Recent Improvements in PET film for Flexible Electronics and Photovoltaic Applications

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1 Recent Improvements in PET film for Flexible Electronics and Photovoltaic Applications Jan LaRiviere, Keith Rollins, Bill MacDonald, and Bob Rustin AIMCAL 2012 Melinex and Mylar are registered trademarks of DuPont Teijin Films U.S. Limited Partnership. Teijin Tetoron is a registered trademarks of Teijin Limited and are licensed to DuPont Teijin Films US, Limited Partnership. Teonex is registered trademark of Teijin DuPont Films Japan Limited and licensed to DuPont Teijin Films U.S. Limited Partnership. Copyright DuPont Teijin Films (UK) Ltd. All rights reserved.

2 Scope Polyester film process Heat stabilized polyester film Latest film developments for flexible electronics Low Bloom, Planarization, Refractive Index control Latest film developments for flexible PV Weatherability, Adhesion Conclusion

3 Polyester Film Technology (1) PET and PEN polyester films Transverse Draw Biaxially oriented, semi-crystalline High stiffness Forward Draw Dimensional stability ptical transparency Solvent resistance Thickness = µm Melinex, Mylar and Teijin Tetoron Polyethylene terephthalate (PET) Teonex Polyethylene naphthalate (PEN) T m = 255 C T m = 263 C T g = 78 C T g = 120 C n n

4 Polyester Film Technology (2) In-line Heat Stabilisation ff-line Heat Stabilisation ven Film can relax in TD but not in MD Leads to shrinkage on subsequent processing Allows relaxation in MD Minimum shrinkage on both directions

5 Heat-Stabilised PEN and PET Films Shrinkage in MD after 30 min at 150 C Minimal shrinkage at temperatures > T g CTLE 0.05% 20 ppm/ C 25 ppm/ C Upper temperature for processing 0.1% C 150 C 4 GPa 1 GPa Young s Modulus at 20 C 5 GPa Young s Modulus at 150 C 3 GPa ST506 (PET) Q65FA (PEN) 1000 ppm 1000 ppm Moisture pick-up at 200 C, 40% RH Haze 78 C 0.7% 0.7% 120 C Glass transition temperature

6 Polyester Films for Flexible Electronics Red denotes new Melinex -A diverse range of heat stabilised PET films Dimensionally stable up to 150C Thickness 50 micron to 250 micron UV stabilised Range of pretreats for enhanced adhesion to functional coatings Tetoron -Low shrink, planarized PET films Ultrasmooth defect free surface for improved device performance Teonex -Leading range of high performance PEN films Dimensionally stable up to C Thickness micron Pretreated for enhanced adhesion to functional coatings White film at 75 micron Teonex - Low shrink, planarized PEN films High temperature performance with ultrasmooth defect free surface 50 and 125 micron film Protect film (one or two side) available

7 Polyester Films for Flexible Electronics To discuss specific requirements please contact Jan LaRiviere (US) Thane Gough (Europe)

8 Films for Touchscreen Rapid Touch Screen Market growth Requires continued optimization for PET Touch Screen Revenue Forecast Source: DisplaySearch 2011 Touch Panel Market Analysis

9 Films for Touchscreen Projected Capacitive Touch is the primary driver for growth Many designs use PET film as the transparent conductor substrate Manufacturing processes expose PET film to very high temperatures for extended periods Heat stabilized film satisfies the shrinkage requirement But, PET will haze-up under these conditions

10 Cyclic ligomers bserved that if PET film is held at temperatures above 100C film starts to go hazy due to migration of cyclic oligomers to the surface <1% Haze Increased Haze 100 o C for 10 min 120 o C for 10 min 140 o C for 10 min PEN PET Polyhedral or hexagonal platelike oligomer crystals form, a few microns in size Soluble in solvents (e.g. MEK)

11 Cyclic Trimer Cyclic trimer Tm 318C present at ca 1.1 to 1.4wt% C C C C C C ther cyclics present but in lower amounts. Trimer is low strain relative to other cyclics.

