MECHANICAL TESTING 555

Effects of abaca fiber reinforcement

on the dynamic mechanical
behavior of vinyl ester composites
Anandraj Mohan Kumar, The present study aims in analyzing the mechanical behavior of natural
Rathinasamy Parameshwaran, fiber (abaca) reinforced polymeric composites under dynamic condi-
Tamil Nadu, Palaniappan Sathish tions. It is evident from the past research reports that natural fiber
Kumar, Samir Kumar Pal, West offers desirable physico-mechanical properties to the added polymers.
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017

Bengal, Mani Mohan Prasath, In the present research work, abaca fiber is utilized for the preparation
Vijayan Krishnaraj and of composites due to its promising mechanical properties and resistance
Rathanasamy Rajasekar, Tamil to salt water corrosion, its lignin content is 15 % and grows up to 3 m.
Nadu, India Abaca is extracted from leaf sheath of Manila hemp plant, it is a kind of
banana family. Influence of temperature on the mechanical behavior of
natural fibers needs to be identified to ensure its usage for high perfor-
mance applications. Pure and chemically treated abaca fiber based vinyl
For personal use only.

ester composites are subjected to dynamic mechanical analysis (DMA).

Article Information
Correspondence Address
Dr. Rathanasamy Rajasekar
Faculty of Mechanical Engineering
Kongu Engineering College
Perundurai
638052, Tamil Nadu, India
E-mail: rajasekar_cr@yahoo.com
Keywords
Composites, abaca fiber, vinyl ester, dynamic
mechanical properties, surface treatment
The reason for the chemical treatment of abaca fiber is to enhance its
interfacial bonding with base matrix. Fourier transform infrared spec-
troscopy (FT-IR) analysis signifies the morphological changes in abaca
fiber after chemical treatment. Storage modulus (E’) and damping
characteristics of abaca fiber reinforced vinyl ester composites are
comparatively higher than in neat polymer. In addition, surface treat-
ment of fiber demonstrates significant enhancement in storage modulus
compound compared to pure and raw fiber reinforced polymer due to
strong physical interaction between fiber and matrix.

Today, many conventional metals and mate-
rials have been replaced by fiber reinforced
polymers due to decrease in greenhouse ef-
fect to the environment. Outstanding phys-
ico-mechanical properties like high specific
strength, modulus and dimensional stability
of the fiber reinforced composites finds ap-
plications in automotive interior, helmets,
paneling, roofing, storage tank, packaging
material, post boxes, carpets, blankets,
mobs, canvas, ropes and furnitures. The ma-
jor parameters that influence the properties
of a composite material are fiber character-
istics, content, orientation, interaction with
matrix, mode of testing, etc. [1].
Several morphological and technical anal-
yses had been carried out to ensure the sig-
nificance of developed composite materials
for specified applications. Composite mate-
rials designed for application under varying
environmental conditions should possess
adequate dynamic mechanical properties.
Dynamic mechanical analysis (DMA) serves
as a sensitive and important tool to deter-
mine the storage modulus (E’), loss modulus
(E’’) and damping factor (tan δ) with respect
to temperature [2]. Transition temperature
of the vinyl and ethylene vinyl acetate in the
grafted kenaf filled poly (vinyl chloride)/
ethylene vinyl acetate composite shifted to
higher temperature with the increased con-
tent of kenaf fiber [3].
The results of the reports based on the
DMA analysis of glass and carbon fibers re-
inforced polymer composites are in higher
dimensions [1]. Some of the researchers re-
ported that the properties of fiber/matrix in-
terface and level of interaction between
them have been interpreted using DMA re-
sults. DMA studies based on synthetic fiber
reinforced composites have been extensively
reported, but mechanical performance of
natural fiber reinforced composites under
dynamic conditions constitutes in lesser di-
mension. Basic characteristics and few ex-
cellent works carried out on natural fiber
reinforced polymeric composites are pre-
sented as follows. Natural fibers are of great
interest due to their unique advantages like
low cost, abundant availability, renewabil-
ity, low density, high specific properties and
biodegradable characteristics [3-5].
The major class of natural fibers, i. e.,
plant fibers, contains cellulose, hemicellu-
lose, pectin and lignin. Natural fibers are
classified into three categories such as
seed hair, bast fibers and leaf fibers. Coco-

59 (2017) 6  © Carl Hanser Verlag, München  Materials Testing

 556 MECHANICAL TESTING
nut belongs to the seed or fruit fibers, coir used in natural fiber reinforced polymeric
is light and hairy. The most common bast composites [4]. Extensive research on sur-
fibers are jute, flax, ramie, hemp and oil face modification of natural fibers has al-
palm. The leaf fibers like sisal, abaca and ready been reported by several researchers
banana are rough. Based on all the fibers, [7]. Hamma et al. analyzed kenaf fiber as-
the most eminent fibers are banana, abaca, pect ratio influencing the thermal and me-
cotton, jute, ramie, flax and sisal [6]. chanical properties of composites [8].
