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Original Article

Charpy impact test of epoxy composites reinforced


with untreated and mercerized mallow fibers夽

Lucio Fabio Cassiano Nascimento ∗ , Sergio Neves Monteiro, Luis Henrique Leme Louro,
Fernanda Santos da Luz, Jheison Lopes dos Santos, Fábio de Oliveira Braga,
Rubens Lincoln Santana Blazutti Marçal
Military Institute of Engineering – IME, Department of Materials Science, Praça General Tibúrcio 80, Praia Vermelha, Urca, 22290-270
Rio de Janeiro, RJ, Brazil

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

Article history: The mallow fiber (Urena lobata, linn) is demonstrating a great potential as reinforcement
Received 10 November 2017 in polymer matrix composites. The difficulty in the use of the mallow, as in other natural
Accepted 13 March 2018 lignocellulosic fibers (NLFs), is its hydrophilic compatibility with polymeric matrices that
Available online 23 August 2018 are typically hydrophobic. In order to improve the adhesion between the fiber surface and
polymeric matrices, mallow fibers were subjected to mercerization treatment. In this work
Keywords: composites were produced with epoxy matrix reinforced with 30 vol% of mallow fibers, both
Mallow fibers untreated and mercerized. By means of XRD analysis it was verified the variation of crys-
Epoxy composite tallinity in fibers treated with different NaOH solutions as well as immersion times and
Mercerization agitation. After this XRD preliminary analysis, a treatment of 5% NaOH solution for 24 h
Charpy impact test without agitation was selected. The objective was to compare the Charpy impact energy of
composites specimens produced with untreated mallow fibers and treated for the higher
crystallinity obtained after the selected mercerization. For the analysis of impact energy
the Tukey test was applied from which it could be assured, with a confidence level of 95%,
that the epoxy specimens reinforced with 30 vol% of untreated mallow fibers, had the best
performance.
© 2018 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier
Editora Ltda. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

same type of NLF may considerably vary its properties depend-


1. Introduction ing on their origin, quality and age of the plant, as well as
fiber diameter, aspect ratio and its preconditioning. This could
Unlike synthetic fibers, natural lignocellulosic fibers (NLFs) significantly affect the performance of polymer composites
do not have uniform properties. In fact, they are microstruc- reinforced with NLFs [1–12]. Another difference between NLFs
turally heterogeneous and have dimensional limitation. The and synthetic fibers is their interaction with water. Due to the


Paper was part of technical contributions presented in the events part of the ABM Week 2017, October 2nd to 6th, 2017, São Paulo, SP,
Brazil.

Corresponding author.
E-mail: lucio coppe@yahoo.com.br (L.F. Nascimento).
https://doi.org/10.1016/j.jmrt.2018.03.008
2238-7854/© 2018 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier Editora Ltda. This is an open access
article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
j m a t e r r e s t e c h n o l . 2 0 1 8;7(4):520–527 521

Table 1 – Physical and mechanical properties of the mallow fibers.


Natural fiber Diameter (␮m) Length (mm) Specific mass (kg/m3 ) Tensile strength (MPa) Elongation at break (%) Modulus of elasticity (GPa)

