DETERMINATION OF MOISTURE INGRESS THROUGH VARIOUS ENCAPSULANTS
IN GLASS/GLASS LAMINATES
Jane Kapur1, Kristof Proost2, C. Anthony Smith3
1. E. I. DuPont de Nemours & Co., Inc., Wilmington, DE 19880
2. E. I. DuPont de Nemours & Co., Inc., Mechelen, Belgium
3. E. I. DuPont de Nemours & Co., Inc., Washington, WV 26181
ABSTRACT
Encapsulant materials can provide protection and
electrical isolation of the solar components in photovoltaic
(PV) modules from the environment. However, some
photovoltaic devices are sensitive to low levels of moisture
and the ingress of water into a module can decrease its
performance significantly during the lifetime of a module.
In glass/glass PV modules, the moisture penetrates
through the encapsulant to the module’s metal
components and degradation can occur. In this study, we
have developed and validated methods to determine
moisture ingress in situ in a laminate. Water permeability
and equilibrium moisture level (which are temperature
dependent) through the encapsulant may affect the
corrosion of metal components. We have measured the
moisture ingress through an encapsulant material from the
glass edge towards the center by an in-situ Fourier
transform infrared (FTIR) spectroscopy technique after
damp-heat exposure. The FTIR measurements were
performed on glass / encapsulant / glass laminates that
were weathered at various times at elevated temperatures
and humidity. The moisture level in the encapsulant can
be determined by integration of the IR band between 1880
and 1990 nm. This peak surface was compared to a
calibration curve, which was obtained using laminates with
known encapsulant moisture levels (determined by Karl-
Fischer titration). The moisture migration through an
encapsulant material from the edge was also measured
using an ASTM D7191 moisture analysis method [1]. The
measurements were made on Al foil/encapsulant/Al foil
laminates that were exposed to 85°C and 85%RH (damp
heat). The experimental data correlated well to a Fickian
diffusion model.
INTRODUCTION
The reduction of moisture penetration through the
encapsulant in a photovoltaic module is critical in certain
solar cell technologies. Moisture can corrode the metal
components in the module and/or increase the
conductivity of the encapsulant, which may result in an
increase in the current leakage of the PV module [2].
Various other defects, such as delamination, bubble
formation and edge cloud, are all known to be influenced
by the presence of moisture [3]. Photovoltaic modules and
encapsulants are affected by elevated levels of moisture
with respect to mechanical integrity, electrical properties
such as resistivity, current leakage and overall cell
efficiency and these factors been the subject of many
studies [4,5]. It is important to understand the factors
influencing the rate and magnitude of moisture ingress into
PV module encapsulants. Under accelerated-aging
conditions, such as damp heat exposure (85°C and 85 %
RH), the rate of moisture ingress is significantly increased.
Photovoltaic modules are exposed to 1000 hours of damp
heat as stated in IEC 61215 or IEC61646 standards and
must retain a certain percentage of their initial power
output in order to pass this part of the standard.
In this work, we have tested various commercial and
developmental encapsulants to elucidate the rate of
moisture ingress through polymeric encapsulants
laminated between impermeable substrates. The
encapsulants in this study are made from EVA -- ethylene
vinyl acetate polymer), DuPont PV5200 -- polyvinylbutyral
(PVB), and DuPont PV5300 – an ionomer; additional
developmental encapsulants were also investigated in this
study. In order to measure the rate of moisture ingress,
we have developed two primary methods to measure the
moisture entering the edge of a glass/glass laminate that
simulates a double glass photovoltaic module.
EXPERIMENTAL PROCEDURE - FTIR METHOD
Glass laminates are exposed to damp heat conditions of
85°C and 85%RH. The 20 x 20 cm glass laminates are
made in an autoclave process and are comprised of a
3mm glass, encapsulant, and 3mm glass. With a Perkin
Elmer BX FTIR spectrophotometer, the following
transmission spectrum spanning from 1600 to 2200 nm
was obtained and is shown in Figure 1 (in this case of a
PVB laminate: 2 lites of 3mm clear glass with 0.76mm
PVB interlayer):
Figure 1: FTIR spectrum in the near infrared (NIR) region Figure 2: Moisture profile measured using NIR technique
of polyvinyl butyral resin (PVB). developed for in-situ glass/glass PV module of ingress
distance and concentration.
A ratio (R) between the height of the CH peak (a) and the
height of the moisture peak (b) is calculated for the PVB Temperature is well-known to have a significant effect on
laminate (R=b/a). The height of the moisture band is taken moisture diffusion. The graph below shows the weight
between the maximum of the peak and the baseline that gain for a given encapsulant material (in 3-mm thick
connects the two minima of the peak. Spectra are plaque form, not laminated to glass) as a function of
obtained for 6 standards with known moisture content and temperature immersed in water.
over the range of interest. These are laminates with known
moisture content determined by Karl-Fischer titration
(ASTM D6869 for polymers). By means of linear
regression, a calibration curve is calculated using these 6
standards.

