Silica nanoparticles to improve erosion and ice resistance ... · Characterization of silica-filled...
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Guilhem QUINTARD, Frédéric LORTIE, Emilie MOLINA, Imane BARBARA, Jocelyne GALY Université de Lyon, CNRS, UMR 5223, Ingénierie des Matériaux Polymères, INSA Lyon 69621 Villeurbanne, France. [email protected] Advanced and Erosion Resistant Composites Silica nanoparticles to improve erosion and ice resistance of composites Optimisation of silica filled materials at Lab scale Conclusions and perspectives EIROS project « 18 partners around europe » Industrial issue Wind turbine blades Aerospace wings leading edges http://www.eirosproject.com W, Stöber ; A. Fink ; E. Bohn, J. Colloid Interface Sci. 1968, 26, 62-69 Extreme weather conditions constitute a serious issue for some industries. It is usually solved by relying on active strategies as heating or chemical bleed. Because of the cost of these methods and environmental concerns, passive solutions are the key for achieving long term-functional performances. Abstract The European funded collaborative project EIROS aims at developing self-renewing, self healing, erosion resistant and ice-repellant composite materials for use in extreme environments (high erosion and very low temperatures). The choosen strategy is to design multi-functionalized nanoparticles (silica particles described here), nanoencapsulated phase-change materials and self-healing nanocapsules) which are subsequently dispersed into epoxy matrix in order to confer ice and erosion resistance to the final composite material. Multi-functional silica nano-particles has been developed and incorporated into composite materials to improve their ice and erosion resistant properties. Characterization of silica-filled epoxy composite (water contact angle, roughness, hardness, SEM…) were first performed at lab scale on composite and aluminum substrates. Silica nanoparticles have been found to be well-dispersed into the epoxy matrix and hydrophobicity is significantly improved if compared to reference uncoated surfaces. Then silica nanoparticles potential has been tested on representative parts and under experimental conditions which are supposed to mimic aeronautical environment. EIROS Strategy SiO 2 PCM Silica capsule 1) 2) 3) Catalyst Microcapsule Crack Healing agent Polymerized healing agent Functionalized silica NP’s for hydrophobicity Functional nano- encapsulated phase change materials Self-healing materials 1 2 3 Incorporation in polymer matrix (epoxy) Repellent functionality Crosslinking and compatibilization with polymer matrix This project has received funding from the European Union's Horizon 2020 research and innovation program. Coated panels (TSS4@NPTMS/ 8552 resin) AS4/8552 composite with deicing bronze mesh Electronic scanning microscopy Ra 3,3µm Ra 3,5µm WCA 84° WCA 65° WCA 105° WCA 95° Scratch test (Wolff Wilborn) Roughness Water Contact Angle Without coating Anodized Aluminium 2024 T3 Aeronautical case study on silica filled parts Manufacturing of a prototype (Wing Leading Edge for Sonaca) 12 layers carbonfiber epoxy + 1 layer bronze mesh Coating by spray application TSS4@NPTMS / 8552 resin on composite material Ice Wind Tunnel Tests and Ice Adhesion - IFAM Rain Erosion tests – Polytech (Denmark) 7H 8H 9H Excellent dispersion of Si nanoparticles Increase of roughness with Si (Ra ref = 0,4µm) Coating 7H hardness Increase of hydrophobicity with Si All those tests were performed again after ageing: climatic chamber, UV and neutral salt spray TEM / SEM particle size Φ = 30 nm 29 Si NMR silanol content = 7,1 SiOH.g -1 degree of functionalization = Si grafted with GPTMS: 5% Ex: GPTMS Silica Characterization SiO 2 OH OH OH HO HO OH 1- Silica NP’s synthesis : Stöber process 2 - Organo-modification of silica NP’s Non-functionalized silica dispersion in solvent: 4,1 to 4.3 ±0.2 wt% Alcohol + TEOS Alcohol + water + ammonia SiO 2 • NPTMS • GPTMS • HMDZ • Fluorinated silane Silanes used for functionalization 3 – Characterization (DLS, SEM/TEM, BET, pyconometry, XPS, EA, NMR)
Transcript of Silica nanoparticles to improve erosion and ice resistance ... · Characterization of silica-filled...