Mallow 42.6 23.8 1374 160 5.2 17.4

presence of hydroxyl groups NLFs are hydrophilic, with high


affinity with humidity. The fiber moisture content can vary
between 5 and 10 wt% [2,3].
The water on the surface of a NLF, reinforcing a composite,
acts as a release agent at the interface of a hydrophobic poly-
mer matrix. Further, due to evaporation of water, voids may
appear in the matrix, resulting in loss of mechanical proper-
ties. One solution to reduce the moisture content and improve
the interfacial adhesion is drying the NLF followed by pretreat-
ing the fibers by chemical modification of the surface [13–22].
Pretreatment enables the creation of increased roughness
on the surfaces, which contributes to better adhesion to the
polymer matrix. Among the different techniques for pretreat- Fig. 1 – Mallow fibers as received by UENF.
ing to produce NLFs surface modification, one of the most used
is the alkaline treatment, also known as mercerization [17].
The mercerization removes both the waxes and greases as a
Table 2 – Types of specimens produced from the
portion of hemicellulose and lignin, enhancing the packing variation of the mercerization parameters.
of the cellulose molecules and increasing crystallinity of the
Concentration NaOH Immersion time NaOH
fibers. This results in a rougher surface with larger contact
surface, aiding in mechanical anchoring and promoting an 3h 24 h 48 h
increase in both the elastic modulus and the tensile strength
5% CP1 CP4 CP7
[23,24]. 10% CP2 CP5 CP8
The mallow fiber (Urena lobata, linn) although widely used 20% CP3 CP6 CP9
for making cordage in clothes as well as carpets, paper money,
crafts among others [25], does not have so far a great use
case, mallow fibers were subjected to NaOH mercerizing treat-
as reinforcing component in industrial composite products.
ment in the combination of parameters, according to Table 2.
However, physical and mechanical properties such as tensile
The choice of immersion times was based on the effective-
strength have shown [26,27] a promising potential for using
ness of the treatment. Indeed, a minimum of 3 h was needed
mallow fibers as reinforcement in polymer matrix composites
to reveal visible microstructural changes. By contrast, more
(PMCs). Table 1 presents some of these properties.
than 48 h treatment caused serious degradation to the fiber
In this context, there is the possibility of using PMCs rein-
integrity. A 24 h treatment time was selected as middle in
forced with mallow fibers in dynamic applications such as
between the extreme conditions.
ballistic armor. Therefore, increased crystallinity of the mal-
After a preliminary selection based on the value of crys-
low fibers and consequently the adhesion to the polymer
tallinity obtained by X-ray diffraction (XRD), one specific
matrix, through the mercerization treatment, may provide
treatment, the CP4 in Table 2 was applied. These treated mal-
improvement in the mechanical properties of the compos-
low fibers were then incorporated into epoxy matrix for impact
ites. This could be the case of Charpy impact energy, which
test. Charpy test specimens with untreated fibers were added
is investigated in the present work.
into epoxy matrix in the volumetric fractions of 0%, 10%, 20%
and 30%. Specimens with 5% NaOH for 24 h treated fibers, rel-
ative to CP4 in Table 2, were added into the epoxy matrix in the
volumetric fraction of 30%. Fig. 2 shows the various compos-
2. Materials and methods ite plates produced. These plates were cut in several Charpy
specimens according to the standard [28].
The mallow fibers were provided by the State University of
The crystallinity index (Ic ) of the cellulose was calculated
North Fluminense (UENF) and acquired from the Textile Com-
by means of Eq. (1).
pany Castanhal, Brazil Fig. 1 shows the as received mallow
fibers. The polymer used as the material of the composite plate I1
matrix was a commercial epoxy resin diglycidyl ether type of Ic = 1 − (1)
I2
bisphenol A (DGEBA) cured with triethylene tetramine (TETA),
using the phr of 13 parts of hardener to 100 parts of resin. where I1 is the intensity of the minimum of diffraction, related
Mallow fibers were added in two different situations as to the amorphous part and I2 is the intensity of the maximum
reinforcement in the manufacture of epoxy composite plates. of diffraction, related to the crystalline part. This method was
In the first case the untreated fibers were cleaned, cut to a developed in 1959 by Segal et al. [29], and has been widely
length of 150 mm and dried in a stove for 24 h. In the second used for the study of natural fibers [30,31]. The XRD analyses
522 j m a t e r r e s t e c h n o l . 2 0 1 8;7(4):520–527

dimensions [28]. The tests were performed in a PANTEC


instrumented pendulum, Model XC-50, 1 × 220 V × 60 Hz. Fig. 3
20% illustrates the prepared specimens for the Charpy tests.
After impact tests, fragments of the ruptured specimens
were collected and analyzed by scanning electron microscopy
10% (SEM), in a model Quanta FEG FEI equipment.
30% with treat.

