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Polymer Testing 23 (2004) 195202

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Test Method

Influence of notching and molding conditions on


determination of EWF parameters in polyamide 6
R.S. Yamakawa a,, C.A. Razzino a, C.A. Correa b, E. Hage Jr. a
a

Department of Materials Engineering, DEMa, University of Sao Carlos, UFSCar Rodovia Washington Luiz, km 235, C.P. 676,
CEP 13565-905 Sao Carlos, SP, Brazil
b
Graduate Program in Materials Engineering and Science/University of Sao Francisco, USF, Itatiba, SP, Brazil
Received 3 May 2003; accepted 1 July 2003

Abstract
The evaluation of the fracture toughness of polymers is highly relevant, particularly because of the ongoing development of new polymeric blends, most of which are aimed at increasing the impact resistance of engineering plastics.
The toughness evaluation method, known as essential work of fracture (EWF), is a relatively simple method, useful
for application on both brittle and ductile materials. This study investigated the effect of thickness, processing and
testing conditions on the fracture behavior of polyamide 6. To this end, test specimens of the DDENT (double deeply
notched tensile) geometry were tensile-tested under low (uniaxial tension) and high (tensile-impact) strain rates. The
results, which are presented in terms of the variation of total fracture energy according to the ligament length, revealed
that injection molded specimens without a pre-cracked notch offered the best choice. The geometrical criterion established by the ESIS protocol (test of the European Structural Integrity Society) for application of the EWF was also
reviewed.
2003 Elsevier Ltd. All rights reserved.
Keywords: EWF method; Toughness; Processing; Pre-crack; Polyamide 6

1. Introduction
Application of the linear elastic fracture mechanics
(LEFM) for characterization of the fracture toughness of
ductile materials is inadequate, since the large plastic
zone at the notch front invalidates basic LEFM criteria.
In response to this need, the J-Integral method was
developed to evaluate the fracture toughness of ductile
materials. Although this technique is adequate, it still has
some disadvantages, i.e. in addition to being time-consuming, it provides unreliable experimental measures
[1].
The essential work of fracture (EWF) method was

Corresponding author. Tel: +5516 2608530; fax: +5516


2615404.
E-mail address: elias@power.ufscar.br (R.S. Yamakawa).

developed as an alternative, less time-consuming method


of measuring the fracture toughness of plastic materials.
Owing to its simplicity, the EWF method has been
applied successfully in the studies of resistance to crack
propagation in both ductile and fragile materials [29].
The EWF concept [10,11] is based on the fact that the
total work of fracture (Wf), or the energy absorbed in the
fracture of a test specimen, can be divided into two basic
components (Fig. 1), i.e.
1. the essential work of fracture (we) performed in the
inner autonomous region named fracture process
zone (FPZ);
2. the non-essential work of fracture (wp) that occurs in
the outer plastic zone.
The total work of fracture can be expressed by the
following equation:

0142-9418/$ - see front matter 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/S0142-9418(03)00080-1

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R.S. Yamakawa et al. / Polymer Testing 23 (2004) 195202

specimens with different ligament lengths during


crack propagation, as illustrated in the load vs. elongation diagrams.
4. The FPZ volume involving the ligament must be proportional to the square of the length of the ligament
. The b parameter relative to the shape of the fracture process zone may be p / 4 (circular), ph / 4
(elliptical) or h / 2 (diamond-shaped), according to
the ESIS protocol for EWF measures [12].

Fig. 1. Test specimen for double deep notched tension specimen (DDENT), highlighting the fracture process and the plastic
zone forming along the ligament.

Wf wet wpb2t

(1)

where is the ligament length, b is a geometry-dependent plastic zone shape factor and t is the specimen
thickness. The term containing we represents the energy
required to create a unit fracture surface area, while the
term containing wp corresponds to the energy dissipated
per unit volume in the whitened zone under tension.
Dividing Eq. (1) by t yields the specific total work of
fracture, wf,
wf we bwp

(2)

Assuming that we is a material parameter and that wp


and b are independent of , when wf is plotted as a function of , according to Eq. (2), there should be a linear
relationship between wf and . By extrapolating this
straight line to a ligament length () equal to zero, we
can be determined by the intersection of the straight line
and the Y axis. The slope of this straight line yields
bwp. However, if b changes with the geometry of the
fracture process zone [8] and with the initial crack
length, a linear relation between wf and can only be
achieved if the geometrical similarity is maintained for
all the ligament lengths.
Application of the EWF method to determine fracture
toughness using the above equations depends on four
assumptions [1]:
1. Before the crack begins, the ligament must be totally yielded.
2. For (we) and (bwp) to remain constant and independent of the ligament length, the equations apply
in theory to the biaxial condition (plane stress). Thus,
the linear relation between wf and may be invalid
if the fracture occurs in a biaxial/triaxial transition
region (plane stress/plane strain).
3. There must be a geometrical similarity among test

