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Material Characterization of Heat Shrinkable Film

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DOI: 10.1520/JTE20130112

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Journal of
Testing and Evaluation
Zehra S. Kalkan-Sevinc1 and Caitlin T. Strobel2

DOI: 10.1520/JTE20130112

Material Characterization of Heat

Shrinkable Film
VOL. 43 / NO. 6 / NOVEMBER 2015
 Journal of Testing and Evaluation

doi:10.1520/JTE20130112 / Vol. 43 / No. 6 / November 2015 / available online at www.astm.org

Zehra S. Kalkan-Sevinc1 and Caitlin T. Strobel2

Material Characterization of Heat

Shrinkable Film

Reference
Kalkan-Sevinc, Zehra S. and Strobel, Caitlin T., “Material Characterization of Heat Shrinkable Film,” Journal
of Testing and Evaluation, Vol. 43, No. 6, 2015, pp. 1531–1539, doi:10.1520/JTE20130112. ISSN 0090-3973

ABSTRACT
Manuscript received January 14, 2014; Shape memory polymers represent a class of polymers that display properties of shape
accepted for publication March 9, 2015;
change under stimulus. The presented research focused on material characterization of
published online June 4, 2015.
thermally stimulated shape memory polymers, more specifically heat shrinkable bands often
1
Baxter Healthcare Corp., Medical
used as packaging in the food and the medical industry. Increasingly, regulatory agencies
Products R & D, 25212 W IL Rt 120,
RLT-14, Round Lake, IL 60073-9799 are pushing for the use of non-PVC materials industry wide. This study represented an
(Corresponding author), experimental approach for evaluation of polyester shrink bands (non-PVC) in comparison
e-mail: kalkan_zehra@hotmail.com
with PVC with regard to thermomechanical and shrinkage properties.
2
Baxter Healthcare Corp., Medical
Products R & D, 25212 W IL Rt 120,
RLT-14, Round Lake, IL 60073-9799. Keywords
shape memory polymer, heat shrinkable tube, material testing, shrink properties

Nomenclature
E ¼ elongation at break
YS ¼ yield stress
SB ¼ stress at break
M ¼ automatic Young’s modulus
EnB ¼ fracture energy
C ¼ clear
W ¼ white
X ¼ crystallinity

Introduction
Shape memory polymers in the form of shrink bands are commonly used for many packaging applica-
tions within the medical device industry to ensure seal. Currently, various shrink band materials made
out of oriented polyesters, polystyrene, polyolefins, biodegradable PLA, PVC, etc. are commercially

