Ijmet 06 10 004

International Journal of Mechanical Engineering and Technology (IJMET)
Volume 6, Issue 10, Oct 2015, pp. 32-38, Article ID: IJMET_06_10_004
Available online at
http://www.iaeme.com/IJMET/issues.asp?JType=IJMET&VType=6&IType=10
ISSN Print: 0976-6340 and ISSN Online: 0976-6359
IAEME Publication
EXAMINING THE MECHANICAL

PROPERTIES OF ANNEALED AND NOT
ANNEALED MULTILAYER FILM
(POLYETHYLENE/ POLYETHYLENE
TEREPHTHALATE/ POLYETHYLENE) BY
DYNAMIC MECHANICAL ANALYSIS
(DMA)
Somashekara Koushik Ayalasomayajula
Department of Polymer Sciences, Hochschule Aalen, Aalen, Germany
ABSTRACT
Heat treatment process like Annealing is used to enhance mechanical and
sometimes the chemical properties of the material. Thermal analysis
techniques like DMA is used to elucidate Tg and some mechanical properties
like strength, stiffness and damping behavior of the material. Performing
DMA on annealed and not annealed samples of material with similar
composition and examining some specific properties and analyzing them is the
main idea involved in this paper. Furthermore, to inspect the morphology and
surface finish of the given polymeric sample microscopy and visual inspection
are performed.
Key words: Annealing, Dynamic Mechanical Analysis (DMA), Glass
transition temperature (Tg), Polyethylene (PE), Polyethylene terephthalate
(PET).
Cite this Article: Somashekara Koushik Ayalasomayajula, Examining The
Mechanical Properties of Annealed and Not Annealed Multilayer Film
(Polyethylene/ Polyethylene Terephthalate/ Polyethylene) by Dynamic
Mechanical Analysis (DMA), International Journal of Mechanical
Engineering and Technology, 6(10), 2015, pp. 32-38.
http://www.iaeme.com/currentissue.asp?JType=IJMET&VType=6&IType=10
1. INTRODUCTION
Examination of mechanical properties of annealed and not annealed sample of a
multilayer film (PE/PET/PE) is performed with aid of DMA to find out the influence
of annealing on the mechanical properties of polymer. Surface analysis of the film is
performed visually and morphological studies are carried out by microtomy and
http://www.iaeme.com/IJMET/index.asp
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microscopy. Experimental proceedings and results were discussed separately for

better understanding of the process.
2. EXPERIMENT
Polymeric sample is first inspected visually for the presence of any surface defects
and then microscopy is performed to study morphology followed by Dynamic
Mechanical Analysis (DMA) to analyse the mechanical properties.
2.1. Visual Inspection

Visual inspection by eye is the oldest and widely employed method that provides a
means of detecting and examining inhomogeneitys such as voids, pores, cracks and
also surface finish.
2.2. Microtomy and Microscopy

Microtomy is a cutting process which cuts the material into extremely thin slices or
organic tissues, known as sections. Microtomes are used in microscopy, allowing for
the preparation of samples for observation under transmitted light or electron
radiation. LEICA RM2165, a fully motorized rotary microtome, known for sectioning
at low temperatures in combination with LN21 Freezing unit and a tissue freezing
medium to hold sample tight is used for this operation [1]. Polymer film is placed
inside a material holder by applying a tissue freezing medium and kept inside the
chamber filled with coolant gas where a glass knife cuts the film into slices of desired
thickness which is controlled by operator. In our case it is 10 m. Now the slice is
placed on the glass slide by applying oil on it and observed under microscope.
Zeiss Axioplan 2 a high-end imaging platform for complex research optimized for
light transmission and extremely high contrast fluorescence imaging is used for
microscopy [2]. The lenses we used are plan-neofluar lenses with magnifications 10X,
20X, 50X, 100X.
2.3. Annealing conditions

Annealing of polymers is defined as a secondary process wherein the polymer is
brought to a certain temperature (below its glass transition temperature) and then
cooled down to room temperature. It is generally performed to enhance mechanical
properties [3]. Polymeric sample is annealed at a temperature of 120C for 2 minutes.
2.4. Dynamic Mechanical Analysis (DMA)

