Composites Science and Technology: Bouchaib Mouhmid, Abdellatif Imad, Noureddine Benseddiq, D. Lecompte

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Composites Science and Technology 69 (2009) 2521–2526

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Composites Science and Technology


journal homepage: www.elsevier.com/locate/compscitech

An experimental analysis of fracture mechanisms of short glass fibre


reinforced polyamide 6,6 (SGFR-PA66)
Bouchaib Mouhmid a, Abdellatif Imad a, Noureddine Benseddiq b,*, D. Lecompte c
a
Laboratoire de Mécanique de Lille, CNRS UMR 8107, Ecole Polytech-Lille, Université de Lille 1, Cité scientifique, Avenue Paul Langevin, 59655 Villeneuve d’Ascq cedex, France
b
Laboratoire de Mécanique de Lille, CNRS UMR 8107, IUT-GMP, BP 179, 2 rue Recherche, 59491 Villeneuve d’Ascq cedex, France
c
Royal Military Academy, Department of Civil and Materials Engineering, Avenue De la Renaissance 30, 1000 Brussels, Belgium

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

Article history: In the present work, toughness of unfilled polyamide 6,6 (PA66) and short glass fibre reinforced polyam-
Received 5 February 2009 ide 6,6 (SGFR-PA66) was investigated. Digital image correlation (DIC) was used with a single camera for
Received in revised form 9 July 2009 in-plane displacement field measurement and then strain computation. The results allowed to extract the
Accepted 10 July 2009
resistance curve for the PA66 and critical stress intensity factors, KIc, for the SGFR-PA66 with three glass
Available online 16 July 2009
fibre contents (15%, 30% and 50% (wt)) and under room temperature (20 °C). The tests were carried out on
single edge notched tension (SENT) specimens. The DIC technique allowed to precise the spatial distribu-
Keywords:
tion of the local strains in a defined region including the crack tip at different steps of the loading. Scan-
A. Glass fibre reinforced composites
B. Toughness
ning electron microscopy observations illustrated different damage mechanisms occurring in the studied
D. Digital image correlation composites: matrix crack, fibre–matrix interface failure and fibres pull out.
Ó 2009 Elsevier Ltd. All rights reserved.

1. Introduction plastic zone prior to crack initiation. In this case, the J-integral pro-
posed by Rice [9] or crack tip opening displacement (CTOD) con-
It is well known that some mechanical properties of plastics are cept are used to quantify ductile tearing. Many authors have
improved by the incorporation of glass fibres. In the case of short applied toughness characterization of polymers using the J-integral
glass fibre reinforced polymer matrices, not only random arrange- [10–14].
ments of fibres but also their random orientations are observed In this paper, an experimental work was investigated in order
and the mechanical properties are highly dependent on these to evaluate the toughness of the PA66 and SGFR-PA66. The influ-
parameters, the matrix, the fibre/matrix interfacial strength and ence of fibre content was analysed in fracture behaviour for
the volume fraction of reinforcement [1–3]. these materials (0%, 15%, 30% and 50% fibre content). The DIC
Short fibre reinforced plastics are applied to automobiles be- technique was used as a fracture mechanics tool for two objec-
cause of their ease of fabrication, their light weight and economy. tives. The first one is to determine the strain distribution around
For such applications, high reliability is required and the investiga- the crack tip and check if critical values in terms of strain and
tion of fracture mechanisms is very important. Many experimental, classical fracture mechanics parameters are reached at the same
numerical and theoretical studies have been carried out in order to time. The second objective is to give a precise idea about the
investigate short glass fibre reinforced composites fracture mecha- spatial distribution of longitudinal strain (major strain) in PA66
nisms [4–7]. and SGFR-PA66. Several authors have used DIC method to study
Linear elastic fracture mechanics (LEFM) is one of the most fre- fracture behaviour and crack growth [15–17]. Scanning electron
quently used methods to characterize brittle fracture of polymers microscopy (SEM) analysis was made on the fracture surface to
and composites. Generally, the fracture toughness can be analyzed visualize the damage process: fibre fracture, matrix rupture,
in terms of the stress-intensity factor, KI, or the strain energy re- and interface rupture.
lease rate, G. According to the LEFM theory, when the parameters The effect of glass fibre content, strain rate and temperature on
KI and G reach critical values KIc and Gc, failure occurs [8]. the SGFR-PA66 mechanical behaviour had been a subject of a pre-
When ductile polymers are involved, fracture toughness charac- vious study [18]. The increase in fibre content leads to an increase
terization can not be carried out using LEFM because of the large in tensile strength and elastic modulus. The evolution of normal-
ized elastic modulus and normalized tensile strength versus rela-
tive density has been described by power laws:
* Corresponding author. Tel./fax: +33 3 26 67 73 26.
E-mail address: noureddine.benseddiq@univ-lille1.fr (N. Benseddiq). E=Em ¼ ðq=qm Þ3:7 ð1Þ

