Materials and Design 89 (2016) 839847

Contents lists available at ScienceDirect

Materials and Design

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

Characterisation of natural cellulosic bre from Pennisetum purpureum

stem as potential reinforcement of polymer composites
M.J.M. Ridzuan a, M.S. Abdul Majid a,, M. Afendi a, S.N. Aqmariah Kanaah a, J.M. Zahri b, A.G. Gibson c
a
b
c

School of Mechatronic Engineering, Universiti Malaysia Perlis, Pauh Putra Campus, 02600 Arau, Perlis, Malaysia
Mechanical Engineering Department, Sultan Abdul Halim Mu'adzam Shah Polytechnic (POLIMAS), Bandar, Darul Aman, 06000 Jitra Kedah, Malaysia
School of Mechanical and Systems Engineering, Stephenson Building, Newcastle University, Newcastle Upon Tyne NE1 7RU, UK

a r t i c l e

i n f o

Article history:
Received 28 May 2015
Received in revised form 12 October 2015
Accepted 13 October 2015
Available online 22 October 2015
Keywords:
Pennisetum purpureum bre
Mechanical properties
Infrared spectroscopy
Thermogravimetric analysis
Natural bre

a b s t r a c t
Pennisetum purpureum (PP) bres were comprehensively characterised to assess their potential as reinforcing
materials in polymer composites. The bres were treated with 5, 7, 10, 12, and 15% sodium hydroxide wt.% concentration for 24 h. The bres were subjected to single bre tensile tests, thermo-gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The average diameter of
the untreated bres was 0.24 0.02 mm, and the treated bres had an average diameter of less than 0.21
0.03 mm, yielding a 1245% reduction in the diameter. The moisture content of the treated bres decreased as
the concentration of the alkali increased. The morphological observation demonstrated that as the alkali concentration increased, the bre becomes more compressed due to collapse the cellular/lumen structure, the void content decreased, and its surface became rougher. The 5% alkali-treated bre achieved an average maximum
ultimate tensile stress of 141 24 MPa. Young's modulus on the other hand, decreased from an average of
5.68 0.14 GPa for untreated bre to only 0.55 0.17 GPa as the alkali concentrations increased from 5 to 15%.
2015 Elsevier Ltd. All rights reserved.

1. Introduction
The current growth in environmental awareness has generated increasing interest in the use of natural bres as alternative reinforcement
materials for polymer composites. This is largely owing to their low environmental impact, low cost, and relatively good specic properties.
Scientists have been striving to develop biodegradable composites
using renewable agro-based materials [1]. Natural bres derived from
plants demonstrate great potentials for use in plastic, automotive, and
packaging industries because of their excellent characteristics such as
low density, high specic stiffness, good mechanical properties, biodegradability, eco-friendliness, toxicologically harmless, good thermal
and acoustic insulation [2,3]. In addition, these cellulosic bres can reduce the overall material costs than the starting polymer [4]. Comprehensive reviews conducted by numbers of publications [510] have
outlined the differences of natural bres with regards to their mechanical properties and its applications. Several authors documented the use
of natural bres such as bamboo [10], ax [11], coir [12], arundo donax
(giant reed) [13], okra [14], jute [15,16], wheat straw [17,18] and alfa
[19] as reinforcement in composite materials.

Corresponding author.
E-mail addresses: ridzuanjamir@unimap.edu.my (M.J.M. Ridzuan),
shukry@unimap.edu.my (M.S. Abdul Majid), afendirojan@unimap.edu.my (M. Afendi),
aqmariah@unimap.edu.my (S.N. Aqmariah Kanaah), zahri@polimas.edu.my (J.M. Zahri),
geoff.gibson@newcastle.ac.uk (A.G. Gibson).

http://dx.doi.org/10.1016/j.matdes.2015.10.052
0264-1275/ 2015 Elsevier Ltd. All rights reserved.

However, there are concerns regarding the attributes of natural bres such as their hydrophilic nature, high moisture absorption, poor reactivity, and poor compatibility with polymeric matrices, all of which
inuence their mechanical properties [2022]. The hydrophilic nature
of natural bre is known to produce weak interfacial adhesion in
polymer-matrix composites [23]. The type of natural bre can also affect
the biological performance of the composites, for example, a composite
manufactured from abaca bre has a much greater moisture content
compared to ax reinforced composites [24]. These problems can be
rectied through modication such as alkali treatment to enhance the
interfacial adhesion between natural bres and composite matrices, in
addition to enhancing the mechanical, physical, and thermal properties
of the bres [25]. Other modications during acetylation can modify the
surface of the bres and enhance their hydrophobicity [24].
Pennisetum purpureum bre, also locally known as Napier grass
(Rumput Gajah), is composed of 46% cellulose, 34% hemicellulose, and
20% lignin [26]. The purpose of the alkali treatment is to remove the
hemicelluloses, split the bres in the brils, and produce a closely
packed cellulose chain owing to the release of the internal strain,
which consequently improves the mechanical properties of the bre
[27]. Following the alkali treatment, the brillation of the bres also increases the effective surface area available for wetting by the resin, and
enhances the bonding between the bre-matrix interfaces within the
polymer composites. The alkali treatment also breaks the hydrogen
bonds and increases the number of free hydroxyl groups of the bre,
thus increasing the bre reactivity [28]. The alkali treatments of various

