Manufacturing of Polymer Composites

OOA Prepreg Technology

Author: Mario Danzi
Laboratory of Composite Materials and Adaptive Structures
ETH Zürich
April 2017

Mario Danzi | 12.04.2017 | 1

Autoclave Processing
Introduction

Boeing 787 Dream Liner fuselage section: autoclave processing

Mario Danzi | 12.04.2017 | 2
Autoclave Processing
Introduction

 Why we use the autoclave in composite

processing?
The high compaction pressure provided by the
autoclave permits to manufacture high quality
laminates:

 High fiber volume content (55-65%) 4-8 bars

 Low void content (less than 2%)

 Why do we need such a high compaction

pressure? How does the compaction pressure acts
on the laminate?
Mario Danzi | 12.04.2017 | 3
Autoclave Processing
Introduction

 Influence of voids on the apparent shear strength.

Reference: Boyd, J. (2003).

Vacuum Bag only Composite Part
Manufacturing (Tutorial Handout)
(pp. 72). Dayton, OH: SAMPE 2003
Technical Conference/Dayton, OH.

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Theory on Laminate Consolidation
Spring / dashpot analogy

 Compaction of a saturated porous media

Fiber
Tows

Liquid
resin

Mechanical analogy proposed by Taylor.

[D.W. Taylor, Fundamental of Soil Mechanics”, John Wiley and Sons, New York, 1948]
Fiber Preform Liquid resin
Spring model Uncompressible fluid
Force ∝ 𝑆𝑡𝑟𝑎𝑖𝑛 Papplied = Pfluid

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Theory on Laminate Consolidation
Spring / dashpot analogy

 Spring analogy

Compaction Pressure
𝜎𝑡𝑜𝑡 𝜎𝑡𝑜𝑡 𝜎𝑡𝑜𝑡
Fluid Pressure
(resin) 𝑝𝑟𝑒𝑠𝑖𝑛 = 𝜎𝑡𝑜𝑡 0 𝑝𝑟𝑒𝑠𝑖𝑛
Spring Pressure
(fiber)
0 𝜎𝑓𝑖𝑏𝑒𝑟 = 𝜎𝑡𝑜𝑡 𝜎𝑓𝑖𝑏𝑒𝑟

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Theory on Laminate Consolidation
Terzaghi’s law

 Terzaghi’s Law

𝜎𝑡𝑜𝑡 = 𝜎𝑓𝑖𝑏𝑒𝑟 + 𝑝𝑟𝑒𝑠𝑖𝑛

where 𝜎𝑡𝑜𝑡 is the total externally applied stress, 𝜎𝑓𝑖𝑏𝑒𝑟 is the stress carried by the fibers
and 𝑝𝑟𝑒𝑠𝑖𝑛 is the hydrostatic pressure of the resin.

 The stress carried by the fiber is determined from the compaction

curve of the textile

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Theory on Laminate Consolidation
Fiber bed compaction

 The compaction curve describes the compaction pressure required to compact

a stack of fiber (fiber bed) to a certain fiber volume fraction
5
x 10 Compaction Curve of a Carbon Fibre Woven Fabric
6 This curve is characteristic of the textile!!!

5
Compaction Pressure [Pa]

N ∗ Aw
vf =
0
0.35 0.4 0.45 0.5 0.55
Fibre Volume Content [-]
0.6 0.65 0.7 𝜌𝑓 ∗ ℎ
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Theory on Laminate Consolidation
Fiber bed compaction
 Fiber bed compaction test:
20 layer of fabric are compacted between two plates, using a mechanical testing machine. Force and
displacement (distance between the plates) are measured. The compaction speed is held constant
and very low (0.1 mm/min) to ensure quasi-static conditions. The average FVF is calculated, knowing
the thickness of the sample (cavity height).

h
Cavity
Setup for Height
compaction F
experiments at
CMASLab

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Theory on Laminate Consolidation
Laminate compaction

