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

This document summarizes a study on improving the adhesion performance of UV-crosslinked styrene-butadiene-styrene (SBS) based pressure sensitive adhesives (PSA) by adding styrene-isoprene-styrene (SIS) and a thiol-ene photocrosslinker. Key findings include: 1) Addition of SIS and the photocrosslinker improved gel content, peel strength, shear adhesion failure temperature, and failure mode compared to SBS only formulations. 2) Optimal adhesion performance was achieved with 15-22.5% SIS content and UV doses of 1000-1400 mJ/cm^2. 3) Thiol-ene photocrosslinking between SBS and

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278 views22 pages

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

This document summarizes a study on improving the adhesion performance of UV-crosslinked styrene-butadiene-styrene (SBS) based pressure sensitive adhesives (PSA) by adding styrene-isoprene-styrene (SIS) and a thiol-ene photocrosslinker. Key findings include: 1) Addition of SIS and the photocrosslinker improved gel content, peel strength, shear adhesion failure temperature, and failure mode compared to SBS only formulations. 2) Optimal adhesion performance was achieved with 15-22.5% SIS content and UV doses of 1000-1400 mJ/cm^2. 3) Thiol-ene photocrosslinking between SBS and

Uploaded by

Eugene Pai
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© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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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,

[email protected] / 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

www.adhesion.org

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
Lab. of Adhesion & Bio-Composites

www.adhesion.org

Introduction
SBS based PSA
High solubility parameter Harder polymers More difficult to tackify High entanglement Good heat resistance

SBS/SIS based PSA

Lab. of Adhesion & Bio-Composites

www.adhesion.org

Introduction
Block copolymer based UV curing system
polystyrene polybutadiene polystyrene

SBS
Semi-Interpenetrated Network

UV

RSH (thiol)
Lab. of Adhesion & Bio-Composites

www.adhesion.org

Purpose of this study

SBS block copolymer Adhesion Performance of UV-crosslinkable hotmelt PSA

SIS block copolymer

Thiol-ene polymerization

Lab. of Adhesion & Bio-Composites

www.adhesion.org

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

Lab. of Adhesion & Bio-Composites

www.adhesion.org

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)

Lab. of Adhesion & Bio-Composites

www.adhesion.org

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

Lab. of Adhesion & Bio-Composites

www.adhesion.org

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
Lab. of Adhesion & Bio-Composites

www.adhesion.org

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

www.adhesion.org

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
Lab. of Adhesion & Bio-Composites

www.adhesion.org

Results and Discussion

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

Sites of Chemical Reaction


Lab. of Adhesion & Bio-Composites

www.adhesion.org

Results and Discussion


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
Lab. of Adhesion & Bio-Composites

www.adhesion.org

Results and Discussion


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


Lab. of Adhesion & Bio-Composites

www.adhesion.org

Results and Discussion


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

Lab. of Adhesion & Bio-Composites

www.adhesion.org

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 )

Lab. of Adhesion & Bio-Composites

www.adhesion.org

Peel strength
Peel strength of SBS/SIS based UV curable PSA SBS+SIS+PI
3500 3000
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
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 )

Lab. of Adhesion & Bio-Composites

www.adhesion.org

SAFT (Shear adhesion failure temperature)


SAFT of SBS/SIS based UV curable PSA SBS+SIS+PI
100
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
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 )

Lab. of Adhesion & Bio-Composites

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
Lab. of Adhesion & Bio-Composites

www.adhesion.org

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


Lab. of Adhesion & Bio-Composites

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