Composite Structures 124 (2015) 152–162

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

Mechanical characterizations of composite material with short Alfa

fibers reinforcement
H. Mechakra, A. Nour ⇑, S. Lecheb, A. Chellil
Dynamic Motors and Vibroacoustics Laboratory, M’Hamed Bougara University of Boumerdes, Algeria

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

Article history: This paper presents an experimental study of mechanical characterization of composite materials, rein-
Available online 16 January 2015 forced with short vegetable fibers and obtained by a new implementation of their extraction from Alfa
bundles. From many previous studies on the chemical treatments of these fibers, to improve the interfa-
Keywords: cial adhesion; an alkaline chemical treatment optimization under different durations was applied to the
Composites fibers and a fatigue behavior analysis was conducted under an acoustic control of polypropylene matrix
Alfa fiber bundles samples with different volume fiber fractions. An SEM observation of the fibers morphology and of the
Chemical treatments
interfacial characteristics of the material during the test before and after the optimized alkaline treat-
Interfaces
Fatigue
ment showed the impact of this treatment by the important increase of the Young module from
28.67% to 132.22% with respect to the virgin PP and of the traction resistance from 11.34% to 30.14% with
respect to the non treated fibers for 30%.
Ó 2015 Elsevier Ltd. All rights reserved.

1. Introduction unsaturated polyester. Treatment with styrene (S) gave an increase

As reinforcements in composite matrices, natural fibers
attracted a particular attention in recent years as substitutes to
synthetic fibers such as glass and carbon fibers. They improve
the mechanical properties and allow a gain in weight and in cost
and can be recycled [1]. Many researches were done to study the
mechanical properties and the interfacial adherence performances
based on natural fiber composites especially between the hydro-
philic natural fibers and the hydrophobic polymer matrices [2,3].
The adhesion between the fibers hydrophilic surface and the
hydrophobic polymer used as the matrix, is affected by the humid-
ity adsorption capacity and the presence of non-cellulosic compo-
nents (waxy material, lignin and hemicelluloses). The fibers in
these cases undergo significantly a damage and therefore, reduce
the material strength [4,5].
Many focused studies on different methods and means of treat-
ment of natural fibers surfaces as a reinforcement of composite
materials were conducted to improve inter facial link properties
and to increase their resistance to humidity [6–8]. A. Bessadok
et al. [9] studied the effect of the chemical treatment with the
maleic anhydride (MA), with the styrene (S), with the acrylic acid
(AA) and with the acetic anhydride (Ac) on the Alfa composite/
⇑ Corresponding author.
E-mail address: abdelkader_nour@hotmail.fr (A. Nour).
in the hydrophobic character and a decrease in roughness, espe-
cially with treated fibers. Alix et al. [10] studied the behavior of flax
fibers chemically modified by the silane (Si) and by the styrene (S)
treatments, depending on the water adsorption. An increase in the
resistance to humidity was found with the styrene treatment.
Rokbi et al. [1] studied the effect of the alkaline treatment on the
Alfa/polyester performance. They found that the mechanical
strength increases when increasing the NaOH concentration. With
a 10% NaOH treatment during 24 h, the strength and the bending
modulus increased by approximately 60% compared to the
untreated fibers. Arrakhiz et al. [11] determined the mechanical
properties of different composite materials of polypropylene with
the esterifies Alfa fiber reinforcement, and treated with an alkaline
treatment, which is the cheapest and least harmful to the environ-
ment. They concluded that the NaOH treated composites give high
mechanical and thermal performances. Arrakhiz et al. [12] proved
that an alkaline treatment of Alfa fibers, coir and bagasse reinforc-
ing the polypropylene, improves the mechanical properties of the
composite and the fiber/matrix cohesion. With a reinforcing rate
of 30% of the Alfa and bagasse fibers, treated with an NaOH solu-
tion at 1.6 mol/l during 48 h, the fibers bending and traction mod-
ules increased by 45% and 75% respectively. From the results
analysis of the previous studies in this area, a compromise could
be reached by an alkaline treatment with a well determined con-
centration and a modification in the treatment protocol, to reduce
the humidity absorption due to the hydroxyl (OH) link.

