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Grenoble INP
LGP2, a center of innovative research

Paper, print media and biomaterials

LGP2, a center of innovative research

LGP2 - Ph.D. thesis defended in 2017

Erwan GICQUEL

December 1st, 2017 - Fluid Mechanics, Energy, Processes
Ph.D. title
Printing and selective sintering of metal based inks on paper. Optimization of electrical properties of RFID-HF loops for industrial production.
Supervision
Julien BRAS, Associate Professor HDR, Grenoble INP-Pagora / LGP2  ♦♦ Céline MARTIN, Associate Professor, Grenoble INP-Pagora / LGP2
Abstract
This project consists to develop and study new hybrid structures based on nanocelluloses and stimuli-responsive polymers, in particular, thermo-responsive polymers. Nanocelluloses - nanoparticles extracted from cellulose - exist in two forms: cellulose nanocrystals (CNC) and cellulose nanofibrils (CNF).
This study focused on the design of CNC hydrogels with stimuli-responsive polymers. Several thermo-responsive polymers have been used for their biocompatibility and lower critical solution temperature (LCST) close to body temperature. This work consisted of preparation of systems using the principles of green chemistry, the rheological study of these thermo-sensitive hydrogels, and the development of smart applications for these unique biomaterials.
Through the use of state of the art technologies (SANS, SAXS), physicochemical interactions between the polymers and CNC have been studied. The use of block copolymers made it possible to create CNC-based hydrogels with specific rheological properties: liquid at ambient temperature to gel at body temperature. These hydrogels can be used in the creation of injectable systems for biomedical applications, as well as thermosensitive surfaces.
Other members of the jury
Bernard CATHALA, Research Director, INRA, Nantes  ♦♦ Wim THIELEMANS, Professor, Université catholique de Louvain, Belgium ♦♦ Emily CRANSTON, Professor, McMaster University, Canada ♦♦ Frédéric BOSSARD, Professor, LRP, Grenoble ♦♦ Bruno JEAN, Researcher, Cermav, Grenoble ♦♦ Frédéric PIGNON, Research Director, LRP, Grenoble

Charlène REVERDY

November 16, 2017 - Materials, Mechanical, Civil Engineering, Electrochemistry
Ph.D. title
Industrial applications of functional nanocelluloses.
Supervision
Julien BRAS, Associate Professor, Grenoble INP-Pagora / LGP2  ♦♦ Naceur BELGACEM, Professor, Grenoble INP-Pagora / LGP2
Abstract
The aim of this work is to implement new properties to a paper based material via the use of functional nanocelluloses. Nanocelluloses are nanoparticles extracted from wood and distinguished in two categories: Cellulose Nanofibrils (CNF) and Cellulose Nanocrystals (CNC).
This work has only been carried out with CNF. The chemical reactivity of CNF was used to functionalize them with organotrialkoxysilanes. The entangled network and highly viscous suspension of CNFs was also used to synthesize silsesquioxane particles with limited size to impart (super)hydrophobic and antimicrobial properties.
Knowledge obtained through the study of model CNF films was then applied to paper based material coating. The functional CNF were evaluated for its use in an antimicrobial, anti-adherent, greaseproof or superhydrophobic paper surface.
Other members of the jury
Gilles SEBE, Associate Professor, ENSCBP, Bordeaux ♦♦ Elisa ZENO, Research Engineer, Centre Technique du Papier, Grenoble ♦♦ Didier LEONARD, Professor, Université Lyon I ♦♦ Monika ÖSTERBERG, Professor, Aalto University, Finland

