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Composites: Part A 38 (2007) 710–718

www.elsevier.com/locate/compositesa

Effect of reprocessing on the fatigue strength of a fibreglass


reinforced polyamide
a,*
A. Bernasconi , P. Davoli a, D. Rossin a, C. Armanni b

a
Politecnico di Milano, Dipartimento di Meccanica, Via La Masa 34, I-20156 Milan, Italy
b
Radici Plastics, Chignolo d’Isola BG, Italy

Received 8 June 2006; received in revised form 28 September 2006; accepted 30 September 2006

Abstract

The mechanical recycling of short fibre reinforced thermoplastics by granulation and subsequent injection moulding allows for recov-
ery of both post consumer waste and in-plant recycled material in many industrial sectors. Parts made of these materials are often sub-
jected to cyclic loads and therefore need to be designed against fatigue. The fatigue behaviour of reprocessed glass fibre reinforced
polyamide 6,6 has been studied, using standard injection moulded specimens containing different percentages of recycled material.
The effect of reprocessing of clean materials is mainly represented by fibre shortening in the injection moulding process and consequent
degradation of the load bearing capacity of material. The relationship between the fatigue strength and the fibre length distribution has
been discussed.
 2006 Elsevier Ltd. All rights reserved.

Keywords: A. Recycling; Short glass fibre reinforced thermoplastics; B. Fatigue; E. Injection moulding

1. Introduction it is becoming necessary to include plastic parts into the


number of items to be recovered and/or recycled, in order
The use of injection moulded fibre reinforced plastics to fulfil the requirements of minimum percentages of the
offers the opportunity of replacing metals in numerous total mass of a vehicle to be recovered/recycled at the
applications in different industrial sectors, because of their end of its life; a requirement which cannot be fulfilled by
high specific mechanical properties, the ease of production recycling the metal parts only, as it happens today.
of parts of complex shape, and the high allowable produc- Different recycling methods exist for plastics, reinforced
tion rates at relatively low cost. The increasing quantities of and unreinforced, depending on the type of resins and rein-
post consumer waste originating from the widespread use forcements. In principle, unlike thermosetting resins, which
of these materials are posing the question of correct dis- can be recycled only by incorporating them in other mate-
posal of parts at the end of their life, in order to reduce rials and therefore downgrading them to the role of fillers,
their environmental impact and particularly to reduce thermoplastic materials can be recycled in closed loop, i.e.,
waste sent to landfills. Alternatives to landfill are reuse of for the same application for which virgin material is used,
parts, recovery of energy (e.g. by incineration) and recy- provided that the effects of degradation from service and of
cling of material. Environmental regulations, like the EU the recycling process are known.
directives for the End of Life Vehicles [1] are driving forces The two recycling options for short fibre reinforced ther-
for the recycling of materials, particularly plastics. In fact, moplastics are mechanical recycling and chemical recycling
[2]. Mechanical recycling of thermoplastics materials con-
sists of granulating and re-moulding, without separating
*
Corresponding author. Tel.: +39 02 2399 8222; fax: +39 02 2399 8202. reinforcing fibres from matrix. Then the material is reused
E-mail address: andrea.bernasconi@polimi.it (A. Bernasconi). as composite. The fibre length distribution and the bonding

1359-835X/$ - see front matter  2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesa.2006.09.012
A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718 711

