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POLYMER
TESTING
Polymer Testing 25 (2006) 544–552
www.elsevier.com/locate/polytest
Material Behaviour
Abstract
In this experimental work, we studied the mechanical behaviour of a short glass fibre reinforced polyamide frequently
used in the automobile industry.
In order to investigate the influence of glass fibre content, temperature and strain rate, we carried out a series of uniaxial
tensile loadings on an unfilled polyamide and glass fibre reinforced polyamide with different weight fractions: 15, 30 and
50 wt%.
Experimental results showed that the studied composite is a strain rate, temperature and fibre volume fraction
dependant material. Both elastic modulus and tensile strength increase with strain rate and decrease with temperature.
Glass fibre reinforced PA66 exhibits improvement in its mechanical strength. The evolution of the normalized modulus
and tensile strength as functions of relative density can be described by a type of power function.
The acoustic emission (AE) technique, which is recognized as an effective tool for non-destructive testing and material
evaluation, has been used to determine the damage threshold and obtain information about fracture mechanisms in the
studied composites.
Scanning electron microscopy (SEM) analysis was made on the fracture surfaces to visualize the damage process: fibre
fracture, matrix rupture and interface rupture.
r 2006 Elsevier Ltd. All rights reserved.
Keywords: Polyamide 66; Glass fibres; Mechanical behaviour; Damage; Acoustic emission
0142-9418/$ - see front matter r 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.polymertesting.2006.03.008
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B. Mouhmid et al. / Polymer Testing 25 (2006) 544–552 545
R 60
one of three regions: the matrix, the fibre or the
fibre/matrix interface [1]. The mechanical properties 150
of thermoplastic composites containing short fibres 60
20
have been the subject of much attention. These
properties result from a combination of the fibre
10
and the matrix properties and the ability to transfer
Fig. 1. Tensile specimen dimensions (mm).
stresses across the fibre/matrix interface, but also
depend on the injection conditions such as screw
and barrel parameters, mould temperature and and strain rates chosen were, respectively, T ¼ 20,
design [2–5]. Variables such as fibre ratio, diameter, 50 and 80 1C and 1, 5 and 50 mm/min corresponding
length, orientation and the interfacial strength are to e_ ¼ 1:1 103 ; 5:6 103 and 5:6 102 s1 .
of prime importance to the final properties of the
thermoplastic composites according to the studies 2.2. Damage analysis technique
led by Thomasson [6] and Shao-Yun Fu [7].
In this study, we characterized mechanically the The tensile test was made with acoustic emission
behaviour of glass fibre reinforced and unreinforced monitoring by the use of a Vallen AMSY 5 system.
polyamide 66. The effects of glass fibre content, Acoustic emission (AE) is elastic radiation gener-
temperature and strain rate have been investigated. ated by the rapid release of energy from sources
An AE monitoring technique was used to identify within a material. These elastic waves are detected
different types of failure in the investigated compo- and converted to voltage signals by small piezo-
sites. In order to visualize the damage process, electric sensors mounted on a convenient surface of
scanning electron microscopy (SEM) analysis was the material. The result is that AE can be used to
made on the fracture surface of the specimens. monitor a structure for active damage even when
The stress–strain response of the PA66 depends ambient noise levels are extremely high. Sources of
strongly on the humidity conditions. PA66 is acoustic emission include in this case all types of
considered as dry when the water absorption is less damage.
than 0.2% and saturated at 7.2%. The tensile
strength in glass fibre reinforced PA66 is 50%
3. Results and discussions
higher in the dry state than in the saturated one [22].