Abaca fiber (musatextilis) is extracted The enhancement in E’ and decrease in
from the trunk of musa sepintum plant and tan δ peak intensity were observed for the
the world’s largest producer is the Republic treated fiber composites compared to un-
of the Philippines. It is also known as Ma- treated fiber composites proving enhance-
nila hemp. The abaca plant belongs to ment in reinforcing efficiency of fiber after
Musaceae, Genus Musa of banana family. surface treatment. Chen et al. concluded
Based on the Indian review, the yield of that E’ and E’’ of poly(butylene succinate)
abaca fiber is 24,875 tons per annum. Ow- composites filled with nano-sized calcium
ing to its wide variety of applications, high carbonate are considerably improved when
strength and flexural properties, it acts as a content of nano-sized calcium carbonate is
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017
good reinforcement for many composite increased up to not more than 3 wt.-% [9].
materials. It is cheap and finds application For the different concentrations (0.25 and
in twines, handicraft goods, ropes, teabags, 1 wt.-%/vol.-%) of alkali and silane treated
sinamay weaving and decorative papers. sisal fiber polyesters composites, it was re-
However, their increase in moisture absorp- ported that the higher value of E’ was ob-
tion and poor wettability with resins leads served at a lower temperature compared to
to weak fiber/matrix interface interaction control specimens. The maximum E’ was
and results in low technical properties. To obtained for untreated silane reinforced
overcome this weakness, a suitable surface fiber composites. Silva et al. observed simi-
modification of the fibers is required prior lar trend of E’ for neat matrix and short sisal
For personal use only.
to composite preparation. The simplest and fiber composites at low temperature [10].
most effective surface modification tech- However, the same composites depicted a
niques is alkali treatment which is widely pronounced effect at high temperature. The
tan δ shifted towards lower temperature and
their corresponding peak intensity was re-
Vinyl Abaca NaOH
duced. However, tan δ peak shifted towards
Sample ester fiber (wt.-%/
(wt.-%) (wt.-%) vol.-%) higher temperature with subsequent in-
crease in peak intensity for untreated wo-
V 100 – –
ven fiber composites. Fiber length and fiber
C1 90 10 – content influence E’ and E’’, but do not
C2 80 20 – change geometric progression [11]. The in-
C3 70 30 – creased addition of flax content showed en-
C4 60 40 – hancement in E’ and reduction in the tan δ
peak values.
4C1 90 10 4
Vijay Kumar Thakur and Amar Singh Sin-
6C1 90 10 6
gha observed that particle composite exhib-
8C1 90 10 8 ited good mechanical properties compared
10C1 90 10 10 to long and short fiber composites [12].
4C2 80 20 4 Fathi et al. observed that the fiber treatment
increased magnitude of E’ [13]. However,
6C2 80 20 6
increase in fiber loading led to enhancement
8C2 80 20 8
in E’’ and corresponding tan δ peak shifted
10C2 80 20 10 towards higher temperature. The compatibi-
4C3 70 30 4 lized system with high fiber content showed
6C3 70 30 6 higher efficiency at elevated temperature. A
small tiny hump above the glass transition
8C3 70 30 8
temperature (Tg) tends their movement to-
10C3 70 30 10
wards the dry cellulose. Pothan et al. re-
4C4 60 40 4 ported the DMA of two, three and four lay-
6C4 60 40 6 ered banana/glass fiber woven-fabric rein-
8C4 60 40 8 forced polyester composites [14]. Gupta et
10C4 60 40 10
al. concluded that maximum values of E’
and E’’ were obtained with 30 wt.-% of jute
Table 1: Sample compositions and sisal fiber in hybrid composite [15].
Developed cyanoethylated jute fiber/poly-
ester composites showed high E’ and as-
cending trend of Tg shift. Esterification reac-
tion of unsaturated monocarboxylic acid
with epoxy resin was carried out to extract
vinyl ester resin. In the present investiga-
tion, the values of E’, E’’ and tan δ of neat
and surface treated abaca fiber reinforced
vinyl ester composites was analyzed. In or-
der to enhance the bonding strength of ma-
trix and fiber, the surface treatment was
carried out using sodium hydroxide (NaOH)
solution. The obtained results showed high
E’ and damping characteristics for surface
treated abaca reinforced vinyl ester compos-
ites compared to untreated fiber based com-
posites and neat polymer.
Experimental procedure
Materials. Vinyl ester resin (POLYFLEX
GR 200-60, pale brownish liquid, Brooke-
field viscosity @ 25 °C = 325 cps, density
@ 25 °C = 1.052 gm × cm-3, volatile con-
tent = 41.8 %) is supplied from Naptha Res-
ins and Chemicals (P) Limited, Bangalore,
India. Abaca fibers (Manila hemp, musa tex-
tilis) were purchased from Maruthi Peach
Finishing Company, Tirupur, Tamil Nadu,
India. Alkali solution (NaOH) for fiber sur-
face treatment, resin curing system cobalt
(accelerator) and methyl ethyl ketone perox-
ide (MEKP) used as catalyst were purchased
from Sigma Aldrich Co. Ltd., India.
Preparation of composites. Prior to the
preparation of composites, both resin and
fiber had been dried at 80 °C and 50 °C un-
der vacuum for 2 h in order to remove the
moisture content [16]. The compositions of
vinyl ester and abaca fiber are listed in Ta-
ble 1. Pure and abaca fiber reinforced vinyl
ester composites were prepared by hand
lay-up method followed by compression
molding process. Abaca fibers were unidi-
rectionally oriented in the vinyl ester ma-
trix. The steel rollers were used to maintain
the uniform orientation of fibers in the com-
posites. After this process, the molds were
closed and kept in hydraulic press under
the compressive force for 4 h to obtain a
single mat. Curing reaction was carried out
by adding 1 vol.-% of cobalt and MEKP in
vinyl ester resin and cured at room tem-
perature for 24 h. Dimensions of the pre-
pared specimens are 300 × 300 × 3 mm3.
