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Joon-Pyo JeunKorea Atomic Energy Research Institute
Phil-Hyun Kang*, Young-Chang Nho
Effect of EB Effect of EB Effect of EB Effect of EB iriririrradiation radiation radiation radiation on the physicochemical characteristics on the physicochemical characteristics on the physicochemical characteristics on the physicochemical characteristics of polyimide film for aerospace materialof polyimide film for aerospace materialof polyimide film for aerospace materialof polyimide film for aerospace material
ContentContentContentContent
• Historical background of Polyimide
• Radiation process (EB curing)
• Effect of EB radiation on Polyimide film
Map of PlasticsMap of PlasticsMap of PlasticsMap of Plastics
PI
PEEK
LCP
PPS
PAI
PEI PES
PSF
PA POM
PBT PETPC
m-PPO
PAR
PE PP ABS PS
PMMA
CrystallineCrystallineCrystallineCrystalline AmorphousAmorphousAmorphousAmorphousCommodity Plastics
Engineering Plastics
Super Engineering Plastics
Price
High High
Heat resistance
LowLow
Development of Development of Development of Development of PolyimidesPolyimidesPolyimidesPolyimides (PI)(PI)(PI)(PI)
DuPontDuPontDuPontDuPontKaptonVespelPyralin
NASANASANASANASA(PI3N)
DynamitDynamitDynamitDynamitNobelNobelNobelNobel(PEsI)
AmocoAmocoAmocoAmoco(PAI)
TRWTRWTRWTRW(PMR-15)
GEGEGEGE(PEI)
Injection moldable PI
UBEUBEUBEUBE(UpilexUpimol)
NissanNissanNissanNissanJSRJSRJSRJSR
HitachiHitachiHitachiHitachi(PI coatingsfor LCD and
semiconductor)
1962
1962
1970
1972
1982
1984
1990~Film,
Molding
Adhesives
Composites
Coatings
N N
O
O O
O
O
n
Characteristics of PICharacteristics of PICharacteristics of PICharacteristics of PI• Structure of typical polyimide: Kapton
• Advantages– Excellent high temperature mechanical performance– Very high tensile and compressive strength– Outstanding bearing and wear properties– Very high purity– Good chemical resistance
• Disadvantages– Difficult to fabricate and require venting of volatiles– Hydroscopic and subject to attacks by alkaline– Comparatively high cost
Typical ApplicationTypical ApplicationTypical ApplicationTypical Applicationssss of PI (1)of PI (1)of PI (1)of PI (1)
•Electric motor and generator insulation
•Flat cable and wire insulation•Magnet wire and capacitor insulation
•Magnetic and pressure sensitive tapes and tube
Electric
•Flexible printed circuit board (FPCB)•Tape automated bonding (TAB)•Bar code label•Spiral tubes•Masking tapes
ElectronicApplicationsFields
FPCBFPCBFPCBFPCB((((www.desow.com/Upfiles)
Magnetic Wire Magnetic Wire Magnetic Wire Magnetic Wire (www.madewww.madewww.madewww.made----inininin----china.comchina.comchina.comchina.com) Flexible flat cableFlexible flat cableFlexible flat cableFlexible flat cable(www.indiamart.com/chainelectronicswww.indiamart.com/chainelectronicswww.indiamart.com/chainelectronicswww.indiamart.com/chainelectronics)
Typical ApplicationTypical ApplicationTypical ApplicationTypical Applicationssss of PI (2)of PI (2)of PI (2)of PI (2)
•Vacuum bags in fabrication of advanced resin matrix composite
•Traction belts on computer printers
•Heating elements and insulator
Composite
•Diaphragms•Alternator heat insulator pads•Sensor and switches•Seals and gasket•Spark plug boot•Speaker part•Disposal pin carrier •3 Radiator plug
Automotive
SpeakerSpeakerSpeakerSpeaker((((www.autotoys.comwww.autotoys.comwww.autotoys.comwww.autotoys.com)Switching systemSwitching systemSwitching systemSwitching system((((www.solvayadvancedpolymers.comwww.solvayadvancedpolymers.comwww.solvayadvancedpolymers.comwww.solvayadvancedpolymers.com) Check ballCheck ballCheck ballCheck ball((((www.plalution.com/4.htmlwww.plalution.com/4.htmlwww.plalution.com/4.htmlwww.plalution.com/4.html)
Traction beltTraction beltTraction beltTraction belt((((www.serpent.comwww.serpent.comwww.serpent.comwww.serpent.com) Dielectric substrate Dielectric substrate Dielectric substrate Dielectric substrate ((((http://http://http://http://www.fraivillig.comwww.fraivillig.comwww.fraivillig.comwww.fraivillig.com)
