Composite Structures 118 (2014) 1–8

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Composite Structures
journal homepage: www.elsevier.com/locate/compstruct

Effect of different commercial oils on mechanical properties

of composite materials
A.M. Amaro a,⇑, P.N.B. Reis b, M.A. Neto a, C. Louro a
a
CEMUC, Depart. Mechanical Engineering, University of Coimbra, Rua Luís Reis Santos, Pinhal Marrocos, 3030-788 Coimbra, Portugal
b
Depart. Electromechanical Engineering, University of Beira Interior, Covilhã, Portugal

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

Article history: Composite materials are used in several engineering applications, where can be exposed to a range of
Available online 18 July 2014 corrosive environments during their in-service life. Thus, it is necessary understanding the impact of a
corrosive environment in the working life of composite. According the authors’ knowledge, the effect
Keywords: of different commercial oils was not yet studied. Therefore, glass fibre/epoxy composites were subjected
Environmental degradation to oil immersion tests, using an universal multi-grade engine oil (15W-40) and an extra high performance
Mechanical properties hydraulic brake fluid (DOT 4), in order to study the effects of oil absorption behaviour on flexural and
Mechanical testing
impact strength properties of glass fibre/epoxy composites. Both solutions affect the flexural properties
Polymer–matrix composites (PMCs)
and the impact strength. However, for all tests performed, the automotive brake fluid promotes the low-
est values comparatively to the automotive engine oil.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction The effect of moisture on the mechanical properties of fibre-

Nowadays, composite materials are used in several engineering
applications, as a consequence of their high specific strength and
stiffness, competitive cost, good static and dynamic properties,
good resistance to corrosion and simplified fabrication. In this con-
text, these materials are exposed at different environment condi-
tions, which affect significantly their mechanical properties.
In terms of moisture, irreversible material degradation occurs
and some chemical changes can be found (relaxation and oxidation
of the matrix material), fibre/matrix debonding and continuous
cracks [1,2]. When the water penetrates into the matrix, by diffu-
sion or by the interface fibre/resin of a composite, it acts as a plas-
ticizer and decreases significantly the glass-transition temperature
[3]. This phenomenon makes composites softer, since the matrix
becomes pliable due to the presence of the plasticizer [3]. How-
ever, the rate at which water is absorbed depends on many factors,
including the properties of fibres and matrix, temperature, differ-
ences of water concentration within the composite and the envi-
ronment [4]. On the other hand, as diffusion is a thermally
activated process, growing temperature accelerates the short-term
diffusion and increases the diffusion coefficient [3,5].
⇑ Corresponding author.
E-mail addresses: ana.amaro@dem.uc.pt (A.M. Amaro), preis@ubi.pt (P.N.B. Reis),
augusta.neto@dem.uc.pt (M.A. Neto), cristina.louro@dem.uc.pt (C. Louro).
reinforced polymer composites was investigated by Selzer and
Friedrich [6]. These authors, did experimental tests, including ten-
sile, compression, fatigue and compression after-impact, for evalu-
ating the effect of moisture on the mechanical properties of two
thermosetting matrices (unmodified and toughness-modified
epoxy) and of one thermoplastic matrix (polyetheretherketone).
The results showed that the absorbed moisture decreases the
mechanical properties of both epoxy resin-based composites, being
this decrease mainly controlled by the matrix or interface, and that
the influence of water on the properties of the thermoplastic mate-
rial was not detectable. The influence of moisture in the thermal
and mechanical properties of Kevlar-49/epoxy-resin laminates
was studied by Akay et al. [7]. They found that, for every 1% of
absorbed moisture, the mechanical properties of compression,
interlaminar shear and flexural strengths have reductions of
around 5%, 4% and 2%, respectively. A Similar tendency was also
observed by Reis et al. [8], on Kevlar/epoxy composites, in which
significant decreases of static and fatigue strengths were reported.
However, when the water is combined with the temperature, it is
possible to observe that all properties referred above decreases sig-
nificantly [3,9–11].
Some studies about the effect of alkaline and acid solutions on
composite materials can also be found in the literature. According
Banna et al. [12] the final mechanical properties of composite
materials subjected to aggressive solutions is determined by the
type of resin used. They also showed that in expositions to higher

