Polymer Testing 30 (2011) 236–242

Contents lists available at ScienceDirect

Polymer Testing
journal homepage: www.elsevier.com/locate/polytest

Material Characterisation

Investigation of Ethylene/Vinyl Acetate Copolymer (EVA) by thermal

analysis DSC and DMA
W. Stark*, M. Jaunich
BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, D-12205 Berlin, Federal Republic of Germany

a r t i c l e i n f o a b s t r a c t

Article history: Two types of commercially applied Ethylene/Vinyl Acetate Copolymers (EVA) for encap-
Received 9 November 2010 sulation of photovoltaic modules were investigated by the thermal analysis methods of
Accepted 21 December 2010 Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) in the
temperature range from
150  C to 200  C. Glass transition, crystal melting and cross-
Keywords: linking were analyzed. The aims of the investigations were to gain more information for
EVA
incoming goods control and to get information about the whole temperature dependent
Thermal analysis
material properties in the investigated temperature range, starting at very low tempera-
DSC
DMA tures up to the crosslinking temperature region.
Glass transition Ó 2010 Elsevier Ltd. All rights reserved.
Crystal melting
Cross-linking

1. Introduction circuit and electrical insulation are guaranteed. The steps in

Ethylene/Vinyl Acetate Copolymer (EVA) is used
worldwide for encapsulation of photovoltaic modules. The
following properties make EVA an outstanding material for
encapsulation [1]:
1) High electrical resistivity which makes it a good electric
insulator,
2) Low processing and cross-linking temperature,
3) Very low water absorption ratio,
4) Good optical transmission.
The whole packaging of a photovoltaic module consists
typically of a five-layer structure: glass front side/EVA for
heat and environmental sealing/photovoltaic module/2nd
EVA sealing film/back face protection. In this way the
protection from environmental damage of the solar cells
* Corresponding author. Tel.: þ49 30 8104 1614; fax: þ49 30 8104 3328.
E-mail address: wolfgang.stark@bam.de (W. Stark).
lamination are first melting of the EVA and bonding of the
solar panel with the front side glass unit and the rear side.
The back face protection is realized by either a glass or
a multilayer sheet of Tedlar-Aluminium-Tedlar. The output
box is also situated at the back side. After that step, the EVA is
cross-linked by a thermally activated reaction with perox-
ides as crosslinking agent. A series of publications dealing
with the properties of EVA in solar panels can be found [2–6].
The aim of our investigations was to demonstrate the
competency of the thermal analysis methods DSC and DMA
for incoming goods control and quality assurance in the
technological process, as thermal analysis equipment,
especially DSC, is often present in industry.
From DSC measurements, crystal melting and cross-
linking behaviour can be well investigated. The maximum
endothermic heat release is correlated with the melting of
the crystals of the most frequently appearing thickness [7–9].
The endothermic peak onset temperature and peak height
give information about size and size distribution of crystals,
the number of peaks gives an indication of different crys-
talline forms (often bimodal), and normalized enthalpy gives
information about degree of crystallinity. Information

0142-9418/$ – see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.polymertesting.2010.12.003
 W. Stark, M. Jaunich / Polymer Testing 30 (2011) 236–242
concerning the cross-linking reaction can be gained from the
exothermic process.
The state of knowledge is summarised by the following
information:
1.1. DSC-measurements starting at temperatures considerably
below room temperature
Vogel and Heinze [10] published DSC results from

