institut Nanosciences et Cryogénie (INAC), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])

Subjects
[CHIM]Chemical Sciences
Abstract

International audience; Les électrodes élaborées avec des architectures nanométriquessont de plus en plus étudiées pour améliorer les performances desbatteries et supercondensateurs. En particulier les nanofils desilicium dopés permettent d’obtenir de hautes valeurs depuissance et d’énergie grâce à de larges surfaces développées etune bonne conductivité jusqu’au collecteur de courant [1].Cependant les mécanismes d’échanges ioniques et lesphénomènes de décomposition de l’électrolyte ayant lieu àl’interface des nanofils varient en fonction de l’électrolyte utiliséet restent largement méconnus.Une meilleure compréhension de ces mécanismes peut êtreobtenue avec la microbalance à quartz électrochimique(EQCM) qui couple l’analyse électrochimique à la mesure desvariations de masse de l’électrode, ce qui permet de distinguerles espèces mises en jeu et la cinétique des échanges ioniques[2].Pour réaliser cette étude, la croissance de nanofils de silicium aété mise au point sur un substrat piézoélectrique en GaPO4compatible avec la température de croissance par CVD à600°C (Fig. 1.a).Des mesures électrogravimétriques effectuées dans diversmilieux organiques et des mélanges de liquides ioniques ontpermis de distinguer différents mécanismes de stockageélectrochimique et leurs cinétiques associées (Fig. 1.b)Références :[1] Aradilla, D.; Gentile, P.; Bidan, G.; Ruiz, V.; Gómez-Romero, P.; Schubert, T. J.; Sahin, H.;Frackowiak, E.; Sadki, S. Nano Energy 2014, 9, 273–281.[2] Escobar-Teran, F.; Arnau, A.; Garcia, J.; Jiménez, Y.; Perrot, H.; Sel, O. ElectrochemistryCommunications 2016, 70, 73–77.

Published
2017

11. Are tomorrow's micro-supercapacitors hidden in a forest of silicon nanotrees?

Author

Thierry Brousse, Gérard Bidan, Pascal Gentile, Saïd Sadki, and Fleur Thissandier

Subjects
Supercapacitor, Materials science, Silicon, Renewable Energy, Sustainability and the Environment, Energy Engineering and Power Technology, chemistry.chemical_element, Nanotechnology, Chemical vapor deposition, Electrolyte, Capacitance, Catalysis, chemistry.chemical_compound, chemistry, Chemical engineering, Electrode, Ionic liquid, Electrical and Electronic Engineering, Physical and Theoretical Chemistry
Abstract

Silicon nanotrees (SiNTrs) have been grown by Chemical Vapor Deposition (CVD) via gold catalysis and a three steps process: trunks and branches growth are separated by a new gold catalyst deposition. The influence of growth conditions and the second gold catalyst deposition method on SiNTrs morphology are investigated. SiNTrs based electrodes show a capacitive behavior and better capacitance than the corresponding silicon nanowires (SiNWs) electrode. Electrode capacitance is increased up to 900 μF cm−2, i.e. 150 fold higher than for bulk silicon. Micro-supercapacitors with SiNTrs electrodes have a remarkable stability (only 1.2% loses of their initial capacitance after more than one million cycles). The use of an ionic liquid based electrolyte leads to a high maximum power density (around 225 mW cm−2) which is competitive with Onion Like Carbon based micro-supercapacitors.

Published
2014

12. Electrochemical performance of silicon nanostructures in low-temperature ionic liquids for microelectronic applications

Author

Gérard Bidan, Elzbieta Frackowiak, Krzysztof Fic, Thomas J. S. Schubert, Anetta Platek, Justyna Piwek, Pascal Gentile, Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), gentile, pascal, Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Silicon, [SPI.NANO] Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, chemistry.chemical_element, Nanotechnology, 02 engineering and technology, Electrolyte, [SPI.MAT] Engineering Sciences [physics]/Materials, 010402 general chemistry, Electrochemistry, 01 natural sciences, 7. Clean energy, Capacitance, [SPI.MAT]Engineering Sciences [physics]/Materials, chemistry.chemical_compound, Microelectronics, General Materials Science, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS, Renewable Energy, Sustainability and the Environment, business.industry, [SPI.NRJ]Engineering Sciences [physics]/Electric power, General Chemistry, 021001 nanoscience & nanotechnology, [PHYS.COND.CM-MS] Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0104 chemical sciences, Freezing point, Chemical engineering, chemistry, Ionic liquid, Electrode, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology, business, [SPI.NRJ] Engineering Sciences [physics]/Electric power
Abstract

Successful implementation of silicon nanostructures as suitable electrodes for microcapacitors performing at low temperatures (up to −40 °C) has been realized. In order to avoid the freezing of the electrolyte solution, two ionic liquids with low freezing points have been synthesized and applied as the electrolyte. Silicon nanotrees selected as the most useful electrode material have been combined with the mixture of two miscible ionic liquids (EMIM TFSI + AMIM TFSI). This allowed the operational voltage equal to 3 V to be achieved. The specific capacitance of 377 μF cm−2 resulted in 2 mJ cm−2 energy output. Furthermore, all electrode materials subjected to the investigation were able to deliver the energy even at high frequency (120 Hz). Hence, the application in microelectronics has been considered.

Published
2017

13. New electrolyte mixture of propylene carbonate and butyltrimethylammonium bis(trifluoromethylsulfonyl)imide (N 1114 TFSI) for high performance silicon nanowire (SiNW)-based supercapacitor applications

Author

Gérard Bidan, Pascal Gentile, David Aradilla, Tao Lé, SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), and Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG)

Subjects
Materials science, General Chemical Engineering, Inorganic chemistry, 02 engineering and technology, Electrolyte, electrolyte, 010402 general chemistry, Electrochemistry, 01 natural sciences, 7. Clean energy, chemistry.chemical_compound, Silicon nanowires, Imide, Power density, ionic liquid, Supercapacitor, supercapacitors, temperature, 021001 nanoscience & nanotechnology, 0104 chemical sciences, mixture, chemistry, Chemical engineering, Ionic liquid, Propylene carbonate, 0210 nano-technology, [CHIM.OTHE]Chemical Sciences/Other
Abstract

International audience; The use of a mixture of propylene carbonate (PC) and N1114 TFSI ionic liquid (50:50% w.t) has been investigated as an optimal electrolyte for symmetric micro-supercapacitors based on SiNWs using a large and stable cell voltage of 3.5 V. The device showed an areal capacitance of 150 μF cm−2, an energy density of 1 mJ cm−2 and a power density of 16 mW cm−2 maintaining an outstanding cycling stability after 3·106 galvanostatic charge-discharge cycles at room temperature. Such properties were comparable to those obtained using the pure ionic liquid. Additionally, the excellent electrochemical performances reported in this study reflect the potential of such mixture to be employed as a promising electrolyte in wide operating temperatures ranging from 0 to 80 °C at large electrochemical windows.

Published
2017

14. Wide-voltage-window silicon nanowire electrodes for micro-supercapacitors via electrochemical surface oxidation in ionic liquid electrolyte

Author

Jean Le Bideau, Gérard Bidan, Pascal Gentile, Thierry Brousse, Fleur Thissandier, Saïd Sadki, Mylène Brachet, Nicolas Berton, Physico-chimie des Matériaux et des Electrolytes pour l'Energie (PCM2E), Université de Tours, 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), Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Institut Nanosciences et Cryogénie (INAC), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Service de Chimie Inorganique et Biologique (SCIB - UMR E3), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Université de Tours (UT), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), and Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Silicon, Inorganic chemistry, chemistry.chemical_element, Electrolyte, Electrochemistry, 7. Clean energy, Capacitance, lcsh:Chemistry, chemistry.chemical_compound, [SPI]Engineering Sciences [physics], Etching (microfabrication), [CHIM]Chemical Sciences, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS, Supercapacitor, business.industry, [SPI.NRJ]Engineering Sciences [physics]/Electric power, chemistry, lcsh:Industrial electrochemistry, lcsh:QD1-999, Electrode, Ionic liquid, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Optoelectronics, business, lcsh:TP250-261
Abstract