David GOSSELIN

October 6, 2017 - Fluid Mechanics, Energy, Processes
Ph.D. title
Towards an integrated Point-of-Care diagnostic device: use of capillarity as well as thermoforming and screen printing processes.
Supervision
Didier CHAUSSY, Professor, Grenoble INP-Pagora / LGP2 ♦♦ Naceur BELGACEM, Professor, Grenoble INP-Pagora / LGP2 ♦♦ Jean BERTHIER, Research Engineer, CEA, Grenoble
Abstract
Developments of microfluidics (the study of flows at the sub-millimetric dimensions) have made possible the integration of most of the macroscopic functions of laboratory fluidic systems in a miniaturized system, thus realizing a lab on a chip. This allows the conception of low cost, sensitive and efficient medical diagnostic device usable outside of a medical infrastructure. Such devices are called Point-of-Care systems. The design and fabrication of such devices requires an elaborated and coherent integration that takes into account all the constraints imposed by the targeted final application.
The work reported here, and performed during the PhD internship, is focused on the study of the concept and development of the integration of a PoC device based on the isothermal LAMP (Loop mediated AMPlification) reaction for the molecular analysis of DNA. In order to offer a cheap and easily industrialized system, we investigate the use of paper as the chip material and thermoforming as the mean to build the channels. These two techniques are currently used in the industry and their adaptation to the fabrication of such devices is easy and low-cost.
In order to perform a LAMP reaction, specific functions such as a heating and a detection system are required. The integration of these functions was carried out using screen printing technology. Heating is done by Joule effect using a layer of carbon-based conductive ink. Detection is performed by a potentiometric method, using polyaniline-covered electrodes. It is shown that this approach is compatible with integration when the screen-printing layers are superposed. Besides they can be printed before thermoforming, resulting in a highly integrated system.
Other members of the jury
Stéphanie BRIANÇON, Professor, Université Claude Bernard Lyon 1 ♦♦ Chantal FOURNIER-WIRTH, Research Director, ESF Pyrénées-Méditerranée, Toulouse ♦♦ Jean-Christophe BARET, Professor, Université de Bordeaux

Ying SHAO

September 29, 2017 - Materials, Mechanical, Civil Engineering, Electrochemistry
Ph.D. title
Use of lignocellulosic materials and 3D printing for the elaboration of conductive carbon strutures.
Supervision
Davide BENEVENTI, CNRS Research Director, Grenoble INP-Pagora / LGP2 ♦♦ Didier CHAUSSY, Professor, Grenoble INP-Pagora / LGP2 ♦♦ Philippe GROSSEAU, Research Director (École des Mines, Saint-Étienne)
Abstract
In this thesis, electrically conductive and mechanically resistant carbon structures were elaborated by 3D printing and subsequent pyrolysis using microfibrillated cellulose, lignosulfonate and cellulose powder (MFC/LS/CP) blends.
The processability of MFC/LS/CP slurries by 3D printing was examined by rheological tests in both steady flow and thixotropic modes. The printed MFC/LS/CP pastes were selfstanding, provided a high printing definition and were proved to be morphologically stable to air drying and the subsequent pyrolysis.
Pyrolysis at a slow rate (0.2°C/min) to a final temperature in the range of 400-1200°C was used to manufacture MFC/LS/CP carbons. The TGA/DTG was applied to monitor the thermal degradation of MFC/LS/CP materials in blends as well as in a separated form. The resulting carbons were further characterized in terms of morphology, microstructure and physical properties (such as density, electrical conductivity and mechanical strength). At 900°C, MFC/LS/CP carbons displayed a high electrical conductivity of 47.8 S/cm together with a low density of 0.74 g/cm3 as well as an important porosity of 0.58. They also achieved an elastic modulus maximum of 6.62 GPa. Such interesting electrical and mechanical properties would lead to a promising application of MFC/LS/CP- derived biocarbons in energy storage devices as electrode materials in close future.
Other members of the jury
Pascaline PRÉ, Professor,  École des Mines, Nantes ♦♦ Sylvain SALVADOR, Professor, École des Mines, Albi ♦♦ Salaheddine SKALI-LAMI, Associate Professor HDR, Université de Lorraine