23  C to 227  C. For non cross-linked material two peaks,
one close to 50  C and one close to 70  C, and an exothermic
double peak in the range from 140  C to 200  C are seen. For
a cross-linked sample only a broad endothermic shoulder
without a peak in the range 20  C–50  C followed by
a distinct peak near 65  C appears. The exothermic peak is
missing.
Varghese et al. [11] showed a DSC curve from
80  C to
250  C. There is an endothermic step from about
40  C
to
10  C passing into a first peak at about 50  C, which is
followed by a second peak close to 85  C.
Khonakdar et al. [12] published DSC curves for EVA
copolymers and also for pure EVA in the range
75  C to
175  C. A peak near 85  C was found. For the blends,
reduced crystallinity of the cross-linked material was
reported.
1.2. DSC-measurements starting at or close to room
temperature
Shi et al. [13] have reported on DSC results in the range
0  C–140  C. A so called L-peak (lower temperature) and
a H-peak were found which are attributed to the primary
and secondary crystallization. Depending on the VAc
content and the thermal treatment, the L-peak is in the
range 40  C–60  C, the H-peak 80  C–90  C. Using WAXD it
was found that many crystals became bigger and more
perfect by thermal ageing.
Marcilla et al. [14] published DSC results in a tempera-
ture range starting from 37  C to 157  C showing two
endothermic peaks - a lower one near 47  C, a higher one
near 70  C.
Agroui et al. [15] investigated two EVA types designated
slow and fast cure. DSC was measured from 40  C to 155  C.
Two endothermic peaks were seen, a more pronounced one
at 50  C and more a shoulder near 70  C.
Reyes-Labarta et al. [16] measured mixtures of PE with
EVA and also pure EVA. DSC results for EVA from 27  C to
227  C showed two endothermic peaks – one near 50  C
and another about 70  C. An exothermic peak in the range
175–215  C appeared. After cross-linking, the lower peak
had vanished. This was interpreted by the reduction in
structural regularity by the created cross-links.
Moly et al. [17] used DSC and WAXS. DSC performed in
the range 40  C–160  C showed a broad shoulder from 40  C
finished by a peak at 80  C. During cooling, a peak at 50  C
followed by a wide shoulder was seen. For blends, a
decrease in crystallinity by cross-linking was found which
was explained by some hindrance to the ordered arrange-
ment of the polymer chains.
Dikobe and Luyt [18] investigated EVA-PP blends, and
also both polymers separately, by DSC and DMA. In a DSC
237
experiment from 60 to 180  C, an endothermic peak close
to 100  C was found.
1.3. DSC-measurements in the temperature range of cross-
linking reaction
For cross-linking of EVA, peroxide is added as curing
agent. At temperatures above 160  C the peroxide decom-
poses. Free peroxide radicals abstract mainly the hydrogen
located at the tertiary carbon of the acetate group of the
vinyl acetate (VAc) co-monomers [10,16]. Often dicumyl
peroxide (DCP) is used - Bianchi et al. [19]. The DSC heating
rates were varied from 2.5 K/min to 40 K/min. For rates of
10 K/min and higher an analysable exothermic peak in the
range 150  C–200  C was seen.
Summarizing the DSC literature data, one can state that
for EVA no results starting at very low and reaching up to
crosslinking temperatures were found. Typical endo-
thermic peaks caused by crystal melting are found whereby
often two endothermic peaks appear: first peak around
40  C–60  C, second peak at 70–90  C. Sometimes, a broad
endothermic shoulder starting from
40  C is observed.
Cross-linking appears in the range 140  C–200  C. The
measurement of cross-linked material in a second run
shows changes in the endothermic peak shape. These
changes are discussed as a consequence of the change in
molecular structure by cross-linking.
1.4. DMA-measurements
The DMA results of Dikobe and Luyt [18] measured at
1 Hz between
80 and þ80  C show a distinct decrease in
storage modulus in the
20  C region. A second decrease
appeared close to 40  C. The tand curves gave a first peak in
the region
10 to 0  C, associated with the glass transition,
and a second peak near 60  C.
Varghese et al. [11] measured at 50 Hz. They found
a decrease of storage modulus from about
30 to 0  C
accompanied by a tand peak at about
10  C. From tand
maxima, a glass transition temperature of
12  C for
uncross-linked and
10.4  C for cross-linked material were
given.
Storage modulus, loss modulus and tand curves
measured at 10 Hz were published by John et al. [20]. A
sharp decrease in storage modulus at about
40  C and
a second decrease at about 40  C were reported. The loss
modulus had a first peak in the region of
130  C and
a second close to
25  C. Tand showed maxima at about

130  C,
20  C and 50  C. The change in material prop-
erties in the temperature region around
40 to 0  C was
brought about in connection with the glass transition.
Tand maxima at
140 and
25  C and a distinct
decrease in loss modulus from
40  C were found also by
Khondakar et al. [21]. The increase of tand between 75 and
95  C was explained by Koshy et al. [22] as melting of
crystalline segments.
To summarize the DMA measurements, a first relaxation
process appears in the
120  C range, followed with
increasing temperature by a glass transition in the range

40 to 0  C. An additional decrease of storage modulus in
238 W. Stark, M. Jaunich / Polymer Testing 30 (2011) 236–242

the range from 40  C and a tand increase are explained by

crystal melting.

