# Testing a hydrogen onboard 70 MPa Composite Pressure Vessel with a new Ionic Liquid Epoxyde matrix

Stéphane Villalonga, Bruno Fournel, Jannick Duchet-Rumeau, Sébastien Livi, Jean-François Gérard, Frederic Démaret

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Stéphane Villalonga, Bruno Fournel, Jannick Duchet-Rumeau, Sébastien Livi, Jean-François Gérard, et al.. Testing a hydrogen onboard 70 MPa Composite Pressure Vessel with a new Ionic Liquid Epoxyde matrix. ECCM21 - 21st European Conference on Composite Materials for Academia and Industry, Ecole Centrale Nantes, Jul 2024, Nantes, France. hal-05469954

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Submitted on 21 Jan 2026

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FASTCURE 2

cea

anr®
agence nationale
de la recherche

ECCM21

02-05 July 2024
Nantes - France

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# Testing an Hydrogen Onboard 70 MPa Composite Pressure Vessel (CPV) with a new Ionic Liquid Epoxyde matrix

Bruno FOURNEL* & Stéphane VILLALONGA, CEA, Le Ripault, FRANCE

Jannick Rumeau, Sebastien Livi, Jean-François Gérard, IMP, INSA LYON, FRANCE

Frédéric Démaret, VITECH COMPOSITES, Sainte Maure de Touraine, FRANCE

2024, July, the 2nd

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INSA

INSTITUT NATIONAL
DES SCIENCES
APPLIQUÉES
LYON

cea

VITECH COMPOSITES
# H₂ Light an Heavy duty vehicles & CPV

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

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# Type IV H₂ CPV

* Plastic liner (PE, PA)

* Metallic boss (Al)

* Composite shell (CF+epoxy)

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

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1 tow of 24k filaments
7µm filament diameter

Carbon fibre mass = 70% Composite mass

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thermoplastic powder

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Epoxy resin

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INSA

INSTITUT NATIONAL
DES SCIENCES
APPLIQUES
LYON

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VITECH COMPOSITES

<figure><img src="image_16.png" /></figure>
# H₂ CPV R&D at CEA Le Ripault
CPV : Composite Pressure Vessel

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

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H2 CPV
R&D
since

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National &
International
R&D
projects

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Industrial
partners
network

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Academic
partners
network

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H2 CPV
Patents
<figure><img src="image_22.png" /><figcaption>Dedicated R&D H₂ CPV plateform at CEA</figcaption></figure>

* **Materials**

* Polymer & Composite : characterisation, ageing

* Material studies: PEPR ANR Hyperstock

* New Fastcuring Epoxy Matrix: ANR Fastcure 2 project

* Rotomolding monitoring: ANR Ulhys project

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ULHYS

FASTCURE 2

* **Design & FE Calculation**

* **Industrial Processes and Manufacturing** (industrial transfer)

* **CPV Testing & SHM**
  Standard, EC79,&R134 Regulation, additional severe condition tests

* **Standard & Regulation contribution & R&D expertise**
  (AFNOR, ISO-TC197, EC-SFEM, UN-UNECE-GTR13, ANR, EC)

* **Industrial support**

## CPV prototyping and testing
### Industrial support (material, design, process)
# H₂ CPV Process and Manufacturing at CEA

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

<figure><img src="image_24.png" /><figcaption>## Rotomolding</figcaption></figure>

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https://www.youtube.com/watch?v=zCE3VibUGJU

<figure><img src="image_27.png" /><figcaption>## Robotic Filament Winding</figcaption></figure>

<figure><img src="image_28.png" /><figcaption>CEA H₂ 62L CPV</figcaption></figure>

<figure><img src="image_29.png" /><figcaption>CEA H₂ full TP 36L CPV</figcaption></figure>

<figure><img src="image_30.png" /><figcaption>CEA H₂ Conformable 36L CPV</figcaption></figure>
## CPV testing facilities at CEA Le Ripault

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(c) Hypactor Project [JTI GA 621194]
CEA Impact with pneumatic canon (5kJ)

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62 L, 70 MPa H₂ CPV

Rotomolding: **40 min**

Filament Winding: **1h30min**

Epoxy Curing at low
temperature: 12h00-18h00

Mean: **15h00**

Total = **17h10**
# 2 matrixes formulated

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

## FASTCURE 2 Project : 2 products developped

* one formulation towpreg

* one formulation for wet winding process

### Ionic Liquids features

* Low vapor pressure

* Less energy release during curing

* Enhanced fire protection

* Recyclability (ANR PEPR Recyclage)

* Cost : Labscale molecules

## Towpreg formulation:

* Specified by CEA

* Formulated by INSA LYON

* Towpreg manufactured by VITECH COMPOSITES

* Tested by CEA (Manufacturing and 48 MPa/70 MPa CPV tests)

