Processing Thermosets Composites

Spring Semester 2017
151-0548-00L Manufacturing of Polymer Composites
Processing of Thermosets
Composites
Paolo Ermanni
9 March 2017
ETH Zurich, Laboratory of Composite Materials and Adaptive Structures Manufacturing of Polymer Composites - Processing of Thermosets Composites | 09.03.2017 | 1
Contents
 Introduction
 Wet-Lamination Process
 Flow in porous media
 Resin curing kinetics
 Resin viscosity
Selection criteria for manufacturing process
Selection
Economical aspects Technical aspects
Criteria
Structural features
 Design and fabrication of highly
Investments integrated monolithic structures
Equipment (reduction of single parts)
 Manufacturing of highly complex
Tooling shapes
 Easy integration of doublers,
Labour costs inserts damping materials and
functional elements such as
Material Costs actuators and sensors.
Series volume Surface quality
Cycle time Laminate features
Safety and health  Mechanical properties
 Fibre architecture
aspects  Fibre volume content
Quality and reproducibility
Top-level Process-chain from constituent materials to
final part
Fabrication route
Constituent Layup, Manufacturing process Final part &

materials Preform material
Impregnation Forming Curing properties
Physical and chemical processes
Capillary driven Pressure driven Chemical

flow flow reaction
Material properties
Quality features
 Fibre distribution
 Void content and distribution
 Delamination
 Fibre/matrix interface
Fibre volume content

Flemming, M.; Ziegmann, G.; Roth S.: Faserverbundbauweisen, Halbzeuge und Bauweisen; Springer-Verlag, Berlin Heidelberg 1996
Overview
Flow- Injection-
Draping Processes
Processes Processes
SMC, GMT Filament Winding, Press technologies Autoclave RTM, VARI

LFI, E-LFI Pultrusion, SCRIMP...
Automated layup
Off-line
Impregnation Prepregs
Fibre
Off-line
Rovings
Impregnation
Textile Intermediate Textile Multi-axial

material Preforming Preform
Process Process material
Weben Vernähen
Flechten Wirken
Stricken Sticken
3D-Form
Contents
 Introduction
 Resin viscosity
Wet Lamination technique
Preparation Forming Impregnation Curing Demolding
 Preparation of fibre layers and cutting to

desired shape and size
 Preparation of the mold
 Resin mixing
 Forming takes place by laying/draping the

layers in resp. on the mold
 Wetting of the fabric
 Vacuum-bagging
 Curing usually takes place at room

temperature.
 Post-curing at higher temperature is
possible after removal from the mold.
 Typical fibre material: glass fabrics vlies and
 Demolding mats
 Resin systems: Unsaturated Polyester,
 Post-processing
Vinylester, Epoxy
Wet Lamination technique
 Preparation of fibre layers and cutting to Surfacing ply

desired shape and size Release agent
 Resin mixing

 Wetting of the fabric Mold reinforcement
 Vacuum-bagging
Mold
Glass fibre mats, vlies and/or fabrics
temperature.
 Simple molds
possible after removal from the mold.  No special requirements with
regard to temperature
 Demolding resistance
 Mold material: often wood or
 Post-processing
resin
Wet lamination technique

 Resin mixing

 Vacuum-bagging

temperature.
 Demolding
 Post-processing
Wet lamination technique

 Resin mixing

 Vacuum-bagging

temperature.
 Demolding
 Post-processing
Main process features
 Well-suited for parts with complex geometries

 Fabrication of small and very large parts
 Easy integration of local reinforcements (dopplers) and inserts
 Good surface quality (on the mold-side)
 Typical fibre volume content: approx. 40%
 Long cycle time
 Low investments
 ‚Open‘ process  Health & safety is a concern!

 Mediocre laminate quality and reproducibility. Part quality strongly
depends on the skills of the technicians
Which of those parts would you fabricate in wet-
lamination technique?
1. Tooling / Mold 2. Airplane structural panel 3. Boot Hull
4. Space antenna 5. F1 Chassis
How relevant are following criteria for the selection
of the appropriate fabrication process?
Criteria
Geometrical complexity ++ -- - - +
Tolerances + ++ = ++ +
Surface quality ++ ++ = + ++
Achievable fibre volume content -- ++ -- ++ +
Mechanical properties -- ++ - ++ +
Laminate quality = ++ -- ++ +
Reproducibility - ++ - ++ +
Investment costs ++ - ++ -- -
Labor expenses - + - -- -
Material costs ++ - ++ -- -
Number of parts p.a. -- = -- -- -
Cycle time -- + -- -- -
Criteria is not Criteria is very
relevant -- - = + ++ relevant
Typical application fields
 Mold construction  Ship hulls
 Wind energy
Wet-lamination technique: Process variants
Vacuum Bag Pressure
Schraubzwinge
Spannrahmen
Dichtung Druck
Verschraubung
gelochtes Blech
fester Deckel Druckstutzen
Rinne für überflüssiges Harz
Druckfolie
Folie
Verstärkung mit Laminat
Trennschicht
Überlauf umlaufende Dichtung
festes Werkzeugunterteil
Ventil zur Laminat
Vakuumpumpe
festes Werkzeugunterteil
Vakuumbehälter für
überflüssiges Harz
Quellen: Ehrenstein, G.W.: Faserverbund-Kunststoffe, Werkstoffe-Verarbeitung-Eigenschaften; Carl Hanser Verlag, München 1992
Process automation example
Scobalit AG, 8604 Winterthur
Contents
 Introduction
 Resin viscosity
Flow in porous media
Pressure driven flow Capillary driven flow

 e.g. Processes: RTM, VARTM,  e.g. Processes:
VARI, etc.
– Pultrusion, filament winding,
hand lamination, prepregging,
etc.
 Darcy‘s law
 Capillary number:
AK u
Q P Ca 
  lv cos 
Flow in porous media - Background
Fluid In Fluid Out