Copyright V
C 2015 by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. 1531
1532 Journal of Testing and Evaluation
available. Demand for non-PVC material use particularly in the
medical industry has increased with the recent movements in
regulatory requirements favoring the use of non-PVC materials.
Therefore, the authors of the presented research empirically eval-
uated the mechanical, shrinkage, and thermal properties of com-
mercially available non-PVC shrink bands, particularly polyesters,
compared to PVC shrink band. No attempt was made specifically
to correlate the results with processing conditions in this study,
as no information was given by material vendors related to
processing parameters of materials under evaluation.
The shape memory effect is characterized by a material’s
ability to convert from its original shape to a programmed
shape and when stimulated return to the original shape. Pro-
grammable stimuli include heat, infrared irradiation, alternating
magnetic fields, and even exposure to water [1]. The shape
memory trait is ideal for programming multiple material states
and has been used in various applications. The presented
research focuses on thermally stimulated shrink bands used in
the packaging industry. Thermally programmed shape memory
polymers are typically created by elongating the material while
increasing the material temperature above the transition tem-
perature, which is often the crystallization temperature or melt-
ing temperature of the polymer [1]. The material is then cooled
while still elongated below the transition temperature, effec-
tively freezing the molecules in place [1]. When the temperature
of the material is again increased above the transition tempera-
ture, the polymer returns to its initial state [1]. Heat shrinkable
polymers are generally investigated as part of shape memory
polymers due to shape change induced by heat stimulus.
Trznadel and Kryszewski [2] describe the shrinkage as a
thermodynamic event driven by the balance between internal
energy, which relates to the interactions between macromolecu-
lar chains, and entropy, which relates to degree of orientation.
The stability of the orientation in macromolecular chains can
be assured if a decrease in internal energy accompanies the
decrease in entropy as a result of molecular orientation [2].
Shrinkage is derived from the entropic tendencies of oriented
macromolecules to form a coiled structure to relieve their inter-
nal stresses [2]. Different techniques were reported to measure
the shrinkage properties of shape memory alloys/polymers.
Riesen and Schawe [3] reported the use of Thermomechanical
Analysis (TMA) to measure the shrinkage and expansion char-
acteristics of poly (ethylene terephthalate) (PET) fibers, calcu-
late the expansivity and the shrinkage coefficient, and measure
Young’s modulus. Surzhikov et al. [4] used a dilatometer to
measure the linear shrinkage properties of composites.
Experimental
MATERIALS
Materials that were analyzed included commercially available
shrink band samples: PVC, PET, and glycol-modified PET
(PETg) by Hishi Plastics, Inc. Samples were either clear or
white. All samples were 0.1 mm thick.
PHASE TRANSITION
A differential scanning calorimetry (DSC) Q1000 manufactured
by TA Instruments was used to measure transition properties,
i.e., glass transition, crystallization, and melting temperatures,
of shrink band samples. An empty aluminum reference pan was
lidded using a manual press. A small sample was cut from
shrink band using a hole punch. The sample was put in an alu-
minum pan and lidded using a manual press. Both reference
and sample pans were placed in a DSC furnace, in which N2 gas
was constantly circulated at 50 ml min–1. PVC samples were
exposed to heat from 20 to 250 C with an increase of 20 C
min–1. PET samples were exposed to heat from 0 to 310 C
with a 20 C min–1 ramp. After maintaining 1 min of isothermal
conditions, samples were cooled down to 0 C using a 20 C
min–1 ramp. After keeping 1 min isothermal conditions, sam-
ples were exposed to the same heating and cooling cycles. A
standard DSC method was used without modulation for PET
samples. TA Universal Analysis 2000 software v4.7A was used
to determine transition temperatures. Crystallinity of non-PVC
samples were calculated by the following equation:
0
(1) %X ¼ ðDHm  DHc Þ  100=DHm
where:
X ¼ crystallinity,
DH ¼ integrated area,
subscripts m and c ¼ melting and cold crystallization,
respectively, and
superscript 0 ¼ 100 % crystalline material property [5,6].
Enthalpy of fusion for 100 % crystalline PET, PETg, and
PVC were 140.1, 88, and 176.0 J g–1, respectively [5,6].
TENSILE PROPERTIES
The tensile properties of shrink band samples were measured
using an Instron 5864 manufactured by Instron with an 890 -N
load cell. Tensile samples were conditioned and tested in a
temperature (22 C–25 C) and humidity (40 %–50 % relative
humidity) controlled lab. Samples (n ¼ 5) were tested in both
the transverse direction (hoop or TD) and machine direction
(MD) (Fig. 1). In order to prepare samples to be tested in the
TD, samples were cut across the TD using a 1.27-cm precision
cutter, leaving the tube intact. A custom fixture was used to
hold the samples to measure the hoop stress. Hoop stress
FIG. 1 Schematic of shrink band.

FIG. 2
Picture of the load cell fixture.
samples were separated 1.27 cm by the fixture and were tested
with 5.08 cm min–1 cross head speed. In order to prepare sam-
ples to be tested in the MD, samples were first cut lengthwise in
MD using a blade and then to 15.2 (length) by 2.5 cm (width)
dimension using a 2.54-cm precision cutter. Those samples
were tested with a 2.54 cm min–1 cross head speed at 10 cm of
grip separation for measuring MD tensile properties. The
Young’s modulus (0.689–6.89 MPa), yield stress, maximum ten-
sile stress, elongation at break, tensile stress at break, and energy
at break were recorded for each condition. Energy at break was
calculated dividing the area under stress-strain curve to the
sample cross-sectional area and gauge length. Yield point was
defined as the points that have a slope of equal or less than zero
determined via software using a least square fit method. Yield
load was selected at the point of highest load within the regions
at yield point and used for calculation of yield stress.
TROUSER TEAR TESTING
The tear properties of shrink band samples were measured
using an Instron 5864 manufactured by Instron with an 890 -N
load cell. Samples were tested in the MD according to ASTM
D1938-14 [7] and cut using an ASTM D1938 die, with a sample
FIG. 3
Schematic of trouser tear samples.
KALKAN-SEVINC AND STROBEL ON HEAT SHRINKABLE FILM 1533
width of 2.54 cm, sample length of 7.6 cm, and leg length of
5 cm (Fig. 2). Sample width was measured and recorded prior to
testing. Samples were tested at a cross-head speed of 25.4 cm
min1 and an initial grip separation of 5 cm. The initial load at
tear, the maximum load, the load at break, and the extension at
break were recorded.
Samples tested in the TD were testing following ASTM
D1938, with modification due to sample geometry. Samples
tested in the TD were cut to a width of 2.54 cm, sample
length of 3.2 cm, and leg length of 1.9 cm, with the sample width
measured prior to testing (Fig. 2). Samples were tested at a
cross-head speed of 25.4 cm min–1 and an initial grip separation
of 2.54 cm. The initial load at tear, the maximum load, the load
at break, and the extension at break were recorded.
SHRINKAGE
Shrink band samples were cut in half lengthwise using a blade.
Flattened samples were cut into 2.54- by 2.54-cm squares using
a precision cutter. The width of the samples was measured in
both the MD and the TD (Fig. 1) using a caliper before testing.
PVC samples were introduced to a heat bath stabilized at 70,
90, and 120 C for 2 and 5 s of dwell time in order to shrink.
1534 Journal of Testing and Evaluation