2. Experimental

2.1. Material

Two commercially available materials applied in photo-

voltaic module production were used:
Material 1: SOLAR EVAÒ RC02B (curing type: fast) from
Mitsui Chemicals Fabro [23].
Material 2: ETIMEXÒ VISTASOLARÒ 486.10 (fast cure)
from ETIMEX Solar GmbH [24].
The materials were supplied as foils with a thickness of
0.64 mm (material 1) and 0.45 mm (material 2). For DSC
measurements, small disks of about 8 mg were cut. For
DMA, 6 mm wide cross-linked strips were prepared in Fig. 2. DMA – loss modulus as function of temperature, material 1.

a compression mould.

E00 ¼ jE jsind
00
2.2. Thermal analysis E – storage modulus

2.2.1. Dynamic mechanical analysis The loss factor tand is calculated from:
In DMA, a sinusoidal mechanical excitation of the
sample is executed whereby force, elongation and the E00
tand ¼
phase shift between them are measured as a function of E0
temperature. The complex modulus E* is calculated from Characteristic changes of moduli E0 and E00 and tand
the measured data and the geometry: caused by thermally activated molecular movements begin
 at definite temperatures.
 l3 F
Edual cantilever ¼  A DMA 242C, Netzsch, Germany, was used for the
16 b h3 A investigations with a dual cantilever holder and a sample
l – sample length, length of 5 mm. The heating rate was 1 K/min and the
b – sample width, amplitude 40 mm. During a single measurement run cycling
h – sample thickness, between the 5 frequencies – 0.33; 1; 3.33; 10 and 33.3 Hz –
F – force, was carried out automatically.
A – deflection.
2.2.2. Differential scanning calorimetry
With the phase shift, the complex E* can be split into DSC evaluates the change of temperature difference
two components: between a sample crucible and a reference crucible during
non-isothermal or isothermal conditions. The difference is

E0 ¼ jE jcosd used to calculate the heat flow into or out of the sample. It
0
E – storage modulus can detect melting, evaporation, glass transition and also

Fig. 1. DMA – storage modulus as function of temperature, material 1. Fig. 3. DMA – tand as function of temperature, material 1.
 W. Stark, M. Jaunich / Polymer Testing 30 (2011) 236–242 239

Table 1
Material 1 - Loss modulus peak temperature of the glass transition for
different frequencies.
00
Frequency, Hz E peak temperature,  C
0.33
32.1
1
30.4
3.33
28.4
10
27.2
33.33
25.0

occurrence of chemical reactions by the consumption or

release of heat [9]. Its special advantage is that only a few
mg of the material are required. A DSC 204 F1 Phoenix,
Netzsch, Germany, was used with standard crucibles and
manually perforated lids. All measurements were carried
out in the non-isothermal mode with a heating and cooling
rate of 10 K/min. Fig. 5. DSC – heat flow in the 1st and 2nd run, material 1.

These values were used to determine an activation

3. Results and discussion
energy from the Arrhenius relation between frequency of
the peak (f) and temperature [26]:
3.1. Material 1

Ea

3.1.1. DMA
The DMA results are presented first because they will be
embraced in the discussion of the DSC results. The DMA
was measured for cross-linked samples only. The cross-
linking conditions were: 30 min at 160  C using a heated
compression mould. For better comparability, the results of
the storage and loss modulus are shown in a normalized
manner, where the values at
150  C were set to unity.
The results for material 1 are given in Figs. 1–3. A small
decrease in storage modulus together with a loss modulus
and tan d peak in the range of
140  C can be explained by
the secondary relaxation caused by side group or end group
motion or backbone “crank-shift” type motions typical for
many polymers [25].
The storage modulus curve shows a distinct decrease
from
40  C. This change is accompanied by a peak in loss
modulus and tand. There is a pronounced correlation
between frequency and location of the peak. For the loss
modulus, the values are shown in Table 1.
f ¼ A e RT
Ea – apparent activation energy,
R – gas constant.
The correlation between ln(f) and 1/T is shown in Fig. 4.
A linear relation was found. From the slope of the straight
line, an apparent activation energy can be calculated. The
activation energy found was 328 kJ/mol, a value in the
range typical for a glass transition [27]. The temperature
range of the glass transition is in accordance with pub-
lished data in [11,18,20].
The next step in storage modulus between 40 and 60  C
was not accompanied by a peak in loss modulus. This will
be discussed together with the DSC data later.
3.1.2. DSC
A basic raw material sample was measured in a 1st run
from
150 to 200  C. The measurement was rerun with the
now cured sample. The results for the 1st and 2nd runs are
given in Fig. 5.
At the beginning of the DSC measurement, the typical
thermal imbalance between the crucibles must be adjusted