Nylon 6 is a thermoplastic whose toughness is very


notch sensitive. The vast application of this material as
an engineering plastic also justifies the interest in studying it. This is a highly hygroscopic material and humidity
is a serious problem in its processing. The main problems encountered in the studies of the fracture behavior
of ductile polymers applying the EWF method involve
the preparation of test specimens and their correct notching. Ductilebrittle transitions that are dependent on the
load rate and specimen geometry (ligament thickness and
length) may also take place and impose drawbacks to
the method [1319]. The purpose of this work was to
investigate the effect of the thickness of test specimens,
the type of processing and the pre-crack made at the
notch front on the validation of the EWF method in polyamide 6. The fact that it is a semi-crystalline polymer
also poses problems in the injection process [19,20],
since uneven surfaces can occur, as well as warping if
the mold cooling system is not well balanced. Differences may also occur in the crystallinity of test specimens if any of the machines conditions are altered.
Another major problem has to do with the preparation
of the notch, owing to the extreme susceptibility of nylon
6 to stress concentration. Thus, great care in the notch
milling is required, since any variation of the notch tip
radius may lead to a substantial dispersion of the EWF
parameters.

2. Materials and methods


2.1. Materials
The main properties of the material used in this study,
the polyamide 6 B3K from Basf Polmeros S/A are listed
in Table 1.
2.2. Methods
2.2.1. Compression molding
Nylon 6 was first vacuum oven-dried for 24 h at 80
C, after which the oven was switched off but the vacuum maintained until the oven was cooled to ambient
temperature to prevent the material from oxidizing. The
material was kept in a dryer until it was molded.

R.S. Yamakawa et al. / Polymer Testing 23 (2004) 195202

197

Table 1
Properties of nylon 6
Properties

Standard

Value

Melt volume-flow rate (cm3/10 min)


Izod impact strength (J/m)
Tensile strength at break (MPa)
Modulus of elasticity (GPa)
Heat distortion temperature (HDT) (C)
n (g/mol)a
Average molecular weight M
Melt temperature (C)b

ISO 1133 (275 C/5 kg)


ASTM D256
ASTM D638 (5 mm/min)
ASTM D638
ASTM D648 (1800 kPa/method A)

120
31.9
52.2
2.9
54.8
21,000
220

a
b

Measured by chemical analysis of end groups of chain.


Basf technical catalog.

The material was pressed at a temperature of 235 C


under a 5-ton load until it was completely melted. The
heating system was then switched off and the water cooling process started.
Because the sheets obtained by injection molding had
a 3.2 mm thickness, it was decided that the thickness of
the sheets should be the same here, since the objective
of this part of the work was to verify the influence of
processing conditions on the EWF parameters. The
DDENT (double deeply notched tensile) test specimens
were taken from these sheets for the uniaxial tension
tests.
2.2.2. Injection molding
Nylon 6 test specimens were molded according to the
manufacturers specifications, using an ARBURG Model
270V injection machine. The material was first vacuum
dried similar to the compression molding conditions.
Sheets 3.2 mm thick and 70 mm wide were employed
in order to work in the plane stress region. In this case,
it is useful to seek a lower thickness-to-width relation,
i.e. a state of plane stress or biaxial tension. This sheet
yielded four test specimens, but only specimens from the
region furthest away from the gate of the injection mold
cavity were used, i.e. the test specimens of positions 3
and 4 in Fig. 2.
2.2.3. Notching with the mill cutter
The test specimens were notched 48 h after molding,
and then left to rest under controlled temperature (~23
C) and humidity (~65%) for 1 week. Dual notches were
milled into the DDENT test specimens, following the
ASTM D6068 standard, as shown in Fig. 3. The notches
were made at varying depths so that the length of the
ligament would vary in 2-mm increments.
2.2.4. Mechanical testing
All the tests were conducted at ambient temperature,
using the DDENT test specimens with a width of 22 mm,
thickness of 1.6 and 3.2 mm and ligament lengths of 6,

Fig. 2. Diagram of the sheet obtained by injection molding,


illustrating the gate and positions from which the test specimens
for the EWF tests were taken.

Fig. 3. Notched bars used in the tensile test prepared according to the ASTM D6068 standard.