12 The Cyclic ligomer Equilibrium PET C C CH 2 CH 2 H Mol Wt =x Driven by -time at temperature in melt -amount of work in extrusion system C Driven by Process control CCH2CH2 PET Mol Wt =x-3 n=3

13 Cycylic ligomer Crystals Perovic, J Mat Sci, 20, 1985, C hexagonal crystals up to 5-6 micron initially but can grow larger with time

14 Traditional Strategy Traditional strategy used is to coat the surface with a coating that acts as a barrier to oligomers migrating to surface IT blocks to an extent but blooming becomes more of an issue with other approaches to conductive films eg printed silver grids etc

15 Strategies for Control -Block Presence of planarizing coatings significantly reduces bloom Coatings acting as a barrier Non planarized PET : 30mins / 120 C planarized PET : 30mins / 120 C

16 Increase in haze % Features of planarized films planarizer Two side planarised Q65WA Uncoated Q65FWA Time / hours Uncoated PEN Time dependence of oligomer migration (measured by haze increase) of PEN and two side planarized PEN at 200C

17 New Strategy for Control -Process Control Through process control at PET polymerisation stage and during film processing it is possible to Significantly reduce the cyclic content in the PET polymer Minimise the reformation of the cyclic oligomers during subsequent filming process

18 New Developments New development grade, 1% haze on ageing at 150 o C /30 mins Now in qualification with customers Able to tailor with respect to surface treatments for specific applications DTF is investigating further strategies to minimise the impact of blooming on subsequent processing For more information contact Nicole Williamson Nicole.M.Williamson@USA.dupont.com

19 Refractive index control Controlling refraction and reflection effects in optical stacks

20 An example: Reduced iridescence in hard coats Typically, hard coated PET films exhibit iridescence or rainbow which is objectionable in display and touch applications Rainbow results from interference fringes stemming from reflections in the optical stack Through optical modelling we can model the effect and design the stack to minimize fringing Monitor the effect of changing specific layer parameters, e.g. refractive index and thickness Look for fringing in visible spectrum as an indication of rainbow effect For more information contact Nori Mandokoro

21 Modeling the transmission spectrum shows the fringing effect Refractive Index of Film Layer, n Frame No. Substrate refractive index is cycled between 1.67 and 1.51 to show effect on fringing (right), Fringing occurs at higher RI values. Modeled Transmission Spectrum Hard Coat (RI=1.5) Substrate (RI varied)

22 In the real world, it s a bit more complex Hard Coat (RI=1.5) Adhesion Primer (RI = X) Note: most top layers require an adhesion priming layer PET Film (RI=1.67) Manipulation and control of the adhesion primer can optically bridge the gap from substrate to top layer

23 DTF primer technology can reduce hard coat fringing %T ACTUAL DATA 93 Transmission spectra of new trial films + hardcoat, compared to standard film control Reduced Iridescence ptimized Iridescence 90 Reduced Iridescence No index matching, high iridescence Wavelength (nm)

24 Visual of the new film s effect New Product Standard PET Competitor X Competitor Y Each sample is hard coated PET and photographed under a monochromatic light source

25 Latest Film Developments for PV

26 Substrates for PV Cells Gen. 2 & 3 Gen I Gen II Gen III Thin Films c-si CdTe CIGS a-si DSSC PV Encapsulation Encapsulation / Cell Front Sheet Cell Superstrate Active Layer Stack Module A complex film development agenda!! Substrate Back Sheet

27 Functionalities Dimensional Stability Surface Quality Barrier Heat Stability Front Sheet Superstrate Active Layer Substrate Back Sheet Weatherability Conductivity Light Management Adhesion

28 Dimensional Stability Surface Quality Barrier Heat Stability Front Sheet Superstrate Active Layer Substrate Back Sheet Weatherability Conductivity Light Management Adhesion

29 Photo-oxidative Degradation This pathway to colour C CCH 2 CH 2 This pathway to chain breaking C. hv + 2 CCH 2 CH 2 hv + 2 n=ca 100 C. CCHCH 2 hv + 2 H n=ca 100 hv + 2 n=ca 100 C CCH 2 CH 2 C. C H CCH 2 CH 2 n=ca 100 C P-H +P. n=ca 100