between the glass fibres and the polymer are affected by the the fatigue strength of SGFR polyamides is particularly
injection moulding process. Bonding can be improved by relevant for the increasing number of load bearing applica-
using coupling agents or by incorporating recycled material tions subjected to repeated loads. For this reason, and for
into virgin material, but fibre shortening constitutes an the increasing industrial interest about recycled composite
important issue for safely using recycled fibre reinforced polymeric materials, we investigated on the effect of repro-
materials. With chemical recycling the fibres and the poly- cessing (in-plant recycling) on the fatigue strength of a
mer are recovered and reused separately. Separation gener- short fibreglass reinforced polyamide.
ally consists of dissolution of the matrix and separation of
fibres. Apart from costs, this may cause safety and environ- 2. Experimental
mental concern, due to the handling and use of the large
amount of solvents required. However, condensation poly- 2.1. Materials and processing
mers such as PET and polyamide can also be de-polymer-
ised, i.e., returned back to their original constituents, by Extrusion compounded pellets of a short glass fibre rein-
hydrolysis. The polymerisation process is reverted and forced polyamide 6,6 containing 35% by weight of fibres
the material broken down to initial monomers. Fibres (PA66 GF 35) were injection moulded into tensile test spec-
can be separated and the monomers used to produce new imens using a Sandretto Serie 7 HP 95 T injection mould-
composites with addiction of new reinforcements. ing machine with maximum injection capacity of 160 cm3/s
Among the different types of polymers, we concentrated and a screw diameter of 45 mm. Injection moulding vari-
on short glass fibre reinforced (SGFR) polyamides, which ables are reported in Table 1.
are widely employed by the automotive industry, for parts The in-plant recycling of the virgin material consisted of
located in the engine compartment and also for load bear- grinding of tensile test specimens in a Dipre GRS 182 A7
ing applications, like the clutch pedal of several car models. granulator of 2.2 kW power at 300 rpm, equipped with 7
Fibreglass reinforced polyamides can be easily recycled by rotary blades and 1 stationary blade of 75 mm length
granulation and remoulding. This process is also of par- mounted on a 180 mm diameter rotor, and subsequent
ticular interest for users of virgin materials, because the injection moulding of specimens containing a blend of vir-
so-called in-plant recycling of off-specification parts and gin and recycled material. A total of four batches of spec-
production scraps is commonly performed. In this context, imens were manufactured, with a content of 0%, 25%, 50%
the mechanical behaviour of reprocessed fibreglass rein- and 100% of reprocessed material. The corresponding val-
forced polyamides has been studied by Eriksson et al. [3], ues of the regrind level, defined as the ratio of the mass of
by submitting injection moulded specimens containing dif- the reprocessed material and the total mass of the speci-
ferent percentages of in-plant recycled material to tensile men, i.e.,
and impact tests. The results of these experiments showed M recyclate M virgin
that the degradation of the composite is mainly related to RL ¼ ¼1 ð1Þ
M tot M tot
the fibre shortening occurring during successive injections,
whereas reprocessing has little if any effect on the proper- ranged from 0 (virgin material) to 1 (material containing
ties of the matrix and of the fibre–matrix interface. 100% of reprocessed material).
On the other hand, unlike in-plant recycled materials,
the mechanical properties of recycled materials originating 2.2. Mechanical testing
from post consumer waste are influenced by factors affect-
ing the matrix properties and the fibre–matrix interface, Mechanical testing consisted of tensile and fatigue tests.
like the presence of impurities and the effects of service, Tensile properties were measured in accordance with the
which implies ageing (thermal oxidation) and fluid contam- procedure in ISO 527-1 standard [11] at crosshead speed
ination. An experimental investigation on these effects on a of 5 mm/min on an MTS Alliance RF 150 machine. Strains
fibreglass reinforced polyamide (both virgin and repro- were measured with a MTS 634.25 extensometer of 50 mm
cessed) has been performed by Eriksson et al. [4], by testing base length. Specimens for both tensile and fatigue tests
samples containing glass beads in order to simulate the had size and dimensions of type 1A tensile test bars,
presence of impurities, and by submitting specimens of according to ISO 527-2 standard for tensile tests [12].
the same material to tensile and creep tests after controlled
thermal and coolant ageing [5–7]. The experimental values Table 1
Injection moulding variables
of the tensile and impact tests of in-plant recycled SGFR
polyamides were predicted by Eriksson et al. [8] on the Mould temperature 70 C
Barrel temperature 270–275 C
basis of the fibre length distributions, by applying a method
Melt temperature 280 C
originally proposed by Bowyer and Bader [9], using a mod- Injection time 3.5 s
ification of the Kelly–Tyson model [10]. Cooling time 6s
These studies concentrated on tensile strength, impact Total cycle time 18 s
resistance and creep of reprocessed SGFR polyamides, Back pressure 5 bar
Hold pressure 60 bar
whereas no fatigue test results were reported. Actually,
712 A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718

