Nanoscale Barrier Coating on BOPP Packaging Film by ALD Presented by: Dr. Johanna Lahti Senior Research Fellow Tampere University of Technology

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1 Nanoscale Barrier Coating on BPP Packaging Film by ALD Presented by: Dr. Johanna Lahti Senior Research Fellow Tampere University of Technology Co-authors: Kimmo Lahtinen (LUT*), Petri Johansson (TUT), Tarja Seppänen (LUT), David C. Cameron (LUT**) * Currently Bemis, ** Currently Masaryk University

2 Content Introduction Packaging materials in general Atomic layer deposition (ALD) and R2R ALD NanoMend project Materials & Methods Results Summary & Conclusions Acknowledgements

3 Introduction Extrusion coated materials and plastic films are used in various packages like flexible packages (such as wrappings, pouches and bags), liquid packages, etc. In packages, the most important function of a packaging material is to shield the product inside the package. Depending on the polymer, extrusion coating and plastic film generally give a barrier against water, water vapor, aroma, grease, oxygen, etc. However, some materials and applications require improved barrier properties. ne way to improve barrier is nanoscale thin layer coating technique - Atomic Layer Deposition (ALD) There is an increasing interest towards thin inorganic coatings as barrier layers for flexible substrates Prevents harmful gas/vapor transmission through material Towards thinner and thinner coatings

4 Atomic Layer Deposition (ALD) ALD is a CVD process, which enables deposition of highly conformal and uniform thickness thin films with monolayer precision. Purpose: thin, tight and stable coating from gaseous precursors Main advantage: the conformality and uniformity which can be obtained regardless of the orientation or shape of the substrate; i.e., there are no pinholes in the film In ALD process, thin films of material are deposited one atomic layer at a time Thickness of a typical ALD layer can vary from 1 to over 100 nm

5 Atomic Layer Deposition (ALD) ALD coating consists of several reaction cycles. ne cycle is able to achieve ~0.1 nm layer depending on the coating material and process parameters. Typically uses two precursors (TMA, trimethyl aluminium and water) to form film material, e.g. aluminium oxide (Al 2 3 ), which is the most studied material.

6 ALD is a chemical vapour deposition process based on chemical reactions on the surface of a substrate Hydroxyl (-H) substrate is exposed to first precursor, TMA (trimethylaluminum). Methane is flushed away from this reaction. H 3 C Al CH 3 CH 3 H H H H CH 4 H 3 C CH 3 Al H Dimethyl aluminum (-Al(CH 3 ) 2 ) substrate is exposed to second precursor, water. Methane is flushed away also from this reaction. H 2 H C CH 3 3 H 3 C CH 3 H 3 C CH 3 Al Al Al H C CH 3 3 Al H 3 H C Al CH 4 H 3 C CH 3 Al The Al 2 3 layer is ready. The process can now be started again from the beginning. H H Al H H Al H H Al

7 ALD as part of a package The targets for ALD technology as part of a packaging can be: Decrease the amount of other materials by extra ALD layer (if the barrier properties of the structure is the reason for thicker layer). Replace the whole layer in the package (e.g. aluminium foil in ultimate case) To create hydrophopic / hydrophilic surface Improve optical properties of the surface Concerning of barrier properties, the ALD process on moving substrate has been a success. The oxygen and water vapor barrier of paper / polymer / Al 2 3 -structures has improved significantly. In addition, UV barrier properties have been achieved. Recently development work with R2R ALD in FP7 NanoMend project

8 NanoMend EU project 7.25million FP7 funded, 4 year long project from Jan 2012, in total 14 partners from Finland, Germany, Switzerland, Netherlands and UK. Enhanced in-line Detection, Cleaning and Repair of Nano-scale Defects for Large Area Substrates (NANMend) The goal of the project is to bypass the state-of-the-art level of defect detection, cleaning and repair technologies in fibre-based packaging material and flexible solar panel productions Defects within these materials reduce the yield (in production), performance and life time of the products Flexible solar modules Food packaging

9 NanoMend EU project NanoMend was a collaborative, end user led project aimed at pioneering novel technologies for in-line detection, cleaning and repair of micro and nano scale defects on thin films deposited on large area substrates in fibre-based packaging and flexible solar panel productions. The aim was to integrate these technologies into systems that work at speeds required for continuous production, thus enabling the new technologies to improve product yield and performance, while keeping manufacturing costs low. Role of TUT & LUT has been research and demonstration relating to production of packaging materials and research of using (R2R) ALD technology in production of packaging materials and creating improved properties.