## Wet wind formulation:

* Specified by CEA

* Formulated by INSA LYON

* Tested by CEA (Manufacturing and 48 MPa/70 MPa CPV tests)
# Towpreg results: 6h

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

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FASTCURE (6h)

* DGEBA **SR 1228** / **IL 105** towpreg formulation patented (2021)
  CYPHOS® IL 105 Trihexyl(tetradecyl)phosphoniumdicyanamide

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Potlife Tamb (>3 months)

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Hotmelt formulation

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Thermo mechanical properties

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Impregnation

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CPV processability

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700 bar CPV performance

* Matrix with similar properties than Epoxy-Amines

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* Validation on prototype manufacturing (130°C => PA liner), dry Tg=136°C, additional work: need to increase the bobbin stiffness

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<figure><img src="image_55.png" /><figcaption>Fastcure 2
towpreg</figcaption></figure>

<figure><img src="image_56.png" /><figcaption>Towpreg Filament
Winding on liner</figcaption></figure>

<figure><img src="image_57.png" /><figcaption>Towpreg Filament
Winding on liner</figcaption></figure>

<figure><img src="image_58.png" /></figure>
# Wet winding result: 6h45

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

<figure><img src="image_59.png" /></figure>

FASTCURE (6h45)

DGEBA LY556 / **IL 104** wet winding formulation patented (2022)

<figure><img src="image_60.png" /></figure>

Potlife (>48 hours)

CYPHOS® IL 104 Trihexyl(tetradecyl)phosphoniumbis(2,4,4-trimethylpentyl)phosphinate

<figure><img src="image_61.png" /></figure>

Low visocisty resin (< 1 Pa.s)

<figure><img src="image_62.png" /></figure>

Thermo mechanical properties

<figure><img src="image_63.png" /></figure>

Impregnation

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CPV processability

<figure><img src="image_65.png" /></figure>

700 bar CPV performance

<figure><img src="image_66.png" /></figure>

* Matrix with similar properties than Epoxy-Amines

* Validation on prototype manufacturing (105°C & 130°C => PE & PA liner)

* 2022-2023 : 48 MPa/70 MPa CPV manufacturing + burst test + cycling test

<figure><img src="image_67.png" /><figcaption>Impregnation Bath
with Fastcure 2 resin</figcaption></figure>

<figure><img src="image_68.png" /><figcaption>Wet Filament
Winding on liner</figcaption></figure>

<figure><img src="image_69.png" /><figcaption>Pull out test with fastcure 2 resin</figcaption></figure>

<figure><img src="image_70.png" /><figcaption>Courbe Force - Déplacement</figcaption></figure>
Wet winding formulation: 6h45

FASTCURE 2

ECCM21

02-05 July 2024

Nantes - France

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# Fatigue test on 48 MPa CPV

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

## Vessel n°23L-C-22-002 (48 MPa, PA liner, Wet winding)

<figure><img src="image_77.png" /><figcaption>Figure 2 : Courbes de pression du réservoir 23L-C-22-002 en fonction du temps</figcaption></figure>

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## Vessel 23L-C-22-002 cycled 2500 times from 2MPa up to 60MPa without default

<table><caption>Tableau 3 : Déplacement maximal des capteurs LVDT lors du test de cycles en pression</caption><thead><tr><td>Capteur LVDT</td><td>Position</td><td>Déplacement maximum mesuré à 600 bar (en mm)</td><td>Moyenne (en mm)</td></tr></thead><tbody><tr><td>160AR23P03</td><td>radial +90° virole (31,5 cm)</td><td>1,04</td><td rowspan="3">1,12</td></tr><tr><td>160AR23P02</td><td>radial virole 0° (31,5 cm)</td><td>1,19</td></tr><tr><td>160AR23P01</td><td>radial virole -90° (31,5 cm)</td><td>1,14</td></tr><tr><td>160AR23P04</td><td>Axial sur bouchon</td><td>4,45</td><td>/</td></tr></tbody></table>
# Burst tests on 70 MPa CPV

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

<table><thead><tr><td>Réservoirs CEA Fastcure 2<br/>23L 500 bar</td><td>Liner</td><td>Process</td><td>Pression<br/>nominale de<br/>fonctionnement<br/>(NWP) (bar)</td><td>Pression<br/>d'éclatement<br/>(bar)</td><td>Burst ratio<br/>(doit être > 2 / R134)</td><td>Remarque</td></tr></thead><tbody><tr><td>23L-C-22-003</td><td>23L PA</td><td>V.H.</td><td>480</td><td>1062</td><td>2.21</td><td>Amorçage de la rupture dans la virole</td></tr><tr><td>23L-C-22-004</td><td>23L PA</td><td>V.H.</td><td>480</td><td>1092</td><td>2.28</td><td>Amorçage de la rupture dans la virole</td></tr><tr><td>23L-C-23-001</td><td>23L PA</td><td>V.H.</td><td>700</td><td>1490</td><td>2.13</td><td>Amorçage de la rupture dans la virole</td></tr></tbody></table>