Fatigue tests were run by applying sinusoidal tensile


loads of constant amplitude, in load control mode, on an
Instron 8501 servo-hydraulic testing machine, equipped
with an actuator of 150 kN capacity and with an additional
load cell of 10 kN, as required to increase the accuracy of
load measurement. Stresses were calculated by dividing
the applied force by the nominal area of the specimen cross
section. Fatigue tests consisted of tension to tension load
cycles, in order to prevent specimens from buckling under
compressive loading. The load ratio, i.e., the ratio between
the minimum and the maximum applied load, R = Fmin/
Fmax was equal to 0.1 for all tests.
In fatigue testing of reinforced thermoplastics, speci-
mens are prone to self heating and cyclic creep. Conse-
quently, load cycles were applied with a cyclic frequency
of 2 Hz, in order to reduce the temperature increase of
the specimen due to the self heating [13]. To measure the
cyclic creep, specimen strain were measured with an Fig. 1. Optical microscope image of the fibres extracted from one sample
Instron 26020-601 extensometer of 50 mm base length. of PA66 GF 35.
Maximum and minimum strain values were recorded for
each load cycle, whereas full stress–strain cycles were About 1000 fibres for each material sample were exam-
recorded at fixed time intervals. Tests were interrupted at ined and their measures were statistically analyzed. Fibres
specimen failure (separation). Load levels were selected in shorter than 0.025 mm not were counted. A fibre length
order to make the number of cycles to failure fall within distribution (FLD) like that reported in Fig. 2 was
the range 103–106. obtained for each material. The FLDs can be described
All mechanical property testing was performed at 23 C by a Weibull probability distribution function. To describe
and at relative humidity of 50%. Specimens were tested FLDs, the number–average and the weight average are
‘‘dry as moulded’’ (DAM). Tensile and fatigue tests were commonly used. The number–average fibre length, which
also performed on the virgin material in conditioned state. is useful for examining the level of fibre damage during
Conditioning consisted of submerging specimens in dis- processing, is expressed by
tilled water for seven days at room temperature and then
PN
allowing them to reach equilibrium with ambient moisture n i li
at 23 C and 50% relative humidity. This stabilisation pro- Ln ¼ Pi¼1N ; ð2Þ
i¼1 ni
cess lasted several weeks and the equilibrium condition was
identified by monitoring the specimen weight. The water
whereas the weight–average fibre length, which reflects the
content at the end of the conditioning process was 1.3%
volume fraction at that length, and is therefore more useful
by weight.

2.3. Analysis of reinforcing fibres

The effect of reprocessing on the fibre length distribution


was studied by measuring the length of fibres extracted
from samples of the four materials. Fibre samples were
obtained from specimens by hot hydrolysis of the matrix,
using a 1:1 aqueous solution of Hydrochloric Acid at
36%w. The fibres were then separated by filtration, washed
and dried using an air circulating oven. Finally, the fibres
were dispersed on a glass microscope slide and photo-
graphed using a Leitz Aristomet optical microscope,
equipped with a Nikon DXM 1200 digital camera con-
nected to a PC. Greyscale micrographs of 1280 · 1024 pixel
size were obtained, see Fig. 1. These micrographs were then
processed using an image analysis software we developed,
based on the Matlab Image Analysis package. Each image
contained several fibres and the reference bar visible in
each picture was used to calibrate the digital analysis sys- Fig. 2. Fibre length distribution of a sample of virgin PA66 GF 35, with
tem. Then each fibre was manually selected and measured. values of Ln and Lw.
A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718 713

in describing the composite mechanical properties which


are mainly related to volume fraction, is expressed by
(assuming fibres of equal diameter)
PN
ni l2i
Lw ¼ Pi¼1
N : ð3Þ
i¼1 ni li