 Resin pressure in processing conditions

5
x 10 Compaction Curve of a Carbon Fibre Woven Fabric
6

5
𝑟𝑒𝑠𝑖𝑛 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 ≈ 2.5 𝑏𝑎𝑟
Compaction Pressure [Pa]

3
𝑟𝑒𝑠𝑖𝑛 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 ≈ 3.5 𝑏𝑎𝑟 In prepreg processing
2
with no bleeding, the
nominal FVC is
1
defined by the
amount of resin.
0
0.35 0.4 0.45 0.5 0.55 0.6 0.65 0.7
Fibre Volume Content [-] Mario Danzi | 12.04.2017 | 10
Autoclave Processing
Void mitigation

 At a certain level of the hydrostatic pressure,

entrapped gases will collapse and dissolve into the
resin

 This pressure level is approximately 3.5 bar (resin

pressure). However, it depends on temperature,
surface tension, moisture, resin composition and
other factors.

 The high autoclave pressure help also to achieve a

better consolidation in corners.

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OOA Prepreg Systems
Motivation

 Disadvantages of autoclave processing

 High costs of autoclaves

 Size constrains
 Low availability
 Long processing cycles
 Operation danger (inert atmosphere - nitrogen)
 Expensive tooling systems
 High energy consumption Autoclave used for production of the Boeing 787 at
Triumph Aerostructures – Vought Aircraft Industries.
North Charleston, South Carolina, USA.

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OOA Prepreg Systems
Introduction 1 bar

 Oven cured under vacuum bag conditions.

(1 bar compaction pressure)

 Entrapped gas can’t be dissolved!!!

 Requirements for aerospace primary structures

 Less than 2 % void content
 High fiber volume content (>50%)

 How is it possible to achieve with OOA prepreg Porosity in a CF laminate observed at

laminates similar quality to autoclave processed the microscope (cross-section)
laminates?

Gas extraction is the key for OOA processing Mario Danzi | 12.04.2017 | 13
OOA Prepreg Systems
Characteristics
 OOA Prepreg systems are specifically designed for processing without the autoclave.
The major differences to autoclave systems are:
 Air permeability of the prepreg
 Resin rheology

 Low void content is achieved by “breathing” out of entrapped gases and volatiles
 Air pathways are created by partially impregnated prepreg
 Initial dry regions (prior to cure) are wetted out during resin cure cycle (consolidation)
 Edges breathing system are used to improve the air extraction from the laminate.
 Vacuum level is a key process parameters (reduce residual air)
Fiber Tow Resin Fiber Tow Resin

Before cure After cure and consolidation

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OOA Prepreg Systems
Characteristics

Lay-up Debulking Cure

 During debulking the uncured prepreg laminate is maintained at room temperature under vacuum
condition.

 In OOA processes, debulking steps are extended to enhance the extraction of air and volatilizes
from the laminate.

 Optimal debulking time depends on the size of the part and on the air permeability of the prepreg
material.

 OOA prepreg manufacturers recommend a minimum of 16 hours debulking at room temperature

under final vacuum bag arrangement (prior to cure).
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OOA Prepreg Systems
Characteristics

 Moisture can’t be extracted with room temperature debulking. Only when the
temperature is increased (curing process), the water become volatile (reach the
boiling point) and can be extracted.
 The resin viscosity should be tuned in order to retain breathability for a sufficient
amount of time.

Full vacuum
range

Source:
SAMPE Seattle
tutorial. Chris
Ridgard, 2010

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OOA Prepreg Systems
Limitations
5
x 10 Compaction Curve of a Carbon Fibre Woven Fabric
6

5
 Due to the low compaction

Compaction Pressure [Pa]

pressure (1bar), the 4
maximal achievable FVC
is in the range of 50-55%, 3

depending on the textile

used. 2

0
0.35 0.4 0.45 0.5 0.55 0.6 0.65 0.7
Fibre Volume Content [-]

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OOA Prepreg Systems
Limitations

 Hand layup of OOA prepreg may not work in cases where:

