history dependent specific volume of (semi- crystalline...
Transcript of history dependent specific volume of (semi- crystalline...
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Dutch Polymer Institute (DPI), Materials Technology (MaTe)Eindhoven University of Technology
history dependent specific volume of (semi-crystalline) polymers
Gerrit W.M. Peters,www.mate.tue.nl
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outline
1. introduction
2. crystallization of polymers- Modelling- pVT-behavior
3. how to measure the influence of flow
4. results
5. conclusions
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Shrinkage characterization of polymers
3
introduction
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Shrinkage characterization of polymers
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Mold
(Product Cavity)
Screw
Heated Cylinder
Raw material input
introduction
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• During cooling:
– thermal contraction– phase changes
Decrease of volume per unit mass
( = specific volume)
Shrinkage / Warpage
introduction
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dimensional stability & accuracy of injection moulded productsamorphous polymers
dimensional stability of PS stored @ 70 0 CPhD Thesis Leo Caspers, 1995
introduction
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dimensional stability & accuracy of injection moulded productssemi-crystalline polymers
introduction
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evolution of yield stress with time: physical ageing
Tom A.P. Engels,Leon E. Govaert, Gerrit W.M. Peters, Han E.H. Meijer
introductionpredicting mechanical performance of polymers
directly from processing conditions
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product
simulation of filling and cooling using MoldFlowTM
processing induced property development
thermal history over thickness
introduction
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resulting yield stress distribution dependence on mold temp.
yield stress varies over thickness!
processing induced property developmentintroduction
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processing induced property development
validation
90 cc/s, melt 285 oC, cooling time 60 s
check mechanical performance
introduction
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both short-term and long-term deformation kinetics are captured !
rate dependent yield stress long-term failure
introductionprocessing induced property development
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experimental numericalvalidation
‘complex’ geometry predict thermodynamic state Sa from IM process
Tm=30˚C Tm=130˚C
mechanical evaluation
Introductionprocessing induced property development
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deformation kinetics also captured for more complex geometries!
rate dependent maximum load long-term failure
introductionprocessing induced property development
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mechanical performance and influence of flow of injection moulded productssemi-crystalline polymers (non solved problem)
introductionprocessing induced property development
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outline
1. introduction
2. crystallization of polymers- Modelling- pVT-behavior
3. how to measure the influence of flow
4. results
5. conclusions
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modelling of crystallizationquiescent and flow-induced crystallization
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quiescent crystallization: Schneider’s equations
modelling of crystallization
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quiescent crystallization: kinetics
modelling of crystallization
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flow-induced crystallization: viscoelastic modelling
modelling of crystallization
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flow-induced crystallization: results of viscoelastic modelling
modelling of crystallization
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outline
1. introduction
2. crystallization of polymers- Modelling- pVT-behavior
3. how to measure the influence of flow
4. results
5. conclusions
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‘Spherulite’
‘Crystals’
Introduction: specific volume
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• Asymptotic pVT-data:– ‘slow cooling’ experiments– empiric
• Coupled crystallization kinetics: – Schneider + Eder– impingement: Avrami– 1 crystalline phase
theory
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crystallization of polymers: pVT-behavior
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crystallization of polymers: pVT-behavior
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crystallization of polymers: pVT-behavior
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crystallization of polymers: pVT-behavior
pressure: 0.1 MPa
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predictions for different cooling rates and high pressures
crystallization of polymers: pVT-behavior
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0.1 [ºC/s] 100 [ºC/s]
crystallization of polymers: pVT-behavior
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outline
1. introduction
2. crystallization of polymers- Modelling- pVT-behavior
3. how to measure the influence of flow
4. results
5. conclusions
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• Observations:– slow developments in modeling specific volume– present models deserve better experimental validation– influence ‘flow’ ?