840

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

lignocellulosic bres such as jute, hemp, kapok, sisal [29], banana [30],
coir [31], and Napier grass [32] have been previously investigated.
Haameem and colleagues recently determined that the maximum ultimate tensile stress of P. purpureum single bres was achieved with
10% alkali treatment. However, this is contradictory to the results of
Reddy et al. which determined that the maximum ultimate tensile
stress of P. purpureum bre was achieved with 5% alkali treatment
[26]. The modulus of jute bres improved by 12%, 68%, and 79% following 4, 6, and 8 h of alkali treatment, respectively. The tenacity of the bre
improved by 46% following alkali treatment for 6 and 8 h, and the breaking strain was reduced by 23% following an 8 h treatment. [33]. Liu et al.,
Rao et al. and Thakur et al. all demonstrated that the natural bres exhibit great potential for use as an alternative to articial glass and carbon bres during the production of thermosetting or thermoplastic
composites [3436].
In this paper, a comprehensive characterisation of P. purpureum bres including their mechanical and thermal properties, as well as
their physical and morphology prior to and following the alkalitreatment are reported. To the best of our knowledge, this is the rst
time an extensive characterisation of this bre has been conducted
and this study should provide new information to the research
community.
2. Materials and methods
2.1. Extraction of P. purpureum bres
P. purpureum plants were harvested from a local plantation in Bukit
Kayu Hitam, Kedah, in northern peninsular Malaysia. Following the
water retting process, the bres were manually extracted from the
stem internodes [37]. To separate the bre strands, the stems were initially cleaned and subsequently crushed into small parts with a mallet.
Subsequently, the short plant stems were immersed under running
tap water for a few weeks to facilitate the separation process. Finally,
the bres were cleaned with distilled water and subsequently dried
under the sun to remove the moisture content [38]. The P. purpureum
plants and its extracted bres are shown in Fig. 1.
2.2. Alkali treatment
To treat natural bres, previous researchers have employed alkali
(sodium hydroxide) solutions of various percentages (2, 5, 7, 10, and
15%) and treatment for various immersion times (1, 3, and 24 h) [39].
Reddy et al. used alkali solutions of 2 and 5% to treat P. purpureum bres
at room temperature [26]. Considering this information, alkali solutions
of 5, 7, 10, 12, and 15% were applied to the P. purpureum bres for 24 h at
room temperature during this investigation. A liquor ratio of 40:1 was
used to remove the hemicelluloses and surface impurities of the bre.

Finally, the bres were cleaned using distilled water and dried at
room temperature.
2.3. Physical measurement
The minimum and maximum diameters, average length, and average mass of both the treated and untreated bres are presented in
Table 1. Prior to tensile testing of the single bres, their diameter, length,
and mass were measured to ensure that the properties of the specimens
were recorded for analysis purposes. Fibres of 150170 mm in length
were selected for the untreated and alkali-treated bres. The mass of
the bres was between 0.00220.0028 g. The diameter of the bre
was measured using a metallurgical microscope (MT8100) with a magnication of 50 . Twenty bre samples were randomly selected for
each alkali concentration, and the diameter of each bre was measured
in three positions, as shown in Fig. 2 [13]. Following the alkali treatment,
the average diameter relating to each alkali concentration was calculated in order to determine the variation in the diameter.
2.4. Determination of moisture content
Bundles of single bres bound together from each alkali concentration were weighed and dried in an air oven at 100 C for 24 h, weighed
using a balance with 4 decimal places accuracy (mg) and recorded as
Md. The samples were then placed in humidity chamber at 70% relative
humidity (RH) at 21 C for 24 h [40]. The humidity chamber was set up
using distilled water and held at room temperature. Subsequently, the
bres were weighed again after exposure in humidity and recorded as
Mh. Finally, the moisture content was determined using Eq. (1):
Moisture content MC

Mh Md
 100%
Mh

where Mh = mass of the sample after exposing it in humidity and Md =

mass of the dried sample.
2.5. Single tensile test
The tensile properties of the bre were determined through the single bre tensile testing method in accordance with ASTM D3822-07
[41]. Prior to the test, the treated and untreated bres were dried in
an oven at 100 C for 24 h [26]. The treated and untreated bres were
weighed using an analytical balance and the length of the bres was
measured. The average diameters of the bres were used to estimate
the cross-sectional areas of the bres. The bre was mounted and
glued onto a tab-shaped piece of paper with a gauge length greater of
100 mm. For each alkali concentration, twenty bre samples were prepared, measured and subjected to tensile testing using a micro universal
testing machine (INSTRON 5848) with a crosshead speed of 1 mm/min

Fig. 1. (a) Pennisetum purpureum grass and (b) the extracted P. purpureum bres.

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

841

Table 1
Physical properties of treated and untreated Pennisetum purpureum bres. (20 samples for
each concentration).
Concentration

Minimum
diameter (mm)

Maximum
diameter (mm)

Average
length (mm)

Average
mass (g)

Untreated
5%
7%
10%
12%
15%

0.21
0.16
0.14
0.13
0.12
0.12

0.27
0.26
0.25
0.18
0.15
0.16

158
163
154
154
155
158

0.0025
0.0024
0.0028
0.0025
0.0023
0.0022

and a load cell of 2 kN. The stress was then computed from the ratio of
the force and estimated cross-sectional area.
2.6. Fourier transforms infrared spectroscopy (FTIR)
Fig. 3. Variation in average diameter of bres.

The Perkin Elmer Spectrum 400 FTIR spectrophotometer was used to

derive the FTIR spectra of the untreated and treated P. purpureum bres.
All the spectra were recorded in the wavenumber range of
6504000 cm1, operating in ATR (attenuated total reectance) mode.
2.7. Thermo-gravimetric analysis (TGA)
The thermal stability behaviour of the P. purpureum was assessed by
TGA using the Gas Controller GC 200 STAR System analyser (Model
METTLER TOLEDO). To prevent oxidation, the TGA analyses were performed under a nitrogen atmosphere at a ow rate of 20 ml/min. The
samples, weighing 68 mg, were crushed and placed in an alumina crucible to avoid any temperature variation in the thermocouple measurements. The heating rate was maintained at 10 C/min during heating
between 30 and 500 C [32].
2.8. Surface morphology of P. purpureum by scanning electron microscopy
(SEM)
The surface and cross-sectional morphologies of the untreated and
treated P. purpureum bre strands were examined using an SEM
(HITACHI Model TM3000). The scanning images were obtained with
an accelerating voltage of 15 kV and magnication of 10001200 .
The layers were not surface coated prior to scanning.
3. Results and discussion
3.1. Effect of alkali treatment on diameter variation