OBTAINING THE MOISTURE INGRESS PROFILE

A special specimen mount was created to allow for

accurate positioning of the glass laminate in the
spectrophotometer compartment. In this way, the beam
location could be well-defined and the sample could be
translated laterally to make various measurements starting
at the edge and inward. The position was indexed from
the edge and measured using a standard sliding caliper
scale.

To establish the efficacy of the methodology,

measurements of samples were conducted for two
different encapsulant materials known to have
substantially different moisture diffusion coefficients and
equilibrium moisture levels. Glass-glass samples (3mm
clear annealed glass) were prepared using DuPont
PV5200 and PV5300 encapsulants and standard
processing conditions. Two environmental exposure
conditions were then evaluated; South Florida outdoor
weathering and full water immersion (maintained at room
temperature). Weathering conditions over the three-year
exposure period averaged 28°C and 82% relative humi dity
according to instrumentation at the weathering site. The
moisture profile data collected is displayed in Figure 2.
Figure 3: Encapsulant weight gain as a function of
temperature at 100% relative humidity conditions. (Not
laminated)
The net influence of temperature on moisture absorption
necessitates very accurate control and monitoring of
chamber temperature to obtain reproducible test results.
Many approaches in measuring diffusion rates for different
materials exist but are often complicated or difficult to
measure over a wide range of temperatures. Since typical
WVTR equipment is very sensitive to film thickness,
control of thickness uniformity and difficulty making
measurements at elevated temperatures, the
determination of the moisture profile within a glass
laminate affords an alternative methodology to better
understand moisture ingress behavior.
A moisture profile was generated by putting a glass–
encapsulant–glass sample in the damp heat chamber at
85oC and 85% RH. The sample was taped on the bottom
and the top with a moisture-barrier tape to ensure that the
moisture is entering the encapsulant in one direction.
After a given time (typically 1000 hours), the sample was
taken out of the damp heat chamber and the moisture
levels were then measured every centimeter, starting from
the edge of the laminate shown in Figure 2 below.
vacuum laminator (Icolam® 10/08) using standard
lamination conditions producing an extrusion-coated Al
foil/Encapsulant/extruded-coated Al foil structure. The
aluminum foil was extrusion-coated with a 25um layer of
Nucrel® acid copolymer resin [DuPont] which provides
good adhesion to the foil and the various encapsulants of
interest. Sample strips (1.27cm in width) were die-cut
from the foil laminates. The moisture level of the sample
was determined using a Computrac® Vapor Pro Rx®
moisture analyzer (Model CT-100) made by Arizona
Instruments. This technique was calibrated to samples
tested using ASTM D-6869 Karl-Fischer titration method
(Figure 5). The weight of the foil was subtracted from the
foil laminate weight to determine the moisture level in the
encapsulant.

Figure 4: Diagram of Glass/Glass Laminate and location of

FT-IR measurements for moisture determination.

The advantage of this method is that moisture

measurements can be made in-situ in a glass laminate
and it can be performed quickly when the moisture peak is
distinguishable. Figure 5: Calibration Curve between Karl-Fischer (ASTM
D6869) and Computrac Vapor Pro ASTM D7191 method.
A peak integration method was also employed for
situations where the moisture peak was not easily The moisture ingress through PV5200 (PVB) laminates
resolved, either due to low intensity and/or broadness of determined by FTIR and ASTM D7191 methods is shown
the peak. The moisture peak in some polymer resin in Figure 6. Both methods correlate very well after the
systems is not well-defined and can be spread over the Vapor Pro measurements have been calibrated.
range of 1925 to 2100 nm. In this case, the peak intensity
is integrated [Fig. 1 (c)] across that wavelength range
yielding much better sensitivity for making determinations
of moisture levels below 0.08% moisture. A calibration
curve was generated in the same manner as for the peak
intensity method described above.