Typical ApplicationTypical ApplicationTypical ApplicationTypical Applicationssss of PI (3)of PI (3)of PI (3)of PI (3)•Wire and cable insulation•Motors/alternators (insulation)•Smoke hoods•Composite bagging film•Cockpit sun shade•Multilayer thermal blankets (satellite)•Speakers (airports) and acoustic insulation•Antenna system (satellite)
Aerospace
www.algor.com/news_pub/cust_app/srs/srstech.aspwww.algor.com/news_pub/cust_app/srs/srstech.aspSatellite antenna systemSatellite antenna systemSatellite antenna systemSatellite antenna system
Cockpit sun shade Cockpit sun shade Cockpit sun shade Cockpit sun shade ((((www.bizbuzzmedia.comwww.bizbuzzmedia.comwww.bizbuzzmedia.comwww.bizbuzzmedia.com) Acoustic insulation Acoustic insulation Acoustic insulation Acoustic insulation ((((www.ferret.com.auwww.ferret.com.auwww.ferret.com.auwww.ferret.com.au)
Chemical structures Chemical structures Chemical structures Chemical structures (commercially(commercially(commercially(commercially available)available)available)available)• AURUM (MITSUI)
• ULTEM (GE)
• UPILEX-R (UBE)
• UPILEX-S (UBE)
• KAPTON (DuPont)
• KEVLAR (DuPont)
N N
O
O O
O
O O
n
N
O
O
O
C
CH3
CH3
O
N
O
O
n
N
O
O
N
O
O
O
n
N
O
O
N
O
O
n
N N
O
O O
O
O
n
n
C
O
C
O
HN
HN
• A form of energy that is emitted from a source and travels in the form of waves or particles through a medium, eg air or a vacuum.
NonNonNonNon----Ionizing radiationIonizing radiationIonizing radiationIonizing radiation : microwaves, IR, radio frequenciesIonizing radiationIonizing radiationIonizing radiationIonizing radiation : α, β, neutron, electron, gamma, X-ray, UV
Non-ionizing radiation Ionizing radiation
Radio frequencies Heat GammaMicrowaves X-rays
Infra red Ultraviolet
Visiblelight
What is Radiation ?What is Radiation ?What is Radiation ?What is Radiation ?
---- The electromagnetic spectrumThe electromagnetic spectrumThe electromagnetic spectrumThe electromagnetic spectrum
Electron Beam ProcessElectron Beam ProcessElectron Beam ProcessElectron Beam Process• Electron beam process creates useful
changes in material properties and performance, such as polymer crosslinkingand chain scissioning.
• Electron beam process is also widely used for medical device sterilization, cosmetics sterilization, and pharmaceutical sterilization.
Electron Beam Curing ProcessElectron Beam Curing ProcessElectron Beam Curing ProcessElectron Beam Curing Process• Nonthermal, nonautoclave curing
method that uses high-energy electrons to initiate polymerization and cross linking reactions.
Comparison of radiation and Comparison of radiation and Comparison of radiation and Comparison of radiation and thermal curing thermal curing thermal curing thermal curing
Environmentally hazardous materials
Fire hazard
Adhesion to different substrate
Damage to sensitive substrate
Chemical resistanceSpeed
Space requirementsRunning costs
Energy consumption
OOXOOHealth &
Safety
XO
XOXO
Technical
XOXOXOXO
Commercial
ThermalUVEBFactor
O : Advantage : Intermediate X : Disadvantage
ExperimentalExperimentalExperimentalExperimental• Materials
– Polyimide film (Kapton HN, 5mil, DuPont)
• Irradiation– Electron beam– Nitrogen atmosphere– Energy of 1.14 MeV, 4 mA– Total radiation dose : 0.2~3.8 x 104 kGy
CharacterizationCharacterizationCharacterizationCharacterization• Dynamic Mechanical
Analyzer (DMA)– Storage/loss modulus– Tan delta
• Tensile properties– Tensile strength– Young’s modulus
• Thermogravimetricanalysis (TGA)– Decomposition temp.– Residue
• Electrical properties– Dielectric constant– Conductivity– LCR meter17.25
17.2517.2517.2517.25
Typical DMA curves of PITypical DMA curves of PITypical DMA curves of PITypical DMA curves of PIββββ2222 relaxationrelaxationrelaxationrelaxation Glass relaxationGlass relaxationGlass relaxationGlass relaxation
0 100 200 300 400 500
500
1000
1500
2000
2500
3000
3500
4000
30