http://dx.doi.org/10.1016/j.compstruct.2014.07.017
0263-8223/Ó 2014 Elsevier Ltd. All rights reserved.
2 A.M. Amaro et al. / Composite Structures 118 (2014) 1–8
temperature solutions or to higher exposure duration, the polyes-
ter resin has lower modulus values than the bisphenol A epoxy
vinyl ester resin. However, in both resins, the average hardness
increases after 2 weeks of exposition and, then, decreases after
4 weeks exposure (but still higher than the unexposed). Finally,
they have concluded that under acid and higher temperature expo-
sures, the microstructure of polyester material degrades more rap-
idly than the microstructure of bisphenol A epoxy vinyl ester resin,
which can be justified by the increased surface roughness, cracks
and diffusion of sulphur into the cracks. Amaro et al. [13,14] com-
pared the effects of alkaline and acid solutions on glass/epoxy com-
posites. Authors showed that the alkaline solution is more
aggressive than the acid solution, promoting the lowest flexural
properties. In terms of acid solutions, for example, the hydrochloric
acid is responsible by the worst results [14]. The ultramicroinden-
tation showed a decreasing of the matrix mechanical properties
and the roughness was higher for the samples immersed in alka-
line solutions [13,14].
In fact, the acid and alkaline solutions significantly affect the
mechanical properties, but their effects are strongly dependent of
the exposure time [13–16], concentration [16–18] and tempera-
ture of the solution [15,17]. Relatively to the exposure time, Mah-
moud and Tantawi [15] found a significant influence of this
parameter on the flexural strength, hardness and Charpy impact
resistance. For Stamenovic et al. [16], the changes observed on
the tensile properties are proportional to the exposure time (num-
ber of days in solution). Moreover, these authors found that ulti-
mate tensile strength and modulus show significant decreases
with increasing the pH value. According Mortas et al. [17], the cor-
rosive environment decreases the impact strength and its effect is
highly dependent of the concentrations of solution. Finally, inde-
pendently of the nature of aggressive solutions and of their con-
centration, the fact is that if composites are exposed to acid
solutions at higher temperatures, the exposure induces a decreas-
ing of the mechanical properties [15,17].
In the literature there are several works about the effect of
moisture, hygrothermal and aggressive solutions (alkaline and acid
solutions) on the mechanical properties of composite materials.
But, according the authors’ knowledge was not yet performed
any study about the effect of different commercial oils in the
mechanical properties of composite materials. Thus, the aim of this
work is to increase the knowledge of those materials’ degradation
under the exposure of two different oil solutions: 15W-40 (an uni-
versal multi-grade engine oil) and DOT 4 (an extra high perfor-
mance hydraulic brake fluid). In this paper, the understanding of
degradation is evaluated in terms of flexural and impact strength
mechanical properties. The bending tests were selected because,
according Banna et al. [12], are the most sensitive to changes of
exposure conditions and, on the other hand, impacts at low veloc-
ity are very dangerous, because they affect dramatically the
mechanical performance of such materials [19–23] and, at same
time, the damages promoted are difficult to detect visually [24,25].
2. Material and experimental procedure
Composite laminates were prepared in the laboratory from
glass fibre Prepreg TEXIPREGÒET443 (EE190 ET443 Glass Fabric
PREPREG from SEAL, Legnano, Italy) and processed in agreement
with the manufacturer recommendations, using the autoclave/vac-
uum-bag moulding process. The laminates were manufactured
with the stacking sequence [02,902]2s. The processing setup con-
sisted of several steps: make the hermetic bag and apply
0.05 MPa vacuum; heat up to 125° C at a 3–5 °C/min rate; apply
a pressure of 0.5 MPa when a temperature of 120–125 °C is
reached; maintaining pressure and temperature for 60 min; cool
down to room temperature maintaining pressure and finally get
the part out from the mould. The plates were manufactured in a
useful size of 300  300  2.1 mm3.
The specimens used in the experiments were cut from these
thin plates, using a diamond saw and a moving speed chosen to
reduce the heat in the specimen. The static three point bending
(3 PB) tests were performed using specimens cut nominally to
100  14  2.1 mm3. Relatively to the impact tests, the samples
used were cut from those thin plates to square specimens with
100 mm side and 2.1 mm thickness (100  100  2.1 mm3).
Finally, the specimens were completely submerged into two types
of oils, 15W-40 (an universal multi-grade engine oil) and DOT 4 (an
extra high performance hydraulic brake fluid). The exposure time
was 15 and 45 days at room temperature. An important remark
is the fact that both faces of the samples were exposed to the oil
solution, what it is not very typical in real conditions. Afterwards,
they were cleaned with tissue paper.
The bending tests were performed according to ASTM D790-2,
using a Shimadzu AG-10 universal testing machine equipped with
a 5 kN load cell and TRAPEZIUM software at a displacement rate of
5 mm/min. All 3PB tests were also carried out at room tempera-
ture, with a span of 34 mm and, for each condition, 5 specimens
were used. Bending strength was calculated as the nominal stress
at middle span section obtained using maximum value of the load.
The nominal bending stress was calculated using Eq. (1):
3PL
r¼ 2
ð1Þ
2bh
where P is the load, L is the span length, b is the width and h is the
thickness of the specimen. The stiffness modulus was calculated by
the linear elastic bending beams theory relationship (Eq. (2)):
DP  L3
E¼ ð2Þ
48Du  I
where I is the moment of inertia of the cross-section and DP, Du are,
respectively, the load range and the flexural displacement range at
middle span for an interval in the linear region of the load versus
displacement plot. The stiffness modulus was obtained by linear
regression of the load–displacement curves considering the interval
in the linear segment with a correlation factor greater than 95%.
The low velocity impact tests were made using a drop weight-
testing machine Instron-Ceast 9340. A hemispherical impactor
with diameter of 10 mm and mass of 3.4 kg was used. The tests
were performed on circular section samples of 70 mm of diameter
and the impactor stroke at the centre of the samples. The samples
were centrally supported by a specimen of 100  100 mm dimen-
sions. The impact energy used for all impacts was 4 J, which corre-
sponds to an impact velocity of 1.53 ms1. For each condition, five
specimens were tested at room temperature. After impact tests, all
the specimens were inspected in order to evaluate the size and
shape of the delaminations. As the glass-laminated plates are
translucent, it is possible to obtain the image of the damage using
photography. Nevertheless, in order to achieve the best possible
definition of the damaged area, the plates were photographed in
counter-light using a powerful light source. Plates were framed
in a window so that all the light could fall upon them.
Based on BS EN ISO 62:1999 standard, the following procedure
was used to obtain the oil absorption: the samples were placed in
an oven at 40 °C for 6 h, then cooled and weighed in order to obtain
the dry weight (DW); afterwards, a series of samples were
immersed in the respective oils (15W-40 and DOT 4) and, periodi-
cally, weighted to obtain the current wet weight (CWW). The oil
absorption, in weight percentage (W%), was calculated using Eq. (3):
CWW  DW
W% ¼  100 ð3Þ
DW
 A.M. Amaro et al. / Composite Structures 118 (2014) 1–8 3