The potential of silicon nanowires (SiNWs) as electrode material for large-voltage window micro-supercapacitors has been investigated. An ionic liquid electrolyte (EMI-TFSI) has been used in order to prevent the previously reported etching of silicon electrodes. Electrochemical oxidation of silicon surface at high anodic potentials leads to an extended operating voltage range (up to 4 V) and slightly enhanced specific capacitance of silicon electrodes. The ability of SiNW electrodes to operate at high frequency was demonstrated and a promising specific power of 472 μW cm−2 was obtained. Keywords: Highly doped silicon nanowires, Micro-supercapacitor, Ionic liquid electrolyte, Electrochemical energy storage, Silicon electrochemical oxidation

Published
2014

15. Synthesis of high quality reduced graphene oxide nanosheets free of paramagnetic metallic impurities

Author

Lionel Dubois, Nanjundan Ashok Kumar, Gérard Bidan, Serge Gambarelli, and Florence Duclairoir

Subjects
Materials science, Renewable Energy, Sustainability and the Environment, Graphene, Orders of magnitude (temperature), Hydrazine, Inorganic chemistry, Oxide, General Chemistry, Chloride, Exfoliation joint, law.invention, Paramagnetism, chemistry.chemical_compound, chemistry, law, medicine, General Materials Science, Metallic impurities, medicine.drug
Abstract

A facile and cost-effective method to prepare paramagnetic-metal free graphene nanosheets based on stannous chloride reduction of graphene oxide (GO) in a strongly acidic medium is reported. Simultaneous exfoliation and reduction is achieved in this room temperature process. Compared to the chemical reduction of GO using hydrazine or iron, the present method showed that Sn–rGO is several orders of magnitude less magnetic and hence does not contain any paramagnetic metallic impurities. With high reduction degree, this simple method shows promising application in energy and magnetic related studies.

Published
2013

16. Designing 3D Multihierarchical Heteronanostructures for High-Performance On-Chip Hybrid Supercapacitors: Poly(3,4-(ethylenedioxy)thiophene)-Coated Diamond/Silicon Nanowire Electrodes in an Aprotic Ionic Liquid

Author

Fang Gao, Georgia Lewes-Malandrakis, Maxime Boniface, Gérard Bidan, Thomas J. S. Schubert, Dmitry Aldakov, Boyan Iliev, David Aradilla, W. Müller-Sebert, Christoph E. Nebel, Pascal Gentile, Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Nanostructures et Magnétisme (NM), Service de Physique des Matériaux et Microstructures (SP2M - UMR 9002), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Fraunhofer Institute for Applied Solid State Physics (Fraunhofer IAF), Fraunhofer (Fraunhofer-Gesellschaft), Ionic Liquids Technologies GmbH (IOLITECH), European Project: 0243492(2003), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut Nanosciences et Cryogénie (INAC), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), and Publica

Subjects
Materials science, Inorganic chemistry, Nanowire, Ionic Liquids, Micro-Supercapacitors, 02 engineering and technology, 010402 general chemistry, High-Energy Density, 01 natural sciences, 7. Clean energy, Capacitance, Conducting Polymers, chemistry.chemical_compound, PEDOT:PSS, Supercapacitors, High-Power, General Materials Science, supercapacitor, Porous Carbon Electrodes, Ethylenedioxy, Conductive polymer, Supercapacitor, [PHYS]Physics [physics], Silicon Nanowires, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Chemical engineering, chemistry, Electrode, Ionic liquid, Doped Silicon Nanowires, Diamond, 0210 nano-technology, Carbide Nanowires
Abstract

International audience; A versatile and robust hierarchically multifunctionalized nanostructured material made of poly(3,4-(ethylenedioxy)thiophene) (PEDOT)-coated diamond@silicon nanowires has been demonstrated to be an excellent capacitive electrode for supercapacitor devices. Thus, the electrochemical deposition of nanometric PEDOT films on diamond-coated silicon nanowire (SiNW) electrodes using N-methyl-N-propylpyrrolidinium bis((trifluoromethyl)sulfonyl)imide ionic liquid displayed a specific capacitance value of 140 F g(-1) at a scan rate of 1 mV s(-1). The as-grown functionalized electrodes were evaluated in a symmetric planar microsupercapacitor using butyltrimethylammonium bis((trifluoromethyl)sulfonypimide aprotic ionic liquid as the electrolyte. The device exhibited extraordinary energy and power density values of 26 mJ cm(-2) and 1.3 mW cm(-2) within a large voltage cell of 2.5 V, respectively. In addition, the system was able to retain 80% of its initial capacitance after 15 000 galvanostatic charge-discharge cycles at a high current density of 1 mA cm(-2) while maintaining a Coulombic efficiency around 100%. Therefore, this multifunctionalized hybrid device represents one of the best electrochemical performances concerning coated SiNW electrodes for a high-energy advanced on-chip supercapacitor.

Published
2016

17. Silicon nanowires and nanotrees: elaboration and optimization of new 3D architectures for high performance on-chip supercapacitors

Author

Dorian Gaboriau, Thierry Brousse, Gérard Bidan, J. Le Bideau, Pascal Gentile, David Aradilla, Mylène Brachet, Saïd Sadki, Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), 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)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), ANR-12-BS09-0032,ISICAP,Supercondensateurs à base de Nanostructures de Si(2012), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), 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), and Université de Nantes (UN)-Université de Nantes (UN)

Subjects
Supercapacitor, Materials science, Nanostructure, Silicon, business.industry, General Chemical Engineering, Doping, chemistry.chemical_element, Nanotechnology, 02 engineering and technology, General Chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Energy storage, 0104 chemical sciences, chemistry, Electrode, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Microelectronics, 0210 nano-technology, business, ComputingMilieux_MISCELLANEOUS, Electrochemical window
Abstract

Micro-supercapacitors are increasingly foreseen as future energy storage or power buffer solutions for small scale integration on-chip. However, widely used electrode materials or electrolytes often proved to be incompatible with microelectronics processes. Although being the material of choice for on-chip integration, nanostructured silicon electrodes only recently caught attention for potential applications, and they displayed promising results especially for bottom-up silicon nanostructures, where the design liberty and fine control of nanostructure morphologies allow considerable improvements. The present work deals with the optimization of highly doped silicon nanowires (Si-NWs) and nanotrees (Si-NTrs) pioneered in the laboratory using an innovative, fast and efficient electroless gold deposition method in order to explore a wide variety of 3D architectures and their physicochemical properties. Through a systematic study of branches and trunks morphologies, the nature inspired nanotrees have been drastically improved compared to previously published works, resulting in excellent electrode properties, showing high energy and power densities, respectively, up to 2.8 mJ cm−2 and 235 mW cm−2. In addition, a cyclability of over a million charge–discharge galvanostatic cycles was determined using an enlarged electrochemical window of 4 V in an ionic liquid electrolyte.

Published
2016

18. Solder-reflow resistant solid-state micro-supercapacitors based on ionogels

Author

Dorian Gaboriau, Sébastien Fantini, Jean Le Bideau, Gérard Bidan, Mylène Brachet, Pascal Gentile, Thierry Brousse, Saïd Sadki, 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), Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Solvionic (FRANCE), ANR-12-BS09-0032,ISICAP,Supercondensateurs à base de Nanostructures de Si(2012), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG)

Subjects
Materials science, Fabrication, Silicon, chemistry.chemical_element, Nanotechnology, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Reflow soldering, Microelectronics, General Materials Science, ComputingMilieux_MISCELLANEOUS, Supercapacitor, Renewable Energy, Sustainability and the Environment, business.industry, General Chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, chemistry, Soldering, Ionic liquid, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Wetting, 0210 nano-technology, business
Abstract

All-solid-state devices and thermal resistance to solder reflow are crucial issues with respect to micro-supercapacitors. While the latter issue can be addressed by using ionic liquids, the former shows promising results by employing the ionogel approach. The present study focuses on a novel formulation of ionogels—for use as solid state electrolytes in micro-supercapacitors with silicon nanowire electrodes—which promotes the crack-free formation of an efficient solid electrolyte onto silicon nanostructures in a single-step sol–gel process. The capacitance obtained was the same as that for a device using a non-confined ionic liquid, showing a good wetting of the 3D nanostructured silicon electrodes by the sol precursor of the solid ionogel. The assembled symmetric micro-supercapacitor exhibits very high cycling stability and can sustain the reflow soldering process used in the fabrication of microelectronic devices without compromising their electrochemical performance, and even improving their frequency response.