smaller than the untreated bres. The average diameter of the untreated
bres was 0.24 0.02 mm, and the treated bres had an average diameter of less than 0.21 0.03 mm. Following the alkali treatment, there
was a 1245% reduction in the diameter. This reduction is owed to the
removal of the amorphous components, collapse the cellular/lumen
structure and the reduction in the hemicelluloses fraction as a result
of the alkali treatment [26]. The hemicelluloses are amorphous and hydrophilic, and they are soluble in alkali solution [43]. Furthermore, lignin is amorphous and hydrophobic in nature, and also soluble in alkali
solution [43]. Therefore, both lignin and hemicelluloses on the bre surfaces can be removed by the alkali treatment. In our study, the chemical
treatment resulted in a smaller and a more uniform diameter.
The bres treated with a higher percentage concentration of alkali
solution exhibited improved removal of lignin and hemicelluloses.
There are no specic standards regarding the percentage concentration
of alkaline solution for use in the chemical treatment of natural bres.
Hence, most studies regarding the chemical treatments of natural bres
are based on trials, which use varying amounts of alkali solutions. Our
study on P. purpureum bres demonstrated that the bres treated
with 5 and 7% alkali solutions exhibited a better physical appearance
than the untreated and other treated bres. The untreated bre was observed with surface impurities whilst higher than 10% treated bres revealed damage texture. Reddy et al. investigated the treatment of
P. purpureum bres with 25% alkali solution and determined that as
the percentage concentration of the alkali solution increased, the diameter of the bre decreased [26].

The diameter variation for the untreated and treated bres is shown
in Fig. 3. It can be observed that the diameters of the treated bres are

Fig. 2. Diameter measurement of a single Pennisetum purpureum bre using a standard optical microscope.

Fig. 4. Moisture content of Pennisetum purpureum bres.

842

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

3.2. Moisture content

Moisture content of untreated and treated P. purpureum bres are
presented in Fig. 4. It can be observed that the untreated bre exhibits
the highest moisture content of 13.9 1.1%. The moisture content
was reduced by over 48%, 7.2 1.0 and 7.1 0.9% for 5 and 7%
alkali-treated bres respectively. The moisture content was further reduced to 3.7 0.8, 3.1 0.7 and 1.7 0.5% for 10, 12 and 15% alkalitreated bres respectively. The reduced moisture content of the bres
is related to the fact that the treatment had caused the removal of hemicelluloses which reduced the amount of bonding sites and compressed
the lumen structure of bres. Moisture content is a very important parameter as it affects the dimension and physical properties of the bres.
They inuence the dimensional stability, electrical resistivity, tensile
strength, porosity and swelling behaviour of natural bre reinforced
composites [44]. Low moisture content of P. purpureum bres is preferable in fabricating P. purpureum bre reinforced polymer composites
due to their lesser ability to hold up water molecules.
3.3. Mechanical properties of P. purpureum bre
Table 2 shows the mechanical elastic properties of untreated and
alkali-treated P. purpureum bres. The 5% alkali-treated bre exhibits
the highest ultimate tensile stress, followed by 7% treated, untreated,
10% treated, 12% treated, and 15% treated bres, respectively. A maximum ultimate tensile stress of 141 24 MPa was achieved with the
5% alkali treatment; this stress was conrmed by a previous study
[26]. The ultimate tensile stress signicantly increased from 73
6 MPa for the untreated bre to 141 24 MPa for 5% alkali-treated
bre, which is an increase of over 90%. However, with a further increase
in the alkali concentration to 7%, the ultimate tensile stress of the bre
decreased to 79 14 MPa; however, the ultimate tensile stress of this
bre was 8% higher than that of the untreated bres. The 10 and 12%
alkali-treated bres exhibited ultimate tensile stress of 50 7 and
49 9 MPa, respectively. The bre treated with 15% alkali exhibited
the lowest ultimate tensile stress, 31 5 MPa. These ndings conrmed
that the bre treated with 5% alkali exhibited a higher ultimate tensile
stress than the untreated bre and the other treated bres.
The inconsistencies in the length, mass, and diameter of all the
tested samples consequently affect the percentage strain at break of
the bres with different respective strength. The results demonstrate
that the untreated bre exhibited the lowest strain at break, 1.40
0.23%. The strain at break drastically increased by more than 90% to
reach approximately (2.30 0.18)(2.27 0.21) % for the 5 and 7%
alkali-treated bres. Subsequently, the strain at break exhibited a significant increase to 4.43 0.25 and 4.81 0.38% for the 10 and 12%
alkali-treated bres respectively. Finally, the maximum strain at
break, 6.40 0.22%, was achieved with the 15% alkali-treated bre.
Other researchers also found that treated bres exhibited an increased strain at break [26,45].
Furthermore, there was a reduction in the Young's modulus of the
treated bres. The untreated bre exhibited the highest Young's modulus of 5.68 0.14 GPa. The 5, 7, 10, 12, and 15% alkali-treated bres exhibited values of 4.86 0.22, 3.77 0.11, 1.00 0.17, 1.02 0.32 and