Alkali treatment. Different weight frac-
tions of abaca fibers were immersed in 4, 6,
8 and 10 wt.-%/vol.-% of NaOH solution at
room temperature for 2 h [16]. Further, the
fibers were washed several times with dis-
tilled water containing few drops of acetic
59 (2017) 6

acid to remove alkali fragments sticking on
the fiber surface. A final pH value of 7 was
maintained. Then, the fibers were dried un-
der sunlight for 3 days.
Dynamical mechanical analysis (DMA).
The E’, E’’ and tan δ of pure vinyl ester and
abaca fiber reinforced vinyl ester compos-
ites were determined as a function of tem-
perature (40-160 °C). DMA 2980 (TA in-
strument, New Castle DE, USA) equipped
with dual-cantilever bending fixture was
used. Testing was performed at a frequency
of 1 Hz, strain amplitude of 10 μm and
heating rate of 5 °C × min-1. Dimensions of
specimens are 35 × 10 × 4 mm3.
Fourier transformation infrared spec-
troscopy (FT-IR). The chemical bonding
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017
existing in the abaca fibers before and after
alkali treatment was analyzed using FT-IR
spectroscopy (Nexus 870, Thermo Nicolet
Corporation, Madison, WI, USA). Transmit-
tance value was measured in the range
from 4000 to 700 cm-1.
Results and discussion
Dynamic mechanical analysis. The E’, E’’
For personal use only.
and tan δ of pure vinyl ester, raw and
chemically treated abaca fiber reinforced
vinyl ester composites with varying fiber
content are shown in Figures 1 to 15.
Effect of weight fraction on storage modu-
lus (E’) with temperature. The E’ curve as a
function of temperature for a polymeric ma-
terial typically consists of three regions,
namely glassy, transition and rubbery. For
vinyl ester resin, the glassy region com-
pletes at 60 °C and further transition is
shifted to the rubbery region at 90 °C. The
variation in E’ with respect to temperature
has been analyzed for pure and raw abaca
fiber reinforced vinyl ester composites (see
Figure 1: E’ of pure and raw abaca fiber reinforced vinyl ester
59 (2017) 6
Figure 1). In the glassy region (at 50 °C), the
specimens C1 and C2 shows higher E’,
whereas C3 and C4 shows drop in E’ com-
pared to V. Composites C1 and C2 shows 7 %
and 30 % increase, C3 and C4 shows 8 % and
9.6 % decrease in E’ compared to V. The
fiber-matrix interaction of C3 and C4 does
not shows any strong effect on E’ up to 60 °C.
However, the E’ values exhibit a uniform
trend above 70 °C. At 100 °C, the compos-
ites C1, C2, C3, C4 shows 1090, 1715, 2112
and 2053 % enhancement in E’ compared to
neat vinyl ester. Similarly at 150 °C, the
composites C1, C2, C3, C4 shows 957, 1950,
2403 and 2149 % improvement in E’ com-
pared to control specimen. This proves that,
in the rubbery region, the polymer-fiber and
fiber-fiber interactions have a marked effect
on E’ value. Addition of abaca fiber up to
30 wt.-% (C3) shows a gradual increase in E’.
The reason may be due to proper wetting of
fibers with resin causing fiber-matrix adhe-
sion. E’ starts to drop for composite C4,
which may be due to insufficient resin con-
tent unsuccessful to wet entire fibers
(40 wt.-%), thereby causing poor fiber-ma-
trix adhesion and nonuniform orientation of
fibers at few spots in the matrix.
Effect of weight fraction on loss modu-
lus (E’’) with temperature. The changes in
E’’ for pure and raw abaca fiber reinforced
vinyl esters are shown in Figure 2. The
neat matrix shows the peak at 71.7 °C with
E’’ value of 187.5 MPa caused by the mobil-
ity of the resin molecules. This peak has
also been considered as the glass transition
temperature (Tg) of the resin [1]. The peak
value of composites C1, C2, C3 and C4 is
shifted towards higher temperature (74.0,
76.2, 77.7 and 74.6 °C) which could be due
to the immobilization of polymer molecules
near the surface of abaca fibers [1]. The E’’
Figure 2: E’’ of pure and raw abaca fiber reinforced vinyl ester
MECHANICAL TESTING 557
value of composites C1, C2, C3, C4 are
195.2, 205.4, 227.7 and 211.2 MPa. Com-
pared to control specimen, composites
show high E’’ value due to fiber content
and extent of reinforcement in the matrix.
C4 shows low E’’ compared to C3. Reinforc-
ing efficiency of fibers with the resin con-
secutively decreases at 40 wt.-% loading
compared to 30 wt.-%. The broadening of
E’’ peaks with increase in the fiber content
up to 30 wt.-% could be due to increase in
energy absorption of the composites [1].
Effect of weight fraction on loss factor
(tan δ) with temperature. Figure 3 demon-
strates the tan δ of neat resin and raw
abaca fiber reinforced vinyl ester compos-
ites. Tan δ is the ratio of loss modulus to
storage modulus (E’’/E’). Neat resin shows
Tg peak at 80.3 °C with the corresponding
peak intensity of 0.76. Composites C1, C2,
C3, C4 shows Tg peak at 81.9, 83.1, 85.1,
83.9 °C with corresponding peak intensi-
ties at 0.55, 0.41, 0.38 and 0.40, respec-
tively. The fiber-matrix interfacial interac-
tion restricts their molecular mobility
which leads to enhancement in tan δ [17].
