Dante Ferrari Celplast Metallized Products Limited

AIMCAL Fall ConferenceOctober 27 – 30, 2013

Presented byDante FerrariPresented byDante Ferrari

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Dante FerrariCelplast Metallized Products Limited

BARRIER PACKAGING IN THE REAL WORLD



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Outline

BackgroundIntroduction Films Laminate structures Adhesive laminating conditions

Pre- and Post-Gelbo Flex Barrier Properties Laminated MET PE High Barrier MET PET Top-Coated MET PET

Bond Strength of Adhesive LaminationsSummaryConclusions



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Introduction

PE and PET are two of the most commonly used base

substrates in flexible packaging

Two most important characteristic of a flexible package Barrier properties

Lamination bond strength

What happens to the package in the real world?



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Introduction

This study was designed to evaluate the practical barrier of pouches

The intention was to simulate flexing and handling that would be

expected through the conversion and distribution chain

Barrier data was collected at various stages in order to estimate and

compare the potential degradation of initial barrier through practical

usage

Gelbo-Flex testing was used to simulate handling



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Introduction: Films

High barrier MET PE Sealant film

Previous studies1 have shown that in a 2-ply structure, barrier properties are similar to a 3-ply structure using a standard metallized PET film, using less material

1 “Sustainable Packaging: Reducing Material and Carbon Footprint with Metallized Barrier Sealants”, Packaging Films, Sept. 2012.

Properties Typical Value Unit Test conditions

Thickness 1.50 mil

OTR 0.06 cc/100in2/day 23 C, 50% RHᵒ

WVTR 0.07 g/100in2/day 38 C, 90% RHᵒ

Metal Adhesion >300 g/in MA-1



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Introduction: Films

Bi-axially oriented high barrier MET PET film


Thickness 0.48 mil

OTR 0.015 cc/100in2/day 23 C, 50% RHᵒ

WVTR 0.015 g/100in2/day 38 C, 90% RHᵒ

Metal Adhesion 400 g/in MA-1



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Introduction: Films Bi-axially oriented inline top-coated MET PET

• Produced using proprietary in-vacuum EB top-coating process, which traps metal and improves barrier2

2 “Improve Barrier Properties and Significantly Reduce Your Carbon Footprint with In-line Metallizing and Top-coating”, AIMCAL Fall Technical Conference, 2011.


Thickness 0.50 mil

OTR 0.003 cc/100in2/day 23 C, 50% RHᵒ

WVTR 0.002 g/100in2/day 38 C, 90% RHᵒ

Metal Adhesion >300 g/in MA-1



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Laminate Structures

3 laminate structures were prepared:

SAMPLE 1 SAMPLE 2

MET PE: 2 ply Laminated Structure MET PET: 3 ply Laminated structure

Layer Description Layer Layer Description Layer Thickness Thickness Clear PET 0.48 mil

Adhesive LaminationHB MET PET 0.48 milAdhesive LaminationPE Sealant Web 1.5 mil

Clear PET 0.48 milAdhesive LaminationMET PE Sealant Web 1.5 mil



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Laminate Structures

SAMPLE 3

Coated MET PET: 3 ply Laminated structure

Layer Description Layer Thickness

Clear PET 0.48 mil

Adhesive Lamination

HB Top-Coated MET PET 0.50 mil

Adhesive Lamination

PE Sealant Web 1.5 mil



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Solvent-less Two part polyester/polyether urethane Standard 4-roll metering Adhesive at 113 °F (45 °C), nip at 113 °F (45 °C) Applied weight 1.1 – 1.25 lb./ream (1.8 to 2.0 GSM) Corona Treater for primary and secondary set to 0.2 WD

Water-Based Two part acrylic urethane Standard gravure application Applied weight 1.5 to 1.7 lb./ream (2.5 to 2.8 GSM) Corona Treater for primary and secondary set to 0.2 WD Two zone dryer set to 170 and 180 °F (77 and 82 °C); nip at 180 °F (82 °C)