8, 10, 12, 14, 16 and 18 mm. The uniaxial tensile tests


were carried out at three different speeds: 5, 50 and 500
mm/min, on a universal INSTRON model 5569 testing
machine, and the data treated with Merlin II software
programs. The impact tests were performed with a 7.5 J

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R.S. Yamakawa et al. / Polymer Testing 23 (2004) 195202

hammer and an impact load rate of 3.7 m/s, using a Resil


25 machine (Ceast. SpA.) with an instrumented data
acquisition system. The data were treated using
D4EXTWIN software.
The analysis of the results included checking whether
nylon 6 followed the validity criteria for application of
the EWF method. The load vs. elongation curves were
compared for each thickness and testing condition. After
the validity criteria and the similarity of the load vs.
elongation curves were checked, the we and bwp parameters were calculated.

3. Results and discussion


3.1. Effect of the type of molding and pre-crack
A simple visual comparison of the sheets obtained by
compression and injection molding revealed a considerable difference in terms of color. The sheet obtained by
compression was rather more opaque. An attempt to
bend the sheets manually demonstrated that the sheet
obtained by compression molding was much stiffer. This
result was confirmed in practice, by an observation of
the force (N) vs. displacement (mm) curves.
The curves of the test specimens obtained by compression molding were in general characteristic of brittle
materials, while the notched and pre-cracked injected
molded specimens showed an intermediary behavior
with some of them breaking in a brittle and others in
a ductile manner. Such behavior tends to preclude the
application of the EWF method in this material. Therefore, the results had to be separated into two groups,
according to the fracture behavior: specimens with ductile and specimens with brittle behavior (Fig. 4). This
difference in behavior is well evidenced in the data
shown in Table 2. This statement is illustrated by the
differences in the values of bwp, which is the measure
of the contributions to the plastic work, i.e. the higher
this value, the greater the materials capacity to absorb
strain energy during the fracture process.
When nylon 6 behaved in a ductile manner (injection
molded and notched with and without pre-cracks), a certain dependence was observed in relation to the specimens geometry, as already observed by Paton and Hashemi [13]. Ligament lengths of less than approximately
one-third of the width should be used for DDENT test
specimens, with possible variations according to the
material being employed. This limit serves to avoid problems with the specimens edges. For the nylon 6 used in
this study, this value was found to be slightly higher
(Fig. 5), i.e. 18 mm, when the expected value would have
been 11 mm. Based on this value, there was an evident
change in the slope of the curve which prevented the
EWF method to be applied, since negative essential work

Fig. 4. Plot of wf as a function of the nylon 6 ligament:


test specimens obtained by compression molding; notched
and pre-cracked injection molded specimens; continuation of
the injection molded test specimens notched but not pre-cracked
(change in the slope of the curve); notched and pre-cracked
injection molded test specimens (specimens with ductile
behavior); continuation of the notched and pre-cracked injection molded test specimens (specimens with ductile behavior,
with a change in the slope of the curve); and notched and
pre-cracked injection molded test specimens (specimens with
brittle behavior).

of fracture values, we, would have been obtained. This


of course, is not physically possible.
An analysis of all the results obtained from the precracked notch test specimen, even the sheets obtained by
compression molding, in which the processing influences
are minimized, showed a great dispersion of the results
and it was found that the manually pre-cracked notch
area possibly affected the results. For this reason, a test
was performed without pre-cracks, containing only the
notch made according to the ASTM D6068 standard,
using a milling cutter that allows one to obtain a very
sharp notch end. Because each lot with different ligament
lengths is cut all at once, this ensures that all the specimens have the same notch measure and depth. The precrack, on the other hand, is made manually in each specimen, which does not ensure a constant notch depth.
This aspect is even more critical for nylon 6 because
this material is highly-notch sensitive. Thus, it was
decided to test the specimens without pre-cracked
notches, which appeared to be the best alternative at
that time.
An analysis of the force (N) vs. displacement (mm)
curves revealed improved repeatability and the assurance
of complete yielding of the ligament. Visually, it was
also possible to see the entire yielding of the fracture
process region. The value of the linear correlation coefficient (R) was also an evidence that the results were
much more closely related to the EWF theory (Table 2)

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199

Table 2
Results obtained from the graph in Fig. 4 for nylon 6. we is obtained from the intersection with the axis of the ordinates; bwp is the
slope of the straight line and R is the linear correlation coefficient
Test specimen

we (kJ/m2)

bwp (MJ/m3)

Pre-cracked notch compression molded specimen


Notched injection molded specimen (no pre-cracking)
Notched and pre-cracked injection molded specimen (brittle fracture)
Notched and pre-cracked injection molded specimen (ductile fracture)

24.37
24.01
15.48
7.39

0.5
15.9
1.83
8.74

0.60
0.99
0.55
0.64

Fig. 5.