Compared to pure compound, the Tg of
composites is shifted towards higher tem-
perature with the consecutive reduction in
peak intensities. However, C4 shows unu-
sual trend compared to C3. This could be
attributed to the good reinforcing efficiency
of fiber to the added matrix up to 30 wt.-%
(C3). High content of fiber (40 wt.-%) addi-
tion in the resin (C4) may lead to lack of
physical bonding between the two compo-
nents at few spots. The reduction in tan δ
peak intensities implies minimum heat
buildup of the composites materials and
indeed promising damping characteristics.
Necessity to undergo surface treatment
of fiber. Rough fiber surface involves pene-
 558 MECHANICAL TESTING
tration of resin into micropores, thereby en-
hancing its reinforcing efficiency with the
matrix. Walls of abaca fiber are covered with
a layer consisting of substances like hemicel-
lulose, lignin and other impurities. Alkali
surface treatment is intended to reduce the
hydrogen bonding in cellulose hydroxyl
groups by the removal of the carboxyl groups
[4]. However, the removal of lignin is a key
step to ultimately develop high modulus
composites. It is observed that the treatment
leads to removal of fiber surface debris re-
sulting in rougher surface morphology. This
will develop mechanical interlocking and
bonding reaction due to exposure of hydroxyl
groups to the matrix, thereby shows better
fiber-matrix interfacial adhesion compared
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017
to raw fiber reinforced composites. Surface of
treated composites indicates the longer pla-
teau on the E’ compared to neat resin. As a
result: (i) the interfacial interaction between
the fiber and matrix decreases the chain mo-
For personal use only.
Figure 3: Tan δ of pure and raw abaca fiber reinforced vinyl ester
Figure 5: E’ of pure, untreated and treated abaca fiber (20 wt.-%)
reinforced vinyl ester
bility, (ii) the effective contact surface area
with the matrix is higher and (iii) the load is
transferred between the matrix and fiber [4].
Effect of fiber surface treatment on stor-
age modulus (E’) of composites. Figures 4 to
7 show the effect of surface treatment on the
E’ of the prepared composite materials. The
significance of alkali surface treatment such
as disruption of hydrogen bonding in the
fiber surface increases the surface rough-
ness. The alkali treatment improves the fiber
matrix interaction by the removal of lignin
and hemicellulose, which leads to the better
incorporation of fiber onto the matrix [4].
Figure 4 shows 10 wt.-% addition of raw
and NaOH (varying  wt.-%/vol.-%) treated
abaca fiber based vinyl ester composites.
The values for E’ at varying temperatures
are presented herewith. Composites 4C1,
6C1, 8C1, 10C1 show increment in E’ of 45,
25, 28 and 10 % at 50 °C, 24, 47, 77 and 18 %
at 100 °C, and 61, 70, 87 and 39 % at 150 °C
Figure 4: E’ of pure, untreated and treated abaca fiber (10 wt.-%)
reinforced vinyl ester
Figure 6: E’ of pure, untreated and treated abaca fiber (30 wt.-%)
reinforced vinyl ester
compared to raw abaca fiber composites.
NaOH treated abaca fiber reinforced compos-
ites exhibit an increase in E’ compared to C1
proving better fiber-matrix adhesion after
fiber surface treatment. 8C1 exhibits high E’
compared to the rest of the specimens.
Composites containing 20, 30 and 40 wt.-%
of raw and NaOH (varying wt.-%/vol.-%)
treated abaca fiber based vinyl ester com-
posites are presented in Figures 5 to 7.
Similar trend in E’ could be inferred for the
composites. Composites with 30  wt.-%
abaca fiber (chemically treated) content
namely 4C3, 6C3, 8C3, 10C3 depict E’ of
1112, 1586, 2808 and 1110 MPa at 50 °C,
158.5, 175.1, 190.7 and 148.1 MPa at
100  °C, and 156.0, 150.4, 134.1 and
125.7 MPa at 150 °C. Composites 8C2 (see
Figure 5), 8C3 (see Figure 6) and 8C4 (see
Figure 7) shows high values for E’ com-
pared to their respective batches at 100 °C.
Hence, 8  wt.-%/vol.-% of NaOH treated
59 (2017) 6

abaca fiber reinforced vinyl ester compos-
ites display maximum attainment of E’. De-
sired surface roughness could have been
achieved by the removal of hemicellulose
and lignin content from the fiber surface,
which indeed creates micropores and con-
traction of cellulose as well. Rough fiber
surface creates strong physical bonding
with the matrix. This involves contribution
of fiber in enhancing the E’ of the compos-
ite material. High concentration of NaOH
treatment (10  wt.-%/vol.-%) with fiber
shows a drop in E’. Excess content of NaOH
may strongly influence the technical prop-
erties of fiber, which indeed affects the ul-
timate strength of the composites. Hence,
optimum fiber content of 30 wt.-% and opti-
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017
mal NaOH concentration of 8 wt.-%/vol.-%
have been determined to obtain significant
enhancement in E’ of the composites.
Effect of surface treatment on loss mod-
ulus (E’’) with temperature. Figures 8 to
For personal use only.