40
50
60
70
80
90
100
0.015
0.020
0.025
0.030
0.035
0.040
0.045
0.050
0.055
0.060
Ta
n d
elta
Lo
ss m
od
ulu
s (M
Pa
)S
tora
ge
mo
du
lus (
MP
a)
Temperature (oC)
Tan delta curves of PITan delta curves of PITan delta curves of PITan delta curves of PI
100 200 300 400
0.015
0.020
0.025
0.030
0.035
0.040
0.045
0.050
0.055
0.060
Ta
n d
elt
a
Temperature (oC)
Control
1.5 x 104 kGy
Relaxation temperatureRelaxation temperatureRelaxation temperatureRelaxation temperature
100
110
120
130
140
150
1.5 x 104
0.5 x 104
1.0 x 104
ββββ2 relaxation
Glass relaxation
Radiation dose (kGy)
Tem
pera
ture
(oC
)
0.0400
410
420
430
440
450
Te
mp
era
ture
(oC
)
Values of tan delta (Glass relaxation)Values of tan delta (Glass relaxation)Values of tan delta (Glass relaxation)Values of tan delta (Glass relaxation)
0.046
0.048
0.050
0.052
0.054
0.056
Ta
n d
elt
a
Radiation dose (kGy)
0.0 0.5 X 104 1.0 X 10
41.5 X 10
4
Mechanical PropertiesMechanical PropertiesMechanical PropertiesMechanical Properties
0
5
10
15
20
1.5 x 104
1.0 x 104
0.5 x 104
Radiation dose (kGy)
Ten
sil
e s
tren
gth
(kg
f/m
m2)
0
80
120
160
200
240
280
320
Mo
du
lus (k
gf/m
m2)
Thermal stabilityThermal stabilityThermal stabilityThermal stability
a Thermal decomposition temperature (on-set) from TGA measurement, scan rate: 10 oC/min, N2 protectionb Temperature at 5% weight loss from TGA measurementc Temperature at 10% weight loss from TGA measurement
58.10580.82557.89570.671.5
59.80582.10560.08571.251.0
60.79583.04562.42571.170.4
61.41583.50563.58571.420
Residue
(%)
T10
(oC)c
T5
(oC)b
Td
(oC)a
Radiation
dose
(x10-4 kGy)
200 300 400 500 600 700 800
60
70
80
90
100
Weig
ht
(%)
Temperature (oC)
Control
0.4 X 104 kGy
1.0 X 104 kGy
1.5 X 104 kGy
Electric propertiesElectric propertiesElectric propertiesElectric properties
-2 0 2 4 6 82.6
2.8
3.0
3.2
3.4
control 8,000 kGy 15,000 kGy
25,000 kGy 33,000 kGy 38,000 kGy
Die
lec
tric
co
ns
tan
t
log f
-2 0 2 4 6 810
-17
10-15
10-13
10-11
10-9
10-7
10-5
Control
8,000 kGy
15,000 kGy
25,000 kGy
33,000 kGy
38,000 kGyC
on
du
ctiv
ity (
ΩΩ ΩΩ-1cm
-1)
log f
SummarySummarySummarySummary• Polyimide films show extensive radiation resistivity• Irradiation leads to decrease in the β2 relaxation
temperature and the thermal decomposition temperature
• The tensile strength decrease insignificantly and Young’s modulus tends to increase slightly with dose
• A significant change of the dielectric constant is observed after electron beam irradiation
• Polyimide is sufficiently endurable to survive the high energy irradiation and temperature fluctuations present in space environments
Brownian movement (motion)Brownian movement (motion)Brownian movement (motion)Brownian movement (motion)• Brownian motionBrownian motionBrownian motionBrownian motion is the random movement of
particles suspended in a liquid or gas or the mathematical model used to describe such random movements, often called a particle theory.
• The mathematical model of Brownian motion has several real-world applications. An often quoted example is stock market fluctuations. Another example is the evolution of physical characteristics in the fossil record
LRC meterLRC meterLRC meterLRC meter
PI filmPI filmPI filmPI film
Stainless steelStainless steelStainless steelStainless steel
Cylindrical instrumentCylindrical instrumentCylindrical instrumentCylindrical instrument
TerminologyTerminologyTerminologyTerminology
• Glass transition temperature– When an amorphous polymer is heated, the
temperature at which it changes from a glass to the rubbery form is called the glass transitionglass transitionglass transitionglass transition
– SSSSegmental motion occurringegmental motion occurringegmental motion occurringegmental motion occurring
• Secondary beta relaxation– The rotation or oscillation of functional groupsrotation or oscillation of functional groupsrotation or oscillation of functional groupsrotation or oscillation of functional groups
occur