http://dx.doi.org/10.1016/j.compstruct.2015.01.010
0263-8223/Ó 2015 Elsevier Ltd. All rights reserved.
 H. Mechakra et al. / Composite Structures 124 (2015) 152–162
In this article is studied the fatigue mechanical properties of the
composite material obtained by a new implementation of fiber
extraction from Alfa bundles and the optimized chemical treat-
ment, to evaluate its impact on the mechanical properties of the
composite with polypropylene matrix. In order to better evaluate
the effect of the chemical treatment, the ratio of natural fibers
(Alfa) chemically treated and untreated was set to 10%, 20%, and
30%. This process has allowed the modification of the fibers struc-
ture. In order to better evaluate the effect of the chemical treat-
ment, the ratio reinforcement of natural fibers (Alfa) chemically
treated and the untreated was studied for different cases of treat-
ment durations.
2. Elaboration of the composite with Alfa short fiber
reinforcement
2.1. Materials and methods
The polypropylene used in this composite is a thermoplastic
polymer supplied by Agro Fibers Plastics Technologies (AFT Plas-
tics), under the commercial reference PPC706-21NAHP, with a
melting temperature of 185 °C. The Alfa wild plant fiber (Latin
word Esperto) is used as reinforcement. Raw and fresh Alfa stems
are gathered from the Meskiana zone steppe of Algeria (Fig. 1). The
Chemical treatment used for the fibers is the NaOH (caustic soda
supplied by SPADO) and the acetic acid CH3COOH (réf.070222).
2.2. Preparation and extraction of Alfa fiber
The extraction of the short fibers from the bundles Alfa is the
most important phase for the implementation of composite rein-
forcing with the short fibers. The raw Alfa Stems bound to crushing
are cut into small pieces of 3–4 cm of length (Fig. 4a and b). A new
procedure which has never been used before is implemented; it
consists of a preliminary stem crushing to get bundles. Previous
published experiments to get plant composite reinforcements have
stopped at the reinforcement by the fiber bundles [12]. This new
technique requires a crushing in two stages. The first crushing is
devoted to obtaining the bundles and to avoid damaging by centri-
fugation of the fibers that constitute the bundles, which stick by
friction between the wall of the mill and the sharp blades
(Fig. 2), and which increases the temperature inside the mill.
Fig. 2a shows the fiber crushing and its damage by the dust debris
appearance. The appeared defects on the fiber bundles during the
crushing by the cutting blades, can be random fiber shears and
fiber distortions (Fig. 2b) that deform their cellulosic architecture,
such as the fibrillar angle and the damage to the inter cellulosic
links (Fig. 2c). These defects of the Alfa vegetal fiber crushing to
Fig. 1. Alfa (a – wild plant of Meskiana Zone in Algeria, b – stem raw Alfa).
153
avoid in order to get short fibers with a very thin diameter (com-
pared to the bundles), increase the material mechanical character-
istics performances. Note that the chemical treatment repairs the
fiber defects obtained by the crushing and makes uniform its sur-
face state.
The second step is to reverse the crushed stems to avoid the
sticking to the mill wall. The whole is placed in an eight stage sieve
of diameter 1–0.125 mm, to clean the fibers and to remove dam-
aged bundles (Fig. 2d) and get rid of the dust. Most previous stud-
ies used bundle reinforcement [12]. The bundle deficiency, in
addition to structure gaps which may contain impurities (lignin,
materials, waxes, hemicelluloses), the used chemical treatments
which are superficial, will be partial since they will not be able
to reach certain fibers parts [12]. That causes a major defect of bun-
dle loosing during the traction or the fatigue tests. Furthermore,
this implementation of the fiber separation constituting the bun-
dles (reduction in large diameter bundles) allows a significant gain
in the composite weight (Fig. 3) but also and mainly the impregna-
tion of the chemical treatment over the entire fiber surface than
that of the fiber inside the bundles where the treatment is partial.
The main idea in this paper is to reduce the diameter of the
Alfa-fiber bundles, in order to get a good distribution throughout
the entire volume of the material matrix, relative to the material
containing bundles fiber of large diameter. On the other hand,
the fiber bundles defibration (Fig. 3) allows the increase of the
adhesion surface (interface) with the matrix for a same volume
fraction, and therefore to improve the mechanical characteristics
of the material.
The chemically treated fibers are then extruded by a mono-vice
extruder with polypropylene to obtain compounds. These latter are
injected by an injection press (Fig. 6) to get samples for mechanical
characterization tests.
2.3. Chemical treatment of Alfa fibers
The Alfa fibers are treated with two treatment durations of 48
and 24 h within NaOH solution.
First, two fiber lots are washed and immersed, each one in a
solution of NaOH of 1.6 mol/l. one is immersed for 48 h and the
other for 24 h. Then, the fibers of each lot are neutralized with
100 ml of acetic acid and dried in the open air for 24 h [11], after
that in an oven for 12 h at 60 °C. These dry fibers are then put in
a vacuum dryer containing P2O5 for 48 h to reduce the humidity
content, [1]. Thus, the fibers obtained by different treatments are
used for the elaboration of the specimens. The aspect of the fibers
and their color show the impact of the two alkaline treatment
durations and the significant role for eliminating waxy materials
and semi cellulosic (Fig. 5). They stick the one to the other in the
154 H. Mechakra et al. / Composite Structures 124 (2015) 152–162

Fig. 2. MEB observation of the grinding fibers morphology.