Porous Medium
AK
 Darcy‘s law: Q P

 Fluid flow is dependent on: material permeability (K), fluid viscosity (μ),
and driving pressure ( p)
 Porosity is a function of compaction (required to adjust the fiber volume
fraction of the composite) of the porous media
Injection experiment in a glass tool
Darcy’s experiment
piezometric
tubes
p1
g
p2
sand g
h1
diameter D
perforated plates h2
Darcy’s experiment (1856)
Inside a composite: Computer Tomograph pictures
highlighting the dual-scale nature of the porous media
Micro-scale structure of the bundles showing

Meso-scale structure showing the bundles
the individual fibres within
the bundles.
Schell, J.S.U., Investigation of the Influence of Meso-scale Flow Effects in Liquid Composite Moulding Processes on the Laminate Quality, Diss. ETH Nr. 17044, 2007
Dual-scale structure is influencing the impregnation
process
Mode 1 of the impregnation model
of woven fabrics

of woven fabrics

of woven fabrics
C. Lekakou, M. G. Bader, Mathematical modelling of macro- and micro- infiltration in resin transfer moulding (RTM), Composites Part A 29 (1998) 29–37.
Fiber/Matrix interface development
 Fibre-wetting is a pre-condition
for developing a ‚good‘ interface!
M. Connor, Consolidation Mechanisms and Interfacial Phenomena in Thermoplastic Powder Impregnated Composites, PhD-Thesis No. 1413, EPF Lausanne, 1995
Capillary pressure
Wetting
Benetzung No wetting
Keine Benetzung
Gas phase (1) Gas phase (1)
Liquid phase (2)

Liquid phase (2)
Solid phase (3) Solid phase (3)
 
0    
2 2
Capillary ascension Capillary depression
Wetting of Fibres
“Surface tension”:
dW  J kg N 
  m2 s2  m 

dA  
Equilibrium condition:
2  12 1
12 cos  13   23

 23 
Capillary height:
 13
3
212 cos 
h
gr
Capillary pressure:
F  2r cos   12 2 cos 

P     12  
A r 2 r
Contents
 Introduction
 Resin viscosity
The processing time is depending on the rheology
properties of the matrix
0,700
0,600
0,500 isotherm bei 50°C

Viskosität / Pa*s
0,400 isotherm bei 90°C
0,300
0,200
0,100
0,000
0 60 120 180 240 300
Zeit / s
Curing kinetics
 Addition polymerisation of epoxy

systems is an exothermal reaction

 Q  dt
H ges
 Kamal-Sourour model:
d
dt

 k1  k 2   m  1   n  
 Ei 
 
ki T   Ai e  RT 
 Coefficients can be extracted from

DSC-curves!
Contents
 Introduction
 Resin viscosity
A simple viscosity model
 Viscosity model:
 B 
 C  
 ( , T )  Ae T 
 Castro und Macosko:

C  D
 B
   g 
 ( , T )  A e T   
   
 g 
With:
A, B, C, D: Constants
g: Curing degree of the resin at gelpoint

Processing Thermosets Composites

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Processing Thermosets Composites

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Spring Semester 2017

151-0548-00L Manufacturing of Polymer Composites

Constituent Layup, Manufacturing process Final part &

Physical and chemical processes

Capillary driven Pressure driven Chemical

Fibre volume content

SMC, GMT Filament Winding, Press technologies Autoclave RTM, VARI

Textile Intermediate Textile Multi-axial

 Preparation of fibre layers and cutting to

 Forming takes place by laying/draping the

 Wetting of the fabric

 Curing usually takes place at room

 Preparation of fibre layers and cutting to Surfacing ply

 Preparation of the mold

 Forming takes place by laying/draping the

 Wetting of the fabric Mold reinforcement

 Preparation of fibre layers and cutting to

 Forming takes place by laying/draping the

 Wetting of the fabric

 Curing usually takes place at room

 Preparation of fibre layers and cutting to

 Forming takes place by laying/draping the

 Wetting of the fabric

 Curing usually takes place at room

 Well-suited for parts with complex geometries

 ‚Open‘ process  Health & safety is a concern!

1. Tooling / Mold 2. Airplane structural panel 3. Boot Hull

4. Space antenna 5. F1 Chassis

 Mold construction  Ship hulls

Vacuum Bag Pressure

Scobalit AG, 8604 Winterthur

Pressure driven flow Capillary driven flow

Fluid In Fluid Out

Darcy’s experiment (1856)

Micro-scale structure of the bundles showing

Mode 2 of the impregnation model

Mode 3 of the impregnation model

Gas phase (1) Gas phase (1)

Liquid phase (2)

Solid phase (3) Solid phase (3)

12 cos  13   23

F  2r cos   12 2 cos 

0,500 isotherm bei 50°C

0,400 isotherm bei 90°C

 Addition polymerisation of epoxy

 Coefficients can be extracted from

 Castro und Macosko:

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