Figure 7: E’ of pure, untreated and treated abaca fiber (40 wt.-%)
reinforced vinyl ester
Figure 9: E’’ of pure, untreated and treated abaca fiber (20 wt.-%)
reinforced vinyl ester
59 (2017) 6
11 explain the variation of E’’ of the pure
vinyl ester and its composites in depend-
ence of temperature. E’’ is a measure of the
energy dissipated or lost as heat per cycle
of sinusoidal deformation. So, the loss fac-
tors are very sensible to molecular mo-
tions. E’’ value is the measure of viscous
response of the material and indicates the
portion of material that will flow under
stress. The Tg obtained from E’’ curves are
displayed in the figures. However, Tg is
represented as the peak of the E’’ curves
found during DMA [16]. The Tg obtained
from E’’ curves for neat vinyl ester is
71.7 °C, whereas the composites 4C, 6C,
8C and 10C show Tg of around 75.1, 77.0,
77.8 and 77.3 °C for 10 wt.-% fiber loading
and 76.9, 77.7, 78.7 and 77.3  °C for
20 wt.-% fiber reinforced composites. In ad-
dition, 30 wt.-% fiber content indicates Tg
for the composites 4C, 6C, 8C and 10C of
about 78.9, 79.9, 80.9 and 79.0 °C as well
Figure 8: E’’ of pure, untreated and treated abaca fiber (10 wt.-%)
reinforced vinyl ester
Figure 10: E’’ of pure, untreated and treated abaca fiber (30 wt.-%)
reinforced vinyl ester
MECHANICAL TESTING 559
as 40 wt.-% abaca loading results in Tg of
76.7, 77.7, 78.8 and 77.5 °C, respectively.
The transition peaks in the composites
could be explained by the mobility of the
loosely bound chains away from the inter-
face and the slight increase in temperature
(from 71.7 °C for the neat resin to approxi-
mately 80.9 °C for the composites 8C3)
could be caused by the restricted mobility
of the chains compared to the neat [7].
Based on the above results, the Tg shifts
towards higher temperature are due to the
presence of alkali treated fiber in the matrix.
The Tg shifts occur because of the decreased
mobility of the matrix chains that indicates
enhanced interfacial interaction between the
fibers and the matrix achieved by the cou-
pling effect of NaOH. The most pronounced
effect of the treated fiber has been achieved
owing to broadening of the transition region
and maximum enhancement of E’’ peak val-
ues. Also, the maximum E’’ peak values show
 560 MECHANICAL TESTING
similar trend for the raw and alkali treated
abaca fiber reinforced composites. Further-
more, the stress field surrounding the parti-
cles induces the shift in Tg and improvement
in E’’ values [18]. It is evident that the E’’
peak values shows increasing trend with in-
crease in alkali content up to the sample 8C
and high concentration of NaOH treatment
(10C) shows drop in E’’ value for the treated
fiber reinforced composites. The sample 8C3
(optimum fiber content and NaOH concentra-
tion) exhibits a shift to higher Tg obtaining
maximum improvement in E’’ values com-
pared to the rest of the specimens.
Effect of surface treatment on loss factor
(tan δ) with temperature. Figures 12 to 15
displays tan δ and peak intensity of neat
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017
resin, raw and chemically treated abaca
fiber reinforced vinyl ester composites as a
function of temperature. In the transition
region (60-90 °C), tan δ measures the im-
perfections in the elasticity of a polymer
For personal use only.
Figure 11: E’’ of pure, untreated and treated abaca fiber (40 wt.-%)
reinforced vinyl ester
Figure 13: Tan δ of pure, untreated and treated abaca fiber (20 wt.-%)
reinforced vinyl ester
with the theory of additional losses occur-
ring at the matrix-fiber interface [16]. It is
evident that the neat resin shows Tg at
80.3 °C with the peak intensity of 0.76,
whereas the Tg and peak intensity of the un-
treated composites are already discussed.
The chemically treated fiber reinforced
composites have a shift of their Tg towards
higher temperature with the consecutive
reduction in peak intensities, which is in
accordance with the E’’ curves. Composites
4C1, 6C1, 8C1 and 10C1 show Tg at 82.2,
82.3, 83.4 and 83.2 °C with corresponding
peak intensities at 0.44, 0.37, 0.34 and
0.41, respectively. Similarly, the samples
4C2, 6C2, 8C2 and 10C2 results in en-
hancement in Tg around 1.4, 2.3, 2.5 and
1.1 % compared to C2 with peak intensities
at 0.39, 0.37, 0.32 and 0.41, respectively.
Composites with 30  wt.-% abaca fiber
(chemically treated) content namely 4C3,
6C3, 8C3 and 10C3 depict tan δ peak at
Figure 12: Tan δ of pure, untreated and treated abaca fiber (10 wt.-%)
reinforced vinyl ester
Figure 14: Tan δ of pure, untreated and treated abaca fiber (30 wt.-%)
reinforced vinyl ester
85.2, 85.5, 86.6 and 85.4 °C with intensi-
ties at 0.37, 0.36, 0.31 and 0.39, respec-
tively. Likewise, complete removal of cel-
lulose and lignin content from the fiber
leads to poor interfacial adhesion due to
higher content (40 wt.-%) of fiber loading
as indicated by Tg at 84.1, 85.0, 85.1 and
84.5 °C with peak intensities at 0.38, 0.38,
0.34 and 0.37 for the composite samples
4C4, 6C4, 8C4 and 10C4. Composites 8C1
(see Figure 12), 8C2 (see Figure 13), 8C3
(see Figure 14) and 8C4 (see Figure 15)
have a shift of Tg towards higher tempera-
ture compared to respective batches of
abaca fiber concentration. Hence, 8 wt.-%/
vol.-% of NaOH treated abaca fiber rein-
forced vinyl ester composites display maxi-
mum reduction in peak intensities. The re-
duction in tan δ peak intensities implies
minimum heat buildup of the composites
materials and indeed promising damping
characteristics. However, the composites
59 (2017) 6

Figure 15: Tan δ of pure, untreated and treated abaca fiber (40 wt.-%)
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017
reinforced vinyl ester
with 10 wt.-%/vol.-% of NaOH concentra-
tion (10C1, 10C2, 10C3 and 10C4) show an
unusual trend compared to 8 wt.-%/vol.-%
of NaOH treatment. Hence, optimum fiber
content of 30 wt.-% and optimal NaOH con-
centration of 8 wt.-%/vol.-% have been de-
termined to obtain significant enhance-
ment in tan δ and reduction in peak inten-
For personal use only.
