robert kultzow trfa 2005 november 15, 2005
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Epoxy Systems For Below Zero Degrees Celsius. Robert Kultzow TRFA 2005 November 15, 2005. Features of Epoxy Resins. High mechanical strength Outstanding dielectric characteristics Excellent adhesive properties Great Chemical resistance Phenomenal thermal endurance. - PowerPoint PPT PresentationTRANSCRIPT
Robert KultzowRobert Kultzow
TRFA 2005TRFA 2005
November 15, 2005November 15, 2005
Epoxy Systems For Below Zero Degrees CelsiusEpoxy Systems For Below Zero Degrees Celsius
Features of Epoxy ResinsFeatures of Epoxy Resins• High mechanical strength • Outstanding dielectric
characteristics• Excellent adhesive
properties• Great Chemical resistance• Phenomenal thermal
endurance
Performance at Lower Performance at Lower Operating TemperaturesOperating Temperatures
• Speed and effectiveness of cure
• Fracture toughness
• Thermal Expansion characteristics
Uses of Epoxies at Lower Uses of Epoxies at Lower Temperatures and Cryogenic Temperatures and Cryogenic
ConditionsConditions
• Nuclear physics apparatus• Super conducting devices comprised of
magnets and transformers• Magnetic imaging devices
Pathways to Development of a Pathways to Development of a Cryogenic SystemCryogenic System
Epoxy Resin Sytem<Title>
Inorganic FillersLow er CTE
Final Cryogenic Epoxy System
Reinforced FibersHigh strength parallel to fiber direction
Chemical M odification of MatrixLim its stresses between metal inserts and epoxy
Epoxy Systems That Exhibit Epoxy Systems That Exhibit Excellent Cryogenic Excellent Cryogenic
PerformancePerformance• System ASystem A• 100pbw - Modified
Bis-A Epoxy• 57pbw - Hardener A• 10 pbw -
Cycloaliphatic Diamine
• System BSystem B• 100pbw – Modified Bis-A
Epoxy• 15pbw – Hardener A• 37pbw – POPDA (High
Molecular Weight)• 20pbw – POPDA (Low
Molecular Weight)• 10pbw – Cycloaliphatic
Diamine
Properties of A and B Properties of A and B Cryogenic SystemsCryogenic Systems
Property System A System B
Viscosity, cps, 25°C 630 1,000
Gel time, min., 25°C 990 1,200
Barcol Hardness 63.5 45.0
Thermal shock, cycles >25 >25
Impact strength, Nm/mm notch
@ 298°K@ 80°K
0.020.01
0.0410.015
Flexural strength, psi@ 298°K@ 77°K@ 4.2°K
12,32540,55529,435
4,64023,200
_Flexural modulus, psi@ 298°K@ 77°K@ 4.2°K
391,0001,044,0001,102,000
101,5001,059,000
-
Thermal Shock Specimen
Epoxy
Steel Bolt
Gel Time vs. Cure SpeedGel Time vs. Cure Speed
• Gel Time is defined as the required time for a system to make an exothermic state change from liquid to solid.
• Cure speed is the time it takes for a system to actually cross link with itself in order to form a lattice structure.
Low Temperature CuringLow Temperature Curing• Phenalkamines -
excellent for low temperature curing
• POPDA – gives excellent properties
• Accelerators such as benzyl alcohol, salicylic acid, and dimethylaminopropyl- amine
Property Amine A Phenalk- amine
Gel time, min., 25°C
66 50
Pencil Hardness 3H 3H
Cure through time (5°C) >24 hours 16 hours
Direct Impact Test (in/lb) 14 12
Cracking of Epoxies in Cracking of Epoxies in Structural ApplicationsStructural Applications
• Epoxies crack in many electrical apparatus due to sudden changes in temperature.
• Cracks usually start in areas of high stress
• High stress areas include places where a metal or ceramic insert is placed.
Fracture ToughnessFracture Toughness• This is measured by
calculating KIc and GIc of a material.
• The above figure illustrates different modes of fracture testing
• The below figure illustrates a double torsion method used on filled materials
[K1c]2 = E* G1c * (1-ν)
Toughening ConceptsToughening Concepts
• Incorporating crack-arresting micro-phases such as fillers, short fibers, micro-voids, glass beads, thermoplastics, and rubbers
• Matrix flexibilization
• Material G1c[J/m2]
• Pure metals
1,000,000• Steel
100,000 Titanium alloys 53,000 Aluminum alloys 30,000• Polypropylene 8000• Polyethersulfone 2500• Rubber toughened-epoxy 2000• Polycarbonate 800• Bis-Aepoxy / DDS 250• Marble 20• Window glass 7
Core-shell TougheningCore-shell Toughening• Incorporates a fine
dispersion of soft particles as a second phase within the epoxy matrix
• Such particles, with sizes less than 1 micron have a core structure that absorbs energy and a shell that provides for good adhesion to the epoxy matrix.
Core-Shell Morphology
Core: Elastomer, high energy absorption
Shell: Thermoplastic, good matrix adhesion
New Development:Shell crosslinked
Particle size < 1 m
Testing Crack Resistance
15034. 3
Specimen for Crack Test
Diverses03/risspey2.ds4
filled epoxy
Thermal Cycle Soak Test
0 10 20 30 40 50 60 70 80 90 100
-60
-50
-40
-30
-20
-10
0
10
20
Tem
pera
ture
[°C]
hours [h ]
d ive rse s0 3/tem ptes t.g rf
2 h
24 h
Tem perature P rofile for H exagonal C rack Test
Results of Soak Testing
+140 +25 0 -20 -40 -50 -600
20
40
60
80
100
HI
T em perature [°C ]
StandardT g = 115-120°C
K IC = 1.7-1.9
T oughenedT g = 115-120°C
K IC = 2.4-2.6
ConclusionsEpoxies noted for:
Excellent mechanical strengthOutstanding dielectric propertiesExcellent chemical resistance
Increased usage in medium and high voltageapplications where subject to hostileenvironments
ConclusionsDifferent approaches are available to formulatorsto improve toughness critical in low temperatureapplications
• Matrix flexibilization• Multiphase toughening