Fig. 4. DMA – Arrhenius plot of logarithm of measuring frequency versus

00
reciprocal E peak temperature, material 1. Fig. 6. DSC – temperature program.
240 W. Stark, M. Jaunich / Polymer Testing 30 (2011) 236–242

Fig. 7. DSC – heat flow results for the temperature program from Fig. 6, Fig. 9. DMA – loss modulus as function of temperature, material 2.
material 1.

changed to a broad shoulder followed by a peak at 63  C. The

[9]. Therefore, a settling region, in Fig. 5 from the start
higher the crystal thickness the higher is the melting
at
150 to
135  C, appears. From
115 to
95  C a double
temperature - Illers and Hendus [7]. Therefore, the change
peak structure is seen. The reason for this is unknown.
from a peak into a broad shoulder is an indication of
From its appearance it looks like the formation of an
a distribution of crystals with reduced thickness as a con-
ordered structure (exothermic peak) followed directly by
sequence of the thermal treatment in the first run.
destruction of this structure (endothermic peak). An
The exothermic reaction peak is missing in the 2nd run,
endothermic step from
40 to about
20  C is observed.
indicating that the cross-linking process was finished. The
Endothermic peaks appear in the 1st run at 47 and 72  C.
step in the range
40 to about
20  C is in accordance with
Additionally, an exothermic peak at 158  C with an
the glass transition discussed for DMA results. Similarity
enthalpy of 14.9 J/g appears.
between 1st and 2nd runs show that the glass transition
A broad endothermic shoulder followed by double peaks
temperature was not noticeable changed by cross-linking.
in the range 50–100  C have also been reported in [10–17].
It is interesting that the DSC peak in the 2nd run at 63  C,
An endothermic peak is typically for crystal melting.
indicating crystal melting, correlates well with the sharp
Multiple endothermic peaks in DSC can be correlated to
decrease of the storage modulus of the cured sample in the
a lamellar thickness distribution – see for example [28].
area between 40 and 70  C.
The exothermic peak with a maximum at 158  C indi-
The change in the endothermic peak structure in the
cates the exothermic cross-linking reaction. Similar results
range from 30 to 80  C between the 1st and 2nd runs is
were reported in [10,16,19]. The reaction enthalpy value is
indication that the crystal structure has changed. Some
rather low in comparison to cross-linking of epoxy resins,
authors assume that this is a consequence of cross-linking
where values in the range of some hundred J/g (400–600)
[16,17]. To find out if the change in melting peaks in the
are typical [29,30].
area 30–80  C has its reason in cross-linking or thermal
In the 2nd run the peak near
100  C is similar to the 1st
history, in an additional experiment, the 1st heating run
run. The endothermic double peak between 40 and 80  C has