5 5

4.5
4 4

3.5
3 3

2.5

2 2

1.5

1 1

0.5

0 0
0 1 2 3 4 5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5

(a) (b)
Fig. 3. Matrix reinforcement (a – fibers of small diameter, b – bundles of larger diameter).

Fig. 4. Grinding (a – Alfa stems washed, b – Alfa stems cut 3–4 cm, c – grinding Alfa).

treated case. Which shows the adhesion between the fibers them- 2.4. Preparation of test samples
selves, and therefore a good adhesion will be with the polypropyl-
ene to obtain the granules, due to their interface devoid of waxy An implementation to elaborate samples of different volume
and semi cellulosic materials and treated by NAOH (Fig. 3b and c). fractions of fibers is conducted (10–30%). The fibers are mixed with
 H. Mechakra et al. / Composite Structures 124 (2015) 152–162 155

Fig. 5. Alfa fibers treatment (a – untreated Alfa fibers, b – treated Alfa fibers during 48 h, c – treated Alfa fiber during 24 h).

Fig. 6. Injection samples (a – granules PP/2 h Alfa dried at 105 °C, b – injection press, c – samples PP/Alfa).

polypropylene using a mono-aim extruder to obtain filaments. The
filaments crushing is performed to get granules bound to elaborate
samples by injection (Fig. 6a and b). During the crushing, the ends
of the fibers in the matrix are in contact with ambient air and due
to their hydrophilic character, they absorb the humidity. For that,
this obtained granules are dried at 105 °C in an oven during two
hours before the injection (Fig. 6a). An injection press of Sandretto
Otto type, with injection capacity of 126 cm3 and closure force of
60 tons is used to inject the dried granules.
3. Characterization of composite
3.1. Tensile testing
Traction properties of prepared samples were determined from
traction tests according to the D-638 M norm advocated by the
ASTM. The tests were conducted with a speed of 2 mm/min on
an INSTRON type universal machine of 100 KN capacity, 3382
model. The strain was measured using an extensometer of a
50 mm maximum graduation (Fig. 7). Six material types have been
elaborated. Six samples of each material type were tested (Table 1).
The values of elastic modulus, of the maximum stress and the
strain at breaking are determined for each specimen.
3.2. Acoustic emissions
The process damage of different types of samples is detected by
acoustic emission, used to evaluate the behavior of the fiber/matrix
interface until the fracture (Fig. 7).
3.3. SEM
Observations on the fracture facies from traction tests were
obtained using a scanning electronic microscope (SEM). The

EA Sensor 1

specimen
extensometer

EA Sensor 2

Fig. 7. Tensile test under acoustic control.

156 H. Mechakra et al. / Composite Structures 124 (2015) 152–162

Table 1
Designations of tested materials.
Materials
Neat Polypropylene
Polypropylene charged with 10% Alfa fibers treated 48 h
Polypropylene charged with 20% Alfa fibers treated 48 h
Polypropylene charged with 30% Alfa fibers treated 48 h
Polypropylene charged with 30% Alfa fibers treated 24 h
Polypropylene charged with 30% Alfa fibers untreated
Fig. 9 show that the Young’s modulus reaches a maximum value
of 3555.33 MPa in the case of the treated PP/Alfa-30% during 24 h
Designation and of 3032.19 MPa for that treated during 48 h. The maximum
Neat PP stress increases with the volume fraction (20.87 ± 0.51 to
PP/Alfa-10%-T48H 24.39 ± 0.54); which shows a rigidity transfer between the matrix
PP/Alfa-20%-T48H and the fiber; and therefore a good interfacial adhesion due to the
PP/Alfa-30%-T48H alkaline treatment. The chemical treatment makes the fiber surface
PP/Alfa-30%-T24H
PP/Alfa-30%-UT

Young's Modulus Tensile strenght

25,0
samples were metalized to make them conductive before the SEM
observation. These observations were performed to identify the 3500 24,5
fracture mechanisms of different materials.
24,0

3000
3.4. loading–unloading tests

Tensile Strenght [MPa]

Yound's Modulus [MPa]
23,5

Loading–unloading traction tests were performed on fixed PP/ 23,0

2500
Alfa samples at 30% of volume fibers fraction. This type of test is 22,5
to require a series of cycles by incrementing successive loads to
evaluate Young’s modulus losses and the damage by each cycle 2000
22,0

without fracturing according to the ASTM D-2290 norm.