Force (N) vs. displacement curves.

than those of the test specimens with pre-cracked notches.


With regard to the fracture toughness given by the
essential work of fracture value, we, it can be seen from
the values in Table 2 that nylon 6, when compression
molded, displayed higher values than when it was injection molded in test specimens with pre-cracked notches.
This evidences the negative influence of the injection
molding process on the fracture toughness of such
material. However, when no pre-cracked notches were

used, the injection molded polyamide 6 showed a we that


was practically identical to that of the specimens
obtained by compression.
3.2. Influence of the thickness and strain rate
The test protocol of the European Structural Integrity
Society (ESIS) for EWF establishes the following geometrical criterion for measurements of EWF in a biaxial
condition (plane stress): 3t W / 3, where t and W

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R.S. Yamakawa et al. / Polymer Testing 23 (2004) 195202

are the thickness and the width of the test specimen.


However, as in other studies [8,15,16], we have used
ligament length values out of this range, considering only
that the ligament is entirely yielded before the propagation of the crack. The similarity of the force vs. displacement plots (Fig. 5, graphs af) was also used as a
criterion to validate the application of the EWF method.
Based on the data shown in the graphs of Fig. 6, Table
3 lists the values of the EWF parameters. These parameters proved consistent, clearly demonstrating a linear
behavior in the wf vs. relation in both thicknesses analyzed, particularly under quasi-static test conditions (5
and 50 mm/min). This is a very interesting behavior,
since polyamide 6 is a semi-crystalline material considered pseudo-ductile, with a strong tendency for
unstable crack propagation. As can be seen, the data
obtained from the 18 mm ligament showed a very differ-

ent behavior from that of the other points, so they were


discarded in order to eliminate a possible border effect.
A reduction in the materials toughness was observed
with increasing strain rate, particularly when the specimens were tested at higher strain rate under dynamic
loading conditions (tensile-impact testing, at 3.7 m/s).
This effect was caused by the polymers viscoelastic
properties and was more evident in the thicker sheet (3.2
mm), as demonstrated by the reduction of the wp value
shown in Table 4. This value represents the materials
yield capacity through micro-strain mechanisms (shear
bands), which are responsible for dissipating the energy
around the FPZ. These mechanisms are strongly dependent upon the material microstructure which, in turn,
depends on the effects of the processing conditions and
differs for each thickness.

4. Conclusions

Fig. 6. Plot of wf vs. ligament in specimens with different


thicknesses for varying testing speed. (a) 1.6 mm thickness; (b)
3.2 mm thickness.

The EWF method can be applied effectively not only


to characterize films but also for much thicker injectionmolded specimens, provided the influence of the processing conditions employed to obtain them are taken
into account. The differences in the EWF parameter
values of the various thicknesses can be attributed to
microstructural changes, particularly in semi-crystalline
polymers.
The geometrical criterion established by the ESIS protocol for application of the EWF method severely
restricts the range of variation of the ligament length and
fails to consistently define the application limits, given
that the results presented here were obtained outside the
specified range of variation and that the conditions of
application of the EWF method were met. It can be concluded that the essential work of fracture, we, was negatively affected by the injection molding of the test specimens. On the other hand, however, the injection molding
process increases the ligaments capacity to absorb plastic energy. The results show that compression molding
is not affected by the surface layer and morphology
gradient, as in the case of injection molding. Therefore,
the toughness of nylon 6 increases, but the plastic energy
absorption decreases because of the greater stiffness of
the compression molded specimen.
It was also concluded that pre-cracks made manually
with a cutting blade led to a wide dispersion of results,
owing to the high notch sensitivity of nylon 6. Hence,
injection molded test specimens notched only with a
milling cutter proved to be a better option for application
of the EWF method than test specimens with notches
manually pre-cracked with razor blades.

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201

Table 3
Results of the thickness and strain rate influence on the EWF parameters
Material: nylon 6

EWF parameters

Thickness (mm)

Testing speed

we (kJ/m2)

bwp (MJ/m3)

1.6

5 mm/min
50 mm/min
500 mm/min
3.7 m/s
5 mm/min
50 mm/min
500 mm/min
3.7 m/s

36.94
28.95
65.75
30.96
11.82
1.61
3.20
26.34

16.77
17.48
14.65
2.90
20.83
20.74
16.16
0.43

0.99
0.99
0.98
0.80
0.99
0.99
0.98
0.41

3.2

Table 4
Injection molding conditions of nylon 6
Condition

Value

Holding pressure (bar)


Nozzle temperature (C)
Mold temperature (C)
Cooling time (s)

700
250
60
20

Acknowledgements
The authors gratefully acknowledge BASF S.A. for
donating the materials used in this study, as well as
FAPESP, CAPES and PRONEX (Brazilian research
funding institutions) for their financial support.