<figure><img src="image_79.png" /></figure>

23L-C-22-003

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23L-C-22-004

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23L-C-23-001

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In accordance
with New R134
(BR > 2)
* 2 epoxy system formulated for thick CPV tank at low curing temperature

* 1 towpreg formulation at 130°C patented, 6 hours heating

* 1 wet winding formulation at 130°C patented, 6h45min heating

* => **curing time divided by 2,22** (15h => 6h45m)

* => heating time **55 %** reduction

* => CPV manufacturing time divided by 1,92 (17h10 => 8h55)

* => CPV overall manufacturing time 48 % reduction

* Further work : Recyclability (in progress PEPR Recyclage)
12 communications

○ S. Villalonga et al, Les verrous technologiques des réservoirs composites pour le stockage embarqué de l'hydrogène à 700 bar, p 37-43, Matériaux et procédés : un savoir faire spécifique, revue Chocs du CEA, n°51, novembre (2021)

○ S. Villalonga et al, Avancées technologiques pour les réservoirs de véhicules électriques à hydrogène, Matinée d'information sur la filière Hydrogène à l'ENSAM Paris, 9 mars, Paris, (2021)

○ S. Villalonga et al, Réservoirs embarqués pour le stockage de l'hydrogène à 700 bar, Journée sur les polymères pour les applications hydrogène, Polymeris, Webconf, 26 mai, (2021)

○ J.F. Gérard et al, Les polymères, des matériaux indispensables aux différentes briques technologiques de l'économie de l'hydrogène, Journée sur les polymères pour les applications hydrogène, Polymeris, Webconf, 26 mai, (2021)

○ S. Villalonga et al, 70 MPa H2 on-board CPV safety factor, International Conference on Hydrogen Safety (ICHS 2021), September 21-24th, Edinburgh, Scotland (2021)

○ S. Villalonga et al, 70 MPa H2 on-board CPV safety factor, Proceedings of 9th International Conference on Hydrogen Safety (ICHS 2021), p418-431, ISBN: 979-12-200-9400-9, September 21-24th, Edinburgh, Scotland (2021)

○ S. Villalonga et al, Les verrous technologiques des réservoirs composites pour le stockage de l'hydrogène gazeux sous pression, Conférence Horizons Hydrogène 2021, November 20-30th, Paris, France (2021)

○ S. Villalonga et al, New Fastcure 2 Towpreg for Hydrogen 70 MPa On-board type IV Composite Pressure Vessel Manufacturing, European Hydrogen Energy Conference (EHEC 2022), May 18-20th, Madrid, Spain, (2022).

○ S. Livi, et al, Ionic Liquids: A New Versatile Platform For The Design of a New Multifunctional Epoxy Networks 2.0 Generation, European Polymer Federation (EPF congress), June 26-1st July, Prague, Czech Republic (2022).

○ S. Livi, et al, Design of a New Multifunctional Epoxy-amine Networks based on Ionic Liquid Monomers, MACRO 2022 - the 49th World Polymer Congress, July 17-22th, Winnipeg, Canada (2022).

○ S. Livi, et al, A New Platform For The Development of a New Functional Epoxy Networks as Smart Coatings, European Corrosion Congress (Eurocorr congress), August 28-2st September, Berlin, Germany (2022).

○ S. Villalonga et al, H2 700 bar type IV on-board CPV, Conférence Horizons Hydrogène 2022, November 14-15th, Paris, France (2022)
## 2 Patents

* **Towpreg formulation**

* WO2023088977A1

* Titre : « RAPID-CURING COMPOSITION FOR THE PRODUCTION OF SEMI-FINISHED PRODUCTS ENABLING THE PRODUCTION OF COMPOSITE TYPE IV PRESSURE TANKS FOR THE ON-BOARD STORAGE OF HYDROGEN GAS »

* **Wet winding formulation**

* WO2023217934A1

* Titre : « RAPID-CURING, LOW-TEMPERATURE COMPOSITION FOR THE PRODUCTION OF PRESSURISED TANKS MADE OF A COMPOSITE MATERIAL FOR THE ON-BOARD STORAGE OF HYDROGEN GAS »
# Acknowledgment

ECCM21

02-05 July 2024

Nantes - France

UNIVERSITE
DE LYON

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INSA

INSTITUT NATIONAL
DES SCIENCES
APPLIQUÉES
LYON

<figure><img src="image_84.png" /></figure>

VITECH COMPOSITES

anr
agence nationale
de la recherche

<figure><img src="image_85.png" /></figure>

FASTCURE 2

ECCM21

02-05 July 2024
Nantes - France

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Audience

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INSA

INSTITUT NATIONAL
DES SCIENCES
APPLIQUÉES
LYON

VITECH COMPOSITES

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