Victor THÉNOT

July 12, 2017 - Fluid Mechanics, Energy, Processes
Ph.D. title
Printing and selective sintering of metal based inks on paper. Optimization of electrical properties of RFID-HF loops for industrial production.
Supervision
Nadège REVERDY-BRUAS, Associate Professor, Grenoble INP-Pagora / LGP2 ♦♦ Denis CURTIL, Research Engineer, Grenoble INP-Pagora / LGP2 ♦♦ Mohamed SAADAOUI, Associate Professor (École des Mines, Saint-Étienne)
Abstract
This work examines the potential of a very smooth paper for the mass production of printed RFID-RF tags. Characterizations on PowerCoat HD paper demonstrate high temperature tolerance and verv low roughness. lt thus represents a serious alternative to the use of polymeric films (PET, PEN, Pl, etc.) enabling the electrical performance of metallic conductive inks to be fully developed.
Two industrial printing processes have been considered: flexography and screen printing, and their use were discussed for the printing of low-cost electronic devices. Moreover, the electrical performances of commercial silver based inks are studied according to the size of their particles. lndeed, the use of metal particles at the nanometric scale can facilitate the activation of the atomic diffusion mechanisms, thus improving the physical contact between the particles and promoting electrical conduction. ln parallel, microparticles inks are cheaper and their conditions of use less restrictive. ln any case, the coalescence of the metal particles after printing cannot be initiated without a thermal sinter ing treatment.
Sintering is usually carried out in an oven or hot air tunnel, the temperature must therefore remain below the tolerance of the substrate. This leads to limited electrical performances for long process duration of several minutes. ln order to take into account the industrial constraints of largescale production and to achieve the best electrical performance in a short time, one of the main explored research areas is the deployment of emerging near- infrared (NIR) and intense pulsed light (IPL) photonic technologies. These latter are based on the absorption of light energy by the ink film thus causing rapid heating. The important absorption differential between the inks and the substrate allows high heating selectivity which makes it possible to limit the degradation of the substrate while the ink temperatures may be greater than 300 ° C. For each sintering process, the influence of the various parameters on the final electrical performance has been studied by using an in situ resistance monitoring, allowing sampling frequency up to 250 kHz.
Finally, RFID-HF loops were printed, sintered under previously optimized conditions and then characterized. An estimate of the production costs was carried out in order to distinguish the contributions related to the ink, the substrate and the silicon chip. The obtained results demonstrate the potential of PowerCoat HD paper, coupled with flexographic roll-to-roll printing and near-infrared technology, enabling the large-scale production of RFID-HF tags at a material cost of the order of 5 euros cents.
Other members of the jury
Philippe DELAPORTE, CNRS Research Director, Aix-Marseille Université ♦♦ Hélène DEBEDA, Associate Professor, Université de Bordeaux ♦♦ Damien DELERUYELLE, Professor, INSA Lyon ♦♦ Tan-Phu VUONG, Professor, Grenoble INP-Phelma ♦♦ Bernard RATIER, Professor, XLIM, Limoges

Megan SMYTH

June 27, 2017 - Materials, Mechanical, Civil Engineering, Electrochemistry
Ph.D. title
A matrix based on stimulable nanocellulose for differentiated growth of cells.
Supervision
Julien BRAS, Associate Professor, Grenoble INP-Pagora / LGP2 ♦♦
Abstract

Other members of the jury
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Sébastien RAYNAUD

February 14, 2017
Ph.D. title
Development of new barrier materials using microfibrillated cellulose.
Supervision
Alain DUFRESNE, Professor, Grenoble INP-Pagora / LGP2 ♦♦ David GUÉRIN, Manager Research Unit, Centre Technique du Papier, Grenoble
Abstract
This study takes place in a context of development of paper-based barrier packaging materials, using microfibrillated cellulose (MFC) that displays renewability, recyclability and biodegradability. Two strategies have been investigated: the wet lamination of a MFC barrier layer on board, and the use of MFC as additive in a water-based barrier coating colour.
The promising use of MFC for the formation of barrier layers has been demonstrated in both cases. The wet lamination of MFC on board led to good oxygen and grease barrier properties, using highly fibrillated MFC. The board-MFC complex presented a strong adhesion after drying, without requiring glue.
For composite barrier coating, in order to obtain low viscosity suspensions leading to high barrier layers, the use of highly fibrillated MFC mixed with a fully-hydrolysed poly(vinyl alcohol (PVOH) with a low degree of polymerisation has been preferred. The addition of MFC in PVOH demonstrated its potential for improving the drying behaviour of water-barrier barrier coating colours. The combined use of MFC and layered silicates evidenced a synergistic effect on their dispersion in a PVOH solution, leading to an improved water vapour barrier while avoiding the formation of aggregates that otherwise damage the oxygen barrier.
The work contributes to demonstrate the potential of MFC to be used for the formation of barrier layers, paving the way for the development of more sustainable barrier packaging materials.
Other members of the jury
Hélène ANGELLIER-COUSSY, Associate Professor, Université de Montpellier  ♦♦ Yves GROHENS, Professor, Université Bretagne Sud ♦♦ Jose-Maria LAGARON, Research Director, Consejo Superior de Investigaciones Científicas, Espagne ♦♦ Laurent HEUX, CNRS Research Director, Université Grenoble Alpes

Written by Anne Pandolfi

Date of update December 13, 2017

Communauté Université Grenoble Alpes