sities of the composites. Similarly, all the
results are in the same trend with Tg from E’’
curves. It can also be explained by the physi-
cal interaction between them. Moreover, the
removal of the lignin and cellulose in abaca
fiber observed by FT-IR analysis leads to a
change in the extent of hydrogen bonding af-
fecting Tg and tan δ peak intensity.
Fourier transform infrared spectroscopy
(FT-IR). The FT-IR spectra of raw and alkali
treated abaca fiber are shown in Figure 16.
Pure fiber shows distinct bands at 3362,
2926, 1731, 1643, 1316, 1258 and 1032 cm-
1. The broad transmittance band observed at
3362.2 cm-1 is related to the hydrogen bond-
ing stretching vibration, 2926.5 cm-1 is re-
lated to C–H aliphatic stretching (present in
many natural fibers), 1731  cm-1 and
1316 cm-1 are caused by CH2 bending
(α-cellulose), 1643.8 cm-1 implies the pres-
ence of lignin, 1258.2 cm-1 is attributed to
C = O stretch of acetyl group and 1032 cm-1
belongs to hydroxyl group of cellulose [4].
Surface treated (NaOH solution) abaca fiber
(8 wt.-%/vol.-%) shows decrease in peak in-
tensity at 2926.5 cm-1 and 1316 cm-1, which
may be due to removal of hemicellulose.
Peak originated at 1731 cm-1 for raw fiber
disappears after alkali treatment implying
complete removal of hemicellulose from the
fiber. Peak at 1643.8 cm-1 and 1258.2 cm-1
shows reduction in intensities after fiber
treatment indicating the removal of lignin
content from the fiber surface. Decrease in
59 (2017) 6
Figure 16: FTIR spectra of raw and treated (8 wt.-%/vol.-%) abaca fiber
peak intensity at 1032 cm-1 shows poor hy-
drogen bonding in cellulose hydroxyl groups
by the removal of carboxyl group [4].
Conclusions
The E’, E’’ and tan δ of pure and chemically
surface treated abaca fiber based vinyl ester
composites were investigated. The chemical
treatment of abaca fiber showed improved
interfacial adhesion between the fiber and
base matrix. Compared to pure compound,
the untreated composites C3 attain higher E’
(161.5 MPa at 100 °C), E’’ (227.7 MPa) and
show maximum shift in Tg towards higher
temperature (85.1 °C) with significant re-
duction in peak intensities (0.38). After sur-
face treatment, the fibers were finer, having
less hemicellulose and lignin content (struc-
tural changes) which was confirmed by FT-
IR analysis showing reduced amount of de-
fects resulting in superior bonding with the
matrix. Compared to raw and chemically
treated fiber reinforced composites, the sam-
ples (8C3) show the maximum enhancement
in E’ value (190.7 °C) at higher temperature.
Tg of neat resin from tan δ curve is 80.3 °C
and loss modulus curve is 71.7 °C, whereas
chemically treated abaca fiber based com-
posites (8C3) depict maximum enhance-
ment in Tg towards higher temperature ow-
ing to the restricted mobility of the resin
molecules due to the presence of fibers.
Composite C4 shows an unusual trend in
both raw and alkali treated fiber reinforced
composites compared to C3. The shift in tan
δ towards higher temperature and reduction
in peak intensities indicate minimum heat
buildup and better damping characteristics
of the prepared composite materials. Finally,
it is evident that the surface treated abaca
fiber based vinyl ester composites are suita-
MECHANICAL TESTING 561
ble for preparation of very high performance
application materials possessing useful en-
gineering properties and appropriate damp-
ing behavior.
References
 1 D. Ray, B. K. Sarkar, S. Das, A. K. Rana: Dynamic
mechanical and thermal analysis of vinyl ester-
resin-matrix composites reinforced with un-
treated and alkali treated jute fibers, Composite
Science and Technology 62 (2002), pp. 911-917
DOI:10.1016/S0266-3538(02)00005-2
 2 K. V. Mahesh Kumar, K. Krishnamurthy,
P. Sathish Kumar, S. Sahoo, E. Uddin, S. K. Pal,
R. Rajasekar: Research updates on graphene
oxide based polymeric nanocomposites, Poly-
mer Composites 35 (2014), pp. 2297-2310
DOI:10.1002/pc.22899
 3 N. A. Bakar, Ching Yern Chee, Luqman Chuah
Abdullah, Chantara Thevy Ratnam, Nor Azowa
Ibrahim: Thermal and dynamic mechanical
properties of grafted kenaf filled poly (vinyl
chloride)/ethylene vinyl acetate composites,
Materials Design 65 (2015), pp. 204-211
DOI:10.1016/j.matdes.2014.09.027
 4 A. Benyahia, A. Merrouche, M. Rokbi, Z. Kouadri:
Study the effect of alkali treatment of natural
fibers on the mechanical behavior of the com-
posite unsaturated Polyester-fiber Alfa, Proc.
