Surface modification of polyethylene terephthalate (PET) and oxide coated PET for adhesion improvement
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1 Surface modification of polyethylene terephthalate (PET) and oxide coated PET for adhesion improvement AIMCAL 2016 Dresden Juliane Fichtner Tobias Beck Frank Simon (IPF, Dresden) page 1
2 Motivation oxygen water vapor organic electronics permeation barrier system flexible solar cell organic electronics page 2 flexible OLED
3 Motivation varnish ZTO / SiOx varnish ZTO / SiOx varnish PET varnish ZTO / SiOx varnish ZTO / SiOx PET 10 µm 50 nm 75 µm sufficient wetting behavior and adhesion for good performance necessary page 3! BUT low surface energies and impurities! surface modification
4 Process parameter low pressure plasma treatment web width: 220 mm dual magnetron bipolar mode electrical power: 1 5 kw web speed: 1 5 m/min process pressure: Pa page 4
5 Varnish layer manufacturing acrylic based varnish layer thickness: 10 µm curing dose: 25 kgy acceleration voltage: 150 kv electron current: 2 ma motion speed: 150 mm/s page 5
6 Characterization wetting behavior surface energy test inks if surface energy change < 5% samples removed dynamic advancing contact angle measurement analyzed by tangent method page 6
7 Characterization surface chemistry x-ray photoelectron spectroscopy (XPS) binding energy chemical bonding characteristics ATR FT-IR spectroscopy varnish adhesion pull-off test page 7
8 Sample comparison - activation intensity X i electrical power: 1 5 kw web speed: 1 5 m/min process pressure: Pa influence on the absolut number of collisions of ions on the sample influences the electrical current X i = (I 1 + I 2 ) t page 8
9 Wetting behavior O 2 -plasma contact angle ZTO surface cleaning PET + SiO x contact angle page 9 surface modification
10 Surface modification - PET - O 2 -plasma Ph C E Sh D F C-atoms of phenyl ring C-atoms with one O-atom and CH 2 C-atoms carboxylic acid ester Peaks of π-electrons C-atoms of keto group C-atoms of carboxyl group page 10
11 Surface modification - PET - O 2 -plasma carboxylic acid ester + carboxyl groups carboxyl group decarboxylation page 11
12 Wetting behavior - SiO x - O 2 -plasma Hybrid SiO x enrichment with oxygen functional groups: hydroxy, keto and carbon acid groups polar character page 12
13 Varnish adhesion - O 2 -plasma adhesion on SiO x = Si-OH groups interact well with water by hydrogen bonds, but no effect on varnish adhesion PET: electron beam additional chemical bonding to the varnish page 13
14 Wetting behavior N 2 -plasma Contact angle similar for all substrates page 14
15 Surface modification - PET - N 2 -plasma atom fraction O:C (0,34 to 0,1) atom fraction N:C (0 to 0,46) carbon nitrides page 15
16 Surface modification - PET - N 2 -plasma atom fraction O:C (0,34 to 0,1) atom fraction N:C (0 to 0,46) carbon nitrides page 16
17 Surface modification - FTIR-ATR - N 2 -plasma C thin layer nitrogen-rich heterocycles 1,3-Diazabenzene or 1,4-Diazabenzene page 17
18 Varnish adhesion - N 2 -plasma max. adhesion: PET 2.3 MPa SiO x 1.5 MPa ZTO 1.2 MPa activation intensity nitrogen content adhesion page 18
19 Process gas mixtures - visual transmittance constant visual transmittance up to 80 v/v% nitrogen page 19
20 Process gas mixtures contact angle nitrogen content ZTO: contact angle + PET: contact angle page 20
21 Process gas mixtures varnish adhesion - ZTO max. adhesion of 0.8 MPa (nitrogen content of 70 v/v%) page 21
22 Atmospheric pressure electron beam radiation e- beam treatment lowers contact angle for all samples dose contact angle page 22
23 Surface modification - PET - N 2 -electron beam PET N 2 - electron beam no cracked or decomposed PET chains potentially carbon acid amides (C=C-NH-C) page 23 Binding Energy [ev]
24 Varnish adhesion - N 2 - electron beam max. adhesion: PET 2.1 MPa SiO x 1.7 MPa ZTO 0,7 MPa activation intensity nitrogen content adhesion page 24
25 Permeation rates plasma gas X i [As] WVTR [g/(m 2 *d)] OTR [cm 3 /(m 2 *d*bar)] non N O Dose WVTR OTR atmosphere [kgy] [g/(m 2 *d)] [cm 3 /(m 2 *d*bar)] N ,069 0,2 no influence of the plasma treatment and electron beam treatment on permeation barrier properties page 25
26 Conclusions low pressure plasma treatment Plasma gas composition varnish adhesion [MPa] PET SiO x ZTO non no wettability 100 v/v% oxygen no wettability 100 v/v% nitrogen v/v% nitrogen 30 v/v% oxygen no value no value 0.8 increasing of varnish adhesion without impact on: transmittance permeation barrier properties page 26
27 Conclusions atmospheric pressure e-beam treatment Dose [kgy] varnish adhesion [MPa] PET SiO x ZTO non no wettability increasing of varnish adhesion without impact on: transmittance permeation barrier properties page 27
28 Thank you for your interest!! Contact: Dipl.-Ing. Juliane Fichtner Fraunhofer FEP Winterbergstr Dresden, Germany Tel: +49 (351) Parts of the results have been obtained within public funded research projects supported by the Free State of Saxony. page 28
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