In order to measure such a large number of fibres, several


images need to be examined. As it is clearly visible in Fig. 1,
some fibres intersect the edges of the pictures. These fibres
cannot be counted because the parts of the fibres outside
the pictures cannot be seen. Consequently the real fibre
length distribution is not captured. The longer is the fibre,
the higher the probability for it to intersect the picture
edges and therefore to be discarded. Consequently both
number–average and weight average are underestimated.
For this reason, a correction of the FLD by taking into ac- Fig. 3. Weibull density functions of the five PA66 GF 35 samples.
count of fibres intersecting the image boundaries was ap-
plied, following the procedure described in Ref. [14]. The 3.2. Tensile tests
corresponding values of Ln and Lw are indicated as Ln,adj
and Lw,adj, respectively. Results of the tensile tests are reported in Table 3. The
reported figures are the mean value over five samples;
standard deviations are reported between parentheses.
3. Results
The elastic modulus and the stress at break decreased
as the content of reprocessed material increased, whereas
3.1. Fibre length
the strain at break increased for higher percentages of
reprocessed material.
Values of the number–average and weight–average fibre
length of all the PA66 GF 35 samples, including pellets of
3.3. Fatigue tests
virgin material and granules of ground virgin material ana-
lyzed prior to being used to feed the injection moulding
The results of the fatigue tests for the specimens contain-
machine, are reported in Table 2. Both the values obtained
ing different percentage of reground material are reported
with and without the above mentioned correction are
in Fig. 4, where the log(maximum applied fatigue stress),
reported for comparison purpose. The average values
or log rmax, is plotted vs. log (cycles to failure) or log Nf.
decreased considerably during the first injection moulding
The corresponding S–N curves, also known as Wöhler
and the subsequent injection had a further fibre shortening
curves, are superimposed to experimental results. These
effect, whereas the sole grinding process left average fibre
curves interpolate linearly the test results; they appear to
length values almost unaltered.
be nearly parallel to each other, with decreasing fatigue
The corresponding Weibull probability distribution
strength with increasing content of reprocessed material.
functions are drawn in Fig. 3. From the shape of the
Based on the above mentioned experimental results, the
curves, it is clearly visible the fibre shortening taking place
following equation was used to describe the relationship
after each injection moulding (pellet vs. virgin material and
between maximum stress and cycles to failure:
virgin material vs. 100% reprocessed). The blends of virgin
and reprocessed material displayed intermediate fibre rmax ¼ rf N b : ð4Þ
length distributions.
The values of fatigue strength exponent b and fatigue
strength coefficient rf for different contents of reprocessed
material are listed in Table 4.
Table 2
Values of the number–average and weight–average fibre length of the Values of rf decreased with increasing content of recy-
PA66 GF 35 samples cled material and the fatigue strength exponent b showed
Material Ln (lm) Ln,adj (lm) Lw (lm) Lw,adj (lm) almost constant values, i.e., the S–N curves had the same
slope. Values of the maximum stress at 105 and 106 cycles
Pellet 338 388 461 539
Virgin 278 324 356 406 to failure, as obtained by applying Eq. (4), are reported
Virgin after grinding 275 321 343 387 as rw (N = 105) and rw (N = 106), respectively. The reduc-
25% reground 252 274 338 367 tion of the fatigue strength coefficient is of 11% when com-
50% reground 228 261 300 335 paring the virgin material with the 100% reprocessed one.
100% reground 213 225 274 288
It is worth noting that for the same applied maximum
714 A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718

Table 3
Results of the tensile tests for the different blends of virgin and reprocessed PA66 GF 35
Material Elastic modulus (GPa) Tensile strength (MPa) Stress at break (MPa) Strain at break (%)
Virgin 10.84 (±0.14) 187.9 (±2.4) 187.4 (±2.7) 2.87 (±0.13)
25% reground 10.75 (±0.13) 185.9 (±0.5) 185.3 (±0.6) 2.85 (±0.06)
50% reground 10.73 (±0.09) 181.6 (±0.7) 180.5 (±1.2) 3.00 (±0.06)
100% reground 10.27 (±0.12) 167.3 (±1.6) 165.5 (±1.4) 3.04 (±0.09)

Fig. 5. Elastic modulus and ultimate tensile strength of the PA66 GF 35 as


Fig. 4. S–N curves of the PA66 GF 35 samples containing different a function of the weight average fibre length.
percentages of reground material.

Table 4
Values of the fatigue strength coefficient and exponent of the PA66 GF 35 samples containing different percentages of reground material
Material rf (MPa) b [–] rw (N = 105) (MPa) rw (N = 106) (MPa)
Virgin 240.5 0.0666 111.7 95.8
25% reground 242.7 0.0686 110.2 94.1
50% reground 219.4 0.0623 107.1 92.8
100% reground 213.6 0.0683 97.3 83.1

