Adhesion Performance of UV-Crosslinked SBS-Based PSA - Effects of SIS Contents

2005 Adhesion Conference on Adhesion
Adhesion Performance of UVcrosslinked SBS-based PSA : Effects of SIS contents

Dong-Hyuk Lim1, Hyun-Sung Do1, Hyun-Joong Kim1, Goan-Hee Yoon2
1Lab.
of Adhesion & Bio-Composites, Major in Environmental Materials Science, Seoul National University, Seoul 151-921, Korea 220-10, Anyang-7 dong, Manan-gu, Anyang-shi, Kyonggi-do, Korea
2Vixxol,
hjokim@snu.ac.kr / www.adhesion.org
www.adhesion.org
Introduction
Classification of PSA manufacture
Solution-borne Emulsion (Water-borne)
PSA
Hot melt (SIS/SBS) Irradiation (UV) UV-polymerizable UV-crosslinkable
Lab. of Adhesion & Bio-Composites
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Introduction
UV-curable Pressure Sensitive Adhesive
Overall process
PSA UV-curing
Coating Wind-up
Compositions 1. Oligomer + Monomer + Tackifier + Photoinitiator System 2. Block copolymer + Monomer + Photoinitiator System 3. Rubber System, Acrylic Hot Melt System
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Introduction
SBS based PSA
High solubility parameter Harder polymers More difficult to tackify High entanglement Good heat resistance
SBS/SIS based PSA
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Introduction
Block copolymer based UV curing system
polystyrene polybutadiene polystyrene
SBS
Semi-Interpenetrated Network
UV
RSH (thiol)
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Purpose of this study
SBS block copolymer Adhesion Performance of UV-crosslinkable hotmelt PSA
SIS block copolymer
Thiol-ene polymerization
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Experimental
Materials
SIS : Vector 4111 (Exxonmobil) SBS : D KX-405-CP (Kraton)
CH2 CH n CH2 CH CH CH2 x CH2 CH CH CH2 m CH2 CH n
Chemical structure of UV curable SBS with vinyl pendant group
Photoinitiator : Micure BK-6 (2,2-dimethoxy-2-phenyl acetonphenone) from Miwon Commercial Co. Photocrosslinker : TRIS (trimetylolpropane mercaptopropionate) Aldrich
O CH 2 O CH 3 CH 2 C C CH 2 CH 2 SH C O CH 2 O C O CH 2 CH 2 SH CH 2 CH 2 SH
CH 2 O
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Experimental
UV-crosslinkable hotmelt PSA composition
SIS IB1 IB2 IB3 IB4 0 7.5 15 22.5 SBS 30 22.5 15 7.5 Tackifier 50 50 50 50 Oil 20 20 20 20
1TRIS 2PI
4.5 4.5 4.5 4.5
9 9 9 9
1. TRIS : Photocrosslinker TRIS (trimetylolpropane mercaptopropionate) 2. PI : Photoinitiator Micure BK-6 (2,2-dimethoxy-2-phenyl acetonphenone)
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Experimental
Film Casting
Automatic applicator No. 22 bar applicator
UV irradiation
UV lamp : high-pressure mercury lamp (100W/cm2, main wavelength : 365nm) UV dose : 0, 200, 600, 1000, 1400 1800 mJ/cm2
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Experimental
FTIR-ATR
Equipment : Nicolet Magna 550 Series II Resolution : 8 cm-1
Pressure plate
Pressure plate Substrate UV --cured film UV Ccured film oating

45o Horizontal ATR crystal
Infrared beam
Gel contents
W24 Gel contents (%) = 100 W0
W24 : weight after dipping for 24 hrs W0 : weight before dipping
Toluene Film
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Experimental
Probe Tack
5mm stainless steel cylinder Contact force : 100g Dwell time : 1 sec. Separation rate : 60mm/min
Peel Strength
Peeling angle : 180 Separation rate : 300mm/min
Peel Strength
Debonding Force force
Time
Start up region
Operation region
Bonding force
Distance Peeled
Bonding process Debonding process Lab. of Adhesion & Bio-Composites
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Experimental
Shear Adhesion Failure Temperature (SAFT)
Constant load : 1kg Heating rate : 0.4 /min
SUS SUS
Shear Failure
PSA Specimen
Constant Load Constant Load
Temp. Checked
Oven
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Results and Discussion
Characteristic peak of 910.8 cm-1, 964.7 cm-1
Sites of Chemical Reaction

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Efficiency of UV curing by thiol-ene polymerization
UV dose : 0, 200, 1000, 2200 mJ/cm2
1.00
1.1
0.95 0.90 0.85
1.0
0.9
0.8 Absorbance
910.8
cm-1
Absorbance
0.80 0.75 0.70 0.65 0.60 0.55 0.50
910.8 cm-1
0.7
0.6
0.5
0.45
964.7 cm-1
0.4
964.7 cm-1
950 Wavenumbers (cm-1) 900
0.40 0.35 0.30 0.25
0.3
0.2 0.1 1000
0.20 0.15 1000 950 Wavenumbers (cm-1) 900
Only SBS
SBS+Photoinitiator +TRIS
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Gel content
100 80
SBS SBS+PI SBS+PI+TRIS
Gel content (%)
60 40 20 0 0 400 800 1200 1600