Clear PVC samples were additionally tested at 130 C for 5 s of

dwell time. Non-PVC samples were tested only at 130 C for 5 s FIG. 5 Comparison of shrinkage properties of non-PVC and PVC.

of dwell time. Samples were patted dry after they were removed
from the heat bath. After shrinkage, the width of the samples
was measured again in both directions and the percent change
was calculated in the TD (ShrinkTD) and MD (ShrinkMD)
following Eqs 2 and 3, respectively.

(2) ShrinkTD ¼ ðWTDpre  WTDpost Þ  100=WTDpre

(3) ShrinkMD ¼ ðWMDpre  WMDpost Þ  100=WMDpre

SHRINK FORCE
Shrink force was measured in both the hoop and MD using a
custom device comprised of an Omega 44-N load cell and signal
conditioner, a multi-meter, and fixture (Fig. 3). Shrink
band samples were prepared in the hoop direction by cutting a
1.27-cm-wide material sample across the TD, resulting in an
intact tube. Two u-rings were used to hold the samples in line
with the linear load cell (Fig. 3, left). Samples were prepared in
the MD by slicing the shrink band lengthwise and then using a
precision cutter to cut a 6.35- by 1.27-cm sample. The samples
were clamped lengthwise with the MD in line with the linear
load cell (Fig. 3, right). A silicon oil bath, heated to a tempera-
ture of 130 C, was used to shrink the samples. Each sample was
immersed into the oil bath for 5 s. Shrink force was calculated
according to Eq 4, while shrink strength was calculated accord-
ing to Eqs 5 and 6 for the shrink force in the hoop direction
and MD, respectively.
(4) ShrinkForce ¼ MaxForce  Forceinitial
(5) ShrinkStrengthhoop ¼ ShrinkForcehoop =ð2  Whoop  thoop Þ
(6) ShrinkStrengthMD ¼ ShrinkForceMD =ðWMD  tMD Þ
FIG. 4 Temperature and time effects on shrinkage of PVC W.
Results
SHRINK PROPERTIES
Increasing temperature and dwell time clearly increased the
amount of shrinkage of PVC (Fig. 4). A higher level of shrink-
age was found in TD than MD due to orientation effects. Rate
of shrinkage as a function of temperature was found to vary
depending on the film direction. The differences in the amount
of shrinkage as a function of dwell time was exaggerated with
decreasing temperature. These results confirm that temperature
relieves the internal stress introduced in the material via stretch-
ing (orientation) [2,8]. Orientation effects on ultimate shrinkage
are reported elsewhere [9].
Figure 5 compares the shrinkage properties of different
shrink band materials. The amount of shrinkage in the TD was
larger than the MD for all shrink bands due to a different degree
of orientation. In general, non-PVC shrink bands showed more
shrinkage than PVC shrink bands in the TD while there was
less shrinkage in the MD. The clear PET samples tested had the
highest shrinkage among non-PVC shrink bands in both testing
direction.
Table 1 shows the comparison of shrink stress properties.
Shrink stress of non-PVC shrink bands was higher in the TD
(hoop) than PVC, while lower in the MD. Moreover, clear PVC
had lower hoop stress than white PVC. Shrink stress overall was
lower in the MD than TD following the same trend aforemen-
tioned for the amount of shrinkage.

TABLE 1 Comparison of shrink stress between PVC and non-PVC.

Designation ShrinkStrengthhoop/kN m2 ShrinkStrengthMD/kN m2

PVC C 841 6 165 517 6 159
PET W 662 6 152 97 6 28
PVC W 1965 6 400 372 6 48
PET C 2130 6 262 283 6 41
PETg W 2372 6 90 393 6 62
 KALKAN-SEVINC AND STROBEL ON HEAT SHRINKABLE FILM 1535

TABLE 2 Phase transition of shrink band samples.