21,5

4. Results and discussion 1500 21,0

20,5
4.1. Tensile test PP T48H 0%-T48H 0%-T48H 0%-T24H 30%-UT
Neat a_10%- _
lf lfa_2 P/Alfa_3 P/Alfa_3 PP/Alfa
PP/A PP/A P P
Fig. 8 shows the stress-deformation curves for different PP/Alfa Types of specimen
composite and neat polypropylene. The Young’s modulus, the max-
imum stress, the at break stress and deformation for each type of Fig. 9. Impact of chemical treatment in Young’s modulus and tensile strength of
material are mentioned in Table 2. From Fig. 8, clearly appears different type of materials with different fibers reinforcements (%).

the impact of the volume fraction of the reinforcing short fibers

and their chemical treatment on the material rigidity.
Improvement contribution Neat PP
Improvement contribution PP/Alfa_30%_UT
100
25
140

Improvement PP/Alfa_30%-UT [%]

% (PP/Alfa_10%-T48H) 80
Improvement Neat PP [%]

20 120
% (PP/Alfa_20%-T48H)
% (PP/Alfa_30%-T48H)
% (PP/Alfa_30%-T24H) 100
Stress [MPa]

60
15 % (PP/Alfa_30%-UT)
% (Polypropylene)
80
40
10
60

20
5 40

20 0
0 8H 8H 8H 4H T
-T4 -T4 -T4 -T2 %-U
0 2 4 6 10% 20% 30% 30% _30
/ A lfa_ / A lfa_ / A lfa_ / A lfa_ P / Alfa
Strain [%] PP PP PP PP P
Types of composite
Fig. 8. Stress–strain curves for neat PP, PP/Alfa with NaOH treatment fibers and PP/
Alfa with untreated fibers reinforcement. Fig. 10. Young modulus improvement of different composite materials.

Table 2
Main value of mechanical characteristics for different types of composite materials with treated and untreated fibers reinforcement, n number of samples.

Materials Young modulus (MPa) Tensile strength (MPa) Breaking stress (MPa) Breaking strain (%) n
Neat PP 1531 ± 23 24.52 ± 0.2 – – 5
PP/Alfa-10%-T48H 1970 ± 85 20.87 ± 0.51 19.992 ± 0.50 3.92 ± 0.5 6
PP/Alfa-20%-T48H 2305 ± 159 21.58 ± 0.15 20.45 ± 0.42 3.84 ± 0.34 6
PP/Alfa-30%-T48H 3042 ± 125 23.27 ± 0.21 22.17 ± 0.29 3.11 ± 0.72 8
PP/Alfa-30%-T24H 3555 ± 183 24.39 ± 0.54 22.60 ± 0.92 3.08 ± 0.51 8
PP/Alfa-30%-NT 2732 ± 168 22.46 ± 0.58 20.59 ± 0.69 2.23 ± 0.23 8
 H. Mechakra et al. / Composite Structures 124 (2015) 152–162 157

waterproof and removes the non-cellulosic components such as 4.2. Assessment of damage by acoustic emission
wax, pectins and hemi cellulosic lignin [4]. The 24 h chemical
treatment duration gave better results than that of 48 h (Fig. 8). In tensile tests on the elaborated bio-composite samples (PP/
Defibration bundles allows a surface chemical treatment of the Alfa-30% treated during 24 and 48 h), two piezoelectric sensors
entire fiber and the reduction of the fiber/matrix section to that for collecting acoustic emission signals generated by the material
of bundles/matrix (Fig. 3), thus increasing the homogenization of damage process are fixed on the tested sample. Acoustic emissions
the composite and its rigidity (Fig. 9). are recorded by an acoustic sensor (Fig. 7); in order to get informa-
To this end, we got an increase of the Young’s modulus of tion on the initiation and propagation of the structure damage.
1970 ± 85 to 3555.33 MPa, representing a ratio from 19.69% to This treatment method allowed the evaluation, for each range
132.33% compared to the neat polypropylene; and from of amplitudes, of a mechanism of structure damage different than
3042 ± 125 to 3555 ± 183 MPa, which represents a ratio from that of the composites materials with organic matrix synthetic
11.33% to 30.45% compared to the 30% reinforced PP/Alfa of the reinforcement. Fig. 11a and b shows the damage process by the
non treated fibers (Fig. 10). The mechanical characteristics increase acoustic emission of the different materials composite (PP/Alfa-
as a function of the volume fraction of 10–30% reinforcement, and 30%) with an evolution of the acoustic signal amplitude with
with respect to the chemical treatment and to its duration (see respect to time. Fig. 11a0 and b0 shows the evolution of the number
Table 3). of hits according to time.
The results show that the scatter plot of the rupture process of
the matrix, of the loosening and of the fiber breakage in the case of
the PP/Alfa-30% of a 48 h treatment (Fig. 11b) is more dense than
Table 3
that of the PP/Alfa-30% of a 24 h (Fig. 11a). The total duration of
Impact of chemical treatment durations and fibers reinforcement (%) in mechanical
characteristics samples. the rupture process in the case of PP/Alfa-30% of a 48 h treatment
(Fig. 11b) is 40 s (from 52 ths to 92 ths) while that of PP/Alfa-30% of
Types of specimen Tensile modulus (MPa) Improvement (%)
a 24 h treatment (Fig. 11a) is 54 s (from 42 ths to 96 th s).
Neat PP 1531 ± 23 100 The isolated points that are not considered (Fig. 11a and b) are
PP/Alfa-10%-T48H 1970 ± 85 28.67
defects related to the air pockets during the injection. This gain in
PP/Alfa-20%-T48H 2305 ± 159 50.56
PP/Alfa-30%-T48H 3042 ± 125 98.69 breaking time which reflects the increase of the rigidity of the
PP/Alfa-30%-T24H 3555 ± 183 132.22 loaded material by the same volume fraction of 30% of the Alfa
PP/Alfa-30%-NT 2732 ± 168 78.45 fibers, is principally related to the treatment duration in the basic
medium.