0.55 0.17 GPa, respectively. Considering these results, the alkali treatment seems to enhance the elasticity of the bre and hence a larger
strain to failure can be achieved. Goda et al. produced similar results
for ramie bres; the elastic modulus decreased as the alkali treatment
concentration increased [45]. Fig. 5 shows the stressstrain responses
for selected of untreated and alkali-treated P. purpureum bres.
The treated bres exhibit a higher ultimate tensile stress and strain
to failure because of the changes in the cellulose crystallinity following
the 5 and 7% alkali treatments [24]. The process involves the removal
of the weak amorphous component so that the bre only retains the
crystalline components. The removal enables the bril to rearrange
themselves in a more compact manner, thus enhancing the tensile
strength of the bre [46]. Following the 10, 12, and 15% alkali treatments, there is an increase in the stiffness and brittleness of the bres
and this results in the decrease in the tensile strength and Young's modulus. In the presence of the 10, 12, and 15% alkali solutions, the main
structural components of the bre were attacked, resulting in the formation of more grooves on the surface of the bre. Consequently, this
leads to further weakening of the bre strength, resulting in a decrease
in the ultimate tensile stress [42]. A similar observation was also reported by Reddy et al. [26]. Therefore, it can be concluded that the
bre treated with 5% alkali exhibits the maximum ultimate tensile
stress, and the 10, 12, and 15% alkali treatments reduced the strength
and Young's modulus of the bres but increased their fracture strain.
3.4. FTIR analysis
The FTIR spectra of the untreated and alkali-treated bres are presented in Fig. 6. From Fig. 6(a), it can be observed that the untreated
bre exhibits well-dened bands at approximately 665, 897, 1033,
1160, 1242, 1371, 1425, 1512, 1604, 1729, 2905, and 3345 cm1 within
its spectra. The small peaks at 665 cm1 associated with the COH out
of plane bending [47] and the peak at 897 cm1 can be attributed to
the presence of -glycosidic linkages between the monosaccharides
[14]. The intense band, centred at 1033 cm 1, is associated with the
CO stretching modes of the hydroxyl and ether groups in the cellulose
[19]. The peak at 1160 cm1 is associated with the COC stretching vibration of the pyranose ring in the polysaccharides [48].
The absorbance peak centred at 1242 cm 1 is owed to the CO
stretching vibration of the acetyl group in the lignin [49], whilst the
peak at 1371 cm1 is attributed to the bending vibration of the CH
group of the aromatic ring in the polysaccharides [50]. The absorbance
at 1425 cm1 is associated with the CH2 symmetric bending [51]. The
next peak at 1512 cm1 is attributed to the C=C stretching of the benzene ring of the lignin [14,52]. The peak centred at 1604 cm1 indicates
the C=C aromatic stretching with conjugated CC bond and this peak is
attributed to lignin content of the bre [20]. The absorption band

Table 2
Mechanical properties of treated and untreated Pennisetum purpureum bres. (20 samples
for each concentration).
Concentration

Ultimate tensile stress

(MPa)

Strain at break
%

Young's modulus
(GPa)

Untreated
5%
7%
10%
12%
15%

73 6
141 24
79 14
50 7
49 9
31 5

1.40 0.23
2.30 0.18
2.27 0.21
4.43 0.25
4.81 0.38
6.40 0.22

5.68 0.14
4.86 0.22
3.77 0.11
1.00 0.17
1.02 0.32
0.55 0.17

Fig. 5. Stressstrain responses for selected untreated and alkali-treated Pennisetum

purpureum bres.

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

843

the alkali-treated bres; this indicates that compositional changes had

occurred. The bands at 1242, 1512, and 1604 cm1 were present for
the untreated bre; these correspond to the lignin. However, the band
at 1729 cm1 is associated with the hemicelluloses [56].
Fig. 6(c) shows the FTIR spectra for the 10, 12, and 15% alkali-treated
bres with bands at 665, 847, 1019, 1459, 1692, and 3458 cm1. The
bands are almost completely different to those of the untreated bre;
the most signicant difference is that the peaks are smaller than those
for the 5 and 7% alkali-treated bres. The bands at 897, 1160, 1242,
1371, 1604, and 2905 cm1 disappear; these primarily correspond to

Fig. 6. FTIR (a) untreated bre, (b) 5 and 7% treated bre, (c) 10, 12, and 15% treated bre.

centred at 1729 cm1 can be attributed to the C=O stretching vibration

of the acetyl groups in the hemicelluloses [53]. The peak at 2905 cm1 is
a characteristic band for the CH stretching vibration of CH and CH2 in
the cellulose and hemicelluloses components [19]. The nal peak at
3345 cm1 is owed to the presence of OH stretching vibrations and
the hydrogen bond of the hydroxyl groups [48,54,55].
FTIR is used to determine the compositional changes that occur during the alkali treatment. The bands for the 5 and 7% alkali-treated bres
are at approximately 665, 897, 1031, 1158, 1368, 1650, and 3342 cm1,
as shown in Fig. 6(b). The bands for the 5 and 7% alkali-treated bres are
relatively similar to those of the untreated bre with little difference.
The bands at 1242, 1512, 1604, and 1729 cm 1 had disappeared for

Fig. 7. TGADTG curves (a) Untreated bre, (b) 5 and 7% treated bre, (c) 10, 12, 15%
treated bre.

844

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

3.5. TGA results

Table 3
Thermo-gravimetric analysis (TGA) of Pennisetum purpureum bre.
Sample

Untreated
5% treated
7% treated
10% treated
12% treated
15% treated

Initial Degradation

Final Degradation

Final residue

IDT (C)

% wt. loss

FDT (C)

% wt. loss

(%)

91.5
104.0
104.0
104.0
104.0
104.0

5.26
4.13
4.13
3.62
3.34
3.02

400.06
365.50
386.30
385.40
385.40
385.40

73.38
52.70
49.83
49.39
49.00
49.00

26.62
47.30
50.17
50.61
51.00
51.00

the hemicelluloses, cellulose, and lignin [56]. Therefore, the FTIR studies
demonstrate that the composition of the bres can change as the alkali
concentration increases. This observation agrees with the poor ultimate
tensile stress of the 10, 12, and 15% alkali-treated bres, as discussed in
Section 3.3.

