prepreg compression molding for high volume … · 2014-08-31 · momentive specialty chemicals,...
TRANSCRIPT
Automotive Composites Conference Exhibition
Novi, September 09-11 2014
Prepreg Compression Molding for high volume manufacturing of Lightweight Epoxy Automotive
Structures
Advances in Thermoset Composites
Principal Author: Alex Schmidt Presenter: Stephen Greydanus
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Momentive Specialty Chemicals, Inc. Confidential Information
Momentive is a $7.8 Billion Specialty Chemicals and Materials Company
Momentive Heritage Businesses Momentive Today
Sales: US $7.8 Billion Headquarters: Columbus, Ohio USA Manufacturing facilities: 100+ worldwide Employees: 10,000 Customers: Serving 20,000 around the globe
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Epoxy ResinsGlobal
Specialty Epoxy
BaseEpoxy
QuartzGlobal
SiliconesGlobal
Oilfield Proppant ResinsGlobal
Forest Product Resins Global
Versatic™ Acids & Derivatives Global
Phenolic Specialty ResinsGlobal
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Composite Technology Shifts in Support of Higher Volume and/or Higher Performance
Prepreg
Structural SMC
SMC
Liquid Compression Molding and
RTM
Perf
orm
ance
Capable Annual Build Rate 3
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Different CFRP molding processes
High Pressure RTM-Process Fast cycle times can be achieved with newly developed fast cure resin systems. Production of difficult 3D shapes possible
Prepreg Compression Molding Easy to control compression molding process. Fast cure cycles, high glass transition temperatures and outstanding mechanical properties
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Prepreg compression molding process and in-process recycling route
60 sec 10 sec 180-300 sec 10 sec
Total cycle time: 260-380 sec
Cutting of waste into 25-50mm pieces
In-process recycling route Allows to use prepreg waste as high quality molding compound
Molding Compound Sheet
Place charge in mold (~80% coverage)
Prepreg Compression Molding Fast process approaching cycle times of high pressure RTM
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Process parameters of Prepreg compression molding and high pressure RTM
Prepreg Compression Molding
High Pressure RTM
Raw materials Newly developed fast curing prepreg system with CF or GF reinforcement
Dry Fabric (NCF, Weave, choped fiber mat…); Fast cure 2 component resin
Achievable Fiber volume content (FVC)
≤ 65% ≤ 55%
Resin System Epoxy Epoxy
Preforming One sided tool + vacuum or two sided tool + press (no heating)
Heated two sided tool + press
Molding pressure 10-50bar 10-80bar
Cure time at °C 3-5 min at 135-170°C 1.5-5 min at 110-130°C
Typical Tg 135-160°C 110-130°C
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Advantages of Prepreg compression molding process
Fast cycle times (<4min) possible Easy to control process Utilization of existing equipment (presses) In house prepreg as viable approach to further reduce cost Hot melt system (not requiring any solvents) Fast and easy preforming Can be used to produce structural as well as exterior parts/components Hybrid parts with metal or SMC possible No handling of dry fibers VOC-free systems
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Automotive applications for prepregs
Dash panel
Hood
Body side
Roof
Inner Structure
A, B & C Pillars Body & Structural parts
Underbody & floor
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EPIKOTE™ Resin 06425 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06825
Possible Applications: Structural applications Reinforcement for metal parts e.g.
B-pillar
Good surface quality for exterior applications (may require adjusted molding cycle)
Cure temperature
Cure time
Tg midpoint, DSC 2nd run
Tg, DMA E´onset
135-150°C 3-5 min 135°C 135-140°C
Momentive fast cure resin systems
Cure temperature
Cure time
Tg midpoint, DSC 2nd run
Tg, DMA E´onset
150-170°C 3-5 min 150°C 150-160°C
EPIKOTE™ Resin 06465 EPIKURE™ Curing Agent 06465
EPIKURE™ Catalyst 06865
Possible Applications: Good surface quality + fast cure
cycle for exterior applications
Good mechanical properties for structural applications
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100
1,000
10,000
100,000
1,000,000
10,000,000
40 50 60 70 80 90 100 110 120
Visc
osity
[mPa
s]
Temperature [°C]
Viscosity of new resin systems
EPIKOTE™ Resin 06465 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06865
EPIKOTE™ Resin 06425 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06825
Heating rate 2K/min
Resin viscosity has been optimized for compression molding process • Controlled resin flow leads to homogenous parts with good surface quality • Faster curing than standard prepreg formulations
Conventional Prepreg System
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Storage stability at 20°C
Uncured Tg determined by DSC (10K/min)
Prepreg resin systems exhibit good storage stability at ambient temperatures as shown by the evolution of uncured Tg over time
• Shelf life at ambient temperature: > 2 weeks • Shelf life at -18°C: 6 months
0 1 2 3 4 5 6 7 8 9
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0 2 4 6 8 10 12 14 16
Unc
ured
Tg
[°C]
time [d]
EPIKOTE™ Resin 06425 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06825
EPIKOTE™ Resin 06465 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06865
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Fast cycle time demonstrated by Dielectric Analysis
2 4 6 8 10 12 14 16Time /min
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
10.5
Log ion visc. /Ohm*cm
60
80
100
120
140
Temp. /°C
-2.0
-1.5
-1.0
-0.5
0.0
0.5
1.0
d(Log ion visc)/dt /((Ohm*cm)/min)
Momentive Prepreg+CF mit TMS gemessen
Log ion visc. (1 Hz)
Log ion visc. (10 Hz)Log ion visc. (100 Hz)Log ion visc. (1 kHz)
Log ion visc. (10 kHz)d(Log ion visc)/dt (1 Hz)
Temp.