Designation Tg/ C (1st Heat) Tcca/ C (1st Heat) Tmb/ C (1st Heat) Tcc/ C (1st Cool) Tgd/ C (2nd Heat) Tm/ C (2nd Heat) Tc/ C (2nd Cool)
PVC W 52.9 6 0.62
PVC C 61.9 6 0.44
PET W 74.8 6 0.18 127 6 0.6 249 6 0.2 181 6 1.2 76.1 6 1.13 249 6 0.2 181 6 1.7
PET C 76.3 6 4.86 128 6 2.1 246 6 0.1 184 6 3.4 74.3 6 0.55 245 6 0.7 184 6 3.1
PETg W 66.9 6 2.33 132 6 1.3 218 6 0.2 183 6 0.4 68.3 6 0.04 216 6 0.01 184 6 0.5
a
cc ¼ for cold crystallization.
b
m ¼ melting.
c
c ¼ crystallization.
d
g ¼ glass transition.

THERMAL PROPERTIES
The phase transition temperatures of non-PVC and PVC
shrink band materials were summarized in Table 2. Clear
PVC had higher glass transition than white PVC. Addition
of colorants, specifically inorganic ones, may cause the free
volume to increase (decrease in glass transition), as it
increases the heterogeneity of the PVC blend. A similar
effect was not concluded for PET due to the larger measure-
ment error seen in the results. White PETg had the lowest
glass transition temperature among other non-PVC shrink
bands, which was as expected due to glycol modification
during polymerization.
The non-PVC shrink band showed cold crystallization dur-
ing the first heating cycle as typical for the partially crystalline
materials that contain aromatic rings in their backbones [10].
White PETg had a higher cold crystallization temperature than
other non-PVC shrink bands. The melting point of PETg was
lower than other non-PVC shrink bands as calculated from
both of the heating cycles. The crystallization temperature of
white PET was lower than other non-PVC shrink bands as
calculated from both cooling cycles. White PET displayed a dip
during glass transition while clear PET did not. Relaxation of
residual-in-stresses arising from previous processing history
may contribute to that behavior.
Crystallinity of the shrink bands was summarized in Table 3.
Crystallinity of non-PVC shrink bands increased during the
second heating cycle after erasing the prior processing history.
White PETg showed the highest crystallinity among other non-
PVC materials during the first heating cycle while the lowest
was shown in the second heating cycle. PVC shrink band had
the lowest crystallinity. Crystallinity was similar between clear
and white grades of PVC shrink band.
MECHANICAL PROPERTIES
Tear properties are critical in many packaging applications with
some applications requiring the shrink bands to be able to be
torn and some requiring better tear resistance. Tear properties
of PVC and non-PVC shrink band was compared in Figs. 6–8.
In general, non-PVC shrink bands required higher force to
progress a tear than PVC (Fig. 6). Orientation effects were sig-
nificant for non-PVC compared with PVC shrink bands, sug-
gesting more balanced properties for PVC (Figs. 6–8). The force
required for a tear failure was much higher for non-PVC shrink
bands. Clear PET performed the best in MD while white PETg
performed the best in TD for applications requiring tear resist-
ance. No significant differences were seen between PVC and
non-PVC shrink bands for tear extension at failure (Fig. 8).
Mechanical properties of shrink bands exhibited under ten-
sile deformation were shown in Figs. 9–13. No significant orien-
tation effects were seen in stress at break (Fig. 9). Non-PVC
shrink bands displayed higher stress at break than PVC indicat-
ing higher force requirements to fail under tension mode. Clear
PET had the highest stress at break among the shrink band
materials studied.
All shrink band materials showed higher modulus in the
MD than in the TD (Fig. 10). The modulus of non-PVC shrink
bands was similar to PVC irrespective of the testing direction
except for PETg in the MD (Fig. 10).

TABLE 3 Crystallinity from DSC.

Designation DHc/J g1 (1st Heat) DHm/J g1 (1st Heat) X/% (1st Heat) DHm/J g1 (2nd Heat) X/% (2nd Heat)
PVC W NA 7 6 0.7 3.7 6 0.4 NA NA
PVC C NA 7.6 6 1.2 4.3 6 0.7 NA NA
PET W 32 6 0.9 45 6 0.8 10 6 0.5 48.2 6 0.97 34.4 6 0.69
PET C 29 6 1.3 40 6 1.0 8 6 1.7 44.8 6 1.39 31.9 6 0.99
PETg W 9 6 0.4 23 6 0.2 16 6 0.3 19.6 6 1.83 22.3 6 2.03
1536 Journal of Testing and Evaluation

FIG. 6 Comparison of force required for initiating a tear. FIG. 9 Comparison of tensile stress at break of shrink bands.