0%
3. Results and discussion
30% no treat.
Fig. 4 shows the FTIR spectra for: (a) untreated and (b) mer-
cerized treated mallow fibers. These spectra reveal significant
changes in the wavenumber interval from 800 to 1800 cm−1 .
By comparing the values in Table 3 to the results of Fig. 4 one
notice that the strong absorption band around 1050 cm−1 for
Fig. 2 – Plates composite fiber percentage from 0 to 30 vol% the untreated fiber, Fig. 4(a), which might correspond to the
without treatment and 30 vol% with treatment C – O stretching in cellulose, hemicellulose and lignin, has
(mercerization – 5% NaOH). been considerably attenuated in the mercerized treated fiber,
Fig. 4(b). Similarly, the absorption band around 1400 cm−1 for
the untreated, Fig. 4(a), which could be associated with CH2
were performed in a Shimadzu diffractometer, model XRD- bending or wagging in lignin, is practically inexistent in the
6000, scan speed of 4◦ /min, power 30 mA × 40 kV and scanning treated fiber. One may then conclude that mercerization sig-
from 5◦ to 80◦ . nificantly affects the participation of lignin, which is a bonding
Fourier transform infrared (FTIR) analysis was conducted substance for the cellulose, in the mallow fiber.
in a model IR Prestige 21-FTIR Shimadzu equipment. Samples Fig. 5 shows DMA results for: (a) neat epoxy and (b) epoxy
of mallow fibers, both untreated and mercerized treated, were composites reinforced with 30 vol % of mallow fibers. By com-
first milled followed by sieved for 20 mesh and then mixed paring the two graphs, in general, it is observed an increase in
with KBr. The mixture was then pressed to produce a film suit- onset of softening temperature of the storage modulus E , as
able for the analysis. Table 3 shows the FTIR absorption bands well as displacement to higher of the perks in the loss mod-
for a natural fiber [32]. ulus “E”, and tangent delta. A possible interpretation for this
Dynamic mechanical analysis (DMA) test was carried out behavior is an interference of the mallow fibers in the mobility
from 20 to 200 ◦ C in a model DMA Q800 TA Instrument using of the epoxy chains, which postpones the occurrence of glass
single cantilever 3 points bending specimens according to transition temperature.
standard. A heating rate of 3 ◦ C/min and nitrogen atmosphere The results obtained from the Charpy impact test for epoxy
was applied for the test. matrix composite reinforced with continuous and aligned
A total of 7 specimens for Charpy impact test were obtained mallow fibers, in percentages 0, 10, 20 and 30 vol% without
by cutting each composite plates according to ASTM D6110 treatment as well as 30 vol% with treatment, CP4 in Table 2,
disclosed a good ability to absorb energy as compared to other
polymer composites reinforced with NLFs [23]. Fig. 6 shows the
results of Charpy absorbed energy (J/m) test for each group. It
Table 3 – FTIR absorption bands for a natural fiber [32].
should be noticed that, as in other works [33,34], occurs an
Frequency (cm−1 ) Assignment
increase in average energy values with the fiber volume frac-
3200–3600 OH stretching tion used in the composite. High impact energy values can be
2905 CH2 and CH3 stretching related to low interfacial bonding, obtained by pullout tests,
1740 Carbonyl (C O) Stretching of carboxylic acid or between the fibers and the matrix [35].
ester
A low interfacial bonding between the mallow fiber and the
1650 H O H bending of absorbed water
epoxy matrix allows for easier decohesion during the impact,
1616 Benzene ring stretching (lignin)
1500 Benzene ring stretching (lignin) which causes fracture by delamination. This mechanism of
1440 CH2 bending in lignin fracture is more effective in composites with greater amount
1411 CH2 and CH3 bending of reinforcement mallow fibers, above 10 vol%.
1357 CH2 bending In this case, it can increase the path to be followed by the
1320 CH2 wagging (lignin) crack, and therefore the absorbed energy required for fracture
1235 C O stretching of acetyl (lignin)
of the composite. Perhaps, because of this, there was a relative
1150 C O C antisymmetric bridge stretching in
cellulose and hemicellulose
reduction of impact energy in the specimens produced with
1110 O H association in cellulose and hemicellulose mercerized fibers as presented in Fig. 6. Due to the increased
1028 C O stretching in cellulose, hemicellulose and crystallinity of the fibers and consequently better adhesion
lignin to the epoxy matrix, cracks found difficult to propagate and
879 ␤-Glucosidic linkage create fractured surfaces that would be associated with higher
600 Out of plant OH bending
impact energy.
j m a t e r r e s t e c h n o l . 2 0 1 8;7(4):520–527 523

Fig. 3 – Specimens with mallow fiber for Charpy test. (a) 0 vol%; (b) 10 vol%; (c) 20 vol%; (d) 30 vol% without treatment and (e)
30 vol% with treatment.

a Mallow fibers b Mallow fibers


FTIR (untreated) FTIR (treated)
100 100

95
95
898

Transmitance (%)
Transmitance (%)

897
669
90

559
518
667
1649

15961504
429

90
1504

85
560

1645
1468

1334
2906

1401
1736

1026
1117
85 80
1399

2906
75
80
1051

3478
3424

4000 3500 3000 2500 2000 1500 1000 500 4000 3500 3000 2500 2000 1500 1000 500
Wavenumbers (cm-1) Wavenumbers (cm-1)

Fig. 4 – (a) FTIR to mallow fibers untreated; (b) FTIR to mallow fibers treated.