of the 21st Congress Francais de Mecanique,
Bordeaux, France (2013), pp. 1-6
 5 R. Sivashankar, P. Sathish Kumar,
S. A. Srinivasan, S. Shankar, R. Rajasekar,
R. Naveen Kumar: Review article on wheat
flour/wheat bran/wheat husk based biocom-
posites, International Journal of Science and
Research Publication 4 (2014), pp. 1-9
 6 S. Ramakrishnan, K. Krishnamurthy,
M. Mohan Prasath, R. Sarath Kumar,
M. Dharmaraj, K. Gowthaman, P. Sathish
Kumar, R. Rajasekar: Theoretical prediction on
the mechanical behavior of natural fiber rein-
forced vinyl ester composites, Applied Science
and Advanced Materials International 1
(2015), pp. 85-92
 7 D. Ray, S. P. Sengupta: Static and dynamic me-
chanical properties of vinyl ester resin matrix
composites reinforced with shellac treated jute
yarns, Industrial and Engineering Chemistry
Research 45 (2015), pp. 2722-2727
DOI:10.1021/ie0512800
 562 MECHANICAL TESTING
 8 A. Hamma, M. Kaci, Z. A. MohdIshak,
R. Ceccato, A. Pegoretti: Starch-grafted-poly-
propylene/kenaf fibers composites – Part 2:
Thermal stability and dynamic-mechanical
response, Journal of Reinforced Plastic
Composites 34 (2015), pp. 2045-2058
DOI:10.1177/0731684415609792
 9 R.-Y. Chen, W. Zou, H.-C. Zhang,G.-Z. Zhang,
Z.-T. Yang, J. Gang, J.-P. Qu: Thermal behavior,
dynamic mechanical properties and rheologi-
cal properties of poly(butylene succinate) com-
posites filled with nanometer calcium carbon-
ate, Polymer Testing 42 (2015), pp. 160-167
DOI:10.1016/j.polymertesting.2015.01.015
10 R. V. Silva, M. M. Ueki, D. Spinelli, W. W. Bose
Filho, J. R. Tarpani: Thermal, mechanical and hy-
groscopic behavior of sisal fiber/polyurethane
resin-based composites, Journal of Reinforced
Plastic Composites 29 (2010), pp. 1399-1417
DOI:10.1177/0731684409102986
11 V. S. Sreenivasan, N. Rajini, A. Alavudeen,
V. Arumugaprabu: Dynamic mechanical and
Materials Testing downloaded from www.hanser-elibrary.com by Hanser - Library on June 6, 2017
thermo-gravimetric analysis of Sansevieria cylin-
drical/polyester composite: Effect of fiber length,
fiber loading and chemical treatment, Composites
Part B – Engineering 69 (2015), pp. 76-86
DOI:10.1016/j.compositesb.2014.09.025
12 Vijay Kumar Thakur, Amar Singh Singha: Phys-
ico-chemical and mechanical characterization of
natural fibre reinforced polymer composites, Ira-
nian Polymer Journal 19 (2010), pp. 3-16
13 B. Fathi, M. Esfandeh, A. Khalifeh Soltani,
H. Taghavian: Effect of corona discharge treat-
ment on dynamic mechanical properties of
For personal use only.
unsaturated polyester/carbon fiber pultruded,
Composites 53 (2014), pp. 162-166
DOI:10.1080/03602559.2013.843703
14 L. A. Pothan, P. Potschke, S. Thomas: The
static and dynamic mechanical properties
of banana and glass fiber woven fabric rein-
forced polyester composites, Proc. of the
ACUN-3, Australia (2001), pp. 452-460
15 M. K. Gupta, R. K. Srivastava: Effect of sisal
fiber loading on dynamic mechanical analysis
and water absorption behavior of jute fiber
epoxy composite, Proc. of the 4th International
Conference on Materials Processing and Char-
acterization, Materials Today: Proceedings 2
(2015), pp. 2909-2917
DOI:10.1016/j.matpr.2015.07.253
16 S. Masud Huda, T. Lawrence, K. Drzal, Amar
Mohanty, Manjusri Misra: Effect of fiber sur-
face treatments on the properties of laminated
biocomposites from poly(lactic acid) (PLA) and
kenaf fibers, Composites Science and Technol-
ogy 68 (2008), pp. 424-432
DOI:10.1016/j.compscitech.2007.06.022
17 R. Rajasekar, Kaushik Pal, Gert Henrich, Amit
Das, C. K. Das: Development of nitrile butadi-
ene rubber-nanoclay composites with epoxi-
dized natural rubber as compatibilizer,
Materials Design 30 (2009), pp. 3839-3845
DOI:10.1016/j.matdes.2009.03.014
18 S. Masud Huda, T. Lawrence, K. Drzal, Amar
Mohanty, Manjusri Misra: Chopped glass and
recycled newspaper as reinforcement fibers in
injection molded poly(lactic acid) (PLA) com-
posites: A comparative study, Composites Sci-
ence and Technology 66 (2006), pp. 1813-1824
DOI:10.1016/j.compscitech.2005.10.015
Bibliography
DOI 10.3139/120.111044
Materials Testing
59 (2017) 6, pages 555-562
© Carl Hanser Verlag GmbH & Co. KG
ISSN 0025-5300
Abstract
Auswirkung der Abaka-Faserverstärkung auf das dynamische mechani-
sche Verhalten von Vinylester-Kompositen. Die diesem Beitrag zugrunde
liegende Studie zielt darauf ab, das mechanische Verhalten von naturfaser-
