1. “Synthesis and study of a crystalline epoxy resin for high heat resistance”
Pradip K. Dubey*, Hitesh. K. Soni, Mahesh Soni, Samir Kanitkar
Thitikan, Patcharaporn
Aditya Birla Chemicals (Thailand) Ltd- Epoxy Division
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada

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Introduction
Emerging needs
Miniaturization of electronic components
High speed data transfer
Lower dielectric constant and high heat resistance
Possible to apply in lower thickness
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada

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Introduction
High Purity resin
Low melt viscosity
High heat resistance
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TRFA Annual Meeting- Montreal, Canada

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Chemical structure and characteristics
Hydrophobic/ saturated backbone – lower dielectric constant
Higher aromatic content - higher heat resistance
Purity/ symmetry- crystalline / lower melt viscosity
High functionality/ high crosslink density – high heat resistance
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TRFA Annual Meeting- Montreal, Canada

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High performance resins
Difunctional DCPD type epoxy resin
Multifunctional DCPD type epoxy resin
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TRFA Annual Meeting- Montreal, Canada

6. High performance resins
Difunctional 1,5-Dihydroxy Naphthalene type epoxy resin
Tetra functional Naphthalene type epoxy resin
Difunctional Dihydroxy Biphenyl type epoxy resin
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada

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Epoxy resins used for present study
Diglycidyl ether of Bisphenol-A (DGEBA)- YD 128
Epoxy Phenol Novolac (EPN)- YDPN 638
Epoxy Tetramethyl Bisphenol-S (ETMBPS)
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TRFA Annual Meeting- Montreal, Canada

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Preparation of ETMBPS
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Properties of various epoxy resin used for present study
Properties
YD 128
YDPN 638
ETMBPS
Epoxy equivalent weight (g/eq)
188.0
175.1
216.7
Hydrolysable chlorine (% w/w)
0.0574
0.072
0.0034
Total chlorine (% w/w)
0.17
0.18
0.062
Viscosity (oC), cPs
12200
@25oC
29094
@ 52oC
119.1
@ 120oC
Number average molecular weight (g/mol)
(Functionality)
380
(2)
600
(3.6)
421
Melting point (oC) -
114
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TRFA Annual Meeting- Montreal, Canada

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GPC of ETMBPS
DSC of ETMBPS
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TRFA Annual Meeting- Montreal, Canada

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Physical form of various epoxy resin used for present study
Epoxy Phenol Novolac (EPN)
Diglycidyl ether of Bisphenol-A (DGEBA)
Epoxy Tetramethyl Bisphenol-S (ETMBPS)
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada

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Melt viscosity Vs. Temperature of various epoxy resins
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TRFA Annual Meeting- Montreal, Canada

13. Curing agents used for present study
Phenol Novolac (PN)
HRJ 1583
Tris(4-hydroxyphenyl) methane (THPM)
3,3’-Diaminodiphenyl Sulphone (3,3’-DDS) Omicure 3,3’-DDS
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada

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Properties of curing agent used for present study
Properties PN
THPM
DDS
Hydroxyl equivalent weight (g/eq)
(Functionality)
106
(3.6) 97
(3) -
Amine equivalent weight (g/eq) 62
(4)
Softening point (oC) 78
102
Melting point (oC)
177
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada

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Mixing ratio used for laminate preparation
Resin
Hardener
Catalyst
Ratio (Part by weight)
YD 128
3,3-DDS
Anchor 1040
100
33.0 1
YDPN 638
35.0
ETMBPS
28.6
HRJ 1583
TPP
56.4
0.5
60.5
49.0
THPM
51.6
55.4
45.0
Binder- Fiber ratio : 30: 70
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TRFA Annual Meeting- Montreal, Canada

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TRFA Annual Meeting- Montreal, Canada

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% Weight loss Vs. Temperature by TGA
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TRFA Annual Meeting- Montreal, Canada

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Stress distribution during fracture by Impact
YD 128/ DDS/ Anchor 1040
YDPN 638/ DDS/ Anchor 1040
ETMBPS/ DDS/ Anchor 1040
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TRFA Annual Meeting- Montreal, Canada

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YD 128/ HRJ 1583/ TPP
YDPN 638/ HRJ 1583/ TPP
ETMBPS/ HRJ 1583/ TPP
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TRFA Annual Meeting- Montreal, Canada

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YD 128/ THPM/ TPP
YDPN 638/ THPM / TPP
ETMBPS/ THPM / TPP
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TRFA Annual Meeting- Montreal, Canada

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Electrical properties of various systems
Property
Test Method
Unit
YD128/ DDS/ Anchor 1040
YDPN 638/ DDS/ Anchor 1040
ETMBPS / DDS/ Anchor 1040
YD128/ HRJ1583/ TPP
YDPN638/ HRJ1583/ TPP
ETMBPS / HRJ1583/ TPP
YD128/THPM / TPP
YDPN638/ THPM / TPP
ETMBPS / THPM / TPP
Volume resistivity
IEC60093
Ohms-cm
1016
Surface resistance
Ohm
1013
Dielectric constant
IEC60250 -
3.50
4.30
3.23
3.85
3.79
3.71
3.28
2.51
Dielectric loss %
1.5
1.9
1.6
1.0
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TRFA Annual Meeting- Montreal, Canada

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TRFA Annual Meeting- Montreal, Canada

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Conclusion:
High purity ETMBPS exhibits lower melt viscosity in uncured form.
ETMBPS shows higher Tg compared to conventional epoxy resin system.
ETMBPS cured systems shows better dielectric constant and dielectric loss compared to other systems.
Mechanical properties of ETMBPS systems are comparable or lower compared to other systems.
Properties at elevated temperature need to be studied further to establish true potential of this resin
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada

27. Potential application areas
Laminates involving high temperature and electrical properties
Electronic molding compounds
Powder coating of electrical and electronic components
One component adhesives
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TRFA Annual Meeting- Montreal, Canada

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Thank You
Sept,11, 2006
TRFA Annual Meeting- Montreal, Canada