After exposure, the roughness profiles were obtained by a Mitutoyo
equipment, model SJ-500. In order to obtain the roughness param-
eters of all samples, measures were made in different zones of sam-
ple. Simultaneous, the surface topology was also observed in a
scanning electron microscope (SEM) and, all specimens, were sput-
tered coated with a 10 nm layer of gold prior to SEM observation.
The morphology was evaluated using Philips XL30 equipment.
Finally, the hardness was evaluated by ultramicroindentation, using
Fisherscope H100 equipment and a load of 500 mN. The hardness
values were corrected for the geometrical imperfections of the Vick-
ers indenter, the thermal drift of the equipment and the uncertainty
in the zero position according with reference [26]. The hardness, H,
is defined as the maximum applied load during the indentation test,
Pmax, divided by the contact area of the indentation immediately
before unloading, AC.
3. Results and discussion
Tensile and bending tests were performed by Banna et al. [12]
in order to evaluate the degradation of composite materials under
aggressive solutions and concluded that the last ones (bending
tests) are the most sensitive. Therefore, Fig. 1 shows an example
of the load versus flexural displacement curves for the control sam-
ples and samples exposed at 15W-40 and DOT 4 solutions, consid-
ering different exposure time. These curves are representative of
700
Control
600 15W40 15 days
DOT4 15 days
500
all conditions tested. Both curves are practically linear until the
maximum load is reached, where – a sudden drop occurs. In order
to explain the differences observed, the failure mechanisms are
presented in Fig. 2. For all conditions tested, the damage starts
by the fracture of the fibres in the tensile surface following, poste-
riorly, different damage mechanisms. Relatively to the control
samples (Fig. 2a), after the fracture of the fibres in tensile, with
small delaminations around the broken fibres, occurs compressive
breakage of the longitudinal fibres in the pin load contact region.
According to Reis et al. [27], this phenomenon is consequence of
the high compressive stress concentration in the pin load contact
region associated to the low compressive strength of the fibres.
For the samples immersed in the 15W-40 solution (Fig. 2b), asso-
ciated to the fracture of the fibres in the tensile surface occurs sig-
nificant delaminations around the broken fibres. Similar damage
can be found for the samples exposed to the DOT 4 solution
(Fig. 2c), however, in this case, extensive delaminations (cracks)
occurs between layers of the mid-thickness in tensile. It is evident
that these solutions promote matrix/fibre interface degradation,
especially for the aggressive one, where this damage mechanism
is more evident (Fig. 2c). These main damages are in agreement
(a)
1 mm
(a)