The TGA and the derivative of thermo-gravimetric (DTG) curves for

the untreated and alkali-treated P. purpureum bres are presented in
Fig. 7. Table 3 shows the data of thermo-gravimetric analysis (TGA)
for the untreated and alkali-treated P. purpureum bres. The purpose
of this analysis is to observe the thermal degradation curves of the
hemicelluloses, cellulose and lignin. Fig. 7(a) shows the typical thermal
decomposition for the cellulose and lignin portion of the untreated bre.
Up to a temperature of 91.5 C, the initial curve indicated a moisture loss
with a weight change of approximately 5.26%. At temperatures above
230 C, degradation of the hemicellulose occurred. Up to 400.06 C,
the percentage of residue remaining was 26.62%, and approximately
73.38% had decomposed. The decomposition of the untreated
P. purpureum bre occurred in two stages. The decomposition of the cellulose initiated between 250 and 380 C and most of the volatile materials decomposed between these temperatures. Therefore, above this

Fig. 8. (af) Surface morphologies of untreated and alkali treated P. purpureum bres.

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

845

Fig. 9. (af) Cross-sectional morphologies of untreated and alkali treated P. purpureum bres.

temperature range, the remaining residues are considered to be char.

The rapid decrease in mass is owed to cellulose volatilization and this
was followed by a slow decrease in the mass of the lignin. In the DTG,
it can be observed that rapid decomposition occurs at 364.7 C; the bres start to burn and the cellulose degrades [57,58]. A peak at

approximately 306.6 C indicates the decomposition of the hemicelluloses. Typically, it is more difcult for the lignin to decompose than
the cellulose, since part of the lignin consists of benzene rings [59,60].
Fig. 7(b) demonstrates the TGADTG curves for the 5 and 7% alkalitreated bres. The initial curve between 30 and 104 C corresponds to

Table 4
Comparison of Pennisetum purpureum bre on span length, diameter, ultimate tensile stress, Young's Modulus and strain at break with other natural bres [20,44,63].
Type of Fibre

Span length
(mm)

Fibre diameter (mm)

Ultimate tensile stress (MPa)

Young's modulus (GPa)

Strain at break (%)

Untreated Pennisetum purpureum

5% treated Pennisetum purpureum
7% treated Pennisetum purpureum f
10% treated Pennisetum purpureum
12% treated Pennisetum purpureum
15% treated Pennisetum purpureum
Betel nut (Areca catechu)
Coir (Cocos nucifera)
Kenaf (Hibiscus cannabinus)

100
100
100
100
100
100
57
0.33.5
1.411

0.210.26
0.180.24
0.190.25
0.140.17
0.120.15
0.130.16
0.47
0.10.45
0.0120.036

73
141
79
50
49
31
124
106175
295930

5.68
4.86
3.77
1.00
1.02
0.55
1.28
46
2260

1.40
2.30
2.27
4.43
4.81
6.40
22.49
1747
2.76.9

846

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

the decomposition of the moisture, and the weight difference is approximately 4.13%. This demonstrates a decrease of approximately 21.5% for
the moisture content of the 5 and 7% alkali-treated bres. There was
47.3% and 50.17% of residue remaining for the 5% (up to 385.5 C) and
7% (up to 386.3 C) alkali-treated bres, respectively. This indicates
that the 5 and 7% alkali-treated bres had decomposed by approximately 52.7 and 49.83%, respectively. This implies that the reduction
of the residue is owed to the increase in the alkali concentration. The
DTG demonstrates the differences in the peaks of the 5 and 7% alkalitreated bres. For the 5% alkali-treated bres, two peaks were recorded
at 309.4 and 356.4 C while only one peak was recorded at 314.3 C for
the 7% alkali-treated bre. This occurred because an increase in the alkali concentration caused a reduction in both the hemicelluloses and
some part of the lignin in the bres.
Fig. 7(c) shows the TGA-DTG curves for the 10, 12, and 15% alkalitreated bres. The moisture contents of the 10, 12, and 15% alkalitreated bres were 3.62, 3.34, and 3.02%, respectively. It was conrmed
that the moisture content of the bres decreased as the alkali concentration increased. There was approximately 5051% residue remaining for
the 10, 12, and 15% alkali-treated bres at 385.4 C. The DTG demonstrates that only two peaks appeared at 43.33 and 310.13 C. The
TGADTG curves for all the P. purpureum bres demonstrated a reduction in the moisture content and residue following the burning of the
bres.
3.6. SEM analysis
The SEM micrographs of the surfaces of the untreated and alkalitreated P. purpureum bres are shown in Fig. 8. It was important to
study the surface morphology of the bres to observe the changes that
occurred on the surface of the P. purpureum bre because of the alkali
treatment.
The SEM images revealed that the P. purpureum bre had a multi cellular structure. Fig. 8(a) shows the SEM images of the untreated bre.
The white layer within the images represents the presence of impurities
on the surface of the bre. Fig. 8(b) shows the SEM image of the 5%
alkali-treated bre. It can be observed that this bre is cleaner than
the untreated bre because of the removal of surface impurities by the
treatment. However, some surface impurities can still be observed.
The surface impurities on the bres are soluble in the alkali solution
and this explains the cleansed surfaces [61]. Fig. 8(cd) shows the 7
and 10% alkali-treated bres. The surfaces of the 7 and 10% alkalitreated bres had a similar appearance to the 5% alkali-treated bre surface but they were cleaner with less impurities.
Fig. 8(ef) shows the 12 and 15% alkali-treated bres. The damaged
textures on the surfaces of the bres can be observed. The 15% alkalitreated bres demonstrated a more twisted and rougher surface than
the 12% alkali-treated bres. If these bres were used as reinforcement
materials in composites, these rough surfaces would be expected to promote good interfacial bonding between the bres and the matrix [29].
However, if the surfaces were rougher than a desired level, this could reduce the mechanical properties of the bres [62]. Following the elimination of the impurities as a result of the alkali treatment, it was apparent
that there was a reduction in the mass of the bre and an improvement
in the surface area of the bre.
Fig. 9 shows the cross-sectional morphologies of the untreated and
treated P. purpureum bres. As mentioned above, the P. purpureum bres exhibit a multi-cellular structure, which indicates a porous structure. A hollow cavity known as a lumen exists inside the unit of the
bre; this can be observed in Fig. 9(a). Fig. 9(bf) demonstrates that
the cellular/lumen structures disappear as the percentage of alkali treatment increases. The bres treated with 15% alkali are shown in Fig. 9(f).
They exhibit a compressed cellular/lumen structure without a void content. Furthermore, the alkali treatment destroyed the cellular/lumen
structure of the bre, and hence reduced the void content of the bres.
This can result in lower water absorption and explain the reduction of

