Douglas J. Sober 713-503-1558 [email protected]Kaneka Texas Corp 2 Northpoint Drive Suite 200 Houston, TX 77060 www.kanekatexas.com Kaneka Core Kaneka Core - - Shell Toughening Shell Toughening Systems for Thermosetting Resins Systems for Thermosetting Resins
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Kaneka Core-Shell Toughening Systems for … · Kaneka Core-Shell Toughening Systems for Thermosetting Resins. What is Core-Shell Rubber (CSR) ? ... Modified Silicone for Sealants
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• No Depression of Tg.• Wide Cure Window.• Consistent Morphology.• Low Ionic and Surfactant Content.• Extremely Stable.• Compatible / synergistic with Secondary Tougheners.• Nano-size particles do not filter.• Composite parts tend to be very translucent.
How does CSR toughen resins?How does CSR toughen resins?
• Core polymer cavitates on impact dissipating energy. Reduced damage area
• Small, evenly dispersed particlesact as a crack terminator.
• Core polymer relieves inherent stress generated during curing.
Inter-laminarbond & peelstrengthimprovement
Dimensional stability& microcrack resistanceNote: Optimization of particle size and inter-particle
distance (volumetric particle concentration) is critical to achieving the best performance
CSR Manufacturing Process
Epoxy
Solid CSRCan only be broken up to 1500 nm minimum with wide particle size
distribution
KANEKA CSR
Process
Epoxy/CSRKane Ace MX
Agglomeration /Drying
Latex
MX Process
Narrow range of 100 nm particles
Basic Properties of MX system
Core Shell Rubber particles are homogeneously dispersed in epoxy resin with long term stability
Core Shell Rubber particles are homogeneously dispersed in epoxy resin with long term stability
Conventional Solid CSR(10 wt%) in epoxy
New MX CSR(25 wt%) in epoxy
Appearance - Cured system“Transparent”
TEM observation - Cured system
Comparison of Kane Ace MX CSR versus Powder CSR
1µm
MX CSR
Powder CSR
Appearance of MX and CTBN (in DGEBA Epoxy)
No toughener
CSR 7.5 phr
CTBN 7.5 phr
What is Kane Ace MX:What is Kane Ace MX:
Kane Ace MX are concentrates comprised typically of 25% by weight of CSR dispersed in various thermosetting resins. The liquids are easily poured after heating and the individual CSR domains remain uniformly dispersed during storage and formulating.
Kane Ace MX Products:Kane Ace MX Products:
Grade CSR Type / Loading Carrier ResinMX 124 St-Bd 25% Liquid Bis A epoxy (lowest viscosity)MX 125 St-Bd 25% Liquid Bis A epoxy MX 133 St-Bd 25% Liquid Bis F epoxy (lower viscosity)MX 135 St-Bd 25% Low crystallizing liquid Bis F epoxyMX 136 p-Butadiene 25% Liquid Bis F epoxy (lower viscosity)MX 153 p-Butadiene 33% Liquid Bis A epoxyMX 156 p-Butadiene 25% Liquid Bis A epoxyMX 210 St-Bd 25% Epoxidized Phenol NovolakMX 227* St-Bd 25% Epoxidized BPA NovolakMX 338 St-Bd 25% Brominated Di-functional epoxyMX 392 St-Bd 25% Brominated Multifunctional epoxyMX 416 p-Butadiene 25% Multifunctional Epoxy Resin (TGMDA)MX 451 St-Bd 25% Multifunctional Epoxy Resin (TGPAP)MX 554 St-Bd 25% Cyclo-Aliphatic epoxy (MX 601* St-Bd 25% Resole NovolakMX 615 St-Bd 25% Di-allyl BPA (for BMI)MX 660 Siloxane 25% Di-allyl BPA (for BMI)MX 715 St-Bd 25% Polypropylene Glycol carrier (mw 400)MX 717 St-Bd 25% Polypropylene Glycol carrier (mw 1000)MX 719 St-Bd 25% Polypropylene Glycol carrier (mw 2000)MX 960 Siloxane 25% Liquid Bis A epoxy
*Developmental grades not yet available in commercial quantities
Example for Comparative TrialExample for Comparative Trial
Part A:
70 parts liquid Bis A resin 52 parts liquid Bis A resin20 parts epoxy resin B 20 parts epoxy resin B10 parts reactive diluent 10 parts reactive diluent
24 parts MX 125
Part B:
30 parts Part B 30 parts Part B
Mix Ratio Part A to B:
100/30 106:30
Core Shell Concentration:
0% 4.4%
Existing System MX Toughened
Basic Properties of MX system
MX 125 Viscosity as a Function of Concentration
0
20,000
40,000
60,000
80,000
100,000
120,000
140,000
0 5 10 15 20 25 30
CSR concentration (wt%)
Visc
osity
(cps
) 25C
50C
WorkingRange
Kaneka Kane Ace MX®Adhesive Applications
T-Peel Strength Kane Ace MX
ASTM D1876
T-Peel Strength of DGEBA Epoxy/MX 120 System
0
5
10
15
20
25
30
35
T-peel S trength / pli
C S R 0% C S R 5% C S R 10%
Lap-Shear Strength OF Kane Ace MX
Adhesive layer
ASTM D1002
0
1000
2000
3000
4000
5000
6000
Lap Shear PSI
0 % Control 5 % CSR 10 % CSR
Lap-shear Strength of DGEBA Epoxy/MX 120
T-peel Strength of MX 120 vs. CTBN in DGEBA Epoxy
C ontrol5%
10%
C TB N
C SR M aster-batch05
1015202530
35
T-peelStrength/pli
Comparison of CSR and CTBNComparison of CSR and CTBNLap-shear Strength of MX 120 vs.
CTBN in DGEBA Epoxy
Control
5%
10%
C T B N
C SR M aster-batch0
1000
2000
3000
4000
5000
6000
Lap-shearStrength/psi
Kaneka Kane Ace MX®Composite Applications
Types of Fractures
Depending on the stress field in the vicinity of the crack tip, three principle fracture modes are possible: Mode I, Mode II, and Mode III.
Mode I bending is tensile, Mode II is shear, Mode III is tearing
Toughening Effect of Epoxy/ Kane Ace MX SystemToughening Effect of Epoxy/ Kane Ace MX System
Three-Point Bending
force
specimen: 6cm x 1.2cm x 0.5cm
pre-crack: 0.6cm depth by blade-tapping
head speed: 1mm/min.
stress
strain
strength
energy
ASTM 5045 CastingASTM 5528 Reinforced
Fracture Toughness of DGEBA Epoxy/MX 120
00.5
11.5
22.5
3
K1c/ MPam1/ 2
CSR 0% CSR 10%
DDSpiperidine
Fracture Toughness of DGEBA Epoxy/MX 120
0
500
1000
1500
2000
2500
G 1c/Jm 2
C SR 0% C SR 10%
DDS
piperidine
Comparison of CSR and CTBNComparison of CSR and CTBNFracture Toughness and Glass Transition Temperature