Amplitude Number of hits

70 250
Matrix cracking Matrix cracking
65 Fibre matrix debonding Fibre matrix debonding
Fibre failure 200 Fibre failure
60
PP/Alfa_30%-24h
Amplitude (dB)

Number of hits

55
150

50

100
45

40
50
35

30 0
0 10 20 30 40 50 60 70 80 90 100 0 10 20 30 40 50 60 70 80 90 100
AFRP

Time (s) Time (s)

(a) (a')
70 250
Matrix cracking Matrix cracking
65 Fibre matrix debonding Fibre matrix debonding
Fibre failure 200 Fibre failure
PP/Alfa_30%-48h

60
Amplitude (dB)

Number of hits

55
150

50

100
45

40
50
35

30 0
0 10 20 30 40 50 60 70 80 90 100 0 10 20 30 40 50 60 70 80 90 100
Time (s) Time (s)
(b) (b')
Fig. 11. Amplitude distribution of acoustic emission signals from a function of time for the different materials (PP/Alfa 10–30% treated 48 h-24 h).
158 H. Mechakra et al. / Composite Structures 124 (2015) 152–162

The fibers breaking begins from 59.5 s of the total test duration
for the 48 h PP/Alfa-30% treatment (Fig. 11b0 ), while it starts from
64s for the 24 h PP/Alfa-30% treatment (Fig. 11a0 ). This 4.5 s gain
expresses an additional strength mainly related to the good surface
treatment of the fibers and the decrease of the number of bundle
residues during their process defibration and their containing
impurities which facilitate the loosening of the fibers during the
traction. It appears from these observations that the interfacial
fiber/matrix adhesion of the 24 h PP/Alfa-30% composite is of a bet-
ter quality compared to that of the 48 h PP/Alfa-30%.
The question that arises is whether this acoustic emission is
really related to these surface treatment interpretations and

Pullout Fiber tearing

fibers
Air pocket and cavities Ball rolling matrix Fiber cracking

Pullout fibers
PP/Alfa-30%-UT

(a) (b)

Pullout of ball rolling matrix

Poor adhesion
fiber matrix

Fiber breakage

Cavities and void Bad adhesion fiber matrix

(c) (d)

Fibers distributions
Fiber tearing
Matrix cracking
Good adhesion

Void and Cavities

Pull out Fiber

PP/Alfa-30%-T48H

(e) (f)

Fibers breakage

Good
adhesion fiber

Fiber breakage

(g) (h)
Fig. 12. Scanning electronic micrograph of tensile fractured PP/Alfa-30% (untreated, treated = 48 h and 24 h).
 H. Mechakra et al. / Composite Structures 124 (2015) 152–162 159

Pullout fibers Pull out of Matrix

Void

Matrix cracking
PP/Alfa-30%-T24H

Fibers

(i) (j)

Breakage fiber Matrix cracking Good fibers matrix

adhesion
Pullout fibers in
lateral position
Good
adhesion
matrix in
fiber Matrix cracking

Good fiber matrix

adhesion

(k ) (l)

Fig. 12 (continued)