Published
2016

19. Organosilyl/-germyl Polyoxotungstate Hybrids for Covalent Grafting onto Silicon Surfaces: Towards Molecular Memories

Author

Guillaume Delapierre, Gérard Bidan, Nicoleta Joo, Séverine Renaudineau, Lise-Marie Chamoreau, Anna Proust, Pierre Gouzerh, and René Thouvenot

Subjects
Silicon, Organic Chemistry, Inorganic chemistry, chemistry.chemical_element, General Chemistry, Crystal structure, Nuclear magnetic resonance spectroscopy, Electrochemistry, Grafting, Triple bond, Catalysis, Crystallography, chemistry, Covalent bond, Cyclic voltammetry
Abstract

Organosilyl/-germyl polyoxotungstate hybrids [PW(9)O(34)(tBuSiO)(3)Ge(CH(2))(2)CO(2)H](3-) (1a), [PW(9)O(34)(tBuSiO)(3)Ge(CH(2))(2)CONHCH(2)C[triple bond]CH](3-) (2 a), [PW(11)O(39)Ge(CH(2))(2)CO(2)H](4-) (3a), and [PW(11)O(39)Ge(CH(2))(2)CONHCH(2)C[triple bond]CH](4-) (4a) have been prepared as tetrabutylammonium salts and characterized in solution by multinuclear NMR spectroscopy. The crystal structure of (NBu(4))(3)1a.H(2)O has been determined and the electrochemical behavior of 1a and 2a has been investigated by cyclic voltammetry. Covalent grafting of 2a onto an n-type silicon wafer has been achieved and the electrochemical behavior of the grafted clusters has been investigated. This represents the first example of covalent grafting of Keggin-type clusters onto a Si surface and a step towards the realization of POM-based multilevel memory devices.

Published
2010

20. Electrochemical signature of the grafting of diazonium salts: A probing parameter for monitoring the electro-addressed functionalization of devices

Author

Fabien Le Floch, Gérard Bidan, and Jean-Pierre Simonato

Subjects
chemistry.chemical_classification, Tetrafluoroborate, Diazonium Compounds, General Chemical Engineering, Aryl, Inorganic chemistry, Substituent, Photochemistry, Electrochemistry, chemistry.chemical_compound, chemistry, Polar effect, Surface modification, Reactivity (chemistry)
Abstract

The reciprocal influence of the phenylsubstituents and diazonium groups allows to monitor the diazonium reactivity and to electrochemically detect the grafting reaction. Extended understanding concerning the grafting of para substituted tetrafluoroborate aryl diazonium salts p-(R–Ph–N2+, BF4−) was obtained by studying comparatively four compounds (R = NO2, NEt2, NHPh, NPh2) by electrochemistry. For R = NEt2, the grafted molecules showed no reversible electroactivity whereas for the aminophenyl substituents, the first oxidation process induced chemical modification of the deposited layers before being totally reversible. The compound with electron withdrawing group (NO2) was the only one able to create spontaneous covalent bounding with the glassy carbon electrode (GCE). We observed that the substituent directly acts upon the diazonium reactivity. This effect can be directly monitored through the potential onset value of the diazonium reduction. In addition, the elimination of the diazonium group during electrografting induces a cathodic shift of the electroactivity of the aminodiphenyl and aminotriphenyl groups covalently attached onto the carbon electrode surface. The shift between these electrochemical values may be considered as a signature of the grafting reaction.

Published
2009

21. 3D hierarchical assembly of ultrathin MnO2 nanoflakes on silicon nanowires for high performance micro-supercapacitors in Li- doped ionic liquid

Author

Pascal Gentile, Pedro Gómez-Romero, David Aradilla, Jan Wimberg, Saïd Sadki, Gérard Bidan, Deepak P. Dubal, Thomas J. S. Schubert, ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Universitat Autònoma de Barcelona (UAB), Polymères Conducteurs Ioniques (PCI), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), European Project: 309143,EC:FP7:ENERGY,FP7-ENERGY-2012-1-2STAGE,NEST(2012), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Silicon, Materials science, Nanowire, chemistry.chemical_element, Energy-Storage, Nanotechnology, Electrolyte, All-Solid-State, Electrochemical Capacitors, 7. Clean energy, Article, Wafer, Fiber, Electrodes, Films, [PHYS]Physics [physics], Supercapacitor, Multidisciplinary, Doping, Oxide, Conversion, Carbon, Porous, chemistry, Electrode, Mesoporous material
Abstract

Building of hierarchical core-shell hetero-structures is currently the subject of intensive research in the electrochemical field owing to its potential for making improved electrodes for high-performance micro-supercapacitors. Here we report a novel architecture design of hierarchical MnO2@silicon nanowires (MnO2@SiNWs) hetero-structures directly supported onto silicon wafer coupled with Li-ion doped 1-Methyl-1-propylpyrrolidinium bis(trifluromethylsulfonyl)imide (PMPyrrBTA) ionic liquids as electrolyte for micro-supercapacitors. A unique 3D mesoporous MnO2@SiNWs in Li-ion doped IL electrolyte can be cycled reversibly across a voltage of 2.2 V and exhibits a high areal capacitance of 13 mFcm−2. The high conductivity of the SiNWs arrays combined with the large surface area of ultrathin MnO2 nanoflakes are responsible for the remarkable performance of these MnO2@SiNWs hetero-structures which exhibit high energy density and excellent cycling stability. This combination of hybrid electrode and hybrid electrolyte opens up a novel avenue to design electrode materials for high-performance micro-supercapacitors.

Published
2015

22. Diamond-coated silicon nanowires for enhanced micro-supercapacitor with ionic liquids

Author

Dorian Gaboriau, Pascal Gentile, Gérard Bidan, Jan Wimberg, W. Mueller-Sebert, Pedro Gómez-Romero, Thomas J. S. Schubert, Girish S. Gund, Deepak P. Dubal, David Aradilla, and Saïd Sadki

Subjects
Supercapacitor, Fabrication, business.industry, Diamond, Chemical vapor deposition, engineering.material, chemistry.chemical_compound, Coating, chemistry, Electrode, Ionic liquid, engineering, Optoelectronics, Wafer, business
Abstract

Silicon nanowires (SiNWs) and diamond-coated SiNWs (D@SiNWs) on highly n-doped silicon wafer substrates were prepared through standard chemical vapor deposition (CVD) method as electrodes for micro-supercapacitors. The surface of electrodes exhibited uniform distribution of SiNWs on silicon wafer and continuous diamond coating on SiNWs. Electrochemical measurements were carried out in order to test the combined effect of using Ionic Liquid electrolytes and diamond coating on SiNWs on energy storage performance. Optimal values of areal capacitance, energy density and power densities were 317 µF cm−2, 0.13 µWh cm−2 and 150 µW cm−2, respectively. So, the work reported here confirms the suitability and compatibility of D@SiNWs electrode materials and ionic liquid electrolytes for the fabrication of high-performing and robust micro-supercapacitors.

Published
2015

23. Vertically aligned graphene nanosheets on silicon using an ionic liquid electrolyte: towards high performance on-chip micro-supercapacitors

Author

Gérard Bidan, Marc Delaunay, Saïd Sadki, Jean-Michel Gérard, David Aradilla, Polymères Conducteurs Ioniques (PCI), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Nanophysique et Semiconducteurs (NPSC), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Silicon, chemistry.chemical_element, Double-Layer Capacitor, Density, Nanotechnology, Energy-Storage, 02 engineering and technology, Electrolyte, 010402 general chemistry, Electrochemistry, 7. Clean energy, 01 natural sciences, Capacitance, Electrochemical Capacitors, law.invention, chemistry.chemical_compound, Fabrication, law, High-Power, General Materials Science, Operation, Supercapacitor, [PHYS]Physics [physics], Renewable Energy, Sustainability and the Environment, business.industry, Graphene, Raman-Spectroscopy, General Chemistry, 021001 nanoscience & nanotechnology, Carbon, 0104 chemical sciences, chemistry, Ionic liquid, Optoelectronics, 0210 nano-technology, business, Current density, Carbide Nanowires
Abstract

International audience; Vertically oriented graphene nanosheets were synthesized by an alternative and simple approach based on electron cyclotron resonance-plasma enhanced chemical vapor deposition (ECR-CVD) onto highly doped silicon substrates. The as-grown graphene electrodes were employed in a symmetric micro-supercapacitor using an aprotic ionic liquid [N-methyl-N-propylpyrrolidinium bis(trifluoromethyl-sulfonylimide); PYR13TFSI] as electrolyte. The device was able to deliver an outstanding specific capacitance value of 2 mF cm(-2), a power density value of 4 mW cm(-2) and an energy density value of 4 mu W h cm(-2) operating at a large and stable cell voltage of 4 V with a quasi-ideal capacitive behaviour. Moreover, the lifetime of the device exhibited a remarkable electrochemical stability retaining 80% of the initial capacitance after 150 000 galvanostatic charge-discharge cycles at a high current density of 1 mA cm(-2). This excellent electrochemical performance results from the obtained channel-based 3-D graphene network promoting rapid electrolyte ion-transport and short diffusion paths.