 The part is a full barrel construction cured in a female mold
 The part has features with local tight female radii
 Uncured ply thickness is greater than the cured ply
thickness. The thickness variation during cure can cause
bridging problems in female radii.
𝑢𝑛𝑐𝑢𝑟𝑒𝑑 𝑝𝑙𝑦 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠 − 𝑐𝑢𝑟𝑒𝑑 𝑝𝑙𝑦 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠
𝐵𝑢𝑙𝑘 𝑓𝑎𝑐𝑡𝑜𝑟 = ≈ 0.2
𝑐𝑢𝑟𝑒𝑑 𝑝𝑙𝑦 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠

before cure after cure and consolidation

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OOA Prepreg Systems
Process steps

 OoA prepreg process:

1. Lamination (intermediate debulking)
2. Vacuum bag layup
3. Debulking
4. Heating to curing temperature (consolidation)
5. Curing process
6. Heating to post-cure temperature
7. Post-cure process

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OOA Prepreg Systems
Process steps – Step 1: Lamination

 OoA prepreg process:

1. Lamination (intermediate debulking) -> Adaptation to mould shape and first ply consolidation
2. Vacuum bag layup
3. Debulking
4. Heating to curing temperature
5. Curing process
6. Heating to post-cure temperature
7. Post-cure process

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OOA Prepreg Systems
Process steps – Step 1: Lamination
 Most carbon fiber reinforced prepregs for hand layup have
some degree of dry fiber paths to permit air and volatile
extraction during an OOA cure.
 Improved laminate surface quality is achieved when the
prepreg is laminated with the drier side towards the mould.

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OOA Prepreg Systems
Process steps – Step 1: Lamination
 Intermediate debulking
 The laminate stack must be debulked at regular intervals during the lay-up process. This ensures that the
prepreg conforms to the tool shape and that an homogeneous consolidation is achieved. Particularly critical are
concave corners.
 During debulking, the laminate is covered with a perforated release film, a suitable breather and a reusable
membrane. The prepreg laminate is kept under vacuum for approximately 5 to 10 minutes. It is recommended that
the lay-up is debulked every 3 or 4 plies.

Recommended bagging arrangement for

intermediate debulking.
Source: Cytec, Application guidance
notes for vacuum bag processing
MTM44-1 dual core epoxy prepreg.

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OOA Prepreg Systems
Process steps – Step 2: Vacuum bag layup

 OoA prepreg process:

1. Lamination (intermediate debulking)
2. Vacuum bag layup -> Good vacuum bag integrity is essential!
3. Debulking
4. Heating to curing temperature (consolidation)
5. Curing process
6. Heating to post-cure temperature
7. Post-cure process

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OOA Prepreg Systems
Process steps – Step 2: Vacuum bag layup
 Layup, bagging techniques and ancillary
material are essentially the same as those
used for autoclave prepreg curing.
 However: Full Vacuum
 Edges breathing system are used to
enhance the extraction of air and volatiles
from the laminate.
 The quality of vacuum become a key
process parameters in oven/vacuum cured
parts.
 A vacuum leak check should be performed
prior to cure and heat-up. The test should
not show more than 0.068 bar vacuum
loss in 10 minutes.

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OOA Prepreg Systems
Process steps – Step 2: Vacuum bag layup

1. Non perforated release film and edge breathing via glass

(most common)

Recommended bagging arrangement for Example of layup on a OoA prepreg plate.

processing MTM®44-1. Note: The glass fiber strings must extend beyond the
Source: ACG, Users’ manual for LTM prepregs. non-perforated release film and be in contact with the
breather.
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OOA Prepreg Systems
Process steps – Step 2: Vacuum bag layup

2. Sealant tape and fiberglass cloth to connect the edges of the laminate with the breather

Vacuum bag arrangement recommended from Cytec for oven cure.

Note: the edge dams need to be higher than the laminate thickness.
Source: Cytec, Cycom 5320-1 epoxy resin system.