400
Load [N]

300
(b)
200
1 mm
100

0
0 1 2 3 4
Displacement [mm]
700
Control (b)
600 DOT4 15 days
DOT4 45 days
500
(c)
Load [N]

400
1 mm
300

200

100
Cracks
0
0 0.5 1 1.5 2 2.5 3 3.5
Displacement [mm]

Fig. 1. Typical load–displacement curves: (a) Effect of the solution; (b) Effect of the Fig. 2. Failure mechanisms: (a) Control samples; (b) Samples exposed to 15W40
exposure time. during 45 days; (c) Samples exposed to DOT4 during 45 days.
4 A.M. Amaro et al. / Composite Structures 118 (2014) 1–8

Table 1
Effect of the solutions on bending properties.

Samples Aver. flexural Std. dev. Aver. flexural Std. dev.

stress (MPa) (MPa) modulus (GPa) (GPa)
Control 826.1 22.4 28.4 1.77
15W40

Load [N]
15 days 810.2 21.9 27.2 2.23
45 days 764.6 21.5 25.3 2.27

Energy [J]
DOT4
15 days 798.9 14.9 26.1 2.70
45 days 735.9 16.3 23.4 2.87

with the studies developed by Amaro et al. [13,14], where the

aggressive solutions promote more extensive delaminations.
Table 1 presents the bending strength, calculated by Eq. (1), and Time [ms]
the bending stiffness modulus, calculated by Eq. (2), in terms of
average values and respective standard deviations. It is possible
to observe that, for the same exposure time (15 days), the hydrau- Displacement [mm]
lic brake fluid (DOT 4) promotes lower bending strength and bend-
Fig. 3. Typical load-time, load–displacement and energy–time curves for the
ing stiffness modulus than the universal multi-grade engine oil
control laminates.
(15W-40) relatively to the control samples. In terms of bending
strength this difference is, respectively, around 3.3% and 1.9% while
for the bending stiffness modulus is about 8.1% and 4.2%. On the
Table 2
other hand, and independently of the solution, the flexural Effect of the solutions and exposure time on the impact parameters.
strength and the flexural modulus decrease with the exposure
Samples Average max. Std. dev. Average max. Std. dev.
time. After 45 days the flexural strength decreases around 7.5%
load (N) (N) disp. (mm) (mm)
for the samples immersed in universal multi-grade engine oil
(15W-40) and 10.9% for the samples immersed in hydraulic brake Control 2737.1 11.0 2.26 0.2
15W40
fluid (DOT 4). Relatively to the flexural modulus these values are 15 days 2694.9 8.4 2.68 0.1
10.9% and 17.6%, respectively. These results agree with the litera- 45 days 2648.7 11.5 2.79 0.1
ture, where the aggressive solutions promote higher decreases of DOT4
the flexural properties [12–17,28]. For example, relatively to the 15 days 2665.6 15.5 2.81 0.1
hydraulic brake fluid (DOT4), the drop observed in terms of flexural 45 days 2515.4 10.3 3.12 0.1
strength (10.9%) and flexural modulus (17.6%), after 45 days of
exposure, is very similar to the values obtained by Amaro et al.
[14] with sulphuric acid (H2SO4) for an exposure time of 36 days the difference between the absorbed energy and the energy at peak
(11.6% and 17.6%, respectively). In this case, the lower flexural load [32,33].
properties were justified by the authors as consequence of the Table 2 presents, in terms of average values, the maximum load
lower Young’s modulus of the matrix and the matrix/fibre interface (Pmax) and maximum displacement obtained for the different solu-
degradation [13,14]. In fact, as shown in Fig. 2, significant delamin- tions and exposure time. After 15 days, for example, Pmax decreases
ations (cracks) occurred for the samples immersed in automotive around 1.5% when the samples are exposed to the universal multi-
brake fluid evidencing the matrix/fibre interface degradation. grade engine oil (15W-40) and 2.6% for the samples immersed in
On the other hand, low velocity impact events are very hydraulic brake fluid (DOT 4) relatively to the control samples.
dangerous, because they affect significantly the residual properties However, these values decrease for 3.2% and 8.1% after 45 days of
[19–23], and occurs frequently in-service or during maintenance exposure, respectively. The same comparison can be done for the
activities. In this context, present study analyses also the effect maximum displacement but, in this case, the opposite tendency
of these solutions on the impact strength. Fig. 3 shows the typical occurs. Relatively to the automotive engine oil this parameter