Published
2015

24. An innovative 3-D nanoforest heterostructure made of polypyrrole coated silicon nanotrees for new high performance hybrid micro-supercapacitors

Author

Pedro Gómez-Romero, Gérard Bidan, Pascal Gentile, Jan Wimberg, Saïd Sadki, Maxime Boniface, Deepak P. Dubal, Thomas J. S. Schubert, Dorian Gaboriau, David Aradilla, Polymères Conducteurs Ioniques (PCI), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Laboratoire d'Etude des Matériaux par Microscopie Avancée (LEMMA ), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Universitat Autònoma de Barcelona (UAB), European Project: 309143,EC:FP7:ENERGY,FP7-ENERGY-2012-1-2STAGE,NEST(2012), European Commission, Commissariat à l'Ènergie Atomique et aux Ènergies Alternatives (France), Ministère de la Défense (France), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG)

Subjects
Materials science, Silicon, Electrochemical Energy-Storage, chemistry.chemical_element, 02 engineering and technology, Chemical vapor deposition, Capacitors, 010402 general chemistry, Polypyrrole, Electrochemistry, 7. Clean energy, 01 natural sciences, Capacitance, chemistry.chemical_compound, Fabrication, Ultracapacitors, Devices, General Materials Science, Arrays, Electrodes, Films, Supercapacitor, Conductive polymer, [PHYS]Physics [physics], Renewable Energy, Sustainability and the Environment, Nanowires, General Chemistry, 021001 nanoscience & nanotechnology, Carbon, 0104 chemical sciences, chemistry, Chemical engineering, Electrode, 0210 nano-technology
Abstract

In this work, an innovative 3-D symmetric micro-supercapacitor based on polypyrrole (PPy) coated silicon nanotree (SiNTr) hybrid electrodes has been fabricated. First, SiNTrs were grown on silicon substrates by chemical vapor deposition (CVD) and then via an electrochemical method, the conducting polymer coating was deposited onto the surface of SiNTr electrodes. This study illustrates the excellent electrochemical performance of a hybrid micro-supercapacitor device using the synergistic combination of both PPy as the electroactive pseudo-capacitive material and branched SiNWs as the electric double layer capacitive material in the presence of an aprotic ionic liquid (N-methyl-N-propylpyrrolidinium bis(trifluoromethylsulfonyl)imide; PYR13TFSI) as the electrolyte. The hybrid device exhibited a specific capacitance as high as ∼14 mF cm−2 and an energy density value of ∼15 mJ cm−2 at a wide cell voltage of 1.5 V using a high current density of 1 mA cm−2. Furthermore, a remarkable cycling stability after thousands of galvanostatic charge–discharge cycles with a loss of approximately 30% was obtained. The results reported in this investigation demonstrated that PPy coated SiNTr-based micro-supercapacitors exhibit the best performances among hybrid micro-supercapacitors made of silicon nanowire electrodes grown by CVD in terms of specific capacitance and energy density., This project has received funding from the European Union's Seventh Program for Research, Technological Development and Demonstration under Grant agreement no. 309143 (2012–2015). Dorian Gaboriau thanks the 'Délégation Générale pour l'Armament' (DGA) and the CEA for financial support.

Published
2015

25. SiNWs-based electrochemical double layer micro-supercapacitors with wide voltage window (4V) and long cycling stability using a protic ionic liquid electrolyte

Author

Pedro Gómez-Romero, Thomas J. S. Schubert, Gérard Bidan, Saïd Sadki, Boyan Iliev, Pascal Gentile, David Aradilla, Vanesa Ruiz, Jan Wimberg, Polymères Conducteurs Ioniques (PCI), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Universitat Autònoma de Barcelona (UAB), Laboratoire d'Electronique Moléculaire Organique et Hybride (LEMOH), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), European Project: 309143,EC:FP7:ENERGY,FP7-ENERGY-2012-1-2STAGE,NEST(2012), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), and Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)

Subjects
Performance, Analytical chemistry, Ionic Liquids, Micro-Supercapacitors, Energy-Storage, Electrolyte, Capacitors, Electrochemistry, 7. Clean energy, Industrial and Manufacturing Engineering, chemistry.chemical_compound, Devices, General Materials Science, Electrical and Electronic Engineering, Deposition, Power density, Chemical Vapor, Supercapacitor, [PHYS]Physics [physics], Silicon Nanowires, Carbon, Dielectric spectroscopy, Surface, chemistry, Chemical engineering, Electrode, Ionic liquid, Doped Silicon Nanowires, Cyclic voltammetry
Abstract

International audience; The present work reports the use and application of a novel protic ionic liquid (triethylammonium bis(trifluoromethylsulfonyl)imide; NEt3H TFSI) as an electrolyte for symmetric planar micro-supercapacitors based on silicon nanowire electrodes. The excellent performance of the device has been successfully demonstrated using cyclic voltammetry, galvanostatic charge-discharge cycles and electrochemical impedance spectroscopy. The electrochemical characterization of this system exhibits a wide operative voltage of 4 V as well as an outstanding long cycling stability after millions of galvanostatic cycles at a high current density of 2 mA cm(-2). In addition, the electrochemical double layer micro-supercapacitor was able to deliver a high power density of 4 mW cm(-2) in a very short time pulses (a few ms). Our results could be of interest to develop prospective on-chip micro-supercapacitors using protic ionic liquids as electrolytes with high performance in terms of power and energy densities.

Published
2015

26. State of partial oxidation of the regioregular sexi (3-octyl thiophene) oligomer in solid phase on electrode surface

Author

Jerzy Zak, S. Guillerez, Gérard Bidan, and Mieczyslaw Lapkowski

Subjects
Materials science, Formal charge, Condensed Matter Physics, Photochemistry, Electrochemistry, Oligomer, Redox, chemistry.chemical_compound, chemistry, Phase (matter), Electrode, Thiophene, Molecule, General Materials Science, Electrical and Electronic Engineering
Abstract

An existence of a new, stable oligomer state of the solid film is reported, which is produced under electrochemical conditions. In this state, a formal charge exchanged in the redox process is about one-half of electron per oligomer molecule. The procedure, which allows controlling precisely the amount of oligomer on the electrode surface, is proposed that together with the coulometric evaluation of the electric charge provides the number of electrons involved in a redox process. This is demonstrated for a case of α-monochloro-substituted regioregular sexi (3-octylthiophene) oligomer (6OTCl). The electrochemical results are discussed together with UV–Vis–NIR spectroelectrochemical data obtained for both solution and solid phase that support the proposed interpretation.

Published
2005

27. Electrochemistry and spectroelectrochemistry of regioregular oligooctylthiophenes

Author

Mieczyslaw Lapkowski, Gérard Bidan, Jerzy Zak, and S. Guillerez

Subjects
Mechanical Engineering, Metals and Alloys, Condensed Matter Physics, Electrochemistry, Photochemistry, Redox, Electronic, Optical and Magnetic Materials, Dication, chemistry.chemical_compound, End-group, chemistry, Radical ion, Tetramer, Mechanics of Materials, Functional group, Polymer chemistry, Materials Chemistry, Thiophene
Abstract

In this work we report on the electrochemical and spectroelectrochemical characterization of the series of α-monochloro substituted regioregular 3-alkylthiophene consisting of 4–8 units of (3-octylthiophene) in solution. The shortest in the series tetramer molecules undergo a fast dimerization process, whereas longer oligomers are not subject to consecutive reactions when oxidized to form the radical cation. Each oxidation stage corresponds to one-electron process; single radical cation and dication are initially produced, which in turn are doubled within each oligomer molecule. Studies of these compounds in solution species were carried out in the thin layer cell on optically transparent electrodes. Clear tendencies are observed with increasing number of thiophene units for the peak potential of the redox reactions and positions of maximum absorbance. Formation of additional electronic bands within the band gap, shifted to the lower energies, has been also observed.