diameter for alkali-treated bres. Therefore, the alkali treatment improves the mechanical and physical properties of the P. purpureum
bre, and thus facilitates its applications in composite structures.
3.7. Comparison between the mechanical properties of P. purpureum and
betel nut, coir and kenaf bres
Table 4 shows a comparison on the diameter, ultimate tensile stress,
Young's modulus, strain at brake and moisture content of untreated and
alkali treated P. purpureum bres with betel nut, coir and kenaf bres reported by Yusriah et al. [44]. These bres are known locally to have good
mechanical properties when used as reinforcement materials in polymer composites. The data presented suggested the mechanical properties of the 5% alkali treated P. purpureum bre are comparable to these
agricultural crops. These ndings imply that the P. purpureum bre
could be used as reinforcement in polymer composites.
4. Conclusion
The physical, mechanical, thermal, compositional, and morphological properties of P. purpureum bres were investigated. The results conrmed that there was a variation in the bre diameter following the
alkali treatment. The untreated bre exhibited the largest diameter
and the diameter further decreased as the concentration of the alkali
treatment increased. The untreated P. purpureum bres exhibited the
highest moisture content as a result of their multi-cellular structures.
Following an increase in the concentration of the alkali treatment,
there is a reduction in the moisture content because the alkali treatment
compresses the multi cellular structures and reduces the void contents
of the bres. This was conrmed by the observation of the crosssectional morphologies. The cross-sections of the P. purpureum bres
were observed. The untreated bres exhibited large lumen structures,
and there was a change in the structure following the alkali treatment.
The surface morphologies of the untreated P. purpureum bres demonstrated the presence of impurities on the surfaces of the bres. The removal of impurities by the alkali treatment results in the brillation
and cleansed surfaces of the bre. The SEM observation of the
P. purpureum bres demonstrated that the alkali treatment increased
the surface roughness of the bre. The TGA-DTG results indicate that
the alkali treatment removed the hemicelluloses of the bres. This
was further supported by the FTIR spectrometry analysis. The 5%
alkali-treated bre achieved the maximum ultimate tensile stress. The
10, 12, and 15% alkali treatments reduced the ultimate tensile stress of
the bres; this was conrmed by SEM observations, which demonstrated the damaged textures and the twisted bres. The study further
supported the feasibility of utilising P. purpureum bres as reinforcing
materials in polymer composites.
Acknowledgements
The authors would like to thank the Universiti Malaysia Perlis and
the Ministry of Education, Malaysia, for providing nancial assistance
(RAGS No.: 9018-00072). The authors are also thankful for the support
of the facility during the course of the research. In addition, the Mechanical Engineering Department of Sultan Abdul Halim Mu'adzam Shah
Polytechnic (POLIMAS), are acknowledged for their fruitful discussions
and input to the project.
References
[1] V. Kommula, O. Kanchireddy, M. Shukla, T. Marwala, Effect of Acid Treatment on the
Chemical, Structural, Thermal and Tensile Properties of Napier Grass Fibre Strands,
2014 4551psrcentre.org.
[2] A.K. Mohanty, A. Wibowo, M. Misra, L.T. Drzal, Effect of process engineering on the
performance of natural ber reinforced cellulose acetate biocomposites, Composites: Part A. 35 (2004) 363370.