Lamination Conditions



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Solvent-Based Two part curing polyester urethane Standard gravure application Applied weight 1.6 to 1.7 lb./ream (2.6 to 2.8 GSM) Corona Treater for primary and secondary set to 0.2 WD Two zone dryer set to 170 and 180 °F (77 and 82 °C); nip at 180 °F (82 °C)

Lamination Conditions


Presented byDante Ferrari

Bond Strengthof

Laminate Structures

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Bond StrengthAll results below shown after 7 days, similar to 24 hour resultsSolventless and solvent-based provided best bondsWater-based gave high bonds, adhesive transfer to PEBond strength units of measurement are all g/in

Note: Blue highlight is the interface tested for bond strength.

ADHESIVEPRODUCT

Clear PET/Met PE Clear PET/Met PET/PE

Clear PET/Coated Met PET/PE

Bond, Hi/Lo

Mode of failure

Bond, H/L

Mode of failure

Bond, H/L

Mode of failure

Solvent-based 551/457 30 –50 % Metal Transfer

1454/488 PE stretch 1463/ 568

Destruct

Solventless 675/539 90 % Metal Transfer

> 1482 Could Not Separate,

PE tear

1669/ 1038

PE tear

Water- Based 300/293 Adhesive transfer

549/505 Adhesive transfer

584/553 Adhesive transfer



Barrier Properties of

Laminate Structure

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The laminations were measured for OTR:

Initial, after 20 and 270 flexesASTM D3985@ 23°C and 0% RH

WVTR: Initial, after 20 and 270 flexesASTM F372@ 38°C and 90% RH

Bond strength Initial, 24 hours and 7 daysInstron Bond testing -10 in/min separation90 degree peel

Barrier & Bond Testing

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Automated or Manual operationFlat material mounted as a tube on each endFlex is both rotational (270 degrees) and compressive

Gelbo-Flex Testing

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2 Ply Clear PET/MET PEAdhesive Lamination

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PET/ MET PE : Oxygen BarrierSolvent-based and solvent-less adhesive based laminate structures provided better barrier than water-based adhesiveThe change in OTR values for all 3 structures were minimal even after 20 and 270 flexesThe effect of Gelbo-flexing is less significant for solvent-based and water-based lamination

Solvent Based Solventless Water Based

0.15 0.15

0.20.1600000000

000010.17

0.21

0.170.18

0.21

Pre-Flex

After 20 Flexes

After 270 Flexes

OT

R (

cc/1

00 in

2/d

ay)

at 0

%

RH

an

d 2

3C

ᵒ

6.7%6.3% 13.3%

5.9%

5% 0%



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PET/ MET PE : Water Vapor BarrierInitial barrier properties indicate that solvent-based and solvent-less adhesive

systems produce a better laminated structure

After the first 20 flexes, the change in WVTR is higher for solvent-less laminate


0.13 0.12

0.22

0.160.18

0.27

0.19 0.19

0.28

Pre-Flex

After 20 Flexes

After 270 Flexes

WV

TR

(g/

100

in2/

day

) at

90

% R

H a

nd

38

Cᵒ

23.1%

18.8%50.0%

5.6%

22.7% 3.7%



3 Ply Clear PET/MET PET/PEAdhesive Lamination

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PET/ MET PET /PE : Oxygen Barrier

All laminated structures showed similar Pre-flex barrier properties

After 20 flexes, the barrier of water-based laminated structure deteriorated

faster than solvent-based and solvent-less laminate structure


0.02 0.03 0.03

0.110.14

0.26

0.12

0.24

0.29Pre-Flex

After 20 Flexes

After 270 Flexes

OT

R (

cc/1

00 in

2/d

ay)

at

0%R

H a

nd

23

Cᵒ

450% 9%366%

71%766%

11%



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PET/ MET PET /PE : Water Vapor BarrierExcellent WVTR values with solvent-based adhesive lamination. No significant

change after 20 or 270 Gelbo-Flexes

Initial WVTR value for water-based was better than solvent-less. However, after

flexing the performance of solvent-less and water-based laminate was similar


0.00200000000000001

0.06

0.0280.002000000

00000001

0.076

0.09

0.00300000000000001

0.1 0.1Pre-Flex

After 20 Flexes

After 270 Flexes

WV

TR

(g/

100

in2/

day

) at

90

% R

H a

nd

38

Cᵒ

0%

31.6%

26.7%

11.1%221%

50%



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Solvent-based Laminations: Oxygen Barrier