stress, in spite of the small differences between the values of mechanical parameters with FLD and provides the follow-
the fatigue strength coefficient, there is a factor of 10 ing expression for the tensile strength of a SGFR
between the numbers of cycles to failure of virgin material composite
and that of the 100% reprocessed composite. (  )
lX lj ¼1
i ¼Lc
sli vi X Lc
rM ¼ g 0 þ ruf vj 1 
li ¼0
d lj ¼Lc
2lj
4. Discussion
þ ð1  vf Þr0m ; ð5Þ
4.1. Relationship between FLD and composite strength
where d is the fibre diameter, s the interfacial shear
Elastic modulus and ultimate tensile strength are plotted strength, li the length of fibres whose volume fraction is
in Fig. 5 vs. the weight average fibre length, together with vi, ruf is the tensile stress of fibres, r0m is the stress carried
the corresponding values of the regrind level (values of by the matrix at the fibre failure strain, Lc is the fibre crit-
Lw,adj are decreasing for increasing RL). Thus, it seems rea- ical length and g0 is an orientation factor. Subscripts i and j
sonable that fibre shortening is responsible for the varia- refers to fibres of sub-critical and super-critical length,
tion of the tensile properties, in agreement with the respectively. The expression for the critical length is
results presented in the cited references. Lc = rufd/2s.
Further understanding of the relationship between FLD The micromechanical parameters ruf, s and g0 can be
and composites strength can be provided by micromechan- identified by applying an iterative method proposed by
ical models, like the Bowyer–Bader model, based on a Thomason [15–17] for materials with non-linear stress
modified Kelly–Tyson model, which combines some micro- strain relationships. The method consists of extending the
A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718 715

validity of Eq. (5) to describe the full stress–strain curve of the additional thermal cycles corresponding to subsequent
a composite prior to failure, obtaining the relationship injection mouldings.
( lj ¼1  ) Even with these limitations, the model allows predicting
lX
i ¼Le
sli vi X E f ec d with high accuracy the reduction of strength for a 100%
rc ¼ g0 þ E f e c vj 1 
li ¼0
d lj ¼Le
4slj content of reprocessed material, whereas the reduction
observed in samples containing 25% and 50% of reground
þ ð1  vf Þrm ; ð6Þ specimens is lower than predicted values. Thus the sensitiv-
where rm is the stress carried by the matrix at the ity of the model to small variations of the FLD seems to be
composite strain ec, and the critical length is replaced by higher than that of the material itself. Moreover, predic-
Le = ecEfd/2s. Thus, values of s and g0 can be determined tions could be improved if models for the variation of the
by making prediction provided by Eq. (6) coincide with micro-mechanical parameters with reprocessing were avail-
experimental stresses recorded in tensile tests for a mini- able. However, predictions are on the conservative side.
mum of two strain level; finally, the value of ruf is obtained By observing the dependence of the fatigue strength at
by equalling the composite tensile strength to the predic- 106 cycles to failure upon the average fibre length, as shown
tion obtained by applying Eq. (5). in Fig. 6, one may suppose that a similar relationship
A comparison between experimental and predicted val- between FLD and fatigue strength exists as well. This is
ues of the ultimate tensile strength of the four blends of further confirmed by the normalised S–N curves of
PA66 GF 35 is reported in Table 5. Composite strength Fig. 7, obtained by dividing maximum stress values by
values were predicted by applying the method proposed the tensile strength of the material sample under examina-
by Thomason, with s = 45 MPa, g0 = 0.67, Lc = 200 lm. tion. All the experimental data fall within the 10–90% pre-
The value of these parameters were determined with tests diction band of the S–N master curve. This signifies that
on the virgin material and subsequently employed to pre- the fatigue strength is proportional to the tensile strength.
dict the strength of the samples containing reground mate- This is a general relationship valid for most of the short
rial, applying Eq. (5) to their respective FLDs. Values of fibre reinforced thermoplastics, provided that fatigue tests
rm were obtained from tensile tests on samples of unrein- are always run using the same specimen geometry, at the
forced PA66 matrix. same frequency and tensile tests are conducted at the same
The values of s, Lc and g0 parameters were kept con- strain rate.
stants for all materials in order to test the ability of the It can then be concluded that, for the particular case of
model to predict the tensile strength values of material materials having the same composition but different FLD,
samples containing reprocessed material on the basis of the modified Kelly–Tyson model is applicable to the pre-
their FLDs and the properties of the virgin material. Actu- diction of the fatigue strength as well, provided that the
ally, a variation of these parameters with the content of values of the fatigue strength coefficient and the exponent
reprocessed material may be expected. In fact, the g0 are known for the virgin material. In fact, on the basis of
parameter is related to the fibre orientation distribution, the FLD of the reprocessed material, which can be easily
which is affected, among other factors related to the injec- obtained with relatively simple analysis tools, and the
tion moulding process, by the fibre properties, particularly micromechanical parameters derived from tensile tests on
the FLD. The variation of g0 for a reprocessed 30% fibre- the virgin material, the ultimate tensile properties of the
glass reinforced polyamide 6,6 was supposed to be negligi- reprocessed material can be predicted. Then, these data
ble by Eriksson et al. [3], who supported this assumption by
comparing the variation of stiffness as a function of the
angle to the flow direction of injection moulded specimens
of virgin and reprocessed material. However, no direct
measurement of the fibre orientation distribution was
available for the specimens used in this work. Moreover,
reprocessing is likely to modify the interfacial shear
strength, and consequently the critical length, because of

