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MATERIALS AS THIN FILMS

Marie-Paule Besland, Valérie Brien [2019, ->],  Luc Brohan [-> 01/04/2016], Antoine Goullet, Agnès Granier, Pierre-Yves Jouan, Maryline Le Granvalet [2019, ->], Mireille Richard-Plouet [2016,->], Pierre-Yves Tessier, Post-doctoral researchers : Solène Béchu [2013-2017], Angelica D’Orlando [2016-2017], Yoan Gazal [2016-2017],   Invited researcher : Dayu Li [2018-2019], PhD students: Pierre-Louis Martin [2021-2024], William Ravisy [2018-2021], Joëlle Zgheib [2018-2021], Michael Rodriguez Fano [2019-2022]


PhDs : Axel Ferrec (2013), Stéphane Elizabeth (2015), Antoine Quenardel (2015),  Julien Keraudy (2015), Solène Béchu (2016), Romain Meunier (2016), Madec Querré (2016), Sabine Fabert (2017), Quentin Hatte (2019)

The deposition of thin films with functional properties is developed by plasma assisted processes [PECVD (Plasma Enhanced Chemical Vapour Deposition) and magnetron sputtering, in DC, pulsed DC and HiPIMS (High Power Impulse Magnetron Sputtering) modes] or in solution by chemical means.
Currently, we investigate the deposition of materials (metal, oxides, nitrides, oxy-nitrides) for their electrical and optical properties, their mechanical properties or their transport properties.
A wide range of applications are addressed: photo catalysis, photovoltaics or anti-bacterial, Thermal sensors, anti-corrosion coatings (coll. GEM), Micro- and Nano-technologies: miniaturized components for memory and neuromorphic applications (coll. PMN) or super-capacitors (coll. ST2E).

Our strategy is to establish a link between the targeted properties, the physicochemical and structural morphological characteristics of the deposited thin layers and the deposition process parameters aiming at getting some insights in the growth mechanisms and optimizing the material for the targeted application.

Keywords      Thin layer/thin film, PECVD process, magnetron sputtering, HIPIMS, Plasma diagnostics, Chemical process in solutionKeywords    
Expertises     Plasma discharges characterization, Deposition chambers design, HIPIMS supply design, Chemistry in solution, XPS and vibrational spectroscopies, Spectroscopic ellipsometry, Morphological chemical and structural characterisation of thin films (XRD, TEM, various spectroscopies...), Optimization of thin films for specific properties, Correlation between microstructure and properties



Oxide and nitride by DC or HIPIMS reactive sputtering

Jérémy Barbé, Valérie Brien, Pierre-Yves Jouan, Antoine Goullet, Mireille Richard-Plouet, Post-doctoral researchers : Axel Ferrec [2014-2015], PhD students: Joëlle Zgheib (2018-2021)

PhDs : Antoine Quenardel (PhD 2015), Julien Kéraudy (PhD 2015), Quentin Hatte (PhD 2019)
COUCHES MINCES Dpt de mtaux nitrures et oxydes par pulvrisation cathodique ractive DC et HiPIMS IMAGE 1000 pi par 1000pi


Reactive sputtering leads to the production of films with targeted properties. Their optimisation is driven by the implementation implementation of plasma diagnostics.
The deposition, carried out under vacuum and without intentional heating in continuous (DC) and pulsed HiPIMS (High Power Impulse Magnetron Sputtering) modes, offers a wide flexibility for the production of films and/or adhesion layers based on Nickel whether metal, oxide, nitrides, oxy-nitrides and silicides of Ni with a control of the stoichiometry, by adjusting the deposition parameters: Keraudy et al 2016 and Keraudy et al 2017.
Depending on the intended composition, these layers have applications in the field of energy (PV as collector layers for photo-generated carriers, energy storage as supercapacitors), temperature sensors, anti-corrosion coatings, or layers to reinforce mechanical properties.
Electrochemical sensors and electrochromic glazing can also be considered.