M.J.M. Ridzuan et al. / Materials and Design 89 (2016) 839847

[3] V.K. Thakur, M.K. Thakur, R.K. Gupta, Synthesis of lignocellulosic polymer with improved chemical resistance through free radical polymerization, Int. J. Biol.
Macromol. 61 (2013) 121126.
[4] V.K. Thakur, M.K. Thakur, R.K. Gupta, Graft copolymers from cellulose: synthesis,
characterization and evaluation, Carbohydr. Polym. 97 (2013) 1825.
[5] V.K. Thakur, M.K. Thakur, Processing and characterization of natural cellulose bers/
thermoset polymer composites, Carbohydr. Polym. 109 (2014) 102117.
[6] U.S. Bongarde, V.D. Shinde, Review on natural ber reinforcement polymer composites, IJESIT 3 (2014) 431436.
[7] V.K. Thakur, M.K. Thakur, R.K. Gupta, Review: raw natural ber-based polymer composites, Int. J. Polym. Anal. Charact. 19 (2014) 256271.
[8] V.K. Thakur, M.K. Thakur, Recent advances in green hydrogels from lignin: a review,
Int. J. Biol. Macromol. 72 (2015) 834847.
[9] L. He, W. Li, D. Chen, D. Zhou, G. Lu, J. Yuan, Effects of amino silicone oil modication
on properties of ramie ber and ramie ber/polypropylene composites, Mater. Des.
77 (2015) 142148.
[10] F. Wang, J. Shao, L.M. Keer, L. Li, J. Zhang, The effect of elementary bre variability on
bamboo bre strength, Mater. Des. 75 (2015) 136142.
[11] J. Moothoo, S. Allaoui, P. Ouagne, D. Soulat, A study of the tensile behaviour of ax
tows and their potential for composite processing, Mater. Des. 55 (2014) 764772.
[12] I.K. Varma, D.S. Varma, M. Varma, Thermal behaviour of coir bres, Thermochim.
Acta 108 (1986) 199210.
[13] V. Fiore, T. Scalici, A. Valenza, Characterization of a new natural ber from Arundo
donax L. as potential reinforcement of polymer composites, Carbohydr. Polym. 106
(2014) 7783.
[14] I.M. De Rosa, J.M. Kenny, D. Puglia, C. Santulli, F. Sarasini, Morphological, thermal
and mechanical characterization of okra (Abelmoschus esculentus) bres as potential
reinforcement in polymer composites, Compos. Sci. Technol. 70 (2010) 116122.
[15] K. Prashant, Mechanical behavior of jute bers and their composites, Indian J.
Technol. 24 (1986) 2932.
[16] P.K. Pal, Jute reinforced plastics: a low cost composite material, Plast. Rubber Process. Appl. 4 (1984) 215219.
[17] J.M. Lawther, R. Sun, W.B. Banks, Fractional characterization of alkali-labile lignin
and alkali-insoluble lignin from wheat straw, Ind. Crop. Prod. 5 (1996) 291300.
[18] R. Sun, M.J. Lawther, W.B. Banks, Fractional and structural characterization of
wheatstraw hemicelluloses, Carbohydr. Polym. 29 (1996) 325331.
[19] M.C. Paiva, I. Ammar, A.R. Campos, R.B. Cheikh, A.M. Cunha, Alfa bres: mechanical,
morphological and interfacial characterization, Compos. Sci. Technol. 67 (2007)
11321138.
[20] S. Indran, R.E. Raj, V.S. Sreenivasan, Characterization of new natural cellulosic ber
from Cissus quadrangularis root, Carbohydr. Polym. 110 (2014) 423429.
[21] K. Obi Reddy, C. Uma Maheswari, M. Shukla, J.I. Song, A. Varada Rajulu, Tensile and
structural characterization of alkali treated Borassus fruit ne bers, Compos. Part B
Eng. 44 (2013) 433438.
[22] M.K. Thakur, R.K. Gupta, V.K. Thakur, Surface modication of cellulose using silane
coupling agent, Carbohydr. Polym. 111 (2014) 849855.
[23] C. Girisha, G.R. Srinivas, Sisal/coconut coir natural bers epoxy composites: water
absorption and mechanical properties, International Journal of Engineering and Innovative Technology (IJEIT) 2 (2012) 166170.
[24] O. Faruk, A.K. Bledzki, H.P. Fink, M. Sain, Biocomposites reinforced with natural bers: 20002010, Prog. Polym. Sci. 37 (2012) 15521596.
[25] X. Li, L. Tabil, S. Panigrahi, Chemical treatments of natural ber for use in natural
ber-reinforced composites: a review, J. Polym. Environ. 15 (2007) 2533.
[26] K.O. Reddy, C.U. Maheswari, M. Shukla, A.V. Rajulu, Chemical composition and structural characterization of napier grass bers, Mater. Lett. 67 (2012) 3538.
[27] A.K. Bledzki, J. Gassan, Composites reinforced with cellulose based bres, Prog.
Polym. Sci. 24 (1999) 221274.
[28] R.D. Ray, B.K. Sarkar, R.K. Basak, A.K. Rana, Study of the thermal behavior of alkalitreated jute bers, J. Appl. Polym. Sci. 85 (2002) 25942599.
[29] L.Y. Mwaikambo, M.P. Ansell, Chemical modication of hemp, sisal, jute, and kapok
bers by alkalization, J. Appl. Polym. Sci. 84 (2002) 22222234.
[30] R. Zuluaga, J.L. Putaux, J. Cruz, J. Vlez, I. Mondragon, P. Gan, Cellulose microbrils
from banana rachis: effect of alkaline treatments on structural and morphological
features, Carbohydr. Polym. 76 (2009) 5159.
[31] H. Gu, Tensile behaviours of the coir bre and related composites after NaOH treatment, Mater. Des. 30 (2009) 39313934.
[32] K.O. Reddy, C.U. Maheswari, D.J.P. Reddy, A.V. Rajulu, Thermal properties of napier
grass bers, Mater. Lett. 63 (2009) 23902392.
[33] D. Ray, B.K. Sarkar, A.K. Rana, N.R. Bose, Mechanical properties of vinylester resin
matrix composites reinforced with alkali-treated jute bres, Compos. Part A Appl.
Sci. Manuf. 32 (2001) 119127.
[34] K. Murali Mohan Rao, K. Mohana Rao, A.V. Ratna Prasad, Fabrication and testing of
natural bre composites: vakka, sisal, bamboo and banana, Mater. Des. 31 (2010)
508513.
[35] Z. Liu, S.Z. Erhan, D.E. Akin, F.E. Barton, Green composites from renewable resources: preparation of epoxidized soybean oil and ax ber composites, J. Agric.
Food Chem. 54 (2006) 21342137.