Published
2005

28. Electrochemical study by a redox probe of the chemical post-functionalization of N-substituted polypyrrole films: Application of a new approach to immobilization of biotinylated molecules

Author

B. Ehui-Avo Bile, M.-L. Calvo-Muñoz, Gérard Bidan, and Martial Billon

Subjects
Fluorophore, General Chemical Engineering, Polypyrrole, Analytical Chemistry, chemistry.chemical_compound, Monomer, chemistry, Ferrocene, Polymer chemistry, Electrochemistry, Molecule, Surface modification, Cyclic voltammetry, Pyrrole
Abstract

In order to study the post-polymerization functionalization of a poly(N-substituted pyrrole) film, the β-ferrocene ethylamine used as redox probe has been immobilized via a chemical coupling on the surface of a preformed polypyrrole film bearing activated ester groups. From the electrochemical response of the anchored ferrocene units, the post-polymerization functionalization efficiency has been evaluated to be 20–22%. This level is the same whatever the length of spacer arm (2, 5 and 12 carbons) linking the activated ester groups to the polypyrrole backbone and the hydrophilic and hydrophobic nature of this polymer. Using a similar strategy based on this chemical grafting, we have developed a new approach to the immobilization of biotin entities onto the ester activated-polypyrrole film surface. From fluorescence measurements, it appears that the anchoring of streptavidine bearing a fluorophore (streptavidin-R-phycoerythrin, SAPE) on this biotinylated polypyrrole film gives a fluorescence intensity similar to the one achieved from the immobilization of SAPE onto a film electrosynthesized from pyrrole monomers bearing biotin units. Thus, this result shows the efficiency of this new functionalization method for attaching biotinylated entities.

Published
2005

29. Investigation by QCM of the Specific and Nonspecific Avidin Interaction onto a Biotinylated Polypyrrole Film

Author

A. Dupont-Filliard, Gérard Bidan, S. Guillerez, and Martial Billon

Subjects
chemistry.chemical_classification, Chromatography, biology, Quartz crystal microbalance, Polymer, respiratory system, Polypyrrole, Analytical Chemistry, chemistry.chemical_compound, Adsorption, chemistry, Chemical engineering, Biotin, Biotinylation, Electrochemistry, biology.protein, Gravimetric analysis, Avidin
Abstract

We have studied by gravimetric measurements using a quartz crystal microbalance (QCM), the adsorption of avidin onto a polypyrrole film. From QCM results, it appears that both the thickness and the redox state of polypyrrole strongly influence the avidin adsorption. This nonspecific interaction is larger for a thick film than for a thin one and, also for when the polymer is in its reduced state. We have also investigated by QCM the specific and nonspecific interaction of avidin onto biotinylated polypyrrole films having either a hydrophilic or hydrophobic character. It is shown that the amount of avidin immobilized by specific recognition is almost the same whatever the nature of the polymer matrix.

Published
2004

30. Bio-Assemblies onto Conducting Polymer Support: Implementation of DNA-Chips

Author

M. Billon, A. Dupont-Fillard, M.-L. Calvo-Muñoz, and Gérard Bidan

Subjects
Conductive polymer, Materials science, Oligonucleotide, Nanotechnology, General Chemistry, Condensed Matter Physics, Polypyrrole, Luminol, Microelectrode, chemistry.chemical_compound, chemistry, Electrochemiluminescence, Surface modification, General Materials Science, Biosensor
Abstract

The electrical deposition(electropolymerization)of polypyrrole, PPy, grafted by different ODN probes is the key to construct oligonucleotides, ODN, arrays on silicon devices bearing a matrix of gold microelectrodes. The straightforward functionalization of PPy allows finalizing a more general grafting based on affinity interactions between a biotinylated polypyrrole support and the biological probe and results in a surface renewable DNA sensor. The electrical monitoring of the thickness of the PPy deposit at the nanometer range allows the real time monitoring of the biological interactions using Surface Plasmon Resonance imaging. Recently, the electroconductivity of the PPy was exploited to trigger the electrochemiluminescence of a DNA sequence labelled with a luminol derivative, ABEI.

Published
2004

31. Transition-metal-templated synthesis of rotaxanes and catenanes: From small molecules to polymers

Author

Gérard Bidan, B. Divisia-Blohorn, Jean-Marc Kern, and Jean-Pierre Sauvage

Subjects
Conductive polymer, chemistry.chemical_classification, Materials science, Polymers and Plastics, Organic Chemistry, Catenane, Nanotechnology, Polymer, Small molecule, Transmetalation, Template, Transition metal, chemistry, Materials Chemistry
Abstract

This article provides an overview of the fundamental principles of the synthesis of metallocatenanes and metallorotaxanes. It also describes the synthesis and properties of electronic conducting polymers-polypyrrole and polythiophene-built around metallocatenanes and metallorotaxanes. The particular properties of this new class of polymers, including the possibility of transmetallation reactions being performed with them and the observation of electronic coupling between the metal centers and the conducting matrix, are discussed.

Published
2003

32. Electrochemical studies of selected regioregular oligooctylthiophenes in solution and in thin film solid state

Author

Wojciech Domagala, Gérard Bidan, Mieczyslaw Lapkowski, and S. Guillerez

Subjects
chemistry.chemical_compound, Radical ion, chemistry, Transition metal, General Chemical Engineering, Electrochemistry, Thiophene, Molecule, Thin film, Photochemistry, Oligomer, Redox
Abstract

Electrochemical studies of a series of regioregular 3-octylthiophene oligomers with 5–8 thiophene rings, chlorine end-capped at one α terminal position, have been conducted in solution and in thin film state. Results indicate gradual coalescing of the oxidation potentials of neutral and radical cation oligomer molecule, indicative of coming close to sufficient length of the molecule to allow for two separate radical cations to exist along its chain. With increasing number of thiophene rings in the molecule, further quasi-reversible oxidation reactions upon which trication and tetracation were formed have been observed at ever decreasing potentials. It was also observed that the oxidation of radical cations comes about more easily than that of electron-paired cations, the latter process being strongly dependent on the length of oligothiophene chain. Thin film electrochemistry revealed that the processes taking place during redox reactions differ from those in solution. Sharp oxidation peaks were observed which were attributed to conformational changes taking place in the oligomer molecules upon transition to the conductive form, alongside the film's oxidative doping process. To shed some light on the issue of charge carriers appearing in the film upon its oxidation, supplemental ESR spectroelectrochemical measurements were carried out and confirmed that, radical cations are generated in the film.

Published
2003

33. Conjugated Polymetallorotaxanes: In-Situ ESR and Conductivity Investigations of Metal−Backbone Interactions

Author

Caroline Borel, § and Jean-Marc Kern, Gérard Bidan, B. Divisia-Blohorn, F. Genoud, and Jean-Pierre Sauvage

Subjects
Inorganic chemistry, chemistry.chemical_element, Zinc, Electrochemistry, Copper, Redox, Surfaces, Coatings and Films, Metal, Crystallography, chemistry, Standard electrode potential, visual_art, Materials Chemistry, visual_art.visual_art_medium, Lithium, Physical and Theoretical Chemistry, Cobalt
Abstract

Electrochemical studies of polymetallorotaxane films of a general formula poly[1,3,Mn+] where Mn+ is copper(I), cobalt(II), zinc(II), or lithium(I) are reported for both metalated and demetalated (poly[1,3,-]) forms. Cyclic voltammograms (CV) recorded for polymetallorotaxanes containing redox-active metals, with an exception of the Li one, in addition to the electroactivity of the complexing metal exhibit two redox couples associated with the consecutive oxidation/reduction of the oligothienylene units in the wiring polymer. For poly[1,3,Cu+], the CV studies are completed by ESR spectroelectrochemical investigations combined with in-situ conductivity measurements as a function of the electrode potentials. In the ESR response, two signals of different origin can be distinguished: a broad signal originating from Cu(II) paramagnetics ions (ΔHpp of ca. 265 G) and that due to unpaired spins of the polymer backbone (ΔHpp of ca. 21 G). Potential dependencies of these two signals as well as potential-induced con...