30 Upon UV light-induced degradation: Yellowness increases formation of new light-absorbing chemical species Haze increases (clear films) bulk + surface scattering Gloss decreases surface roughens Light transmittance decreases more absorption and scattering Mechanical properties i.e. %ETB, UTS decrease chains break down

31 UV Stabilisers UV stabilizers work by: Energy dissipation ie radiation is absorbed and then dissipated (heat, fluorescence) Radical deactivation and retardation of propagation of degradation reactions Singlet oxygen quenching Peroxide decomposition Efficacy of a UV stabilizer depends on: How its optimum absorption wavelength(s) fits with the optimum degradation wavelength(s) of the polymer Its efficiency at converting UV radiation into less harmful energy (heat) Its intrinsic UV stability Its thermal stability to survive PET processing temperatures

32 Weatherability UV Resistance Lifetime perception: Polyester films degrade rapidly under UV light exposure In reality, only non-uv stabilised films will! Polyester films can be modified to have improved resistance to UV light Typical results from Weather-meter ageing of a DTF UV stabilised film 1) Mechanical properties: 120% % Retention of Elongation to Break 120% % Retention of Ultimate Strength 100% 100% 80% 80% 60% 60% 40% 20% ` UV stabilised PET film Standard PET film 40% 20% ` UV stabilised PET film Standard PET film 0% Method: ASTM Hours in the Weatherometer 0% Hours in the Weatherometer

33 Weatherability UV Resistance Typical results from Weather-meter ageing of a DTF UV stabilised film 2) ptical properties: % Retention of Light Transmittance % Increase of Yellowness Index 105% 300% 100% 250% 95% 200% 150% 90% 85% ` Standard PET film UV stabilised PET film 100% 50% ` Standard PET film UV stabilised PET film 80% % Hours in the Weatherometer Hours in the Weatherometer 10,000 hours in Weather-meter Equivalent irradiation = 5 (Florida) to 11 years (Northern Europe) This is not a lifetime guarantee

34 ETB (%) Weatherability Hydrolysis Resistance Lifetime perception: Polyester films hydrolyse rapidly This is very slow under normal atmospheric (T,P) conditions! Polyester films can be modified to pass the standard Damp Heat test Retention of 10% ETB after 1000 h at 85 C / 85% RH Some industry interest in higher performance PET films for extended testing times (2000+ hours in Damp Heat test) 200 % Elongation at Break (Melinex 238) DTF's filled Melinex 238 at 50 µm reaches 2000 h at 85 C / 85% RH DTF can also apply this technology to optically clear films Damp Heat Test (hours)

35 Hydrolysis of PET Catalysed by CH end groups in PET

36 Strategies for Improving Hydrolysis Resistance Raising Mol Wt of film Chemically modifying end groups Affecting film crystallinity

37 Dimensional Stability Surface Quality Barrier Heat Stability Front Sheet Sun-facing Substrate PV Active Layer Non Sun-facing Substrate Back Sheet Weatherability Conductivity Light Management Adhesion

38 Adhesion Multi-layer adhesion is appearing as one of the most challenging technical areas and is key to optimise device/module lifetime and lab certification DTF has designed Melinex films with enhanced adhesion to EVA (a typical cell backside encapsulant) - Received positive market feedback Similarly films with excellent adhesion to DuPont Surlyn have also been developed

39 Adhesion to Glass Industry-standard bonding interlayer eg polyvinyl butyral (PVB) ionoplast systems such as DuPont s SentryGlas 48 These do not show good adhesion to many standard PET film pretreatments, but specialist systems are available. The key parameter in this respect is the bonding or laminating temperature required to give good adhesion and whether this is in excess of what can be tolerated by the completed o-pv cell. This remains an area of active research.

40 Conclusion Recent improvements in PET film support emerging flexible electronics and flexible PV markets Active continuing innovation to meet future needs Underlying science that affect processing on polyester films being researched Knowhow on how to get the most out of the handling and processing on polyester film available to users Please contact us with any questions you may have THANK YU!

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