0266-3538/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2009.07.003
2522 B. Mouhmid et al. / Composites Science and Technology 69 (2009) 2521–2526

Fig. 1. Tensile and fracture specimens.

and

rr rrm ¼ ðq=qm Þ2:8 ð2Þ

where qm, Em and rrm are, respectively, the density, the elastic mod- Fig. 3. A sequence of CCD images illustrating crack growth in PA66.
ulus and the tensile strength of PA66 matrix and q, E and rr are,
respectively, the density, the elastic modulus and the tensile
strength of SGFR-PA66. Similar expressions have been suggested
PA66-0%
in other studies [19–21]. The loss of ductility is confirmed by the 3500
PA66-15%
rupture specimen profile. In fact, the unreinforced PA66 clearly PA66-30%
develops a necking zone. Contrariwise, the GFR-PA66 shows a brit- PA66-50%

tle fracture profile. 2500


Load (N)

2. Experimental procedure 1500

Chopped E-glass and PA66 were used to produce moulded com-


posites with 0%, 15%, 30% and 50% (wt) glass content. The glass 500
bundles and PA66 pellets, pre-dried at 110 °C in a vacuum oven
for 8 h, were blended to the desired glass content and compounded
0 2 4 6 8
on a single screw extruder. The compounds were moulded on an -500
80 ton moulding machine. Compounding and moulding tempera- Displacement (mm)
tures were, respectively, 275 and 280 °C with a mould temperature
of 80 °C. The mechanical properties testing were performed at a Fig. 4. Load–displacement curves for different materials.
relative humidity of 50% using ISO 527 specimens (Fig. 1a) in order
to determine the elastic modulus E, the yield strength ry, the ten-
sile strength rr and the failure strain er of the different materials. J=32,29(Δa)0,36
Fracture tests were carried out using SENT specimens (Fig. 1b) 50
under a crosshead speed of 1 mm/min. In all cases, tensile tests
J (KPa.m)

2σy
were carried out on a 10 KN Instron machine. 40
One side of each SENT specimen was sprayed with black paint 1

in order to form the speckle pattern to be used by the DIC 30


technique. JIc
The DIC technique, developed in the 1980s [22–24], consists of
20
displacement and strain determination. Since then, it has been
widely used in various domains. At each load step, an image, cor-
responding to a given state of deformation, is taken with a CCD 10

0
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2 2.2 2.4 2.6
Δa (mm)

Fig. 5. J–R curve for PA66.

camera and digitalized. It is then compared to the undeformed


state image (reference image) using a mathematical correlation
function. The software used for calculation of strains is Aramis.
The fundamental principal of Aramis is based on the fact that
the distribution of grey scale values of a rectangular area (facet)
in the undeformed state corresponds to the distribution of grey
Fig. 2. Measurement points represented by crosses. scale values of the same area in the deformed state.
B. Mouhmid et al. / Composites Science and Technology 69 (2009) 2521–2526 2523

2500 Zone 1 Zone 2 Zone 3

2000

1500
Load (N)
A
1000

500

O
0
0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0
Displacement (mm)

Fig. 6. PA66 fracture chronology.