Published
2003

34. Conjugated polyrotaxanes: improvement of the polymer properties by using sterically hindered coordinating units

Author

Jean-Marc Kern, Gérard Bidan, Jean-Pierre Sauvage, B. Divisia-Blohorn, and Pierre-Louis Vidal

Subjects
chemistry.chemical_classification, Steric effects, chemistry.chemical_element, General Chemistry, Polymer, Conjugated system, Electrochemistry, Copper, Catalysis, Metal, chemistry.chemical_compound, chemistry, visual_art, Polymer chemistry, Materials Chemistry, Thiophene, visual_art.visual_art_medium, Derivative (chemistry)
Abstract

A new conjugated copper-complexed polyrotaxane has been prepared by electropolymerization of a thiophene derivative; the rings are threaded onto a multi-1,10-phenanthroline (phen) axle, copper(I) acting as a template. The presence of CH3 groups ortho to the nitrogen atoms of the phen nuclei belonging to the conjugated backbone has a profound effect on the stability of the polymer, on its electrochemical properties and on its ability to be remetallated once the template metal centre (copper(I)) has been removed.

Published
2002

35. Tuning silicon nanowires doping level and morphology for highly efficient micro-supercapacitors

Author

Gérard Bidan, Saïd Sadki, Nicolas Pauc, Pascal Gentile, Thierry Brousse, Fleur Thissandier, Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Institut Nanosciences et Cryogénie (INAC), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), 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), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), and Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS.PHYS.PHYS-OPTICS]Physics [physics]/Physics [physics]/Optics [physics.optics], Materials science, Silicon, Renewable Energy, Sustainability and the Environment, Doping, chemistry.chemical_element, Nanotechnology, Chemical vapor deposition, Capacitance, Dielectric spectroscopy, chemistry, [PHYS.QPHY]Physics [physics]/Quantum Physics [quant-ph], Electrode, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [SPI.OPTI]Engineering Sciences [physics]/Optics / Photonic, General Materials Science, Wafer, Electrical and Electronic Engineering, Cyclic voltammetry, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS
Abstract

Silicon nanowires (SiNWs) are grown by Chemical Vapor Deposition on highly doped silicon wafer via localized gold catalysis with monitored length, diameter, density and doping level. This work highlights the influence of SiNWs morphological characteristics on their electrochemical performances and analyses in details the key role of the doping level for exhibiting a typical double layer capacitive behavior. The electrochemical performances of silicon and SiNWs electrodes are evaluated in an organic electrolyte by electrochemical impedance spectroscopy and cyclic voltammetry. Electrode capacitance has been improved up to 440 µF cm−2, i.e. about 75 fold that of bulk and about 10 fold that of the one previously reported.

Published
2014

36. Ultra-dense and highly doped SiNWs for micro-supercapacitors electrodes

Author

Denis Buttard, Fleur Thissandier, Gérard Bidan, Saïd Sadki, Pascal Gentile, Thierry Brousse, Ludovic Dupré, Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Institut Nanosciences et Cryogénie (INAC), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), 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), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), and Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Nanoporous, micro-supercapacitors, General Chemical Engineering, Doping, Nanowire, Nanotechnology, Porous alumina, Electrolyte, CVD, 7. Clean energy, Capacitance, Nanowire battery, Anode, law.invention, silicon nanowires, law, Electrode, Electrochemistry, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], ionic liquid
Abstract

International audience; The use of nanoporous anodic alumina as a template for silicon nanowire growth enables the production of ultra dense nanowire arrays with density up to 8.109cm(-2). The integration of such nanowire arrays in micro-supercapacitor electrodes significantly improves the electrode capacitance per planar surface area and nanowires length unit compared to electrodes made from silicon nanowires grown from gold colloids (from 5.2 mu F.cm(-2).mu m to 36.7 mu F.cm(-2).mu m). Micro-supercapacitors with such electrodes and ionic liquid as electrolyte have a very promising cycling stability featuring less than 1% of losses after 300000 cycles. (C) 2013 Elsevier Ltd. All rights reserved.

Published
2014

37. Novel hybrid micro-supercapacitor based on conducting polymer coated silicon nanowires for electrochemical energy storage

Author

Gérard Bidan, Hülya Sahin, Pascal Gentile, Vanesa Ruiz, Patrick Weathers, Thomas J. S. Schubert, Pedro Gómez-Romero, Saïd Sadki, Fleur Thissandier, David Aradilla, Polymères Conducteurs Ioniques (PCI), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Service de Chimie Inorganique et Biologique (SCIB - UMR E3), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Centre National de la Recherche Scientifique (CNRS), Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Universitat Autònoma de Barcelona (UAB), Institut de Ciència de Materials de Barcelona (ICMAB), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Ionic Liquids Technologies GmbH (IOLITECH), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), European Commission, and Commissariat à l'Ènergie Atomique et aux Ènergies Alternatives (France)

Subjects
Materials science, General Chemical Engineering, Nanotechnology, 02 engineering and technology, Electrolyte, engineering.material, 010402 general chemistry, Electrochemistry, 01 natural sciences, 7. Clean energy, Capacitance, [SPI]Engineering Sciences [physics], Coating, Specific energy, [CHIM]Chemical Sciences, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS, Power density, Supercapacitor, Conductive polymer, [SPI.NRJ]Engineering Sciences [physics]/Electric power, General Chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Chemical engineering, engineering, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology
Abstract

The development of a novel hybrid symmetric micro-supercapacitor based on poly(3,4-ethylenedioxythiophene) coated silicon nanowires using an ionic liquid (N-methyl-N-propylpyrrolidinium bis(trifluoromethylsulfonyl)imide) as an electrolyte has been demonstrated. The hybrid supercapacitor device was able to deliver a specific energy of 10 W h kg-1 and a maximal power density of 85 kW kg-1 at a cell voltage of 1.5 V. The hybrid device exhibited long lifetime and an outstanding electrochemical stability retaining 80% of the initial capacitance after thousands of galvanostatic charge-discharge cycles at a high current density of 1 mA cm-2. The improvement of the capacitive properties compared with the bare SiNWs was attributed to the pseudo-capacitive behavior induced by the conducting polymer coating., The authors acknowledge the CEA for financial support of this work. This project has received funding from the European Union's Seventh Programme for research, technological development and demonstration under grant agreement no. 309143 (2012–2015).

Published
2014

38. High performance of symmetric micro-supercapacitors based on silicon nanowires using N-methyl-N-propylpyrrolidinium bis(trifluoromethylsulfonyl)imide as electrolyte

Author

Gérard Bidan, Pascal Gentile, Elzbieta Frackowiak, Pedro Gómez-Romero, Vanesa Ruiz, Hülya Sahin, Saïd Sadki, Thomas J. S. Schubert, David Aradilla, Commissariat à l'Ènergie Atomique et aux Ènergies Alternatives (France), European Commission, Silicon Nanoelectronics Photonics and Structures (SiNaps), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Universitat Autònoma de Barcelona (UAB), Faculty of Chemical Technology, Poznan University of Technology (PUT), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Chemical vapour deposition, Materials science, Silicon, micro-supercapacitors, Micro-supercapacitors, Inorganic chemistry, chemistry.chemical_element, 02 engineering and technology, Chemical vapor deposition, Electrolyte, 010402 general chemistry, Electrochemistry, 01 natural sciences, 7. Clean energy, Capacitance, chemical vapor deposition, ionic liquids, chemistry.chemical_compound, Silicon nanowires, General Materials Science, Electrical and Electronic Engineering, Supercapacitor, Renewable Energy, Sustainability and the Environment, electrochemical energy storage, [SPI.NRJ]Engineering Sciences [physics]/Electric power, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Ionic liquids, Chemical engineering, chemistry, Ionic liquid, Electrochemical energy storage, 0210 nano-technology, Faraday efficiency
Abstract

This work describes the development and performance of a symmetric micro-supercapacitor made of nanostructured electrodes based on silicon nanowires (SiNWs) deposited using chemical vapor deposition (CVD) on silicon substrates. The performance of the SiNWs micro-supercapacitor employing an aprotic ionic liquid (N-methyl-N-propylpyrrolidinium bis(trifluoromethylsulfonyl)imide) (PYR13TFSI) as an electrolyte was able to deliver a maximal power density of 182mWcm-2 and a specific energy of 190μJcm-2 operating at a wide cell voltage of 4V with a quasi-ideal capacitive behavior. The lifetime of the device exhibited a remarkable electrochemical stability retaining 75% of the initial capacitance after several million galvanostatic charge-discharge cycles at a high current density of 1mAcm-2. Furthermore, a coulombic efficiency of approximately 99% was obtained after galvanostatic cycling test without structural degradation on the morphology of SiNWs., The authors acknowledge the CEA for financial support of this work. This project has received funding from the European Union׳s Seventh Program for Research, Technological Development and Demonstration under Grant agreement no. 309143 (2012–2015).