reduction of the bundles, or to another phenomenon. Thus, to
reach there and answer this question, microscopic SEM observa-
tions of the fracture facies samples were highlighted.
4.3. Scanning electron microscopy (SEM)
The scanning electronic microscopy is a current method for
analyzing the fiber/matrix adhesion level. Many studies were con-
ducted to assess the link (the interface) fiber/matrix and the chem-
ical impact applied on the fibers. The analysis of the morphological
characteristics of the fiber surfaces, the effect of the chemical treat-
ment and also the aspect of the fracture surfaces observed by the
SEM is an important tool for determining the cause of the fracture
beginning in the matrix, the reinforcement, the interfacial adhe-
sion and the failure process in the materials (hydrophilic/
hydrophobic).
Fig. 12 shows SEM pictures of the fracture after the traction test
specimens PP/Alfa-30% non-treated and PP/Alfa-30% treated dur-
ing 48H and 24H. The reinforced PP/Alfa with non treated fiber
shows the clearly visible presence of cavities and the fiber loosen-
ing under the applied stress; the fibers are easily melamine and
extracted from the matrix. This indicates a poor adhesion between
the fiber and the matrix (Fig. 12a–c). The polypropylene is in drop-
lets form on the non treated fiber surface, due the hydrophilic mor-
phology of the fibers and the hydrophobic component of the
polymer matrix (Fig. 12b).
A break in the interface is also observed (inter facial ungluing or
adhesive fracture) (Fig. 12d). These interface ungluing then generate
a loosening followed by a fiber fracture (Fig. 12a). This may be due to
the interface quality which can be attributed to the physicochemical
properties of the matrix and to its ability to adhere to the fiber. We
also can see the degraded state of the Alfa fiber (Fig. 12b–d).
The morphology of the two composite surfaces with treated
fibers at 48H and 24H presents a reduced number of loosened
fibers in the structure, which shows the improvement of the sur-
face state of the fibers with the alkaline treatment, the elimination
of non-cellulosic components and a better affinity of the fiber/
matrix interface with the reduced number of gaps (vacuum) in
the structure, which take place during the samples injection, and
which is a major indicator of material damage and crack initiation
(Fig. 12e–i). The 48 h fiber treatment shows the presence of a num-
ber of broken fibers with a torn structure; indicating that the dura-
tion of the alkaline treatment for 48H in a basic environment
facilitates the fiber damage (Fig. 12g and h).
NaOH treatment significantly improves the link between the
fiber and the matrix. The 24 h duration treatment shows, on the

Table 4
Mechanical properties of PP/Alfa with 30% content treated and untreated fibers for different cycles.

Materials PP/Alfa-30%-UT PP/Alfa-30%-T48H PP/Alfa-30%-T24H

Cycles number E (MPa) e (%) r (MPa) E (MPa) e (%) r (MPa) E (MPa) e (%) r (MPa)
Cycle 1 2744 0.17 4.52 3009 0.16 4.87 3324 0.15 4.87
Cycle 2 2724 0.38 8.99 2985 0.37 9.72 3155 0.32 9.72
Cycle 3 2590 0.62 13.49 2851 0.64 14.57 2811 0.57 14.57
Cycle 4 2312 0.96 17.97 2316 1.07 19.42 2718 0.98 19.42
Cycle 5 2197 1.58 22.47 2091 1.99 24.03 2071 2.05 24.28
160 H. Mechakra et al. / Composite Structures 124 (2015) 152–162

SEM pictures, the loosening process reduction of the fibers during 4.4. Loading–unloading tests
the traction, and a better inter facial adhesion, just as the matrix
rupture without a fiber rupture and the fiber rigidity growth The loading–unloading tests are performed to determine the
(Fig. 12k, l, j). mechanical properties of each type of material compared to the
Fig. 12j, l, k show that the surface of the 24 h treated fibers and mechanical properties of its first cycle. They are shown in Table 4.
their inter-facial adhesion are better than the 48 h treated ones Fig. 13 presents the loading–unloading loops of each material
(Fig. 12g and h). (untreated and treated PP/Alfa with a volume fraction at 30%). Each
test has an elastic field. Each mechanical discharge causes residual
strains. After each one, we observe hysteresis loops. The loops bend
after each new test and a slope decrease measured at each unload-
ing explains the loss of rigidity due to the presence of damage.
PP/Alfa_30%-UT PP/Alfa_30%-T48H PP/Alfa_30%-T24H In determining the loss of rigidity in Fig. 14 of the different
30 materials (48 h untreated PP/Alfa-30%wt and 24 h treated PP/
Alfa-30%wt), we grouped the stiffness loss curves E/E0 according
to the maximum stress rmax. It is noticed that the rigidity loss
25
changes slightly; the 48 h loaded PP/Alfa-30%wt with treated fibers
retains about 58% of its initial modulus after loading. The 24 h
20 loaded PP/Alfa-30%wt with treated fibers retains about 69% of its
Stress (MPa)

initial modulus. It is concluded that the rigidity losses are 31%

and 42% respectively for the 24 h treated PP/Alfa-30% and the
15
48 h untreated PP/Alfa-30% (Table 5). Fig. 15 shows the evolution
of the stiffness based on the number of cycles for PP/Alfa with
10 30% of treated and untreated fibers.

4.5. Confrontation of results

5

For an objective results assessment of implementing the Alfa

0 short fibers preparation, of the optimization of the chemical treat-
0,0 0,5 1,0 1,5 2,0 2,5 3,0 ments and mechanical characterization, a confrontation is made
Strain (%) with the previous research work (Table 6) of the composite

Fig. 13. Charge–discharge test of PP/Alfa-30% content treated and untreated fibers.

