Design from nanoscale of carbon fiber-based functional composite materials: Special attention on thermoset matrices and interfaces

J.F. GERARDIngénierie des Matériaux PolymèresUMR CNRS # 5223Université de Lyon – INSA Lyonjean-francois.gerard@insa-lyon.fr

http://www.imp.cnrs.fr

• Shaping of composite reinforcements and long fiber-basedprepregs

• Experimental testing and simulation of composite structures

• Acoustics of composite structuresIdentification of sources

• NDT analyses of • composite materials• and structures

(US, RX, acoustics)

• Synthetic and bio-sourcedthermoplastics and thermosets(from synthesis to rheology)

• Processingcomposites(RTM, prepregs,UV, etc)

• Fiber sizingsInterfaces

• Recycling• Paints, coatings, adhesives

• Ceramic-based composite materials• Acoustic emission analyses applied to fiber-based

composites• Microstructure analyses (SEM, TEM, ESEM, FIB, etc)

• Mechanics of composite structures foraeronautics and building constructionLarge scale testing facilities

• Composite materials for building repair• Inorganic-based composites for building

PARTNERSHIPS / COMPOSITE MATERIALS

Nodes ofcompetitiveness

• Components : SOLVAY, ARKEMA, CRAY VALLEY, HEXCEL, CHOMARAT, PORCHER Ind., DOW Chem, TRANSFURAN Chem (E), BROCHIER, NANOCYL, CYTEC, OCV, FLOWTITE (N)

• Aeronautics: AIRBUS (IVW, ASTRIUM, EUROCOPTER)(F&D), MBDA, AIRCELLE,COEXPAIR, QUICKSTEP, SAFRAN, ONERA,

• Automobile: VOLVO, MICHELIN, PLASTIC-OMNIUM, MCR, RENAULT, NIEF, CEA, COMPOSE TOOL• Rail : NEWRAIL (UK), AIRBUS (D)• Sport : ROSSIGNOL, BABOLAT• Energy : ALSTOM, EDF

• IFTH, PEP, PPE, SWEREA/SICOMP (S), INASMET (E), PyCO Fraunhofer (D), ICT Fraunhofer (D)

Industries

R&D Centers / Platforms

PARTNERSHIPS / COMPOSITE MATERIALS

Nodes ofcompetitiveness

• ENS Cachan, ESPCI, ECL et PolyTech Nantes, CERMAV, INP-PAGORA, ENSAIT

• INTEMA (Arg)KU Leuven (B), Perugia Univ. (I), Université Stuttgart (D), Université Erlengen (D), EZRT Fraunhofer (D)FORTH ICE-HT (Greece)Weizmann Inst. (Isr),Université Twente (NL), Swansea University (UK), Newcastle Univ. (UK), QMUL London (UK), Cambridge Univ. (UK), Université Akron (USA), Univerity Massachusetts (USA)

Universities / Academics

Design of Composite Materials at Different Scales

Tailoring components and microstructures at different scales

Taking into account the processing steps and techniques

INTERFACESFiber sizingsFunctional

(self-healing)WettabiityIFSS

NEW MATRICESSynthetic and bio-basedThermosets and ThermoplasticsNanostructured / Nanocomposite-based Functionalities(fire retardancy, conductivity…)

COMPOSITE MATERIALSViscoelastic, mechanicalElectricalSurface properties incl.wettability, paints, functionalcoatings (anti-icing, superhydrophobic)

Taking Into Account Processing of Composite Materials

Tailoring components and microstructures at different scales

REACTIVE PROCESSES Thermosets

epoxy, cyanates, BMI, UP, …toughened resins

Thermoplasticsfrom in-situ polymerization

Curing: thermal, UV, mW

NON-REACTIVELaser consolidation (high-Tg TP)Latex-based preforms

IN-SITU STUDIES OF THE PROCESSING STEPSWettability of the fiber fabricsIn-situ recording polymerization and/or crystallization

processes on composite parts (dielectrical, NIR)

COMBINATION OF STRATEGIES Interleaf particles films (toughening, self healing)Powdering for preform shaping and tougheningSoluble TP fibers for in-situ dispersion of TP and NPInsertion of piezo-electric polymer films (energy

harvesting)

Innovative Matrices for Composite Materials

Toughening from BCP nanoadditives of TS matrices in combination with processing

BCP-powdered CF-plies (400µm) 12 wt.% BCP

Consolidation stepBCP flows on/in the preform

Mold filling Impregnation of the preform + Dissolution of the BCP phase

0

1000

2000

3000

4000

5000

6000

7000

8000

h b

a

L

7,000 1,350 (+84%)

3,790 8602,280 220 (-40%)

Neat M25A50M25S28B28M44

GIIC (J.m-2)

0.5 mm.min-1

BCP nanostructuration

in composites confirmed by DMA

Inhomogeneous plate

Innovative Matrices for Composite Materials

Fire retardancy improvement from POSS nanoadditives of TS matrices

10” 30” 1’ 2’ 3’time

Extinguished after 3’ - burnt until clamps – resid.

mass: 6%

Extinguished before 3’ – flame propagated until clamps – resid.

mass: 59%

MVR

MVR-POSSOH-

Al

Molecular silica / POSS clustersPOSS-modifiedepoxies

Processing of TP-based composites from reactive processing

RTM (Resin Transfer Molding) processing of P6-GF composites

(a): ε-caprolactam

(b): N-acetylcaprolactam

(c): methylmagnesium bromide

ROP polymerizationof caprolactame

Reactive TP-RTMPA6 – GF composites / fracture surface

Dielectric sensors for followingpolymerization and crystallization

Processing of high Tg TP-based composites

Laser consolidation of PES – CF composites during filament winding

Filament winding / laser consolidation

Prepreg ribbon

Laser beam

Heating

Processing of high Tg TP-based composites

Laser consolidation of PES – CF composites during filament winding

Polymer chains

Carbon fiberInterdiffusion

of chains

Matrix

Carbon fibersTP matrix/CF ribbon

Macro scaleInter-ply scale

Micro scale Molecular scale

Multiscale approach

Tailoring processingconditions and materials

Fiber surface treatment for self-healable interfaces

Design and characterization of self-healable interfaces in epoxy-GF

Covalent bonding–reversible –(D-A)

Ra=5.64 ± 3.60nm

+BMI

Force gauge max 10N Displacement rate 0.1mm/min

Self-healing solution

Cured resin microdroplet

AFM analysis of treated CF surface

Interfacial adhesion

Functional composite materials

Electrically conductive matrices from CNT containing soluble fibers and CNT-yarns

Yarn in preform

A.E. signal acquisition

Piezo-electricsensor

40mm

Load

CNT yarn(coll. Cambridge Univ.)

CNT grown on ex-PAN CF

Introduction of CNT and/or high-Tg TP

Acoustic emission and electrical conductivity on

single-yarn CF or CNT