2000 300 5000 800


78.79°C
a 94.80°C DMA b 96.91°C DMA
67.33°C
72.56°C
250
4000 84.86°C 0.4
1500 0.6 600
Storage modulus (MPa)

70.60°C(I)
Storage modulus (MPa)

Loss modulus (MPa)


Loss modulus (MPa)

200

71.26°C 3000 77.89°C(I) 0.3


70.60°C(I)
Tan delta
Tan delta

1000 0.4 150 400


78.99°C
2000 0.2
100

500 0.2 200


1000 0.1
50

0 0 0 0
0 50 100 150 200 0 50 100 150 200
Temperature (°C) Temperature (°C)

Fig. 5 – (a) DMA to neat epoxy; (b) DMA to epoxy composites reinforced with 30 vol% of mallow fibers.

Fig. 7 shows the diffractograms obtained for each mercer- fibers in epoxy matrix composites as well as the treatment of
ized sample, according to the various combinations of the mercerizing has different effects on the Charpy impact energy.
parameters: concentration, immersion time and agitation. In The Tukey test was applied for comparison, using a con-
this figure, 5% NaOH, 24 h immersion and without agitation, fidence level of 95%, to determine which volumetric fraction
CP4 was found in Fig. 7(a) to have a fiber crystallinity index of mallow fibers provided better results in terms of Charpy
(Ic ) of 84.49%. This is higher than the value obtained for the impact energy. The less significant difference (LSD) obtained
other mercerization combinations and for the untreated mal- was 77.34. The results for the differences between the mean
low fibers (82.24%) in Fig. 7(b). values of Charpy impact energy are shown in Table 5.
From the results obtained, the analysis of variance (Table 4) Based on these results, with 5% significance level, the
rejects the hypothesis that the means are equal to 5% signifi- reinforced composite with 30 vol% mallow fibers without
cance level for the statistical “F”, on this account: F calculated treatment showed better performance since it exhibited a
>F critical (tabled). Therefore, the volume fraction of mallow higher average energy value of Charpy impact (905.49 J/m).
524 j m a t e r r e s t e c h n o l . 2 0 1 8;7(4):520–527

Table 4 – Analysis of variance of the average impact energies obtained for the epoxy matrix composites reinforced with
percentages from 0% to 30 vol% of mallow fibers.
Variation causes DF Sun of squares Mean square F calc. F crít (tab.)

Treatments 4 3468899.11 867224.78 348.18 2.69


Residue 30 74721.76 2490.73

Total 34 3543620.88

Table 5 – Results for the differences between the mean values of Charpy impact energy in the volume fractions of mallow
fiber 0 to 30% after application of the Tukey test.
Volumetric fraction of mallow fibers 0% 10% 20% 30% without treatment 30% with treatment

0% 0 46.59 470.63 809.41 65.36


10% 46.59 0 424.04 762.83 18.77
20% 470.63 424.04 0 338.78 405.27
30% without treatment 809.41 762.83 338.78 0 744.05
30% with treatment 65.36 18.77 405.27 744.05 0

1200 (161 J/m) of 30 vol % treated mallow fiber composite (CP4),


Results of charpy impact test for the epoxy matrix composites Fig. 4, which is much lower than those of 20% and 30 vol %
reinforced with mallow fibers
and treated mallow fiber composite.
Average charpy energy absorbed (J/m)

1000
One possible explanation would be that the percentage of
10 vol% in mallow fibers were not sufficient to produce an
800
effective reinforcement in the epoxy matrix, which is asso-
ciated with low results in Charpy impact energy. In all test
600 specimens there was a similar complete rupture, making valid
the results. In Fig. 8 it is shown the specimens ruptured after
905.49 the Charpy test.
400
By visual analysis it can be seen a brittle fracture tendency
566.71
in specimens with 0% and 10 vol% untreated and 30 vol%
200
treated, which was confirmed by the impact energy values pre-
142.66 161.44 sented in Fig. 4. This figure shows a higher increase of more
96.07
0 than 6 times in going from 10% to 20 vol% mallow fibers. The
0% 10% 20% 30% 30%
Untreated Treated (CP4) SEM images in Figs. 9–11 show the way fracture mechanisms
Volumetric fraction mallow fibers (%vol) are involved in the impact process.
In Fig. 9(a) and (b) it is perceived clearly the brittle fracture
Fig. 6 – Results of Charpy impact test for the epoxy matrix
mechanism by the presence of “river marks”, both in the spec-
composites reinforced with mallow fibers.
imen with 100% epoxy as well as the composite with 10 vol%
of fiber. These show that there was no effective reinforcement
with low percentage of fibers.
This is significantly distinct from the others because the dif-
For untreated composites with 20 vol% of mallow fibers it
ferences are higher than LSD (77.34). Another important point
was observed a greater amount of energy absorption owing to
to emphasize is the comparatively lower for the impact energy