In this section, the influence of an intrinsic
2. Experimental procedure
parameter (glass fibre content) and two extrinsic
parameters (strain rate e_ and temperature T) on the
2.1. Material and tensile test conditions
three mechanical properties of tensile elastic mod-
ulus E, tensile strength sr and the failure strain er ,
Chopped E-glass and PA66 were used to produce
has been investigated.
moulded composites with 0, 15, 30 and 50% (wt)
glass content. The glass bundles and pre-dried PA66
pellets were dry blended to the desired glass content 3.1. Glass fibre content effect
and compounded on a single screw extruder. The
compounds were moulded on an 80 ton moulding Fig. 2 shows stress–strain curves obtained for the
machine. Compounding and moulding tempera- studied composites at T ¼ 20 1C and e_ ¼ 5:6
tures were respectively 275 and 280 1C with a mould 103 s1 . We can note the typical stress–strain
temperature of 80 1C. curves of reinforced materials showing high strength
The mechanical properties testing were performed levels and low deformation capabilities. Indeed,
at a relative humidity of 50% using ISO 527 glass fibre reinforced PA66 presents brittle beha-
specimens (Fig. 1). The tensile tests were carried viour with a failure strain of about 5.5%, whereas
out in a 10 kN Instron machine equipped with a unreinforced PA66 presents ductile behaviour with
temperature controlled chamber. The temperatures a failure strain of about 25%. This figure also shows
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546 B. Mouhmid et al. / Polymer Testing 25 (2006) 544–552
180.0 2.80
50%
160.0 2.60
y = 1x2.8
140.0 2.40 R2 = 0.99
30%
120.0 2.20
15%
σ (MPa)
100.0 2.00
σr/σr0
80.0 1.80
60.0 0% 1.60
40.0 1.40
20.0 1.20
0.0 1.00
0.0 5.0 10.0 15.0 20.0 25.0 30.0 1 1.1 1.2 1.3 1.4 1.5
ε (%) ρ/ρ0
Fig. 2. Stress–strain curves with different glass fibre ratios at Fig. 3. Variation of normalized tensile strength as a function of
20 1C and 5:6 103 s1 . relative density.
2.50
modulus and the tensile strength of the unreinforced
PA66, vf is the fibre volume fraction and a and b are
the fibre orientation factors [8]. In our case, the 2.00
average values of a and b are: a ¼ 0:24 and
b ¼ 0:072, these values depend on the fibre length
1.50
and orientation.
The evolution of these two mechanical para-
meters can also be modelled using a phenomen- 1.00
ological description based upon the relative 1 1.1 1.2 1.3 1.4 1.5
representations: normalized tensile strength sr =srm , ρ/ρ0
normalized elastic modulus E=E m versus relative
Fig. 4. Variation of normalized modulus as a function of relative
density r=r0 where r0 is the density of unreinforced
density.
PA66. Figs. 3 and 4 illustrate these evolutions and
show that they are described by power relationships
as follows:
expressions in a study about the mechanical
2:8 3:7
sr r E r behaviour of expanded polystyrene.
¼ and ¼ , This observation is in good agreement with
srm r0 Em r0
literature data [10,11] and can be explained by the
with a good correlation coefficient: R2 ¼ 0:99 for contribution of the glass fibre as a brittle and tough
both formulas. Imad [9] has suggested similar material. The loss of ductility is confirmed by the
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B. Mouhmid et al. / Polymer Testing 25 (2006) 544–552 547
90.0
70.0
Stress MPa
50.0
rupture specimen profile. In fact, the unreinforced In order to evaluate the effect of temperature on
PA66 clearly develops a striction zone. Contra- the tensile properties of the glass fibre reinforced
riwise, the glass fibre reinforced PA66 shows a PA66, the stress–strain curves were plotted. Typical
brittle fracture profile as shown in Figs. 5ab. stress–strain curves at a constant strain rate of 5:6
103 s1 are shown in Fig. 9.
3.2. Strain rate effect It is noted that the tensile behaviour of the
studied materials is strongly dependant on the
Fig. 6 illustrates the stress–strain curves obtained temperature. It can be seen that there is an obvious
from uniaxial tensile tests on unreinforced region AC called the ‘‘toe region’’ as shown in
PA66 specimens at room temperature (20 1C) with Fig. 10. The ‘‘toe region’’ does not represent a
the following strain rates: e_ ¼ 1:1 103 ; 5:6 material property but it is an artifact caused by the
103 and 5:6 102 s1 . These curves show that in take up of slack as observed, e.g., by Shi et al. [15].