Table 5
Values of the tensile strength of the PA66 GF 35 samples containing
different percentages of reground material as predicted by the modified
Kelly–Tyson model, compared to experimental data
Material rM Bowyer–Bader rM Experimental Error
(MPa) (MPa) (%)
Virgin 188 188 –
25% reground 175 186 5.9
50% reground 169 182 7.1
Fig. 6. Fatigue strength at 106 cycles to failure of the PA66 GF 35 as a
100% reground 165 167 1.2
function of the weight average fibre length.
716 A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718

conditioned material, with water content in equilibrium


with an ambient at 23 C and 50% r.h. (1.3% by weight).
Water absorption has a plasticizing effect on the poly-
amide matrix, which consists of a significant reduction of
strength and stiffness, whereas the elongation at break is
almost doubled. The effect on fatigue strength is shown
in Fig. 8, where the S–N curves of the DAM and the con-
ditioned material are plotted on the same graph. The pres-
ence of water in the matrix and at the fibre–matrix interface
modifies both the position and the slope of the S–N curve,
and the fatigue strength is drastically reduced.
The plasticizing effect is related to the influence of water
absorption on the glass transition temperature (Tg) of
polyamides, which is lowered below 23 C for water
content reaching equilibrium with our test environment
[19,20]. Consequently the enhancement of ductility is simi-
Fig. 7. Normalised S–N curves of PA66 GF 35 samples containing lar to that obtainable by raising the environment tempera-
different percentages of reground material. ture over the glass transition temperature of the dry
material. Also the difference in position and slopes of S–
can be used to derive the S–N curve of the reprocessed N curves can be explained in terms of water absorption.
material by means of the master curve of Fig. 7. It has been shown that a change in the slope of S–N curves
occurs when the test temperature is raised over the Tg, i.e.,
curves at T > Tg are lower and relatively flatter than those
4.2. Effects of water absorption
at T < Tg [13]. Similarly, when water absorption lowers the
Tg below the test temperature, the same effect is observed,
All the experimental results presented in this article refer
as in the case of our tests.
to material samples kept in the DAM state until the begin-
The effect of water absorption on the fatigue mechanism
ning of each test. The temperature of the laboratory was
has been thoroughly described by Horst and Spoormaker
23 C, with a relative humidity of 50%. In these conditions,
[21,22]. The fatigue damage is characterized by gradual
the polyamide matrix tends to absorb moisture by a diffu-
degradation of the bonding between fibres and matrix,
sion process from the surface to the core. For given sample
starting at fibre ends and propagating along the fibres.
geometry, ambient moisture and temperature, the amount
These voids grow and coalesce, thus forming cracks, which
of water uptake depends on exposure time. Fatigue testing
start propagating. In conditioned polyamide, due to the
was performed at low cyclic frequencies, therefore it may
higher ductility of the matrix because of water absorption,
allow for long exposure times, particularly in the case of
this process is accelerated. The increase of ductility is visi-
lower stress levels, corresponding to high number of cycles
ble on fracture surfaces, which are characterized by numer-
to failure. The water uptake of specimens during fatigue
ous filaments of highly drawn matrix (crack faces remain
testing was not measured. However, the test conditions
were the same for all material samples, thus allowing for
comparison of the S–N curves.
In order to reach the hygrothermal equilibrium state of
the matrix with an ambient at 23 C and 50% r.h., exposure
times considerably longer than those corresponding to long
fatigue tests are required [18]. Moreover, the modifications
of the bulk properties of the specimens, like tensile and fati-
gue behaviour, are considerably more significant when the
material has reached a stable equilibrium with ambient
moisture. These modifications are shown in Table 6, where
tensile properties of two samples of virgin PA66 GF 35 are
reported; the first refers to the DAM state, the second to a