l (Counts)
600
a lc = 82.24%
400

200

0
10 20 30 40 50 60 70
Theta-2Theta (deg)
l (Counts)
1500
b lc = 84.49% (CP4)
1000

500

0
10 20 30 40 50 60 70
Theta-2Theta (deg)

Fig. 7 – (a) Diffractogram for untreated mallow fibers; (b) diffractogram for mallow fibers mercerizing (CP4).
j m a t e r r e s t e c h n o l . 2 0 1 8;7(4):520–527 525

fracture mechanisms. Indeed, Fig. 10(a) revealed broken and


detached fibers of the matrix, and a very effective encasement
of the broken fibers by the epoxy matrix. On the contrary,
the mercerized treated mallow fiber composite, evidence of
delamination, i.e. separation between fiber and epoxy matrix,
is observed in Fig. 10(b).
In the image of Fig. 11(a) for the untreated 30 vol% mallow
fiber composites one sees the fibers rupture, and the interfa-
cial detachment from the epoxy matrix. These failure mecha-
nisms led to the high absorption of impact energy as compared
to the other percentages of untreated mallow fiber composites.
However, the image of Fig. 11(b) for the mercerized-treated
30 vol% shows the fracture surface like those of com-
posites reinforced with untreated 0% and 10 vol% fibers.
Thus, the fracture was brittle and the absorbed energy was
similar to that measured for reinforcement with 10 vol%
fiber.
Finally, Table 6 displays a comparison between the young
modulus and tensile strength obtained in quasi-static, test
velocity of 2 mm/mm, and the impact energy. In this table one
should notice that a relationship exists between the quasi-
Fig. 8 – Specimens completely fractured after Charpy
static mechanical properties and the absorbed impact energy.
impact test. (a) 0 vol%; (b) 10 vol%; (c) 20 vol%; (d) 30 vol%
Indeed, the higher the amount of mallow fiber in the compos-
without treatment and (e) 30 vol% with treatment.
ite, the higher the stiffness, strength and impact energy. This
emphasize the relevant effect of mallow fibers as reinforce-
ment of epoxy composites.

Fig. 9 – (a) Epoxy composite with 0 vol% mallow fibers; (b) composite with 10 vol% mallow fibers.

Fig. 10 – (a) Composite with 20 vol% mallow fibers; (b) mallow fiber detail in composite with 20 vol% of fibers.
526 j m a t e r r e s t e c h n o l . 2 0 1 8;7(4):520–527

Fig. 11 – (a) Epoxy composite reinforced with 30 vol% untreated mallow fibers; (b) epoxy composite reinforced with 30 vol%
mallow fibers mercerized (5% NaOH, 24 h and without agitation – CP4).

Table 6 – Comparison between tensile strength, young modulus and Charpy impact energy to composites reinforced
with mallow fibers.
Percentage of mallow fibers Tensile strength (MPa) Young modulus (GPa) Charpy impact energy (J/m)

0% 32.98 ± 14.61 3.89 ± 0.03 96.07 ± 21.15


10% 90.01 ± 21.35 11.60 ± 0.11 142.66 ± 8.23
20% 109.85 ± 21.70 15.73 ± 0.17 566.71 ± 52.54
30% 177.49 ± 17.80 20.50 ± 0.10 905.49 ± 94.56

4. Conclusions Acknowledgements

The Charpy impact energy increase with the volume fraction The authors thank the support to this investigation by the
of mallow fibers incorporated into the epoxy matrix. Among Brazilian agencies: CNPq, CAPES and FAPERJ; and UENF for
the specimens evaluated by the Tukey test with 95% con- supplying the mallow fibers.
fidence level, the composite with 30 vol% of mallow fibers
without treatment was the one that exhibited the best results
in terms of Charpy impact energy. This particular case indi-
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