PP/Alfa_30%-UT PP/Alfa_30%-T24H PP/Alfa_30%-T48H

PP/Alfa_30%-UT PP/Alfa_30%-T24H PP/Alfa_30%-T48H
3500

1,0
Young's Modulus [MPa]

0,9 3000
E/E0 [MPa]

0,8

2500

0,7

0,6 2000
0 5 10 15 20 25 0 1 2 3 4 5
Maximum Stress [MPa] Cycles Number

Fig. 14. Loss of stiffness as function of tensile strength for PP/Alfa with 30% of Fig. 15. Evolution of the stiffness based on the number of cycles for PP/Alfa with
fibers. 30% of treated and untreated fibers.

Table 5
Loss of Young’s modulus of untreated PP/Alfa as maximum Stress rmax.

Types of Sp PP/Alfa-30%-T48H PP/Alfa-30%-T24H PP/Alfa-30%-UT

cycles Nbr E (MPa) E/E0 (%) E (MPa) E/E0 (%) E (MPa) E/E0 (%)
Cycle 1 3009 ± 1.414 100 3324 ± 32.03 100 2744 ± 118.08 100
Cycle 2 2985 ± 24.74 99.20 3155 ± 32.17 94.91 2724 ± 137.88 99.27
Cycle 3 2851 ± 9.192 94.74 2811 ± 28.14 84.56 2590 ± 74.95 94.38
Cycle 4 2316 ± 222.05 76.96 2718 ± 34.94 81.76 2312 ± 19.09 84.25
Cycle 5 2091 ± 140.71 69.49 2071 ± 2.05 62.30 2197 ± 113.84 80.06
 H. Mechakra et al. / Composite Structures 124 (2015) 152–162 161

Table 6
Summary of mechanical properties of composite with plant fibers reinforcements.

Vf (%) Young’s modulus Tensile strength Type of Nature of fibres Type of Chemical treatments Reference
E [MPa] [MPa] fibre matrix
30 3555 ± 183 24.39 ± 0.54 Alfa Short PP NaOH 24 h (1.6 mol/l) Present work
30 3042 ± 125 23.27 ± 0.21 Alfa Short PP NaOH 48 h (1.6 mol/l) Present work
– 257 25.80 Agave Short 3 mm Epoxy NaOH (5%) 30 min K. Mylsamy (2011) [6]
– 238 21 Agave Short 7 mm Epoxy NaOH (5%) 30 min K. Mylsamy (2011) [6]
– 229 17.80 Agave Short 10 mm Epoxy NaOH (5%) 30 min K. Mylsamy (2011) [6]
5–30 1110–1663 31.82–29.01 Alfa Short PP NaOH 48 h (1.6 mol/l) F.Z. Arrakhiz (2013) [12]
5–30 1186–1489 33.92–27.92 Coir Short PP NaOH 48 h (1.6 mol/l) F.Z. Arrakhiz (2013) [12]
5–30 1080–1469 30.82–30.45 Bagasse Short PP NaOH 48 h (1.6 mol/l) F.Z. Arrakhiz (2013) [12]
20 1230 31 Alfa Short PP NaOH 48 h (1.6 mol/l) F.Z. Arrakhiz (2012) [11]
20 940 32.08 Alfa Short PP Etherification F.Z. Arrakhiz (2012) [11]
20 1405 32.08 Alfa Short PP Esterification F.Z. Arrakhiz (2012) [11]
10 1408 ± 28 – Alfa Long 7 cm UPR Styrène (S) A. Bessadok (2009) [9]
10 1465 ± 37 – Alfa Long 7 cm UPR Maleic Anhydride A. Bessadok (2009) [9]
40 3002 ± 45 79 ± 1.8 Sisal Long 3 cm PR NaOH 30 min (5%) P.A. Sreekumar (2009) [8]
40 2431 ± 28 70 ± 1.8 Sisal Long 3 cm PR Benzoylation P.A. Sreekumar (2009) [8]
40 2697 ± 14 72 ± 1.5 Sisal Long 3 cm PR KMnO4 P.A. Sreekumar (2009) [8]
40 2444 ± 45 76 ± 2.2 Sisal Long 3 cm PR Couplage de type silane P.A. Sreekumar (2009) [8]
30 2280 ± 34 56.9 ± 1.6 P100 Long UPR NaOH (5%) 30 min D. Shanmugam (2013) [14]
30 2840 ± 34 60.3 ± 1.59 PL75J25 Long UPR NaOH (5%) 30 min D. Shanmugam (2013) [14]
30 2450 ± 40 64.3 ± 1.95 PL50J50 Long UPR NaOH (5%) 30 min D. Shanmugam (2013) [14]
30 3780 ± 60 83.3 ± 5.13 PL25J75 Long UPR NaOH (5%) 30 min D. Shanmugam (2013) [14]
30 5070 ± 20 77.1 ± 3.27 J100 Long UPR NaOH (5%) 30 min D. Shanmugam (2013) [14]
10–40 1106–1722 34–81 Flax Nonwoven PP Protein coating (Zein type) M.J. John (2009) [7]