Dynamic mechanical analysis (DMA) is a thermal analysis technique that is used to
provide information about the mechanical properties of any viscoelastic material [4]
as they are deformed under periodic stress. Specifically, a variable sinusoidal stress is
applied, and the resultant sinusoidal strain is measured.
A purely elastic material exhibits no phase difference between stress and strain
waves i.e. phase difference is 0o and if the material is viscous it exhibits 90o phase
difference. Polymers generally exhibit viscoelastic behaviour and thus show phase
differences between those extremes. This phase difference along with amplitudes of
stress strain waves, is used to deduce some material parameters such as Storage
Modulus E', Loss Modulus E", Complex Modulus E* and loss tangent tan [5].
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Examining The Mechanical Properties of Annealed and Not Annealed Multilayer Film
(Polyethylene/ Polyethylene Terephthalate/ Polyethylene) by Dynamic Mechanical Analysis
(DMA)
Figure 1 stress-strain behaviour of viscoelastic material
Figure 2 stress-strain behaviour of a purely elastic material
Two dumb bell shaped specimens of the same polymeric material comprising of
PET and PE are prepared as per ISO 6721-1 (Plastics- Determination of dynamic
mechanical properties) standards [6]. One of the samples is annealed at certain
conditions as discussed in earlier section. EPLEXOR 150 N machine is used to
perform DMA and the test conditions are as follows:
Table 1 Test conditions for performing DMA
Frequency
10 Hz
Temperature
-50C to 180C
Heat rate
2K/min
Static load
1.0%
Dynamic load
0.3%
Maximum force
80N
Minimum force
40N
Soak time
1800 sec
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3. RESULTS AND DISCUSSIONS

Observing the given polymeric sample through naked eye it is clear that the
provided film is colourless, flat with uniform thickness and with no surface defects.
Furthermore light passes through the film which says it is transparent and placing the
film in sunlight we can find the direction of extrusion of the film.
Figure 3 Morphology showing different layers
Fig.3 shows the morphology of the given sample. From the microscopic image we
can infer that the film was composed of 3 layers and the thickness of layers are
137.4m, 281.75m and 156.14m respectively. Furthermore the sealing layers look
alike thus making the film as ABA type. The difference in observed values of
thickness of layers might be because of microtome cut. By observing the morphology
it can be said that core layer is of PET and sealing layers are comprised of PE. The
thickness of core layer is nearly 300m and the sealing layers 150m each
constituting for 600m for the entire film.
The results of DMA scan with a constant heating rate of 2K/min at constant
frequency of 10Hz for both annealed and not-annealed samples are presented in Fig 4
and Fig 5 as variation of E',E",E* and tan with temperature which clearly explains
that DMA we performed is temperature sweep but not frequency sweep or
temperature-frequency sweep.
Figure 4 DMA graph for annealed film

Material: PE/PET/PE.
DMA: Frequency: 10 Hz, Temperature: -50oC 180oC, static strain = 1.0 %, dynamic strain =
0.3 %
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(DMA)
Figure 5 DMA graph for not annealed film

0.3 %
Figure 6 Comparison of complex modulus for both samples

0.3 %
Primary analysis of complex modulus curve of both samples reveal that the
complex modulus curve for annealed sample is decreasing at slow rate when
compared to that of not annealed sample, which says that annealed material is stiffer
than that of not annealed one. Variation in mechanical loss factor tan with
temperature for both samples is shown in Fig 7. Comparing the area under graphs we
can observe that area covered by not annealed film is more than that of annealed film
which clearly states that damping is higher for not annealed film.
The main aim of performing DMA is to determine glass transition temperature Tg.
Tg can be calculated by the following ways [5].
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Evaluation of modulus step:
Step method employed for DSC curves (start, half step height and end of glass
transition),
Inflection point method,

2% offset method (start of glass transition),
Tangent method (start of glass transition).
Evaluation of peaks from plots of loss factor and loss modulus:
Maximum loss factor,
Maximum loss modulus.
Evaluating the peak of loss factor is widely employed to determine Tg.
Figure 7 Comparison of loss tangent