FIG. 7
Comparison of force required for tear failure.

FIG. 8
Tear extension at failure.

FIG. 10 Comparison of modulus of shrink bands.
White PETg had the lowest yield stress among other shrink
band materials (Fig. 11). Even though white PET had yielding
and breaking in the TD, it did not show an apparent yield point
in the MD. Orientation effects were significant for toughness of
non-PVC shrink bands, which was different from PVC (Fig. 12).
White PETg shrink bands had a similar toughness to PVC
shrink bands. Even though clear PET was tougher than PVC in
both directions as exhibited by high energy at fracture, white
PET was tougher only in the TD.
Significant differences were seen in the failure behavior
of white PET as a function of the film direction, which was dif-
ferent from clear PET (Fig. 13).
Discussion
Experimental data from this study confirms the correlation
between shrink stress and shrinkage (Fig. 14).
White PET had the lowest shrinkage among other non-
PVC shrink bands. The stretch ratio and temperatures during
processing are known to significantly influence the ultimate
shrinkage [2,8,9,11].
FIG. 11 Comparison of yield stress of shrink bands.
KALKAN-SEVINC AND STROBEL ON HEAT SHRINKABLE FILM 1537
FIG. 12 Comparison of fracture energy of shrink bands.
A correlation was found between the shrink stress and
tensile modulus (Fig. 15). The modulus is known to be sensi-
tive to processing effects (crystallinity, orientation factor,
thermal history) and intrinsic properties, such as molecular
weight, chemical structure, etc. [12]. No other tensile prop-
erty was found to correlate well with the shrinkage properties
of the material. Total crystallinity was not correlated with
shrinkage (Table 3). These findings are attributed to differen-
ces in degree of orientation (MD versus TD) arising from
previous processing history and possible variations in molec-
ular weight. The literature reports the effect of molecular
weight and processing history on shrinkage of oriented
polymers [13,14].
Significant difference in fracture failure of white PET was
observed as a function of film direction. While white PET
showed shear yielding via necking in TD, it fractured from both
ends without any indication of necking in MD. On the contrary,
clear PET showed shear yielding with the formation of necking
in both directions (Fig. 13). Plastic flow sets in at the yield point,
and then the neck appears in the samples as typical for partially
crystalline materials and some amorphous polymers [15]. This
phenomenon appears with either shear yielding as observed via
necking due to cold drawing and apparent yield point in the
FIG. 13 Representative stress-strain curve for PET shrink bands.
1538 Journal of Testing and Evaluation
FIG. 14 Correlation between shrinkage and shrink stress.
stress-strain curve or crazing due to voids or micro deformation
zones present in the polymer [15]. Material failing due to
crazing does not display an apparent yield point as a result of a
brittle fracture. It is shown in the literature that mechanical
properties of PET widely vary depending on the processing
conditions and post-processing treatment [12]. Differences in
the degree of orientation in both directions of white PET are
apparent from higher tensile stress in the TD than the MD.
Therefore, differences in the degree of orientation of white PET
may explain the great difference observed in the failure
behavior. On the other hand, white PETg did not display brittle
failure in MD. It is noteworthy that white PETg was a softer
material looking at the lower glass transition temperature and
also had lower modulus than PET.
Conclusions
Shrink strength was correlated well with the amount of
shrinkage for all PVC and non-PVC shrink bands studied. A
FIG. 15 Correlation between mechanical and shrink properties.
mathematical correlation was found between the shrink prop-
erties (strength and shrinkage) and tensile modulus while no
correlation was found between shrink properties and total
crystallinity. Differences in orientation factors arising from
previous processing history and molecular weight may con-
tribute to the correlation between modulus and shrink prop-
erties. Orientation effects are apparent from tensile properties
and failure mode between the white and clear formulations
of PET.
All non-PVC shrink bands were found to have more tear
resistance than PVC based on the force required to have tear
failure. Non-PVC shrink bands can replace PVC after verifying
the sealing because of measured differences in shrink properties
(strength and shrinkage).
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[3] Riesen, R. and Schawe, J. E. K., “Expansion and Shrinkage
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[7] ASTM D1938-14: Standard Test Method for Tear-
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