References
[1] Y.-W. Mai, S.-C. Wong, X.-H. Chen, in: D.R. Paul, C.B.
Bucknall (Eds.), Application of Fracture Mechanics for
Characterization of Toughness of Polymer Blends, Performance, vol. 2, Wiley, New York, 2000.
[2] D.M. Laura, H. Keskkula, J.W. Barlow, D.R. Paul, Effect
of glass fiber and maleated ethylene-propylene rubber content on the impact fracture parameters of nylon 6, Polymer
42 (2001) 6161.
[3] O. Okada, H. Keskkula, D.R. Paul, Fracture toughness of
nylon 6 blends with maleated ethylene/propylene rubbers,
Polymer 41 (2000) 8061.
[4] R.A. Kudva, H. Keskkula, D.R. Paul, Fracture behavior of
nylon 6/ABS blends compatilized with an imidized acrylic
polymer, Polymer 41 (2000) 335.
[5] O.O. Santana, M.L. Maspoch, A.B.P. Martinez, Plane
strain essential work of fracture in SENB geometry at low
and high strain rates of PG/ABS blends, Polym. Bull. 39
(1997) 511.
[6] Y. Yokoyama, T. Ricco, Toughening of polypropylene by
different elastomeric systems, Polymer 39 (1997) 3675.

[7] Y.-W. Mai, On the plane-stress essential fracture work in


plastic failure of ductile materials, Int. J. Mech. Sci. 35
(1993) 995.
[8] H. Heino, P. Hietaoja, J. Seppala, T. Harmia, K. Friedrich,
Studies on fracture behavior of tough PA6/PP blends, J.
Appl. Polym. Sci. 66 (1997) 2209.
[9] G. Wildes, H. Keskkula, D.R. Paul, Fracture characterization of PC/ABS blends: effect of reactive compatibilization, ABS type and rubber concentration, Polymer 40
(1999) 7089.
[10] Y.-W. Mai, B. Cotterell, Effect of specimen geometry on
the essential work of plane stress ductile fracture, Eng.
Fract. Mech. 21 (1985) 123.
[11] Y.-W. Mai, P. Powell, Essential work of fracture and Jintegral measurements for ductile polymers, J. Polym. Sci.
29 (1991) 785.
[12] Test Protocol for Essential work of Fracture (Version 5),
ESIS-European Structural Integrity Society, October 5,
1997.
[13] C.A. Paton, S. Hashemi, Plane-stress essential work of
ductile fracture for polycarbonate, J. Mat. Sci. 27 (1992)
2279.
[14] M.L. Maspoch, D. Ferrer, A. Gordillo, O.O. Santana, A.B.
Martinez, Effect of the specimen dimensions and the test
speed on the fracture toughness of iPP by the essential
work of fracture (EWF) method, J. Appl. Polym. Sci. 73
(1999) 177.
[15] J. Karger-Kocsis, T. Czigany, E.J. Moskala, Thickness
dependence of work of fracture parameters of an amorphous copolyester, Polymer 38 (1997) 4587.
[16] J. Karger-Kocsis, T. Czigany, E.J. Moskala, Deformation
rate dependence of the essential and non-essential work of
fracture parameters in an amorphous copolyester, Polymer
39 (1998) 3939.
[17] M.L. Maspoch, J. Ga mez-Pe rez, A. Gordillo, M. Sa nchezSoto, J.I. Velasco, Characterization of injected EPBC plaques using the essential work of fracture (EWF) method,
Polymer 43 (2002) 4177.
[18] P. Luna, C. Bernal, A. Cisilino, P. Frontini, B. Cotterell,
Y.-W. Mai, The application of the essential work of fracture methodology to the plane strain fracture of ABS 3point bend specimens, Polymer 44 (2003) 1145.
[19] J. Karger-Kocsis, T. Barany, Plane stress fracture behavior

202

R.S. Yamakawa et al. / Polymer Testing 23 (2004) 195202

of syndiotactic polypropylenes of various crystallinity as


assessed by the essential work of fracture method, Polym.
Eng. Sci. 42 (2002) 1410.
[20] D. Ferrer-Balas, M.L. Maspoch, A.B. Martinez, O.O. San-

tana, Influence of annealing on the microstructural, tensile


and fracture properties of polypropylene films, Polymer
42 (2001) 1697.

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