load-time (black colour), load–displacement (blue colour) and increases about 18.6% and 23.5%, while for the DOT4 solution the
energy-time (red1 colour) curves for the first impact relatively to values are around 24.3% and 38.1% after, respectively, 15 days
the control samples. These curves are representative of all samples and 45 days of exposure. Fig. 4 shows the elastic energy and
tested and are in agreement with those reported in literature damaged area against exposure time.
[13,14,29–33]. As expected, the elastic energy (restitution energy) decreases
The load–time and load–displacement curves are characterised with the exposition to the both solutions and shows to be depen-
by an increasing of the load up to a maximum value (Pmax) fol- dent with the exposure time. Consequently the damaged area
lowed by a drop after the peak load. In all tests the impactor sticks increases. For example, when the elastic energies are compared
into specimens and rebound always, which means that the maxi- with the other ones obtained for the control samples, a decreasing
mum impact energy was not high enough to infiltrate full penetra- of 9.7% and 20.6% occurs for the samples immersed in 15W-40
tion [32,33]. From the curves that represent the evolution of the solution during 15 and 45 days, respectively. However, these val-
energy with time, the beginning of the plateau of the curve coin- ues increase to 17.2% and 32.3%, respectively, for the DOT 4 solu-
cides with the loss of contact between the striker and the speci- tion. The same comparison for both solutions, but in terms of
men. This energy coincides with that absorbed by the specimen damaged area, presents values of 19.7% and 35.2% higher for the
and the elastic energy (restitution energy) can be calculated as samples immersed in automotive engine oil but 32.4% and 47.9%
higher for the samples immersed in automotive brake fluid. These
1
For interpretation of color in Fig. 3, the reader is referred to the web version of results agree with the other ones obtained previously by the flex-
this article. ural tests and with the open literature [13,14]. According with
 A.M. Amaro et al. / Composite Structures 118 (2014) 1–8 5

250 70 the bibliography, an interaction mechanism between matrix crack-

ing and delamination occurs on composite materials submitted to
60 low velocity impact [25,34,35]. On the other hand, the corrosive
225 solutions increase the number of cracks on the laminates, which
50 interacting with the delaminations promotes higher damaged
Damaged area [mm2]

Elastic energy [%]

areas (consequently the elastic energy decreases) [13,14]. Simulta-
200 40 neously, a poor fibre–matrix connection promotes the weakness of
the load carrying capacity of material [13,14,16].
175 30 In order to explain these results some additional tests were
done. The weight gain was obtained and Table 3 shows the results
20 for both solutions. It is possible to observe a small tendency to
150 15W40 DOT4 weight gain in terms of 15W-40 solution, but an inverse tendency
15W40 DOT4 10 can be found for the DOT 4 solution. In this case, compared with
the dry samples, a decrease about 2.16% can be found after 45 days
125 0 of exposure.
0 10 20 30 40 50
The surface topology was observed in a scanning electron
Exposure time [days] microscope (SEM) and Fig. 5 shows the typical pictures obtained.
Fig. 4. Damaged area and elastic energy against exposure time.
The unexposed samples (control samples) are characterised by a
smooth surface, Fig. 5a, but the exposition to the solutions increase
the roughness of the surface (micro-cracks). In order to quantify
Table 3
Effect of the solutions and exposure time on the weight gain.
this phenomenon, Table 4 presents the statistic of the roughness
measurements. It is evident the effect of the solutions on surface
Solution Exposure time (days) Weight gain (%) Std. dev. (%)
topology and the exposure time. For example, in terms of Rz (aver-
15W40 15 0.21 0.08 age peak to valley height), it is possible to observe a small tendency
45 0.38 0.12 to increase on the samples exposed to the 15W-40 solution
DOT 4 15 0.43 0.14 (11.62 lm after 15 days and 13.22 lm after 45 days) relatively to
45 2.16 0.18 the control samples (10.59 lm). However, according with Fig. 5,