Keywords:           Continuous and pulsed magnetron reactive sputtering (HiPIMS), Transition metal coatings,Applications in the field of energy , Anti-corrosion coatings, mechanical properties
Expertises :         Control of plasma parameters to optimise a film with targeted properties, Plasma diagnostics, Microstructural characterisation of films and surfaces, ellipsometry, Monitoring of optical and electrical properties
Collaborations:   LTeN, CEISAM, GEM & GePEA (Nantes), MOLTECH-Anjou (Angers), ISCR (Rennes), Laboratoire d’études et de recherches sur les matériaux, les procédés et les surfaces (LERMPS), (Belfort-Montbéliard), Linköping University (Suède), IRT Jules Verne (Nantes), CEA (Saclay)

Resistive Switching in Mott materials

Marie-Paule Besland, Marie-Paule Besland, Pierre-Yves Jouan, Collaboration PMN team : Laurent Cario, Etienne Janod, Benoit Corraze, Post-doctoral researchers PMN : Julien Tranchant, PhD student : Michael Rodriguez Fano [2019- 2022]

PhD: Madec Querré (2016)

Mott cross section Since the IMN’s discovery highlighting the existence of a resistive switching induced by electric pulse in a wide range of materials, i.e. the Mott insulators, we investigate thin layers of Mott materials [Patents 2007, 2012).
The switching properties have been retrieve in crystallized thin layers obtained by Magnetron Sputtering (MS) of two materials GaV4S8 et V2O3:Cr (thickness range: 25-500 nm) [Patent 2009]. Following our works, these materials are considered as an emergent technology for memory [Adv. Func. Mat., 2015] and neuromorphic applications [Adv. Func. Mat., 2017] : the Mott-RAM technology.

 To know more                                            Review on IMN works on Mott materials      
                                    Mott materials for neuromorphism                        Properties of V203:Cr thin layers

Keywords               Thin layers, magnetron sputtering, Buffer annealing
Collaborations       PNF2 Platform Toulouse, CIRIMAT

Thin layers of TiO2 and TiO2 / SiO2 by PECVD

Antoine Goullet, Agnès Granier, Maryline Le Granvalet, Mireille Richard-Plouet , Invited researcher: Dayu Li [2018-2019], PhD student: William Ravisy [2018-2021]

PhD :   Stéphane Elisabeth (2015)

COUCHES MINCES Couches Minces deTiO2 et TiO2 substitu metal par PECVD Agnes Mireille

Our expertise in the PECVD process (low pressure inductively coupled RF plasma) for depositing thin layers from organometallic precursors has enabled us to optimize the process in order to synthesize at low temperature, on polymers, photo -catalytic TiO2 thin films by applying RF power in pulsed mode. High-resolution transmission electron microscopy (TEM) analyses revealed the columnar morphology of the thin films, completely crystallized in anatase form in continuous mode (T = 130 ° C) and crystallized only at the surface of the film in pulsed mode (T <80 ° C).
Recently, thin films of metal substituted anatase TiO2 (Nb5+, W5+/6+) have been obtained by injecting an organometallic precursor of the dopant. Their photo-catalytic properties in the visible and transparent conductive oxide are under study (ANR PATIO project in collaboration with LIST in Luxembourg, W. Ravisy PhD).

Keywords           nanomaterials, thin films, desalloying, flexible electronics, sensors
Expertises          PECVD, Analyse de surface XPS, MET, Ellipsométrie
Collaborations   LIST (Luxembourg) CHiPS, Université de Mons (Belgique)

Al-X-N-O thin films by magnetron sputtering

Valérie Brien, Pierre-Yves Jouan, Mireille Richard-Plouet, Pierre-Louis Martin [2021-2024]

AlCuNO BrienThis activity aims at developing and optimizing new compounds as thin films exhibiting specific photocatalytic properties, that is antibacterial, in order to fight against hospital diseases. The films of Al-X-N-O composition are elaborated by magnetron sputtering, a deposition technique very common in industry. It allows one to control the nature, the nanostructuration and the morphology of the films via the plasma parameters.
The synthesis and the structural, chemical, morphological or surface characterizations are achieved at IMN. The antibacterial properties and mechanisms are studied at another CNRS lab : Laboratoire de Chimie Physique et Microbiologie pour les Matériaux et l'Environnement, LCPME (Nancy). The stability of phases and the electronic structure are evaluated by DFT calculation in Thessaloniki University (Greece). These simulations bring us elements to progress on the understanding of properties.