Table 6
Comparison of the tensile properties of virgin PA66 GF 35 DAM and
conditioned
Material E (GPa) rM (MPa) eb (%)
DAM 10.84 (±0.14) 187.9 (±2.4) 2.87 (±0.13)
Fig. 8. Comparison of the S–N curves of PA66 GF 35 in the DAM and
Conditioned 7.71 (±0.11) 125.8 (±0.1) 5.11 (±0.32)
conditioned state.
A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718 717

bridged by highly deformed matrix filaments until final Tests were run with specimens in the dry as moulded
fracture occurs), whereas the same material in the DAM state. The effect of water content has also been investigated
state shows a more brittle behaviour at the microscale. on the virgin material only, in order to provide a quantita-
The effects of moisture absorption are also important for tive assessment of the modifications of the S–N curves tak-
the design against fatigue of real parts, which are prone to ing place when the material is conditioned, i.e., has been
water absorption. Therefore, care must be exercised when allowed to absorb water. Ductility of the matrix is
using the master S–N curve of Fig. 7, obtained with DAM enhanced by the presence of water and therefore mechani-
specimens, to design parts against fatigue, in order not to cal properties are modified. Stiffness, tensile strength and
neglect the reduction of strength and the change in slope. fatigue strength are considerably lower than those of the
In facts, the fatigue assessment of parts containing repro- DAM material, whereas the elongation at break is higher.
cessed material should be performed on the basis of material Furthermore, the slope of S–N curves is decreased. Never-
data referring to the conditioned state, or if not available, theless, the design of real parts, usually prone to water
fatigue master curves should be modified with reference to absorption, is still possible by taking into account these
the S–N curve of the virgin material in the conditioned state. effects in the use of the S–N master curve.
The presence of water in the matrix does not signifi-
cantly affect the possibility of reprocessing the material,
Acknowledgements
since ground material is usually exsiccated prior to being
fed into the injection machine. However other factors orig-
The authors gratefully acknowledge financial support
inating from service conditions may contribute to the deg-
provided by the Italian Ministry for University and Tech-
radation of the composite and make reprocessing of
nological and Scientific Research (MIUR) under Grant
materials from post consumer waste difficult, namely con-
No. 2003094300 004 (PRIN 2003). They also wish to thank
taminations from solid impurities and service fluids and
Mr. Allevi, Mr. Troiani and Mr. Gornati for help in con-
thermal ageing. Difficulties may arise when trying to deter-
ducting the experiments.
mine the effect of real service conditions by testing materi-
als recovered from post consumer waste, if the history of
the part to be recovered is not known. References