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OOA Prepreg Systems
Process steps – Step 2: Vacuum bag layup

 Relevance of edge breathing

Configurations 1 & 2

Configuration 1
Initial thickness: 2mm
Configuration 2
Configuration 3

Configurations 3

Reference: Gas transport in out-of-autoclave prepreg laminates, B.Louis, 2007.

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OOA Prepreg Systems
Process steps – Step 2: Vacuum bag layup

3. Z direction breathing using perforated release film (resin bleeding)

Recommended bagging arrangement for processing of Example of bleeding of the prepreg resin in a
prepreg systems foreseeing bleeding of resin in excess. VB process. The air bobbles follow in
Source: ACG, Users’ manual for LTM prepregs. direction of the pressure gradient.

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OOA Prepreg Systems
Process steps – Step 3: Debulking

 OoA prepreg process:

1. Lamination (intermediate debulking)
2. Vacuum bag layup
3. Debulking -> Air extraction and ply consolidation.
4. Heating to curing temperature (consolidation) Extract as much air and volatiles as possible
5. Curing process before starting the curing process.
6. Heating to post-cure temperature
7. Post-cure process

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OOA Prepreg Systems
Process steps – Step 3: Debulking

 Prepreg air permeability during debulking (@ 25°C)

The air permeability of the prepreg is

reduced during debulking.
Most change in permeability occurs
initially. A plateau around 60% of the
initial value.

Reference: Gas transport in out-of-autoclave prepreg laminates, B.Louis, 2007. Mario Danzi | 12.04.2017 | 30
OOA Prepreg Systems
Process steps – Step 3: Debulking

 Gas evacuation model developed by Arafath et al.* for MTM45-1 / 5HS for 1-D in-plane
gas evacuation
1

u L  1 2
 m  0 . 54
time   ln   
Po k  0 . 92  m o  
For 1 meter long laminate breathing on one side
µ dynamic viscosity of air (1.82E-5 Pa*s)
% gas removed (m/mo) Time Required Po atmospheric pressure (101 325 Pa)
10% 0.9 ~ 1.7 min L in-plane evacuation length
m/mo mass fraction of gas remaining in laminate
50% 0.5 ~ 55 min
Reference: Arafath, A. R. A., Fernlund, G., Poursartip, A.
80% 0.2 ~ 4.4 hours (2009, July 27-31). Gas Transport in Prepregs: Model and
Permeability Experiments. Paper presented at the ICCM-17,
90% 0.1 ~ 8.6 hours Edinburgh Scotland.

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OOA Prepreg Systems
Process steps – Step 4: Heating up and consolidation

 OoA prepreg process:

1. Lamination (intermediate debulking)
2. Vacuum bag layup
3. Debulking
4. Heating to curing temperature (consolidation) -> Final consolidation of the laminate. Moisture
5. Curing process is extracted. Resin rheology plays an important
6. Heating to post-cure temperature role.
7. Post-cure process

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OOA Prepreg Systems
Process steps – Step 4: Heating up and consolidation
 During heating up and curing phase, resin viscosity drops and
fills vacuum channels
 Consolidation and fully impregnation of the textile layers take
place.
 Prepreg resin viscosity (data for the MTM44-1 resin system,
DoC close to zero)
@ 25°C: 500 Pa*s @ 80°C: 200 Pa*s
@ 130°C: 10 Pa*s (curing temperature) @ 160°C: 1.5 Pa*s

Laminate cross-sections prior (left) and after (right) cure: 8-plies MTM45-1/5HS.
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OOA Prepreg Systems
Process steps – Step 4: Heating up and consolidation

 Prepreg air permeability during heating up phase (relevant for moisture evacuation)
6E-14
2-Ply
4-Ply
5E-14 8-Ply

4E-14
Permeability (m )
2

3E-14

2E-14

1E-14

0
30 40 50 60 70 80 90 100 110 120
Temperature (°C)

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OOA Prepreg Systems
Process steps – Step 5: Curing process

 OoA prepreg process:

