water vapour permeation testing of ultra-barriers › pdfs › vs4 › wvtr.pdf · measurement...
TRANSCRIPT
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Christoph Zerwas
Water Vapour Permeation
Testing of Ultra-Barriers
Limitations of Current Methods and Advancements
Resulting in Increased Sensitivity
17th October 2013
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MOCON Headquarter Lippke
MOCON Asia
Dansensor
MOCON Worldwide
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Andreas Roos
MOCON in Europe
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Our Service
Installation and Training
Maintenance
Stocking on Spare parts
Seminars
Support at Qualification
Measurement as a service
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Andreas Roos
Introduction
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Water vapour barrier
g.m2.day-1
Polymer films 1-100
Food packaging 0.1-10
Electro-Chromics 0.001-0.05
Flexible PV 0.00001-0.001
Flexible OLEDs 0.0000001-0.00001
Barrier layer requirements on plastic
substrates
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Andreas Roos
Imagine a polymer sheet of the size of a football pitch.
How much water would pass through this over a MONTH at various
barrier performance levels?
~ 100 m
~ 50 m
Dr. Alf Smith, Centre of Process Innovation, UK
What does that mean?
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Andreas Roos
100 10 1 1 x 10-2 1 x 10-4 1 x 10-6
Raw film Food packaging OPV OLED
Dr. Alf Smith, Centre of Process Innovation, UK
What does that mean?
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Andreas Roos
• ASTM F 1249
• Tunable diode laser
absorbtion spectroscopy
• Calcium test
WVTR = water vapour transmission rate
Current methods of WVTR measurement
Indirect
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Andreas Roos
• Radioactive method
• Modified ASTM F 1249
WVTR = water vapour transmission rate
Current methods of WVTR measurement
Direct
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Andreas Roos
Current methods of WVTR measurement
Modified ASTM F 1249
Cellblock
Generated
RH
Carriergas
H2O
N2+H2O
H2O
N2
RH probe
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Andreas Roos
Current methods of WVTR measurement
Modified ASTM F 1249
• Chemical Reaction
P2O5+ H2O →2 HPO3
4 HPO3→2 P2O5+ 2 H2 + O2
• Electrical Current is proportional to the Permeation
• Test Range down to 0,00005 g/m²/day
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Andreas Roos
• Temperature
• Leaks
• Calibration / sensor
• System noise
• Correlation to established methods
Limitations in measuring permeation
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Andreas Roos
1 °C temperature increase
causes a 5 – 7 % higher
transmission rate
10 °C more can double the
transmission rate.
Limitations in measuring permeation
Temperature
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Andreas Roos
Limitations in measuring permeation
Temperature
WVTR
(85C, 50C, 23C)
0
100
200
300
400
500
600
0 50 100 150 200 250Hours
mg
/(m
2 d
ay)
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Andreas Roos
Since permeation
measurement means
detecting very small amounts
of permeate, additional gas
penetrating through leaks
distort the results.
Several components of each
permeation measurement
system like valves and others
are weak points which allow
“side” permeation.
Limitations in measuring permeation
Leaks
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Andreas Roos
Comparative sensors require calibration.
As a general rule of measurement calibration has to
be done in the range which the sensors are used in.
I.e. calibration is a potential source of errors.
Limitations in measuring permeation
Calibration
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Andreas Roos
All technical measurement systems show noise.
Electronics, outgasing and carrier gas variability are
reasons for noise of permeation measurement
systems.
The better noise is reduced or compensated the more
sensitive a measurement can be.
Limitations in measuring permeation
Noise
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Andreas Roos
When measurement values cannot be correlated to
results obtained from an established and accepted
method, they will not be taken reliable.
The better a barrier the lower the WVTR values the
more difficult is such validation.
Limitations in measuring permeation
Missing Correlation
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Andreas Roos
• Temperature
• Leaks
• Calibration / sensor
• System noise
Advancements in permation measurement
technology
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Andreas Roos
AQUATRAN 2:
- Temperature Range: 10-40°C
- Accuracy of adjustment +/- 0,1°C
=> eliminates any temperature related errors.
Advancements in permation measurement
Technology - temperature
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Andreas Roos
TruSeal Technology
Optimised design and material
quality improve the tightness
of the whole system.
Advancements in permation measurement
Technology - leaks
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Andreas Roos
Modified electronics lower the base noise level.
Advancements in permation measurement
Technology- Noise
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Andreas Roos
Absolute sensors do not require
calibration.
It is not affected by pressure,
temperature, flow or vibration.
Test Limit of the AQUATRAN 2 is
5 x 10-5 g/m²/day
The potential sensitivity of MOCON’s
new AQUATRACETM Gold sensor itself
is 2 x 10-6 g/m²/day.
Advancements in permation measurement
Technology – calibration / sensor
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Andreas Roos
As barrier quality continues to increase, so too must permeation
measurement methods and systems.
Several hurdles exist when measuring permeation of high barriers.
Existing methods often are deficient in these areas, thus producing
unreliable results in the low range of transmission rates.
New generation instruments eliminate calibration with the addition of an
absolute sensor and increase sensitivity by reducing the weak points.
MOCON improved their well established instrument AQUATRAN 1 by
measures like increasing the tightness, modifying the sensor and
improving the temperature control. The new generation AQUATRAN 2
allows measuring WVTR down to 5 x 10-5 g/m²/day; 10 times better than
before.
Conclusion
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Andreas Roos
Thank you for your attention!