5. Conclusions [1] Directive 2000/53/EC of the European Parliament and of the Council
of 18 September 2000 on End-of-Life Vehicles. Council of the
European Parliament. 2000.
We have studied the effect of reprocessing on the fatigue [2] Arnold JC. Reprocessing. In: Ballie C, editor. Green composites.
behaviour of a short glass fibre reinforced polyamide 6,6 Polymer composites and the environment. Cambridge: CRC Press,
with 35% by weight of fibreglass. Reprocessing consisted Woodhead Publishing Ltd; 2004.
of in-plant recycling, i.e., granulation of injection moulded [3] Eriksson PA, Albertsson AC, Boydell P, Eriksson K, Månson JAE.
Reprocessing of fiberglass reinforced polyamide 66: influence on
parts (in this case the tensile test bars) and use of the
short term properties. Polym Compos 1996;17(6):823–9.
ground material to feed the injection moulding machine. [4] Eriksson PA, Albertsson AC, Boydell P, Månson JAE. Influence of
Different blends of virgin and reground material have been impurities on mechanical properties of recycled glass fiber reinforced
studied, with a content of reprocessed material of 25%, polyamide 66. Polym Eng Sci 1998;38(5):749–56.
50% and 100%, as well as the virgin material. [5] Eriksson PA, Boydell P, Eriksson K, Månson JAE, Albertsson AC.
Tensile tests confirmed the role of fibre length distribu- Effect of thermal-oxidative ageing on mechanical, chemical, and
thermal properties of recycled polyamide 66. J Appl Polym Sci 1997;
tion on the mechanical properties of reprocessed material. 65:1619–30.
Fibre length distributions of samples of the materials tested [6] Eriksson PA, Boydell P, Månson JAE, Albertsson AC. Durability
were obtained by digital analysis of optical microscope study of recycled glass-fiber-reinforced polyamide 66 in a service
images of fibres extracted from specimens. The fibre short- related environment. J Appl Polym Sci 1997;65:1631–41.
[7] Eriksson PA, Albertsson AC, Boydell P, Månson JAE. Durability of
ening due to the injection moulding process has been con-
in-plant recycled glass fiber reinforced polyamide 66. Polym Eng Sci
firmed as responsible of the decrease of stiffness and 1998;38(2):348–56.
strength and a modified Kelly–Tyson model allowed pre- [8] Eriksson PA, Albertsson AC, Boydell P, Prautzsch G, Månson JAE.
dicting this effect. Prediction of mechanical properties of recycled fiberglass reinforced
Fatigue tests were conducted on the four materials and polyamide 66. Polym Compos 1996;17(6):830–9.
S–N curves were derived, for specimen lives comprised in [9] Bowyer WH, Bader MG. On the re-inforcement of thermoplastics by
imperfectly aligned discontinuous fibres. J Mater Sci 1972;7:
the range 103–106 cycles to failure. Results showed that 1315–1321.
fatigue strength was reduced by the presence of the [10] Kelly A, Tyson WR. Tensile properties of fibre-reinforced metals:
reground material by the same amount as tensile strength. copper/tungsten and copper/molybdenum. J Mech Phys Solids 1965;
This allowed deriving a master S–N curve for PA66 GF 35 13:329–50.
[11] ISO 527-1. Plastics – determination of tensile properties – Part 1:
containing reprocessed material. The effect of reprocessing
General principles. International Organization For Standards 1993.
on the fatigue strength can be easily predicted on the basis [12] ISO 527-2. Plastics – determination of tensile properties – Part 2: Test
of fibre length distributions, which can be obtained with conditions for moulding and extrusion plastics. International Orga-
relatively simple analysis tools, and the S–N master curve. nization For Standards 1993.
718 A. Bernasconi et al. / Composites: Part A 38 (2007) 710–718

[13] Handa K, Kato A, Narisawa I. Fatigue characteristics of a glass- [18] Jia N, Fraenkel HA, Kagan VA. Effects of moisture conditioning
fiber-reinforced polyamide. J Appl Polym Sci 1999;72:1783–93. methods on mechanical properties of injection molded nylon 6. J
[14] Fu S-Y, Mai Y-W, Ching EC-Y, Li RKY. Correction of the Reinf Plast Compos 2004;23:729–37.
measurement of fiber length of short fiber reinforced thermoplastics. [19] Batzer H, Kreibich UT. Influence of water content on thermal
Composites: Part A 2002;33:1549–55. transitions in natural polymers and synthetic polyamides. Polym Bull
[15] Thomason JL. The influence of properties of the performance of 1981;5:585–90.
glass-fibre-reinforced polyamide 6,6. Compos Sci Technol 1999;59: [20] Ishisaka A, Kawagoe M. Examination of the time–water content
2315–28. superposition on the dynamic viscoelasticity of moistened polyamide
[16] Thomason JL. Micromechanical parameters from macromechanical 6 and epoxy. J Appl Polym Sci 2004;93:560–7.
measurements on glass reinforced polyamide 6,6. Compos Sci [21] Horst JJ, Spoormaker JL. Fatigue fracture mechanism and fractog-
Technol 2001;61:2007–16. raphy of short-glassfibre-reinforced polyamide 6. J Mater Sci
[17] Thomason JL. Interfacial strength in thermoplastic composites – at 1997;32:3641–51.
last an industry friendly measurement method? Composites: Part A [22] Horst JJ, Spoormaker JL. Mechanism of fatigue in short glass fiber
2002;33:1283–8. reinforced polyamide 6. Polym Eng Sci 1996;36:2718–26.

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