After 20 flexes, the barrier of Met PE 2-ply laminated structure is close to

High Barrier Met PET 3-ply structure, likely would be better than Standard

Barrier Met PET 3-ply structure

Pre-Flex After 20 Flexes

After 270 Flexes

-0.0499999999999998

2.35922392732846E-16

0.0500000000000002

0.1

0.15

0.2

0.25

0.3

Met PEHB Met PET

OTR

(cc/

100

in2/

day)



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Solventless Laminations: Oxygen Barrier

After 20 flexes, the barrier of Met PE 2-ply laminated structure is nearly same

as High Barrier Met PET 3-ply structure, is even better at 270 flexes

Pre-Flex After 20 Flexes After 270 Flexes0

0.05

0.1

0.15

0.2

0.25

0.3

Met PEHB Met PET

OTR

(cc/

100

in2/

day)



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Water-Based Laminations: Oxygen Barrier

After 20 flexes, the barrier of Met PE 2-ply laminated structure is better than

High Barrier Met PET 3-ply structure

2-ply barrier after 20 flexes would be significantly better than Standard

Barrier Met PET 3-ply structure

Pre-Flex After 20 Flexes

After 270 Flexes-0.0499999999999998

2.35922392732846E-16

0.0500000000000002

0.1

0.15

0.2

0.25

0.3

Met PEHB Met PET

OTR

(cc/

100

in2/

day)



3 Ply Clear PET/Coated MET PET/PE

Adhesive Lamination

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PET/ Coated MET PET /PE : Oxygen Barrier

Coated Met PET retains OTR properties better than HB Met PET in equivalent 3-ply structure, both before and after Gelbo flexing

Pre-Flex 20 Flex 270 Flex Pre-Flex 20 Flex 270 Flex Pre-Flex 20 Flex 270 FlexSolvent-based Solventless Water-based

-0.0499999999999997

2.91433543964104E-16

0.0500000000000003

0.1

0.15

0.2

0.25

0.3

HB Met PETCoated Met PET

OTR

(cc/

100

in2/

day)



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PET/ Coated MET PET /PE : Water Vapor Barrier

For solvent-based laminations, both met PET films perform very wellFor solventless and water-based laminations, Coated Met PET retains WVTR properties much better than HB Met PET in equivalent 3-ply structure

Pre-

Flex

20 F

lex

270

Flex

Pre-

Flex

20 F

lex

270

Flex

Pre-

Flex

20 F

lex

270

Flex

Solvent-based Solventless Water-based

-0.02

2.08166817117217E-17

0.02

0.04

0.06

0.08

0.1

0.12

HB Met PETCoated Met PET

WVT

R (g

/100

in2/

day)



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ConclusionsBond strengths were higher with solvent-based and solventless laminations

for all three structures being studied, water-based bonds still acceptable for

most applications

The effect of Gelbo-Flexing on barrier properties was more significant for

MET PET compared to MET PE

For solventless and water-based adhesive systems, 2-ply lamination with

Met PE holds oxygen barrier better than 3-ply lamination with High Barrier

Met PET

3-ply structures with Coated Met PET retain their oxygen barrier better (~

2x) than the same structure using High Barrier Met PET, and retain their

water vapour barrier much better (~ 3x)



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Special Thanks

A special thank you to Larry Jopko and the entire team at the Dow

Chemical Adhesive Research Centre in Buffalo Grove, IL for preparing

the laminations using Dow adhesives and carrying out the Gelbo Flex

testing, bond strength testing and barrier measurements.

Dante Ferrari Celplast Metallized Products Limited

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