2
2000
2400
UV dose (mJ/cm )
Gel contents of UV crosslinked SBS

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Mechanism of Thiol-ene polymerization
Photoinitiator
hv
R.
CH2 CH CH2 CH CH2 CH CH2 CH
CH2 CH CH2 CH R CH2 CH CH2 . CH
SBS & Photoinitiator
SBS & Photoinitiator & Photocrosslinker

CH2 CH
Inter reaction
CH2 CH R CH2 CH
CH2
Intra reaction
.CH
CH2
CH
CH2 CH CH2 CH R CH2 CH CH2 CH CH2 CH
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Probe tack
Probe tack of SBS/SIS based UV curable PSA SBS+SIS+PI
1000 800
No TRIS SIS:SBS=0:30 SIS:SBS=7.5:22.5 SIS:SBS=15:15 SIS:SBS=22.5:7.5
SBS+SIS+PI+TRIS
1000
TRIS SIS:SBS=0:30 SIS:SBS=7.5:22.5 SIS:SBS=15:15 SIS:SBS=22.5:7.5
800
Probe tack (gf)
600 400 200 0 0 400 800 1200

2
Probe tack (gf)
600 400 200 0
1600
2000
400
800
1200
2
1600
2000
UV dose (mJ/cm )
UV dose (mJ/cm )
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Peel strength
Peel strength of SBS/SIS based UV curable PSA SBS+SIS+PI
3500 3000
SBS+SIS+PI+TRIS
2000
TRIS SIS:SBS=0:30 SIS:SBS=7.5:22.5 SIS:SBS=15:15 SIS:SBS=22.5:7.5
Peel strength (gf)
2000 1500 1000 500 0 0 400 800 1200

2
Peel strength (gf)
2500
1500
1000
500
0 1600 2000 0 400 800 1200

2
1600
2000
UV dose (mJ/cm )
UV dose (mJ/cm )
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SAFT (Shear adhesion failure temperature)

SAFT of SBS/SIS based UV curable PSA SBS+SIS+PI
100
SBS+SIS+PI+TRIS
100
SIS:SBS=0:30 SIS:SBS=7.5:22.5 SIS:SBS=15:15 SIS:SBS=22.5:7.5
80
80
SAFT ( C)
SAFT ( C)
60
60
40
40
20 0 200 400 600

2
20
800
1000
200
400
600
2
800
1000
UV dose (mJ/cm )
UV dose (mJ/cm )
www.adhesion.org
Failure mode of holding power (40oC)

Adhesive failure
SBS+SIS+PI +TRIS
UV dose (mJ/cm2)
200
600
1000
1400
SBS+SIS+PI
UV dose (mJ/cm2)
200
600
1000
1400
Cohesive failure
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Conclusion
Probe tack
Not detected
Adhesion performance of SBS/SIS based UV curable PSA
SIS content
Only SBS UV dose SIS content Peel strength SIS content SAFT
Only SBS Only SBS UV dose UV dose


Adhesion Performance of UV-Crosslinked SBS-Based PSA - Effects of SIS Contents

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Adhesion Performance of UV-Crosslinked SBS-Based PSA - Effects of SIS Contents

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2005 Adhesion Conference on Adhesion

Adhesion Performance of UVcrosslinked SBS-based PSA : Effects of SIS contents

Solution-borne Emulsion (Water-borne)

Lab. of Adhesion & Bio-Composites

SBS/SIS based PSA

Lab. of Adhesion & Bio-Composites

Purpose of this study

SBS block copolymer Adhesion Performance of UV-crosslinkable hotmelt PSA

SIS block copolymer

Lab. of Adhesion & Bio-Composites

Chemical structure of UV curable SBS with vinyl pendant group

Lab. of Adhesion & Bio-Composites

4.5 4.5 4.5 4.5

Lab. of Adhesion & Bio-Composites

Lab. of Adhesion & Bio-Composites

Pressure plate Substrate UV --cured film UV Ccured film oating

Debonding Force force

Results and Discussion

Characteristic peak of 910.8 cm-1, 964.7 cm-1

Sites of Chemical Reaction

Results and Discussion

0.80 0.75 0.70 0.65 0.60 0.55 0.50

0.40 0.35 0.30 0.25

0.2 0.1 1000

0.20 0.15 1000 950 Wavenumbers (cm-1) 900

Results and Discussion

Gel content (%)

60 40 20 0 0 400 800 1200 1600

Gel contents of UV crosslinked SBS

Results and Discussion

CH2 CH CH2 CH R CH2 CH CH2 . CH

SBS & Photoinitiator

SBS & Photoinitiator & Photocrosslinker

CH2 CH CH2 CH R CH2 CH CH2 CH CH2 CH

Lab. of Adhesion & Bio-Composites

Probe tack (gf)

600 400 200 0 0 400 800 1200

Probe tack (gf)

600 400 200 0

Lab. of Adhesion & Bio-Composites

Peel strength (gf)

2000 1500 1000 500 0 0 400 800 1200

Peel strength (gf)

0 1600 2000 0 400 800 1200

Lab. of Adhesion & Bio-Composites

SAFT (Shear adhesion failure temperature)

20 0 200 400 600

Lab. of Adhesion & Bio-Composites

Failure mode of holding power (40oC)

Adhesion performance of SBS/SIS based UV curable PSA

Only SBS Only SBS UV dose UV dose

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