Fig. 8. DMA – storage modulus as function of temperature, material 2. Fig. 10. DMA – tand as function of temperature, material 2.
 W. Stark, M. Jaunich / Polymer Testing 30 (2011) 236–242
Table 2
Material 2 - Loss modulus peak temperature of the glass transition for
different frequencies.
00
Frequency, Hz E peak temperature,  C
0.33
31.7
1
29.9
3.33
28.2
10
26.7
33.33
24.6
was stopped at 100  C, a cooling run and a 2nd heating run
to 200  C were added followed by additional cooling and
heating runs – the temperature program is illustrated in
Fig. 6. All DSC curves are collected in Fig. 7.
The clear change in the 30–80  C area from a double
peak in the 1st heating to a broad shoulder followed by one
peak in the 2nd heating comes from thermal treatment –
heating to 100  C and cooling under definite conditions.
This general change with the appearance of a broad
shoulder instead of a peak is obviously not caused by cross-
linking. However, in the 3rd run after cross-linking the
remaining peak following the shoulder has shifted to lower
temperatures. This effect comes from heating to 200  C
including cross-linking and indicates an additional drop in
crystal perfection.
3.2. Material 2
3.2.1. DMA
The DMA results for material 2 are shown in Figs. 8–10.
Generally, the curves are similar for both materials. Also,
material 2 shows a significant decrease in storage modulus
starting from about
40  C which, together with the peak
in storage modulus, is typical for the glass transition. Just as
for material 1, in the 50  C region a further drop in the
storage modulus appears. This was discussed for material 1
to be caused by melting of crystalline regions. With mate-
rial 2, the contact with the DMA clamp was lost behind
120  C and this also occurred when the measurements
were repeated. Fig. 9 gives the course of the loss modulus.
As with material 1, a peak in the area
130 to
150  C
Fig. 11. DSC – heat flow in the 1st and 2nd run, material 2.
241
Fig. 12. DSC – heat flow in the 1st, 2nd and 3rd heating run, material 2.
appears. The temperature values of the loss modulus peak
are summarized in Table 2.
From these data, an activation energy of 330 kJ/mol is
calculated – a value nearly identical with that for material 1.
The peak temperatures are very close to those of material 1
which means that the glass transition temperature is nearly
identical for both materials. Fig. 10 illustrates the results for
tand. The tand curves of material 2 resemble those of
material 1 in shape but they show slightly higher values.
3.2.2. DSC
In Fig. 11, DSC results for the 1st and 2nd runs are shown.
The results of material 2 are similar to material 1. In the 1st
run, a step followed by two endothermic peaks appears.
The exothermic curing reaction is in the region of 130–
180  C, whereby there is indication of a double peak. The
reaction enthalpy is found to be 16.0 J/g. For material 2 also,
a separate thermal treatment with the temperature regime
from Fig. 6 was applied. The results in Fig. 12 are also very
similar to material 1 in Fig. 7. A difference in the 2nd run for
material 2 is that an endothermic step at about 110  C
appears for which we have no explanation. Also for mate-
rial 2, the thermal treatment during 1st heating and 1st
cooling causes the form of the endothermic peaks to
change from two distinct peaks into a broad shoulder and
only one peak, as for material 1. Also for material 2, the
thermal treatment during 1st heating and 1st cooling
caused a change in the DSC curve for the 2nd heating run.
The two endothermic peaks in the 1st run have changed to
a broad shoulder and only one remaining peak. This is
similar to the results for material 1 and can be interpreted
by a change in allocation of crystal size distribution as
a consequence of both thermal treatment and of heating to
200  C including cross-linking.
4. Conclusions
Two commercially available types of EVA - SOLAR EVAÒ
RC02B (material 1) from Mitsui Chemicals Fabro and
ETIMEXÒ VISTASOLARÒ 486.10 (material 2) from ETIMEX
Solar GmbH were investigated by DSC and DMA in
the temperature range from
150–200  C. This wide
temperature range, the synchronous application of DMA
242 W. Stark, M. Jaunich / Polymer Testing 30 (2011) 236–242
and DSC and the combination of the measurement of the
original material with measurements of the material ther-
mally treated by the measurement to 100  C and cured
during the preceding measurement to 200  C go beyond
previously published data.
Both materials show very similar characteristic behav-
iour as a function of temperature which can be concluded
as follows:
– A glass transition appears in the range
40 to
20  C,
– The glass transition is not shifted perceptibly by cross-
linking,
– For original, non thermally treated material two crys-
talline melting processes indicated by two endothermic
peaks exist,
– Crystal melting is accompanied by a dip in storage
modulus,
– For material heated to 100  C, cooled down and heated
once more the endothermic double peak has changed
into a broad endothermic shoulder followed by only
one pronounced endothermic peak,
– Cross-linking appears in the temperature region from
140 to 180  C,
– After heating to 200  C including cross-linking the
remaining endothermic peak shifted to lower temper-
ature giving a hint that this process also has changed
crystal perfection.
Knowledge of the characteristic DMA and DSC curve
progressions is of high interest for good incoming control of
basic raw material.
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