(a)

50 µm

(b) (c)

50 µm 50 µm

(d) (e)

50 µm 50 µm

Fig. 5. SEM pictures for: (a) Control samples; (b) Samples exposed to 15W40 during 15 days; (c) Samples exposed to 15W40 during 45 days; (d) Samples exposed to DOT4
during 15 days; (e) Samples exposed to DOT4 during 45 days.
6 A.M. Amaro et al. / Composite Structures 118 (2014) 1–8

Table 4 Table 6
Statistics of the roughness measurements. Number of impacts to failure.

Samples/statistic values (lm)
Control samples
Arithmetic average, Ra
Root mean square, Rq
Average peak to valley height, Rz 10.59 ± 0.29
Core roughness depth, Rk
Reduced peak height, Rpk
Reduced valley depth, Rvk
15W40
Arithmetic average, Ra
Root mean square, Rq
Average peak to valley height, Rz
Core roughness depth, Rk
Reduced peak height, Rpk
Reduced valley depth, Rvk
DOT4
Arithmetic average, Ra
Root mean square, Rq
Average peak to valley height, Rz
Core roughness depth, Rk
Reduced peak height, Rpk
Reduced valley depth, Rvk
250
200
Indentation Load [mN]
Exposure time (days) Samples Number of impacts to failure
0 15 45 Control 12
15W40
15 days 11
2.07 ± 0.16 – –
45 days 11
2.52 ± 0.19 – –
– – DOT4
6.45 ± 0.17 – – 15 days 10
2.49 ± 0.18 – – 45 days 8
1.22 ± 0.17 – –
– 2.38 ± 0.16 2.71 ± 0.15
– 3.39 ± 0.15 3.44 ± 0.16 of the load-penetration depth curves obtained. These curves agree
– 11.62 ± 0.21 13.22 ± 0.27 with other ones presented in the literature [13,14,26] and the
– 6.34 ± 0.18 8.25 ± 0.16 important quantities in this loading–unloading cycle are maximum
– 6.78 ± 0.19 5.03 ± 0.12 load, maximum depth, final depth after unloading and the slope of
– 2.19 ± 0.17 1.68 ± 0.16
the upper portion of the unloading curve known as the elastic con-
tact stiffness. Table 5 presents the average values of hardness,
– 2.88 ± 0.14 3.99 ± 0.15
indentation modulus (ER) and Young’s modulus (E) of the matrix.
– 3.57 ± 0.15 5.51 ± 0.18
– 15.05 ± 0.28 24.01 ± 0.29 It is possible to conclude that the measured hardness decreases,
– 9.58 ± 0.18 10.46 ± 0.17 independently of the solution and exposure time, in comparison
– 3.93 ± 0.19 3.53 ± 0.16 with the control samples (0.288 GPa). For example, after 45 days
– 2.53 ± 0.17 11.61 ± 0.15
of exposition, the average value of hardness decreases around
10.8% and 11.5%, respectively, for universal multi-grade engine
oil (15W-40) and hydraulic brake fluid (DOT 4). Finally, the inden-
tation modulus (ER) and Young’s modulus of the matrix was
Control obtained according with Antunes et al. [26], where the indentation
15 days- 15W40 modulus (ER) is a function of the Young’s modulus (E) and the Pois-
son ratio (m) of the specimen and the indenter. For both parame-
45 days - 15W40
ters, a similar evolution to the hardness can be found. After

