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B ARRIER P ACKAGING IN THE R EAL W ORLD. Dante Ferrari Celplast Metallized Products Limited. Outline. Background Introduction Films Laminate structures Adhesive laminating conditions Pre- and Post- Gelbo Flex Barrier Properties L aminated MET PE High Barrier MET PET - PowerPoint PPT Presentation
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AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
1
Dante FerrariCelplast Metallized Products Limited
BARRIER PACKAGING IN THE REAL WORLD
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
2
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
3
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?
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
4
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
5
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
6
Introduction: Films
Bi-axially oriented high barrier MET PET film
Properties Typical Value Unit Test conditions
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
7
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.
Properties Typical Value Unit Test conditions
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
8
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
9
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
10
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
11
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante Ferrari
Bond Strengthof
Laminate Structures
12
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
13
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
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante Ferrari
Barrier Properties of
Laminate Structure
14
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante Ferrari
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
15
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante Ferrari
Automated or Manual operationFlat material mounted as a tube on each endFlex is both rotational (270 degrees) and compressive
Gelbo-Flex Testing
16
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante Ferrari
2 Ply Clear PET/MET PEAdhesive Lamination
17
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
18
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%
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
19
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
Solvent Based Solventless Water Based
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%
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante Ferrari
3 Ply Clear PET/MET PET/PEAdhesive Lamination
20
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
21
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
Solvent Based Solventless Water Based
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%
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
22
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
Solvent Based Solventless Water Based
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%
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
23
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)
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
24
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)
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
25
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)
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante Ferrari
3 Ply Clear PET/Coated MET PET/PE
Adhesive Lamination
26
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
27
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)
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
28
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)
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
29
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)
AIMCAL Fall ConferenceOctober 27 – 30, 2013
Presented byDante FerrariPresented byDante Ferrari
30
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.
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