unreinforced PA66 the tensile strength increases The slope between the origin B and point D on
with the increase of strain rate, whereas the failure the elastic section in the stress–strain curve is taken
strain drops, which means the material gets less as the Young’s modulus according to ASTM
ductile. An explanation is that for high values of standard D882-97 [16].
strain rate, molecular rearrangement does not have The effect of temperature on the Young’s
time to take place. This is in accordance with other modulus is shown in Fig. 11. We can see that the
results in the specialized literature [12]. The strain normalized Young’s modulus decreases with the
rate does not seem to have any significant effect on testing temperature, following a nonlinear relation-
the modulus in the range considered. ship. The normalized tensile strength also decreases
In glass fibre reinforced PA66, a typical stress– with increasing temperature as shown in Fig. 12.
strain curve is shown in Fig. 7. Elastic modulus and It can be noted that the failure strain increases as
tensile strength slightly increase as strain rate the temperature is increased up to 80 1C for the 15%
increases. Contrariwise, the failure strain is not (wt) short glass fibre reinforced PA66. Globally, the
affected by the strain rate in the range considered. effect of temperature on the failure strain is much
The tensile modulus and the tensile strength are more accentuated in unreinforced PA66 than in
plotted against logarithms of strain rate in Figs. 8a short glass fibre reinforced PA66, as shown in
and b and can be modelled using a simple regression Fig. 13.
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160.0
5mm/min
140.0
50mm/min
1mm/min
Stress (Mpa) 120.0
100.0
80.0
60.0
40.0
20.0
0.0
0.0 1.0 2.0 3.0 4.0 5.0 6.0
Strain (%)
Fig. 7. Stress–strain curves of 30% glass fibre reinforced PA66 for different strain rates.
6000
5500
5000
Modulus (MPa)
4500 PA66 0%
4000
PA66 15%
3500
PA66 30%
3000
2500 PA66 50%
2000
1500
1000
-7.00 -6.00 -5.00 -4.00 -3.00 -2.00
(a) Ln (strain rate)
200
180
160
Tensile strength (MPa)
140
120
100
80
60
PA66 0%
PA66 15% 40
PA66 30%
20
PA66 50%
0
-7 -6 -5 -4 -3 -2
(b) Ln (strain rate)
Fig. 8. (a) Variation of modulus as a function of ln ð_eÞ. (b) Variation of modulus as a function of ln ð_eÞ.
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B. Mouhmid et al. / Polymer Testing 25 (2006) 544–552 549
Table 1
Values of aE and bE for the different studied materials
0% SGFR PA66 15% SGFR PA66 30% SGFR PA66 50% SGFR PA66
90
20°C
80 Relative modulus
50°C
70 80°C 0% GFR PA66
Stress (MPa)
2.00
60 15% GFR PA66
1.80
50 30% GFR PA66
1.60
40 1.40 50% GFR PA66
30 1.20
E/Em
20 1.00
10 0.80
0 0.60
0 2 4 6 8 10 0.40
0.20
Strain (%)
0.00
Fig. 9. Stress–strain curves of 15% glass fibre reinforced PA66 at 0 20 40 60 80 100
strain rate of 5:6 103 s1 at different temperatures. Temperature (°C)
D 1.40
1.20
σ/σm
15 1.00
0.80
0.60
10 0.40
0.20
0.00
5 0 20 40 60 80 100
C Temperature (°C)
70
60
50
Failure strain (%)
40
PA00
PA15
30
PA30
PA50
20
10
0
20 40 60 80 100
Temperature (T°C)
For more comprehension of rupture mechanisms, Fig. 15. Unreinforced PA66 failure facies.
fracture surfaces have been observed by SEM.
Fig. 15 is a fracture surface photography of an crystalline defects, is the most probable hypothesis.
unreinforced PA66 showing craters. Cavitations Craze propagation led then to cracks. This stage
could have occurred and produced crazing. Crazing relates to the ductile behaviour of unreinforced
could also have occurred near initial voids or an PA66. Once the crack is created, it weakens the
existing defect that took place during moulding. material and primes the brittle rupture of the
However, the presence of spherolites, that are remaining ligament.
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