Published
2014

39. Comparison by QCM and photometric enzymatic test of the biotin-avidin recognition on a biotinylated polypyrrole

Author

Martial Billon, A. Dupont-Filliard, Gérard Bidan, and S. Guillerez

Subjects
Chromatography, biology, Quartz crystal microbalance, respiratory system, Polypyrrole, Analytical Chemistry, chemistry.chemical_compound, Biotin, chemistry, Biotinylation, Monolayer, biology.protein, Glucose oxidase, Biosensor, Avidin
Abstract

By gravimetric measurements using a quartz cristal microbalance (QCM), we have studied the immobilization of biotinylated glucose oxidase enzymes (B-GOx) bound through on an intermediate avidin layer to a biotinylated polypyrrole film. The aim is to assess the amount of B-GOx specifically anchored on the biotinylated polypyrrole/avidin assembly thank to the biotin/avidin interaction between avidin and B-GOx. Indeed the estimated amount from the QCM measurement corresponds to the specific recognition of avidin/B-GOx added to a non-specific recognition (adsorption) of B-GOx. In order to discriminate these two phenomena, we have carried out a study by QCM of the anchoring of B-GOx on an avidin layer linked by adsorption to a polypyrrole free from biotin units. From QCM measurements we have deduced for the biotinylated polypyrrole/avidin assembly that the amount of B-GOx bound via the biotin/avidin interaction and those due to the avidin adsorption process correspond to 3.9 pmol cm−2 (1.3 equivalent of B-Gox monolayer) and 1.4 pmol cm−2 (0.46 equivalent of B-GOx monolayer) respectively. These values have been corroborated by measurements of the enzymatic activity of GOx.

Published
2001

40. Effects of the redox state on the morphology of the regioregular sexi-3-alkylthiophene

Author

Mieczysław Łapkowski, M. Kolodziej-Sadlok, Jerzy Zak, S. Guillerez, and Gérard Bidan

Subjects
Transition metal, Chemistry, General Chemical Engineering, Phase (matter), Inorganic chemistry, Electrochemistry, Electrolyte, Cyclic voltammetry, Thin film, Photochemistry, Voltammetry, Redox
Abstract

The electrochemical properties of solid phase α-monochloro substituted regioregular 3-alkylthiophene consisting of six units of 3-octylthiophene (6OT) were studied in nonaqueous electrolyte solutions using cyclic voltammetry and electrochemical atomic force microscopy (EC AFM). As confirmed by voltammetry, the 6OT molecules in an oxidized form of monocation radical are not subject to consecutive reactions, due to the presence of the α-substituent. In situ AFM images of the thin films of 6OT cast on metal substrates revealed reversible, drastic changes of the film morphology while applied potential was switched between values corresponding to the particular redox state. Dimerization of the oligomers and π-stacks formation is postulated to explain the observed morphology changes in the 6OT films.

Published
2001

42. Immobilization of a Series of Dawson Type Heteropolyanions

Author

Timothy McCormac, Dennis Drennan, David Farrell, and Gérard Bidan

Subjects
Conductive polymer, endocrine system, Chemistry, Inorganic chemistry, Protonation, Buffer solution, Polypyrrole, Electrochemistry, Redox, Analytical Chemistry, chemistry.chemical_compound, Electrode, Pyrrole
Abstract

Attempts to immobilize a series of Dawson type heteropolyanions (HPAs) by anodization and the use of polymeric, polyvinylpyridine (PVP), and conducting pyrrole and N-methylpyrrole, films has been undertaken. A stable film of the Dawson Parent, [P2W18O62]6–, HPA was obtained on an anodized carbon electrode, the film exhibited thin layer behavior and was stable up to a pH value of 2.00. The same HPA was successfully immobilized in a protonated PVP film with the resultant modified electrode being stable between pH values of 1.00 and 8.00, with the redox activity of the immobilized HPA exhibiting the same pH dependence as shown by the solution phase species. It was shown that a stable polypyrrole film doped with the Dawson parent HPA was obtained when the cycling of the film was restricted to the first two tungsten-oxo based redox processes in buffer solutions more alkaline than 2.00. The CuII Dawson HPA was successfully immobilized in a polypyrrole matrix exhibiting good stability and clear redox activity for the CuII HPA. Poly(N-methylpyrrole) was found to be the most suitable conducting polymer film for the immobilization of the FeIII Dawson HPA. The film was found to be extremely stable to electrochemical cycling in a buffer solution of pH 4.50. The redox activity of the immobilized HPA was clearly observed and well behaved. In addition to this the electrocatalytic properties of the FeIII HPA towards the reduction of nitrite, as observed in solution, was preserved in the immobilized state.

Published
2001

43. Electrochemical investigation of regioregular alkyl substituted oligothiophenes

Author

Mieczysław Łapkowski, Marek Barth, Gérôme Bras, Stephan Guilerez, and Gérard Bidan

Subjects
chemistry.chemical_classification, General Chemical Engineering, Radical, Photochemistry, Electrochemistry, Medicinal chemistry, Redox, chemistry.chemical_compound, Transition metal, Radical ion, chemistry, Thiophene, Alkyl, Dichloromethane
Abstract

Radical cation stabilities and their dimerization reactions have been studied through the series of regioregular oligothiophenes (n=2–6 where n is the number of thiophene rings) with chlorine protected at one α-terminal position. The oligomers with two and three rings undergo one oxidation reaction to produce the radical cations, oligomers with four, five and six rings undergo two stepwise oxidations to produce the radical cations and dications, respectively. The radicals coupled to form dimers in following reactions. Based on double-potential-step data we observed that the dimerization rate decreases as n is increased. This result suggests that the stability of the radical increases with increasing size of its oligothiophene chain.

Published
2000

44. π-Conjugated Ligand Polymers Entwined around Copper Centres

Author

Pierre-Louis Vidal, Jean-Louis Hazemann, Gérard Bidan, Jean-Pierre Sauvage, B. Divisia-Blohorn, and Jean-Marc Kern

Subjects
Steric effects, chemistry.chemical_classification, Ligand, Organic Chemistry, chemistry.chemical_element, Polymer, General Chemistry, Conjugated system, Electrochemistry, Copper, Catalysis, Bond length, chemistry.chemical_compound, Crystallography, Monomer, chemistry
Abstract

We describe conjugated polymers entwined around Cu1 with alternating alpha-quaterthienyl (poly[Cu(T2)2]) or 3',4',3'''',4''''-tetrahexyl-alpha-sexythienyl (poly[Cu(T3)2]) moieties and 1,10-phenanthroline complexing sites. Our strategy is to synthesise the 2,9-bis(oligothienyl)-1,10-phenanthroline precursors, then to assemble these ligands by means of Cu1 templating followed by electropolymerisation. Poly[Cu(T2)2] shows separate electroactivities for Cu redox centres and conjugated backbones, whereas the electroactivities overlap in the case of poly[Cu(T3)2]. An X-ray absorption study on these polymers in their reduced state at the Cu-K edge identifies, in both cases, four nitrogen atoms as the closest copper(I) neighbours. For poly[Cu(T2)2], the Cu1 environment is a distorted tetrahedron similar to a monomer model compound, but with a slightly higher number of steric constraints. The Cu1 environment for poly[Cu(T3)2] is a less distorted tetrahedron with an unusually short Cu1-N average bond length. Cu1 removal in poly[Cu(T2)2] induces an irreversible collapse of the structure, whereas the reversibility of Cu1 binding is almost perfect for poly[Cu(T3)2], as the hexyl chains prevent irreversible gliding of the wires after copper removal. Combined electrochemical and resistance measurements reveal that the Cu centres in poly[Cu(T2)2] play the role of mechanical support for the structure with no significant electronic interactions with the conjugated backbone, whereas in the case of poly[Cu(T3)2] copper centres contribute to the conductivity of the structure.