• Problem definition:– general lack of experimental data for model validation– commercially available equipment not relevant to industrial
processing conditions– no technique present to investigate influence ‘flow’
influence of flow: problem definition
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Shrinkage characterization of polymers
33
• Design and building of a dedicated dilatometer to measure specific volume as a function of thermal-mechanical history
• To quantify the influence of thermal-mechanical history ( P,T,T,γ,γ ) on the specific volume of semi-crystalline polymers
• To perform experiments near industrial processing conditions
• •
a new design: objectives
••
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experimental methods
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Shrinkage characterization of polymers
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A)
B)
C)
experimental methods- design-
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experimental methods- final design-
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experimental methods
- prototype dilatometer-
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• Correction for thermal gradients:
– conduction + crystallization heat
– N homogeneously cooled layers, ∂T/∂x ≤ 1 [°C]
– Over-all specific volume to compare with experiments
– viscous heating neglected
experimental methods- thermal issues-
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Shrinkage characterization of polymers
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• Procedure
– A) Heating ~ 10 oC/min
– B) Holding Tmax ~ 10 min
– C) Pressurizing
– D) Isobaric cooling
– E) Shear flow
T
tP
t
t
.γ
[s-1]
[Pa]
[ºC]A)
B)
D)
C)
E)
experimental procedure
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shearing cooling
experimental methods- testing -
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• Confined Compression(Δx ~ ΔV)
• shear rate ≤ 80 [1/s]• shear ≤ 110 [-]• P ≤ 100 [MPa]• T ≈ 101 - 102 [K/s]
• MTS 858 Mini Bionix(axial-torsional)
(we broke already a few pressure cells)
·
·
experimental methods- summary -
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a new dilatometer
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features of the dilatometer: p
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features of the dilatometer: V
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features of the dilatometer: T
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features of the dilatometer: T●
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features of the dilatometer: Y●
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control software
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control software
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sample preparation
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• Density Gradient Column– reference specific volume
• Optical Microscopy– morphology (10 - 100 μm)
• WAXD– degree of crystallinity– orientation of crystallites
characterization: experimental methods
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computer (automate)manualControl
300 ºC300 ºCTemperature
100 ºC/s100 ºC/sCooling rate
100 MPa100 MPaPressure
200 s-180 s-1Shear rate
no limit (g=135/ round)270º (g=104)Rotation angle
New DesignPrototype
features
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outline
1. introduction
2. crystallization of polymers- Modelling- pVT-behavior
3. how to measure the influence of flow
4. results
5. conclusions
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• Materials:
– iPP-K2XMOD: Mw = 365 [kg/mol], Mw/Mn = 5.4 (Borealis )
• CF- Dilatometer (Gnomix) – (Moldflow)
validation of the set-up
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validation of the set-up
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• Materials:
– iPP-1: Mw = 365 [kg/mol], Mw/Mn = 5.2 ( HD120MO, Borealis )
– iPP-2: Mw = 500 [kg/mol], Mw/Mn = 6.0 ( Stamylan P13E10, DSM )
influence of cooling rate and shear flow
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Shrinkage characterization of polymers
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T
R~130 μm
R~10 μm
R~75 μm
Δν
ΔT
P = 40 MPa
part 1: influence of cooling rate
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Shrinkage characterization of polymers
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- Morphology analysis
• WAXD– ESRF, Grenoble (France)– Materials Beamline ‘ID11’– λ = 0.4956 Å– Beam area = 0.2 x 0.2 mm
• ESEM– Philips XL30 ESEM
‘Prepared’ Sample
influence of shear flow
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influence of shear flowWide Angle X-ray Diffraction (WAXD) patterns (iPP)
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Influence of pressure during flow
P = 20 MPa P = 40 MPa
P = 60 MPa
Material: iPP-1 (Mw = 365 kg/mol)
P = 20 - 60 Mpa
Cooling rate = 1.4 oC/s
Shear rate = 78.0 1/s for 1.5 s
Tγ = 140 oC
T = 140 oC
influence of shear flow
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Shrinkage characterization of polymers
61Measurements: M.E.H.v.d.Beek
influence of shear flowInfluence of temperature during flow
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Shrinkage characterization of polymers
62Measurements: M.E.H.v.d.Beek
influence of shear flowInfluence of temperature during flow
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Influence of temperature during flow
193 oC 154 oC 139 oC
193 oC 154 oC 139 oCiPP-1
iPP-2
influence of shear flow
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0 50 100 150 200 250 3000,0
0,2
0,4
0,6
0,8
1,0
v* [-]
T [C]
P = 20 MPa P = 40 MPa
0 50 100 150 200 250 3000,0
0,2
0,4
0,6
0,8
1,0
P = 40 MPa
v* [-]
T [C]
quiescent T = 250C T = 260C
influence of pressure: nylon 6.6
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influence of pressure & shear flow: HDPE
Temperature of flow
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outline
1. introduction
2. crystallization of polymers- Modelling- pVT-behavior
3. influence of flow
4. conclusions
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– a fully automated dilatometer was built to measure the influence of cooling rate and shear flow on specific volume
– quantitatively measured the influence of thermal-mechanical history on specific volume at (near-) industrial processing conditions
– crystallization kinetics enhanced with: P ↑, T ↓, Mw ↑
– near future: isothermal measurements:
conclusions