15 days- DOT4
150 45 days of exposure a decrease about 23.2% and 33.0% occurs,
45 days- DOT4
respectively, for the 15W-40 solution and DOT 4 solution in com-
parison to the control samples. Therefore, this can explain also
100 the lower flexural properties observed associated to the matrix/
fibre interface degradation.
Finally, the effect of these solutions on laminates subjected to
50 multi impacts will be analysed. Table 6 shows the impact resis-
tance and the laminates are considered failed when full perforation
occurs. Full perforation is defined when the impactor completely
0 moves through the samples. The performance of the laminates to
0 2 4 6 8
repeated low velocity impacts is dependent of the solutions. After
Indentation depth [mm]
45 days of immersion, for example, the impact resistance decreases
Fig. 6. Schematic representation of the typical load-penetration depth curves. around 8.3% for the 15W-40 solution and 33.3% for the DOT 4 solu-
tion, when compared with the control samples. This was expected,
because the automotive brake fluid promotes major damages on
the exposition to the DOT 4 solution promotes the highest values, the laminates, in terms of matrix and interface matrix/fibre, as seen
where Rz increases around 42.1% and 126.7% after 15 days and previously. Fig. 7 shows the aspect of the samples (one impact
45 days of exposure time, respectively, relatively to the control before of the full penetration) for each condition tested, where is
samples. Therefore, besides the effect on the adhesion between evident the matrix/fibre interface degradation.
the fibres and matrix, DOT 4 solution promotes multiple cracks Fig. 8 presents the evolution of the elastic energy (restitution
on the matrix. energy) against the normalised impact numbers (N/Nf), where
The hardness was also evaluated by ultramicroindentation and the last impact it is not represented because occurs full penetration
Fig. 6 shows, for all conditions tested, a schematic representation (elastic energy = 0). N is the current number of impact and Nf is the

Table 5
Effect of the solutions on average values of hardness, indentation modulus and Young’s modulus of the polymeric matrix.

Samples Aver. hardness VH (GPa) Std. dev. (GPa) Aver. ER (MPa) Std. dev. (MPa) Aver. E (GPa) Std. dev. (GPa)
Control samples 0.288 0.01 8.50 1.59 7.83 1.47
15W40
15 days 0.258 0.01 6.73 0.66 6.13 0.62
45 days 0.257 0.01 6.55 0.85 6.01 0.80
DOT4
15 days 0.256 0.01 6.35 0.59 5.83 0.50
45 days 0.255 0.01 6.19 0.84 5.25 0.78
 A.M. Amaro et al. / Composite Structures 118 (2014) 1–8 7

(a) (b)

(c)
Fig. 7. Aspect of the samples, one impact before of the full penetration, for: (a) Control samples; (b) Samples immersed in 15W40 solution during 15 days; (c) Samples
immersed in DOT4 solution during 15 days.

80 4. Conclusions

70 This work studied the flexural and low velocity impact response
60 of a glass fibre/epoxy composite after immersion in universal
multi-grade engine oil (15W-40) and in extra high performance
Elastic energy [%]

50 hydraulic brake fluid (DOT 4).

It is possible to conclude that both solutions affect the flexural
40 strength and flexural modulus. In terms of impact parameters, the
Control samples exposition to these solutions promotes lower maximum loads and
30
higher maximum displacements relatively to the control samples.
15W40 - 15 days
20 The elastic energy decreases with the exposition for both solutions
DOT4 - 15 days
and shows to be very dependent with the exposure time. Finally,
10 15W40 - 45 days the performance of the laminates to repeated low velocity impacts
DOT4 - 45 days depends of the solution. However, for all tests performed, the auto-
0 motive brake fluid promotes the lowest values comparatively to
0.0 0.2 0.4 0.6 0.8 1.0 the automotive engine oil.
N/Nf According with the complementary tests performed, the
decreasing of the mechanical properties observed can be explained
Fig. 8. Elastic energy against number of impacts.
by the lower Young’s modulus, in terms of matrix, associated to the
matrix/fibre interface degradation. In this context, the load carrying
70 1000 capacity of the composites decreases. On the other hand, when the
laminates are in contact with the solutions, especially with the auto-
60 motive brake fluid, multiple cracks occur on the matrix. These cracks
800 interact with the delaminations and higher damaged area occurs.
Damage area [mm2]

50
Elastic energy [%]

Acknowledgement
40 600
This research is sponsored by FEDER funds through the program
30 COMPETE – Programa Operacional Factores de Competitividade –
400
and by national funds through FCT – Fundação para a Ciência e a
20 Tecnologia, under the project PEst-C/EME/UI0285/2013.
Control samples
15W40 - 45 days
200
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