Published
2000

45. Electropolymerization as a Versatile Route for Immobilizing Biological Species onto Surfaces

Author

Katia Galasso, Gérard Bidan, Eric Vieil, Luz Maria Torres-Rodriguez, Thierry Livache, Andre Roget, Martial Billon, and Gérard Mathis

Subjects
chemistry.chemical_classification, Conductive polymer, Materials science, Bioengineering, General Medicine, Polymer, Quartz crystal microbalance, Applied Microbiology and Biotechnology, Biochemistry, Combinatorial chemistry, Microelectrode, chemistry.chemical_compound, chemistry, Copolymer, Organic chemistry, Biochip, Molecular Biology, Biosensor, Biotechnology, Pyrrole
Abstract

Biosensors based on electronic conducting polymers appear particularly well suited to the requirements of modern biological analysis—multiparametric assays, high information density, and miniaturization. We describe a new methodology for the preparation of addressed DNA matrices. The process includes an electrochemically directed copolymerization of pyrrole and oligonucleotides bearing on their 5′ end a pyrrole moiety. The resulting polymer film deposited on the addressed electrode consists of pyrrole chains bearing covalently linked oligonucleotides (ODN). An oligonucleotide array was constructed on a silicon device bearing a matrix of 48 addressable 50 × 50 µm gold microelectrodes. This technology was successfully applied to the genotyping of hepatitis C virus in blood samples. Fluorescence detection results show good sensitivity and a high degree of spatial resolution. In addition, gravimetric studies carried out by the quartz crystal microbalance technique provide quantitative data on the amount of surface-immobilized species. In the case of ODN, it allows discrimination between hybridization and nonspecific adsorption. The need for versatile processes for the immobilization of biological species on surfaces led us to extend our methodology. A biotinylated surface was obtained by coelectropolymerization of pyrrole and biotin-pyrrole monomers. The efficiency for recognition (and consequently immobilization) of R-phycoerythrin-avidin was demonstrated by fluorescence detection. Copolymerization of decreasing ratios of pyrrole-biotin over pyrrole allowed us to obtain a decreasing scale of fluorescence.

Published
2000

46. Biochips on CMOS: an active matrix address array for DNA analysis

Author

P Caillat, P Peltié, Thierry Livache, F Revol-Cavalier, C. Massit, M. Belleville, Gérard Bidan, F. Clerc, A. Roget, D David, and E Crapez

Subjects
Materials science, Oligonucleotide, Hybridization probe, Metals and Alloys, Nanotechnology, Condensed Matter Physics, Chip, Multiplexer, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, Active matrix, law.invention, CMOS, law, Materials Chemistry, Electrical and Electronic Engineering, DNA microarray, Biochip, Instrumentation
Abstract

This paper reports a new development using a fully silicon active substrate and DNA probe electro-immobilisation. The DNA chip described is using CMOS 0.8 μm technology and an integrated multiplexer to address successively the electrode on which a specific DNA probe will be deposited. This approach is well adapted for low to medium range number of probes (50–1000) device. Applications targeted by this kind of device are wide, from specific kit of diagnosis to cancerology and agronomy. The final demonstrator is a 128 DNA probe chip which is used for the analysis of genes involved in Oncology.

Published
1999

47. Conjugated Polyrotaxanes Incorporating Mono- or Divalent Copper Complexes

Author

Gérard Bidan, Jean-Marc Kern and, and Bernadette Divisia-Blohorn, Jean-Pierre Sauvage, Jean-Louis Hazemann, and Pierre-Louis Vidal

Subjects
chemistry.chemical_classification, Absorption spectroscopy, Chemistry, Inorganic chemistry, chemistry.chemical_element, Conjugated system, Electrochemistry, Copper, Divalent, Inorganic Chemistry, chemistry.chemical_compound, Monomer, Polymer chemistry, Proton NMR, Physical and Theoretical Chemistry, Lithium Cation
Abstract

A conjugated polyrotaxane poly[Cu(1.2)+] has been synthesized via copper(I)-templated strategy and electropolymerization. The polymer backbone contains alternating quaterthiophene moieties and 1,10-phenanthroline complexes. It is threaded by coordinating cyclic units. Copper(I) binding was reversible only if lithium cation was present during copper removal, as a labile scaffolding, maintaining the topography of the free coordinating sites and of the organic matrix, as demonstrated by 1H NMR studies on monomer precursors. Electrochemistry has been coupled with X-ray absorption spectroscopy at the Cu K edge to study the interactions between the complexed copper centers and the conjugated backbone. The spectra of poly[Cu(1.2)n+] in various oxidation states have been analyzed and compared with those of monomeric model compounds. For all of the samples four nitrogen atoms are the closest neighbors. No dramatic geometric and electronic differences exist between monomeric and polyrotaxane Cu(I) binding sites. Ho...

Published
1999

48. Immobilisation at an electrode surface of calix[4]arenes bearing electropolymerisable pyrrole moieties at the upper rim

Author

L Chalumeau, I Soury-Lavergne, Gérard Bidan, and A Buffenoir

Subjects
chemistry.chemical_classification, General Chemical Engineering, Chronoamperometry, Electrochemistry, Photochemistry, Analytical Chemistry, chemistry.chemical_compound, chemistry, Transition metal, Calixarene, Polymer chemistry, Acetonitrile, Alkyl, Cyclophane, Pyrrole
Abstract

The first example of electrochemical homopolymerisation of calix[4]arenes modified by grafting N-substituted pyrrole moieties at their upper rim is presented. In a first step, a preliminary study was carried out on two model compounds (i.e. pyrroles bearing a p-amido-anisyl group via an alkyl spacing arm) to determine the conditions of electropolymerisation under potentiodynamic conditions. A minute change in the alkyl spacing arm length from ethyl to butyl has a remarkable influence, allowing better electropolymerisation when longer. Moreover, we have proved that dicyclohexylcarbodiimide, a coupling reagent used during synthesis has an inhibiting effect on pyrrole electropolymerisation. Similar results were obtained in the calix[4]arene series, i.e. film growth is enhanced with the calixarene containing the butyl spacing arm.

Published
1998

49. New oligothienyl-phenanthroline ligands: precursors for polymers consisting of conjugated links entwined around transition metal

Author

B. Leroy, Pierre-Louis Vidal, B. Divisia-Blohorn, Gérard Bidan, J. M. Kern, Jean-Pierre Sauvage, and Martial Billon

Subjects
chemistry.chemical_classification, chemistry.chemical_compound, Transition metal, Chemistry, Phenanthroline, Polymer chemistry, Polymer, Conjugated system, Biochemistry
Abstract

Une nouvelle famille de complexes a ligands encastres, Cu(T 1 ) 2 - et Cu(T 2 ) 2 + , a ete synthetisee respectivement a partir de la 2,9-di-(2-thienyl)-1,10--phenanthroline (T 1 ) et de la 2,9-di-(2-bithienyl)-1,10-phenanthroline (T 2 ) Leurs proprietes spectroscopiques et electrochimiques sont etudiees. L'electropolymerisation sur electrode de platine des ligands et des complexes est decrite. Cu(T 1 ) 2 - conduit a des monocouches ne contenant plus de centres metalliques En revanche, le film obtenu a partir de Cu(T 2 ) 2 + presente a la fois une electroactivite du centre metallique et de la matrice polythiophene

Published
1998

50. Polypyrrole DNA Chip on a Silicon Device: Example of Hepatitis C Virus Genotyping

Author

Joseph Marchand, Gérard Bidan, Robert Teoule, Thierry Livache, Gérard Mathis, Brigitte Fouque, and Andre Roget

Subjects
Quality Control, Silicon, Materials science, Genotype, Oligonucleotides, Biophysics, chemistry.chemical_element, Nanotechnology, Hepacivirus, Polypyrrole, Sensitivity and Specificity, Biochemistry, Matrix (chemical analysis), chemistry.chemical_compound, Electrochemistry, Fluorescence microscope, Pyrroles, Molecular Biology, Genotyping, Conductive polymer, Oligonucleotide, Nucleic Acid Hybridization, DNA, Cell Biology, Combinatorial chemistry, Microelectrode, chemistry, DNA, Viral, Microelectrodes, Biotechnology
Abstract

We describe in this article an oligonucleotide array constructed on a silicon device bearing a matrix of addressable 50-μm microelectrodes. Each electrode was covered by a conducting polymer (polypyrrole) grafted by an oligonucleotide (ODN). The DNA chip was prepared by successive electrochemically addressed copolymerizations of 5′ pyrrole-labeled ODN and pyrrole. Following hybridization of the biotinylated amplified sample on the chip bearing a series of probes, detection was carried out by fluorescence microscopy through an R-phycoerythrin label. This technology was successfully applied to the genotyping of hepatitis C virus in blood samples. Results show good sensitivity and a high degree of dimensional resolution.

Published
1998

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