EXPERIMENTAL PROCEDURE - ASTM D7191 METHOD

An alternate method was also developed for measurement

at low moisture levels (i.e., below 0.1%) or in the case for
EVA where the spectral moisture peak coincides with the
characteristic peaks of the polymers making the NIR
method more difficult and less reliable. The moisture
migration through an encapsulant material from the edge
can also be measured by a relative humidity sensor
method, ASTM D7191. The measurements were made on
aluminum foil/encapsulant/aluminum foil laminates that Figure 6: Moisture Ingress after 2 weeks of damp heat
were exposed to damp heat for two- and six-week time exposure through DuPont PV5200 encapsulant using
periods. The foil laminates were prepared on a Meier
FTIR and ASTM D7191 method (before and after
calibration).
RESULTS AND DISCUSSION
We compared the moisture ingress of several commercial
PVB materials laminated between two lites of glass. The
laminates were exposed to 1000 hours of damp heat. The
measurements were determined by the FTIR method
(Figure 7). The difference in moisture levels among the
PVB sheets is minimal. After 1000 hours of accelerated-
aging, the moisture levels do not change beyond 6 cm into
the laminate.
We also measured the moisture ingress through the
PV5300 encapsulant which is ionomer-based. The
moisture penetrates approximately 5 cm into the laminates
after 3000 hours of accelerated aging. The moisture
levels are much lower than that of PVB.
Figure 7: Moisture ingress after 1000h of damp heat
exposure through four commercially available PVBs--
DuPont PV5200 encapsulant and three PVBs obtained
from other sources-in glass/glass laminates.
Figure 8: Moisture Ingress through PV5300 Encapsulant in
glass/glass laminate after various times in damp heat
(measured by FTIR method).
The moisture ingress through EVA after damp heat
(85°C/85%RH) exposure was measured at 2 and 6-week
periods. Data is compared to a Fickian Diffusion model in
Figure 9. The moisture ingress through the edge of a
polymer laminated between two lites of glass can be
modeled as Fickian diffusion through semi-infinite media.
The solution to this problem is given by Crank [6] in the
following equation:
C − Ci = (Cs − Ci ) ⋅ erfc( x / 4 Dt ) (1)
where C is the moisture fraction, Ci is the initial
concentration of moisture in the encapsulant, Cs is the
surface concentration at the laminate edge or equilibrium
moisture concentration of the encapsulant x is the distance
from the laminate edge, D is the diffusion coefficient, and t
is the exposure time. The equation is valid at relatively
short times (t) and short distances from the laminate edge
(x<<L, where L is the length of the laminate). Kempe [7]
reports that the D is 6.3 x 10-6 cm2/s and the surface
concentration is 0.0055 at 85C at high humidity. The
experimental data compares well to the model indicating
that the diffusion of water vapor in EVA is Fickian.

Figure 9: Moisture Ingress through EVA encapsulant
after 2 and 6 weeks of damp heat (85C/85%RH) exposure
compared to the Fickian Diffusion model where the
diffusion coefficient of water vapor is D = 6.3 x 10-6 cm2/s
and the surface concentration, Cs = 0.0055 (taken from
literature [7]).
We have also measured the ingress of moisture through
developmental encapsulants. Results show that the
moisture level is lower than that of commercial EVA
encapsulants after six weeks of damp heat exposure. The
experimental data can be fitted to Eq. 1 to determine the
diffusion coefficient of water vapor in the developmental
encapsulants. The diffusion coefficient of DuPont PV5300
is approximately 4 times slower than that of EVA. Figure
10 indicates that PV5300 and the developmental
encapsulants can significantly slow the migration of water
vapor (compared to EVA) into a photovoltaic module.
Figure 10: Moisture Ingress after 1000hr of damp heat
exposure.
CONCLUSIONS
We have developed two methods to accurately measure
moisture ingress through encapsulants over time. The
methods have been correlated to the Karl-Fischer titration
method. The methods have been shown to be effective in
measuring moisture ingress profiles for various
encapsulant materials and characterize their performance
as a function of temperature and various environmental
exposure conditions. This methodology can be applied to
the development of enhanced encapsulant materials
possessing both lower moisture ingress rates and
equilibrium levels.
ACKNOWLEDGEMENTS
The authors would like to thank Douglas Evans, Michael
Evans, John Jensen and Joseph Winward for their help in
completing this work.
REFERENCES
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