Guilhem QUINTARD, Frédéric LORTIE, Emilie MOLINA, Imane BARBARA, Jocelyne GALY
Université de Lyon, CNRS, UMR 5223, Ingénierie des Matériaux Polymères, INSA Lyon 69621 Villeurbanne, France.
Advanced and Erosion Resistant Composites
Silica nanoparticles to improve erosion and ice resistance of composites
Optimisation of silica filledmaterials at Lab scale
Conclusions and perspectives
EIROS project
« 18 partners
around europe »
Industrial issue
Wind turbine blades Aerospace wings leading
edges
http://www.eirosproject.com
W, Stöber ; A. Fink ; E. Bohn, J. Colloid Interface Sci. 1968, 26, 62-69
Extreme weather conditions constitute a serious
issue for some industries. It is usually solved by
relying on active strategies as heating or chemical
bleed. Because of the cost of these methods and
environmental concerns, passive solutions are
the key for achieving long term-functional
performances.
AbstractThe European funded collaborative project EIROS aims at developing self-renewing, self healing, erosion resistant and ice-repellant composite materials for use in extreme environments
(high erosion and very low temperatures). The choosen strategy is to design multi-functionalized nanoparticles (silica particles described here), nanoencapsulated phase-change materials
and self-healing nanocapsules) which are subsequently dispersed into epoxy matrix in order to confer ice and erosion resistance to the final composite material.
Multi-functional silica nano-particles has been developed and incorporated into composite materials to improve their ice and erosion resistant properties.
Characterization of silica-filled epoxy composite (water contact angle, roughness, hardness, SEM…) were first performed at lab scale on composite and aluminum substrates. Silica
nanoparticles have been found to be well-dispersed into the epoxy matrix and hydrophobicity is significantly improved if compared to reference uncoated surfaces. Then silica
nanoparticles potential has been tested on representative parts and under experimental conditions which are supposed to mimic aeronautical environment.
EIROS Strategy
SiO2
PCM Silica capsule
1)
2)
3)
Catalyst
Microcapsule
Crack
Healing agent
Polymerized
healing agent
Functionalized silica
NP’s for
hydrophobicity
Functional nano-
encapsulated phase
change materials
Self-healing
materials
1
2
3
Inco
rpo
ratio
n in
po
lym
er
ma
trix (ep
oxy
)
Repellent
functionality
Crosslinking and
compatibilization
with polymer matrix
This project has received funding from the European Union's Horizon 2020 research and innovation program.
Coated panels
(TSS4@NPTMS/
8552 resin)
AS4/8552
composite with
deicing bronze mesh
Electronic scanning
microscopy
Ra 3,3µm Ra 3,5µm
WCA 84° WCA 65°WCA 105° WCA 95°
Scratch test (Wolff
Wilborn)
Roughness
Water Contact
Angle
Without coating
Anodized
Aluminium
2024 T3
Aeronautical case study on silica filled partsManufacturing
of a prototype
(Wing Leading
Edge for
Sonaca)
12 layers
carbonfiber
epoxy
+
1 layer bronze
mesh
Coating by spray
application TSS4@NPTMS
/ 8552 resin on
composite material
Ice Wind Tunnel Tests and Ice
Adhesion - IFAM
Rain Erosion tests – Polytech
(Denmark)7H
8H
9H
Excellent
dispersion of
Si
nanoparticles
Increase of
roughness
with Si (Ra
ref = 0,4µm)
Coating 7H
hardness
Increase of
hydrophobicity
with Si
All those tests were performed again after ageing: climatic chamber, UV
and neutral salt spray
TEM / SEM �particle size
Φ = 30 nm
29Si NMR �silanol content = 7,1 SiOH.g-1
� degree of functionalization =
Si grafted with GPTMS: 5%
Ex: GPTMS
Silica Characterization
SiO2
OH
OH
OH
HO
HO
OH
1- Silica NP’s synthesis : Stöber process 2 - Organo-modification of silica NP’s
Non-functionalized silica
dispersion in solvent: 4,1
to 4.3 ±0.2 wt%
Alcohol + TEOS Alcohol + water
+ ammonia
SiO2
• NPTMS
• GPTMS
• HMDZ
• Fluorinated
silane
Silanes used for functionalization
3 – Characterization(DLS, SEM/TEM, BET, pyconometry, XPS, EA, NMR)