verstärkten (Abaka) Polymerkompositen unter dynamischen Bedingungen
zu analysieren. Es ist aus vergangenen Forschungsberichten bewiesen,
dass Naturfasern die erforderlichen physikalisch-mechanischen Eigen-
schaften für die hinzugegebenen Polymere bereitstellen. In der vorliegen-
den Forschungsarbeit wurden Abaka-Fasern verwendet, um Komposite her-
zustellen, da diese vielversprechende mechanische Eigenschaften und Re-
sistenz gegenüber Salzwasserkorrosion aufzeigen, wobei der Ligningehalt
15 % betrug und bis zu 3 m anwuchs. Abaka wird von dem Blattschuh der
Manila-Hanfpflanze extrahiert, die eine Art der Bananenfamilie darstellt. Es
ist notwendig, den Einfluss der Temperatur auf das mechanische Verhalten
der Naturfasern zu identifizieren, um ihre Nutzung für High-Perfomance-
Anwendungen sicher zu stellen. Es wurden reine und auf chemisch behan-
delte Abaka-Faser basierende Vinylester-Komposite dynamischen mecha-
nischen Analysen (Dynamic Mechanical Analysis – DMA) unterworfen. Der
Grund der chemischen Behandlung der Abaka-Faser ist es, ihre Grenzflä-
chenbindung mit der Basismatrix zu steigern. Die Analyse mittels Fourier-
Transformations-Infrarotspektroskopie (FT-IR) zeigt die morphologischen
Veränderungen in der Abaka-Faser nach der chemischen Behandlung. Der
Speichermodul (E’) und die Dämpfungscharakteristika der abakafaserver-
stärkten Vinylester-Komposite sind vergleichsweise höher als des ur-
sprünglichen Polymers. Zusätzlich zeigt die Oberflächenbehandlung der
Faser eine signifikante Steigerung des Speichermodules im Vergleich zum
reinen und rohfaserverstärkten Polymer aufgrund der starken physikali-
schen Wechselwirkung zwischen Faser und Matrix.
The authors of this contribution Engineering, Indian Institute of Technology,
Kharagpur, West Bengal. Since 1981, he has been
Anandraj Mohan Kumar, born in 1984, completed working as a member of the faculty in the Depart-
his B.E in Mechanical Engineering at the Erode ment of Mining Engineering, Indian Institute of
Sengunthar Engineering College, Tamil Nadu, In- Technology in Kharagpur. 
dia, in 2006. He obtained his M.E degree in Com- Dr. Vijayan Krishnaraj, obtained his BEng,
puter Aided Design at the Government College of MEng and PhD in the field of drilling of composites
Engineering, Salem, Tamil Nadu, India in 2010. in 1994, 1999 and 2007, respectively. He also com-
He is currently working as Assistant Professor in pleted his postdoc in France in 2008 and 2009.
the Department of Mechanical Engineering at Currently, he is working as Associate Professor in
Kongu Engineering College, Tamil Nadu, India. the Department of Production Engineering, PSG
Dr. Rathinasamy Parameshwaran, born in 1976, College of Technology, Tamil Nadu, India.
obtained his PhD degree at Kongu Engineering Col- Mani Mohan Prasath, born in 1991, finished his
lege, Perundurai, in Performance Management in Bachelor’s degree in Engineering (mechanical
2009. He gained his Master’s degree in Industrial stream) at KSR College of Engineering, Tiruchengode,
Engineering at Regional Engineering College, Tamil Nadu, India in 2013. He received his Master of
Trichy, Tamil Nadu, India. He is working as Head Engineering at Kongu Engineering College, Tamil
and Professor in the Department of Mechatronics Nadu, India which he finished in 2015 with distinc-
Engineering at Kongu Engineering College, India. tion in the stream of engineering design. Currently,
Palaniappan Sathish Kumar, born in 1991, he is pursuing PhD in Universiti Teknologi Malaysia.
finished his Bachelor’s degree in Engineering Dr. Rathanasamy Rajasekar, born in 1982, ob-
(mechanical stream) at University College of En- tained his MS and PhD degrees at Indian Institute
gineering Villupuram (A Constituent College of of Technology, Kharagpur, in Materials Science in
Anna University, Chennai), Tamil Nadu, India in 2008 and 2011, respectively. He gained postdoc-
2012. He received his Master of Engineering toral research experience in the Department of
from Kongu Engineering College, Tamil Nadu, Polymer & Nano Engineering at Chonbuk Na-
India, which he finished in 2014 with distinc- tional University, South Korea in 2011 and 2012.
tion in the stream of CAD/CAM. Since 2012, he has been working as Associate
Prof. Samir Kumar Pal completed his B.Tech, Professor in the Department of Mechanical Engi-
M.Tech and his PhD in the Department of Mining neering at Kongu Engineering College, India.
59 (2017) 6