The pictures resolution used is 28 lm and the distance between The data files resulting from DIC allowed extracting at each load
the measurement points is 0.29 mm (Fig. 2). Displacements and step a point of the load–displacement curve as shown in Fig. 4.
strains could then be calculated at every point of the studied Fig. 3 shows a selected sequence of CCD images depicting crack
region. growth in PA66 sample exhibiting a ductile tear. Time t = 0 s corre-
sponds to the beginning of loading.
3. Results and discussion At every loading step ti, corresponding to a displacement di and
the crack extension Dai, J is calculated according to [25] and the J–R
3.1. PA66-0% fracture behaviour curve is plotted in Fig. 5.
Critical value of J, JIc is about 27 kPa m = 27 kJ/m2. It is found by
For usual standard specimens, J-integral can be directly ex- determining the intersection of J–Da curve and a 0.2 mm offset line
pressed as a function of the deformation energy, U, according to parallel to the theoretical blunting line J = 2ryDa, where ry is the
the ASTM D6068-96 [25]: yield stress and Da is the crack growth.
Fig. 6 highlights three essential zones characterizing the PA66
U
J¼g ð3Þ behaviour at fracture:
BðW  aÞ
where B, W and a are, respectively, the specimen thickness, speci-  Zone 1: A non linear elastic zone which corresponds to the notch
men width and the crack length. g is a shape function. U is the area blunting. It extends to crack initiation point A. The deformation
under the load–displacement curve: takes place essentially through the bending and stretching of the
Z amorphous phase of the PA66.
di
U¼ PðdÞdd ð4Þ  Zone 2: A stable propagation zone where plastic deformations
0 develop as the crack is propagating. Extensive shear yielding,
and micro voids and matrix micro cracks occur during this ductile
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi fracture process. When the PA66 undergoes fracture, there is
 a 2 a clearly a creation of new surface which can only occur by sever-
g¼ 1þ  ð5Þ
ance of either primary (covalent) or secondary (van der Walls or
W a W a
hydrogen) bonds or both.

Fig. 7. Longitudinal strain distribution for the PA66.


2524 B. Mouhmid et al. / Composites Science and Technology 69 (2009) 2521–2526

Y 10 The following two images (Fig. 7) illustrate the evolution of the


y=6,620
9 longitudinal strain ey distribution and the size of the plastic zone
y=5,332
prior the crack tip during the loading.
8 y=4,467
It also shows that the strain field can be considered as homog-
Longitudinal strain εy (%)

y=3,603
7 enous far from the crack tip.
y=3,026
6 y=2,450
Fig. 8 is an example of evolution ey versus the x at different val-
ues of y-coordinate. It expresses the fact that ey is smaller on fur-
5 y
ther lines from the crack line.
4

3 3.2. SGFR-PA66 fracture behaviour


2
Crack tip The reinforcement of PA66 by short glass fibres increases the
1 x
toughness and the damage chronology is similar at different glass
0 fibre rates as shown in Fig. 9.
0 5 10 15 20 The DIC technique allowed highlighting three main steps in the
x : distance behind the crack tip (mm) damage process:

Fig. 8. Longitudinal strain versus x at different values of y-coordinate for the PA66.
 Zone 1: A linear elastic zone where the notch blunting is much
less significant than in unreinforced PA66 because of the glass
fibres toughening effect. The end of this zone is characterized
 Zone 3: An unstable propagation zone leading to load drop and by the crack initiation.
specimen failure.  Zone 2: A stable propagation zone where the load increases mod-
erately and non linearly. Plasticity is restricted compared to the
Let us focus the analysis on the longitudinal strain. At initiation, unreinforced PA66.
the strain level is about 25% 1 mm behind the crack tip and only 5%  Zone 3: An unstable propagation with a load drop and the spec-
when the distance behind the crack tip is greater than 4 mm. imen failure.