10 Roll-to-Roll Atomic Layer Deposition (R2R ALD) A new R2R ALD process opens up a possibility to perform highthroughput ALD processing for flexible substrates. Beneq WCS 500 R2R ALD system at LUT (Mikkeli, Finland) Process description available in YouTube

11 Target of this study Since nanocoatings are very thin, they are typically very sensitive and susceptible to defects Before the coating process: the substrate has to be as clean and as defect free as possible After the coating process: even a slight contact on the coated surface may deteriorate, e.g. the barrier properties of the obtained coating Careful web handling is required This paper summarises the studies reported in Tappi European PLACE Conference 2013 (Dresden) and Tappi 2014 PLACE Conference (Ponte Vedra, FL) investigating the surface coatability properties of biaxially-oriented polypropylene (BPP) in an atomic layer deposition (ALD) process. Target: to improve barrier properties of BPP and to evaluate the influence of substrate contamination, web handling and surface treatments on the thin film quality

12 Materials & Methods BPP substrate Thickness: 58 µm Low additive level ne side of the film is corona treated by the supplier ALD-Al 2 3 depositions Equipment used: Beneq TFS 500 Thickness: 30 nm (400 ALD cycles to produce appr. 30 nm Al 2 3 layers) The non-corona-treated side of the substrate Precursors: trimethylaluminum (TMA) and ozone ( 3 ) Self-limiting sequential process to produce one atomic layer at a time (400 cycles). Measurements: xygen transmission rate (TR)

13 A 3D batch ALD process (LUT) Equipment used: Beneq TFS cm 2 sheets Temperature 65 C Pressure 1 mbar 400 ALD cycles to produce appr. 30 nm Al 2 3 layers

14 xygen transmission rate ( 2 TR) Mocon x-tran Model 2/21 ASTM D 3985 Measuring conditions: 23 C, 0% RH

15 ur facilities Versatile Roll-to-Roll pilot lines Production of packaging materials via (co)extrusion coating and lamination dispersion coating cast film (co)extrusion Max. speed ~400 m/min, max. width 550 mm YouTube: NanoMEND pilot line Coatings, treatments and functionalisation of surfaces, e.g. plasma, IR, UV, LFS 15 Well-equipped laboratory for packaging materials and packages Barrier properties (WVTR, TR, C2, grease) Sealability & hot tack Surface energy Adhesion etc. etc.

16 Target and trial points To evaluate effects of Corona pre-treatment Surface contamination (i.e. different shipping procedures) Mechanical contact (web handling) on the oxygen barrier of ALD coated BPP film

17 Influence of surface contamination and pretreatments before the ALD coating UNTREATED = Roll sample THRUGH LINE=film has been run through the pilot line Reference: plain BPP: 2TR 1100

18 Trial points for evaluation effects after ALD coating 2&7 7&8 5-8

19 Influence of different mechanical stresses after the ALD coating on oxygen barrier performance Blue: effect of R2R handling Red: effect of shipment Green: effect of corona treatment

20 Analysis of all factors: Index TR TR 2 TR TR REF % 1 = the factor influences the result 0 = the factor is not influencing the result REF = uncoated BPP Process The share of the barrier improvement which is lost Corona, plasma or flame pretreatment 1% (average) Shipment between Al-foils 2 12 % Surface contamination before ALD coating 7 17 % Mechanical stresses caused by winding 26% after ALD coating For further scientific analysis: K. Lahtinen, J. Lahti, P. Johansson, T. Seppänen, DC. Cameron J. Coat. Technol. Res. DI: /s

21 Conclusions This study focused on the effects of pretreatment, surface contamination and web handling on the ALD thin film quality Even small differences in the thin film coating process can cause a significant variation in the oxygen barrier of thin film coated BPP However, with 30 nm thick Al 2 3 coating, 2 TR of BPP was decreased from 1100 (cm 3 /m 2 /24h) down to 20 (cm 3 /m 2 /24h)

22 Conclusions Significant effect: Surface contamination of the substrate before the ALD coating process and mechanical stresses faced by the already deposited material in roll-to-roll winding. Minor effect: the shipment of the coated material between aluminium foils and the post corona treatment for which the coating was exposed. Cleaning or avoiding contamination before ALD coating is very important Protecting of the ALD coating from significant mechanical stresses is very important

23 Further research: Role of defects in packaging materials Besides contaminants, pinholes are defects that affect barrier performance of packaging materials Pinholes are microholes and like other discontinuity or nonhomogeniety, they strongly reduce barrier properties of materials Pinholes in material or coating layer can restrict or even prevent the usage of the material in certain applications Pinholes, which can be random or cumalative, usually form during extrusion coating process and can be caused by various reasons like -Air bubbles in the polymer melt -Impurities in the polymer melt, e.g. gels -Uneven or rough substrate -Impurities on the surface of the chill roll or other rolls In NanoMend project, target is to develop and study novel in-line R2R detection and cleaning methods to ensure the quality of produced packaging materials

24 TUT pilot line as a demonstrator for detection and cleaning systems for packaging materials The commercialisation of the technologies developed in NanoMend will significantly enhance film quality, yields and product lifetimes as well as minimising manufacturing costs and materials wastage. The two in-line defect detection systems installed, one high resolution for lower line speeds, and the other a high speed system for high line speeds, both utilise novel optical inspection methods and are capable of detecting micro-scale defects within continuous R2R production. 24

25 Acknowledgements & Further information This research work has been funded by EC FP7 programme. Project no We wish to thank Innovia Films Ltd. for material support

26 Thank you! PRESENTED BY Dr. Johanna Lahti Senior Research Fellow Tampere University of Technology

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