1. Lamination (intermediate debulking)
2. Vacuum bag layup
3. Debulking
4. Heating to curing temperature (consolidation)
5. Curing process -> Consolidation and air extraction until gelation
6. Heating to post-cure temperature
7. Post-cure process

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OOA Prepreg Systems
Process steps – Step 6: Heating up

 OoA prepreg process:

1. Lamination (intermediate debulking)
2. Vacuum bag layup
3. Debulking
4. Heating to curing temperature (consolidation)
5. Curing process
6. Heating to post-cure temperature
7. Post-cure process

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OOA Prepreg Systems
Process steps – Step 7: Post-cure process

 OoA prepreg process:

1. Lamination (intermediate debulking)
2. Vacuum bag layup
3. Debulking
4. Heating to curing temperature (consolidation)
5. Curing process
6. Heating to post-cure temperature
7. Post-cure process

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OOA Prepreg Systems
Process steps
Typical process parameters for VB processing
200 9
3 4 5 6 7
180 8

Compaction pressure [bar]

160 2 h @ 180°C 7
Temperature [°C]

140 6
2 h @ 130°C
120 5
100 4 Temperature

80 Cure Post-cure 3 Compaction Pressure

60 2
40 1
20 0
0 50 100 150 200 250 300 350 400 450
Time [min]

Generally, OoA prepregs are cured at lower temperature than autoclave prepregs.
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OOA Prepreg Systems
Applications

 Major application sectors:

 Tooling
 Prototyping in aerospace
 Infrastructure
 Marine
 Wind energy
 Tidal energy
 Aerospace structures

Mario Danzi | 12.04.2017 | 39

OOA Prepreg Systems
Applications

 Tooling
 One of the main requirements for a
composite tool is vacuum integrity
(Leak Prevention Frame technique)
 Special techniques for the incorporation of
inserts, temperature control systems and
monitoring systems are required
 Tool of a Volvo 70 sailboat, two days of
lamination

Source: SAMPE Seattle tutorial. Chris Ridgard, 2010

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OOA Prepreg Systems
Applications

 Tooling

Source: SAMPE Seattle tutorial. Chris

Ridgard, 2010 and Cirrus aircraft.

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 OOA Prepreg Systems
Applications

 Prototyping in aviation

Source: Source: Source: SAMPE Seattle tutorial.

http://www.virgingalactic.com/multimedia/album http://www.learjet85.com/en/multime Chris Ridgard, 2010
/graphics-and-illustrations/ dia.html#a64-74
Spaceship 2 and White Knight 2 ( Bombardier Learjet 85 McDonnell Douglas Bird of Prey
Scaled Composites (California, USA) Fuselage and wings Cytec 5320 OOA Material: LTM10 first generation
OOA Material: Advanced Composites Group OOA prepreg
MTM45-1 (Umeco)
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OOA Prepreg Systems
Applications

 Marine
 High performance yachts
 Interior trim and structure
 Low temperature curing resins
(VTM260 @ 65°C)

Source: SAMPE Seattle tutorial. Chris Ridgard, 2010

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OOA Prepreg Systems
Applications

 Aviation: Boeing demonstrator launch fairing

 Constructed of Cytec 5320 prepreg

Sectioned Boeing fairing Cross-section cut of laminate

Source: Composites World. www.compositesworld.com
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OOA Prepreg Systems
Applications

 Space
 Delta Launcher Fairrings
(LTM45EL Doublers)

Source: SAMPE Seattle

tutorial. Chris Ridgard, 2010

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OOA Prepreg Systems
Applications

 Infrastructures

Source: SAMPE Seattle tutorial. Chris Ridgard, 2010

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Thank you for your attention
Questions?
Contact:

Mario Danzi
ETH Zürich
Institute of Design, Materials
and Fabrication
LEE O 225
Leonhardstrasse 21
8092 Zürich

Phone: +41 44 632 26 24

E-Mail: mdanzi@ethz.ch Production of OOA components for the Clean Sky A4 Demonstrator,
www.structures.ethz.ch Clean Sky Eco Design ITD.

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