Fig. 9. Damage chronology in SGFR-PA66.


B. Mouhmid et al. / Composites Science and Technology 69 (2009) 2521–2526 2525

SGFR-PA66 7

KIc = 3,81(ρ / ρ o) - 0,0591 6


5.5 PA66-15% : εy=3,7x-0,5
R2 = 0,98
5 R2=0,8

εy (%)
KIc (MPa.m 1/2)

5 4

3
4.5
2

1
4
0
0 2 4 6 8 10
3.5
1 1.05 1.1 1.15 1.2 1.25 1.3 1.35 1.4 1.45
x (mm)
ρ /ρ o Fig. 12. Strain distribution on the crack line in the SGFR-PA66-15% case.

Fig. 10. Toughness evolution with the fibre content.

We can note that:

The toughness parameter used for these brittle materials is KIc, 1. On an average, the strain ey in the 15% case is 40% higher than in
the critical stress intensity factor. According to the ASTM D5045-99 the other two cases. In deed, ey could reach 6% in the 15% case,
[26], we can evaluate, from the load–displacement curve, the whereas in the other two cases (30% and 50%), ey remains less
quantity than 3.5%.
2. Near the crack tip, the longitudinal strain ey reaches high values
PQ  a  compared to the values far from the crack tip (x > 4 mm) where
K Q ¼ pffiffiffiffiffiffi f ð6Þ
B W W ey is stabilized around 1.5% for the 15% case and 1% for the 30%
and 50% cases.
where PQ is the load at intercept with 95% slope, B is the specimen 3. In all cases, ey is well modelled by a power law that can be writ-
thickness, W its width and a the crack length. The function f is de- ten as:
fined as follows:
pffiffiffi a
5 a ey ¼ pffiffiffi ð8Þ
f ðaÞ ¼ pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi ð7Þ x
20  13a  7a2
 2
K
If the condition 2:5 rQy  a; W  a; B is satisfied then KIc = KQ where a is a material constant.
otherwise the test is invalid. ry is the yield strength of the material. The values of the correlation coefficient R show that the model
Fracture toughness tests were carried out on GFR-PA66PA66 results are in good agreement with the experimental ones.
SENT specimens with a crosshead speed of 1 mm/min. From result- We know that the local stress state, near the crack tip, is related
ing load–displacement curves (Fig. 9), we determined the critical to the applied load and the cracked specimen geometry as estab-
values of stress intensity factor for the three composites with lished by Irwin:
15%, 30% and 50% of glass fibre content and plotted KIc as a function
K
of q=qm in Fig. 10. ry ¼ pffiffiffiffiffiffiffiffiffi ð9Þ
Displacement at break is much higher in unfilled PA66 than in 2px
the GFR-PA66 because of the loss of ductility due to fibres pres- where K is the stress intensity factor.
ence. The brittle profile of SGFR-PA66 is illustrated in Fig. 11. Eq. (9) is another way to express Irwin’s formula in terms of
The DIC technique allowed determining the longitudinal strain strain. This is well justified as the plasticity is confined and a linear
ey in 0.258 mm spaced out points in both directions. At crack initi- relationship between ry and ey can be assumed.
ation, the distribution of longitudinal strain along the crack line is Combining (8) and (9), we determined the theoretical values of
represented in Figs. 12–14. a. Table 1 shows that these values are in good agreement with the
experimental ones.

3.5

3 PA66-30% : εy = 2,9x-0,5
R2 = 0,8
2.5
εy (%)

1.5

0.5

0
0 2 4 6 8 10

x (mm)

Fig. 11. Brittle profile of SGFR-PA66 fracture. Fig. 13. Strain distribution on the crack line in the SGFR-PA66-30% case.
2526 B. Mouhmid et al. / Composites Science and Technology 69 (2009) 2521–2526

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