847

[36] V.K. Thakur, M.K. Thakur, R.K. Gupta, Rapid synthesis of graft copolymers from natural cellulose bers, Carbohydr. Polym. 98 (2013) 820828.
[37] M.J. Haameem, M.S. Abdul Majid, M. Haslan, M. Afendi, E.A. Helmi, F. Idris, Effects of
alkaline treatments on the tensile strength of napier grass bres, Appl. Mech. Mater.
695 (2014) 340343.
[38] O. R. Kanchireddy and E. Muzenda, Effect of ber surface treatments on the tensile
properties of polycarbonate-coated napier grass bers, International Conference on
Research in Science, Engineering and Technology (ICRSET2014), March 2122,
2014 Dubai (UAE).
[39] R. Mahjoub, J.M. Yatim, A.R. Mohd Sam, S.H. Hashemi, Tensile properties of kenaf
ber due to various conditions of chemical ber surface modications, Constr.
Build. Mater. 55 (2014) 103113.
[40] S.M. Mortazavi, M. Kamali Moghaddam, An analysis of structure and properties of a
natural cellulosic ber (Learan), Fibers Polym. 11 (2010) 877882.
[41] S. T. Method, Standard Test Method for Tensile Properties of Single Textile Fibers,
2013 110.
[42] A. Roy, S. Chakraborty, S.P. Kundu, R.K. Basak, S. Basu Majumder, B. Adhikari, Improvement in mechanical properties of jute bres through mild alkali treatment
as demonstrated by utilisation of the Weibull distribution mode, Bioresour. Technol.
107 (2012) 222228.
[43] M.M. Kabir, H. Wang, K.T. Lau, F. Cardona, Tensile properties of chemically treated
hemp bres as reinforcement for composites, Compos. Part B Eng. 53 (2013)
362368.
[44] L. Yusriah, S.M. Sapuan, E.S. Zainudin, M. Mariatti, Characterization of physical, mechanical, thermal and morphological properties of agro-waste betel nut (Areca catechu) husk bre, J. Clean. Prod. 72 (2014) 174180.
[45] K. Goda, M.S. Sreekala, A. Gomes, T. Kaji, J. Ohgi, Improvement of plant based natural
bers for toughening green compositeseffect of load application during mercerization of ramie bers, Compos. Part A Appl. Sci. Manuf. 37 (2006) 22132220.
[46] E.T.N. Bisanda, Effect of alkali treatment on the adhesion characteristics of sisal bres, Appl. Compos. Mater. 7 (2000) 331339.
[47] A. Bezazi, A. Belaadi, M. Bourchak, F. Scarpa, K. Boba, Novel extraction techniques,
chemical and mechanical characterisation of Agave americana L. natural bres,
Compos. Part B Eng. 66 (2014) 194203.
[48] H. Yang, R. Yan, H. Chen, D.H. Lee, C. Zheng, Characteristics of hemicellulose, cellulose and lignin pyrolysis, Fuel 86 (2007) 17811788.
[49] W. Liu, A.K. Mohanty, L.T. Drzal, P. Askel, M. Misra, Effects of alkali treatment on the
structure, morphology and thermal properties of native grass bers as reinforcements for polymer matrix composites, J. Mater. Sci. 39 (2004) 10511054.
[50] M. Le Troedec, D. Sedan, C. Peyratout, J.P. Bonnet, A. Smith, R. Guinebretiere, V.
Gloaguen, P. Krausz, Inuence of various chemical treatments on the composition
and structure of hemp bres, Compos. Part A Appl. Sci. Manuf. 39 (2008) 514522.
[51] N. Sgriccia, M.C. Hawley, M. Misra, Characterization of natural ber surfaces and natural ber composites, Compos. Part A Appl. Sci. Manuf. 39 (2008) 16321637.
[52] S.S. Saravanakumar, A. Kumaravel, T. Nagarajan, P. Sudhakar, R. Baskaran, Characterization of a novel natural cellulosic ber from Prosopis juliora bark, Carbohydr.
Polym. 92 (2013) 19281933.
[53] J. Biagiotti, D. Puglia, L. Torre, J.M. Kenny, A. Arbelaiz, G. Cantero, C. Marieta, R. LlanoPonte, I. Mondragon, A systematic investigation on the inuence of the chemical
treatment of natural bers on the properties of their polymer matrix composites,
Polym. Compos. 25 (2004) 470479.
[54] J. Jayaramudu, B.R. Guduri, A. Varada Rajulu, Characterization of new natural cellulosic fabric Grewia tilifolia, Carbohydr. Polym. 79 (2010) 847851.
[55] Y. Seki, M. Sarikanat, K. Sever, C. Durmukahya, Extraction and properties of Ferula
communis (chakshir) bers as novel reinforcement for composites materials,
Compos. Part B Eng. 44 (2013) 517523.
[56] F. Xu, J. Yu, T. Tesso, F. Dowell, D. Wang, Qualitative and quantitative analysis of lignocellulosic biomass using infrared techniques: a mini-review, Appl. Energy 104
(2013) 801809.
[57] N. Sgriccia, M.C. Hawley, Thermal, morphological, and electrical characterization of
microwave processed natural ber composites, Compos. Sci. Technol. 67 (2007)
19861991.
[58] Z.N. Azwa, B.F. Yousif, A.C. Manalo, W. Karunasena, A review on the degradability of
polymeric composites based on natural bres, Mater. Des. 47 (2013) 424442.
[59] R.K. Sharma, J.B. Wooten, V.L. Baliga, X. Lin, W.G. Chan, M.R. Hajaligol, Characterization of chars from pyrolysis of lignin, Fuel 83 (2004) 14691482.
[60] A. Gani, I. Naruse, Effect of cellulose and lignin content on pyrolysis and combustion
characteristics for several types of biomass, Renew. Energy 32 (2007) 649661.
[61] L. Boopathi, P.S. Sampath, K. Mylsamy, Investigation of physical, chemical and mechanical properties of raw and alkali treated Borassus fruit ber, Compos. Part B
Eng. 43 (2012) 30443052.
[62] I. Taha, G. Ziegmann, A comparison of mechanical properties of natural ber lled
biodegradable and polyolen polymers, J. Compos. Mater. 40 (2006) 19331946.
[63] T. Gurunathan, S. Mohanty, S.K. Nayak, A review of the recent developments in
biocomposites based on natural bres and their application perspectives, Compos.
Part A Appl. Sci. Manuf. 77 (2015) 125.