mechanical characteristics such as vegetable reinforcement Alfa
[11,12], agave [6], jute, [13] coir and bagasse [12], sisal [9] and
the flax [7,14].
One of the techniques used to achieve this goal are the plant
fiber chemical treatments, among them the alkaline treatment
[11,12,15], which is the most common for techno-economic rea-
sons. [11,16] Other techniques are more complex to implement
because of the cost ant the realization. Several studies were con-
ducted on the alkaline treatment to modify the fiber surface. From
Arrakhiz et al. [12](Table 4), we establish an improvement of the
Young’s modulus of the PP/Alfa 5% at 30% of short treated Alfa
fibers with NaOH from 1501 to 1663 MPa. For the same chemical
treatment protocol and volume fraction of croie short fibers or
bagasse as reinforcement, the Young’s modules are E = 1186–
1489 MPa and E = 1072–1446 MPa.
With an Etherification and Esterification treatments, Arrakhiz
et al. [11]found an improvement for PP/Alfa-20% Young modulus
of Alfa short fibers reinforcement of 960 and 1405 MPa and of
1220 MPa with an NAOH treatment.
With a styrene (S) and an anhydride Maliek treatment Bessadok
et al. [9] found the Young’s modulus of PP/Alfa-10% of long fibers
(7 cm) equal to 1408 ± 28 and 1465 ± 37 MPa. Sreekumar et al.
[8] used as each type of treatment, NaOH, benzoylation, KMnO4
and the silane type coupling. They found an improvement of the
Young’s modulus of the UPR/Sisal-40% long fiber (3 cm) of
3002 ± 45, 2431 ± 28, 2697 ± 14 and 2444 ± 45 MPa.
Shanmugam and Thiruchitrambalam [14] used the same NaOH
treatment (5%) 30 min with the same volume fraction of 30% of
Jute or Palm Leaf long fibers. They found the Young modules of
5070 ± 0.2 and 2280 ± 0.34 MPa. For three combinations of these
two fiber types (PL75J25, PL50J50, PL25J75), the Young’s modules
are 2840 ± 0.34, 2450 ± 0, 4 and 3780 ± 0.6 MPa. These mechanical
characteristics are high but obtained with UPR.
With a (type Zein) protein coating on Non Woven flax fiber rein-
forcement of the PP, for a volume fraction of 10–40%, John et al. [7]
found a 1106–1722 MPa Young’s module.
In our study the PP/Alfa Young’s modulus with a 30% rate of Alfa
24 h treated fiber reinforcement is 3555 ± 183 MPa. Except for the
thermoset matrix composites reinforced with long fibers of jute or
palm leaf, or their combination, which is in fact more expensive; all
the other studies showed lower characteristics.
5. Conclusion
This paper deals with the mechanical fatigue properties of the
composite material obtained by an extraction implementation of
fresh short fibers from Alfa bundles in two stages. The first crush-
ing is devoted to obtaining the bundles and avoiding damage by
centrifugation of the architecture and the inter-cellulosic fiber
linkages by crushing and random shear distortions such as the
fibrillar angle.
The second step is to reverse the bundles and grinding for more
defibrating and avoiding their sticking. The main idea is to obtain a
maximum grinding bundles to increase the interfacial adhesion
surface fiber/matrix (decrease of the important bundles diameters
for the same volume fraction). The whole is cleaned from damaged
bundles and dust, which allows a significant gain in terms of the
composite weight. Most of the previous studies used the bundles
reinforcement which may contain impurities (lignin, materials,
waxes, hemicelluloses); thus the used chemical treatments will
be superficial and partial since they will not be able to reach cer-
tain parts of the bonded fibers. Which, under load, results in an
important bundle loosening defect.
From a large topography of fibers chemical treatments of previ-
ous studies, an optimization of alkaline chemical treatment of dif-
ferent durations was used for the fibers over their entire surfaces,
and kept dry after, until their injection in various volume fractions.
An analysis of the samples fatigue behavior until fracture, under
the acoustic control and an SEM morphology visualization of the
treated and non treated fibers and of inter-facial characteristics,
showed the impact of the latter on the important increase in the
Young’s modulus from 28.67% to 132.22% compared to the virgin
PP, and from 11.34% to 30.14% of the tensile strength compared
to the non treated fibers: thus a high rigidity.
Except for the thermoset matrix composites reinforced with
long fibers of jute or palm leaf or their combination which is more
expensive to perform, all previous studies showed lower mechan-
ical characteristics.
162 H. Mechakra et al. / Composite Structures 124 (2015) 152–162
Acknowledgments
The authors would like to acknowledge for experimental sup-
port, Engineering and Materials Science Laboratory of Reims
University of Champagne-Ardenne and Roberval Laboratory of
Compiegne University of Technology, France.
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