0.3 %
It is evident from Fig.7 that the Tg of not annealed specimen is about 96oC and
annealed specimen is about 120oC which clearly explains that heat treatment process
like annealing increases Tg of material [7].
4. CONCLUSION
Heat treatment process like annealing forms additional crystals while cooling down to
room temperature. From the results of performed Dynamic Mechanical Analysis we
conclude that annealed material has more glass transition temperature when compared
to that of not annealed material. Also annealed sample has high stiffness and less
damping when compared to that of not annealed because of formation of additional
crystals. Glass transition temperature observed using peak analysis of loss modulus is
different from Tg obtained from other methods. Exact reason for this is unknown,
leaving space for research in this area. With the increase in glass transition
temperature the area of application of the polymeric material is increased and also
performing some other thermal analysis techniques like DSC, TGA one can easily
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(DMA)
understand the behaviour of the material at higher temperatures and also there is a
possibility in achieving traditional polymeric materials with enhanced properties.
5. ACKNOWLEDGEMENT
I would like to thank my Professor Dr. Achim Frick and Mr. Muralidharan
Vibunanthan for providing me the opportunity and for extending their support
throughout the experiment.
REFERENCES
[1]
[2]
[3]
[4]
[5]
[6]
[7]
[8]
[9]
[10]
Leica microsystems, operating manual, Nussloch, pp: 6, [online]

http://www.leicamicrosystems.com/fileadmin/downloads/Leica%20RM2165/Brochures/RM2165_
germ.pdf, Viewed on: 11-June-2015.
Zeiss, Axioplan 2 imaging and Axiophot 2 Universal Microscopes Operating
manual, Jena, pp: 83, [online] https://physics.ucsd.edu/neurophysics/
Manuals/Zeiss/Axioplan%202%20imagine%20and%20Axiophot%202.pdf,
Viewed on: 11-June-2015.
LeGrand. D.G, Encyclopedia of Polymer Science and Technology, (Wiley Online
library, John Wiley & Sons, Inc. Feb-2011).
Faria.R, Duncan. J.C, Brereton. R.G. Dynamic mechanical analysis and
Chemometrics for polymer identification. In: Polymer Testing, 26(3), May 2007,
pp: 403.
Erhenstein.G.W, Riedel. G, Trawiel. P, Thermal Analysis of Plastics Munich,
Carl Hanser, 2009, pp: 236-239,243,244,247.
ISO standard; ISO 6721-1 (Plastics- Determination of dynamic mechanical
properties).
Gupta.S, Dixit.M, Sharma.K, Saxena. N.S. Mechanical study of metalized
polyethylene terephthalate (PET) films. In: Surface and Coating technology,
204(5), Dec-2009, pp: 664.
Siddhant Datta, B.M. Nagabhushana, R. Harikrishna, A New Nano-Ceria
Reinforced Epoxy Polymer Composite with Improved Mechanical Properties,
International Journal of Advanced Research in Engineering & Technology
(IJARET), 3(2), 2012, pp. 248 - 256.
N. Kumar, P. L. Meena, A. S. Meena and K. S. Meena, Physico-Mechanical
Properties OF SSBR Styrene 40%, Vinyl Content 46% Based Truck Tyre Tread
Cap Compounds with LPCA and HPCA Oils, International Journal of Advanced
Research in Engineering & Technology (IJARET), 5(2), 2014, pp. 121 - 127.
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Properties of Al-SICP Composites, International Journal of Mechanical
Engineering and Technology, 3(3), 2012, pp. 565 573.
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International Journal of Mechanical Engineering and Technology (IJMET)

EXAMINING THE MECHANICAL

Somashekara Koushik Ayalasomayajula

microscopy. Experimental proceedings and results were discussed separately for

2.1. Visual Inspection

2.2. Microtomy and Microscopy

2.3. Annealing conditions

2.4. Dynamic Mechanical Analysis (DMA)

Figure 1 stress-strain behaviour of viscoelastic material

Figure 2 stress-strain behaviour of a purely elastic material

Somashekara Koushik Ayalasomayajula

3. RESULTS AND DISCUSSIONS

Figure 3 Morphology showing different layers

Figure 4 DMA graph for annealed film

Figure 5 DMA graph for not annealed film

Figure 6 Comparison of complex modulus for both samples

Somashekara Koushik Ayalasomayajula

Evaluation of modulus step:

Inflection point method,

Evaluating the peak of loss factor is widely employed to determine Tg.

Figure 7 Comparison of loss tangent

Leica microsystems, operating manual, Nussloch, pp: 6, [online]

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