Temp.
End: 3.0 min
Percent Cure: 99.594 %Percent Cure: 91.894 %
Peak: 1.5 min
Dielectric analysis - measuring changes in the electrical properties of polymers during processing - is used to investigate the curing behavior of thermosetting resin systems. Measurements taking directly inside the compression mold show the fast cure properties of the resin system.
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Fast cycle time video
Video containing: 1. Preform placement 2. Press close 3. Press opening 4. Demold Ca. 90sec (time lapse for cure process)
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Retention of flexural modulus at elevated temperatures
50
55
60
65
70
75
80
85
90
95
100
100 110 120 130 140 150 160 170 180
Rela
tive
Flex
. Mod
ulus
[%]
Temperature [°C]
Easy de-molding possible
Sufficient stiffness for painting and adhesive bonding
Modulus retention of High Tg system allows painting and adhesive bonding processes at temperatures between 150C and 175C
EPIKOTE™ Resin 06425 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06825
EPIKOTE™ Resin 06465 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06865
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Momentive Specialty Chemicals, Inc. Confidential Information
Momentive fast cure prepreg properties
Process parameters Unit EPIKOTE™ Resin 06425 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06825
EPIKOTE™ Resin 06465 EPIKURE™ Curing Agent 06465 EPIKURE™ Catalyst 06865
Test Method
Molding temperature °C 135-150 150-170
Curing time min 3-5 3-5
Glass Transition Temperature
Midpoint DSC 2nd run
E´onset DMA
°C
°C
135°C
135-140°C
155-158°C
153-160°C
ISO 11357-1
Prepreg Tack - Very low Very low
Shelf life 23 °C
-18 °C
Weeks
months
2
6
2
6
Tack life @ 23°C days 5 5
ILSS pure UD laminate (FVC ~59%) MPa 91 90 ISO 14130
Flexural Strength pure UD laminate (FVC ~59%)
MPa 1610 1654 ISO 14125
Flexural Modulus pure UD laminate (FVC ~59%)
GPa 108 110 ISO 14125
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Application technology examples
R-Class roof segment:
Flat panel – Compression molded Roof segment- Compression molded
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Paint system used for demonstrator parts
Sanding P800
Primer and Basecoat
Sealer
Clear coat
UD CF surface
Clear coat contains Cardura™ Glycidyl ester monomer 17
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E-Coat simulation (parts stable up to 200°C)
Demonstrator part was heated up to 200°C for 30 min to simulate E-Coat Part showed no deformations and was successfully painted
Small panel heated up to 210°C for 2 hours As result part only shows slight yellowing
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Prepreg scrap in-process recycling
Prepreg waste resulting from the cutting of preforms can be recycled as high quality molding compound
• Waste is cut into pieces of 25 – 50mm length • The resulting material can be placed into a mold and
compression molded (SMC like process) • Approximately 80-90% of mold need to be covered to achieve good results • Parts exhibit good mechanical properties and high heat resistance • Molding compound can be used in combination with prepreg to
produce hybrid parts
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Conclusion
New prepreg systems allow rapid manufacturing of automotive parts due to fast cure cycles
Prepreg compression molding can be complementary offering to RTM Suitable for structural and exterior applications
Systems offer:
• Good storage stability • High mechanical performance • High glass transition temperature • Good surface quality
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Momentive Specialty Chemicals, Inc. Confidential Information
EPON™ Epoxy Resins EPIKOTE™ Epoxy Resins EPIKURE™ Curing Agents
Heloxy™ Additives are registered trademarks of
Momentive Chemicals Inc. or an affiliate of Momentive
Specialty Chemicals Inc.
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Momentive Specialty Chemicals, Inc. Confidential Information
DISCLAIMER The information provided herein was believed to be accurate at the time of preparation or prepared from sources believed to be reliable, but it is the responsibility of the user to investigate and understand other pertinent sources of information, to comply with all laws and procedures applicable to the safe handling and use of any product of Momentive Specialty Chemicals Inc. or Momentive Performance Materials Inc. and/or their respective subsidiaries (individually, and collectively, “Momentive”) and to determine the suitability of any Momentive product for its intended use. All products supplied by Momentive are subject to Momentive’s terms and conditions of sale. MOMENTIVE MAKES NO WARRANTY, EXPRESS OR IMPLIED, CONCERNING THE PRODUCT OR THE MERCHANTABILITY OR FITNESS THEREOF FOR ANY PURPOSE OR CONCERNING THE ACCURACY OF ANY INFORMATION PROVIDED BY MOMENTIVE, except that the product shall conform to Momentive’s specifications. Nothing contained herein constitutes an offer for the sale of any product.
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