Keywords:  nitride, photocatalytic, antibacterial, TEM
Expertises: Morphological and chemical characterization of thin films, Transmission Electron Microscopy, Correlations between physico-chemical features of thin films and macroscopic properties
Collaborations :  LCPME (Nancy), IJL (Nancy), Synchrotron Soleil (Saclay), Université de Strathclyde (Ecosse, Royaume Uni), EPFL (Suisse), Synchrotron Diamond (Oxford Royaume Uni), Université de Thessalonique (Grèce).

Transition metal oxides by "chimie douce" and chemical solution deposition

Mireille Richard-Plouet,  Luc Brohan [-> 01/04/2016], Collaboration PMN team: Bernard Humbert , Post-doctoral researcher : Angélina D’Orlando [2016-2017]

PhD: Solène Béchu  (2017)

chimie douce photo

Soft chemistry processes, involving autoclaving or reflux treatment of crystals of[Ti8O12 (H2O)24]Cl8, HCl, 7H2 in the presence of water and a suitable organic solvent makes it possible to have colloidal solutions of nanocrystals of TiO2 of the anatase variety (El Kass et al., 2017*).

These very stable solutions can be used to prepare thin films by chemical solution deposition and nanocomposites by pulsed injection in a low-pressure plasma [lien web vers nanocomposites]. 

Moreover, the control of hydrolysis and condensation of the precursor TiOCl2●1,4HCl●7H2O in N,N dimethylformamide has made it possible to synthesise sols and gels with original photo-electrochemical properties. The exploitation of these properties may lead to the development of new photo-devices, which requires sol shaping and characterisation by XPS  (Bechu et al., 2016*) and Infrared spectrometry under illumination in order to elucidate the mechanisms involved (Bechu et al., 2018*).

Keywords :             Chimie douce, spectroscopies and in situ UV illumination
Collaborations :     CEA-INES Chambéry

 

Thin films for solar energy thermal conversion

Christophe Cardinaud, Nicolas Gautier, Antoine Goullet, Jonathan Hamon, Mireille Richard-Plouet, Post-Doctoral researchers: Yoan Gazal [2016-2017]

 The ANR SiNOCH project has made it possible to synthesize, by plasma processes, organosilicon matCOUCHES MINCES Couches minces pour le solaire Thermique Antoineerials of the silicon nitride or carbide type. To this end, the OPTIMIST platform, coupled with an XPS spectrometer, was implemented according to different deposition process configurations. The link between deposition conditions and characteristics (in situ and ex-situ) of the materials has been established. The study is currently continuing with the ANR NANOPLAST (see website) project for the development of thin films for solar energy thermal conversion. Thus, SiC / metal (W) nanocomposite materials are promising candidates as absorbers of solar radiation. The work carried out at IMN focuses on the study by TEM microscopy and XPS spectrometry of the nanostructuring and atomic arrangement of these materials, in relation to the optical properties assessed by ellipsometry.

To go further
Impact of deposition conditions on the SiCN :H : nitride /Silicon carbide layers composition
PECVD growth mechanism and SiCN :H thin films characteristics

Keywords                PECVD processes, organosilicon, solar energy thermal conversion, dielectric-metal nanocomposites
Expertises              TEM microscopy, XPS spectrometry, ellipsometry
Collaborations        PROMES (Perpignan), ICCF (Clermont-Ferrand)

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